A bio-based furan polyester bulked continuous filament and its application

Abstract

The present invention belongs to the field of fiber technology, and specifically discloses a bio-based furan polyester bulked continuous filament, and also discloses its application. The bio-based furan polyester bulked continuous filament provided by the present invention adopts bio-based furan polyester as raw material, and is prepared by melt spinning and bulking treatment; wherein, the bio-based furan polyester is obtained by esterification and polycondensation of 2,5-furandicarboxylic acid and bio-based diol. The bio-based furan polyester bulked continuous filament provided by the present invention has good bulkiness and elastic recovery, large curling rate, and good properties such as heat resistance, solvent resistance, wear resistance, antistatic, hydrolysis resistance, and easy dyeing. It can be woven and processed into various loop pile carpets, cut pile carpets, and square carpets, etc., and is widely used in the fields of daily home furnishings, automobiles, passenger aircraft, and floor decoration in various public places.

Description

Technical Field

[0001] The invention belongs to the field of fiber technology, and specifically relates to a bio-based furan polyester bulked continuous filament, and also relates to an application thereof. Background Art

[0002] Bulk Continuous Filament (BCF) technology is a process that uses hot fluid jet deformation processing to produce chemical fiber bulk filaments. The produced BCF is an important fiber variety for home decoration in the chemical fiber family. Currently, more than 90% of floor coverings and carpets use chemical fibers as raw materials, mainly polypropylene (PP), nylon (PA), polyester (PET), etc. Among them, polyester has high strength, good heat resistance, corrosion resistance, and light resistance. Compared with nylon 6, polyester has better toughness and impact resistance, higher modulus, and better shrinkage. However, the pile resilience of polyester is not as good as that of nylon and polypropylene, and it can only be dyed with disperse dyes under high temperature and high pressure or with a carrier, so there are certain deficiencies in its application.

[0003] As people's awareness of ecological protection increases, the new generation of carpets and floor coverings are facing huge challenges in terms of recycling of raw materials, development of renewable resources, research and development and application of biotechnology and products, and waste recycling and utilization, which also brings new development opportunities. As an important variety of home furnishing fibers, the development and application of environmentally friendly bulked continuous filaments (BCF) are increasingly valued by the industry. At present, there are no reports on all-biobased polyester bulked continuous filaments. The development of bio-based polyester bulked continuous filaments is in line with the development and application direction of eco-friendly BCF technology and the trend of innovative development of the new generation of carpets and floor coverings.

[0004] In view of the above reasons, the present application aims to provide a fully bio-based polyester bulked continuous filament. Summary of the invention

[0005] The purpose of the present invention is to provide a bio-based furan polyester bulked continuous filament and also provide its application. The bio-based furan polyester bulked continuous filament is prepared using all-bio-based furan polyester raw materials and is a new type of environmentally friendly bulked continuous filament with excellent comprehensive performance and sustainability.

[0006] To achieve this object, the present invention adopts the following technical solutions.

[0007] In a first aspect, the present invention provides a bio-based furan polyester bulked continuous filament, which is prepared by melt spinning and bulking of bio-based furan polyester as a raw material; wherein the bio-based furan polyester is obtained by esterification and polycondensation of 2,5-furandicarboxylic acid and bio-based diol.

[0008] As an embodiment of the present invention, the raw materials for preparing 2,5-furandicarboxylic acid are non-food crops, such as Jerusalem artichoke, chicory, burdock, cassava, etc.; the purity of 2,5-furandicarboxylic acid is ≥99.9wt%.

[0009] As an embodiment of the present invention, the bio-based diol is selected from one or more of bio-based ethylene glycol, 1,3-propylene glycol, 1,4-butanediol, 2,3-butanediol, 1,2-pentanediol, 1,5-pentanediol, 2,5-furan dimethanol, 2,5-tetrahydrofuran dimethanol, and isosorbide.

[0010] As an embodiment of the present invention, the molar ratio of 2,5-furandicarboxylic acid and bio-based diol monomer is: 2,5-furandicarboxylic acid: bio-based diol = 1: (1.4-2.2), preferably 2,5-furandicarboxylic acid: bio-based diol = 1: (1.8-2.2).

[0011] As an embodiment of the present invention, the bio-based furan polyester bulked continuous filament provided by the present invention has a single filament fineness of 1 to 50 dtex, preferably 5 to 30 dtex.

[0012] As an embodiment of the present invention, in the melt spinning, the spinning temperature is 240-280°C, the heat deformation temperature is 200-240°C, the drafting multiple is 2.0-5.5 times, the network degree is 20-40 / m, and the spinning speed is 500-2000m / min. The melt spinning obtains the primary yarn, and the primary yarn is then expanded and wound to obtain the bio-based furan polyester bulked continuous filament.

[0013] As an embodiment of the present invention, in melt spinning, the spinning assembly adopts a clover-shaped or hollow eccentric spinneret, and the spinneret preferably has an aperture of 0.5 to 1.5 mm and a number of 36 to 96 holes.

[0014] As a preferred embodiment of the present invention, in melt spinning, the heat deformation temperature is 200-220°C.

[0015] As a preferred embodiment of the present invention, in the melt spinning, the drafting ratio is 2.5 to 4.0 times.

[0016] As a preferred embodiment of the present invention, in the melt spinning, the spinning speed is 1000-1500 m / min, more preferably 1200 m / min.

[0017] As a preferred embodiment of the present invention, in melt spinning, the spinning assembly adopts a clover-shaped or hollow eccentric spinneret, preferably with 48 holes.

[0018] As an embodiment of the present invention, the temperature for the esterification reaction of 2,5-furandicarboxylic acid and bio-based diol is 170-220°C, preferably 180-190°C.

[0019] As an embodiment of the present invention, during the esterification reaction, an antioxidant and / or an esterification catalyst is also added to the reaction system.

[0020] Preferably, the antioxidant is at least one of antioxidant 1010, antioxidant SEED, and antioxidant B215, and antioxidant B215 is more preferred.

[0021] Preferably, the antioxidant is added in an amount of 0.05% to 0.5% by mass of the 2,5-furandicarboxylic acid; further preferably, the antioxidant is added in an amount of 0.05% to 0.15% by mass of the 2,5-furandicarboxylic acid.

[0022] Preferably, the esterification catalyst is selected from metal acetate and germanium oxide, wherein the metal acetate is preferably at least one selected from zinc acetate, manganese acetate and cadmium acetate. Further preferably, the esterification catalyst is selected from germanium oxide and zinc acetate.

[0023] Preferably, the amount of the esterification catalyst added is 0.01% to 0.1% of the mass of the 2,5-furandicarboxylic acid; further preferably, the amount of the esterification catalyst added is 0.01% to 0.05% of the mass of the 2,5-furandicarboxylic acid.

[0024] As an embodiment of the present invention, the esterification reaction product of 2,5-furandicarboxylic acid and bio-based diol is polycondensed to prepare bio-based furan polyester.

