Method for recovering polyethylene terephthalate by using selected raw materials

Abstract

A process for producing a first intermediate product comprising the steps of: a. Providing a feedstock comprising a first polyester wherein the first polyester in the feedstock is in the form of a plurality of fragments; b. Contacting the raw material in a volume section V1 with a first amount of a first organic compound to obtain a first initial mixture wherein the first amount is in liquid form; c. Contacting the first polyester with a further organic compound, preferably in volume segment V3, to obtain a further initial mixture; d. Reducing the weight average molar mass of the first polyester, preferably in the volume segment V3, to obtain a first intermediate mixture comprising: i. The first intermediate product, ii. Another organic compound; wherein 30 wt% or less, more preferably 27 wt% or less, even more preferably 23 wt% or less, and further preferably 20 wt% or less of the fragments have a thickness equal to or greater than 1.0 mm, based on the total mass of the plurality of fragments in the feedstock.

Description

Field of the Invention

[0001] The present invention relates to a method for producing a first intermediate product from a first polyester, for example, a method for producing a polyethylene terephthalate (PET) oligomer from a PET flake. The present invention also relates to a first intermediate product obtained by the above method. The present invention also relates to a method for producing another intermediate product using the first intermediate product, for example, using a PET oligomer to produce a PET polymer. The present invention also relates to another intermediate product. The present invention also relates to a product comprising another intermediate product, for example, a PET yarn.

[0002] background

[0003] Polyethylene terephthalate (PET) is one of the most widely used and economically important thermoplastic polymers. PET is used, for example, in clothing fibers, food and beverage containers (such as bottles) and films.

[0004] Due to the widespread use of PET and its non-biodegradability, products containing PET have caused serious ecological problems. Therefore, methods for recycling PET are very important for reducing the amount of PET waste. One recycling method is to reduce PET to chemical components used to produce PET, and then polymerize the chemical components to obtain recycled PET. This is called chemical recycling. The disadvantages of the chemical recycling process include that the recycling process is usually very energy-saving, not environmentally friendly, and has low yields. In particular, if PET is depolymerized into monomers, a long depolymerization time is required and a large amount of degradation products that cannot be removed from the recycled PET are produced. It is also usually necessary to mix the chemically recycled PET with the original PET to obtain a recycled PET product of sufficiently high quality.

[0005] For example, chemical recycling of polyethylene terephthalate is described in Bartolome et al. (2012), Recent Developments in the Chemical Recycling of PET, Material Recycling–Trends and Perspectives. EP3778744A1 discloses a method for recycling PET, comprising mixing virgin PET liquid material with recycled PET (virgin PET liquid material is defined as the chemical components required to produce virgin PET, i.e. PET obtained without using a recycling method). CN109134244 A discloses a method for recycling PET, which uses ethylene glycol and methanol to depolymerize PET. CN108395373 A discloses a method for recycling PET, which uses ethylene glycol and propylene glycol.

[0006] Purpose

[0007] It is an object of the present invention to at least partially overcome at least one of the disadvantages encountered in the prior art.

[0008] Another object of the present invention is to provide a method for producing a first intermediate product, wherein the method provides improved control over the heating rate of the first polyester.The first intermediate product is obtained from the first polyester.

[0009] Another object of the present invention is to provide a method for producing a first intermediate product, wherein the method provides improvement in embrittlement of the first polyester.The first intermediate product is obtained from the first polyester.

[0010] Another object of the present invention is to provide a method of producing a first intermediate product, wherein the method provides a greater reduction in the intrinsic viscosity of the first polyester.The first intermediate product is obtained from the first polyester.

[0011] Another object of the present invention is to provide a method for producing a first intermediate product, wherein the method provides a reduction in the depolymerization time of the first polyester.The first intermediate product is obtained from the first polyester.

[0012] Another object of the present invention is to provide a method for producing a first intermediate product, wherein the method provides for an increase in the useful life of one or more filters used in a plant for producing the first intermediate product.

[0013] Another object of the present invention is to provide a method for producing a first intermediate product, wherein the method can remove more impurities during the production of the first intermediate product. The impurity source includes a raw material (for the method for producing the first intermediate product) containing impurities such as sand and polyvinyl chloride.

[0014] Another object of the present invention is to provide a method for producing a first intermediate product, wherein the method can remove more alkali during the production of the first intermediate product. The presence of alkali may be due to, for example, the raw material (used in the method for producing the first intermediate product) having been washed with alkali.

[0015] Another object of the present invention is to provide a method for producing a first intermediate product, wherein the method can more effectively remove a binder adhering to a raw material (a method for producing a first intermediate product).

[0016] Another object of the present invention is to provide a method for producing a first intermediate product, wherein the transport rate of the raw material through the production plant is increased. Here, the raw material refers to the raw material of the method for producing the first intermediate product, and the production plant refers to the plant for producing the first intermediate product.

[0017] Another object of the present invention is to provide a method for producing a first intermediate product, wherein the method has an increased transportation efficiency through the plant, for example, the number of blockages occurring in a production plant for producing the first intermediate product when transporting, for example, raw materials, a first polyester, a first intermediate product or another intermediate product is reduced.

[0018] Another object of the present invention is to provide a method for producing a first intermediate product which requires less energy.

[0019] Another object of the present invention is to provide a method for producing a first intermediate product, wherein the method has an increased yield.

[0020] It is another object of the present invention to provide a method for producing a first intermediate product, wherein the method has a reduced carbon footprint.

[0021] Another object of the present invention is to provide a method for producing a first intermediate product, wherein the first intermediate product has an improved purity.

[0022] Another object of the present invention is to provide a method for producing a first intermediate product, wherein the method reduces degradation of the first intermediate product.

[0023] Another object of the present invention is to provide a first intermediate product that can be used in a process for producing another intermediate product.

[0024] Another object of the present invention is to provide a method for producing another intermediate product, wherein the method requires less energy.

[0025] It is another object of the present invention to provide a process for producing another intermediate product, wherein the process has a reduced carbon footprint.

[0026] Another object of the present invention is to provide a method for producing another intermediate product, wherein the method has an increased yield.

[0027] Another object of the present invention is to provide a process for producing another intermediate product, wherein the process has a reduced polymerization time.

[0028] Another object of the present invention is to provide a method for producing another intermediate product, wherein the another intermediate product has improved color quality.

[0029] Another object of the present invention is to provide a method for producing a further intermediate product, wherein the further intermediate product has an improved purity.

[0030] Another object of the present invention is to provide a method for producing another intermediate product, wherein the another intermediate product has improved strength.

[0031] Another object of the present invention is to provide another intermediate product having improved color quality.

[0032] Another object of the present invention is to provide another intermediate product with improved purity.

[0033] Another object of the present invention is to provide another intermediate product which has improved strength.

[0034] Another object of the present invention is to provide a method for producing another intermediate product, wherein the another intermediate product is obtained by using an increased amount of a first intermediate product. For example, the another intermediate product is a PET polymer obtained by polymerizing PET oligomers and PET monomers (first intermediate product), wherein the PET oligomers and PET monomers are obtained by depolymerization of PET products; and further, the PET polymer is obtained by adding less than 1% of original PET oligomers and esters that can be used to produce PET.

[0035] Preferred embodiments of the present invention

[0036] Any embodiment of the present invention helps to at least partially achieve at least one of the above objectives.

[0037] The first embodiment of the present invention is a method for producing a first intermediate product, comprising the following steps:

[0038] a. providing a raw material comprising a first polyester, wherein the first polyester in the raw material is in the form of a plurality of fragments;

[0039] b. In volume segment V 1 contacting the feedstock with a first amount of a first organic compound to obtain a first initial mixture, wherein the first amount is in liquid form;

[0040] c. contacting the first polyester with another organic compound, preferably in volume segment V 3 to obtain another initial mixture;

[0041] d. reducing the weight average molar mass of the first polyester, preferably in the volume segment V 3 to obtain a first intermediate mixture, wherein the first intermediate mixture comprises

[0042] i. The first intermediate product,

[0043] ii. another organic compound;

[0044] in,

[0045] Based on the total mass of the plurality of fragments in the raw material, 30 wt-% or less, more preferably 27 wt-% or less, even more preferably 23 wt-% or less, and further preferably 20 wt-% or less of the fragments have a thickness equal to or greater than 1.0 mm.

[0046] In an optional aspect of the first embodiment, based on the total mass of the plurality of fragments in the feedstock, fragments in the range of 1 wt-% to 30 wt-%, optionally in the range of 2 wt-% to 27 wt-%, optionally in the range of 5 wt-% to 23 wt-%, or optionally in the range of 7 wt-% to 20 wt-% have a thickness equal to or greater than 1.0 mm. In one aspect of the first embodiment, preferably, the wt-% range applies to fragments having a thickness in the range of 1.0 mm to 4.0 mm, more preferably in the range of 1.0 mm to 3.5 mm, and further preferably in the range of 1.0 mm to 2.7 mm. In one aspect of the first embodiment, preferably, the first intermediate mixture further comprises a first organic compound. In one aspect of the first embodiment, preferably, the other organic compound is in liquid form. In one aspect of the first embodiment, preferably, before the feedstock is contacted with the first amount of the first organic compound, at least a portion of the first amount of the first organic compound is introduced into the volume segment V. 1 In this regard, it is preferred that the volume section V 1 The temperature of at least a portion of the first amount of the first organic compound fed into the first polyester is in the range of 100° C. to 160° C., more preferably in the range of 115° C. to 145° C. In one aspect of the first embodiment, the first polyester is preferably fed to the volume segment V before the feedstock is contacted with the first amount of the first organic compound. 1 In this regard, it is preferred that the volume section V 1 The temperature of the first polyester fed in the volume section V is in the range of 0° C. to 60° C., more preferably in the range of 10° C. to 40° C. In one aspect of the first embodiment, it is preferred that before the feedstock is contacted with the first amount of the first organic compound, at least a portion of the first amount of the first organic compound and the feedstock are separately fed into the volume section V 1 For example, the first volume portion and the raw material are fed to the volume segment V using different inlets. 1 Medium feed.

[0047] In a preferred embodiment of the method for producing the first intermediate product, the density of the first polyester in the raw material is 1.25 g / cm 3 Up to 1.55g / cm 3 In the range of 1.28 g / cm 3 Up to 1.50g / cm 3 and further preferably within the range of 1.31 g / cm 3 Up to 1.47g / cm 3 This preferred embodiment is the second embodiment of the present invention, which is preferably dependent on the first embodiment of the present invention.

[0048] In one aspect of the second embodiment, the first polyester is an example of a polyester having a density of 1.33 g / cm 3 Up to 1.39g / cm 3 Amorphous PET in the range of 1.455 g / cm 3 Single crystal PET.

[0049] In a preferred embodiment of the method for producing the first intermediate product, the first polyester is selected from polyethylene terephthalate, polybutylene terephthalate, polylactic acid, polytrimethylene terephthalate, polyethylene naphthalate, polycarbonate, polyester carbonate, polyarylate, polyester resin (preferably unsaturated polyester resin) and a combination of two or more thereof. This preferred embodiment is the third embodiment of the present invention, which is preferably dependent on any one of the first to second embodiments of the present invention.

[0050] In one aspect of the third embodiment, it is particularly preferred that the first polyester is polyethylene terephthalate.

[0051] In a preferred embodiment of the method for producing the first intermediate product, the raw material contains at least 65 wt-%, more preferably at least 85 wt-%, even more preferably at least 95 wt-%, and further preferably at least 99 wt-% of the first polyester based on the total mass of the raw material. This preferred embodiment is the fourth embodiment of the present invention, which is preferably dependent on any one of the first to third embodiments of the present invention.

[0052] In one aspect of the fourth embodiment, the first polyester is preferably polyethylene terephthalate. In another aspect of the fourth embodiment, the feedstock preferably contains less than 1 wt-%, more preferably less than 0.1 wt-%, and further preferably less than 0.01 wt-% of polyamide, based on the total mass of the feedstock.

[0053] In a preferred embodiment of the method for producing the first intermediate product, the bulk density of the raw material is between 0.10 g / cm 3 Up to 0.75g / cm 3 In the range of 0.15 g / cm 3 Up to 0.65g / cm 3 In the range of 0.18 g / cm 3 Up to 0.50g / cm 3 In the range of 0.20 g / cm 3 Up to 0.40g / cm 3 In the range of 0.22 g / cm 3 Up to 0.37g / cm 3 This preferred embodiment is the fifth embodiment of the present invention, which is preferably dependent on any one of the first to fourth embodiments of the present invention.

[0054] In a preferred embodiment of the method for producing the first intermediate product, the raw material further comprises at least one impurity. This preferred embodiment is the sixth embodiment of the present invention, which preferably depends on any one of the first to fifth embodiments of the present invention.

[0055] In a preferred embodiment of the method for producing the first intermediate product, at least one impurity in the raw material is in the range of 10 ppm wt to 10000 ppm wt, more preferably in the range of 20 ppm wt to 4000 ppm wt, even more preferably in the range of 30 ppm wt to 3000 ppm wt, and further preferably in the range of 40 ppm wt to 2500 ppm wt, wherein the mass is based on the total mass of the raw material. This preferred embodiment is the 7th embodiment of the present invention, which is preferably dependent on the 6th embodiment of the present invention.

[0056] In one aspect of the seventh embodiment, the ppm value of at least one impurity is preferably measured after the raw material has been subjected to a washing step. In another aspect of the seventh embodiment, the ppm value given for at least one impurity is preferably measured when the first polyester is provided in the form of a plurality of chips.

[0057] In a preferred embodiment of the method for producing the first intermediate product, the form of the fragments is selected from flakes, wires, fibers, particles, fragments, sheets, films, and combinations of two or more thereof. This preferred embodiment is the 8th embodiment of the present invention, which is preferably dependent on any one of the 1st to 7th embodiments of the present invention.

[0058] In one aspect of the eighth embodiment, a thin sheet is particularly preferred.

[0059] In a preferred embodiment of the method for producing a first intermediate product, at least 50 wt-%, more preferably at least 60 wt-%, even more preferably at least 70 wt-%, further preferably at least 80 wt-%, even further preferably at least 85 wt-% of the fragments have at least one or all of the following properties, based on the total mass of the plurality of fragments in the feedstock:

[0060] a. The first dimension is in the range of 0.1 mm to 25.0 mm, more preferably in the range of 0.5 mm to 20.0 mm, even more preferably in the range of 1.0 mm to 15.0 mm, and further preferably in the range of 2.5 mm to 13 mm;

[0061] b. The thickness is in the range of 0.1 mm to 3.5 mm, more preferably in the range of 0.2 mm to 3.0 mm, and further preferably in the range of 0.3 mm to 2.7 mm.

[0062] This preferred embodiment is the 9th embodiment of the present invention, which is preferably dependent on any one of the 1st to 8th embodiments of the present invention.

[0063] Examples of the first dimension in the ninth embodiment are width and length. In one aspect of the ninth embodiment, all possible combinations of features a. and b. are preferred aspects of this embodiment. These combinations are, for example, a; b; a+b.

[0064] In a preferred embodiment of the method for producing a first intermediate product, the plurality of fragments are sorted at least in part according to physical characteristics. This preferred embodiment is the 10th embodiment of the present invention, which preferably depends on any one of the 1st to 9th embodiments of the present invention.

[0065] In one aspect of the tenth embodiment, the fragments are preferably at least partially sorted based on at least one of the following properties: mass, thickness, color, optical sorting based on light absorption, electrical properties, aerodynamic properties, width, length, geometry (e.g., curvature), or a combination of two or more thereof. In one aspect of the tenth embodiment, the sorting is preferably performed prior to contacting the feedstock with the first amount of the first organic compound. In one aspect of the tenth embodiment, the physical property is preferably not the density of the fragments.

[0066] In a preferred embodiment of the method for producing a first intermediate product, the plurality of fragments are at least partially sorted using at least one or all of the following:

[0067] a. sieve;

[0068] b. Gravity separator;

[0069] c. means suitable and arranged for settling;

[0070] d. Centrifuge.

[0071] This preferred embodiment is the 11th embodiment of the present invention, which is preferably dependent on the 10th embodiment of the present invention.

[0072] In one aspect of the 11th embodiment, all possible combinations of features a. to d. are preferred aspects of this embodiment. These combinations are, for example, a; b; c; d; a+b; a+c; a+d; b+c; b+d; c+d; a+b+c; a+b+d; a+c+d; b+c+d; a+b+c+d. In one aspect of the 11th embodiment, it is preferred to use a device that does not utilize the density of the first polyester for the above-mentioned at least partial classification. In one aspect of the 11th embodiment, a gravity separator is particularly preferred. In this aspect, a gravity separator that does not require a fluid for at least partial classification is more preferred. Suitable gravity separators can be obtained, for example, from Cimbria Heid GmbH (Austria).

[0073] In a preferred embodiment of the method for producing a first intermediate product, the first organic compound has at least one or all of the following characteristics:

[0074] a. comprising at least two hydroxyl groups, for example a diol having 2 hydroxyl groups, a triol having 3 hydroxyl groups;

[0075] b. The molar mass is at least 60 g / mol;

[0076] c. A boiling point of at least 192°C, more preferably at least 195°C.

[0077] This preferred embodiment is the 12th embodiment of the present invention, which is preferably dependent on any one of the 1st to 11th embodiments of the present invention.

[0078] Examples of the first organic compound include (mono)ethylene glycol, propylene glycol and glycerol. In one aspect of the twelfth embodiment, all possible combinations of features a. to c. are preferred aspects of this embodiment. These combinations are, for example, a; b; c; a+b; a+c; b+c; a+b+c. In one aspect of the twelfth embodiment, it is particularly preferred that the first organic compound is (mono)ethylene glycol, more preferably monoethylene glycol. In one aspect of the twelfth embodiment, it is particularly preferred that the first organic compound is not propylene glycol.

[0079] In a preferred embodiment of the method for producing a first intermediate product, the volume segment V 1 The temperature of the first initial mixture in the range of 50° C. to 90° C., more preferably in the range of 55° C. to 85° C., even more preferably in the range of 55° C. to 80° C., further preferably in the range of 60° C. to 80° C., and even further preferably in the range of 65° C. to 77° C. This preferred embodiment is the 13th embodiment of the present invention, which preferably depends on any one of the 1st to 12th embodiments of the present invention.

[0080] In one aspect of the 13th embodiment, it is particularly preferred that the temperature of the first initial mixture is lower than the glass transition temperature of the first polyester. In one aspect of the 13th embodiment, it is preferred that the volume segment V 1 The temperature and volume of the first polyester in the segment V 1 The temperature of the first organic compound in the reaction mixture differs by less than 4%, more preferably by less than 2%, and further preferably by less than 1%.

[0081] In a preferred embodiment of the method for producing a first intermediate product, the volume segment V 1The mass ratio of the raw material (more preferably the first polyester) to the first organic compound is preferably in the range of 0.02 to 3, more preferably in the range of 0.04 to 2.8, even more preferably in the range of 0.06 to 2.6, further preferably in the range of 0.08 to 2.4, even further preferably in the range of 0.09 to 2.2. This preferred embodiment is the 14th embodiment of the present invention, which is preferably dependent on any one of the 1st to 13th embodiments of the present invention.

[0082] In one aspect of the 14th embodiment, the volume segment V 1 The mass ratio of the raw material (more preferably the first polyester) to the first organic compound is preferably in the range of 0.02 to 1.3, more preferably in the range of 0.04 to 0.5, even more preferably in the range of 0.06 to 0.28, further preferably in the range of 0.08 to 0.22, even more preferably in the range of 0.09 to 0.16. In one aspect of the 14th embodiment, the volume segment V is preferably 1 The temperature in the volume segment V is in the range of 55°C to 80°C. In one aspect of the 14th embodiment, it is more preferred that the volume segment V 1 The temperature in the volume is lower than 79° C. In one aspect of the 14th embodiment, the volume segment V 1 The temperature in the range of 65°C to 77°C.

[0083] In a preferred embodiment of the method for producing a first intermediate product, the volume segment V 1 The intrinsic viscosity of the first polyester in the present invention is in the range of 0.50 dL / g to 1.00 dL / g, more preferably in the range of 0.60 dL / g to 0.95 dL / g, even more preferably in the range of 0.70 dL / g to 0.90 dL / g, and further preferably in the range of 0.76 dL / g to 0.84 dL / g. This preferred embodiment is the 15th embodiment of the present invention, which is preferably dependent on any one of the 1st to 14th embodiments of the present invention.

[0084] In a preferred embodiment of the method for producing a first intermediate product, in volume segment V 1 The intrinsic viscosity of the first polyester in the present invention varies by less than 15%, more preferably less than 10%, even more preferably less than 7%, further preferably less than 5%, even further preferably less than 3%.

[0085] This preferred embodiment is the 16th embodiment of the present invention, which is preferably dependent on any one of the 1st to 15th embodiments of the present invention.

[0086] In a preferred embodiment of the method for producing a first intermediate product, in volume segment V 1The weight average molar mass of the first polyester in the present invention varies by less than 20%, more preferably less than 15%, even more preferably less than 10%, further preferably less than 7%, even further preferably less than 5%.

[0087] This preferred embodiment is the 17th embodiment of the present invention, which is preferably dependent on any one of the 1st to 16th embodiments of the present invention.

[0088] In one aspect of the 17th embodiment, all possible combinations of features a. and b. are preferred aspects of this embodiment. These combinations are, for example, a; b; a+b.

[0089] In a preferred embodiment of the method for producing the first intermediate product, at least one or all of the following apply:

[0090] a. before contacting with the first amount of the first organic compound, the weight average molar mass of the first polyester is in the range of 50 000Da to 73 000Da, more preferably in the range of 54 000Da to 68 000Da, and further preferably in the range of 57000Da to 65 000Da;

[0091] b. Leave volume segment V 1 The weight average molar mass of the first polyester is in the range of 40 000 Da to 76 000 Da, more preferably in the range of 44 000 Da to 74 000 Da, even more preferably in the range of 48 000 Da to 72 000 Da, and further preferably in the range of 50 000 Da to 70 000 Da.

[0092] This preferred embodiment is the 18th embodiment of the present invention, which is preferably dependent on any one of the 1st to 17th embodiments of the present invention.

[0093] In one aspect of the 18th embodiment, all possible combinations of features a. and b. are preferred aspects of this embodiment. These combinations are, for example, a; b; a+b. In one aspect of the 18th embodiment, it is preferred to leave the volume segment V 1 The weight average molar mass of the first polyester is in the range of 51 000 Da to 55 000 Da.

[0094] In a preferred embodiment of the method for producing the first intermediate product, the number of particles per unit area of ​​at least one impurity in the raw material is proportional to the volume segment V 1 The relative proportion of the number of particles per unit area of ​​at least one impurity at the outlet is equal to or greater than 15, more preferably equal to or greater than 20, even more preferably equal to or greater than 25, further preferably equal to or greater than 30, even further preferably equal to or greater than 35. This preferred embodiment is the 19th embodiment of the present invention, which is preferably dependent on any one of the 6th to 18th embodiments of the present invention.

[0095] In one aspect of the 19th embodiment, it is preferred that the number of particles per unit area of ​​at least one impurity in the raw material is proportional to the volume segment V 1 The relative proportion of the number of particles per unit area of ​​at least one impurity at the outlet is equal to or less than 1000, more preferably equal to or less than 500, even more preferably equal to or less than 250.

[0096] In a preferred embodiment of the method for producing a first intermediate product, the first polyester is in a volume segment V 1 The residence time in is 5 minutes to 45 minutes, more preferably 8 minutes to 40 minutes, and further preferably 10 minutes to 30 minutes. This preferred embodiment is the 20th embodiment of the present invention, which preferably depends on any one of the 1st to 19th embodiments of the present invention.

[0097] In a preferred embodiment of the method for producing a first intermediate product, the volume segment V 1 The pressure in the reactor is in the range of 75 kPa to 130 kPa, more preferably in the range of 90 kPa to 115 kPa, further preferably in the range of 95 kPa to 107 kPa, and even further preferably in the range of 98 kPa to 103 kPa. This preferred embodiment is the 21st embodiment of the present invention, which preferably depends on any one of the 1st to 20th embodiments of the present invention.

[0098] In one aspect of the 21st embodiment, the preferred volume segment V 1 The pressure in is atmospheric pressure.

[0099] In a preferred embodiment of the method for producing a first intermediate product, the method further comprises in the volume section V 1 This preferred embodiment is the 22nd embodiment of the present invention, which preferably depends on any one of the 1st to 21st embodiments of the present invention.

