Method for producing recycled resin

Abstract

To provide a method for producing a recycled resin, which can reduce volatile components in the recycled resin.SOLUTION: A method for producing a recycled resin includes the steps of: feeding crushed raw materials for recycling, which contains volatile components and resin for recycling, into a filling tank; and washing the crushed raw materials for recycling by distributing steam in a filling tank. A temperature in the filling tank is between 100°C and 115°C, and a processing time for the step of washing the crushed material is 150 minutes or longer.SELECTED DRAWING: None

Description

[Technical field]

[0001] The present invention relates to a method for producing recycled resin. [Background technology]

[0002] Plastic bottles have traditionally been used as packaging containers for liquid ingredients such as shampoo, fabric softener, and beverages, and solid ingredients such as food. Many of these plastic bottles are made of materials containing polyolefins, making them eligible for recycling.

[0003] For example, Patent Document 1 describes an invention of a cleaning method and device for recycling waste plastic materials. Paragraph 0033 of Patent Document 1 attempts to reduce the odor generated by waste plastics by contacting the waste plastics with steam for 2 seconds to clean them. [Prior art documents] [Patent documents]

[0004] [Patent Document 1] JP 2003-251627 A Summary of the Invention [Problem to be solved by the invention]

[0005] Many of the shampoos and fabric softeners available today are characterized by their strong residual fragrance. Various fragrances remain in the packaging containers in which such products are enclosed, and this tendency is particularly strong in packaging containers of filling bottles made of polyolefin, and the method of Patent Document 1 was insufficient in reducing the odor caused by the fragrance. Therefore, further improvements in the method for reducing volatile components such as fragrances have been desired.

[0006] The present invention relates to a method for producing recycled resin, which reduces the volatile components in the recycled resin. [Means for solving the problem]

[0007] The present invention relates to the following [1] to

[10] . [1] A method for producing recycled resin, comprising the steps of: supplying crushed raw material for recycling, which contains volatile components and resin for recycling, to a filling tank; and circulating steam through the filling tank to wash the crushed raw material for recycling, wherein the temperature in the filling tank is 100°C or higher and 115°C or lower, and the processing time for the step of washing the crushed material is 150 minutes or longer. [2] The manufacturing method described in [1] above, wherein the crushed material for recycling is obtained through a crushing process for crushing the raw material for recycling. [3] The manufacturing method according to [1] above, wherein the crushed material for recycling is obtained through a crushing process for crushing the raw material for recycling, and then through a washing process for washing the resultant material with water. [4] The method according to any one of the above [1] to [3], wherein the linear velocity of the water vapor flowing through the packed vessel is 0.04 m / s or more and 0.75 m / s or less. [5] The method according to any one of the above [1] to [4], wherein the volatile component comprises a fragrance. [6] The manufacturing method according to any one of the above [1] to [5], wherein the particle size distribution of the crushed material for recycling is 1 mm or more and 15 mm or less, and the median diameter is 3 mm or more and 12 mm or less. [7] The manufacturing method according to any one of the above [1] to [6], wherein the filling rate of the crushed material for recycling in the filling tank is 30 to 100%. [8] The manufacturing method according to any one of the above [1] to [7], wherein the crushed material for regeneration in the filling tank is washed in a batch manner. [9] The manufacturing method according to any one of the above [1] to [8], wherein the raw material for recycling includes packaging containers of plastic bottles.

[10] A recycled resin produced by the production method according to any one of [1] to [9] above. Effect of the Invention

[0008] According to the present invention, there is provided a method for producing recycled resin, which reduces the volatile components in the recycled resin. [Brief description of the drawings]

[0009] [Figure 1] FIG. 1 is a schematic diagram of the device (steam treatment device) used in Example 1 for washing the crushed material for recycling. DETAILED DESCRIPTION OF THE PREFERRED EMBODIMENTS

[0010] The method for producing recycled resin of the present invention includes a step of supplying crushed raw material for recycling, which contains volatile components and resin for recycling, to a filling tank, and a step of washing the crushed raw material for recycling by circulating water vapor through the filling tank, wherein the temperature in the filling tank is 100°C or higher and 115°C or lower, and the processing time for the step of washing the crushed material is 150 minutes or longer.

