CN109111550A - A kind of preparation method of sole reclaiming rubber powder - Google Patents
A kind of preparation method of sole reclaiming rubber powder Download PDFInfo
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- CN109111550A CN109111550A CN201810758833.2A CN201810758833A CN109111550A CN 109111550 A CN109111550 A CN 109111550A CN 201810758833 A CN201810758833 A CN 201810758833A CN 109111550 A CN109111550 A CN 109111550A
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F279/00—Macromolecular compounds obtained by polymerising monomers on to polymers of monomers having two or more carbon-to-carbon double bonds as defined in group C08F36/00
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F226/00—Copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by a single or double bond to nitrogen or by a heterocyclic ring containing nitrogen
- C08F226/06—Copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by a single or double bond to nitrogen or by a heterocyclic ring containing nitrogen by a heterocyclic ring containing nitrogen
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J11/00—Recovery or working-up of waste materials
- C08J11/04—Recovery or working-up of waste materials of polymers
- C08J11/06—Recovery or working-up of waste materials of polymers without chemical reactions
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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
- Y02W—CLIMATE CHANGE MITIGATION TECHNOLOGIES RELATED TO WASTEWATER TREATMENT OR WASTE MANAGEMENT
- Y02W30/00—Technologies for solid waste management
- Y02W30/50—Reuse, recycling or recovery technologies
- Y02W30/62—Plastics recycling; Rubber recycling
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- Chemical & Material Sciences (AREA)
- Health & Medical Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Organic Chemistry (AREA)
- Life Sciences & Earth Sciences (AREA)
- Sustainable Development (AREA)
- Separation, Recovery Or Treatment Of Waste Materials Containing Plastics (AREA)
- Processes Of Treating Macromolecular Substances (AREA)
Abstract
The invention discloses a kind of preparation methods of sole reclaiming rubber powder, are related to regenerated plastics field, comprising the following steps: (1) waste old sole cleans and crush into waste and old rubber particle；(2) waste and old rubber particle cleans；(3) waste and old rubber particle grafted maleic anhydride, melt pelletization；(4) pellet grinds obtained sole reclaiming rubber powder；The present invention is grafted waste old by maleic anhydride, improves the mechanical property of waste old, improves the crack resistance and stretch-resistance of waste old, increase the recycling property of waste old, solve the problems, such as the recycling of waste old sole, economize on resources, environmentally protective.
Description
Technical field
The present invention relates to regenerated plastics fields, and in particular to a kind of preparation method of sole reclaiming rubber powder.
Background technique
It accumulates and stores up with waste old, and the ever-increasing status of new waste rubber, scientific waste tire recycle benefit
With having become a current chemical technology problem urgently to be solved.
Chinese patent CN1834206B provides a kind of rubber tyre pyrolytic system and method, is espespecially relevant to one
The method of kind pyrolytic system, is converted to several form of energy for whole rubber tyre and environmental pollution is preferably minimized journey
Degree, protects environment to the maximum extent.The system includes a tire transmission device, a waste energy conversion device, it includes
One converts cabinet, and there is a reaction cabin to be used to receive the rubber tyre and a high-temperature decomposition reaction from the tire transmission device for it
Device is used to pyrolytic rubber tyre in the reaction cabin and then the rubber tyre is resolved into fuel oil, methane gas and charcoal
The wire is removed in the black and rubbery cover tyre from the rubber tyre and is recycled.The present invention is before not adverse condition
The processing for solving the problems, such as waste tire is put, there is application value.
Chinese patent CN200610035601.1 discloses a kind of method of waste tire catalytic pyrolysis fuel oil, this document
It discloses and waste tire is removed into steel wire, be ground into particle, be added in catalyst for cracking barium titanium ore composite oxides feeding furnace and mix
The processes such as cracking are closed, fuel oil is finally obtained.Above-mentioned four patent documents are disclosed will in such a way that high-temperature catalytic cracks
Waste tire is converted into the resource that fuel oil and carbon black etc. can utilize again, has accomplished to turn waste into wealth, it may be said that is to overcome combustion
Burning method and the defect for burying method.
Rubber soles occupy very big ratio in sole material at present, and the discarding amount of waste old sole is on constantly
It rises, therefore is badly in need of solving the problems, such as the regeneration recycling of waste and old sole rubber material, reduce the occupied space of waste old sole.
Summary of the invention
Aiming at the problems existing in the prior art, the present invention provides a kind of preparation sides of sole reclaiming rubber powder
Method, the present invention are grafted waste old by maleic anhydride, improve the mechanical property of waste old, improve the crack resistance of waste old
And stretch-resistance, increase the recycling property of waste old, solves the problems, such as the recycling of waste old sole, economize on resources, green
Environmental protection.