[0025] Preferably, a heat stabilizer and / or a polycondensation catalyst is added to the esterification reaction product of 2,5-furandicarboxylic acid and bio-based diol, and the polycondensation reaction is carried out after reacting at normal pressure for 5 to 10 minutes.

[0026] Preferably, the heat stabilizer is selected from at least one of phosphoric acid, phosphorous acid, hypophosphorous acid, triphenyl phosphate, diphenyl phosphate, triphenyl phosphite, diphenyl phosphorus, ammonium phosphite, and diammonium phosphate; more preferably phosphoric acid.

[0027] Preferably, the amount of the heat stabilizer added is 0.005% to 0.1% of the mass of the 2,5-furandicarboxylic acid, and more preferably 0.01% to 0.05% of the mass of the 2,5-furandicarboxylic acid.

[0028] Preferably, the polycondensation catalyst is selected from antimony-based and titanium-based catalysts, more preferably at least one of antimony trioxide, antimony glycol, titanium dioxide, tetrabutyl titanate, and tetraethyl titanate, and more preferably antimony glycol and tetrabutyl titanate.

[0029] Preferably, the added amount of the polycondensation catalyst is 0.01% to 0.1% of the mass of the 2,5-furandicarboxylic acid, and more preferably 0.05% to 0.08% of the mass of the 2,5-furandicarboxylic acid.

[0030] As a preferred embodiment of the present invention, the polycondensation of the esterification reaction product of 2,5-furandicarboxylic acid and bio-based diol includes a pre-polycondensation treatment and a final polycondensation treatment, wherein the pre-polycondensation treatment is firstly performed and then the final polycondensation treatment is performed to obtain the bio-based furan polyester.

[0031] Preferably, the pre-polycondensation reaction temperature is 230-250° C., the pressure is less than 0 MPa, and the reaction time is 0.5-1 h.

[0032] Preferably, the final polycondensation reaction temperature is 240-260° C., the vacuum degree is ≤70 Pa, and the reaction time is 2-5 h.

[0033] As an embodiment of the present invention, the intrinsic viscosity of the bio-based furan polyester prepared by the present invention is 0.63-0.85 dl / g; further, the intrinsic viscosity of the bio-based furan polyester prepared by the present invention is 0.69-0.75 dl / g.

[0034] As an embodiment of the present invention, the bio-based furan polyester prepared by the present invention is discharged and granulated to obtain bio-based furan polyester chips.

[0035] Preferably, the bio-based furan polyester chips are dried and used as raw materials to prepare bio-based furan polyester bulked continuous filaments through melt spinning and puffing. More preferably, the drying temperature is 100-150° C., and the drying time is 4-12 hours.

[0036] In a second aspect, the present invention provides an application of a bio-based furan polyester bulked continuous filament, specifically, an application of the bio-based furan polyester bulked continuous filament as a raw material for making floor coverings or carpets.

[0037] The bio-based furan polyester bulked continuous filament provided by the present invention adopts 2,5-furandicarboxylic acid (FDCA) as a preparation raw material, which is a biomass monomer with stable properties. The 100% bio-based furan polyester synthesized with FDCA as a dibasic acid and a diol also derived from biomass has excellent comprehensive performance and can get rid of dependence on petroleum-based raw materials. It is low-carbon and environmentally friendly, and is in line with sustainable and carbon neutral development strategies.

[0038] The present invention obtains a bio-based furan polyester raw material with excellent performance by esterifying and polymerizing the bio-based monomer 2,5-furandicarboxylic acid and the bio-based diol under certain conditions; the bio-based furan polyester raw material is then processed by melt spinning and expansion deformation process to prepare a fully bio-based furan polyester bulked continuous filament (BCF). By controlling the relevant process parameters in the process of melt spinning and other processes, the prepared bio-based furan polyester bulked continuous filament has high strength, good bulkiness and elastic recovery, large curling rate, stable three-dimensional curling formation, excellent hand feel, and also has good properties such as heat resistance, solvent resistance, wear resistance, antistatic, hydrolysis resistance, easy dyeing, etc., and can achieve dyeing with disperse dyes and cationic dyes. It is a new type of environmentally friendly bulked continuous filament with excellent comprehensive performance and sustainability.

[0039] The bio-based furan polyester expanded continuous filament provided by the present invention can be woven into various loop pile carpets, cut pile carpets, square carpets, etc., and can be widely used in the fields of floor decoration in daily homes, cars, passenger planes and various public places. BRIEF DESCRIPTION OF THE DRAWINGS

[0040] Figure 1 This is the GPC spectrum of the bio-based furan polyester obtained in Example 1 of the present invention. DETAILED DESCRIPTION

[0041] The technical solution of the present invention is further described in detail below. It should be understood by those skilled in the art that the specific implementation is only to help understand the present invention and should not be regarded as a specific limitation of the present invention.

[0042] It should be noted that, unless otherwise specified, the technical means used in the following examples are conventional means well known to those skilled in the art, and the raw materials used are all commercially available conventional products.

[0043] The bio-based furan polyester bulked continuous filament provided by the present invention is obtained by a preparation method comprising the following steps:

[0044] (1) Preparation of bio-based furan polyester

[0045] Adding 2,5-furandicarboxylic acid, bio-based diol, esterification catalyst and antioxidant into a polymerization reactor, wherein the molar ratio of 2,5-furandicarboxylic acid to bio-based diol is controlled at 1:(1.4-2.2), the amount of esterification catalyst added is 0.01%-0.1% of the mass of 2,5-furandicarboxylic acid, and the amount of antioxidant added is 0.05%-0.5% of the mass of 2,5-furandicarboxylic acid;

[0046] The air in the reactor is replaced by nitrogen through vacuum pumping, and nitrogen protection is finally maintained; the polymerization reactor is heated by circulating heat medium, and the stirring motor is turned on to help the materials mix and react;

[0047] First, the esterification reaction is carried out at a reaction temperature of 170-220°C and a reaction time of 1-2 hours. When the water output reaches 95% of the theoretical value and no more output is produced, the esterification reaction is completed.

[0048] Add a polycondensation catalyst and a heat stabilizer to the esterification reaction product, wherein the amount of the polycondensation catalyst added is 0.01% to 0.1% of the mass of 2,5-furandicarboxylic acid, and the amount of the heat stabilizer added is 0.005% to 0.1% of the mass of 2,5-furandicarboxylic acid, and nitrogen replacement is performed, followed by reaction at normal pressure for 5 to 10 minutes; then a preliminary polycondensation reaction is performed, the temperature in the kettle is 230 to 250° C., the pressure is less than 0 MPa, and the reaction time is 0.5 to 1 hour; then a final polycondensation reaction is performed, the temperature is 240 to 260° C., the vacuum degree is ≤70 Pa, and the reaction time is 2 to 5 hours; after the reaction is completed, stirring is stopped, nitrogen is passed through to pressurize the material, and granulation is performed to obtain bio-based furan polyester chips;

[0049] (2) Preparation of bio-based furan polyester bulked continuous filaments

[0050] The bio-based furan polyester chips are dried in a vacuum drum oven at a temperature of 100 to 150°C for 4 to 12 hours;

[0051] Then melt spinning is carried out with a spinning temperature of 240-280°C, a heat deformation temperature of 200-240°C, a drafting multiple of 2.0-5.5 times, a network density of 20-40 pcs / m, and a spinneret of clover type or hollow eccentric core type with an aperture of 0.5-1.5mm and a number of holes of 36-96; the single yarn fineness is 1-50dtex, and the spinning speed is 500-2000m / min to obtain the primary yarn, which is then fully expanded and wound to successfully obtain the bio-based furan polyester expanded continuous filament.