[0011] The recycled raw material in the present invention includes a volatile component and a recycled resin. Examples of the recycled raw material include packaging containers used for compositions containing volatile components (e.g., shampoos, fabric softeners, laundry detergents, body soaps, household cleaners, etc.). Examples of such general packaging containers include plastic bottles.

[0012] Bottles often contain polyolefins and are a preferred example of the raw material for recycling in the present invention.

[0013] The packaging containers to which the present invention is directed are usually used, but may be entirely or partially unused.

[0014] The volatile component in the present invention may be one or more of a fragrance, a medicine, an agricultural chemical, a solvent, and the like. The fragrance in the present invention includes fragrances blended in laundry detergents and laundry softeners. From the viewpoint of removability, fragrances containing fragrances having a CLogP value of, for example, 0.1 to 7 are suitable for removal.

[0015] Here, the LogP value is a coefficient indicating the affinity of a compound to water and 1-octanol. The 1-octanol / water partition coefficient P is the ratio of the equilibrium concentration of a compound in each solvent when a trace amount of a compound is dissolved as a solute in a solvent consisting of two liquid phases, 1-octanol and water, and reaches distribution equilibrium, and is generally expressed in the form of their logarithm LogP to the base 10. Nowadays, the value of "calculated LogP (CLogP)" calculated by a calculation program using the fragment value of the atomic group determined by the number of atoms constituting the compound molecule and the type of chemical bond is widely used. In this specification, the value of CLogP is calculated using the software EPI Suite (registered trademark; The Estimations Programs Interface for Windows version 4.11) jointly developed by the United States Environmental Protection Agency and Syracuse, Inc. The larger the CLogP value, the higher the fat solubility.