[0100] In one aspect of the 22nd embodiment, the first initial mixture is preferably stirred using a mechanical device designed and arranged for stirring, a non-mechanical device designed and arranged for stirring, or a combination thereof. In this aspect, it is further preferred that the mechanical device, the non-mechanical device, or both are designed and arranged to suspend particles in a liquid, such as suspending multiple fragments of a raw material in a first organic compound. For example, the suspension of particles can be achieved by using a mechanical stirring device with a rotation speed per minute higher than a minimum value. In one aspect of the 22nd embodiment, the first initial mixture is preferably stirred so that impurities can float on the surface of the first initial mixture. This can be achieved, for example, by using a stirring device with a rotation speed per minute lower than a maximum value.

[0101] In a preferred embodiment of the method for producing a first intermediate product, the method further comprises at least partially removing from the volume segment V 1 The preferred embodiment is the 23rd embodiment of the present invention, which is preferably dependent on any one of the 1st to 22nd embodiments of the present invention.

[0102] In one aspect of the 23rd embodiment, at least one impurity is preferably present in the feedstock. In one aspect of the 23rd embodiment, at least one impurity is preferably at least partially removed using a floatable separation device. In another aspect of the 23rd embodiment, at least one impurity is preferably at least partially removed using skimming, filtering, or a combination thereof.

[0103] In a preferred embodiment of the method for producing a first intermediate product, the method further comprises the step of converting the first polyester preferably from a volume segment V 1 Transport to volume segment V 2 This preferred embodiment is the 24th embodiment of the present invention, which preferably depends on any one of the 1st to 23rd embodiments of the present invention.

[0104] In one aspect of the 24th embodiment, preferably in the volume segment V 1 After the raw material has been contacted with the first amount of the first organic compound, the first polyester is conveyed to the volume section V 2 In another aspect of the 24th embodiment, it is preferred that the volume segment V 1 At least a portion of the first organic compound in the volume segment V is transported together with the first polyester 2 In another aspect of the 24th embodiment, the preferred volume segment V 2 At least a portion of the first organic compound in the volume segment V 2 Transport (eg, flow) to volume segment V 1 In one aspect of the twenty-fourth embodiment, the first polyester is preferably delivered to the volume segment V before the first polyester is contacted with the other organic compound. 2 In one aspect of the 24th embodiment, the first polyester preferably passes through a volume segment V 2 The conveying direction is at least partially opposite to the direction of gravity, more preferably opposite to the direction of gravity. In one aspect of the 24th embodiment, the volume segment V 2 At least partially vertical arrangement, more preferably vertical arrangement. At least partially vertical arrangement should preferably be understood as volume segment V 2 The longest dimension (e.g., length) of is not parallel to the ground. For example, if the volume segment V 2 Arranged vertically, the volume segment V 2 The length is perpendicular to the ground.

[0105] In a preferred embodiment of the method for producing a first intermediate product, the volume segment V2 is at least partially filled with a first organic compound, wherein

[0106] i. Volume segment V 1 The height of the first organic compound level from the floor is H 1 ,and

[0107] ii. Volume segment V 2 The height of the first organic compound level from the floor is H 2 ,

[0108] and

[0109] Among them, H 1 <H 2 .

[0110] This preferred embodiment is the 25th embodiment of the present invention, which is preferably dependent on the 24th embodiment of the present invention.

[0111] In one aspect of the 25th embodiment, the preferred volume segment V 2 At least a portion of the first organic compound in the volume segment V 1 In another aspect of the 25th embodiment, the volume segment V 2 At least a portion of the first organic compound in the volume segment V 2 At least one inlet is added, for example an inlet of another type and an inlet of yet another type. In this regard, it is preferred that the volume segment V 2 At least 50 wt-%, more preferably at least 60 wt-%, and further preferably at least 70 wt-% of the first organic compound in the volume segment V is due to 2 The wt-% is based on the volume segment V 2 The total mass of the first organic compound in the volume segment V is preferably siphoned. 1 Transport to volume segment V 2 .

[0112] In a preferred embodiment of the method for producing a first intermediate product, the difference H 2 -H 1 At least 1 cm, more preferably at least 10 cm, further preferably at least 30 cm, even further preferably at least 60 cm. This preferred embodiment is the 26th embodiment of the present invention, which is preferably dependent on the 25th embodiment of the present invention.

[0113] In one aspect of the 26th embodiment, preferably the difference H 2-H 1 Less than 250 cm, more preferably less than 180 cm, even more preferably less than 160 cm, and further preferably less than 140 cm.

[0114] In a preferred embodiment of the method for producing a first intermediate product, upon entering the volume segment V 2 Before, the first polyester is transported in a further direction, wherein the further direction is at least partially opposite to the direction of gravity. This preferred embodiment is the 27th embodiment of the present invention, which preferably depends on any one of the 24th to 26th embodiments of the present invention.

[0115] In one aspect of the twenty-seventh embodiment, it is preferred that at least a portion of the first organic compound is transported in a direction opposite to the further direction. For example, the first polyester and a portion of the first organic compound are transported in opposite directions.

[0116] In a preferred embodiment of the method for producing the first intermediate product, the angle between the further direction and the horizontal plane is in the range of 12° to 45°, more preferably in the range of 17° to 40°, even more preferably in the range of 20° to 35°, further preferably in the range of 24° to 32°. This preferred embodiment is the 28th embodiment of the present invention, which is preferably dependent on the 27th embodiment of the present invention.

[0117] In one aspect of the 28th embodiment, an example of a horizontal plane is a floor, such as a floor of a recycling plant. In one aspect of the 28th embodiment, the horizontal plane is preferably perpendicular to the direction of gravity.

[0118] In a preferred embodiment of the method for producing the first intermediate product, the method further comprises the step of contacting the first polyester with a further amount of the first organic compound, preferably in a volume segment V 2 This preferred embodiment is the 29th embodiment of the present invention, which preferably depends on any one of the 1st to 28th embodiments of the present invention.

[0119] In an aspect of the twenty-ninth embodiment, the first polyester is contacted with an additional amount of the first organic compound, preferably prior to contacting the first polyester with the other organic compound.

[0120] In a preferred embodiment of the method for producing a first intermediate product, the method further comprises the step of increasing the temperature of the first polyester, preferably in the volume segment V 2 This preferred embodiment is the 30th embodiment of the present invention, which preferably depends on any one of the 1st to 29th embodiments of the present invention.

[0121] In one aspect of the 30th embodiment, the temperature is preferably increased by contacting the first polyester with an additional amount of the first organic compound. In one aspect of the 30th embodiment, the temperature is preferably increased before the first polyester is contacted with the other organic compound.

[0122] In a preferred embodiment of the method for producing a first intermediate product, the volume segment V 2 The temperature in the range of 50° C. to 220° C., more preferably in the range of 60° C. to 210° C., more preferably in the range of 65° C. to 205° C., and further preferably in the range of 68° C. to 200° C. This preferred embodiment is the 31st embodiment of the present invention, which preferably depends on any one of the 24th to 30th embodiments of the present invention.

[0123] In one aspect of the 31st embodiment, the preferred volume segment V 2 The temperature in is the temperature of the mixture including the first polyester and the first organic compound.

[0124] In a preferred embodiment of the method for producing a first intermediate product, the volume segment V 2 Includes the first region and another region where at least one or all of the following apply:

[0125] a. a relative ratio of the temperature of the first region to the temperature of the other region is in the range of 0.2 to 1.0, more preferably in the range of 0.3 to 0.9, and further preferably in the range of 0.4 to 0.8;

[0126] b. The relative ratio of the mass ratio of the first polyester to the first organic compound in the first region to the mass ratio of the first polyester to the first organic compound in another region is in the range of 0.01 to 0.90, more preferably in the range of 0.02 to 0.60, even more preferably in the range of 0.03 to 0.30, and further preferably in the range of 0.04 to 0.15.

[0127] This preferred embodiment is the 32nd embodiment of the present invention, which preferably depends on any one of the 24th to 31st embodiments of the present invention.

[0128] In one aspect of the 32nd embodiment, all possible combinations of features a. and b. are preferred aspects of this embodiment. These combinations are, for example, a; b; a+b.

[0129] In a preferred embodiment of the method for producing a first intermediate product, the volume segment V 2 Includes the first region and another region where at least one or all of the following apply:

[0130] a. The temperature of the first zone is in the range of 50°C to 220°C, preferably in the range of 50°C to 190°C, more preferably in the range of 60°C to 180°C, even more preferably in the range of 65°C to 170°C, further preferably in the range of 68°C to 160°C, and even further preferably in the range of 68°C to 150°C;

[0131] b. the temperature of another zone is 120 ℃ to 220 ℃, more preferably 130 ℃ to 210 ℃, even more preferably 135 ℃ to 205 ℃, and further preferably 138 ℃ to 200 ℃;

[0132] c. the mass ratio of the first polyester to the first organic compound in the first region is 0.1 to 0.9, more preferably 0.2 to 0.8, even more preferably 0.3 to 0.6, and further preferably 0.4 to 0.5;

[0133] d. The mass ratio of the first polyester to the first organic compound in the other region is in the range of 1 to 20, more preferably in the range of 2 to 16, even more preferably in the range of 3 to 12, and further preferably in the range of 5 to 10.

[0134] This preferred embodiment is the 33rd embodiment of the present invention, which preferably depends on any one of the 24th to 32nd embodiments of the present invention.

[0135] In one aspect of the 33rd embodiment, all possible combinations of features a. to d. are preferred aspects of this embodiment. These combinations are, for example, a; b; c; d; a+b; a+c; a+d; b+c; b+d; c+d; a+b+c; a+b+d; a+c+d; b+c+d; a+b+c+d. In one aspect of the 33rd embodiment, it is preferred that the temperature of the first region increases from the first end of the first region to the other end of the first region. For example, the temperature increases from 70°C measured at the first end of the first region to 145°C measured at the other end of the first region. In this aspect, it is preferred that the first end of the first region is located downstream of the other end of the first region. For example, the first end of the first region is located in the volume segment V 2 The first polyester enters the volume segment V through the inlet 2 In another aspect of the 33rd embodiment, the temperature of the other region preferably increases from the first end of the other region to the other end of the other region. For example, the temperature increases from 140°C measured at the first end of the other region to 200°C measured at the other end of the other region. In this regard, it is preferred that the first end of the other region is located downstream of the other end of the other region. For example, the other end of the other region is located in the volume segment V 2 The first polyester leaves the volume segment V through the outlet 2 For example, from the volume segment V 2The inlet of the first region moves to the outlet, and the ends of the regions are arranged in the following order: the first end of the first region, the other end of the first region, the first end of the other region, and the other end of the other region. In another aspect of the 33rd embodiment, it is preferred that the other end of the first region forms the first end of the other region. In one aspect of the 33rd embodiment, in feature a., it is particularly preferred that the temperature in the first region is in the range of 50°C to 190°C, more preferably in the range of 60°C to 180°C, even more preferably in the range of 65°C to 170°C, further preferably in the range of 68°C to 160°C, and even further preferably in the range of 68°C to 150°C. In one aspect of the 33rd embodiment, in feature a., it is preferred that the temperature in the first region is in the range of 60°C to 210°C, more preferably in the range of 60°C to 200°C, further preferably in the range of 65°C to 197°C, and even further preferably in the range of 67°C to 196°C. In one aspect of the 33rd embodiment, feature a., it is particularly preferred that the temperature in the first region is in the range of 50°C to 196°C, more preferably in the range of 55°C to 196°C, even more preferably in the range of 60°C to 196°C, further preferably in the range of 65°C to 196°C, and even more preferably in the range of 68°C to 196°C. In one aspect of the 33rd embodiment, feature a., it is preferred that the temperature of the first region is lower than the boiling point of the first organic compound. In one aspect of the 33rd embodiment, feature b., it is preferred that the temperature of the other region is in the range of 160°C to 220°C, more preferably in the range of 170°C to 210°C, even more preferably in the range of 180°C to 200°C, further preferably in the range of 185°C to 196°C, even more preferably in the range of 190°C to 196°C. In one aspect of the 33rd embodiment, feature b., it is preferred that the temperature of the other region is lower than the boiling point of the first organic compound.

[0136] In a preferred embodiment of the method for producing the first intermediate product, at least one or all of the following apply:

[0137] a. a first portion of the first organic compound in contact with the first polyester in an additional amount in the form of a gas, such as steam;

[0138] b. Another portion of the additional amount of the first organic compound contacted with the first polyester is in liquid form.

[0139] This preferred embodiment is the 34th embodiment of the present invention, which preferably depends on any one of the 29th to 33rd embodiments of the present invention.

[0140] In the 34th embodiment, the first part and the further part are measured in wt-%, based on the total mass of the further amount of the first organic compound contacted with the first polyester. In one aspect of the 34th embodiment, all possible combinations of features a. and b. are preferred aspects of this embodiment. These combinations are, for example, a; b; a+b. In the 34th embodiment, "part" (e.g., first part, further part) should preferably be understood as including a value of 100 wt-%. For example, in one aspect of the 34th embodiment, where only feature a. applies, the first part will be 100 wt-%. In the 34th embodiment, the first part should preferably be understood as including the first organic compound that was initially in gaseous form but condensed before contacting with the first polyester. In one aspect of the 34th embodiment, feature a., it is preferred that the temperature of the first part of the further amount of the first organic compound is above the boiling point of the first organic compound. In one aspect of the 34th embodiment, feature a., it is preferred that the temperature of the first part of the further amount of the first organic compound is in the range of 200°C to 240°C, more preferably in the range of 210°C to 230°C. In one aspect of the 34th embodiment, feature b., preferably, the temperature of the other portion of the additional amount of the first organic compound is below the boiling point of the first organic compound. In one aspect of the 34th embodiment, feature b., preferably, the temperature of the other portion of the additional amount of the first organic compound is in the range of 180° C. to 196° C., more preferably in the range of 190° C. to 196° C.

[0141] In a preferred embodiment of the method for producing the first intermediate product, the first part accounts for 50 wt-% to 90 wt-%, more preferably 55 wt-% to 85 wt-%, even more preferably 60 wt-% to 80 wt-%, and further preferably 65 wt-% to 75 wt-% of the additional amount of the first organic compound. The wt-% is based on the total mass of the additional amount of the first organic compound. This preferred embodiment is the 35th embodiment of the present invention, which is preferably dependent on the 34th embodiment of the present invention.

[0142] In the 35th embodiment, the sum of the wt-% of the first part and the wt-% of the other part is 100 wt-%. For example, if the first part accounts for 55 wt-% of the other amount of the first organic compound, the other part accounts for the remaining 45 wt-% of the other amount of the first organic compound.

[0143] In a preferred embodiment of the method for producing a first intermediate product, the first polyester enters the volume section V through at least one inlet of a first type. 2 , where at least one or all of the following apply:

[0144] a. A further amount of at least a portion (eg, a first portion) of the first organic compound, preferably in the form of a gas, enters the volume segment V through at least one other type of inlet 2 , wherein the at least one inlet of the other type is adapted and arranged such that the additional amount of the first organic compound entering through the at least one inlet of the other type passes through the volume segment V 2 The flow direction is at least partially along the first polyester through the volume segment V 2 The direction of transport;

[0145] b. A further amount of at least a portion (eg, another portion) of the first organic compound, preferably in liquid form, enters the volume segment V through at least one further type of inlet 2 , wherein the at least one further type of inlet is adapted and arranged such that the additional amount of the first organic compound entering through the at least one further type of inlet passes through the volume segment V 2 The flow direction is at least partially connected to the first polyester through the volume segment V 2 The transport direction is opposite.

[0146] This preferred embodiment is the 36th embodiment of the present invention, which preferably depends on any one of the 29th to 35th embodiments of the present invention.

[0147] In one aspect of the 36th embodiment, all possible combinations of features a. and b. are preferred aspects of this embodiment. These combinations are, for example, a; b; a+b. In one aspect of the 36th embodiment, it is preferred that the first polyester passes through a volume segment V 2 The conveying direction is parallel to the volume segment V 2 In one aspect of the 36th embodiment, it is preferred that the first polyester passes through the volume segment V 2 The transport direction is at least partially opposite to the direction of gravity. In this aspect, it is more preferred that the transport direction is opposite to the direction of gravity. In one aspect of the 36th embodiment, it is preferred that the portion in feature a. is the first portion of the additional amount of the first organic compound. In one aspect of the 36th embodiment, it is preferred that the portion in feature b. is another portion of the additional amount of the first organic compound.

[0148] In a preferred embodiment of the method for producing a first intermediate product, at least one impurity is present in volume segment V 2 This preferred embodiment is the 37th embodiment of the present invention, which preferably depends on any one of the 24th to 36th embodiments of the present invention.

[0149] In the 37th embodiment, an example of the at least one impurity is an impurity present in the raw material, and the impurity is from the volume segment V 1 Transport to volume segment V 2 .

[0150] In a preferred embodiment of the method for producing a first intermediate product, the volume segment V 2 comprising a first region and another region, wherein a relative ratio of the number of particles per unit area of ​​at least one impurity in the first region to the number of particles per unit area of ​​at least one impurity in the another region is equal to or greater than 10, more preferably equal to or greater than 15, even more preferably equal to or greater than 20, further preferably equal to or greater than 25, even further preferably equal to or greater than 30. This preferred embodiment is the 38th embodiment of the present invention, which is preferably dependent on the 37th embodiment of the present invention.

[0151] In one aspect of the 38th embodiment, preferably, the relative ratio of the number of particles per unit area of ​​at least one impurity in the first region to the number of particles per unit area of ​​at least one impurity in another region is equal to or less than 1000, more preferably equal to or less than 500, and even more preferably equal to or less than 250.

[0152] In a preferred embodiment of the method for producing a first intermediate product, at least one or all of the following apply to volume segment V 2 :

[0153] a. The pressure is in the range of 80 kPa to 135 kPa, more preferably in the range of 95 kPa to 120 kPa, further preferably in the range of 100 kPa to 115 kPa, even further preferably in the range of 104 kPa to 109 kPa;

[0154] b. The overpressure range is 2 kPa to 12 kPa, more preferably 4 kPa to 8 kPa, and further preferably 5 kPa to 7 kPa.

[0155] This preferred embodiment is the 39th embodiment of the present invention, which is preferably dependent on any one of the 24th to 38th embodiments of the present invention.

[0156] In one aspect of the 39th embodiment, all possible combinations of features a. and b. are preferred aspects of this embodiment. These combinations are, for example, a; b; a+b.

[0157] In a preferred embodiment of the method for producing a first intermediate product, the first polyester is in a volume segment V 2 The residence time in the range of 30 minutes to 270 minutes, more preferably in the range of 50 minutes to 250 minutes, and further preferably in the range of 80 minutes to 220 minutes. This preferred embodiment is the 40th embodiment of the present invention, which preferably depends on any one of the 24th to 39th embodiments of the present invention.

[0158] In a preferred embodiment of the method for producing a first intermediate product, the method further comprises the step of reducing at least one or all of the following, preferably in the volume segment V 2 middle:

[0159] a. the weight average molar mass of the first polyester;

[0160] b. The intrinsic viscosity of the first polyester.

[0161] This preferred embodiment is the 41st embodiment of the present invention, which is preferably dependent on any one of the 1st to 40th embodiments of the present invention.

[0162] In one aspect of the 41st embodiment, all possible combinations of features a. and b. are preferred aspects of this embodiment. These combinations are, for example, a; b; a+b. In one aspect of the 41st embodiment, at least one or all of steps a. and b. in the 41st embodiment are preferably performed before contacting the first polyester with another organic compound.

[0163] In a preferred embodiment of the method for producing the first intermediate product, at least one or all of the following apply:

[0164] a. The weight average molar mass of the first polyester is preferably in the volume segment V 2 The amount of the product is reduced by at least 50%, more preferably at least 60%, even more preferably at least 70%, further preferably at least 75%, even further preferably at least 80%, particularly preferably at least 85%;

[0165] b. The intrinsic viscosity of the first polyester is preferably in the volume segment V 2 The molecular weight of the raw material is preferably reduced by at least 40%, more preferably by at least 50%, even more preferably by at least 60%, further preferably by at least 70%, further preferably by at least 75%.

[0166] This preferred embodiment is the 42nd embodiment of the present invention, which is preferably dependent on the 41st embodiment of the present invention.

[0167] In one aspect of the 42nd embodiment, all possible combinations of features a. and b. are preferred aspects of this embodiment. These combinations are, for example, a; b; a+b. In one aspect of the 42nd embodiment, it is preferred that the intrinsic viscosity of the first polyester is reduced by 97% or less, more preferably 95% or less, even more preferably 93% or less, and further preferably 90% or less. In one aspect of the 42nd embodiment, it is preferred that the intrinsic viscosity of the first polyester is reduced by a value in the range of 70% to 80%. In one aspect of the 42nd embodiment, it is preferred that the weight average molar mass of the first polyester is reduced by 97% or less, more preferably 95% or less, and further preferably 93% or less. In one aspect of the 42nd embodiment, it is preferred to reduce the weight average molar mass of the first polyester by a value in the range of 85% to 93%.

[0168] In a preferred embodiment of the method for producing a first intermediate product, after completion of the reducing step, preferably in the volume segment V 2 In the method, the first polyester has at least one or all of the following properties:

[0169] a. an intrinsic viscosity in the range of 0.08 dL / g to 0.45 dL / g, more preferably in the range of 0.10 dL / g to 0.35 dL / g, even more preferably in the range of 0.12 dL / g to 0.25 dL / g, and further preferably in the range of 0.12 dL / g to 0.20 dL / g;

[0170] b. The weight average molar mass is in the range of 3000 Da to 7500 Da, more preferably in the range of 3200 Da to 7300 Da, even more preferably in the range of 3800 Da to 7100 Da, and further preferably in the range of 4000 Da to 6900 Da.

[0171] This preferred embodiment is the 43rd embodiment of the present invention, which is preferably dependent on any one of the 41st to 42nd embodiments of the present invention.

[0172] In one aspect of the 43rd embodiment, all possible combinations of features a. and b. are preferred aspects of this embodiment. These combinations are, for example, a; b; a+b. In one aspect of the 43rd embodiment, the preferred features a. and b. are the exit volume segment V 2 In one aspect of the 43rd embodiment, the weight average molar mass is preferably in the range of 4000Da to 5000Da.

[0173] In a preferred embodiment of the process for producing a first intermediate product, the first polyester is fed:

[0174] I. / When the first polyester has a value greater than or equal to Y IV,1 When the intrinsic viscosity is , the conveyor is transported in a first direction at least partially opposite to the direction of gravity, wherein Y IV,1 0.10 dL / g, more preferably 0.15 dL / g, even more preferably 0.20 dL / g, and further preferably 0.30 dL / g; and

[0175] II. / When the first polyester has less than or equal to Y IV,2 When the intrinsic viscosity is at least partially in the direction of gravity, the transport direction Y IV,2 It is 0.09 dL / g, more preferably 0.07 dL / g, and even more preferably 0.05 dL / g.

[0176] This preferred embodiment is the 44th embodiment of the present invention, and is preferably subordinate to any one of the 1st to 43rd embodiments of the present invention.

[0177] In the 44th embodiment, Y 1,IV >Y 2,IV In one aspect of the 44th embodiment, the term "delivery" is preferably understood to mean at least one or all of the following:

[0178] The first polyester is transferred from the first volume section to another volume section (e.g., from volume section V 1 Convey to volume segment V 2 , from volume segment V 2 Convey to volume segment V 3 ), and conveying the first polyester to pass through a volume segment (e.g., volume segment V 1 , volume segment V 3 In one aspect of the 44th embodiment, it is preferred to first transport the first polyester to a first direction and then transport the first polyester to another direction. In one aspect of the 44th embodiment, it is preferred that in the volume segment V 1 After contacting the first polyester with the first amount of the first organic compound in the first direction, the first polyester is transported in the first direction. In one aspect of the 44th embodiment, when the intrinsic viscosity of the first polyester is Y 2,IV To Y 1,IV In one aspect of the 44th embodiment, when the first polyester is transported in the first direction, at least a portion of the organic compound (preferably the first organic compound) is transported in the reverse direction of the first direction. In one aspect of the 44th embodiment, when the first polyester is transported in the other direction, at least a portion of the organic compound (preferably the other organic compound) is transported in the other direction. In one aspect of the 44th embodiment, Y IV,1 and Y IV,2 One of the following combinations of values ​​in features I. / and II. / : Y IV,1 is 0.10dL / g and Y IV,2 0.09dL / g; Y IV,1 0.15dL / g, Y IV,2 0.07dL / g; Y IV,1 0.20dL / g, Y IV,2 0.05dL / g; Y IV,1 0.30dL / g, Y IV,2 0.05dL / g; Y IV,1 0.10dL / g, Y IV,2 0.05 dL / g; or Y IV,1 0.30dL / g, Y IV,2 In one aspect of the 44th embodiment, the transport of the first polyester in the first direction preferably includes at least one or all of the following:1 Transport to volume segment V 2 , transport through volume segment V 2 In one aspect of the 44th embodiment, preferably, conveying the first polyester in another direction comprises conveying through the volume segment V 3 In one aspect of the 44th embodiment, the first polyester is preferably in the form of a plurality of fragments.