[0052] The following is a detailed explanation through examples.

[0053] Example 1

[0054] The bio-based furan polyester bulked continuous filament provided in this embodiment is prepared by the following steps:

[0055] 1500g of 2,5-furandicarboxylic acid, 1463g of bio-based 1,3-propylene glycol, 1.5g of antioxidant B215 and 0.5g of zinc acetate were added to the polymerization kettle. After the feeding was completed, the kettle was sealed and the air in the kettle was replaced by nitrogen through vacuum pumping. This was repeated 3 times. Finally, nitrogen was filled as a protective gas at a pressure of 25kPa. Then, the circulating heat medium was started to start heating and stirring was started at the same time.

[0056] The esterification reaction begins. During the esterification process, the temperature is controlled at 180-190°C. The esterification time is about 2 hours. When the water output reaches 95% of the theoretical value and no more output occurs, the esterification reaction is completed.

[0057] 1.0 g of tetrabutyl titanate and 0.5 g of phosphoric acid were added to the esterification reaction product, and the mixture was reacted at normal pressure for 10 min after nitrogen substitution; then a negative pressure pre-polycondensation reaction was carried out, the reaction temperature was controlled at 230° C., the reaction time was 1 h, and the pressure in the autoclave was less than 0 MPa; then a final polycondensation reaction was carried out, the reaction temperature was 260° C., the reaction time was 4 h, and the vacuum degree was ≤70 Pa; after the melt reached the viscosity requirement, stirring was stopped, nitrogen was introduced to normal pressure, and then the mixture was allowed to stand for 3 min, and nitrogen was introduced again to discharge and granulate the mixture to obtain bio-based furan polyester chips;

[0058] The obtained bio-based furan polyester chips were dried in a drum oven at a temperature of 110°C and a drying time of 12 hours until the moisture content was ≤100ppm; then melt spinning was carried out at a spinning temperature of 245°C, a box temperature of 250°C, a heat deformation temperature of 210°C, a drafting multiple of 3.0 times, a network degree of 30 / m, a clover-shaped spinneret with an aperture of 0.8mm, a number of holes of 48, a spinning specification of 1500D / 48, a single yarn fineness of 30dtex, and a spinning speed of 1200m / min to obtain nascent yarns; after the nascent yarns were fully expanded, they were wound to obtain bio-based furan polyester expanded continuous filaments.

[0059] Example 2

[0060] The bio-based furan polyester bulked continuous filament provided in this embodiment is prepared by the following steps:

[0061] 1500g of 2,5-furandicarboxylic acid, 1730g of bio-based 1,4-butanediol, 1.5g of antioxidant B215 and 0.5g of zinc acetate were added to the polymerization kettle. After the feeding was completed, the kettle was sealed and the air in the kettle was replaced by nitrogen through vacuum pumping. The process was repeated twice, and finally nitrogen was filled as a protective gas at a pressure of 25kPa. Then, the circulating heat medium was started to start heating and stirring was started at the same time.

[0062] The esterification reaction begins. During the esterification process, the temperature is controlled at 180-190°C. The esterification time is about 2 hours. When the water output reaches 95% of the theoretical value and no more output occurs, the esterification reaction is completed.

[0063] 1.0 g of tetrabutyl titanate and 0.5 g of phosphoric acid were added to the esterification reaction product, and the mixture was reacted at normal pressure for 10 min after nitrogen substitution; then a negative pressure pre-polycondensation reaction was carried out, the reaction temperature was controlled at 230° C., the reaction time was 1 h, and the pressure in the autoclave was less than 0 MPa; then a final polycondensation reaction was carried out, the reaction temperature was 260° C., the reaction time was 4 h, and the vacuum degree was ≤70 Pa; after the melt reached the viscosity requirement, stirring was stopped, nitrogen was introduced to normal pressure, and then the mixture was allowed to stand for 3 min, and nitrogen was introduced again to discharge and granulate the mixture to obtain bio-based furan polyester chips;

[0064] The obtained bio-based furan polyester chips are taken and dried in a drum oven at a temperature of 110°C and a drying time of 12 hours until the moisture content is ≤100ppm; then melt spinning is carried out at a spinning temperature of 240°C, a box temperature of 245°C, a heat deformation temperature of 210°C, a drafting multiple of 3.5 times, a network degree of 30 / m, a clover-shaped spinneret with an aperture of 0.8mm, a number of holes of 48, a spinning specification of 1500D / 48, a single yarn fineness of 30dtex, and a spinning speed of 1200m / min to obtain a nascent yarn; after the nascent yarn is fully expanded, it is wound to obtain a bio-based furan polyester expanded continuous filament.

[0065] Example 3

[0066] The bio-based furan polyester bulked continuous filament provided in this embodiment is prepared by the following steps:

[0067] 1500g of 2,5-furandicarboxylic acid, 2000g of bio-based 1,5-pentanediol, 1.5g of antioxidant B215 and 0.5g of zinc acetate were added to the polymerization kettle. After the feeding was completed, the kettle was sealed and the air in the kettle was replaced by nitrogen through vacuum pumping. The process was repeated 3 times. Finally, nitrogen was filled as a protective gas at a pressure of 25kPa. Then, the circulating heat medium was started to start heating and stirring was started at the same time.

[0068] The esterification reaction begins. During the esterification process, the temperature is controlled at 180-190°C. The esterification time is about 2 hours. When the water output reaches 95% of the theoretical value and no more output occurs, the esterification reaction is completed.

[0069] 1.0 g of tetrabutyl titanate and 0.5 g of phosphoric acid were added to the esterification reaction product, and the mixture was reacted at normal pressure for 10 min after nitrogen substitution; then a negative pressure pre-polycondensation reaction was carried out, the reaction temperature was controlled at 230° C., the reaction time was 1 h, and the pressure in the autoclave was less than 0 MPa; then a final polycondensation reaction was carried out, the reaction temperature was 260° C., the reaction time was 4 h, and the vacuum degree was ≤70 Pa; after the melt reached the viscosity requirement, stirring was stopped, nitrogen was introduced to normal pressure, and then the mixture was allowed to stand for 3 min, and nitrogen was introduced again to discharge and granulate the mixture to obtain bio-based furan polyester chips;

[0070] The obtained bio-based furan polyester chips were dried in a drum oven at a temperature of 110°C and a drying time of 12 hours until the moisture content was ≤100ppm; then melt spinning was carried out at a spinning temperature of 240°C, a box temperature of 245°C, a heat deformation temperature of 210°C, a drafting multiple of 3.0 times, a network degree of 30 / m, a clover-shaped spinneret with an aperture of 0.8mm, a number of holes of 48, a spinning specification of 1500D / 48, a single yarn fineness of 30dtex, and a spinning speed of 1200m / min to obtain nascent yarns; after the nascent yarns were fully expanded, they were wound to obtain bio-based furan polyester expanded continuous filaments.

