CN112341588B - Low-density polyurethane mid-sole composite material containing recyclable waste particles and preparation method of mid-sole - Google Patents
Low-density polyurethane mid-sole composite material containing recyclable waste particles and preparation method of mid-sole Download PDFInfo
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- CN112341588B CN112341588B CN202011186379.1A CN202011186379A CN112341588B CN 112341588 B CN112341588 B CN 112341588B CN 202011186379 A CN202011186379 A CN 202011186379A CN 112341588 B CN112341588 B CN 112341588B
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G18/00—Polymeric products of isocyanates or isothiocyanates
- C08G18/06—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen
- C08G18/28—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen characterised by the compounds used containing active hydrogen
- C08G18/65—Low-molecular-weight compounds having active hydrogen with high-molecular-weight compounds having active hydrogen
- C08G18/66—Compounds of groups C08G18/42, C08G18/48, or C08G18/52
- C08G18/6633—Compounds of group C08G18/42
- C08G18/6637—Compounds of group C08G18/42 with compounds of group C08G18/32 or polyamines of C08G18/38
- C08G18/664—Compounds of group C08G18/42 with compounds of group C08G18/32 or polyamines of C08G18/38 with compounds of group C08G18/3203
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- A—HUMAN NECESSITIES
- A43—FOOTWEAR
- A43B—CHARACTERISTIC FEATURES OF FOOTWEAR; PARTS OF FOOTWEAR
- A43B13/00—Soles; Sole-and-heel integral units
- A43B13/02—Soles; Sole-and-heel integral units characterised by the material
- A43B13/04—Plastics, rubber or vulcanised fibre
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G18/00—Polymeric products of isocyanates or isothiocyanates
- C08G18/06—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen
- C08G18/28—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen characterised by the compounds used containing active hydrogen
- C08G18/30—Low-molecular-weight compounds
- C08G18/32—Polyhydroxy compounds; Polyamines; Hydroxyamines
- C08G18/3271—Hydroxyamines
- C08G18/3275—Hydroxyamines containing two hydroxy groups
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G18/00—Polymeric products of isocyanates or isothiocyanates
- C08G18/06—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen
- C08G18/28—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen characterised by the compounds used containing active hydrogen
- C08G18/30—Low-molecular-weight compounds
- C08G18/32—Polyhydroxy compounds; Polyamines; Hydroxyamines
- C08G18/3271—Hydroxyamines
- C08G18/3278—Hydroxyamines containing at least three hydroxy groups
- C08G18/3281—Hydroxyamines containing at least three hydroxy groups containing three hydroxy groups
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G18/00—Polymeric products of isocyanates or isothiocyanates
- C08G18/06—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen
- C08G18/28—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen characterised by the compounds used containing active hydrogen
- C08G18/40—High-molecular-weight compounds
- C08G18/42—Polycondensates having carboxylic or carbonic ester groups in the main chain
- C08G18/4244—Polycondensates having carboxylic or carbonic ester groups in the main chain containing oxygen in the form of ether groups
- C08G18/4247—Polycondensates having carboxylic or carbonic ester groups in the main chain containing oxygen in the form of ether groups derived from polyols containing at least one ether group and polycarboxylic acids
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G18/00—Polymeric products of isocyanates or isothiocyanates
- C08G18/06—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen
- C08G18/28—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen characterised by the compounds used containing active hydrogen
- C08G18/40—High-molecular-weight compounds
- C08G18/42—Polycondensates having carboxylic or carbonic ester groups in the main chain
- C08G18/4244—Polycondensates having carboxylic or carbonic ester groups in the main chain containing oxygen in the form of ether groups
- C08G18/4247—Polycondensates having carboxylic or carbonic ester groups in the main chain containing oxygen in the form of ether groups derived from polyols containing at least one ether group and polycarboxylic acids
- C08G18/4252—Polycondensates having carboxylic or carbonic ester groups in the main chain containing oxygen in the form of ether groups derived from polyols containing at least one ether group and polycarboxylic acids derived from polyols containing polyether groups and polycarboxylic acids
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P20/00—Technologies relating to chemical industry
- Y02P20/50—Improvements relating to the production of bulk chemicals
- Y02P20/584—Recycling of catalysts
Abstract
The invention relates to a low-density polyurethane midsole composite material containing recyclable waste particles and a preparation method of a midsole, belonging to the technical field of polyurethane. The mass ratio of the sum of the components A and C to the component B of the composite material is 100:50-70 parts of; the component A comprises: 1-40% of polyether ester polyol, 225-60% of polyester polyol, 3-8% of chain extender, 0.3-1.5% of cross-linking agent, 0.3-1.0% of foam stabilizer, 0.5-2.5% of catalyst and 0.5-1.5% of foaming agent; and the component B comprises: 1-20% of polyether ester polyol, 3-50% of polyester polyol, 50-80% of isocyanate and 10ppm of storage stabilizer; the component C is recyclable waste particles. The insole prepared by the invention has the advantages of high recoverable waste particles content, low density, excellent mechanical property and the like; meanwhile, the invention provides a simple and easy-to-implement preparation method.