[0179] In a preferred embodiment of the method for producing a first intermediate product, the method further comprises conveying the first polyester to a volume section V 3 This preferred embodiment is the 45th embodiment of the present invention, which preferably depends on any one of the 1st to 44th embodiments of the present invention.

[0180] In one aspect of the 45th embodiment, the first polyester is preferably 1 Transport to volume segment V 3 , more preferably via volume segment V 2 In other words, the first polyester can be transported from volume segment V 1 Transport to volume segment V 3 Without the first polyester passing through the volume segment V 2 However, it is more preferred that the first polyester be from volume segment V 2 Transport to volume segment V 3 .

[0181] In a preferred embodiment of the method for producing a first intermediate product, the other organic compound has at least one or all of the following characteristics:

[0182] a. comprising at least two hydroxyl groups, for example a diol having 2 hydroxyl groups, a triol having 3 hydroxyl groups;

[0183] b. The molar mass is at least 60 g / mol;

[0184] c. A boiling point of at least 192°C, more preferably at least 195°C.

[0185] This preferred embodiment is the 46th embodiment of the present invention, which is preferably dependent on any one of the 1st to 45th embodiments of the present invention.

[0186] Examples of the other organic compound include (mono)ethylene glycol, propylene glycol and glycerol. In one aspect of the 46th embodiment, all possible combinations of features a. to c. are preferred aspects of this embodiment. These combinations are, for example, a; b; c; a+b; a+c; b+c; a+b+c. In one aspect of the 46th embodiment, it is particularly preferred that the other organic compound is (mono)ethylene glycol, more preferably monoethylene glycol. In one aspect of the 46th embodiment, it is particularly preferred that the other organic compound is not propylene glycol.

[0187] In a preferred embodiment of the method for producing a first intermediate product, 3 This preferred embodiment is the 47th embodiment of the present invention, which is preferably dependent on any one of the 1st to 46th embodiments of the present invention.

[0188] In one aspect of the 47th embodiment, stirring is preferably performed using a mechanical device designed and arranged for stirring, a non-mechanical device designed and arranged for stirring, or a combination thereof.

[0189] In a preferred embodiment of the method for producing a first intermediate product, preferably in volume section V 3 At the inlet end of the first polyester, the mass ratio of the first polyester to the other organic compound in the other initial mixture is greater than 1.0. This preferred embodiment is the 48th embodiment of the present invention, which preferably depends on any one of the 1st to 47th embodiments of the present invention.

[0190] In one aspect of the 48th embodiment, the inlet end is preferably the first polyester entry volume segment V 3 location.

[0191] In a preferred embodiment of the method for producing a first intermediate product, the temperature of the further initial mixture, preferably in the volume section V 3 In the range of 180° C. to 220° C., more preferably in the range of 180° C. to 210° C. This preferred embodiment is the 49th embodiment of the present invention, which preferably depends on any one of the 1st to 48th embodiments of the present invention.

[0192] In a preferred embodiment of the method for producing a first intermediate product, the volume segment V 3 The pressure in the range of 75 kPa to 131 kPa, more preferably in the range of 90 kPa to 116 kPa, further preferably in the range of 95 kPa to 108 kPa, even further preferably in the range of 98 kPa to 104 kPa. This preferred embodiment is the 50th embodiment of the present invention, which preferably depends on any one of the 45th to 49th embodiments of the present invention.

[0193] In one aspect of the 50th embodiment, preferably, the volume segment V 3 The pressure in is atmospheric pressure.

[0194] In a preferred embodiment of the method for producing a first intermediate product, the other initial mixture is in a volume segment V 3The residence time in the range of 100 minutes to 560 minutes, more preferably in the range of 140 minutes to 440 minutes, and further preferably in the range of 170 minutes to 380 minutes. This preferred embodiment is the 51st embodiment of the present invention, which preferably depends on any one of the 45th to 50th embodiments of the present invention.

[0195] In a preferred embodiment of the method for producing the first intermediate product, the first intermediate mixture contains at least 70wt-%, more preferably at least 80wt-%, even more preferably at least 85wt-%, further preferably at least 90wt-%, and further preferably at least 94wt-% of the first intermediate product. This preferred embodiment is the 52nd embodiment of the present invention, which preferably depends on any one of the 1st to 51st embodiments of the present invention.

[0196] In the 52nd embodiment, the wt-% is based on the total mass of the first intermediate mixture. In an optional aspect of the 52nd embodiment, the first intermediate mixture comprises a first intermediate product in a range of 70 wt-% to 99 wt-%, optionally in a range of 80 wt-% to 95 wt-%, and optionally in a range of 88 wt-% to 92 wt-%.

[0197] In a preferred embodiment of the method for producing the first intermediate product, at least 40 wt-%, more preferably at least 50 wt-%, even more preferably at least 60 wt-%, further preferably at least 65 wt-%, even further preferably at least 70 wt-% of the first intermediate product is in the form of an oligomer having 2 to 35 repeating units, more preferably 2 to 30 repeating units, even more preferably 2 to 25 repeating units, further preferably 2 to 20 repeating units. This preferred embodiment is the 53rd embodiment of the present invention, which preferably depends on any one of the 1st to 52nd embodiments of the present invention.

[0198] In the 53rd embodiment, the wt-% is based on the total mass of the first intermediate product in the first intermediate mixture. In one aspect of the 53rd embodiment, preferably, at least 40 wt-%, more preferably at least 50 wt-%, even more preferably at least 60 wt-%, further preferably at least 65 wt-%, and even further preferably at least 70 wt-% of the first intermediate product is in the form of oligomers having the number of repeating units in at least one of the following ranges: 3 to 30, 4 to 30, 6 to 30, 8 to 30, 3 to 20, 4 to 20, 6 to 20. In one aspect of the 53rd embodiment, preferably, at least 70 wt-% of the oligomers have the number of repeating units in the range of 2 to 35, more preferably in the range of 2 to 30, even more preferably in the range of 2 to 25, and further preferably in the range of 2 to 20. Preferred oligomers include repeating units of ethylene terephthalate. In one aspect of the 53rd embodiment, preferably, at least 40 wt-%, more preferably at least 50 wt-%, even more preferably at least 60 wt-%, further preferably at least 65 wt-%, and even further preferably at least 70 wt-% of the first intermediate product is in the form of oligomers having the number of repeating units in the range of 2 to 15, more preferably in the range of 2 to 12, and further preferably in the range of 2 to 10.

[0199] In a preferred embodiment of the method for producing the first intermediate product, at least one or all of the following apply:

[0200] a. The first intermediate product contains 30 wt-% or less, more preferably 25 wt-% or less, even more preferably 20 wt-% or less, further preferably 15 wt-% or less, and even further preferably 10 wt-% or less of monomers;

[0201] b. The first intermediate product contains at least 70 wt-%, more preferably at least 75 wt-%, even more preferably at least 80 wt-%, further preferably at least 85 wt-%, and even further preferably at least 90 wt-% of oligomers.

[0202] This preferred embodiment is the 54th embodiment of the present invention, which preferably depends on any one of the 1st to 53rd embodiments of the present invention.

[0203] In the 54th embodiment, the wt-% is based on the total mass of the first intermediate product in the first intermediate mixture. In one aspect of the 54th embodiment, all possible combinations of features a. and b. are preferred aspects of this embodiment. These combinations are, for example, a; b; a+b. For example, the first intermediate product comprises 20 wt-% of monomer and 80 wt-% of oligomer. In the 54th embodiment, an example of a monomer is BHET. In the 54th embodiment, an example of an oligomer is a PET oligomer. In an optional aspect of the 54th embodiment, the first intermediate product comprises monomers in the range of 15 wt-% to 30 wt-%, and optionally comprises monomers in the range of 20 wt-% to 25 wt-%. In an optional aspect of the 54th embodiment, the first intermediate product comprises oligomers in the range of 70 wt-% to 85 wt-%, and optionally comprises oligomers in the range of 75 wt-% to 85 wt-%. In one aspect of the 54th embodiment, particularly preferred oligomers have 2 to 10 repeating units.

[0204] In a preferred embodiment of the method for producing the first intermediate product, at least one or all of the following apply:

[0205] a. The first intermediate product comprises at least 20 wt-%, more preferably at least 30 wt-%, even more preferably at least 40 wt-%, further preferably at least 50 wt-%, even further preferably at least 60 wt-% of monomer;

[0206] b. The first intermediate product comprises at least 20 wt-%, preferably at least 30 wt-%, more preferably at least 40 wt-%, and further preferably at least 50 wt-% of oligomers.

[0207] This preferred embodiment is an alternative embodiment of the 54th embodiment of the present invention, which preferably depends on any one of the 1st to 53rd embodiments of the present invention. In one aspect of the present invention, any one of the 55th to 106th embodiments of the present invention preferably depends on this alternative embodiment of the 54th embodiment of the present invention.

[0208] In an alternative 54th embodiment, the wt-% is based on the total mass of the first intermediate product in the first intermediate mixture. In an alternative 54th embodiment, an example of a monomer is BHET. In an alternative 54th embodiment, an example of an oligomer is a PET oligomer. In one aspect of the alternative 54th embodiment, all possible combinations of features a. and b. are preferred aspects of this embodiment. These combinations are, for example, a; b; a+b. In a preferred aspect of the alternative 54th embodiment, feature a., the first intermediate product contains monomers in the range of 20 wt-% to 60 wt-%, more preferably monomers in the range of 30 wt-% to 50 wt-%, and further preferably monomers in the range of 35 wt-% to 40 wt-%. In this regard, it is preferred that the remaining wt-% of the first intermediate product consists of oligomers. In an aspect of the alternative 54th embodiment, particularly preferred oligomers have 2 to 10 repeating units.

[0209] In a preferred embodiment of the method for preparing the first intermediate product, the first intermediate product has at least one or all of the following characteristics:

[0210] a. an intrinsic viscosity in the range of 0.010 dL / g to 0.120 dL / g, more preferably in the range of 0.030 dL / g to 0.090 dL / g, further preferably in the range of 0.040 dL / g to 0.070 dL / g, further preferably in the range of 0.045 dL / g to 0.065 dL / g;

[0211] b. The weight average molar mass is in the range of 350Da to 800Da, more preferably in the range of 450Da to 650Da, further preferably in the range of 500Da to 600Da.

[0212] This preferred embodiment is the 55th embodiment of the present invention, which preferably depends on any one of the 1st to 54th embodiments of the present invention.

[0213] In one aspect of the 55th embodiment, all possible combinations of features a. and b. are preferred aspects of this embodiment. These combinations are, for example, a; b; a+b.

[0214] In a preferred embodiment of the method for producing the first intermediate product, at least one or all of the following apply:

[0215] a. The first intermediate mixture comprises 20 wt-% or less, more preferably 15 wt-% or less, even more preferably 12 wt-% or less, further preferably 10 wt-% or less, even further preferably 8 wt-% or less of another organic compound;

[0216] b. The first intermediate mixture contains less than 15 wt-%, more preferably less than 10 wt-%, and further preferably less than 5 wt-% of a dicarboxylic acid, such as terephthalic acid.

[0217] This preferred embodiment is the 56th embodiment of the present invention, which preferably depends on any one of the 1st to 55th embodiments of the present invention.

[0218] In one aspect of the 56th embodiment, all possible combinations of features a. and b. are preferred aspects of this embodiment. These combinations are, for example, a; b; a+b. In the 56th embodiment, the wt-% is based on the total mass of the first intermediate mixture. In one aspect of the 56th embodiment, the other organic compound should preferably be understood as free, i.e., not chemically bound to the first intermediate product by a covalent bond. In an optional aspect of the 56th embodiment, the first intermediate mixture contains another organic compound in the range of 5 wt-% to 20 wt-%, optionally in the range of 7 wt-% to 15 wt-%, optionally in the range of 9 wt-% to 12 wt-%.

[0219] In a preferred embodiment of the method for producing a first intermediate product, the method further comprises the first intermediate mixture, preferably from the volume segment V 3 , transported to volume segment V 4 This preferred embodiment is the 57th embodiment of the present invention, which preferably depends on any one of the 1st to 56th embodiments of the present invention.

[0220] In one aspect of the 57th embodiment, preferably, the intrinsic viscosity of the first intermediate product is in the volume range V 4 In another aspect of the 57th embodiment, preferably, the intrinsic viscosity of the first intermediate product is less than 5%, more preferably less than 3%, further preferably less than 1%, and even more preferably less than 0.1%. 4 In another aspect of the 57th embodiment, preferably, the intrinsic viscosity of the first intermediate product is less than 5%, more preferably less than 3%, further preferably less than 1%, and even more preferably less than 0.1%. 4 The average change (neither increase nor decrease) is less than 5%, more preferably less than 3%, further preferably less than 1%, and even further preferably less than 0.1%.

[0221] In a preferred embodiment of the method for producing a first intermediate product, the method further comprises the step of adding a first particulate material to the first intermediate mixture, preferably in volume segment V 4 This preferred embodiment is the 58th embodiment of the present invention, which preferably depends on any one of the 1st to 57th embodiments of the present invention.

[0222] In one aspect of the 58th embodiment, preferably, the first particulate material is designed and arranged for adsorption. In another aspect of the 58th embodiment, preferably, the first particulate material is designed and arranged for decolorization. In another aspect of the 58th embodiment, preferably, the first particulate material is porous. In one aspect of the 58th embodiment, particularly preferably, the first particulate material is designed and arranged for filtration, more preferably microfiltration. Microfiltration is the filtration of particles in the range of 0.5 μm-10 μm. In one aspect of the 58th embodiment, preferably, the first particulate material is added after the weight average molar mass of the first polyester is reduced.

[0223] In a preferred embodiment of the method for producing the first intermediate product, the median pore size of the first granular material is in the range of 5.0 μm to 20.0 μm, preferably in the range of 10.0 μm to 20.0 μm, and further preferably in the range of 15.0 μm to 18.0 μm. This preferred embodiment is the 59th embodiment of the present invention, which is preferably dependent on the 58th embodiment of the present invention.

[0224] In a preferred embodiment of the method for preparing the first intermediate product, the first particulate material has a pore size distribution in which at least one mode is in the range of 8000nm to 20000nm, more preferably in the range of 10000nm to 18000nm, and further preferably in the range of 10000nm to 15000nm. This preferred embodiment is the 60th embodiment of the present invention, which preferably depends on any one of the 58th to 59th embodiments of the present invention.

[0225] In a preferred embodiment of the method for producing a first intermediate product, the first particulate material has a pore size distribution having at least two modes in the range of 8000 nm and 20000 nm, wherein

[0226] a. at least one mode in the range of 8000nm to 15000nm, preferably in the range of 10000nm to 15000nm;

[0227] b. At least one mode is in the range of >15000nm to 20000nm, preferably in the range of 16000nm to 18000nm.

[0228] This preferred embodiment is the 61st embodiment of the present invention, which preferably depends on any one of the 58th to 60th embodiments of the present invention.

[0229] In one aspect of the 61st embodiment, all possible combinations of features a. and b. are preferred aspects of the embodiment. These combinations are, for example, a; b; a+b. In one aspect of the 61st embodiment, preferably, the mode in feature a. is a secondary mode. In one aspect of the 61st embodiment, preferably, the mode in feature b. is a primary mode.

[0230] In a preferred embodiment of the method for producing a first intermediate product, the first particulate material has a pore size distribution, wherein at least one first mode is in the range of 9000nm to 15000nm, and at least one other mode is in the range of >15000nm to 20000nm, wherein the ratio of the first mode to the other mode is in the range of 0.30 to 1.00, preferably in the range of 0.40 to 0.90, and further preferably in the range of 0.45 to 0.85. This preferred embodiment is the 62nd embodiment of the present invention, which preferably depends on any one of the 58th to 61st embodiments of the present invention.

[0231] In a preferred embodiment of the method for producing a first intermediate product, the first particulate material has at least one or all of the following characteristics:

[0232] a. For pores with diameters between 9000nm and 20000nm, the cumulative pore volume is 0.6cm 3 / g to 1.9cm 3 / g range, preferably within 0.9cm 3 / g to 1.7cm 3 / g range, more preferably within 1.1cm 3 / g to 1.5cm 3 / g range;

[0233] b. For pores with diameters between 10,000 nm and 15,000 nm, the cumulative pore volume is 0.5 cm 3 / g to 1.4cm 3 / g range, preferably within 0.6cm 3 / g to 1.2cm 3 / g range, more preferably 0.8cm 3 / g to 1.0cm 3 / g range;

[0234] c. And for pores with diameters in the range of >15000nm to 20000nm, the cumulative pore volume is 0.10cm 3 / g to 0.80cm 3 / g range, preferably within 0.20cm 3 / g to 0.60cm 3 / g, more preferably within 0.25cm 3 / g to 0.40cm 3 / g range.

[0235] This preferred embodiment is the 63rd embodiment of the present invention, which preferably depends on any one of the 58th to 62nd embodiments of the present invention.

[0236] In one aspect of the 63rd embodiment, all possible combinations of features a. to c. are preferred aspects of this embodiment. These combinations are, for example, a; b; c; a+b; a+c; b+c; a+b+c.

[0237] In a preferred embodiment of the method for producing a first intermediate product, the first particulate material has at least one or all of the following characteristics:

[0238] a. a permeability in the range of 0.7 Darcy to 10.0 Darcy, preferably in the range of 1.5 Darcy to 7.5 Darcy, more preferably in the range of 3.0 Darcy to 5.0 Darcy, and further preferably in the range of 3.5 Darcy to 4.5 Darcy;

[0239] b. The median particle size is in the range of 25 mm to 60 mm, preferably in the range of 35 mm to 55 mm, more preferably in the range of 40 mm to 50 mm, and further preferably in the range of 43 mm to 50 mm.

[0240] This preferred embodiment is the 64th embodiment of the present invention, which preferably depends on any one of the 58th to 63rd embodiments of the present invention.

[0241] In one aspect of the 64th embodiment, all possible combinations of features a and b are preferred aspects of this embodiment. These combinations are, for example, a; b; a+b.

[0242] In a preferred embodiment of the method for producing the first intermediate product, the first particulate material is selected from activated carbon (e.g., activated carbon), activated clay, diatomaceous earth, perlite, bentonite, cellulose, and a combination of at least two thereof. This preferred embodiment is the 65th embodiment of the present invention, which preferably depends on any one of the 58th to 64th embodiments of the present invention.

[0243] In one aspect of the 65th embodiment, it is particularly preferred that the first particulate material is diatomaceous earth.

[0244] In a preferred embodiment of the method for preparing the first intermediate product, the volume segment V 4 The mass ratio of the first granular material to the first intermediate mixture is 5.0x10 -4 Up to 2.5x10 -3 range, more preferably within 1.0x10 -3 Up to 2.0x10 -3 range, and more preferably within 1.2x10 -3 Up to 1.8x10 -3 This preferred embodiment is the 66th embodiment of the present invention, which preferably depends on any one of the 58th to 65th embodiments of the present invention.

[0245] In a preferred embodiment of the method for producing a first intermediate product, the volume segment V 4 The temperature of the first intermediate mixture in the mixture is in the range of 160° C. to 230° C., more preferably in the range of 170° C. to 220° C., even more preferably in the range of 180° C. to 215° C., further preferably in the range of 185° C. to 209° C., even further preferably in the range of 190° C. to 205° C. This preferred embodiment is the 67th embodiment of the present invention, which preferably depends on any one of the 57th to 66th embodiments of the present invention.

[0246] In a preferred embodiment of the method for producing a first intermediate product, the volume segment V 4 The first intermediate mixture in the mixture is stirred. This preferred embodiment is the 68th embodiment of the present invention, which preferably depends on any one of the 57th to 67th embodiments of the present invention.

[0247] In one aspect of the 68th embodiment, the first intermediate mixture is preferably agitated using a mechanical device designed and arranged for agitation.

[0248] In a preferred embodiment of the method for preparing a first intermediate product, the first intermediate mixture is in a volume range V 4 The residence time in is 10 hours or less, more preferably 7 hours or less, further preferably 5 hours or less. This preferred embodiment is the 69th embodiment of the present invention, which preferably depends on any one of the 57th to 68th embodiments of the present invention.

[0249] In an optional aspect of the 69th embodiment, the first intermediate mixture is in the volume segment V 4 The residence time in the mixture is at least 0.1 hours, optionally at least 1 hour, optionally at least 3.5 hours.

[0250] In a preferred embodiment of the method for producing a first intermediate product, the method further comprises the step of conveying the first intermediate mixture to a filtering device, preferably from the volume segment V 4 This preferred embodiment is the 70th embodiment of the present invention, which preferably depends on any one of the 1st to 69th embodiments of the present invention.

[0251] In a preferred embodiment of the method for producing the first intermediate product, the filtering device is selected from a leaf filter, a sheet clarifier, a candle filter, a porous filter, a sintered filter, a wire mesh, a rotary drum filter, and a combination of two or more thereof. This preferred embodiment is the 71st embodiment of the present invention, which is preferably dependent on the 70th embodiment of the present invention.

[0252] In one aspect of the 71st embodiment, the preferred filtering device is a leaf filter, more preferably a vertical leaf filter.

[0253] In a preferred embodiment of the method for producing the first intermediate product, the pressure in the filtration device is in the range of 80 kPa to 1000 kPa, more preferably in the range of 140 kPa to 800 kPa, even more preferably in the range of 170 kPa to 610 kPa, and further preferably in the range of 200 kPa to 545 kPa. This preferred embodiment is the 72nd embodiment of the present invention, which preferably depends on any one of the 70th to 71st embodiments of the present invention.

[0254] In a preferred embodiment of the method for producing the first intermediate product, the temperature in the filtration device is in the range of 150° C. to 215° C., more preferably in the range of 160° C. to 205° C., even more preferably in the range of 165° C. to 200° C., and further preferably in the range of 170° C. to 195° C. This preferred embodiment is the 73rd embodiment of the present invention, which preferably depends on any one of the 70th to 72nd embodiments of the present invention.

[0255] In a preferred embodiment of the method for producing the first intermediate product, the method further comprises a step of pre-coating the filter means, preferably using the first granular material. This preferred embodiment is the 74th embodiment of the present invention, which preferably depends on any one of the 70th to 73rd embodiments of the present invention.

[0256] In one aspect of the 74th embodiment, a pre-coating step is preferably performed prior to at least partially removing at least one or all of: at least one impurity, the first particulate material.

[0257] In a preferred embodiment of the method for producing the first intermediate product, the method further comprises a step of at least partially removing at least one impurity from the first intermediate mixture, preferably using a filtering device. This preferred embodiment is the 75th embodiment of the present invention, which preferably depends on any one of the 1st to 74th embodiments of the present invention.

[0258] In one aspect of the 75th embodiment, the first particulate material is preferably at least partially removed from the first intermediate mixture, more preferably using a filtering device. For example, at least one impurity and the first particulate material are at least partially removed. In one aspect of the 75th embodiment, the particles (e.g., at least one impurity, the first particulate material) preferably removed have a particle size greater than 100 nm, more preferably greater than 150 nm, and further preferably greater than 200 nm. In one aspect of the 75th embodiment, preferably, the particles (e.g., at least one impurity, the first particulate material) removed have a particle size of 50 mm or less, more preferably 20 mm or less, even more preferably 10 mm or less, and further preferably 5 mm or less.

[0259] In a preferred embodiment of the method for producing a first intermediate product, the method further comprises conveying the first intermediate mixture to a volume section V 5 This preferred embodiment is the 76th embodiment of the present invention, which preferably depends on any one of the 1st to 75th embodiments of the present invention.