[0071] Example 4

[0072] The bio-based furan polyester bulked continuous filament provided in this embodiment is prepared by the following steps:

[0073] 1500g of 2,5-furandicarboxylic acid, 2540g of bio-based 2,5-tetrahydrofuran dimethanol, 1.5g of antioxidant B215 and 0.5g of zinc acetate were added to the polymerization kettle. After the feeding was completed, the kettle was sealed and the air in the kettle was replaced by nitrogen through vacuum pumping. This was repeated 3 times. Finally, nitrogen was filled as a protective gas at a pressure of 25kPa. Then, the circulating heat medium was started to start heating and stirring was started at the same time.

[0074] The esterification reaction begins. During the esterification process, the temperature is controlled at 180-190°C. The esterification time is about 2 hours. When the water output reaches 95% of the theoretical value and no more output occurs, the esterification reaction is completed.

[0075] 1.0 g of tetrabutyl titanate and 0.5 g of phosphoric acid were added to the esterification reaction product, and the mixture was reacted at normal pressure for 10 min after nitrogen substitution; then a negative pressure pre-polycondensation reaction was carried out, the reaction temperature was controlled at 230° C., the reaction time was 1 h, and the pressure in the autoclave was less than 0 MPa; then a final polycondensation reaction was carried out, the reaction temperature was 260° C., the reaction time was 4 h, and the vacuum degree was ≤70 Pa; after the melt reached the viscosity requirement, stirring was stopped, nitrogen was introduced to normal pressure, and then the mixture was allowed to stand for 3 min, and nitrogen was introduced again to discharge and granulate the mixture to obtain bio-based furan polyester chips;

[0076] The obtained bio-based furan polyester chips are taken and dried in a drum oven at a temperature of 110°C and a drying time of 12 hours until the moisture content is ≤100ppm; then melt spinning is carried out at a spinning temperature of 250°C, a box temperature of 255°C, a heat deformation temperature of 220°C, a drafting multiple of 3.0 times, a network degree of 30 / m, a clover-shaped spinneret with an aperture of 0.8mm, a number of holes of 48, a spinning specification of 1500D / 48, a single yarn fineness of 30dtex, and a spinning speed of 1200m / min to obtain a nascent yarn; after the nascent yarn is fully expanded, it is wound to obtain a bio-based furan polyester expanded continuous filament.

[0077] Example 5

[0078] The bio-based furan polyester bulked continuous filament provided in this embodiment is prepared by the following steps:

[0079] 1500g of 2,5-furandicarboxylic acid, 1170g of bio-based 1,3-propylene glycol, 562g of bio-based isosorbide, 1.5g of antioxidant B215 and 0.5g of zinc acetate were added to the polymerization kettle. After the feeding was completed, the kettle was sealed and the air in the kettle was replaced by nitrogen through vacuum pumping. This was repeated 3 times. Finally, nitrogen was filled as a protective gas at a pressure of 25kPa. After that, the circulating heat medium was started to start heating and stirring was started at the same time.

[0080] The esterification reaction begins. During the esterification process, the temperature is controlled at 180-190°C. The esterification time is about 2 hours. When the water output reaches 95% of the theoretical value and no more output occurs, the esterification reaction is completed.

[0081] 1.0 g of tetrabutyl titanate and 0.5 g of phosphoric acid were added to the esterification reaction product, and the mixture was reacted at normal pressure for 10 min after nitrogen substitution; then a negative pressure pre-polycondensation reaction was carried out, the reaction temperature was controlled at 230° C., the reaction time was 1 h, and the pressure in the autoclave was less than 0 MPa; then a final polycondensation reaction was carried out, the reaction temperature was 260° C., the reaction time was 4 h, and the vacuum degree was ≤70 Pa; after the melt reached the viscosity requirement, stirring was stopped, nitrogen was introduced to normal pressure, and then the mixture was allowed to stand for 3 min, and nitrogen was introduced again to discharge and granulate the mixture to obtain bio-based furan polyester chips;

[0082] The obtained bio-based furan polyester chips are taken and dried in a drum oven at a temperature of 110°C and a drying time of 12 hours until the moisture content is ≤100ppm; then melt spinning is carried out at a spinning temperature of 245°C, a box temperature of 250°C, a heat deformation temperature of 220°C, a drafting multiple of 3.0 times, a network degree of 30 / m, a clover-shaped spinneret with an aperture of 0.8mm, a number of holes of 48, a spinning specification of 1500D / 48, a single yarn fineness of 30dtex, and a spinning speed of 1200m / min to obtain a nascent yarn; after the nascent yarn is fully expanded, it is wound to obtain a bio-based furan polyester expanded continuous filament.

[0083] Example 6

[0084] The bio-based furan polyester bulked continuous filament provided in this embodiment is prepared by the following steps:

[0085] 1500g of 2,5-furandicarboxylic acid, 1463g of bio-based 1,3-propylene glycol, 1.5g of antioxidant B215 and 0.5g of zinc acetate were added to the polymerization kettle. After the feeding was completed, the kettle was sealed and the air in the kettle was replaced by nitrogen through vacuum pumping. This was repeated 3 times. Finally, nitrogen was filled as a protective gas at a pressure of 25kPa. Then, the circulating heat medium was started to start heating and stirring was started at the same time.

[0086] The esterification reaction begins. During the esterification process, the temperature is controlled at 180-190°C. The esterification time is about 2 hours. When the water output reaches 95% of the theoretical value and no more output occurs, the esterification reaction is completed.

[0087] Add 1.0 g of ethylene glycol antimony and 0.5 g of phosphoric acid to the esterification reaction product, and react at normal pressure for 10 min after nitrogen replacement; then carry out negative pressure pre-polycondensation reaction, the reaction temperature is controlled at 230° C., the reaction time is 1 h, and the pressure in the autoclave is less than 0 MPa; then carry out final polycondensation reaction, the reaction temperature is 260° C., the time is 4 h, and the vacuum degree is ≤70 Pa; after the melt reaches the viscosity requirement, stop stirring, introduce nitrogen to normal pressure, and then stand for 3 min, introduce nitrogen again to discharge and granulate, and obtain bio-based furan polyester chips;

[0088] The obtained bio-based furan polyester chips are taken and dried in a drum oven at a temperature of 110°C and a drying time of 12 hours until the moisture content is ≤100ppm; then melt spinning is carried out at a spinning temperature of 240°C, a box temperature of 250°C, a heat deformation temperature of 210°C, a drafting multiple of 3.0 times, a network degree of 30 / m, a clover-shaped spinneret with an aperture of 0.8mm, a number of holes of 48, a spinning specification of 1500D / 48, a single yarn fineness of 30dtex, and a spinning speed of 1200m / min to obtain a nascent yarn; after the nascent yarn is fully expanded, it is wound to obtain a bio-based furan polyester expanded continuous filament.