Description
Technical Field
The invention relates to a low-density polyurethane midsole composite material containing recyclable waste particles and a preparation method of a midsole, belonging to the technical field of polyurethane.
Background
Materials such as PU and EVA are widely used due to their excellent properties, and thus a large amount of aged waste is generated, so that recycling of the waste materials is a problem to be solved urgently in recent years. The waste materials are crushed into fine pieces or particles by a crushing method to be used as the filler, so that the waste materials are recycled, the recycling of waste resources is realized, the product cost can be effectively reduced, and the method is the development direction of recycling the waste materials such as PU, EVA and the like at present.
The recyclable waste particles are used as fillers to prepare the mid-soles or the insoles, the main problems are that the filling amount is small, the mechanical property is poor, and after the recyclable particles account for more than 20 percent of the product by weight, the molding defective rate and the mechanical property of the product are seriously attenuated, so that the actual use requirements are difficult to meet.
Disclosure of Invention
The invention aims to solve the technical problems that the defects in the prior art are overcome, the low-density polyurethane midsole composite material containing the recyclable waste particles is provided, and the manufactured midsole has the advantages of high content of the recyclable waste particles, low density, excellent mechanical property and the like; meanwhile, the invention provides a simple and easy-to-implement preparation method of the low-density polyurethane midsole.
The low-density polyurethane mid-sole composite material containing recyclable waste particles consists of a component A, a component B and a component C, wherein the mass ratio of the sum of the component A and the component C to the component B is 100:50-70, wherein:
the component A comprises the following raw materials in percentage by mass:
the total mass of the polyether ester polyol 1 and the polyester polyol 2 is 100 percent;
the component B comprises the following raw materials in percentage by mass:
the component C is recyclable waste particles, and the mass ratio of the component A to the component C is 100:10-120.
The polyether ester polyol 1 is prepared by carrying out polycondensation reaction on micromolecular dihydric alcohol, micromolecular polyether polyol and adipic acid, and the number average molecular weight is 1000-4000;
the polyester polyol 2 is prepared by carrying out polycondensation reaction on one or a mixture of more of ethylene glycol, diethylene glycol and 1, 4-butanediol and one or two of adipic acid and terephthalic acid, and the number average molecular weight is 1000-3500;
the polyester polyol 3 is prepared by one or a mixture of more of ethylene glycol, diethylene glycol and 1, 4-butanediol and adipic acid through polycondensation, and has the number average molecular weight of 1000-2500.
The micromolecular dihydric alcohol is one or more of ethylene glycol, diethylene glycol or 1, 4-butanediol.
The micromolecular polyether polyol is polyether polyol with the functionality of 2.0-2.2 and the number average molecular weight of 500-1500.
The chain extender is one or more of Ethylene Glycol (EG), diethylene glycol (DEG), 1, 4-butanediol (1, 4-BG), 1, 3-propanediol (1, 3-PDO), dipropylene glycol (DPG) or 1, 6-hexanediol.
The cross-linking agent is one or more of Triethanolamine (TEA), diethanolamine (DEOA), glycerol, and trimethylolpropane.
The foam stabilizer is a polysiloxane-oxyalkylene block copolymer, preferably DC-193 (air chemical Co., ltd., U.S.A.).
The catalyst is tertiary amine catalyst, and the tertiary amine catalyst is preferably triethylene diamine; the blowing agent is preferably water.
The isocyanate is preferably one or more of pure MDI, carbodiimide modified MDI, MDI-50 and polymeric MDI.
The density of the recyclable waste particles is 200-500g/L, the particle size of the particles is less than or equal to 1cm, and the types of the particles are one or more of PU, EVA, PVC and PE-PP.