In order to achieve the above object, the present invention is achieved through the following technical solutions:
A kind of preparation method of sole regnerated rubber powder, includes the following steps；
(1) it by after waste old sole clean and reuse, send to pulverizer and is crushed to 10-20 mesh, removed with strong magnetic magnetic separator de-ironing
Wherein iron filings impurity obtains waste and old rubber particle；
(2) cleaning agent, polypropylene glycerol ether, epoxidized soybean oil and water are added into waste and old rubber particle to be uniformly mixed
Afterwards, it is placed in ball mill and carries out ground and cleaned, until more than waste and old rubber particle as low as 80 mesh greatly, filtering is cleaned repeatedly with clear water
4-6 is after, until being dried to moisture content lower than 5% in 80-90 degrees Celsius of baking oven；
(3) product of step (2) and initiator, second comonomer, maleic anhydride, age resister are added in high-speed mixer
After being warming up to 50-60 degrees Celsius of 15-20 minutes with the speed of 10 degrees celsius/minutes, extruding pelletization is added twin-screw extrude,
It is granulated on pelleter after sink is cooling；
(4) it after pellet being cleaned 3 times with deionized water, under 85-90 degrees Celsius, after 20 hours dry, send to pulverizer
In be crushed to pellet to 150-300 mesh to get the sole reclaiming rubber powder.
Preferably, waste and old rubber particle, cleaning agent, polypropylene glycerol ether, epoxidized soybean oil and the water in the step (2)
Dosage mass ratio be 100:3:0.5:0.8:100 mixing composition.
Preferably, the product and initiator, second comonomer, maleic anhydride of the step (2) in the step (3), anti-aging
The mass ratio of agent is 100:3-5:3-5:6-8:2-4.
Preferably, the product and initiator, second comonomer, maleic anhydride of the step (2) in the step (3), anti-aging
The mass ratio of agent is 100:3.5:4.4:7:2.8.
Preferably, the initiator is ammonium persulfate, potassium peroxydisulfate, benzoyl peroxide, benzoyl peroxide
It is combined with one or more of methyl ethyl ketone peroxide.
Preferably, second comonomer is at least one of triallyl isocyanurate and triallyl cyanurate.
Preferably, the age resister is that antioxidant and ultra-violet stabilizer are formed according to mass ratio 3:1 mixing.
Preferably, the antioxidant is three (2,4- di-tert-butyl-phenyl) phosphites, β-(3,5- di-t-butyl -4-
Hydroxy phenyl) propionate, one of β-(3,5- di-tert-butyl-hydroxy phenyl) propionic acid octadecanol ester or several
Kind combines.
Preferably, the ultra-violet stabilizer is salicylic acid esters, benzophenone, benzotriazole, substituted acrylonitrile
One or more of class and triazines combine.
Preferably, double screw extruder extrusion temperature is 265-272 degrees Celsius in the step (3), screw speed 80-
90 revs/min.
The present invention have it is following the utility model has the advantages that
(1) present invention is grafted waste old by maleic anhydride, improves the mechanical property of waste old, improves waste old
Crack resistance and stretch-resistance, increase the recycling property of waste old, solve the problems, such as the recycling of waste old sole, save money
Source, it is environmentally protective.
(2) second comonomer triallyl isocyanurate and triallyl cyanurate contain the double bond there are three allyl,
Thus during rubber cross, it can play a part of increasing the degree of cross linking, i.e., under the initiation for crossing initiator, the two can increase
The effect for adding the degree of cross linking increases substantially the grafting rate of maleic anhydride, improves the flexibility and mechanical shock resistance of waste old,
Improve poor, the easy to crack disadvantage of waste old flexibility.
(3) present invention cleans waste old using cleaning agent, polypropylene glycerol ether, epoxidized soybean oil and water mixed grinding
Grain, can be enhanced the clean type of waste and old rubber particle, while softening waste and old rubber particle, improves the comprehensive of waste and old rubber particle
Energy.
Specific embodiment
Below with reference to embodiment, further description of the specific embodiments of the present invention, and following embodiment is only used for more
Technical solution of the present invention is clearly demonstrated, and not intended to limit the protection scope of the present invention.
Embodiment 1
A kind of preparation method of sole regnerated rubber powder, includes the following steps；
(1) it by after waste old sole clean and reuse, send to pulverizer and is crushed to 10 mesh, wherein with the removal of strong magnetic magnetic separator de-ironing
Iron filings impurity, obtains waste and old rubber particle；
(2) cleaning agent, polypropylene glycerol ether, epoxidized soybean oil and water are added into waste and old rubber particle to be uniformly mixed
Afterwards, it is placed in ball mill and carries out ground and cleaned, until more than waste and old rubber particle as low as 80 mesh greatly, filtering cleans 4 with clear water repeatedly
After, until being dried to moisture content lower than 5% in 80 degrees Celsius of baking oven；
(3) product of step (2) and initiator, second comonomer, maleic anhydride, age resister are added in high-speed mixer
50 degrees Celsius are warming up to after 15 minutes with the speed of 10 degrees celsius/minutes, extruding pelletization are added twin-screw extrude, through sink
It is granulated on pelleter after cooling；
(4) after pellet being cleaned 3 times with deionized water, under 85 degrees Celsius, after 20 hours dry, powder is sent into pulverizer
Pellet is broken to 150 mesh to get the sole reclaiming rubber powder.