[0089] Example 7

[0090] The bio-based furan polyester bulked continuous filament provided in this embodiment is prepared by the following steps:

[0091] 1500g of 2,5-furandicarboxylic acid, 1463g of bio-based 1,3-propylene glycol, 1.5g of antioxidant B215 and 0.5g of germanium oxide were added to the polymerization kettle. After the feeding was completed, the kettle was sealed and the air in the kettle was replaced by nitrogen through vacuum pumping. This was repeated 3 times. Finally, nitrogen was filled as a protective gas at a pressure of 25kPa. After that, the circulating heat medium was started to start heating and stirring was started at the same time.

[0092] The esterification reaction begins. During the esterification process, the temperature is controlled at 180-190°C. The esterification time is about 2 hours. When the water output reaches 95% of the theoretical value and no more output occurs, the esterification reaction is completed.

[0093] 1.0 g of tetrabutyl titanate and 0.5 g of phosphoric acid were added to the esterification reaction product, and the mixture was reacted at normal pressure for 10 min after nitrogen substitution; then a negative pressure pre-polycondensation reaction was carried out, the reaction temperature was controlled at 230° C., the reaction time was 1 h, and the pressure in the autoclave was less than 0 MPa; then a final polycondensation reaction was carried out, the reaction temperature was 260° C., the reaction time was 4 h, and the vacuum degree was ≤70 Pa; after the melt reached the viscosity requirement, stirring was stopped, nitrogen was introduced to normal pressure, and then the mixture was allowed to stand for 3 min, and nitrogen was introduced again to discharge and granulate the mixture to obtain bio-based furan polyester chips;

[0094] The obtained bio-based furan polyester chips are taken and dried in a drum oven at a temperature of 110°C and a drying time of 12 hours until the moisture content is ≤100ppm; then melt spinning is carried out at a spinning temperature of 240°C, a box temperature of 250°C, a heat deformation temperature of 210°C, a drafting multiple of 3.0 times, a network degree of 30 / m, a clover-shaped spinneret with an aperture of 0.8mm, a number of holes of 48, a spinning specification of 1500D / 48, a single yarn fineness of 30dtex, and a spinning speed of 1200m / min to obtain a nascent yarn; after the nascent yarn is fully expanded, it is wound to obtain a bio-based furan polyester expanded continuous filament.

[0095] Example 8

[0096] The bio-based furan polyester bulked continuous filament provided in this embodiment is prepared by the following steps:

[0097] 1500g of 2,5-furandicarboxylic acid, 1463g of bio-based 1,3-propylene glycol, 1.5g of antioxidant B215 and 0.5g of zinc acetate were added to the polymerization kettle. After the feeding was completed, the kettle was sealed and the air in the kettle was replaced by nitrogen through vacuum pumping. This was repeated 3 times. Finally, nitrogen was filled as a protective gas at a pressure of 25kPa. Then, the circulating heat medium was started to start heating and stirring was started at the same time.

[0098] The esterification reaction begins. During the esterification process, the temperature is controlled at 180-190°C. The esterification time is about 2 hours. When the water output reaches 95% of the theoretical value and no more output occurs, the esterification reaction is completed.

[0099] 1.0 g of tetrabutyl titanate and 0.5 g of phosphoric acid were added to the esterification reaction product, and the mixture was reacted at normal pressure for 10 min after nitrogen substitution; then a negative pressure pre-polycondensation reaction was carried out, the reaction temperature was controlled at 230° C., the reaction time was 1 h, and the pressure in the autoclave was less than 0 MPa; then a final polycondensation reaction was carried out, the reaction temperature was 260° C., the reaction time was 4 h, and the vacuum degree was ≤70 Pa; after the melt reached the viscosity requirement, stirring was stopped, nitrogen was introduced to normal pressure, and then the mixture was allowed to stand for 3 min, and nitrogen was introduced again to discharge and granulate the mixture to obtain bio-based furan polyester chips;

[0100] The obtained bio-based furan polyester chips are dried in a drum oven at a temperature of 110°C and a drying time of 12 hours until the moisture content is ≤100ppm; then melt spinning is carried out at a spinning temperature of 240°C, a box temperature of 250°C, a heat deformation temperature of 200°C, a drafting multiple of 3.0 times, a network degree of 30 / m, a clover-shaped spinneret with an aperture of 0.8mm, a number of holes of 48, a spinning specification of 1500D / 48, a single yarn fineness of 30dtex, and a spinning speed of 1200m / min to obtain nascent yarns; after the nascent yarns are fully expanded, they are wound to obtain bio-based furan polyester expanded continuous filaments.

[0101] Example 9

[0102] The bio-based furan polyester bulked continuous filament provided in this embodiment is prepared by the following steps:

[0103] 1500g of 2,5-furandicarboxylic acid, 1463g of bio-based 1,3-propylene glycol, 1.5g of antioxidant B215 and 0.5g of zinc acetate were added to the polymerization kettle. After the feeding was completed, the kettle was sealed and the air in the kettle was replaced by nitrogen through vacuum pumping. This was repeated 3 times. Finally, nitrogen was filled as a protective gas at a pressure of 25kPa. Then, the circulating heat medium was started to start heating and stirring was started at the same time.

[0104] The esterification reaction begins. During the esterification process, the temperature is controlled at 180-190°C. The esterification time is about 2 hours. When the water output reaches 95% of the theoretical value and no more output occurs, the esterification reaction is completed.

[0105] 1.0 g of tetrabutyl titanate and 0.5 g of phosphoric acid were added to the esterification reaction product, and the mixture was reacted at normal pressure for 10 min after nitrogen substitution; then a negative pressure pre-polycondensation reaction was carried out, the reaction temperature was controlled at 230° C., the reaction time was 1 h, and the pressure in the autoclave was less than 0 MPa; then a final polycondensation reaction was carried out, the reaction temperature was 260° C., the reaction time was 4 h, and the vacuum degree was ≤70 Pa; after the melt reached the viscosity requirement, stirring was stopped, nitrogen was introduced to normal pressure, and then the mixture was allowed to stand for 3 min, and nitrogen was introduced again to discharge and granulate the mixture to obtain bio-based furan polyester chips;

[0106] The obtained bio-based furan polyester chips are taken and dried in a drum oven at a temperature of 110°C and a drying time of 12 hours until the moisture content is ≤100ppm; then melt spinning is carried out at a spinning temperature of 240°C, a box temperature of 250°C, a heat deformation temperature of 220°C, a drafting multiple of 3.0 times, a network degree of 30 / m, a clover-shaped spinneret with an aperture of 0.8mm, a number of holes of 48, a spinning specification of 1500D / 48, a single yarn fineness of 30dtex, and a spinning speed of 1200m / min to obtain a nascent yarn; after the nascent yarn is fully expanded, it is wound to obtain a bio-based furan polyester expanded continuous filament.