The storage stabilizer is preferably phosphoric acid or benzoyl chloride.
The preparation method of the low-density polyurethane mid-sole containing the recyclable waste particles comprises the following steps:
(1) A component material: the measured polyether ester polyol 1, polyester polyol 2, chain extender, cross-linking agent, foam stabilizer, catalyst and foaming agent are put into a reaction kettle at normal temperature, and the mixture is stirred for 1 to 2 hours to obtain a component A;
(2) B, component material: adding polyether ester polyol 1 and polyester ester polyol 3 based on formula amount into a reaction kettle at normal temperature, stirring and heating to 90-110 ℃, dehydrating and degassing for 2-3 hours under vacuum condition, then cooling to 50 ℃, adding metered isocyanate, and reacting for 2-3 hours at 80-85 ℃ to obtain a component B;
(3) Respectively injecting the component A and the component B into a charging bucket of a low-pressure casting machine, premixing the component A and the component C at a machine head, mixing the component A and the component C with the component B at the machine head, injecting the mixture into a mold at 40-60 ℃, and opening the mold after 4-5min to obtain the low-density polyurethane insole containing the recyclable waste particles.
Compared with the prior art, the invention has the following beneficial effects:
(1) The low-density polyurethane midsole containing recyclable waste particles is prepared by adopting the composite material provided by the invention, the problem of intersolubility between polyester and polyether in the material A can be effectively solved, the polyether ester mainly contains a polyester chain segment and a polyether chain segment, and can have better intermiscibility with the polyester, and the polyester chain segment and the polyether chain segment simultaneously contained in the polyether ester have different polarities, so that the low-density polyurethane midsole has better adhesiveness with recyclable waste particles made of different materials, the mechanical property of a product is remarkably enhanced, the addition amount of the recyclable waste particles can be remarkably increased, and the recyclable waste particles can account for 35 percent of the weight of the product;
(2) The polyether ester can obviously improve the open pore property of the product, and the density of the product is as low as 250kg/m 3 The shrinkage problem does not occur in the case of (2);
(3) The preparation method of the low-density polyurethane midsole is scientific, reasonable, simple and feasible, and is beneficial to industrial production.
Detailed Description
The present invention is further described below with reference to examples.
The mass unit of each component in the following examples is Kg.
Example 1
C, component A: mass ratio of component C
Recyclable PE-PP particles 100:40
A component material: polyether polyol 1 with the number average molecular weight of 2000 is prepared by the polycondensation reaction of polyether polyol with the molecular weight of 500 and the functionality of 2.0, diethylene glycol, 1, 4-butanediol and adipic acid. The polyester polyol 2 with the number average molecular weight of 1500 is prepared by the polycondensation reaction of glycol, diethylene glycol and 1, 4-butanediol with adipic acid. Mixing the raw materials in the formula according to a ratio, stirring for 1 hour, sampling, and inspecting to obtain the component A.
B, component material: the polyester polyol 3 with the number average molecular weight of 2500 is prepared by the polycondensation reaction of ethylene glycol, 1, 4-butanediol and adipic acid. And (2) putting the polyether ester polyol 1 and the polyester polyol 3 based on the formula amount into a reaction kettle at normal temperature, stirring and heating to 100 ℃, and dehydrating and degassing for 2 hours under a vacuum condition. And then cooling to 50 ℃, adding metered isocyanate, reacting for 2 hours at 80 ℃, and obtaining the component B after the component B is qualified through inspection.
When the material is used, the component A and the component B are respectively injected into a charging bucket of a low-pressure casting machine, the material type of recyclable waste particles is PE-PP, the particle density is 400g/L, and the particle size is less than or equal to 1cm. Premixing the component A and the recyclable waste particles at the machine head according to the mixture ratio in the table to obtain a mixture, mixing the mixture with the component B at the machine head according to the mass ratio of the mixture A + C: B =100, injecting the mixture into a mold at 50 +/-10 ℃, and opening the mold after 4min to obtain the low-density polyurethane insole containing the recyclable waste particles.
After aging for 3 days at room temperature, the performance indexes of the sample, such as density, hardness, right-angle tearing, bending times and the like, are tested.