[0016] The perfume in the present invention includes perfumes that are blended in laundry detergents and fabric softeners. Preferred perfumes to be removed include acetyl cedrene (ClogP value: 5.0), aldehyde C-6 (ClogP value: 1.8), aldehyde C-10 (ClogP value: 3.8), aldehyde C-14 (ClogP value: 3.1), aldehyde C-16 (ClogP value: 3.0), allyl amyl glycolate (ClogP value: 2.3), α-Damascone (ClogP value: 4.3), amyl salicylate (ClogP value: 4.6), amber core (Amber core), and aldehyde C-10 (ClogP value: 3.8). core, ClogP value: 4.1), Ambroxan, ClogP value: 4.8, Amyl cinnamic aldehyde, ClogP value: 4.3, Anis aldehyde, ClogP value: 1.8, Benzyl acetate, ClogP value: 2.1, Benzyl alcohol, ClogP value: 1.1, Benzyl benzoate, ClogP value: 3.5, Benzyl salicylate, ClogP value: 4.3, β-Damascone, ClogP value: 4.4, β-Pinene, ClogP value: 4.4, Boisambrene forte forte, ClogP value: 5.5), Calone, ClogP value: 2.4, Canthoxal, ClogP value: 2.5, Cedryl methyl ether, ClogP value: 5.0, cis-3-Hexenol, ClogP value: 1.6, cis-3-Hexenyl acetate, ClogP value: 2.6, cis-3-Hexenyl benzoate, ClogP value: 4.1), cis-3-Hexenyl hexanoate (ClogP value: 4.6), cis-3-Hexenyl salicylate (ClogP value: 4.8), Citral (ClogP value: 3.5), Citronellol (ClogP value: 3.6), Citronellyl acetate (ClogP value: 4.6), Citronellyl nitrile (ClogP value: 3.6), Coumarin (ClogP value: 1.5), Cyclohexyl salicylate (ClogP value: 4.8), salicilate, ClogP value: 4.9), Cyclotene, ClogP value: 1.3, Damascenone, ClogP value: 4.2, δ-Damascone, ClogP value: 4.2, Dihydro myrcenol, ClogP value: 3.6, Diphenyl oxide, ClogP value: 4.1, Dynascone, ClogP value: 4.5, Ethyl acetate, ClogP value: 0.86, Ethyl butyrate, ClogP value: 1.9, Ethyl maltol, ClogP value: 0.30, Ethyl 2-methylbutyrate, ClogP value: 2.3, Ethyl vanillin vanilin, ClogP value: 1.6), Ethylene brassylate, ClogP value: 4.7, Eugenol, ClogP value: 2.7, Farnesol, ClogP value: 5.8, Floralozone, ClogP value: 3.9, Floramat, ClogP value: 4.8, Floropal, ClogP value: 3.1, Fructone, ClogP value: 1.3, Fruitate, ClogP value: 3.6, γ-Terpinene, ClogP value: 4.8), Geraniol (ClogP value: 3.5), Geranyl acetate (ClogP value: 4.5), Geranyl propionate (ClogP value: 5.0), Helional (ClogP value: 2.5), Heliotropine (ClogP value: 1.8), Hexyl acetate (ClogP value: 2.8), Hexyl cinnamic aldehyde (ClogP value: 4.8), Hexyl salicylate (ClogP value: 5.1), Hydroxy citronellal (ClogP value: 2.1), Indoflor crystal (ClogP value: 2.1), crystal, ClogP value: 1.8), Indol, ClogP value: 2.1, Ionone alpha, ClogP value: 4.3, Ionone beta, ClogP value: 4.4, Iso-Amyl acetate, ClogP value: 2.3, Iso-Amyl salicylate, ClogP value: 4.5, Iso E super, ClogP value: 5.2, Iso-Longiforanone, ClogP value: 3.8, Lactone C-10 gamma, ClogP value: 2.6, Lactone C-11 gamma, ClogP value: 3.0, Lactone C-12 delta delta, ClogP value: 3.6), Lactone C-12 gamma, ClogP value: 3.6, Lemonile, ClogP value: 4.0, Ligustral SB, ClogP value: 4.8, Lilar, ClogP value: 3.3, Lilial, ClogP value: 4.4, Limonene, ClogP value: 4.8, Linalool, ClogP value: 3.4), Linalool oxide, ClogP value: 2.0, Linalyl acetate, ClogP value: 4.4, Manzanate, ClogP value: 2.8, Mayol, ClogP value: 3.5, l-Menthol, ClogP value: 3.4, l-Menthone, ClogP value: 2.9, Methyl dihydrojasmonate, ClogP value: 3.5, Methyl ionone-G, ClogP value: 4.8, Methyl jasmonate, ClogP value: 2.8, Musk C-14 C-14, ClogP value: 4.2), Nectaryl, ClogP value: 5.1, Nerol, ClogP value: 3.5, Nerolidol, ClogP value: 5.7, ot-Butylcyclohexyl acetate, ClogP value: 4.4, Pamplefleur, ClogP value: 3.4, p-Cymene, ClogP value: 4.0, p-Menthane, ClogP value: 5.3, pt-Butylcyclohexyl acetate, ClogP value: 4.4, Phenoxyethanol, ClogP value: 1.1, Phenyl ethyl alcohol, ClogP value: 1.6, Phenylethyl salicylate ethyl salicylate, ClogP value: 4.8), Phenyl propyl alcohol, ClogP value: 2.1, Poirenate, ClogP value: 4.0, Prenyl acetate, ClogP value: 2.2, Raspberry ketone, ClogP value: 1.5, Rose oxide, ClogP value: 3.6, Styrallyl acetate, ClogP value: 2.5), styrallyl alcohol (ClogP value: 1.5), styrallyl propionate (ClogP value: 3.0), terpineol (ClogP value: 3.3), terpinolene 90 (ClogP value: 4.9), terpinyl acetate (ClogP value: 4.3), tetrahydro linalool (ClogP value: 3.6), tetrahydro muguol (ClogP value: 3.6), thymol (ClogP value: 3.5), tricyclo decenyl acetate (ClogP value: 2.9), tricyclo decenyl propionate (ClogP value: 3.0), At least one selected from the group consisting of propionate (ClogP value: 3.3), Triplar (ClogP value: 2.9), Undecavertol (ClogP value: 4.1), Vanillin (ClogP value: 1.1), Veloutone (ClogP value: 4.3), etc. is preferred, and at least one selected from the group consisting of Triplar, Fruitate, and Iso-E-Super is more preferred.