[0260] In one aspect of the 76th embodiment, the first intermediate mixture is preferably removed from the volume segment V 3 Convey to volume segment V 5 However, more preferably, the first intermediate mixture is removed from volume segment V via at least one or all of the following: 3 Convey to volume segment V 5 :Volume segment V 4 , filtering device. In this aspect, it is particularly preferred to convey the first intermediate mixture from the filtering device to the volume section V 5 .

[0261] In a preferred embodiment of the method for producing a first intermediate product, the method further comprises adjusting, preferably in the volume section V 5 In the step of adjusting the b value of the Hunter Lab color coordinates of the first intermediate mixture, b≤0, more preferably b≤-1, and further preferably b≤-2. This preferred embodiment is the 77th embodiment of the present invention, which preferably depends on any one of the 1st to 76th embodiments of the present invention.

[0262] In one aspect of the 77th embodiment, preferably, adjusting, preferably in the volume segment V 5 The Hunter Lab color coordinates of the first intermediate mixture are such that b is in the range of -10 to -3, more preferably in the range of -9 to -4, and further preferably in the range of -8 to -6.

[0263] In a preferred embodiment of the method for producing a first intermediate product, the method further comprises adjusting, preferably in the volume section V 5 In the step of adjusting the L value of the Hunter Lab color coordinates of the first intermediate mixture, L≥65, more preferably L≥70, and further preferably L≥75. This preferred embodiment is the 78th embodiment of the present invention, which preferably depends on any one of the 1st to 77th embodiments of the present invention.

[0264] In one aspect of the 78th embodiment, preferably, adjusting, preferably in the volume segment V 5 The Hunter Lab color coordinates of the first intermediate mixture are such that L is in the range of 65 to 92, more preferably in the range of 70 to 86, and further preferably in the range of 75 to 82.

[0265] In a preferred embodiment of the method for producing a first intermediate product, by introducing, preferably in a volume segment V 5 In the first intermediate mixture, at least one colorant is added to adjust the Hunter Lab color coordinates L, b or both. This preferred embodiment is the 79th embodiment of the present invention, which preferably depends on any one of the 77th to 78th embodiments of the present invention.

[0266] Suitable colorants are well known to those skilled in the art and are commercially available from Avient Corporation (USA) and Clariant AG (Switzerland).

[0267] In a preferred embodiment of the method for producing a first intermediate product, the amount of the at least one colorant added to the first intermediate mixture is determined by at least one or all of the following:

[0268] a. adding less than 200ppm wt, more preferably less than 100ppm wt, even more preferably less than 50ppm wt, further preferably less than 20ppm wt, even further preferably less than 15ppm wt, and particularly preferably less than 10ppm wt of a red colorant;

[0269] b. adding less than 300ppm wt, more preferably less than 150ppm wt, even more preferably less than 70ppm wt, further preferably less than 30ppm wt, even further preferably less than 20ppm wt, and particularly preferably less than 15ppm wt of a blue colorant;

[0270] c. Adding a red colorant and a blue colorant, wherein the ratio of the red colorant to the blue colorant is in the range of 0.1 to 10.0, more preferably in the range of 0.1 to 6.0, even more preferably in the range of 0.1 to 3.0, further preferably in the range of 0.1 to 1.0, even further preferably in the range of 0.3 to 0.8, and particularly preferably in the range of 0.4 to 0.7.

[0271] This preferred embodiment is the 80th embodiment of the present invention, which is preferably dependent on the 79th embodiment of the present invention.

[0272] In the 80th embodiment, the ppm mass value is based on the total mass of the first intermediate mixture. In one aspect of the 80th embodiment, all possible combinations of features a. to c. are preferred aspects of this embodiment. These combinations are, for example, a; b; c; a+b; a+c; b+c; a+b+c. In one aspect of the 80th embodiment, feature a., optionally at least 1 ppm wt, optionally at least 2 ppm wt, optionally at least 3 ppm wt of red colorant is added. In one aspect of the 80th embodiment, feature b., optionally at least 0.8 ppm wt, optionally at least 1.8 ppm wt, optionally at least 2.7 ppm wt of blue colorant is added. In the 80th embodiment, in feature c., the ratio of red colorant to blue colorant is calculated by dividing the ppm wt of the added red colorant by the ppm wt of the added blue colorant. In a preferred aspect of the 80th embodiment, feature c., both the red colorant and the blue colorant are added before any colorant is added, and the L value of the first intermediate mixture is preferably in the range of 80 to 90, more preferably in the range of 82 to 88. In a preferred aspect of the 80th embodiment, feature c., both the red colorant and the blue colorant are added before any colorant is added, and the b value of the first intermediate mixture is preferably in the range of 0.8 to 2.0, more preferably in the range of 1 to 2.

[0273] In a preferred embodiment of the method for producing the first intermediate product, at least one colorant is selected from a dye, a toner, a pigment and a combination of at least two. This preferred embodiment is the 81st embodiment of the present invention, which preferably depends on any one of the 79th to 80th embodiments of the present invention.

[0274] In one aspect of the 81st embodiment, it is particularly preferred that at least one colorant is a pigment, a dye, or a combination thereof. In this regard, pigments are more preferred than dyes. In another aspect of the 81st embodiment, it is preferred that at least one colorant is not an acid dye. In another aspect of the 81st embodiment, it is preferred that at least one colorant is a pigment having a particle size of less than 20 microns, more preferably less than 10 microns, even more preferably less than 1 micron, and further preferably less than 0.5 microns.

[0275] In a preferred embodiment of the method for producing a first intermediate product, the first polyester passes through a volume segment V 2 The conveying direction is at least partially opposite to the direction of gravity. In one aspect of this embodiment, it is preferred that the conveying direction is opposite to the direction of gravity. In a preferred embodiment of the method for producing a first intermediate product, the volume segment V 2 At least partially vertical arrangement, more preferably vertical arrangement. At least partially vertical arrangement is preferably understood as volume segment V 2 The longest dimension (e.g., length) of is not parallel to the ground. For example, if the volume segment V2 Arranged vertically, the volume segment V 2 The length is perpendicular to the ground.

[0276] In a preferred embodiment of the method for producing a first intermediate product, the intrinsic viscosity of the first intermediate product is in the volume range V 4 In a preferred embodiment of the method for producing a first intermediate product, the intrinsic viscosity of the first intermediate product is in the volume segment V 4 In a preferred embodiment of the method for producing a first intermediate product, the intrinsic viscosity of the first intermediate product is less than 5%, more preferably less than 3%, further preferably less than 1%, and even further preferably less than 0.1%. 4 The average change (neither increase nor decrease) is less than 5%, more preferably less than 3%, further preferably less than 1%, and even further preferably less than 0.1%.

[0277] The 82nd embodiment of the present invention is a method for producing another intermediate product, comprising the following steps:

[0278] a. providing a first intermediate mixture comprising a first intermediate product, wherein the first intermediate product can be obtained by a method for producing a first intermediate product according to the present invention, preferably a method according to any one of Embodiments 1 to 81 of the present invention;

[0279] b. Increasing the weight average molar mass of the first intermediate product in the first intermediate mixture, preferably in the volume segment V 6 to obtain another intermediate mixture comprising another intermediate product.

[0280] In an optional aspect of the 82nd embodiment, the first intermediate mixture comprises at least one or all of the following: a first organic compound, another organic compound. The first organic compound and / or another organic compound in the other intermediate mixture may be present due to, for example, one of the following reasons: the first organic compound and / or another organic compound is removed from another volume segment (e.g., volume segment V 5 ) is transported to volume segment V 6 ; The first organic compound and / or the other organic compound are bound and released during the increase in weight average molar mass. In another optional aspect of the 82nd embodiment, the other intermediate mixture comprises at least one or all of the following: the first organic compound, the other organic compound. In one aspect of the 82nd embodiment, preferably in the volume segment V 6At least one or all of the following are at least partially removed from the mixture: a first organic compound, another organic compound. In another aspect of the 82nd embodiment, it is preferred that the other intermediate mixture contains less than 1 wt-%, more preferably less than 0.1 wt-%, and further preferably less than 0.01 wt-% of at least one or all of the following: a first organic compound, another organic compound, based on the total mass of the other intermediate mixture. In one aspect of the 82nd embodiment, it is preferred that less than 20 wt-%, more preferably less than 10 wt-%, even more preferably less than 5 wt-%, and further preferably less than 1 wt-% of the original product is used to obtain the other intermediate product. The wt-% is based on the total mass of the first intermediate mixture. Here, the original product has the following characteristics: a.) It is a monomer, an oligomer, a polymer or a combination thereof, preferably a first polyester; b.) It is obtained by chemical synthesis, wherein the chemical synthesis does not include depolymerization and solvent decomposition. An example of the original product is a BHET monomer obtained by esterification of terephthalic acid with ethylene glycol.

[0281] In a preferred embodiment of the method for producing a further intermediate product, by conveying the first intermediate mixture to the volume section V 6 To provide a first intermediate mixture. This preferred embodiment is the 83rd embodiment of the present invention, which preferably depends on the 82nd embodiment of the present invention.

[0282] In one aspect of the 83rd embodiment, the first intermediate mixture is preferably removed from the volume segment V 3 Convey to volume segment V 6 However, more preferably, the first intermediate mixture is removed from the volume segment V by at least one or all of the following: 3 Convey to volume segment V 6 :Volume segment V 4 , filtration device, volume segment V 5 In this respect, it is particularly preferred to remove the first intermediate mixture from the volume segment V 5 Convey to volume segment V 6 .

[0283] In a preferred embodiment of the method for producing another intermediate product, at least one or all of the following substances are added to the first intermediate mixture:

[0284] a. an amount of catalyst in the range of 20 ppm to 600 ppm, more preferably in the range of 30 ppm to 500 ppm, and further preferably in the range of 40 ppm to 400 ppm;

[0285] b. An amount of stabilizer in the range of 1 ppm to 120 ppm, more preferably in the range of 5 ppm to 100 ppm, even more preferably in the range of 10 ppm to 80 ppm, further preferably in the range of 20 ppm to 60 ppm.

[0286] This preferred embodiment is the 84th embodiment of the present invention, which preferably depends on any one of the 82nd to 83rd embodiments of the present invention.

[0287] In the 84th embodiment, the ppm value is based on the total mass of the first intermediate mixture. In one aspect of the 84th embodiment, all possible combinations of features a. and b. are preferred aspects of this embodiment. These combinations are, for example, a; b; a+b. In one aspect of the 84th embodiment, the preferred catalyst is Sb 2 O 3 , tetrabutoxytitanium, PTO(K 2 TiO(C 2 H 4 ) 2 *2H 2 O) or a combination of at least two thereof. In this aspect, Sb 2 O 3 In one aspect of the 84th embodiment, at least one or all of the following is preferably applied: in the first intermediate mixture entering the volume section V 6 Add the catalyst before; in volume segment V 6 The catalyst is added to the first intermediate mixture, preferably before increasing the weight average molar mass of the first intermediate product. In one aspect of the 84th embodiment, the preferred stabilizer is diphenylamine, 4-aminobenzoic acid, orthophosphoric acid, or a combination of at least two thereof. In one aspect of the 84th embodiment, at least one or all of the following is preferably applicable: before the first intermediate mixture enters the volume segment V 6 Preferably, the stabilizer is added to the volume segment V before increasing the weight average molar mass of the first intermediate product. 6 in the first intermediate mixture.

[0288] In a preferred embodiment of the method for producing a further intermediate product, at least one or all of the following apply to volume segment V 6 :

[0289] a. a temperature in the range of 260°C to 295°C, more preferably in the range of 268°C to 289°C, and further preferably in the range of 272°C to 285°C;

[0290] b. The pressure is equal to or less than 3.7 kPa, more preferably equal to or less than 3.3 kPa, and further preferably equal to or less than 2.8 kPa.

[0291] This preferred embodiment is the 85th embodiment of the present invention, which preferably depends on any one of the 83rd to 84th embodiments of the present invention.

[0292] In one aspect of the 85th embodiment, all possible combinations of features a. and b. are preferred aspects of the embodiment. These combinations are, for example, a; b; a+b. In one aspect of the 85th embodiment, the preferred pressure is in the range of 0.01 kPa to 3.70 kPa, more preferably in the range of 0.05 kPa to 3.30 kPa, and further preferably in the range of 0.10 kPa to 2.80 kPa.

[0293] In a preferred embodiment of the method for producing a further intermediate product, the first intermediate mixture is present in a volume segment V 6 The residence time in is less than 750 minutes, more preferably less than 500 minutes, even more preferably less than 350 minutes, and further preferably less than 200 minutes. This preferred embodiment is the 86th embodiment of the present invention, which preferably depends on any one of the 83rd to the 85th embodiments of the present invention.

[0294] In one aspect of the 86th embodiment, the first intermediate mixture is preferably in a volume segment V 6 The residence time in the reaction mixture is 40 minutes or longer, more preferably 70 minutes or longer, and further preferably 150 minutes or longer.

[0295] In a preferred embodiment of the method for producing a further intermediate product, the further intermediate product preferably leaves the volume segment V 6 Another intermediate product having at least one or all of the following characteristics:

[0296] a. an intrinsic viscosity in the range of 0.15 dL / g to 0.45 dL / g, more preferably in the range of 0.18 dL / g to 0.40 dL / g, and further preferably in the range of 0.20 dL / g to 0.30 dL / g;

[0297] b. The weight average molar mass is in the range of 5000 Da to 30000 Da, more preferably in the range of 9000 Da to 24000 Da, even more preferably in the range of 12000 Da to 20000 Da, and further preferably in the range of 14000 Da to 16500 Da.

[0298] This preferred embodiment is the 87th embodiment of the present invention, which preferably depends on any one of the 82nd to 86th embodiments of the present invention.

[0299] In one aspect of the 87th embodiment, all possible combinations of features a. and b. are preferred aspects of this embodiment. These combinations are, for example, a; b; a+b.

[0300] In a preferred embodiment of the method for producing a further intermediate product, the method further comprises conveying the further intermediate mixture, preferably from volume segment V 6 Transport to volume segment V 7 , steps. This preferred embodiment is the 88th embodiment of the present invention, which preferably depends on any one of the 82nd to 87th embodiments of the present invention.

[0301] In a preferred embodiment of the method for producing a further intermediate product, the method further comprises the step of further increasing the weight average molar mass of the further intermediate product in the further intermediate mixture, preferably in the volume segment V 7 This preferred embodiment is the 89th embodiment of the present invention, which preferably depends on any one of the 82nd to 88th embodiments of the present invention.

[0302] In a preferred embodiment of the method for producing another intermediate product, at least one or all of the following apply to volume segment V 7 :

[0303] a. a temperature in the range of 240°C to 310°C, more preferably in the range of 258°C to 298°C, and further preferably in the range of 264°C to 288°C;

[0304] b. The pressure is equal to or less than 0.4 kPa, more preferably equal to or less than 0.35 kPa, and further preferably equal to or less than 0.32 kPa.

[0305] This preferred embodiment is the 90th embodiment of the present invention, which preferably depends on any one of the 88th to 89th embodiments of the present invention.

[0306] In one aspect of the 90th embodiment, all possible combinations of features a. and b. are preferred aspects of this embodiment. These combinations are, for example, a; b; a+b. In one aspect of the 90th embodiment, the temperature given in the preferred embodiment is in the volume segment V 7 The temperature measured at the inlet of the intermediate mixture, preferably at the inlet of the intermediate mixture into the volume segment V 7 In one aspect of the 90th embodiment, the pressure is preferably in the range of 0.001 kPa to 0.400 kPa, more preferably in the range of 0.005 kPa to 0.350 kPa.

[0307] In a preferred embodiment of the method for producing a further intermediate product, the further intermediate mixture is present in a volume segment V 7The residence time in is less than 300 minutes, more preferably less than 200 minutes, even more preferably less than 150 minutes, and further preferably less than 100 minutes. This preferred embodiment is the 91st embodiment of the present invention, which preferably depends on any one of the 88th to the 90th embodiments of the present invention.

[0308] In one aspect of the 91st embodiment, preferably, the other intermediate mixture is in the volume segment V 7 The residence time in the reaction mixture is 10 minutes or longer, more preferably 25 minutes or longer, and further preferably 40 minutes or longer.

[0309] In a preferred embodiment of the method for producing a further intermediate product, the further intermediate product preferably leaves the volume segment V 7 Another intermediate product having at least one or all of the following characteristics:

[0310] a. an intrinsic viscosity in the range of 0.50 dL / g to 0.80 dL / g, more preferably in the range of 0.57 dL / g to 0.75 dL / g, and further preferably in the range of 0.62 dL / g to 0.67 dL / g;

[0311] b. The weight average molar mass is in the range of 40000 Da to 60000 Da, more preferably in the range of 44000 Da to 54000 Da, and further preferably in the range of 46000 Da to 52000 Da.

[0312] This preferred embodiment is the 92nd embodiment of the present invention, which preferably depends on any one of the 82nd to 91st embodiments of the present invention, and more preferably is based on any one of the 88th to 91st embodiments of the present invention.

[0313] In one aspect of the 92nd embodiment, all possible combinations of features a. and b. are preferred aspects of this embodiment. These combinations are, for example, a; b; a+b.

[0314] In a preferred embodiment of the method for producing a further intermediate product, the method further comprises a step of at least partially removing at least one organic compound, preferably in volume segment V 6 , Volume segment V 7 This preferred embodiment is the 93rd embodiment of the present invention, which preferably depends on any one of the 82nd to 92nd embodiments of the present invention.

[0315] In one aspect of the 93rd embodiment, it is preferred that the at least one organic compound is at least one or all of the following: a first organic compound, another organic compound. In another aspect of the 93rd embodiment, it is preferred that the at least one organic compound is at least partially removed from at least one or all of the following: a first intermediate mixture and another intermediate mixture. In another aspect of the 93rd embodiment, it is preferred that the first organic compound is at least partially removed by flash distillation. In one aspect of the 93rd embodiment, it is preferred that the at least one organic compound is at least partially removed simultaneously with at least one or all of the following: increasing the weight average molar mass of the first intermediate product, and increasing the weight average molar mass of another intermediate product.

[0316] In a preferred embodiment of the method for producing another intermediate product, the other intermediate product is another polyester. This preferred embodiment is the 94th embodiment of the present invention, which preferably depends on any one of the 82nd to 93rd embodiments of the present invention.

[0317] In a preferred embodiment of the method for producing another intermediate product, the other polyester is selected from polyethylene terephthalate, polybutylene terephthalate, polylactide, polytrimethylene terephthalate, polyethylene naphthalate, polycarbonate, polyester carbonate, polyarylate, polyester resin (preferably unsaturated polyester resin) and a combination of two or more thereof. This preferred embodiment is the 95th embodiment of the present invention, which is preferably dependent on the 94th embodiment of the present invention.

[0318] In one aspect of the 95th embodiment, it is particularly preferred that the other polyester is polyethylene terephthalate.

[0319] In a preferred embodiment of the method for producing another intermediate product, the other intermediate product is in the form of a liquid (e.g., a melt or a molten polymer), a particle, or a combination thereof. This preferred embodiment is the 96th embodiment of the present invention, which preferably depends on any one of the 82nd to 95th embodiments of the present invention.

[0320] In one aspect of the 96th embodiment, the particles are generally referred to as chips. In one aspect of the 96th embodiment, the particles are preferably obtained by extruding and cooling a hot melt.

[0321] In a preferred embodiment of the method for producing another intermediate product, the other intermediate product undergoes at least one processing step to obtain a product. This preferred embodiment is the 97th embodiment of the present invention, which preferably depends on any one of the 82nd to 96th embodiments of the present invention.

[0322] In one aspect of the 97th embodiment, it is preferred that the other intermediate product has a volume range of V 6 downstream, more preferably in volume segment V 7downstream of which undergoes at least one processing step.

[0323] In a preferred embodiment of the method for producing another intermediate product, at least one processing step comprises at least one or all of the following: cooling, spinning, texturing, coloring (preferably by adding at least one colorant), melting, injection molding, blow molding, coating (preferably spin coating), cutting, extrusion, or a combination of at least two thereof. This preferred embodiment is the 98th embodiment of the present invention, which is preferably dependent on the 97th embodiment of the present invention.

[0324] The 99th embodiment of the present invention is a first intermediate product obtainable by the method for producing a first intermediate product according to the present invention, preferably the method according to any one of the 1st to 81st embodiments of the present invention.

[0325] The 100th embodiment of the present invention is another intermediate product obtainable by a method for producing another intermediate product according to the present invention, preferably a method according to any one of the 82nd to 98th embodiments of the present invention.

[0326] In one aspect of the 100th embodiment, the other intermediate product is preferably another polyester.

[0327] In a preferred embodiment of the further intermediate product, the further intermediate product has at least one or all of the following characteristics:

[0328] a. a weight average molar mass in the range of 40000Da to 100000Da, more preferably in the range of 44000Da to 80000Da, and further preferably in the range of 48000Da to 60000Da;

[0329] b. an intrinsic viscosity in the range of 0.50 dL / g to 0.80 dL / g, more preferably in the range of 0.57 dL / g to 0.75 dL / g, and further preferably in the range of 0.62 dL / g to 0.67 dL / g;

[0330] c. In Hunter Lab color coordinates, the L value is at least 48 and the b value is 6 or less.

[0331] This preferred embodiment is the 101st embodiment of the present invention, which is preferably dependent on the 100th embodiment of the present invention.

[0332] In one aspect of the 101st embodiment, all possible combinations of features a. to c. are preferred aspects of this embodiment. These combinations are, for example, a; b; c; a+b; a+c; b+c; a+b+c. In one aspect of the 101st embodiment, feature c., it is preferred that the other intermediate product has an L value in the range of 45 to 75 in Hunter Lab color coordinates, more preferably in the range of 50 to 70, and further preferably in the range of 55 to 65. In one aspect of the 101st embodiment, feature c., it is preferred that the other intermediate product has a b value in the range of 0 to 6 in Hunter Lab color coordinates, more preferably in the range of 1 to 5, and further preferably in the range of 2 to 4.

[0333] The 102nd embodiment of the present invention is a product comprising another intermediate product according to the present invention, preferably another intermediate product according to any one of the 100th to 101st embodiments of the present invention.

[0334] In a preferred embodiment of the product, the product is selected from yarn, textile, shaped article (e.g., bottle), molding material, film, sheet, granule, composite material, foam, fiber, lubricant, adhesive, thickener, suspending agent, flocculant, resin, plastic, coating, building material, absorbent material, medicine, material for controlled release of active substance, powder and a combination of at least two or more thereof. This preferred embodiment is the 103rd embodiment of the present invention, which is preferably dependent on the 102nd embodiment of the present invention.

[0335] In one aspect of the 103rd embodiment, it is particularly preferred that the product is a yarn, more preferably a yarn for textiles. Examples of yarns include fully stretched yarns, stretched textured yarns, and partially oriented yarns.

[0336] In a preferred embodiment of the product, the product has at least one or all of the following characteristics:

[0337] a. In the Hunter Lab color coordinates, the L value is at least 62, more preferably at least 68, and further preferably at least 73;

[0338] b. In the Hunter Lab color coordinates, the b value is at least 1, more preferably at least 2, and further preferably at least 3;

[0339] c. The tensile strength is 1.5 g / Denier or more, preferably 2.0 g / Denier or more, and further preferably 2.5 g / Denier or more;

[0340] d. a weight average molar mass in the range of 40,000 to 100,000 Da, more preferably in the range of 44,000 to 80,000 Da, further preferably in the range of 48,000 to 60,000 Da;

[0341] e. an intrinsic viscosity in the range of 0.50 dL / g to 0.80 dL / g, more preferably in the range of 0.57 dL / g to 0.75 dL / g, further preferably in the range of 0.62 dL / g to 0.67 dL / g;

[0342] f. The elongation is in the range of 5% to 175%, more preferably in the range of 10% to 150%, further preferably in the range of 20% to 125%.

[0343] This preferred embodiment is the 104th embodiment of the present invention, which preferably depends on any one of the 102nd to 103rd embodiments of the present invention.