Example 2
C, component A: mass ratio of component C
Recyclable PE-PP particles 100:80
A component material: polyether polyol 1 with the number average molecular weight of 3000 is prepared by the polycondensation reaction of polyether polyol with the molecular weight of 1000 and the functionality of 2.0, ethylene glycol, diethylene glycol and adipic acid. The polyester polyol 2 with the number average molecular weight of 2000 is prepared by the polycondensation reaction of ethylene glycol, 1, 4-butanediol, adipic acid and terephthalic acid. Mixing the raw materials in the formula according to a ratio, stirring for 2 hours, sampling, and inspecting to obtain the component A.
B, component material: the polyester polyol 3 with the number average molecular weight of 2000 is prepared by the polycondensation reaction of ethylene glycol, diethylene glycol, 1, 4-butanediol and adipic acid. And (2) putting the polyether ester polyol 1 and the polyester polyol 3 based on the formula amount into a reaction kettle at normal temperature, stirring and heating to 100 ℃, and dehydrating and degassing for 2 hours under a vacuum condition. And then cooling to 50 ℃, adding metered isocyanate, reacting for 2 hours at 80 ℃, and obtaining the component B after the component B is qualified through inspection.
When the material is used, the component A and the component B are respectively injected into a charging bucket of a low-pressure casting machine, the material type of the recyclable waste particles is EVA, the particle density is 200g/L, and the particle size is less than or equal to 1cm. Premixing the component A and the recyclable waste particles at the machine head according to the mixture ratio in the table to obtain a mixture, mixing the mixture with the component B at the machine head according to the mass ratio of the mixture A + C: B =100 to obtain a mixture, injecting the mixture into the machine head at 50 +/-10 ℃, and opening the mold after 4min to obtain the low-density polyurethane mid-sole containing the recyclable waste particles.
After being cured for 3 days at room temperature, the sample is tested for performance indexes such as density, hardness, right-angle tearing, bending times and the like.
Example 3
C, component A: mass ratio of component C
Recoverable PE-PP particles 100:120
A component material: polyether polyol 1 with the number average molecular weight of 4000 is prepared by carrying out polycondensation reaction on polyether polyol with the molecular weight of 1500 and the functionality of 2.2, diethylene glycol and adipic acid. Glycol, diethylene glycol and adipic acid are subjected to polycondensation reaction to prepare polyester polyol 2 with the number average molecular weight of 3500. Mixing the raw materials in the formula according to a ratio, stirring for 1 hour, sampling, and inspecting to obtain the component A.
B, component material: 1, 4-butanediol and adipic acid are subjected to polycondensation reaction to prepare polyester polyol 3 with the number average molecular weight of 1000. And (2) putting the polyether ester polyol 1 and the polyester polyol 3 based on the formula amount into a reaction kettle at normal temperature, stirring and heating to 100 ℃, and dehydrating and degassing for 2 hours under a vacuum condition. And then cooling to 50 ℃, adding metered isocyanate, reacting for 2 hours at 80 ℃, and obtaining the component B after the test is qualified.
During the use, pour into the low pressure casting machine material jar respectively with A component, B component, recoverable old and useless granule material kind chooses PU for use: EVA is mixed according to 1. Premixing the component A and the recyclable waste particles at the machine head according to the mixture ratio in the table to obtain a mixture, mixing the mixture with the component B at the machine head according to the mass ratio of the mixture A + C: B =100, injecting the mixture into a machine head at 50 +/-10 ℃, and opening the mold after 5min to obtain the low-density polyurethane mid-sole containing the recyclable waste particles.
After aging for 3 days at room temperature, the performance indexes of the sample, such as density, hardness, right-angle tearing, bending times and the like, are tested.
Comparative sample 1 is a commercially available midsole product made using recyclable waste particles.
The performance test data for the samples prepared in examples 1-3 and comparative sample 1 are shown in Table 1.
TABLE 1 sample Performance data Table
As can be seen from the data in Table 1, the weight ratio of the recoverable waste particles of the midsole product prepared in example 2 is close to that of the comparative sample 1, but the density of the product is significantly lower than that of the comparative sample 1, and the mechanical properties such as right-angle tearing and bending times are still kept at a good level. The weight ratio of the recoverable waste particles of the midsole product prepared in the embodiment 3 is obviously higher than that of the comparative sample 1, meanwhile, the density of the product is obviously lower than that of the comparative sample 1, and the mechanical properties such as right-angle tearing and bending times are still kept at a better level.