[0107] Example 10

[0108] The bio-based furan polyester bulked continuous filament provided in this embodiment is prepared by the following steps:

[0109] 1500g of 2,5-furandicarboxylic acid, 1463g of bio-based 1,3-propylene glycol, 1.5g of antioxidant B215 and 0.5g of zinc acetate were added to the polymerization kettle. After the feeding was completed, the kettle was sealed and the air in the kettle was replaced by nitrogen through vacuum pumping. This was repeated 3 times. Finally, nitrogen was filled as a protective gas at a pressure of 25kPa. Then, the circulating heat medium was started to start heating and stirring was started at the same time.

[0110] The esterification reaction begins. During the esterification process, the temperature is controlled at 180-190°C. The esterification time is about 2 hours. When the water output reaches 95% of the theoretical value and no more output occurs, the esterification reaction is completed.

[0111] 1.0 g of tetrabutyl titanate and 0.5 g of phosphoric acid were added to the esterification reaction product, and the mixture was reacted at normal pressure for 10 min after nitrogen substitution; then a negative pressure pre-polycondensation reaction was carried out, the reaction temperature was controlled at 230° C., the reaction time was 1 h, and the pressure in the autoclave was less than 0 MPa; then a final polycondensation reaction was carried out, the reaction temperature was 260° C., the reaction time was 4 h, and the vacuum degree was ≤70 Pa; after the melt reached the viscosity requirement, stirring was stopped, nitrogen was introduced to normal pressure, and then the mixture was allowed to stand for 3 min, and nitrogen was introduced again to discharge and granulate the mixture to obtain bio-based furan polyester chips;

[0112] The obtained bio-based furan polyester chips are taken and dried in a drum oven at a temperature of 110°C and a drying time of 12 hours until the moisture content is ≤100ppm; then melt spinning is carried out at a spinning temperature of 240°C, a box temperature of 250°C, a heat deformation temperature of 210°C, a drafting multiple of 4.0 times, a network degree of 30 / m, a clover-shaped spinneret with an aperture of 0.8mm, a number of holes of 48, a spinning specification of 1500D / 48, a single yarn fineness of 30dtex, and a spinning speed of 1200m / min to obtain a nascent yarn; after the nascent yarn is fully expanded, it is wound to obtain a bio-based furan polyester expanded continuous filament.

[0113] Embodiment 11

[0114] The bio-based furan polyester bulked continuous filament provided in this embodiment is prepared by the following steps:

[0115] 1500g of 2,5-furandicarboxylic acid, 1463g of bio-based 1,3-propylene glycol, 1.5g of antioxidant B215 and 0.5g of zinc acetate were added to the polymerization kettle. After the feeding was completed, the kettle was sealed and the air in the kettle was replaced by nitrogen through vacuum pumping. This was repeated 3 times. Finally, nitrogen was filled as a protective gas at a pressure of 25kPa. Then, the circulating heat medium was started to start heating and stirring was started at the same time.

[0116] The esterification reaction begins. During the esterification process, the temperature is controlled at 180-190°C. The esterification time is about 2 hours. When the water output reaches 95% of the theoretical value and no more output occurs, the esterification reaction is completed.

[0117] 1.0 g of tetrabutyl titanate and 0.5 g of phosphoric acid were added to the esterification reaction product, and the mixture was reacted at normal pressure for 10 min after nitrogen substitution; then a negative pressure pre-polycondensation reaction was carried out, the reaction temperature was controlled at 230° C., the reaction time was 1 h, and the pressure in the autoclave was less than 0 MPa; then a final polycondensation reaction was carried out, the reaction temperature was 260° C., the reaction time was 4 h, and the vacuum degree was ≤70 Pa; after the melt reached the viscosity requirement, stirring was stopped, nitrogen was introduced to normal pressure, and then the mixture was allowed to stand for 3 min, and nitrogen was introduced again to discharge and granulate the mixture to obtain bio-based furan polyester chips;

[0118] The obtained bio-based furan polyester chips are taken and dried in a drum oven at a temperature of 110°C and a drying time of 12 hours until the moisture content is ≤100ppm; then melt spinning is carried out at a spinning temperature of 240°C, a box temperature of 250°C, a heat deformation temperature of 210°C, a drafting multiple of 3.5 times, a network degree of 30 / m, a clover-shaped spinneret with an aperture of 0.8mm, a number of holes of 48, a spinning specification of 1500D / 48, a single yarn fineness of 30dtex, and a spinning speed of 1200m / min to obtain a nascent yarn; after the nascent yarn is fully expanded, it is wound to obtain a bio-based furan polyester expanded continuous filament.

[0119] Example 12

[0120] The bio-based furan polyester bulked continuous filament provided in this embodiment is prepared by the following steps:

[0121] 1500g of 2,5-furandicarboxylic acid, 1463g of bio-based 1,3-propylene glycol, 1.5g of antioxidant B215 and 0.5g of zinc acetate were added to the polymerization kettle. After the feeding was completed, the kettle was sealed and the air in the kettle was replaced by nitrogen through vacuum pumping. This was repeated 3 times. Finally, nitrogen was filled as a protective gas at a pressure of 25kPa. Then, the circulating heat medium was started to start heating and stirring was started at the same time.

[0122] The esterification reaction begins. During the esterification process, the temperature is controlled at 180-190°C. The esterification time is about 2 hours. When the water output reaches 95% of the theoretical value and no more output occurs, the esterification reaction is completed.

[0123] 1.0 g of tetrabutyl titanate and 0.5 g of phosphoric acid were added to the esterification reaction product, and the mixture was reacted at normal pressure for 10 min after nitrogen substitution; then a negative pressure pre-polycondensation reaction was carried out, the reaction temperature was controlled at 230° C., the reaction time was 1 h, and the pressure in the autoclave was less than 0 MPa; then a final polycondensation reaction was carried out, the reaction temperature was 260° C., the reaction time was 4 h, and the vacuum degree was ≤70 Pa; after the melt reached the viscosity requirement, stirring was stopped, nitrogen was introduced to normal pressure, and then the mixture was allowed to stand for 3 min, and nitrogen was introduced again to discharge and granulate the mixture to obtain bio-based furan polyester chips;

[0124] The obtained bio-based furan polyester chips are taken and dried in a drum oven at a temperature of 110°C and a drying time of 12 hours until the moisture content is ≤100ppm; then melt spinning is carried out at a spinning temperature of 240°C, a box temperature of 250°C, a heat deformation temperature of 210°C, a drafting multiple of 2.5 times, a network degree of 30 / m, a clover-shaped spinneret with an aperture of 0.8mm, a hole number of 48, a spinning specification of 1500D / 48, a single yarn fineness of 30dtex, and a spinning speed of 1200m / min to obtain a nascent yarn; after the nascent yarn is fully expanded, it is wound to obtain a bio-based furan polyester expanded continuous filament.