[0017] The regenerative raw material may contain surfactants derived from the contents. The surfactant may be any known surfactant that can be blended in laundry detergents, laundry softeners, etc. More specifically, examples of the surfactant in the present invention include anionic surfactants, nonionic surfactants, amphoteric surfactants, and cationic surfactants.

[0018] Examples of the anionic surfactant include alkylbenzenesulfonates, alkyl or alkenyl ether sulfates, alkyl or alkenyl sulfates, olefinsulfonates, alkanesulfonates, saturated or unsaturated fatty acid salts, alkyl or alkenyl ether carboxylates, α-sulfonic fatty acid salts, N-acylamino acid surfactants, phosphate mono- or diester surfactants, and sulfosuccinate esters.

[0019] Examples of nonionic surfactants include polyoxyethylene alkyl ethers, polyoxyethylene alkenyl ethers, higher fatty acid sucrose esters, polyglycerin fatty acid esters, higher fatty acid mono- or diethanolamides, polyoxyethylene hydrogenated castor oil, polyoxyethylene sorbitan fatty acid esters, polyoxyethylene sorbit fatty acid esters, alkyl saccharide surfactants, alkylamine oxides, and alkylamidoamine oxides.

[0020] Examples of amphoteric surfactants include imidazolines, carbobetaines, amidobetaines, sulfobetaines, hydroxysulfobetaines, and amidosulfobetaines.

[0021] Examples of the cationic surfactant include dodecyl trimethyl ammonium chloride, tetradecyl trimethyl ammonium chloride, hexadecyl trimethyl ammonium chloride, dodecyl benzyl dimethyl ammonium chloride, tetradecyl benzyl dimethyl ammonium chloride, didecyl dimethyl ammonium ethyl sulfate, and dioctyl dimethyl ammonium ethyl sulfate.

[0022] The recycled resin in the present invention includes containers for shampoo, fabric softener, etc. Suitable examples of the recycled resin material include those containing polyolefin. Examples of polyolefin include those containing at least one selected from the group consisting of polyethylene, polypropylene, and ethylene-vinyl alcohol copolymer, and from the viewpoint of recyclability of the recycled resin, preferably contain polyethylene. From the same viewpoint, the polyolefin may be polyethylene. As the polyethylene, commercially available ones such as high density polyethylene (HDPE), medium density polyethylene (MDPE), low density polyethylene (LDPE), ultra-low density polyethylene (ULDPE), linear low density polyethylene (LLDPE), etc. are applicable to the present invention without any particular limitation.

[0023] From the viewpoint of recyclability, the content of the recycled resin in the recycled raw material is preferably 90% by mass or more, more preferably 95% by mass or more, and even more preferably 99% by mass or more, while the upper limit is not limited, it is usually less than 100% by mass.

[0024] In contrast, from the viewpoint of recyclability, the content of volatile components in the raw material for recycling is preferably 10% by mass or less, more preferably 5% by mass or less, and even more preferably 1% by mass or less, while the lower limit is not limited, but is 0.001% by mass or more.

[0025] In addition to the recycled resin, the raw material for recycling may contain components other than the recycled resin, such as plasticizers, viscosity modifiers, ultraviolet absorbers, antioxidants, compatibilizers, gas barrier agents, and antistatic agents, to the extent that they do not interfere with recycling. From the viewpoint of recyclability, it is preferable that the amount of components other than the recycled resin is small. Specifically, the content of components other than the recycled resin in the raw material for recycling is preferably 10% by mass or less, more preferably 5% by mass or less, and even more preferably 1% by mass or less, while the lower limit is not limited, but is 0.001% by mass or more.

[0026] The crushed raw material for recycling may be in the form of, for example, flakes, powder, or lumps. The size of the crushed material can be adjusted to a desired level, for example, by appropriately setting the size of the screen opening of the crusher. For example, the size of the raw material for regeneration after the crushing process can be set to a screen opening of the crusher of preferably 8 mm or more, preferably 50 mm or less, from the viewpoint of ease of handling, and if further fineness is required, the screen opening can be set to 1 mm or more, 3 mm or more, preferably 8 mm or less.