[0344] In one aspect of the 104th embodiment, all possible combinations of features a. to f. are preferred aspects of the embodiment. These combinations are, for example, a; b; c; d; e; f; a+b; a+c; a+d; a+e; a+f; b+c; b+d; b+e; b+f; c+d; c+e; c+f; d+e; d+f; e+f; a+b+c; a+b+d; a+b+e; a+b+f; a+c+d; a+c+e; a+c+f; a+d+e; a+d+f; a+e+f; b+c+d; b+c+e; b+c+f; b+d+e; b+d+f; b+e+f; c+d+e; c+d+f; c+e+f; d+ e+f;a+b+c+d;a+b+c+e;a+b+c+f;a+b+d+e;a+b+d+f;a+b+e+f;a+c+d+e;a+c+d+f;a+c+e+f;a+d+e+f;b+c+d+e;b+c+d+ f; b+c+e+f; b+d+e+f; c+d+e+f; a+b+c+d+e; a+b+c+d+f; a+b+c+e+f; a+b+d+e+f; a+c+d+e+f; b+c+d+e+f; a+b+c+d+e+f. In one aspect of the 104th embodiment, feature a., if the product is a yarn, it is preferred that the product has an L value in the Hunter Lab chromaticity coordinates ranging from 62 to 95, more preferably, ranging from 68 to 90, and further preferably, ranging from 73 to 87. In one aspect of the 104th embodiment, feature b., if the product is a yarn, it is preferred that the product has a b in the Hunter Lab chromaticity coordinates ranging from 1 to 7, more preferably, ranging from 2 to 6, and further preferably, ranging from 3 to 5. In the 104th embodiment, tensile strength and elongation are measured according to standard ASTM D2256 / D2256M-21.

[0345] The 105th embodiment of the present invention is the use of the first intermediate product according to the present invention (preferably the first intermediate product according to the 99th embodiment of the present invention) for producing another intermediate product (preferably further polyester).

[0346] In one aspect of the 105th embodiment, preferably, another intermediate product produced is any one of the 100th to 101st embodiments of the present invention.

[0347] The 106th embodiment of the present invention is the use of another intermediate product according to the present invention (preferably according to any one of the 100th to 101st embodiments of the present invention) for producing a product, preferably a product produced according to any one of the 102nd to 104th embodiments of the present invention.

[0348] Detailed description of the invention

[0349] Throughout the document, the disclosure of a range should preferably be understood as including both endpoints of the range. In addition, the disclosure of each range in the document should preferably be understood as also disclosing a preferred sub-range in which one endpoint is excluded or both endpoints are excluded. For example, the disclosure of a range of 60°C to 75°C should be understood as disclosing a range including both endpoints of 60°C and 75°C. In addition, it should also be understood as disclosing a range including endpoint 60°C but not including endpoint 75°C, a range excluding endpoint 60°C but including endpoint 75°C, and a range excluding both endpoints of 60°C and 75°C.

[0350] Throughout the document, preferred embodiments and preferred aspects that disclose two or more features with preferred ranges or alternatives should be understood to include all possible combinations of these features. For example, an embodiment in which "wt-%a of feature A, more preferably wt-%b of feature A, and further preferably wt-%c of feature A has a length of x, more preferably wt-%c of feature A has a length of y, and further preferably wt-%c of feature A has a length of z" discloses all embodiments having the following combinations of features: a, x; a, y; a, z; b, x; b, y; b, z; c, x; c, y; c, z.

[0351] Some preferred embodiments and preferred aspects may include different combinations of features. If various combinations are listed, the combinations are separated by semicolons (";"). For example, the list "a; a+b; a+c+d" should be understood to disclose an embodiment including feature "a", an embodiment including features "a" and "b", and an embodiment including features "a", "c", and "d".

[0352] The following abbreviations are used in the description: polyethylene terephthalate (PET), polyvinyl chloride (PVC), ethylene glycol (EG), monoethylene glycol (MEG), bis(2-hydroxyethyl)terephthalate (BHET).

[0353] Volume Segment

[0354] "Volume segment" (e.g., V 1 、V 2 ) is best understood to refer to a volume designed and arranged to receive a certain amount of solids, liquids, gases, or a combination thereof. Examples of "volume segments" include storage tanks, storage vessels, reactors (e.g., depolymerization reactors), pipelines, siphons, or a combination of two or more thereof. The numbering of volume segments is best understood as a means of identifying the volume segment. For example, if in volume segment V 1 and V 3 The method of producing the first intermediate product is performed in the volume segment V, which does not mean that the method is also performed in the volume segment V 2 Executed in.

[0355] In one aspect of the present invention, it is preferred that at least two volume segments at least partially intersect in space. 1 The first amount of the first organic compound is contacted with the first organic compound, while the volume segment V 3 The weight average molar mass of the first polyester is reduced. If the volume segment V 1 and V 3 refers to the same internal volume of the reactor, then the volume segment V 1 and V 3 Intersect in space. If two volume segments (e.g. a first volume segment and a further volume segment) intersect in space, the volume segments differ from one another in that at least one physical parameter (e.g. temperature) in the volume segments differs by at least 15%. For example, the average temperature of the first volume segment is 60° C. and the average temperature of the further volume segment is 120° C. If two volume segments (e.g. a first volume segment and a further volume segment) intersect in space, for example, the transfer of the first initial mixture from the first volume segment to the further volume segment should preferably be understood to mean that at least one physical parameter (e.g. temperature) in the volume segment changes by at least 15%.

[0356] In another more preferred aspect of the present invention, at least two, more preferably at least three, even more preferably at least four, and further preferably all volume segments spatially intersect less than 30%, more preferably less than 20%, and further preferably less than 10%. In this regard, preferably at least two volume segments are located in the same container, such as a reactor or a storage tank. However, in this regard, more preferably the volume segments are located in different containers, such as reactors or storage tanks.

[0357] In one aspect of the present invention, it is preferred that the first polyester is from volume segment V 1 Transport to volume segment V 2 In this aspect, it is preferred that the first polyester exit volume segment V 1 At least one outlet is arranged at a distance from the volume segment V 1 The bottom of the first polyester is less than 50 cm, more preferably less than 40 cm, and further preferably less than 35 cm. In this aspect, it is preferred that the first polyester enters the volume segment V 2 At least one inlet (eg, an inlet of the first type) is arranged at a distance from the volume segment V 2 The bottom of the volume segment is less than 50 cm, more preferably less than 40 cm, and further preferably less than 30 cm. The distance from the bottom of the volume segment to the inlet (or outlet) is measured from the bottom of the volume segment to the point closest to the bottom of the inlet (or outlet).

[0358] In one aspect of the present invention, preferably at least one, more preferably at least two, even more preferably at least three, and further preferably all volume segments are fluidly connected. In another aspect of the present invention, preferably at least one or all of the following apply: volume segment V 1 With volume segment V 2 Fluid communication; volume segment V 2 With volume segment V 3 Fluid communication; volume segment V 3 With volume segment V 4 Fluid communication; volume segment V 4 With volume segment V 5 Fluid communication; volume segment V 5 With volume segment V 6 Fluid communication; volume segment V 6 With volume segment V 7 Fluid communication; volume segment V 1 With volume segment V 3 Fluid communication; volume segment V 3 With volume segment V 5 Fluid communication; volume segment V 3 With volume segment V 7 Fluid communication; volume segment V 5 With volume segment V 7 Fluid connected.

[0359] In one aspect of the present invention, preferably at least one, more preferably at least two, even more preferably at least three, and further preferably all volume segments are in fluid communication with at least one filtering device. In one aspect of the present invention, preferably at least one or all of the following apply: volume segment V 4 Connected to at least one filtering device fluid; volume segment V 5 In fluid communication with at least one filter device.

[0360] In one aspect of the present invention, preferably the volume segment V 2 The invention has a first region and another region. In this aspect, the other region is preferably located downstream of the first region. In this aspect, the mass ratio of the first polyester to the first organic compound in the first region is preferably different from the mass ratio of the first polyester to the first organic compound in the other region. It is further preferred that the mass ratio of the first polyester to the first organic compound in the first region is smaller than the mass ratio of the first polyester to the first organic compound in the other region.

[0361] In one aspect of the present invention, preferably, the volume segment V 2 There is a first region and another region, wherein the first region and the another region are not adjacent to each other.

[0362] In another aspect of the present invention, preferably the volume segment V 2There is a first region and a further region, wherein the first region and the further region are adjacent to each other. In this aspect, preferably the first region and the further region are at least partially separated by a boundary. Preferably the boundary is a physical boundary and an imaginary boundary, or a combination thereof. Preferably the imaginary boundary is defined as a volume segment V 2 A location in a volume where a measurable physical property changes rapidly. An example of a physical property is a volume segment V 2 The mass ratio of the first polyester to the first organic compound in the volume segment V is preferably defined as a value of a physical property that changes by at least 50%, more preferably at least 60%, and further preferably at least 70% within a distance of less than 50 cm, more preferably less than 30 cm, and further preferably less than 15 cm. For example, the imaginary boundary can be defined by the volume segment V 2 An example of a physical boundary between the first region and the further region is a sieve.

[0363] In one aspect of the present invention, preferably, the volume segment V 1 Adapted and arranged to at least one or all of: remove at least one impurity from the surface of the first polyester (e.g., remove a label from a PET sheet), remove at least one impurity from the first initial mixture, and remove at least one impurity from the raw material (e.g., dust).

[0364] In one aspect of the present invention, preferably the volume segment V 2 The method is designed and arranged to at least one or all of: remove at least one impurity from a mixture comprising a first polyester and a first organic compound, at least partially depolymerize the first polyester (preferably by solvolysis), and embrittle the first polyester. "Embellishing" is preferably understood as a process of making the first polyester more brittle. For example, if the first polyester is in the form of PET flakes, the force required to break the flakes into smaller fragments after embrittlement is less than the force required to break the PET flakes into smaller fragments before embrittlement.

[0365] In one aspect of the present invention, preferably, the volume segment V 3 Designed and arranged to at least partially depolymerize the first polyester, preferably using solvolysis.

[0366] In one aspect of the present invention, preferably, the volume segment V 4 Suitable and arranged for at least one or all of: mixing a liquid with a particulate material, and heating the liquid.

[0367] In one aspect of the present invention, preferably, the volume segment V 5 Designed and arranged to at least one or all of the following: store liquid, maintain the temperature of liquid, heat liquid, or a combination of at least two thereof.

[0368] In one aspect of the present invention, preferably, the volume segment V 6 Designed and arranged to at least partially polymerize, more preferably by polycondensation, at least one or all of the following: monomers and oligomers.

[0369] In one aspect of the present invention, preferably, the volume segment V 7 Designed and arranged to at least partially polymerize, more preferably by polycondensation, at least one or all of the following: monomers and oligomers.

[0370] In one aspect of the present invention, preferably, A1.) the first polyester and the volume segment V 2 A2.) the weight average molar mass of the first polyester is in the volume segment V 2 In this respect, preferably, steps A1.) and A2.) are carried out at least partially simultaneously.

[0371] In one aspect of the present invention, preferably, B1.) the first polyester and the volume segment V 3 and B2.) the weight average molar mass of the first polyester is in the volume segment V 3 In this respect, steps B1.) and B2.) are preferably carried out at least partially simultaneously.

[0372] Fluid connections

[0373] The phrase "fluid communication" should preferably be understood as meaning that if the first component (e.g., volume segment V 1 ) and another component (e.g. volume segment V 2 ) are in fluid communication with each other, then a fluid, a gas or a combination thereof can flow from a first component to another component, or from another component to the first component, or both. It should also be preferably understood that if components are "in fluid communication" with each other, this does not mean that the components must be adjacent to each other. For example, a further component is arranged between the first component and the further component. If, for example, a fluid can flow from the first component to the further component, the first component and the further component are "in fluid communication".

[0374] In one aspect of the present invention, if a first component is in fluid communication with another component, and the other component is in fluid communication with the further component, this should preferably be understood to mean that the first component and the further component are in fluid communication with each other.

[0375] In one aspect of the present invention, preferably, at least one or all of the following can be transported between two components in fluid communication with each other: a solid, a mixture of a solid and a fluid, a mixture of a solid and a gas, and a mixture of a solid, a liquid, and a gas. For example, a mixture comprising PET flakes and MEG can be transported between two volume segments in fluid communication with each other using an Archimedean screw, a siphon, or a combination thereof.

[0376] Mass ratio of the first polyester to the organic compound

[0377] The mass ratio of the first polyester to the organic compound (eg, the first organic compound, the further organic compound) is preferably understood as the mass ratio of the first polyester to the free organic compound.

[0378] raw material

[0379] In one aspect of the present invention, a "feedstock" comprising a first polyester is provided. In this aspect, the feedstock may optionally contain one or more other components, such as at least one impurity. In various aspects and preferred aspects of the present invention, the first polyester is contacted with an organic compound (e.g., a first organic compound, another organic compound). Such contact of the first polyester with the organic compound is preferably understood to include the following two situations: a.) before contacting with the organic compound, at least one other component of the feedstock is at least partially separated from the first polyester (i.e., the originally provided feedstock no longer exists or its composition has been changed), and it is the first polyester (wherein at least one other component is at least partially removed) that is contacted with the organic compound; b.) the feedstock is contacted with the organic compound without at least partially removing at least one other component. The above, after necessary modifications, preferably applies to the transportation of the first polyester.

[0380] For example, the first polyester and the first organic compound are in the volume segment V 1 The first polyester is provided as part of a feedstock that also contains impurities. Impurities are not removed prior to contact. That is, the contact of the first polyester with the first organic compound is equivalent to the contact of the feedstock with the first organic compound. 1 In the process, the impurities are partially removed and the first polyester together with some of the impurities that have not been removed is conveyed to volume section V 2 Here, the first polyester and the impurities transported are no longer identical to the raw material originally supplied.

[0381] Multiple fragments

[0382] "Product item" is preferably understood to mean an item comprising the first polyester. Examples of product items include: items that have been used at least once, preferably by a consumer (e.g., post-consumer waste); items that have been produced but never used (e.g., items that have been rejected due to not meeting quality requirements); items that are by-products of a production process (e.g., scraps). Examples of product items include bottles and thermoformed items. In a preferred aspect of the present invention, the product item is a bottle and a thermoformed item, more preferably a bottle.

[0383] In one aspect of the present invention, it is preferred that the first polyester in the raw material is in the form of a plurality of fragments. In this aspect, it is preferred that the plurality of fragments is obtained by processing the product article. Examples of processing the product article include shredding, grinding, or a combination thereof. For example, a PET bottle is provided, which is first shredded to obtain PET flakes, and the PET flakes are subsequently ground. In another example, a textile comprising PET is provided, and the textile is shredded to obtain textile fragments. In this aspect in which the raw material is in the form of a plurality of fragments, it is preferred that the product article is processed to obtain a plurality of fragments, wherein at least 50%, more preferably at least 60%, and further preferably at least 70% of the fragments have at least one physical dimension, and the difference between the physical dimension and the average value of at least one physical dimension is less than 50%, more preferably less than 40%, and further preferably less than 30%. An example of at least one physical dimension is the width, length, and thickness of the fragments. For example, at least 70% of the fragments have a width that is less than 40% of the difference from the average width of the plurality of fragments. In another aspect of the present invention, it is preferred that the product is processed before the raw material is contacted with the first amount of the first organic compound.

[0384] The "fragments" of the first polyester preferably have physical dimensions (e.g., length, width, thickness) that are all below the upper limit. Preferably, the upper limit is less than 5 cm, more preferably less than 4 cm, and further preferably less than 3 cm. An example of a plurality of "fragments" is PET flakes, which are well known to those skilled in the art of recycling technology.

[0385] The "first dimension" of a fragment is preferably understood to mean the width, length or both of the fragment. The "length" of a fragment is preferably understood to mean the largest dimension of the fragment. The "width" of a fragment is preferably understood to mean the second largest dimension of the fragment. The "thickness" of a fragment is preferably understood to mean the smallest dimension of the fragment.

[0386] In a preferred aspect of the invention, the geometry of the fragments is not limited. For example, the fragments may be flat, parabolic or irregularly shaped.

[0387] In one aspect of the invention, preferably the plurality of fragments comprises a plurality of first type fragments and a plurality of other type fragments. "First type fragments" are preferably understood as fragments having a maximum thickness of less than 1.0 mm. "Other type fragments" are preferably understood as fragments having a maximum thickness of 1.0 mm or more. Examples of "first type fragments" are fragments obtained by shredding the walls of a PET beverage container. Examples of "other type fragments" are fragments obtained by shredding the bottom of a PET beverage container.

[0388] In the preferred embodiments and description, if "fragments" are mentioned, then preferably fragments constituting a plurality of fragments are to be understood.

[0389] At least one impurity

[0390] In one aspect of the invention, it is preferred that the feedstock contains at least one impurity. In this regard, it is preferred that the feedstock contains less than 3.0 wt-%, more preferably less than 2.0 wt-%, even more preferably less than 1.0 wt-%, further preferably less than 0.5 wt-%, even further preferably less than 0.1 wt-% of at least one impurity based on the total mass of the feedstock.

[0391] Examples of "at least one impurity" include adhesives, paper, sand (e.g., in the form of dust), stones (e.g., gravel), wood, food scraps, at least one metal (e.g., Sb, Fe, Ti, Al), at least one polyolefin (e.g., high-density polyethylene, polyethylene, polypropylene), polystyrene, polyvinyl chloride, fuel (e.g., paraffin, gasoline, diesel), or a combination of two or more thereof. An example of at least one polyolefin impurity is a bottle cap.

[0392] In a preferred aspect of the present invention, wherein the first polyester in the raw material is provided in the form of a plurality of fragments, examples of the at least one impurity are one or all of the following: at least one impurity adhered to the outer surface of the fragments (e.g., labels adhered to the outer surface of PET flakes), at least one impurity mixed with the plurality of fragments (e.g., gravel mixed with PET flakes), or a combination thereof.

[0393] In one aspect of the invention, the raw material is preferably washed, preferably using at least one or all of: water, alkali wash. The preferred alkali wash comprises sodium hydroxide. In this regard, preferably, the raw material is washed before contacting the raw material with the first amount of the first organic compound. For example, according to the present invention, the raw material used in the method for producing the first intermediate product is washed before contacting with the first amount of the first organic compound.

[0394] Number of particles per unit area

[0395] In one aspect of the present invention, at least one or all of the following are preferably applied:

[0396] a. Volume segment V 1 The number of particles per unit area of ​​at least one impurity is at least 100,000 particles / cm 2 , more preferably at least 1,000,000 particles / cm 2 , more preferably at least 3,000,000 particles / cm 2 ;

[0397] b. Volume segment V 2 The number of particles per unit area of ​​at least one impurity in the first region is 3000 particles / cm 2 Up to 350,000 particles / cm 2 The particle size is preferably within the range of 30,000 particles / cm 2 Up to 250,000 particles / cm 2 The particle size is preferably within the range of 100,000 particles / cm 2 Up to 200,000 particles / cm 2 within the scope;

[0398] c. Volume segment V 2 In another area of ​​the 2 Up to 12000 particles / cm 2 In the range of 500 particles / cm 2 Up to 6000 particles / cm 2 In the range of 1000 particles / cm 2 Up to 2000 particles / cm 2 within the range.

[0399] In the above aspects, all possible combinations of features a. to c. are preferred. These combinations are, for example, a; b; c; a+b; a+c; b+c; a+b+c.

[0400] Entrance

[0401] "First type of inlet" is best understood as an inlet designed and arranged to allow the first polyester to enter the volume segment. For example: the volume segment is a reactor and the first type of inlet is an opening in the side of the reactor.

[0402] "Another type of inlet" is best understood to mean an inlet designed and arranged to allow an organic compound (e.g., a first organic compound) to enter the volume segment. A preferred another type of inlet is designed and arranged to allow the organic compound to enter the volume segment in the form of a gas (e.g., a steam). An example of another type of inlet is a gas nozzle, such as a high-pressure gas nozzle.

[0403] A further type of inlet is preferably understood to mean an inlet designed and arranged to allow an organic compound (e.g. a first organic compound) to enter the volume segment. A preferred further type of inlet is designed and arranged to allow an organic compound to enter the volume segment in the form of a liquid. An example of a further type of inlet is a nozzle, e.g. a nozzle designed and arranged to spray a liquid.

[0404] Molar mass

[0405] In one aspect of the present invention, preferably, the first polyester has a number average molar mass in the range of 12000 Da to 18500 Da, more preferably in the range of 12700 Da to 17700 Da, and further preferably in the range of 13200 Da to 17200 Da before contacting with the first amount of the first organic compound.

[0406] In one aspect of the present invention, preferably, the exit volume segment V 1 The number average molar mass of the first polyester is in the range of 10100 Da to 21800 Da, more preferably in the range of 10900 Da to 21100 Da, further preferably in the range of 11400 Da to 20600 Da.

[0407] In one aspect of the present invention, preferably, there is a volume segment V 2 The number average molar mass of the first polyester is in the range of 500 Da to 2500 Da, more preferably in the range of 700 Da to 2000 Da, further preferably in the range of 1000 Da to 1500 Da.

[0408] In one aspect of the present invention, preferably, the number average molar mass of the first intermediate product is in the range of 200 Da to 600 Da, more preferably in the range of 300 Da to 500 Da, further preferably in the range of 350 Da to 400 Da.

[0409] In one aspect of the present invention, preferably, the exit volume segment V 6 The number average molar mass of another intermediate product is in the range of 200 Da to 600 Da, more preferably in the range of 3000 Da to 6500 Da, and further preferably in the range of 3700 Da to 5500 Da.

[0410] In one aspect of the present invention, preferably, the exit volume segment V 7 The number average molar mass of another intermediate product is in the range of 6500 Da to 10500 Da, more preferably in the range of 7500 Da to 10000 Da, and further preferably in the range of 8000 Da to 9500 Da.

[0411] In one aspect of the present invention, it is preferred that the first polyester is in the form of a plurality of first type fragments and a plurality of another type fragments. In this aspect, it is preferred that at least one or all of the following apply:

[0412] A.) before contacting with the first amount of the first organic compound, the weight average molar mass of the plurality of first type fragments is in the range of 55000 Da to 72000 Da, more preferably in the range of 60000 Da to 68000 Da, and further preferably in the range of 62000 Da to 66000 Da;

[0413] B.) before contacting with the first amount of the first organic compound, the weight average molar mass of the plurality of another type of fragments is in the range of 50,000 Da to 70,000 Da, more preferably in the range of 55,000 Da to 64,000 Da, and further preferably in the range of 57,000 Da to 62,000 Da;

[0414] C.) Leave volume segment V 1 The mass average molar mass of the plurality of first type fragments is in the range of 47000 Da to 58000 Da, more preferably in the range of 49000 Da to 56500 Da, and further preferably in the range of 51000 Da to 54500 Da;

[0415] D.) Leave volume segment V 1 The mass average molar mass of the plurality of another type of fragments is in the range of 44000 Da to 77000 Da, more preferably in the range of 48000 Da to 73000 Da, and further preferably in the range of 50000 Da to 71000 Da;

[0416] E.) Leave volume segment V 2 The mass average molar mass of the plurality of first type fragments is in the range of 3700Da to 6000Da, more preferably in the range of 4100Da to 5300Da; F.) leaving the volume segment V 2 The mass average molar mass of the plurality of another type of fragments is in the range of 2300 Da to 7500 Da, more preferably in the range of 3200 Da to 7200 Da.

[0417] In the above aspects, all possible combinations of features A. to F. are preferred. These combinations are, for example, a; b; c; d; e; f; a+b; a+c; a+d; a+e; a+f; b+c; b+d; b+e; b+f; c+d; c+e; c+f; d+e; d+f; e+f; a+b+c; a+b+d; a+b+e; a+b+f; a+c+d; a+c+e; a+c+f; a+d+e; a+d+f; a+e+f; b+c+d; b+c+e; b+c+f; b+d+e; b+d+f; b+e+f; c+d+e; c+d+f; c+e+f; d+ e+f;a+b+c+d;a+b+c+e;a+b+c+f;a+b+d+e;a+b+d+f;a+b+e+f;a+c+d+e;a+c+d+f;a+c+e+f;a+d+e+f;b+c+d+e;b+c+d+ f; b+c+e+f; b+d+e+f; c+d+e+f; a+b+c+d+e; a+b+c+d+f; a+b+c+e+f; a+b+d+e+f; a+c+d+e+f; b+c+d+e+f; a+b+c+d+e+f.

[0418] Direction relative to gravity

[0419] If a direction (e.g., a first direction) is "at least partially opposite to the direction of gravity," it is best understood that if the direction is decomposed into three perpendicular components, the orientation of the component parallel to the direction of gravity is such that the component is opposite to the direction of gravity. If a direction (e.g., a first direction) is "at least partially along the direction of gravity," it is best understood that if the direction is decomposed into three perpendicular components, the orientation of the component parallel to the direction of gravity is such that the component is along the direction of gravity, i.e., points in the same direction as gravity.