[0125] Example 13

[0126] The bio-based furan polyester bulked continuous filament provided in this embodiment is prepared by the following steps:

[0127] 1500g of 2,5-furandicarboxylic acid, 1463g of bio-based 1,3-propylene glycol, 1.5g of antioxidant B215 and 0.5g of zinc acetate were added to the polymerization kettle. After the feeding was completed, the kettle was sealed and the air in the kettle was replaced by nitrogen through vacuum pumping. This was repeated 3 times. Finally, nitrogen was filled as a protective gas at a pressure of 25kPa. Then, the circulating heat medium was started to start heating and stirring was started at the same time.

[0128] The esterification reaction begins. During the esterification process, the temperature is controlled at 180-190°C. The esterification time is about 2 hours. When the water output reaches 95% of the theoretical value and no more output occurs, the esterification reaction is completed.

[0129] 1.0 g of tetrabutyl titanate and 0.5 g of phosphoric acid were added to the esterification reaction product, and the mixture was reacted at normal pressure for 10 min after nitrogen substitution; then a negative pressure pre-polycondensation reaction was carried out, the reaction temperature was controlled at 230° C., the reaction time was 1 h, and the pressure in the autoclave was less than 0 MPa; then a final polycondensation reaction was carried out, the reaction temperature was 260° C., the reaction time was 4 h, and the vacuum degree was ≤70 Pa; after the melt reached the viscosity requirement, stirring was stopped, nitrogen was introduced to normal pressure, and then the mixture was allowed to stand for 3 min, and nitrogen was introduced again to discharge and granulate the mixture to obtain bio-based furan polyester chips;

[0130] The obtained bio-based furan polyester chips are dried in a drum oven at a temperature of 110°C and a drying time of 12 hours until the moisture content is ≤100ppm; then melt spinning is carried out at a spinning temperature of 240°C, a box temperature of 250°C, a heat deformation temperature of 210°C, a drafting multiple of 3.0 times, a network density of 30 / m, a hollow eccentric spinneret, a pore size of 0.8mm, a number of holes of 48, a spinning specification of 1500D / 48, a single yarn fineness of 30dtex, and a spinning speed of 1200m / min to obtain nascent yarns; after the nascent yarns are fully expanded, they are wound to obtain bio-based furan polyester expanded continuous filaments.

[0131] Comparative Example 1

[0132] This comparative example provides a polyester bulked continuous filament, the preparation steps of which are:

[0133] 1500g of terephthalic acid, 1374g of bio-based 1,3-propylene glycol, 1.5g of antioxidant B215 and 0.5g of zinc acetate were added to the polymerization kettle. After the feeding was completed, the kettle was sealed and the air in the kettle was replaced by nitrogen through vacuum pumping. This was repeated 3 times. Finally, nitrogen was filled as a protective gas at a pressure of 25kPa. Then, the circulating heat medium was started to start heating and stirring was started at the same time.

[0134] The esterification reaction begins. During the esterification process, the temperature is controlled at 200-220°C. The esterification time is about 2 hours. When the water output reaches 95% of the theoretical value and no more output occurs, the esterification reaction is completed.

[0135] Add 1.0 g of tetrabutyl titanate and 0.5 g of phosphoric acid to the esterification reaction product, and react at normal pressure for 10 min after nitrogen replacement; then carry out negative pressure pre-polycondensation reaction, the reaction temperature is controlled to 230° C., the reaction time is 1 h, and the pressure in the autoclave is less than 0 MPa; then carry out final polycondensation reaction, the reaction temperature is 260° C., the time is 4 h, and the vacuum degree is ≤70 Pa; after the melt reaches the viscosity requirement, stop stirring, introduce nitrogen to normal pressure, and then stand for 3 min, introduce nitrogen again to discharge and granulate to obtain polyester chips;

[0136] The obtained polyester chips are dried in a drum oven at a temperature of 110°C and a drying time of 12 hours until the moisture content is ≤100ppm; then melt spinning is carried out at a spinning temperature of 240°C, a box temperature of 250°C, a heat deformation temperature of 210°C, a drafting multiple of 3.0 times, a network degree of 30 / m, a clover-shaped spinneret with an aperture of 0.8mm, a number of holes of 48, a spinning specification of 1500D / 48, a single yarn fineness of 30dtex, and a spinning speed of 1200m / min to obtain nascent yarns; the nascent yarns are fully expanded and then wound to obtain polyester bulked continuous filaments.

[0137] Performance Testing

[0138] The bulked continuous filaments (BCF) obtained from the above examples and comparative examples were subjected to performance tests, and the test items and methods are as follows.

[0139] The intrinsic viscosity is tested with reference to GB / T 14190-2017.

[0140] The boiling water shrinkage rate is tested in accordance with GB / T6505-2017.

[0141] Mechanical properties: Use an electronic single yarn strength tester to test the BCF monofilament strength and elongation. Use a clamp to fix the yarn, input the yarn fineness, set the initial length of the clamp to 20 cm, and the stretching speed to 25 cm / min. The final result is based on the average value of 5 measurement data.

[0142] Thermal curling rate: 10m of yarn is wound by a yarn length measuring machine, and then it is taken down and wound into an "8"-shaped tow. The tow is fixed on the upper end of a vertical ruler, and a certain mass of weight is hung on the lower end. A pre-tension of 0.2±0.02cN / dtex is applied to it. After standing for 30s, the fiber length L is read. 0 ; Then place it in a vacuum drying oven, set the temperature to 150°C, take it out after 15 minutes, and use the same method to measure the length La of the tow at this time; the thermal curvature of the fiber is calculated according to the following formula:

[0143]

[0144] Dye uptake: The absorbance of the residual dyeing liquid and the original dyeing liquid after dyeing is measured by UV-2600 spectrophotometer. The formula for calculating the dye uptake is:

[0145]

[0146] Among them, Aa is the absorbance of the dyeing residual solution, A 0 is the absorbance of the dye stock solution.

[0147] The performance test results of the bulked continuous filaments (BCF) obtained in Examples 1-13 and Comparative Example 1 are shown in Table 1.

[0148] Table 1

[0149]

[0150] In Examples 1-5, different bio-based diols were used to synthesize the corresponding polyester raw materials, and then further melt-spinning and puffing treatment were performed to obtain BCF. The bio-based furan polyester obtained in Example 1 was measured by GPC, and the GPC spectrum of the obtained bio-based furan polyester is shown in Figure 1 The number average relative molecular weight of the bio-based furan polyester obtained in Example 1 is 17546, the weight average molecular weight is 29489, and the distribution index is 1.68. In Example 3, the bio-based diol is 1,5-pentanediol, and the synthesized bio-based furan polyester has a relatively low intrinsic viscosity. In Example 4, the bio-based diol is 2,5-tetrahydrofuran dimethanol, and the synthesized bio-based furan polyester has a relatively high intrinsic viscosity.