[0027] The particle size distribution of the crushed material for recycling is preferably 1 mm or more, more preferably 2 mm or more, and even more preferably 3 mm or more from the viewpoint of preventing outflow and scattering from the recovery mesh, while from the viewpoint of contact efficiency between the cleaning solvent and cleaning medium and the crushed material surface in the cleaning process, it is preferably 15 mm or less, more preferably 12 mm or less, and even more preferably 10 mm or less. Furthermore, the median diameter of the crushed material for recycling is preferably 3 mm or more, more preferably 5 mm or more, and even more preferably 6 mm or more from the viewpoint of suppressing compaction and adhesion in the packed state, while from the viewpoint of flowability when supplied from a popper or the like to a processing device, it is preferably 12 mm or less, more preferably 11 mm or less, and even more preferably 10 mm or less.

[0028] The crushed material of the raw material for recycling can be obtained, for example, by crushing the raw material for recycling. Such a crushing process can be carried out using a crusher such as a single-axis crusher, a two-axis crusher, a three-axis crusher, a cutter mill, a mesh mill, or a washing crusher. For example, the PFS-40 type manufactured by Nippon Seam Co., Ltd. is capable of dry crushing or washing crushing, and the raw material for recycling can be crushed using a mesh mill HA2542 type manufactured by Horai Co., Ltd.

[0029] The crushing step may be carried out once in a single crusher, or may be carried out multiple times in the same or different crushers. By carrying out the crushing step multiple times, crushed material having a smaller size can be easily obtained.

[0030] In order to remove contents and dirt adhering to the raw material for recycling, a water washing step may be performed before or after the crushing step to wash the raw material for recycling with water. The washing can be performed, for example, by rinsing the raw material for recycling with water or an aqueous surfactant solution. In particular, it is preferable to use a washing and crushing machine because washing and crushing can be performed simultaneously.

[0031] The treatment time, i.e., the time for passing the water vapor, is 150 minutes or more, preferably 180 minutes or more, more preferably 210 minutes or more, and even more preferably 240 minutes or more, from the viewpoint of removing volatile components. The upper limit of the treatment time is not particularly limited, but is preferably 600 minutes or less, more preferably 540 minutes or less, from the viewpoint of work efficiency.

[0032] Steam is supplied to the packing vessel and circulated within the vessel, whereby the steam comes into contact with the crushed material, reducing the amount of volatile components in the raw material for regeneration. The temperature of the water vapor is preferably in the same temperature range as the treatment temperature range from the viewpoint of removing volatile components and suppressing fusion of the crushed materials.

[0033] The linear velocity of the water vapor flowing through the packed tank is preferably 0.04 m / s or more, more preferably 0.35 m / s or more, and even more preferably 0.50 m / s or more, from the viewpoint of washing away volatile components, while from the viewpoint of preventing the outflow of crushed material, it is preferably 0.90 m / s or less, more preferably 0.85 m / s or less, even more preferably 0.80 m / s or less, and even more preferably 0.75 m / s or less.

[0034] The temperature in the filling tank, i.e., the processing temperature in the process of washing the crushed material for recycling, is preferably equal to or lower than the melting point of the resin with the lowest melting point among the resins for recycling. By setting the temperature in this range, it is possible to suppress the melting of the resin for recycling to the inner wall of the tank and the melting of the crushed material. The processing temperature referred to here is the temperature in the filling tank (product temperature). For example, from the viewpoint of facilitating washing and removal of volatile components, the treatment temperature is 100°C or higher, preferably 102°C or higher, and more preferably 104°C or higher. On the other hand, from the viewpoint of suppressing adhesion of the molten resin to the inner wall of the tank and from the viewpoint of equipment costs and energy consumption, the treatment temperature is 115°C or lower, preferably 110°C or lower, and more preferably 105°C or lower.

[0035] The filling rate of the crushed material for recycling in the filling tank is preferably high from the viewpoint of productivity, specifically, preferably 30% or more, more preferably 60% or more, and even more preferably 99% or more. On the other hand, the upper limit of the filling rate is preferably 100%. In this specification, the filling rate of the crushed material for recycling in the filling tank is a value calculated as follows. 100 x (weight of crushed material [g] / bulk density of crushed material [g / cc]) / capacity of filling tank [cc]

[0036] The steam treatment is carried out under normal pressure, but from the viewpoint of promoting the removal of volatile components, the steam treatment can also be carried out under reduced pressure. In this case, the pressure in the filling tank is preferably 0.10 kPa or less, more preferably 0.01 kPa or less.