Claims (9)
1. A low-density polyurethane mid-sole composite material containing recyclable waste particles is characterized in that: the paint consists of a component A, a component B and a component C, wherein the mass ratio of the sum of the component A and the component C to the component B is 100:50-70, wherein:
the component A comprises the following raw materials in percentage by mass:
polyether ester polyol 1-50%
2 to 90 percent of polyester polyol
Chain extender 3-8%
0.3 to 1.5 percent of cross-linking agent
0.3 to 1.0 percent of foam stabilizer
Catalyst 0.5-2.5%
0.5 to 1.5 percent of foaming agent;
the total mass of the polyether ester polyol 1 and the polyester polyol 2 is 100 percent;
the component B comprises the following raw materials in percentage by mass:
polyether ester polyol 1-20%
3 to 50 percent of polyester polyol
50-80% of isocyanate
10ppm of storage stabilizer;
the component C is recyclable waste particles, and the mass ratio of the component A to the component C is 100:10-120;
the polyether ester polyol 1 is prepared by the polycondensation reaction of micromolecular dihydric alcohol, micromolecular polyether polyol and adipic acid, and the number average molecular weight is 1000-4000;
the polyester polyol 2 is prepared by carrying out polycondensation reaction on one or a mixture of more of ethylene glycol, diethylene glycol and 1, 4-butanediol and one or two of adipic acid and terephthalic acid, and the number average molecular weight is 1000-3500;
the polyester polyol 3 is prepared by the polycondensation of one or a mixture of more of ethylene glycol, diethylene glycol and 1, 4-butanediol and adipic acid, and the number average molecular weight is 1000-2500;
the density of the recyclable waste particles is 200-500g/L, the particle size of the particles is less than or equal to 1cm, and the type of the particles is PE-PP.
2. The low density polyurethane mid-sole composite material containing recyclable waste particles as defined in claim 1, wherein: the small molecular dihydric alcohol is one or more of ethylene glycol, diethylene glycol or 1, 4-butanediol.
3. The low density polyurethane mid-sole composite material containing recyclable waste particles as defined in claim 1, wherein: the micromolecular polyether polyol is polyether polyol with the functionality of 2.0-2.2 and the number average molecular weight of 500-1500.
4. The low density polyurethane mid-sole composite material containing recyclable waste particles as defined in claim 1, wherein: the chain extender is one or more of ethylene glycol, diethylene glycol, 1, 4-butanediol, 1, 3-propanediol, dipropylene glycol or 1, 6-hexanediol.
5. The low density polyurethane mid-sole composite material containing recyclable waste particles as defined in claim 1, wherein: the cross-linking agent is one or more of triethanolamine, diethanolamine, glycerol or trimethylolpropane.
6. The low density polyurethane mid-sole composite material containing recyclable waste particles as defined in claim 1, wherein: the foam stabilizer is polysiloxane-oxyalkylene block copolymer.
7. The low density polyurethane mid-sole composite material containing recyclable waste particles as defined in claim 1, wherein: the catalyst is tertiary amine catalyst; the foaming agent is water.
8. The low density polyurethane mid-sole composite material containing recyclable waste particles as defined in claim 1, wherein: the isocyanate is one or more of pure MDI, carbodiimide modified MDI, MDI-50 or polymeric MDI.
9. A method for preparing a low-density polyurethane mid-sole containing recyclable waste particles, prepared from the composition according to any one of claims 1 to 8, wherein the method comprises the following steps: the method comprises the following steps:
(1) A component material: the measured polyether ester polyol 1, polyester polyol 2, chain extender, cross-linking agent, foam stabilizer, catalyst and foaming agent are put into a reaction kettle at normal temperature, and the mixture is stirred for 1 to 2 hours to obtain a component A;
(2) B, component material: adding polyether ester polyol 1 and polyester ester polyol 3 based on formula amount into a reaction kettle at normal temperature, stirring and heating to 90-110 ℃, dehydrating and degassing for 2-3 hours under vacuum condition, then cooling to 50 ℃, adding metered isocyanate, and reacting for 2-3 hours at 80-85 ℃ to obtain a component B;
(3) Respectively injecting the component A and the component B into a charging bucket of a low-pressure casting machine, premixing the component A and the component C at a machine head, then mixing the component A and the component B at the machine head, injecting the mixture into a mold at 40-60 ℃, opening the mold after 4-5min, and obtaining the low-density polyurethane insole containing the recyclable waste particles.
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