[0151] In Examples 6-7, the polycondensation catalyst or the esterification catalyst was replaced respectively. It can be seen from the intrinsic viscosity and the performance indicators of the expanded continuous filament in Table 1 that antimony ethylene glycol and germanium oxide also have good catalytic effects in the synthesis of bio-based furan polyester.

[0152] Examples 8-12 investigated the spinning process during the preparation of bio-based furan polyester bulked continuous filaments, mainly investigating the effects of heat deformation temperature and draft ratio on BCF.

[0153] It can be seen from Table 1 that as the heat deformation temperature increases, the curling rate increases, but the breaking strength and elongation both decrease. If the heat deformation temperature is too low, the expansion degree is poor and the curling rate decreases.

[0154] It can also be seen from Table 1 that the increase in the draft ratio makes the macromolecular chains or segments inside the yarn preferentially arranged along the direction of the external force field, increasing the orientation of the fiber and inducing its crystallization, so the breaking strength and thermal curling rate of the bulked continuous filament increase, while the draft ratio is insufficient, the mechanical strength is poor, and the curling rate is insufficient. The draft ratio is preferably 3.0-4.0.

[0155] In Example 13, a hollow eccentric spinneret was selected, and the prepared expanded continuous filaments had higher thermal curling performance and the dyeing rate of the two dyes was also improved.

[0156] In summary, by comparing Examples 1-13 with Comparative Example 1, it can be clearly seen that the bio-based furan polyester bulked continuous filaments of the present invention have excellent mechanical properties, thermal curling rate and boiling water shrinkage rate, and show a high dyeing rate for cationic dyes and disperse dyes; at the same time, the polymerization process in the present invention can make the intrinsic viscosity of the bio-based furan polyester meet the spinning requirements. The bio-based furan polyester bulked continuous filaments provided by the present invention are suitable for the production of floor coverings or carpets.

[0157] Although the present invention has been described in detail above by means of general description, specific implementation methods and tests, it is obvious to those skilled in the art that some modifications or improvements may be made to the present invention. Therefore, these modifications or improvements made without departing from the spirit of the present invention all fall within the scope of protection claimed by the present invention.

Claims

1. A bio-based furan polyester bulked continuous filament, characterized in that: Bio-based furan polyester is used as raw material and is prepared by melt spinning and puffing treatment; wherein the bio-based furan polyester is obtained by esterification and polycondensation of 2,5-furandicarboxylic acid and bio-based diol; In the melt spinning, the heat deformation temperature is 200-220°C, and the drafting ratio is 3.0-4.0 times; a clover-shaped or hollow eccentric spinneret is used in the spinning assembly; The raw materials for preparing 2,5-furandicarboxylic acid are non-grain crops, and the purity is ≥99.9wt%; The bio-based diol is selected from one or more of bio-based ethylene glycol, 1,3-propylene glycol, 1,4-butanediol, 2,3-butanediol, 1,2-pentanediol, 1,5-pentanediol, 2,5-furan dimethanol, and 2,5-tetrahydrofuran dimethanol; the molar ratio of 2,5-furandicarboxylic acid and bio-based diol monomer is: 2,5-furandicarboxylic acid: bio-based diol = 1: (1.4~2.2).

2. The bio-based furan polyester bulked continuous filament according to claim 1, characterized in that: The single filament fineness of the bio-based furan polyester bulked continuous filament is 1-50 dtex.

3. The bio-based furan polyester bulked continuous filament according to claim 1, characterized in that: In the melt spinning, the spinning temperature is 240-280° C., the network density is 20-40 / m, the spinning speed is 500-2000 m / min; the hole diameter of the spinneret is 0.5-1.5 mm, and the number of holes is 36-96.

4. The bio-based furan polyester bulked continuous filament according to claim 3, characterized in that: The spinning speed is 1000-1500 m / min; the hole diameter of the spinneret is 0.5-1.5 mm, and the number of holes is 48.

5. The bio-based furan polyester bulked continuous filament according to claim 1, characterized in that: The temperature of the esterification reaction of 2,5-furandicarboxylic acid and bio-based diol is 170-220° C.; During the esterification reaction, an antioxidant and an esterification catalyst are added to the reaction system; the antioxidant is at least one of antioxidant 1010, antioxidant SEED, and antioxidant B215; the amount of the antioxidant added is 0.05% to 0.5% of the mass of the 2,5-furandicarboxylic acid; The esterification catalyst is selected from metal acetate and germanium oxide, wherein the metal acetate is selected from at least one of zinc acetate, manganese acetate and cadmium acetate; the added amount of the esterification catalyst is 0.01% to 0.1% of the mass of the 2,5-furandicarboxylic acid.

6. The bio-based furan polyester bulked continuous filament according to claim 5, characterized in that: The esterification reaction product of 2,5-furandicarboxylic acid and bio-based diol is polycondensed to prepare bio-based furan polyester; Add a heat stabilizer and a polycondensation catalyst to the esterification reaction product of 2,5-furandicarboxylic acid and bio-based diol, react at normal pressure for 5 to 10 minutes, and then perform a polycondensation reaction; The heat stabilizer is selected from at least one of phosphoric acid, phosphorous acid, hypophosphorous acid, triphenyl phosphate, diphenyl phosphate, triphenyl phosphite, diphenyl phosphorus, ammonium phosphite, and diammonium phosphate; the amount of the heat stabilizer added is 0.005% to 0.1% of the mass of the 2,5-furandicarboxylic acid; The polycondensation catalyst is selected from at least one of antimony trioxide, antimony glycol, titanium dioxide, tetrabutyl titanate, and tetraethyl titanate; and the amount of the polycondensation catalyst added is 0.01% to 0.1% of the mass of the 2,5-furandicarboxylic acid.

7. The bio-based furan polyester bulked continuous filament according to claim 6, characterized in that: The polycondensation includes a pre-polycondensation treatment and a final polycondensation treatment, wherein the pre-polycondensation treatment is firstly performed and then the final polycondensation treatment is performed to obtain the bio-based furan polyester; The reaction temperature of the pre-polycondensation treatment is 230-250°C, the pressure is less than 0 MPa, and the reaction time is 0.5-1 h; the reaction temperature of the final polycondensation treatment is 240-260°C, the vacuum degree is ≤70 Pa, and the reaction time is 2-5 h; The intrinsic viscosity of the prepared bio-based furan polyester is 0.63-0.85 dl / g.

8. The bio-based furan polyester bulked continuous filament according to claim 7, characterized in that: The bio-based furan polyester is discharged and granulated to obtain bio-based furan polyester chips; the bio-based furan polyester chips are dried and used as raw materials to prepare bio-based furan polyester bulked continuous filaments through melt spinning and puffing; the drying temperature is 100-150° C., and the drying time is 4-12 hours.

9. Use of the bio-based furan polyester bulked continuous filament according to any one of claims 1 to 8 as a raw material for making floor coverings.

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