[0037] The crushed material for regeneration in the filling tank is preferably washed in a batch manner. For example, the crushed material for regeneration is fed into the filling tank, washed for a predetermined treatment time, and then the washed crushed material for regeneration is discharged from the filling tank.

[0038] The type of washer that can be used in the steam washing step can be any type of washer known in the field of the present invention, without any particular limitations. For example, a steam heating device (Aroma Reduced Pressure Steam Distillation Device, manufactured by Motomura Seisakusho Co., Ltd.) that contacts the crushed material with saturated steam generated inside a tank can be used, and a high-speed mixer (FS VDGS-5JED type, manufactured by EarthTechnica Co., Ltd.) that can ventilate steam inside a closed stirring tank can also be used.

[0039] The crushed material for regeneration obtained through the washing step may be further dried.

[0040] From the viewpoint of the recyclability of the resin, the present invention preferably further includes a melt-kneading step. In the melt-kneading step, the raw material for recycling obtained in the drying step is targeted. By melt-kneading the raw material for recycling, a recycled resin such as recycled polyolefin can be produced, for example, in the form of pellets.

[0041] The melt-kneading step in the present invention may be any of a batch type, a semi-batch type, and a continuous type. The operating conditions and the equipment used in carrying out the melt-kneading step may be those known in the field of the present invention.

[0042] From the viewpoint of recycling, the recycled resin produced by the method of the present invention is suitable as a raw material for packaging containers. The packaging container produced from the recycled resin produced by the method of the present invention can be used as a raw material for recycling after use. That is, from the viewpoint of recycling, the raw material for recycling preferably contains recycled resin, and more preferably contains recycled resin produced by the present invention. EXAMPLES

[0043] The present invention will be specifically described below with reference to examples and comparative examples, but the present invention is not limited to the following examples.

[0044] Reference example 1 [Crushing process] The contents of a bottle (HDPE material, capacity 520 mL) containing a softener composition containing aldehyde C-14, a fragrance compound, were removed, and the label and cap were removed. Next, 100 mL of tap water was poured into the bottle, and the bottle was rinsed by shaking it by hand. After this operation was repeated twice, the bottle was crushed in a crusher (manufactured by Nippon Seam Co., Ltd., PFS-40 type, screen opening: 8 mm) to obtain a crushed product. Approximately 100 pieces of crushed material were randomly selected, and the size of each was measured with a vernier caliper, and the crushed material was classified by size to calculate the mass ratio. The results are shown in Table 1.

[0045] [Table 1]

[0046] [Water washing process] The crushed material was washed with water while stirring in a separatory flask equipped with a crescent-shaped stirring blade. The crushed material and water were charged in a mass ratio of 1:14, and the crushed material was washed with water by stirring for 60 minutes while heating to 50°C in a water bath. The crushed material after washing was collected, placed on a paper towel and mixed to absorb the water from the crushed material into the paper towel, thereby drying the crushed material and obtaining a "washed product."

[0047] [GC / FID analysis] Approximately 2.0 g of this "water-washed product" was weighed into a screw tube, 4 mL of 2-propanol was added, and extraction treatment was carried out at 60°C for 2 days. The extract was then filtered. Next, GC analysis of the filtrate was carried out under the following conditions to quantitatively evaluate the fragrance components.

[0048] The conditions for GC / FID analysis were as follows: GC device: 7890B (Agilent Technologies) Column: DB-1 HT Dimethylpolysiloxane (30m x 0.25mm x 0.25μm) (Agilent Technologies) Carrier gas (N2): 3.27mL / min Temperature conditions: 80℃→(10℃ / min)→300℃ hold 10min Inlet temperature: 250℃ Detector: FID Injection volume: 1μL

[0049] The results are shown in Table 2. In the above "rinsed product", multiple fragrance components were found at concentrations exceeding 10 ppm. In addition, the "rinsed product" had a strong fabric softener smell. Therefore, it was determined that the washing process in this reference example was insufficient to remove volatile components.