[0420] Stirring in the volume segment

[0421] The stirring in the volume segment is preferably performed using a mechanical device suitable for stirring, a non-mechanical device suitable for stirring, or a combination thereof. Examples of suitable mechanical devices include stirrers, such as vertical blade stirrers, turbines, impellers, and propellers. Examples of suitable non-mechanical devices include injecting at least one fluid (e.g., in the form of a gas, a liquid, or a combination thereof) into the volume segment (preferably under pressure) and ultrasound. For example, another organic compound is injected as a liquid into the volume segment V through a nozzle. 3 .

[0422] Organic compounds

[0423] Preferred "organic compounds" (e.g., the first organic compound, the other organic compound) are compounds suitable for reducing the molar mass (e.g., weight average molar mass, number average molar mass) of the first polyester, preferably by solvolysis. For example, if the first polyester is PET, the weight average molar mass of the first polyester can be reduced by a solvolysis process using (mono)ethylene glycol, alcohol or methanol. Preferred "organic compounds" (e.g., the first organic compound, the other organic compound) are selected from (mono)ethylene glycol, diethylene glycol, triethylene glycol, dipropylene glycol, polypropylene glycol, alcohol, methanol and a combination of at least two thereof, wherein (mono)ethylene glycol is more preferred, and monoethylene glycol is particularly preferred.

[0424] "Free" organic compound is preferably understood to mean an organic compound that is not chemically bound to, for example, the first polyester, the first intermediate product, the further intermediate product, by a covalent bond. "Free" organic compound is in contrast to "bound" organic compound, which is chemically bound to, for example, the first polyester, the first intermediate product, the further intermediate product, by a covalent bond. For example, during the solvolysis of PET using MEG, some MEG is chemically bound to PET oligomers. This bound MEG is not free MEG.

[0425] In one aspect of the present invention, it is preferred that the first organic compound and the further organic compound are the same organic compound. For example, it is preferred that the first organic compound and the further organic compound are both (mono)ethylene glycol.

[0426] Initial mixture

[0427] In one aspect of the invention, it is preferred that the first initial mixture comprises a first polyester and a first organic compound. In one aspect of the invention, it is preferred that a further initial mixture comprises a first polyester and another organic compound. In this aspect, it is further preferred that a further initial mixture also comprises a first organic compound. In one aspect of the invention, it is preferred that a further initial mixture comprises a first polyester and a first organic compound.

[0428] First granular material

[0429] First particulate materials suitable for use in the present invention are commercially available from, for example, Merck KGaA (Germany) and Donau Carbon GmbH (Germany).

[0430] The "mode" of a first particle material is a well-known measure of a statistical distribution. The mode of a first particle material will be referred to below in conjunction with Figure 8 Further description.

[0431] Further aspects and definitions

[0432] In one aspect of the invention, it is preferred that the feedstock contains less than 5 wt-%, more preferably less than 1 wt-%, and further preferably less than 0.1 wt-% of colorant. For example, the feedstock contains PET flakes obtained by crushing colorless bottles. In one aspect of the invention, it is preferred that the feedstock contains less than 5 wt-%, more preferably less than 1 wt-%, and further preferably less than 0.1 wt-% of colored fragments.

[0433] In one aspect of the present invention, it is preferred that the process of the present invention is operated continuously, semi-continuously or batchwise. Examples of these processes are "a process for producing a first intermediate product" and "a process for producing another intermediate product".

[0434] A preferred example of the "method for producing a first intermediate product" is a method in which the first intermediate product is produced by recycling the first polyester. A preferred example of the "method for producing another intermediate product" is a method in which the another intermediate product is produced by recycling the first polyester.

[0435] The process step of "contacting" the component (e.g., the first polyester) with the organic compound preferably includes at least one or all of the following: a process step of mixing the organic compound with the component (e.g., mixing the organic compound and the component in a volume section using a stirring device); a process step of keeping the organic compound and the component in contact with each other (e.g., the component and the organic compound form a mixture, the component is suspended in the organic compound, or the component is at least partially dissolved in the organic compound); a process step of passing the organic compound through the component (e.g., passing steam through a porous component, or the component is in the form of a plurality of fragments and passing steam between the fragments); or a combination of at least two or more thereof.

[0436] The process step of "reducing the weight-average molar mass of the first polyester" preferably includes at least one or all of the following: at least partially depolymerizing the first polyester (for example, by solvent decomposition); heating the first polyester; photodegrading the first polyester; shearing the first polyester; or a combination of at least two or more thereof.

[0437] In one aspect of the invention, it is particularly preferred to reduce the weight average molar mass of the first polyester by solvolysis. Examples of solvolysis include hydrolysis, glycolysis, alcoholysis and aminolysis. For example, if the first polyester is PET, water can be used to depolymerize PET into terephthalic acid and ethylene glycol (hydrolysis). For example, if the first polyester is PET, methanol can be used to depolymerize PET into dimethyl terephthalate and ethylene glycol (methanolysis). For example, if the first polyester is PET, (mono) ethylene glycol can be used to depolymerize PET into BHET and other PET glycolysis products (glycolysis). In this regard, glycolysis is particularly preferred.

[0438] The process step of "increasing the weight average molar mass of the intermediate product" (e.g., the first intermediate product or another intermediate product) preferably comprises at least one or all of the following: at least partially polymerizing the intermediate product; crosslinking the intermediate product; transesterification of the intermediate product; or a combination of at least two or more thereof. In one aspect of the present invention, it is particularly preferred to increase the weight average molar mass of the intermediate product by at least partially polymerizing the intermediate product. In this regard, polycondensation is preferred.

[0439] "Intrinsic viscosity" is preferably understood to mean the average intrinsic viscosity.

[0440] The "first direction" is preferably understood as a direction at least partially opposite to the direction of gravity. The "another direction" is preferably understood as a direction at least partially along the direction of gravity.

[0441] "Ambient pressure" in a volume segment is preferably understood to mean the pressure in the head space of the volume segment. "Overpressure" in a volume segment is preferably understood to mean the pressure difference relative to the ambient pressure, for example the atmospheric pressure at the location of the volume segment.

[0442] A "repeat unit" is preferably understood as a part of a polymer, which is repeated to produce a polymer chain. For example, a polymer is formed by linking "repeat units" together. A "dimer" is preferably understood as a chain consisting of two "repeat units". A "trimer" is preferably understood as a chain consisting of three "repeat units". In one aspect of the invention, a preferred repeat unit has the form

[0443]

[0444] The "first intermediate product" is preferably understood to be a product obtained by reducing the weight-average molar mass of the first polyester. Examples of the "first intermediate product" are oligomers of the first polyester, monomers of the first polyester, or combinations thereof. In one aspect of the present invention, preferably the "first intermediate product" includes at least one or all of the following: monomers of the first polyester, oligomers of the first polyester, or both.

[0445] "Oligomer" is preferably understood to mean a chain of repeating units, wherein the number of repeating units does not exceed 50.

[0446] Test Method

[0447] The following test methods are used within the scope of the present invention. Unless otherwise stated, the measurements are carried out at an ambient temperature of 25° C., an ambient pressure of 100 kPa (0.986 atm) and a relative air humidity of 65%. Unless otherwise stated, the margin of error of the measurement method is ±5%.

[0448] In the following test methods, when reference is made to PET, it is understood that the particular test method is applicable to any polyester without adapting the test method.

[0449] Bulk density of raw materials

[0450] When the raw material contains multiple fragments, the bulk density of the raw material p BULK，FEED Calculated according to standard ASTM D1895-17 B. The bulk density of the feedstock is measured before the feedstock is contacted with the first amount of the first organic compound. The method is described using a PET flake feedstock as an example.

[0451] Volume segment V 1 and V 2 The bulk density of the first polyester

[0452] If the first polyester is in the form of multiple fragments, the volume segment V 1 Middle and volume segment V 2 The bulk density of the first polyester in the first region is determined as follows. The method is described using a PET sheet as an example.

[0453] a. Assume that you leave the volume segment V 1 Bulk density and volume segment V of PET flakes 1 The packing density of the flakes in BULK,V1 Same. BULK,V1 The value of the volume segment V 1 Take 10 samples of PET flakes at the outlet and calculate p using the same procedure as for the bulk density of the raw material. BULK,V1 to be sure.

[0454] b. Due to the volume segment V 2 The pressure in the first region, the PET sheet will be compressed, resulting in a bulk density p in the first region. BULK,V2,Z1 Increase. The bulk density is calculated as follows:

[0455] p BULK,V2,Z1 =C FACTOR ×p BULK,V1 ,

[0456] Among them, C FACTOR is the compression factor.

[0457] c. Volume segment V 2 The bulk density of the PET flakes in another region p BULK,V2,Z2 By in volume segment V 2 Take 10 samples of PET flakes at the outlet and calculate p using the same procedure as for the bulk density of the raw material. BULK,V2,Z2 to be sure.

[0458] Compression coefficient C FACTOR Determine as follows:

[0459] a. Volume segment V 2 Head pressure at the bottom p HEAD,V2 The calculation is as follows:

[0460] p HEAD,V2 =[H MEG,V2 ×(p PET -p MEG )+(H REACTOR,V2 –H MEG,V2 )×p BULK,V2,Z2 ]×a GRAV ,

[0461] Among them, H MEG,V2 is the volume segment V 2 The height of the first organic compound (eg MEG) in the volume segment V 2 Measured from the bottom of the REACTOR,V2 is the volume segment V 2 The height, p PET is the density of PET (SI unit) (1380kg / m 3 ), p MEG is the density of MEG (SI unit) (1110kg / m 3 ), p BULK,V2,Z2 is the SI unit system, a GRAV is the acceleration due to gravity (9.81 m / s). HEAD,V2 The value is in N / m 2 As unit.

[0462] b. 500ml PET sheet (V PET,C-TEST,INITIAL ) was placed in a cylindrical container with a diameter of 50 mm. The PET flake samples were taken from the raw material without mixing with any organic compounds.

[0463] c. Use a cylindrical rod with a diameter of 12 mm to apply pressure to the PET sheet. The pressure applied by the rod is p ROD,TEST The calculation is as follows:

[0464] p ROD,TEST =p HEAD,V2 ×(A CONTAINER / A ROD ),

[0465] Among them, A CONTAINER is the diameter of the cylindrical container (1964mm 2 ), A ROD is the diameter of the rod (13mm 2 ).

[0466] d. The pressure p ROD,TEST The rod was then removed and the volume (V PET,C-TEST,AFTER ).

[0467] e. The above experiment was performed 10 times. Compression factor C FACTOR The calculation is as follows:

[0468] C FACTOR =V PET,C-TEST,INITIAL,AVG –V PET,C-TEST,AFTER,AVG ,

[0469] Among them, V PET,C-TEST,INITIAL,AVG (500 ml) is the average volume of the PET flake in 10 repeated experiments, measured before using the rod, and V PET,C-TEST,AFTER,AVG is the average volume of the PET flake in 10 replicates, measured after removing the rod.

[0470] Mass ratio of the first polyester to the organic compound

[0471] The mass ratio of the first polyester to the organic compound is determined as follows: This method is described by taking PET flakes as the first polyester, MEG as the first organic compound and another organic compound as an example.

[0472] Volume segment V 1 The mass ratio of PET to MEG in the solution was determined as follows. Fig. 9 By first measuring the first initial mixture M SAMPLE,TOTAL,V1 The mass ratio is determined by the mass of the collective sample. Then MEG is poured out from the collective sample, and the remaining PET flakes are placed in an oven at 250°C for 1 hour. After 1 hour, the PET flakes are taken out and weighed to obtain the PET flake M SAMPLE,PET,V1 Therefore, the collective sample M SAMPLE,MEG,V1 The MEG mass in

[0473] M SAMPLE,MEG,V1 =M SAMPLE,TOTAL,V1 -M SAMPLE,PET,V1 Given.

[0474] The volume segment V is then calculated as follows 1 Mass ratio of PET to MEG:

[0475] R PET / MEG,SAMPLE,V1 =M SAMPLE,PET,V1 / M SAMPLE,MEG,V1 .

[0476] I. Volume segment V 2 The mass ratio of PET to MEG in the first region R PET / MEG,V2,Z1 The calculation method is as follows:

[0477] a. Filling ratio V of the sheet F-RATIO,PET,V2 The calculation formula is as follows:

[0478] V F-RATIO,PET,V2,Z1 =pBULK,V2,Z1 / p PET ,

[0479] where p BULK,V2,Z1 is the volume segment V 2 The packing density of the flakes in the first region is calculated as described above, p PET is the density of PET (1380kg / m 3 ).

[0480] b. Filling ratio V of MEG F-RATIO,MEG,V2,Z1 The calculation method is as follows:

[0481] V F-RATIO,MEG,V2,Z1 =1–V F-RATIO,PET,V2,Z1 .

[0482] c. Then calculate the filling ratio R F-RATIOS,V2,Z1 The ratio is as follows

[0483] R F-RATIOS,V2,Z1 =V F-RATIO,PET,V2,Z1 / V F-RATIO,MEG,V2,Z1 .

[0484] d. Calculate the volume segment V using the following formula 2 The mass ratio of PET to MEG in the first region R PET / MEG,V2,Z1 :

[0485] R PET / MEG,V2,Z1 =R F-RATIOS,V2,Z1 ×(p PET / p MEG ),

[0486] Among them, p MEG is the density of MEG (1113kg / m 3 ).

[0487] II. Volume Segment V 2 The mass ratio R of PET to MEG in another region PET / MEG,V2,Z2 is obtained by 2 10 PET flake samples were taken out for calculation. Each sample weighed 100g. MEG was adhered to the surface of the PET flakes in the sample. Sample R SAMPLE,PET / MEG The mass ratio is calculated as follows:

[0488] a. The mass of the sample is expressed as M SAMPLE,V2,Z2 This mass is the PET sheet M SAMPLE,PET,V2,Z2 The quality and adhesion to PET film M SAMPLE,MEG,V2,Z2 The sum of the masses of the MEGs on the .

[0489] b. Place the sample on a tray, then place the tray in an oven and bake at 250°C for at least 1 hour. Take out the sample every 20 minutes, weigh it with an analytical balance, and return it to the oven. Repeat this process until the mass measurement value changes by no more than 0.2% for three consecutive times. The average of the last three measurements is M. SAMPLE,PET,V2,Z2 The quality of MEG is determined by

[0490] M SAMPLE,MEG,V2,Z2 =M SAMPLE,V2,Z2 –M SAMPLE,PET,V2,Z2 Given.

[0491] c. Therefore, the mass ratio of PET to MEG in the sample is given by

[0492] R SAMPLE,PET / MEG,V2,Z2 =M SAMPLE,PET,V2,Z2 / M SAMPLE,MEG,V2,Z2 Given.

[0493] d. Mass ratio R PET / MEG,V2,Z2 Calculated as follows: R calculated for 10 samples SAMPLE,PET / MEG,V2,Z2 The average of the values.

[0494] Characteristics changes

[0495] The percent change in a physical property (e.g., intrinsic viscosity of the first polyester) is determined as follows:

[0496] χ=100×|P 2 –P 1 | / P 1 ,

[0497] Where χ is the percentage change, P 1 is the average value of the characteristic measured at the first position, P 2 is the average of the property measured at the second location. A change can be an increase or decrease. The physical property at the first location should be measured 10 times with 5 minutes between each measurement. 1 is the average of 10 measurements taken at the first location. Similarly, 10 measurements of the physical property at the second location should be taken, with 5 minutes between each measurement. 2 is the average of 10 measurements made at the second position.

[0498] To determine the volume segment V 1 The percentage change of the intrinsic viscosity and molar mass (e.g., weight average molar mass, number average molar mass) of the first polyester in the volume segment V 1 P is measured at the entrance 1 , and in the first polyester leaving volume segment V 1 P is measured at the outlet 2 .

[0499] To determine the volume segment V 2 The percentage change of the intrinsic viscosity and molar mass (e.g., weight average molar mass, number average molar mass) of the first polyester in the volume segment V 2 P is measured at the entrance 1 , while in the first polyester leaving volume segment V 2 P is measured at the outlet 2 .

[0500] Changes in physical properties should be calculated using values ​​expressed in the units used for that property in the description, for example, changes in temperature should be calculated using values ​​expressed in °C.

[0501] Relative proportions of characteristics

[0502] Unless otherwise stated, the relative proportion β of a physical property (e.g., the number of particles per unit area of ​​at least one impurity) is determined as follows:

[0503] β=P 1 / P 2 ,

[0504] Among them, P 1 is the average value of the characteristic measured at the first position, and P 2 is the average of the properties measured at the second location. 1 Outside the value, P 1 and P 2 The value of is calculated as described in the method for determining the "Characteristic Change".

[0505] In order to determine the number of particles per unit area and volume segment V of at least one impurity in the raw material 1 The relative proportion of the number of particles per unit area of ​​at least one impurity at the outlet is the same as that of the raw material when it is transported to the volume section V. 1 Previously, P was measured in the raw material 1 , while in the first polyester leaving volume segment V 1 P is measured at the outlet 2 For the raw material, P was tested at 10 different positions in the raw material. 1 10 measurements were performed at locations evenly distributed throughout the volume of the material.

[0506] To determine the volume segment V 2 The relative ratio of the temperature of the first region to the temperature of the other region is in the first polyester entering the volume segment V 2 P is measured at the entrance 1 , while in the first polyester leaving volume segment V 2 P is measured at the outlet 2 .

[0507] To determine the volume segment V 2 The relative ratio of the number of particles per unit area of ​​at least one impurity in the first region to the number of particles per unit area of ​​at least one impurity in another region is determined when the first polyester enters the volume segment V 2 P is measured at the entrance 1 , and in the first polyester leaving volume segment V 2 P is measured at the outlet 2 .

[0508] Volume segment V 2 The relative ratio β of the mass ratio of the first polyester to the first organic compound in the first region to the mass ratio of the first polyester to the first organic compound in another region PET / MEG,V2,Z1 / Z2 The calculation is as follows:

[0509] β PET / MEG,V2,Z1 / Z2 =R PET / MEG,V2,Z1 / R PET / MEG,V2,Z2 ,

[0510] Among them, R PET / MEG,V2,Z1 and R PET / MEG,V2,Z2 Calculated as above.

[0511] Relative proportions should be calculated using values ​​expressed in the units used for the characteristic in the description, for example, relative proportions of temperature should be calculated using values ​​expressed in °C.

[0512] Density of the first polyester

[0513] The density of the first polyester is well known in the art and can be found, for example, in CA Harper, Modern Plastics Handbook: Handbook, McGraw-Hill Professional, New York, 2000 and https: / / en.wikipedia.org / wiki / Polyethylene_terephthalate.

[0514] Composition of raw materials

[0515] Raw Material C PVC The PVC content in the raw material is determined by selecting 10 samples containing PET flakes from the raw material. The samples should be evenly distributed in the volume of the raw material. Sample C SAMPLE,PVC The PVC content of the product is determined as follows:

[0516] i.) Weigh out 250g of sample. The sample weighed is of mass W A Place sample A on the tray.

[0517] ii.) Place the tray in an oven at 200°C for 2 hours.

[0518] iii.) Remove the tray from the oven and allow Sample A to cool to room temperature (25°C or lower).

[0519] iv.) Remove any burnt or blackened parts or pieces from Sample A - the removed parts or pieces form Sample B.

[0520] v.) Weigh sample B. The mass of sample B is W B .

[0521] vi.) PVC content of the sample C SAMPLE,PVC The calculation is as follows:

[0522] C SAMPLE,PVC =W B / W A ×10 6 ,

[0523] Among them, C SAMPLE,PVC It is the PVC content in ppm.

[0524] Weigh Sample A and Sample B using an analytical balance. Raw Material C PVC The PVC content in the sample is the C SAMPLE,PVC The average of the values.

[0525] Determine the raw material C by selecting 10 samples containing PET flakes from the raw material F The sample locations should be evenly distributed in the volume of the raw material. Sample C SAMPLE,C The floatable impurities content is determined as follows:

[0526] i.) Pour 500 ml of distilled water into a plastic beaker.

[0527] ii.) Weigh out 250g of sample. The raw material weighed is of mass W C Sample C.

[0528] iii.) Transfer Sample C to a plastic beaker and stir the distilled water and Sample C for 10 minutes.

[0529] iv.) Allow the mixture of distilled water and Sample C to sit for 10 minutes.

[0530] v.) Remove any floating material from the surface of the distilled water and place the removed material in a petri dish. Measure the mass of the petri dish with the material removed, W D .

[0531] vi.) Place the dish in an oven and bake at 110°C for 1 hour.

[0532] vii.) Take the Petri dish out of the oven and place it in a desiccator to cool. Measure the mass of the Petri dish after cooling. E .

[0533] viii.) Floatability content C of the sample SAMPLE,F The calculation is as follows:

[0534] C SAMPLE,F =(W E –W D ) / W C ×10 6 .

[0535] Weigh sample C and the petri dish using an analytical balance. F The floatable impurities content in the sample is determined by the C SAMPLE,F The average of the values.

[0536] Determine the raw material C by selecting 10 samples containing PET flakes from the raw material S The solid impurity content in the raw material. The sample selection location should be evenly distributed in the volume of the raw material. Sample C SAMPLE,S The solid impurity content of the product is determined as follows:

[0537] i.) Weigh out 250g of sample. The sample weighed is specimen F, and its mass is W. F .

[0538] ii.) Spread specimen F on the surface of a stainless steel tray and place it in the tray.

[0539] iii.) The following types of impurities were manually screened out from specimen F: labels, adhesive labels, caps and closures, colored debris (e.g., blue, green, red, yellow, and other colors), metals, stones, rubber, any other unidentified materials.

[0540] iv.) Provide a G of the petri dish.

[0541] v.) Put the impurities sorted out manually into a petri dish and weigh the petri dish. The mass of the petri dish containing impurities is W H .

[0542] ix.) Solid content C SAMPLE,S The calculation is as follows:

[0543] C SAMPLE,S =(W H –W G ) / W F ×10 6 .

[0544] Weigh sample F and the petri dish using an analytical balance. Raw material C S The solid impurity content in the sample is C SAMPLE,S The average of the values.

[0545] wt-% of PET in raw material (PET wt-％ ) is determined as follows:

[0546] PET wt-％ =100% – (C PVC –C F –C S ) / 10 6 .

[0547] Percentage associated with multiple fragments

[0548] In many preferred embodiments and aspects of the present invention, the feedstock includes a plurality of fragments. Many of these aspects and embodiments have the following features: "at least X wt-% of the fragments" or "X wt-% or less of the fragments" have certain geometric properties, such as a thickness greater than 1 mm. Geometric properties include the thickness, width and length of the fragments. Here X is a variable, which is calculated as follows

[0549] X=M ％ / M FRAGMENT,TOTAL ,

[0550] Among them, M ％ is the mass of the fragment with the specified properties, M FRAGMENT,TOTAL is the mass of a selected sample among multiple fragments.

[0551] To determine X, a sample of 10 pieces is selected from evenly distributed locations in the stock, each piece weighing 250 g. Thus M FRAGMENT,TOTAL The weight of the fragment is 2.5 kg. The geometrical properties (e.g., thickness) of each fragment are measured at 5 locations evenly distributed on the fragment. The geometrical properties are measured using a caliper. The maximum value of the measurement is defined as the value of the geometrical property of the fragment. For example, if the thickness of the fragments is measured to be 1.3 mm, 1.2 mm, 1.7 mm, 1.4 mm, and 1.2 mm, the thickness of the fragment is 1.7 mm.

[0552] Particle size of the first particulate material

[0553] The median particle size of the first particulate material is measured using the following particle analyzer and apparatus: Helos / BR+Rodos+Vibri / L. The particle analyzer and apparatus can be purchased from Sympatec GmbH (Germany).

[0554] temperature

[0555] The temperature was measured using a resistance thermometer commercially available from WIKA Alexander Wiegand SE & Co. KG (Germany).

[0556] The volume segment V is measured at 10 different equidistant positions in the first region. 2 The temperature of the first region in the volume segment V is determined from the average of 10 measurements. The temperature of the first region is determined from 10 different equidistant positions in another region. 2 The temperature of another area in the sample is determined by taking the average of 10 measurements.

[0557] Molar mass

[0558] Number average molar mass M n Defined as

[0559] Weight average molar mass M w Defined as

[0560] Among them, in the above two expressions, M i is the mass of polymer i with chain length L, N i is the number of polymers with chain length L.