[0050] Example 1 In Example 1, a "water-washed product" was prepared in the same manner as in Reference Example 1 above, and then further washed in the steam treatment step described below to obtain a "steam-treated product A".

[0051] [Steam treatment process] As the apparatus used in this process, an apparatus was fabricated, as shown in Fig. 1, in which a SUS pipe was used as a packed tank 5, to which a pump 3, an oil bath 4, a cooler 9, etc. were connected by tubes. The inside of the packed tank 5 was cylindrical. By adjusting the output of the pump 3, the linear velocity of the water vapor in the packed tank 5 was set to a predetermined value. After the crushed material "washed product" was placed in the filling tank, water supplied by a pump 3 was heated in an oil bath 4 to prepare steam, and this steam was continuously passed through the filling tank 5 containing the "washed product" to carry out the cleaning process. It is possible to install a mesh at the steam outlet of the filling tank to prevent the crushed material from flowing out, but in order to confirm the outflow behavior of the crushed material due to an increase in the linear velocity of the steam, which is evaluated in this example, the cleaning process was carried out without installing a mesh. As shown in FIG. 1, it is preferable to supply steam from the bottom of the packing vessel 5, since this allows the steam to come into contact with the entire crushed material.

[0052] [Production of steam-treated product A] 25 g of the "water-washed product", equivalent to 30 volume % of the capacity of the filling tank, was placed in the filling tank and treated with heated steam under the conditions of linear velocity: 0.15 m / s, temperature in the filling tank: 100°C, and treatment time: 240 min. After that, the treated product was removed from the filling tank, placed on a paper towel, and dried by stirring to absorb the moisture into the paper towel, thereby obtaining "steam-treated product A".

[0053] GC analysis of "steam-treated product A" was carried out in the same manner as above. The main conditions and results are shown in Table 2.

[0054] It was confirmed that the concentration of all fragrance components in "steam-treated product A" was reduced to less than 1 ppm, and it was determined that the steam treatment provided a high cleaning effect.

[0055] Comparative Example 1 In Comparative Example 1, the treatment time was changed from 240 minutes to 60 minutes in Example 1, and the same operations were carried out. The results are shown in Table 2.

[0056] Comparative Example 2 In Comparative Example 2, the same operations were carried out as in Comparative Example 1, except that the linear velocity was changed from 0.15 m / s to 1.1 m / s. The results are shown in Table 2.

[0057] Comparative Example 7 In Comparative Example 7, the same operations were carried out as in Example 1, except that the linear velocity was changed from 0.15 m / s to 0.04 m / s. The results are shown in Table 2.

[0058] Example 5 Example 5 was carried out in the same manner as in Comparative Example 7, except that the treatment time was changed from 240 minutes to 360 minutes. The results are shown in Table 2.

[0059] [Table 2]

[0060] Example 6 In Example 6, 42 g of the "water-washed product", equivalent to 50% of the capacity of the filling tank, was placed in the filling tank, and the heated steam was operated under the following conditions: linear velocity: 0.15 m / s, temperature inside the filling tank: 100°C, treatment time: 360 min. Except for this, the same operation as in Example 1 was carried out. The results are shown in Table 3.

[0061] Comparative Example 3 In Comparative Example 3, the treatment time was changed from 360 minutes to 60 minutes in Example 6, but all operations were the same. The results are shown in Table 3.

[0062] Comparative Example 10 In Comparative Example 10, the same operations were carried out as in Example 6, except that the linear velocity was changed from 0.15 m / s to 0.04 m / s. The results are shown in Table 3.

[0063] Comparative Example 4 In Comparative Example 4, the same operation as in Example 6 was carried out except that the linear velocity was changed from 0.15 m / s to 1.5 m / s. However, the crushed material flowed out of the packing tank, and the operation was interrupted. The results are shown in Table 3.

[0064] [Table 3]

[0065] Example 7 In Example 7, 62.5 g of the "water-washed product", equivalent to 75% of the capacity of the packed vessel, was placed in the packed vessel, and the heated steam was operated under the following conditions: linear velocity: 1.1 m / s, temperature in the packed vessel: 100°C, treatment time: 360 min. Except for this, the same procedure as in Example 1 was carried out. The results are shown in Table 4.

[0066] Example 3 In Example 3, the treatment time was changed from 360 minutes to 240 minutes in Example 7, but all operations were the same. The results are shown in Table 4.

[0067] Comparative Example 5 In Comparative Example 5, the treatment time was changed from 360 minutes to 60 minutes in Example 3, and the same operations were carried out. The results are shown in Table 4.

[0068] Example 2 In Example 2, the same operations were carried out as in Example 3, except that the linear velocity was changed from 1.1 m / s to 0.74 m / s. The results are shown in Table 4.

[0069] Comparative Example 8 In Comparative Example 8, the same operations were carried out as in Example 2, except that the linear velocity was changed from 0.74 m / s to 0.15 m / s. The results are shown in Table 4.

[0070] [Table 4]

[0071] Example 8 In Example 8, 82.5 g of the "water-washed product", which corresponds to 99% of the capacity of the packed tank, was placed in the packed tank, and the heated steam was operated under the following conditions: linear velocity: 0.74 m / s, temperature inside the packed tank: 100° C., treatment time: 360 min. Except for this, the same operation as in Example 1 was carried out. The results are shown in Table 5.

[0072] Comparative Example 11 In Comparative Example 11, the same operations were carried out as in Example 8, except that the linear velocity was changed from 0.74 m / s to 0.15 m / s. The results are shown in Table 5.

[0073] [Table 5]

[0074] Example 4 In Example 4, the same operations were performed as in Example 8, except that the linear velocity was changed from 0.74 m / s to 1.1 m / s and the processing time was changed from 360 min to 240 min. The results are shown in Table 6.

[0075] Comparative Example 6 In Comparative Example 6, the treatment time was changed from 240 minutes to 60 minutes in Example 3, and the same operations were carried out. The results are shown in Table 6.

[0076] Comparative Example 9 In Comparative Example 9, the same operations were carried out as in Example 4, except that the linear velocity was changed from 1.1 m / s to 0.15 m / s. The results are shown in Table 6.

[0077] [Table 6] [Industrial Applicability]

[0078] The manufacturing method of the present invention can be applied to the recycling of used plastic bottle packaging containers for shampoos and liquid laundry detergents. [Explanation of symbols]

[0079] 1 water 2 Tubes 3. Pump 4. Oil bath 5 Filling tank 6 Crushed material 7 Thermometer 8. Pressure gauge 9 Cooler 10 Collection container

Claims

1. A method for producing recycled resin, comprising the steps of: supplying crushed material of a raw material for recycling, which contains volatile components and a resin for recycling, to a filling tank; and washing the crushed material of the raw material for recycling by circulating water vapor through the filling tank, wherein the temperature in the filling tank is 100°C or higher and 115°C or lower, and the processing time for the step of washing the crushed material is 150 minutes or longer.

2. The method according to claim 1, wherein the crushed material for recycling is obtained through a crushing step of crushing the material for recycling.

3. The method according to claim 1, wherein the crushed material for recycling is obtained by a crushing step of crushing the material for recycling, followed by a washing step of washing the crushed material with water.

4. The method according to any one of claims 1 to 3, wherein the linear velocity of the water vapor flowing through the packed vessel is 0.04 m / s or more and 0.75 m / s or less.

5. The method according to any one of claims 1 to 4, wherein the volatile component comprises a fragrance.

6. The method according to any one of claims 1 to 5, wherein the particle size distribution of the crushed material for recycling is 1 mm or more and 15 mm or less, and the median diameter is 3 mm or more and 12 mm or less.

7. The method according to any one of claims 1 to 6, wherein the filling rate of the crushed material for recycling in the filling tank is 30 to 100%.

8. The method according to any one of claims 1 to 7, wherein the washing of the crushed material for regeneration in the packing tank is carried out in a batch manner.

9. The method according to any one of claims 1 to 8, wherein the raw material for recycling includes packaging containers of plastic bottles.

10. A recycled resin produced by the method according to any one of claims 1 to 9.

Images