[0561] The molar mass (e.g., weight average molar mass, number average molar mass) of the first polyester is measured using gel permeation chromatography (GPC). This method is suitable for determining number average molar mass and weight average molar mass. The method is performed as follows:

[0562] i.) A sample of the first polyester was mixed with an eluent to produce a solution having a first polyester concentration of 3.0 mg / ml. The eluent was 1,1,1,3,3,3-hexafluoro-2-propanol (HFIP) + 0.05 M potassium trifluoroacetate (KTFAc).

[0563] ii.) The solution was maintained at a temperature of 23°C for 12 hours.

[0564] iii.) Filter the solution using a polytetrafluoroethylene syringe filter with a nominal porosity of 1.0 μm.

[0565] iv.) 50 μL of the filtrate was injected into the detector using a PSS SECurity 1260 autosampler. The flow rate was 1.0 mL / min. The detector used was a PSS SECurity 1260RI detector. To evaluate the measurement results, the software PSS-WinGPC UniChrom Version 8.33 was used. The autosampler, detector and software can be purchased from PSS Polymer Standards Service GmbH (Germany). The column temperature was 25°C.

[0566] In order to evaluate the measurement results, the measurement results must be calibrated. The calibration method is as follows:

[0567] a.) A routine calibration is performed using a narrow distribution standard made of polymethyl methacrylate (PMMA), which reproduces the separation behavior of a gel permeation chromatography (GPC) column. The PMMA is measured using the same eluents and parameter values ​​as described in points i.) to iv.) above.

[0568] b.) Eight broad distribution standards of a first polyester (eg PET) are then measured.

[0569] c.) M according to the known first polyester standard w The value is used to determine the calibration of the first polyester standard using PMMA calibration. This calibration is performed using mathematical calculations. This provides the absolute molar mass for the first polyester sample. Based on the first polyester calibration curve, the molar mass distribution and molar mass mean value of the first polyester sample are calculated by the strip method. In addition, the calculation is performed using a computer.

[0570] The calibration curve used for the above calibration is shown in FIG6 . Fig. 6A The calibration curve for PMMA is shown, which corresponds to the following data:

[0571]

[0572]

[0573] Figure 6B A first polyester standard is shown being measured, wherein the first polyester is PET. Figure 6C The calibration curve used to determine the molar mass of the first polyester is shown. Figure 6C The curve in corresponds to the following data:

[0574] Vp / mL Mp / Da Standard No. Increase deviation% 13.71 931380 Calibration point 1 -0.33 -2.20 14.31 564864 Calibration point 2 -0.32 3.47 15.15 310414 Calibration point 3 -0.30 3.44 16.05 181563 Calibration point 4 -0.29 -4.27 17.33 77600 Calibration point 5 -0.29 -5.25 18.42 35482 Calibration point 6 -0.30 -1.03 19.45 15649 Calibration point 7 -0.31 9.11 20.41 7942 Calibration point 8 -0.33 5.20 21.35 4063 Calibration point 9 -0.36 -2.66 22.35 1872 Calibration point 10 -0.39 -10.53 23.35 609 Calibration point 11 -0.43 6.48

[0575] for Fig. 6A and 6C The following calibration parameters were used for the fit:

[0576] <![CDATA[ Fig. 6A ]]> <![CDATA[ Figure 6C ]]> parameter value value substance PPMA PET Eluent HFIP+0.05KTFAc HFIP+0.05KTFAc Fitting Polynomial 3 Polynomial 3 R 1.000 1.000 Mark-Houwink K - 1.5834 mL / g Mark-Houwink alpha - -0,02914

[0577] for Figures 6A to 6C The measurements shown in , used the following columns: PSSPFG, 7 μm, precolumn, 8 mm x 50 mm; and two PSSPFG, 7 μm, linear M, 8 mm x 300 mm. These columns can be purchased from PSSPolymer Standards Service GmbH (Germany).

[0578] The above method is also used to measure the first intermediate product (e.g., PET oligomer), another intermediate product (e.g.,

[0579] Recycled PET) and the molar mass of the product (e.g., weight average molar mass, number average molar mass).

[0580] Composition of the first intermediate mixture

[0581] The amount of free MEG in the first intermediate mixture (comprising, for example, PET oligomers and free MEG) is determined as follows:

[0582] i.) Prepare periodic acid solution: Add 23 g of periodic acid into a 1000 ml volumetric flask. Dissolve the periodic acid in distilled water. The volumetric flask must be filled with distilled water so that 1000 ml of solution is obtained.

[0583] ii.) Preparation of 10% sulfuric acid: Add 25 ml of distilled water to a 100 ml volumetric flask. Add 10 g of 98% sulfuric acid to the volumetric flask. Cool the solution to 23°C. Then, fill the volumetric flask with distilled water to obtain 100 ml of solution.

[0584] iii.) Prepare 10% potassium iodide: Add 10 g of potassium iodide into a beaker. Add 90 ml of distilled water into the beaker and shake vigorously.

[0585] iv.) Standardization of 0.1N sodium arsenite solution: Add 125±0.1 mg potassium iodate to a 300 ml conical flask. Dissolve potassium iodate in 100 ml distilled water at 50°C. Add 4 g solid potassium iodide and 4 ml 10% sulfuric acid (prepared in step ii) to the flask. Place the solution in a sealed flask and protect from light for 5 minutes. Then add 12 g solid sodium bicarbonate and dilute with distilled water. Titrate the iodine formed with the arsenite solution, using starch as an indicator. Calculate the F factor:

[0586] F-factor = KIO 3 Initial mass (mg) / 3.567x consumed arsenic solution (ml).

[0587] v.) Preparation of starch indicator solution: Add 1 g starch powder into a 100 ml beaker, add 10 ml distilled water, and then add 100 ml boiling distilled water.

[0588] vi.) Take a sample of the first intermediate mixture, grind the sample finely, and determine the initial mass of the sample based on the expected ethylene glycol content.

[0589] Ethylene glycol content (%) Initial sample mass (mg) 1 9300 5 1860 10 930 15 620 20 465 30 311 40 233 50 186

[0590] vii.) Accurately weigh the sample and transfer it to a 300 ml conical flask and prepare a slurry with 100 ml of distilled water. Acidify the slurry with 3 drops of 10% sulfuric acid (prepared in step ii.) and then add 25 ml of periodic acid solution (prepared in step i.) using a burette. Loosely stopper the flask and let the flask stand at 23°C for 30 minutes. Shake occasionally. Then, add 10 g of solid sodium bicarbonate and 10% potassium iodide (prepared in step iii.) to the flask. Shake vigorously and immediately titrate with 0.1N sodium arsenite solution (prepared in step iv.) until it turns light yellow. Then, add 1 ml of starch indicator solution (prepared in step v.) and continue titrating until the blue color disappears completely. The endpoint of the titration is marked by the disappearance of the blue color. The color disappearance must last for 3 minutes.

[0591] viii.) A blank was determined as described in previous step vii.), i.e. 25 ml of periodic acid solution (prepared in step i.), i.e. except for the sample addition, all added chemicals were added as described in previous step vii.).

[0592] ix.) The percentage of free MEG is determined as follows:

[0593] %MEG content=[(BW–V)x F x 0.31] / E

[0594] Wherein, BW is the 0.1 N sodium arsenite solution consumed in the blank experiment (ml), V is the 0.1 N sodium arsenite solution consumed in the sample experiment (ml), F is the factor of the 0.1 N sodium arsenite solution, and E is the initial mass of the sample (in g).

[0595] Mass ratio of the first particulate material to the first intermediate mixture

[0596] The mass ratio R of the first particulate material to the first intermediate mixture PM / FIM The calculation formula is

[0597] R PM / FIM =M PM / M FIM ,

[0598] Among them, M PM is the mass of the first particle material, MFIM is the mass of the first intermediate mixture.

[0599] Intrinsic viscosity

[0600] The intrinsic viscosity IV of the first polyester is measured according to standard ASTM D4603:2018, but with the following changes: the flow time of the solution in the capillary viscometer is determined at 25° C. instead of 30° C. (as given in the standard).

[0601] The above method is also used to measure the intrinsic viscosity of the first intermediate product, the further intermediate product and the product.

[0602] Unless otherwise stated, the volume segment V 1 The intrinsic viscosity of the first polyester is in the first polyester leaving volume segment V 1 Unless otherwise stated, the volume segment V 2 The intrinsic viscosity of the first polyester in another region is in the first polyester exit volume segment V 2 The intrinsic viscosity of the first intermediate product is measured at the outlet of the first intermediate product. 3 Measured at the exit.

[0603] Number of particles per unit area of ​​at least one impurity

[0604] 10 pieces of the first polyester (e.g., 10 PET flakes) were selected. A scanning electron microscope (SEM) image was taken for each piece, with an image area of ​​100 mm x 100 mm (see Figure 7 ). Count the number of impurities in each image to obtain the number of particles per square centimeter in each image, N. i The subscript i here refers to the number of particles per square centimeter determined for the i-th fragment. In addition, the number of impurities is calculated on the surface of the fragment, not on the edge of the fragment. The number of particles per unit area P COUNT Determine as follows:

[0605]

[0606] Here, i = from 1 to 10. Therefore, the number of particles per unit area is determined by averaging the values ​​determined for the 10 images.

[0607] For the feedstock, a fragment for determining the number of particles per unit area of ​​the feedstock is selected prior to contacting the feedstock with a first amount of a first organic compound.

[0608] If the volume segment V 2 Having a first region and another region: when the debris enters the volume segment V 2The fragments for determining the number of particles per unit area in the first region are selected at the inlet of the first type (i.e., the inlet of the first type). Ten fragments are selected every 5 minutes until all ten fragments are selected.

[0609] In the fragment leaving volume segment V 2 At the exit of the selection is used to determine the number of particles per unit area in another region. And select the entry volume segment V 2 The fragments are similar, 10 fragments are selected every 5 minutes until all 10 fragments are selected.

[0610] pressure

[0611] The pressure was measured using a pressure gauge commercially available from WIKA Alexander Wiegand SE & Co. KG (Germany).

[0612] Dwell time

[0613] Residence time T RES Determined by the following formula:

[0614] T RES =V REACTOR / F PRODUCT VOLUME RATE ,

[0615] Among them, V REACTOR is the volume of the volume space, such as the reactor volume, F PRODUCT VOLUME RATE is the volume rate of the mixture (eg, the first intermediate mixture, another intermediate mixture) leaving the volume segment.

[0616] Color coordinates

[0617] The color coordinates of, for example, the first intermediate mixture and the product (eg, yarn) are measured using an UltraScan VIS spectrophotometer commercially available from Hunter Lab (USA).

[0618] The color coordinates of a sample, such as a first intermediate mixture (eg, comprising PET oligomer and MEG) or a product, are measured when the temperature of the sample is in the range of 22°C to 25°C.

[0619] Properties of the First Granular Material

[0620] The properties of the first particulate material, such as total pore surface area, total pore volume, average pore size, median pore size, mode pore size and total pore volume, were measured using mercury (Hg) porosimetry. The mercury porosimetry analysis was performed according to ISO 15901-1 (2005). A packing volume of 460.82 mm 3 / g blank was calibrated with Thermo Fisher Scientific PASCAL 140 (low pressure up to 4 bar) and PASCAL 440 (high pressure up to 4000 bar) and SOLID software version 3.0.2 (both provided by Thermo Fisher Scientific, Inc.). During the measurement, the pressure was continuously increased or decreased and was automatically controlled by the instrument operating in PASCAL mode, with the invasion speed set to 3 and the extrusion speed set to 7. The evaluation was performed using the "cylinder and plate" model and the density of Hg was corrected according to the actual temperature. The surface tension value of Hg is 0.48 N / m and the contact angle is 140°. The sample size of the first granular material ranged from 0.28 g to 0.29 g.

[0621] The invention will now be illustrated by means of non-limiting examples and exemplary embodiments.In the examples and figures, the following abbreviations are used: polyethylene terephthalate (PET), monoethylene glycol (MEG), bis(2-hydroxyethyl)terephthalate (BHET).

[0622] Attached photos

[0623] List of Figures

[0624] The accompanying drawings are used to illustrate the present invention and should not be considered as limiting the present invention. In addition, the accompanying drawings are not drawn to scale.

[0625] Figures 1A to 1C : Schematic diagram of an apparatus and a method according to the invention for producing a first intermediate product and a further polyester.

[0626] Figure 2A and Figure 2B : Schematic diagram of the angle between another direction and the horizontal plane.

[0627] Figure 3 : Flowchart showing the exemplary steps of the method according to the present invention for producing a first intermediate product.

[0628] Figure 4 : Flowchart showing the exemplary steps of the method according to the present invention for producing another intermediate product.

[0629] Figure 5A and Figure 5B: The orientation of the direction relative to gravity.

[0630] FIG. 6A to FIG. 6C : Calibration diagram used in methods for measuring molar mass.

[0631] Figure 7 : Scanning electron microscope image of PET flakes, showing impurities on the surface of the PET flakes.

[0632] Figure 8 : A graph showing the pore size distribution of a first particulate material.

[0633] Fig. 9 :Determine the volume segment V 1 Description of the test method for the mass ratio of the raw material, more preferably the first polyester, to the first organic compound. BRIEF DESCRIPTION OF THE DRAWINGS

[0634] In the description of the figures, reference is made to a raw material comprising PET flakes obtained by shredding PET plastic bottles. Additionally or alternatively, the raw material may comprise textile scraps and / or threads obtained by shredding textiles. Therefore, in the description of the figures, the term "PET flakes" should preferably be understood as a generic term for PET flakes obtained from shredding bottles and / or textile scraps and / or threads obtained from shredding textiles.

[0635] Figure 1 is a schematic diagram of an apparatus and method for producing a first intermediate product and another polyester (eg, PET) according to the present invention. More specifically, Figure 1 shows an apparatus and method for recycling used PET.

[0636] Figure 1A A cross section of a first part of the apparatus as viewed from the side is shown. A raw material 101 comprising PET flakes (a first polyester in the form of a plurality of fragments) is provided. Residual impurities such as glue, polyvinyl chloride (PVC) labels, food preservatives and flavorings adhere to the surface of the PET flakes. The raw material may also contain other impurities such as sand. The PET flakes are obtained by crushing PET plastic bottles for beverages. The raw material 101 is placed in a hopper 102. The raw material 101 is conveyed from the hopper 102 to a volume segment V 1 103. The conveying of the raw material 101 can be performed using, for example, a conveying screw, gravity, or a combination thereof. Volume segment V 1 103 may be, for example, a container, a tank, or a reactor (eg, a wash reactor).

[0637] Liquid MEG (a first amount of a first organic compound) is added to volume segment V via inlet 104. 1103, and mixed (contacted) with the PET flakes and impurities constituting the raw material 101 to obtain a first initial mixture 105 containing PET flakes and liquid MEG. The first initial mixture 105 is stirred (stirring device is not shown) to improve the mixing of the PET flakes and MEG. The stirring is performed mechanically. MEG can remove impurities on the surface of the PET flakes. This is partly because MEG is a strong solvent, and its ability to remove organic contaminants is enhanced at moderate temperatures. Stirring the first initial mixture 105 can also at least partially remove glue on the surface of the PET flakes by friction between the PET flakes.

[0638] At least a portion of the impurities (e.g., bottle cap fragments containing polyolefins) float on the surface 106 of the first initial mixture 105. These floating impurities can be removed by using, for example, skimming or filtering. The impurities are removed from the volume segment V through the outlet 123. 1 103. In contrast, the PET flakes in the first initial mixture 105 sink into volume segment V 1 Bottom 107 of 103.

[0639] The PET flakes and part of the MEG in the first initial mixture 105 are conveyed to a volume section V partially filled with MEG. 2 108. The conveying is performed using a conveying screw 109 (Archimedes screw) and a conveying screw 109 and a volume segment V 2 108 fluid is connected to the siphon (not shown). Other conveying devices not shown can also be used, such as additional conveying screws or pumps. In addition, the volume segment V 2 108 and volume segment V 1 103 fluid communication. Volume segment V 2 108 may be, for example, a container, a tank or a reactor, such as a pre-glycolysis reactor. The delivery screw 109 is arranged so that the delivery to the volume section V 2 The PET sheet 108 is transported in a direction 110 (another direction) at least partially opposite to the gravity direction 161 .

[0640] The PET flakes enter the volume segment V through the first type of inlet 115. 2 108. Figure 1A In the example, the first type of inlet 115 is a volume segment V 2 108. In addition, MEG (another amount of the first organic compound) is injected into the volume segment V 2 108. A first portion of MEG is injected in the form of steam through another type of inlet 116. The first portion may include MEG in the form of steam, but in the injection volume V 2Another type of inlet 116 is a nozzle which is adapted and arranged to inject MEG vapor under pressure into the volume segment V. 2 108. Although only one inlet 116 of another type is shown, there may be a plurality of inlets 116 of another type. Another portion of the MEG is injected in liquid form through yet another type of inlet 117. This yet another type of inlet 117 is a nozzle designed and arranged to spray liquid MEG into the volume segment V. 2 108. Volume segment V 2 The PET flakes in 108 are partially depolymerized by glycolysis (reducing the weight-average molar mass), thereby reducing the volume segment V 2 The weight average molar mass of the PET flakes in the volume segment V 2 Depolymerization into oligomers.

[0641] The screw conveyor (not shown) conveys the volume segment V in an upward conveying direction 118 2 PET flakes (and PET oligomers, if present) in 108 enter volume segment V through another type of inlet 116 2 The MEG vapor 108 also flows in an upward direction, ie in a conveying direction 118. In contrast, the MEG vapor enters the volume section V through a further type of inlet 117. 2 The liquid MEG at 108 flows in a downward direction, ie, opposite to the conveying direction 118 .

[0642] Volume segment V 2 The liquid MEG in 108 includes the volume segment V 1 103, liquid MEG injected through yet another type of inlet 117, and any condensed MEG vapor injected through yet another type of inlet 116. Liquid MEG does not completely fill volume segment V. 2 108. Thus, the surface (or level) of the liquid MEG forms a boundary 119 which separates the volume segment V 2 108 is divided into a first area 120 and another area 121. Another area 121 is located downstream of the first area 120.

[0643] The first region 120 is filled with another initial mixture, which includes a mixture of PET flakes (and PET oligomers, if present) immersed in MEG. Another region 121 includes the PET flakes and any liquid MEG adhering to the surface of the PET flakes, as well as MEG vapor. Another region 121 may also include PET oligomers.

[0644] like Figure 1A As shown, the volume segment V 1The level 111 of MEG in 103 is lower than that of volume segment V 2 108 in MEG level 113. Figure 1A Also shown are the levels 111 and 113 of the MEG from the ground 114 (eg, the floor of a recycling plant) to the volume segment V 1 103 and V 2 The liquid MEG surface in 108 is measured. Due to the difference between the MEG levels 111 and 113, the volume segment V 2 A portion of the liquid MEG in 108 flows back to volume segment V through the conveying screw 109. 1 103. Volume segment V 1 The floating impurities not removed in 103 and transported to volume segment V 2 108 (together with the transport of the PET flakes) the floatable impurities can thus be transported back to the volume segment V 1 103. The PET flakes (and PET oligomers, if present) with MEG adhered to their surfaces leave the volume segment V through the outlet 122. 2 108.

[0645] Figure 1B A cross section of another part of the device is shown, seen from the side. The PET flakes (and PET oligomers, if present) flowing out through the outlet 122 are conveyed to the volume section V 3 124, this part is a reactor (for example, a glycolysis reactor). Volume segment V 3 124 and volume segment V 2 108 fluid communication. PET flakes (and PET oligomers, if present) enter volume segment V via inlet 125 3 124, and flows through volume segment V as indicated by arrow 136 3 124. Volume segment V 3 The inlet 125 of 124 is also located in the volume segment V 2 108 is located below the outlet 122. In other words, when the PET flakes (and PET oligomers, if present) are removed from the volume segment V 2 108 is delivered to volume segment V 3 At 124, the PET flakes (and PET oligomers, if present) are at least partially conveyed in the direction of gravity.

[0646] MEG (another organic compound) is fed into volume section V via inlet 143 3 124. PET and MEG (feed volume segment V 3 ) results in another initial mixture comprising PET flakes (and PET oligomers, if present) and MEG. When the other initial mixture flows through the volume segment V3 At 124, the MEG in the other initial mixture causes the partially depolymerized PET flakes (and PET oligomers, if present) to undergo further glycolysis (reducing the weight-average molar mass of the first polyester). Thus, a first intermediate mixture is obtained. A delivery pipe 144 in fluid communication with the outlet 126 is located in the volume segment V 3 124. The first intermediate mixture leaves volume section V through delivery pipe 144 and outlet 126 3 124. Leave volume segment V 3 The first intermediate mixture at outlet 126 of 124 includes free MEG and first intermediate products (including BHET and PET oligomers). Oligomers are polymers with multiple repeating units (e.g., dimers, trimers, and oligomers with more than three repeating units). Some PET flakes that have not been depolymerized into oligomers or BHET may also be present in the first intermediate mixture.

[0647] like Figure 1B As shown by the arrow in FIG. 1 , the first intermediate mixture leaves the volume segment V through the outlet 126. 3 124, and then transported to volume segment V 4 127, Volume segment V 4 127 and volume segment V 3 124 fluid communication. Volume segment V 4 127 can be, for example, a container or a tank, such as a stirred tank. The first intermediate mixture enters the volume section V through the inlet 128. 4 127. In volume segment V 4 In 127, the first intermediate mixture is mixed with diatomaceous earth (first particulate material). Stirring volume segment V 4 127 to improve mixing of the first intermediate mixture and diatomaceous earth.

[0648] like Figure 1B As shown by the arrow in FIG. 1 , the first intermediate mixture containing diatomaceous earth leaves the volume segment V through the outlet 129. 4 127, and is conveyed to the vertical leaf filter 130 (filter device), which is connected to the volume segment V 4 127 fluid communication. The first intermediate mixture containing diatomaceous earth enters the vertical leaf filter 130 through the inlet 131. The first intermediate mixture flows through the leaf filter 130 and flows between the leaf filter 130 and the volume segment V 4127 (not shown), so that each filter disc of leaf filter 130 is coated with diatomaceous earth. Initially, the filtrate (intermediate mixture) will be turbid. However, if each filter disc has been fully coated, the filtrate will become clear. Once the filtrate becomes clear, the intermediate mixture can leave vertical leaf filter 130 through outlet 132. Vertical leaf filter 130 filters out diatomaceous earth and other particulate materials (i.e., impurities) in the first intermediate mixture, as well as any PET flakes that have not yet been depolymerized into oligomers or BHET. The first intermediate mixture leaving vertical leaf filter 130 through outlet 132 contains only trace amounts of impurities and diatomaceous earth.

[0649] like Figure 1B As shown by the arrow in FIG. 1 , the first intermediate mixture flowing out of the vertical leaf filter 130 is delivered to the volume section V in fluid communication with the vertical leaf filter 130 through the outlet 132. 5 133. The first intermediate mixture enters the volume section V through the inlet 134 5 133. Volume segment V 5 133 may be, for example, a container or a tank, such as a distillation tank. Volume segment V 5 133 is used to determine and correct the color of the first intermediate mixture. If necessary, in the volume segment V 5 At least one colorant is added to the first intermediate mixture at 133. If at least one colorant is added to the first intermediate mixture, the first intermediate mixture is stirred to better mix the first intermediate mixture with the at least one colorant. The first intermediate mixture (which may contain at least one colorant) leaves the volume segment V through outlet 135. 5 133.

[0650] Figure 1C A cross section of another part of the device is shown, seen from the side. A first intermediate mixture, which may contain at least one colorant, is conveyed from outlet 135 to volume section V 6 137, the volume segment and the volume segment V 5 133 fluid connection. The first intermediate mixture enters volume section V through inlet 138 6 137. When entering volume segment V 6 137, a catalyst and a stabilizer may be added to the first intermediate mixture. The PET flakes in the raw material are obtained by crushing used PET bottles. During the production of PET for bottles, a catalyst is usually added. Therefore, the PET flakes of the raw material usually already contain a catalyst, and further catalyst may not need to be added during the recycling process. Volume segment V 6137 is a prepolymerization reactor, which polymerizes the oligomers and BHET in the first intermediate mixture (increasing the weight average molar mass of the first intermediate product) to obtain a polymer (another intermediate product). Thus, another intermediate mixture containing a polymer (i.e., a PET polymer) and MEG is obtained. In volume segment V 6 In 137, up to 95% of the excess MEG is evaporated under vacuum conditions. The excess MEG is transported to volume section V 6 The free MEG in the volume and the bound MEG released by polymerization. Another intermediate mixture leaves the volume segment V through the outlet 139. 6 137.

[0651] like Figure 1C As shown by the arrow in FIG. 1 , the volume segment V is exited through the outlet 139. 6 Another intermediate mixture of 137 is conveyed to volume section V 7 140, Volume segment V 7 140 and volume segment V 6 137 fluid connection. Another intermediate mixture enters volume section V through inlet 141 7 140. Volume segment V 7 140 is a polymerization reactor, such as a cage reactor, for further increasing the weight average molar mass of the polymer and any remaining oligomers in the other intermediate mixture (by polymerization). In addition, any remaining MEG in the other intermediate mixture is also in volume segment V 7 140 is evaporated under vacuum conditions. The remaining MEG is transported to volume section V 7 The free MEG in the volume segment V and the bound MEG released by polymerization. Another intermediate mixture containing another intermediate product leaves the volume segment V through the outlet 142. 7 140. In volume segment V 7 Another intermediate product (i.e., recycled PET) obtained after the completion of the polymerization in 140 is in the form of a hot melt. The hot melt can be used to produce yarn (product example) and particles generally referred to as chips. The chips can be obtained by extruding and cooling the hot melt. Therefore, another intermediate product is a further polyester.

[0652] Although not shown, the first intermediate mixture is pumped to achieve the first intermediate mixture in the volume section V 3 、V 4 、V 5 、V 6 and the vertical blade filter. This also applies to the other intermediate mixture, that is, the other intermediate mixture in the volume section V 6 and V 7 Pumping between.

[0653] (not shown in the figure): The further intermediate product can then be used to produce further products, such as yarn for textiles. For example, the further intermediate product in molten form is pumped through a spinning pack. The spinning pack is conceptually similar to a household shower head. The number of holes in the spinning pack determines the number of filaments in the yarn produced. The molten further intermediate product stream leaving the spinning pack is cooled and coalesced into a single yarn. The single yarn is then wound onto a bobbin. The further intermediate product can be obtained without using virgin PET. For example, virgin PET monomers and oligomers are not mixed with the first intermediate product before polymerization. For example, virgin PET polymer is also not mixed with the further intermediate product.

[0654] Back to Figure 1A and 1B :These figures show that when the intrinsic viscosity of PET flakes is greater than or equal to Y IV,1 When the intrinsic viscosity of the PET flakes is less than Y IV,2 When the value (here Y IV,1 and Y IV,2 represents a variable, where Y IV,1 >Y IV,2 ), the PET sheet is transported in another direction at least partially along the direction of gravity.

[0655] like Figure 1A As shown, in volume segment V 1 After contacting MEG in 103, the PET flakes are transported along direction 110 to volume segment V 2 108, which is at least partially opposite to the direction of gravity 161. 2 108, the PET sheet is transported along a transport direction 118, which is opposite to the direction of gravity 161, i.e., the volume segment V 2 The average conveying direction of the PET flakes in 108 is upward. Figure 1A In the context of , the first direction can be defined as the direction from the volume segment V 1 The bottom 107 of 103 to the volume segment V 2 108 is directed toward the outlet 122. However, the foregoing should not be considered a general definition of the first direction. Conveying PET (e.g., in the form of flakes) along the first direction should generally be understood as providing that the intrinsic viscosity of the PET flakes is greater than or equal to the value Y IV,1 , the PET chips (eg in the form of flakes) are conveyed at least partially in the direction of gravity.

[0656] like Figure 1B As shown, when the PET flake enters the volume segment V through the inlet 125 3 At 124, the PET sheet is transported in a direction 136, which is oriented along the direction of gravity 161. Figure 1B In the context of , direction 136 defines another direction. However, the foregoing should not be considered as a general definition of this other direction. The transport of PET (e.g., in the form of flakes) along this other direction should generally be understood as the transport of PET flakes (e.g., in the form of flakes) at least partially along the gravity direction, as long as the intrinsic viscosity of the PET flakes is less than or equal to the value Y. IV,2 However, once the PET is depolymerized, the PET oligomers and / or monomers can be transported against or along the direction of gravity.

[0657] FIG. 2 is a schematic diagram 200 showing how to measure the angle between the further direction 210 and the horizontal plane 214. The horizontal plane 214 is perpendicular to the gravity direction 261. The angle is measured as the minimum angle between the further direction 210 and the horizontal plane 214. Figure 2A and Figure 2B In these figures, angle 262 is defined as the angle between further direction 210 and horizontal plane 214, rather than angle 263.

[0658] Figure 3 is a flow chart illustrating steps for producing a first intermediate product according to an embodiment of a method 300 of the present invention. Figure 3 The optional steps in are indicated by dashed boxes. A description of the method steps is given below.

[0659] Steps: Description:

[0660] 301: Providing a feedstock comprising a first polyester, wherein the first polyester in the feedstock is in the form of a plurality of fragments; and wherein, based on the total mass of the plurality of fragments in the feedstock, 30 wt-% or less, more preferably 27 wt-% or less, even more preferably 23 wt-% or less, and further preferably 20 wt-% or less of the fragments have a thickness equal to or greater than 1.0 mm.

[0661] 302: In volume segment V 1 The method further comprises contacting a feedstock with a first amount of a first organic compound to obtain a first initial mixture, wherein the first amount is in liquid form.

[0662] 303: Optionally, the first polyester is removed from the volume segment V 1 Convey to volume segment V 2 .

[0663] 304: Optionally, in volume segment V 2 The first polyester is contacted with an additional amount of a first organic compound.

[0664] 305: Optionally, in volume segment V 2 The weight average molar mass of the first polyester is reduced.

[0665] 306: Optionally, the first polyester is removed from the volume segment V 2 Convey to volume segment V 3 .

[0666] 307: In volume segment V 3 The first polyester is contacted with another organic compound to obtain another initial mixture.

[0667] 308: In volume segment V 3 The method further comprises reducing the weight average molar mass of the first polyester to obtain a first intermediate mixture, wherein the first intermediate mixture comprises the first intermediate product and the another organic compound.

[0668] 309: Optionally, the first intermediate mixture is removed from the volume segment V 3 Convey to volume segment V 4 .

[0669] 310: Optionally, to volume segment V 4 The first particulate material is added to the first intermediate mixture.

[0670] 311: Optionally, the first intermediate mixture is removed from the volume segment V 4 Transport to the filtration device.

[0671] 312: Optionally, using a filtering device to at least partially remove the following substances from the first intermediate mixture: the first particulate material, at least one impurity.

[0672] 313: Optionally, the first intermediate mixture is conveyed from the filtration device to the volume section V 5 .

[0673] 314: Optionally, to volume segment V 5 At least one colorant is added to the first intermediate mixture.

[0674] exist Figure 3 In one aspect of the embodiment of , preferably, steps 304 and 305 are at least partially performed simultaneously. Figure 3 In one aspect of the embodiment of the present invention, preferably, steps 307 and 308 are performed at least partially simultaneously.

[0675] Figure 4 is a flow chart showing the steps of an embodiment of a method 400 according to the present invention for producing another intermediate product. Figure 4 The optional steps in are indicated by dashed boxes. A description of the method steps is given below.

[0676] Steps: Description:

[0677] 401: Provide a first intermediate mixture containing a first intermediate product. The first intermediate product and the first intermediate mixture are Figure 3 By transferring the first intermediate mixture from the filtering device to the volume section V 6 , so that in the volume segment V 6 A first intermediate mixture is provided.

[0678] 402: In volume segment V 6 The mass average molar mass of the first intermediate product in the first intermediate mixture is increased to obtain another intermediate mixture containing another intermediate product. The other intermediate mixture further includes at least one or all of the following: a first organic compound, another organic compound.

[0679] 403: Optionally, the other intermediate mixture is conveyed to volume segment V 7 .

[0680] 404: Optionally, in volume segment V 7 The mass average molar mass of another intermediate product in another intermediate mixture is further increased.

[0681] 405: Optionally, at least partially remove at least one organic compound, such as the first organic compound or another organic compound, from another intermediate mixture. This step can be at least partially performed simultaneously with at least one or all of steps 402 and 404.

[0682] exist Figure 4 In one aspect of the embodiment of the present invention, it is preferred that step 405 is at least partially performed simultaneously with at least one or all of steps 402 and 405. In a preferred embodiment of the present invention, according to the present invention, the method for producing another intermediate product comprises steps 301 to 314 and steps 401 to 405. For example, Figure 3 The steps can be Figure 4 A combination of steps, where Figure 3 The steps are Figure 4 In such a combination, Figure 3 and Figure 4 The optional steps described in remain optional.

[0683] FIG. 5 shows how the orientation relative to the direction of gravity is defined. Figure 5A A direction 570 is shown that is at least partially opposite to the gravity direction 561. The direction 570 can be decomposed into three components. The direction 570 has a component 571 parallel to the gravity direction 561 and a component 572 perpendicular to the gravity direction (another component perpendicular to the gravity direction is not shown). The direction of the component 571 is opposite to the gravity direction.

[0684] Figure 5BA direction 570 is shown that is at least partially along the direction of gravity 561. Figure 5A Similarly, direction 570 has a component 571 parallel to the gravity direction 561 and a component 572 perpendicular to the gravity direction. Figure 5A on the contrary, Figure 5B The direction of component 571 in is along the direction of gravity.

[0685] Figure 7 An SEM image of a PET flake is shown. Impurities on the surface of the PET flake can be identified as white particles. Figure 7 Three impurities 781a, 781b and 781c are marked. Figure 7 is an example of a SEM image used to determine the number of particles per unit area of ​​the at least one impurity.

[0686] Figure 8 The pore size distribution of the first particulate material is shown. Figure 8 It can be seen that the first particle material has modes at about 17100 nm, 15100 nm, 12300 nm, 10600 nm and 9300 nm. The modes are where the quantity dV / dlogD has a maximum value (either a local maximum or a global maximum). dV is the differential volume and dlogD is the differential of the logarithm of the pore size of the first particle material. The primary mode refers to the global maximum value of dV / dlogD. The secondary mode refers to the second largest maximum value of dV / dlogD. Figure 8 The cumulative pore size of the first particulate material is also shown.

[0687] Fig. 9 is used to determine the volume segment V 1 A graphical representation of a method for determining the mass ratio of the raw material (more preferably the first polyester) to the first organic compound. Fig. 9 Shows Figure 1A Volume segment V 1 103 is an enlarged view of the cross section (for ease of explanation, Fig. 9 The volume segment V 1 103 size and Figure 1A The volume segment V 1 size has changed compared to the previous one).

[0688] Volume segment V 1 The first initial mixture 105 in is divided into a plurality of height sections H, such as Fig. 9 The first height portion H1 consists of a volume segment V 1 103 and the bottom 107 and the height A1, the second height portion H2 is defined by the heights A1 and A2, and so on. The last height portion H6 is defined by the height A5 and the surface 106 of the first initial mixture 105. Fig. 9Six height sections H are shown, but the number of height sections is determined by the volume segment V. 1 The height of each height section should be 20 cm, but the last height section ( Fig. 9 For example, if the volume segment V 1 If the filling height of the first initial mixture is 150 cm, the first initial mixture is divided into 8 height segments, 7 of which are 20 cm high and the last is 10 cm high. The height of the first height segment H1 bounded by the bottom 107 is measured from the lowest point of the bottom 107.

[0689] Take 5 samples of the first initial mixture in each height section. The volume of each sample is 250 ml. Then all samples are combined to obtain a collective sample. Use the collective sample to determine the mass ratio.

[0690] If during normal operation of the PET recycling process the stirring volume segment V 1 , then the stirring volume section V 1 In this case, the five samples taken in the height segment should be taken at the same location in the height segment, with a two-minute interval between two subsequent samples. Fig. 9 , where the five samples in the height segment H1 are collected at the position B1, and the sampling interval is two minutes. The height segment position where the five samples are collected can be any position in the height segment.

[0691] If the stirring device is a physical stirring device (e.g. Fig. 9 164), which does not allow the collection of samples below a certain height, the lowest height A at which the sample can be collected without interfering with the stirring device min Replace the bottom 107 in the above procedure, that is, the first height segment is A min For the boundary. Fig. 9 A new height portion I is shown, which has been adjusted for the presence of the stirring device 164. Similar to the height portion H, the height of the height portion I is also 20 cm, except for the height portion I5 bordering the surface 106.

[0692] If the volume segment V is not 1 If stirring is performed, the five samples collected in the height section should be collected at positions evenly distributed in the direction perpendicular to the height of the first initial mixture. Fig. 9 Shown as positions C1 to C5.

[0693] Example

[0694] The present invention is further illustrated below by way of examples. The present invention is not limited to the examples. In the tables given in the examples, the magnitude of the technical effect is indicated by one or more "-" or "+". The scale from low to high is as follows: "---, -, -, +, ++, +++". The Ref value represents a reference value, i.e., the increase or decrease of the technical effect is relative to the Ref value. A value of 0 represents no change relative to the reference value. When the Ref value is used, the scale from low to high is as follows: "---, -, Ref, +, ++, +++".

[0695] Basic Settings

[0696] Unless otherwise noted, the basic setup described below applies to all examples.

[0697] A raw material comprising PET flakes is provided. The PET flakes are obtained by processing (e.g., shredding) old PET bottles. The PET flakes are Figure 1A In other words, the PET flake passes through the volume segment V 1 and V 2 Transport, where the volume segment V 2 There is a first region and another region. In the volume segment V 1 and V 2 In the volume segment V, the PET flakes are in contact with the MEG. 1 The following parameters were used: PET to MEG mass ratio ranged from 0.06–0.25, temperature ranged from 60°C to 65°C, pressure ranged from 98 kPa to 103 kPa, and residence time ranged from 20 min to 30 min. Volume segment V 2 Use the following parameters: Volume Segment V 2 The mass ratio of PET to MEG at the inlet is in the range of 0.3–0.5, and the volume segment V 2 The mass ratio of PET to MEG at the outlet is in the range of 5–20, the temperature is in the range of 60°C to 200°C, the overpressure is in the range of 4 kPa to 8 kPa, and the residence time is in the range of 110 min to 150 min.

[0698] like Figure 1B As shown, the PET sheet is then 2 Transport to volume segment V 3 (Glycolysis reactor). Volume segment V 3 The PET flakes in the volume segment V are also in contact with MEG. 3 In the present study, the following parameters were used for the glycolysis process: temperature ranged from 195 °C to 240 °C, overpressure ranged from 0.7 kPa to 0.9 kPa, and residence time ranged from 250 min to 420 min.

[0699] In V3 In the embodiment of the present invention, depolymerization is carried out by glycolysis to obtain a first intermediate mixture comprising BHET, PET oligomers and free MEG. The first intermediate mixture comprises 85 wt-% to 93 wt-% of the first intermediate product (BHET and PET oligomers), and the remaining first intermediate mixture consists of free MEG and residual impurities (to be filtered out). The wt-% value is based on the total mass of the first intermediate mixture.

[0700] like Figure 1B As shown, the intermediate product is from volume segment V 3 Transport to volume segment V 4 In volume segment V 4 The first intermediate mixture is stirred in the volume segment V while the first particulate material is added to the first intermediate mixture. The first intermediate mixture now containing the first particulate material is removed from the volume segment V 4 The first intermediate mixture is transported to a filtration device, where it undergoes a filtration step. The filtration step also includes Figure 1B The filtered first intermediate mixture is then polymerized, as described in the pre-coating step. Figure 1C This results in recycled PET. The recycled PET is used to produce yarn.

[0701] Example 1

[0702] This example was repeated using different weight percentages of PET flakes having a thickness of 1 mm or more in the feedstock as shown in Table 1 below.

[0703] Table 1

[0704]

[0705] The technical effects described in Table 1 are as follows:

[0706] Transport efficiency: How efficiently can the PET flakes (raw material and / or partially depolymerized PET flakes) be transported to ensure that a component of the recycling plant (such as the Archimedean screw) does not get blocked. The expectation is to improve transport efficiency and reduce the occurrence of blockages.

[0707] Controlled heating of PET flakes: How to effectively control the volume segment V 2 It is desirable to increase the controlled heating of PET flakes.

[0708] • Embrittlement of PET flakes: The brittleness of PET flakes increases. It is desirable to increase the brittleness of PET flakes.

[0709] • Intrinsic viscosity reduction: The percentage by which the intrinsic viscosity is reduced is the percentage by which it is desired to increase.

[0710] Depolymerization time: volume segment V3 The time required for PET flakes to depolymerize into oligomers. It is desirable to reduce this time.

[0711] Recycling plant output: the amount of PET that can be recycled, measured in mass per time interval. It is desirable to increase output.

[0712] Purity of recycled PET: The impurity concentration in the PET obtained from the recycling process. This applies to impurities with a size less than 10 mm. It is desirable to increase the purity, i.e. reduce the impurity concentration.

[0713] Quality breaks / ton: Quality breaks / ton refers to the number of breaks in the spinning process of yarn produced from recycled PET. This applies to yarns with a thickness of 0.05 denier. It is desirable to reduce the number of yarn breaks.

[0714] Filter life: The number of hours a filter in a recycling plant can be used before it needs to be cleaned or replaced. It is, for example, a filter used to filter the first intermediate mixture comprising oligomers obtained from depolymerized PET flakes. It is desirable to increase this filter life.

[0715] Unless otherwise stated, the "basic settings" described above also apply to the examples below. In the tables given in the examples below, the size of the technical effect is indicated by one or more "-" or "+". The scales arranged from low to high are as follows: "------, -----, ----, ---, -, +, ++, +++, ++++, ++++++, ++++++". The value "Ref" represents the reference value, that is, the increase or decrease of the technical effect is relative to the "Ref" value. The value "0" means no change relative to the reference value. When the "Ref" value is used, the scales arranged from low to high are as follows: "------, -----, ----, ---, -, Ref, +, ++, +++, ++++, +++++, ++++++".

[0716] Example 2

[0717] Example 2 is a continuation of Example 1. That is, Example 2 shows additional changes in the use of different weight percentages of PET flakes having a thickness of 1 mm or more in the raw material, as shown in Table 2 below. Note that the magnitude of the technical effect in Table 2 (indicated using one or more "-" and "+") is not based on the same ratio used in Table 1. In Table 2, the difference between "0" and "+++" is about 5%.

[0718] Table 2

[0719]

[0720] The technical effects described in Table 2 are the same as those in Table 1, but have the following additional technical effects:

[0721] Degradation of PET: PET flakes and / or PET oligomers may degrade in bulk. This degradation can lead to the formation of undesirable by-products such as diethylene glycol. It is desirable to reduce the embrittlement of PET flakes.

[0722] Example 3

[0723] This example was repeated using different weight percentages of PET flakes having a thickness of 1 mm or more in the feedstock as shown in Table 3 below. Table 3 also uses the scale used in Table 1 to indicate the magnitude of the technical effect.

[0724] Table 3

[0725]

[0726]

[0727] The technical effects in Table 3 are the same as those in Table 2.

[0728] Reference Mark List

[0729] 100 Apparatus and method for producing another polyester

[0730] 101 Raw Materials

[0731] 102 Hopper

[0732] 103 Volume segment V 1

[0733] 104 Volume segment V 1 Entrance

[0734] 105 First initial mixture

[0735] 106 The surface of the first initial mixture

[0736] 107 Volume segment V 1 Bottom

[0737] 108 Volume segment V 2

[0738] 109 conveying screw

[0739] 110 Another direction

[0740] 111 The first organic compound level H 1

[0741] 112 Volume segment V 2 Bottom

[0742] 113 The first organic compound level H 2

[0743] 114 Ground

[0744] 115 Volume segment V 2 The first type of entrance

[0745] 116 Volume segment V 2 Another type of entrance

[0746] 117 Volume segment V 2 Another type of entrance

[0747] 118 Conveying direction

[0748] 119 Boundary

[0749] 120 First Area

[0750] 121 Another area

[0751] 122 Volume segment V 2 Export

[0752] 123 Volume segment V 1 Export

[0753] 124 Volume segment V 3

[0754] 125 Volume segment V 3 Entrance

[0755] 126 Volume segment V 3 Export

[0756] 127 Volume segment V 4

[0757] 128 Volume segment V 4 Entrance

[0758] 129 Volume segment V 4 Export

[0759] 130 Vertical Leaf Filter

[0760] 131 Vertical leaf filter inlet

[0761] 132 Vertical leaf filter outlet

[0762] 133 Volume segment V 5

[0763] 134 Volume segment V 5 Entrance

[0764] 135 Volume segment V 5 Export

[0765] 136 Through volume segment V 3 Flow direction

[0766] 137 Volume segment V 6

[0767] 138 Volume segment V 6 Entrance

[0768] 139 Volume segment V 6 Export

[0769] 140 Volume segment V 7

[0770] 141 Volume segment V 7 Entrance

[0771] 142 Volume segment V 7 Export

[0772] 143 Volume segment V 3 Entrance

[0773] 144 Delivery pipe

[0774] 161 Gravity Direction

[0775] 200 The measured angle between another direction and the horizontal plane

[0776] 210 Another direction

[0777] 214 Horizontal plane

[0778] 261 Gravity Direction

[0779] 262 Define the angle of another direction relative to the horizontal plane

[0780] 263 Incorrect Angle

[0781] 500 Direction of orientation

[0782] 561 Gravity Direction

[0783] 570 Direction

[0784] 571 Component parallel to gravity

[0785] 572 Component perpendicular to gravity

[0786] 700 SEM image for determining the number of foreign particles per unit area

[0787] 781 Impurities

Claims

1. A method for producing a first intermediate product, comprising the following steps a. providing a raw material comprising a first polyester, wherein the first polyester in the raw material is in the form of a plurality of fragments; b. In volume segment V 1 contacting the feedstock with a first amount of a first organic compound to obtain a first initial mixture, in, the first amount is in liquid form; c. contacting the first polyester with another organic compound, preferably in volume segment V 3 to obtain another initial mixture; d. Reduce the weight average molar mass of the first polyester, preferably in the volume segment V 3 to obtain a first intermediate mixture, wherein the first intermediate mixture comprises: i. The first intermediate product, ii. another organic compound; in, Based on the total mass of the plurality of fragments in the raw material, 30% or less of the fragments have a thickness equal to or greater than 1.0 mm.

2. The method according to claim 1, in, The first polyester is selected from polyethylene terephthalate, polybutylene terephthalate, polylactic acid, polytrimethylene terephthalate, polyethylene naphthalate, polycarbonate, polyester carbonate, polyarylate, polyester resin and a combination of two or more thereof.

3. The method according to any one of the preceding claims, in, At least 50 wt-% of the fragments, based on the total mass of the plurality of fragments in the feedstock, have at least one or all of the following characteristics: a. The first dimension is in the range of 0.1 mm to 25.0 mm; b. Thickness is in the range of 0.1mm to 3.5mm.

4. The method according to any one of the preceding claims, in, The first organic compound has at least one or all of the following characteristics: a. Containing at least two hydroxyl groups; b. The molar mass is at least 60 g / mol; c. The boiling point is at least 192°C.

5. The method according to any one of the preceding claims, in, The method further comprises mixing the first polyester with a first organic compound in a volume range V 2 Steps of contact.

6. The method according to claim 5, in, The method further includes the step of reducing at least one or all of the following in the volume segment V 2 : a. the weight average molar mass of the first polyester; b. The intrinsic viscosity of the first polyester.

7. The method according to any one of the preceding claims, in, The other organic compound has at least one or all of the following characteristics: a. Containing at least two hydroxyl groups; b. The molar mass is at least 60 g / mol; c. The boiling point is at least 192°C.

8. The method according to any one of the preceding claims, in, At least 40 wt-% of the first intermediate product is in the form of an oligomer having 2 to 35 repeating units.

9. The method according to any one of the preceding claims, in, The method further comprises the step of at least partially removing at least one impurity from the first intermediate mixture, preferably using a filtering device.

10. A method for producing another intermediate product, The following steps are involved: a. providing a first intermediate mixture comprising a first intermediate product, wherein the first intermediate product can be obtained by the method according to any one of claims 1 to 9; b. increasing the mass average molar mass of the first intermediate product in the first intermediate mixture, preferably in the volume segment V 6 to obtain another intermediate mixture comprising another intermediate product.

11. A first intermediate product obtained by the method according to any one of claims 1 to 9.

12. A further intermediate product obtainable by the process according to claim 10.

13. A product comprising another intermediate product according to claim 12.

14. Use of the first intermediate product according to claim 11 for producing another intermediate product.

15. Use of another intermediate product according to claim 12 for producing a product.

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