The dosage quality of waste and old rubber particle, cleaning agent, polypropylene glycerol ether, epoxidized soybean oil and water in step (2)
It is formed than being mixed for 100:3:0.5:0.8:100.
The product and initiator of step (2) in step (3), second comonomer, maleic anhydride, age resister mass ratio be
100:3:3-5:6-8:2-4。
Initiator is ammonium persulfate.
Second comonomer is triallyl isocyanurate.
Age resister is that antioxidant and ultra-violet stabilizer are formed according to mass ratio 3:1 mixing.
Antioxidant is three (2,4- di-tert-butyl-phenyl) phosphites.
Ultra-violet stabilizer is salicylic acid esters.
Double screw extruder extrusion temperature is 265 degrees Celsius in step (3), and screw speed is 80 revs/min.
Embodiment 2
A kind of preparation method of sole regnerated rubber powder, includes the following steps；
(1) it by after waste old sole clean and reuse, send to pulverizer and is crushed to 20 mesh, wherein with the removal of strong magnetic magnetic separator de-ironing
Iron filings impurity, obtains waste and old rubber particle；
(2) cleaning agent, polypropylene glycerol ether, epoxidized soybean oil and water are added into waste and old rubber particle to be uniformly mixed
Afterwards, it is placed in ball mill and carries out ground and cleaned, until more than waste and old rubber particle as low as 80 mesh greatly, filtering is cleaned repeatedly with clear water
4-6 is after, until being dried to moisture content lower than 5% in 90 degrees Celsius of baking oven；
(3) product of step (2) and initiator, second comonomer, maleic anhydride, age resister are added in high-speed mixer
60 degrees Celsius are warming up to after twenty minutes with the speed of 10 degrees celsius/minutes, extruding pelletization are added twin-screw extrude, through sink
It is granulated on pelleter after cooling；
(4) after pellet being cleaned 3 times with deionized water, under 90 degrees Celsius, after 20 hours dry, powder is sent into pulverizer
Pellet is broken to 300 mesh to get the sole reclaiming rubber powder.
The dosage quality of waste and old rubber particle, cleaning agent, polypropylene glycerol ether, epoxidized soybean oil and water in step (2)
It is formed than being mixed for 100:3:0.5:0.8:100.
The product and initiator of step (2) in step (3), second comonomer, maleic anhydride, age resister mass ratio be
100:5:5:8:4。
Initiator is potassium peroxydisulfate.
Second comonomer is triallyl cyanurate.
Age resister is that antioxidant and ultra-violet stabilizer are formed according to mass ratio 3:1 mixing.
Antioxidant is β-(3,5- di-tert-butyl-hydroxy phenyl) propionate.
Ultra-violet stabilizer is benzophenone.
Double screw extruder extrusion temperature is 272 degrees Celsius in step (3), and screw speed is 90 revs/min.
Embodiment 3
A kind of preparation method of sole regnerated rubber powder, includes the following steps；
(1) it by after waste old sole clean and reuse, send to pulverizer and is crushed to 15 mesh, wherein with the removal of strong magnetic magnetic separator de-ironing
Iron filings impurity, obtains waste and old rubber particle；
(2) cleaning agent, polypropylene glycerol ether, epoxidized soybean oil and water are added into waste and old rubber particle to be uniformly mixed
Afterwards, it is placed in ball mill and carries out ground and cleaned, until more than waste and old rubber particle as low as 80 mesh greatly, filtering cleans 5 with clear water repeatedly
After, until being dried to moisture content lower than 5% in 86 degrees Celsius of baking oven；
(3) product of step (2) and initiator, second comonomer, maleic anhydride, age resister are added in high-speed mixer
56 degrees Celsius are warming up to after 18 minutes with the speed of 10 degrees celsius/minutes, extruding pelletization are added twin-screw extrude, through sink
It is granulated on pelleter after cooling；
(4) after pellet being cleaned 3 times with deionized water, under 88 degrees Celsius, after 20 hours dry, powder is sent into pulverizer
Pellet is broken to 220 mesh to get the sole reclaiming rubber powder.
The dosage quality of waste and old rubber particle, cleaning agent, polypropylene glycerol ether, epoxidized soybean oil and water in step (2)
It is formed than being mixed for 100:3:0.5:0.8:100.
The product and initiator of step (2) in step (3), second comonomer, maleic anhydride, age resister mass ratio be
100:4:4:7:3。
Initiator is benzoyl peroxide.
Second comonomer is triallyl isocyanurate.
Age resister is that antioxidant and ultra-violet stabilizer are formed according to mass ratio 3:1 mixing.
Antioxidant is β-(3,5- di-tert-butyl-hydroxy phenyl) propionic acid octadecanol ester.
Ultra-violet stabilizer is benzotriazole.
Double screw extruder extrusion temperature is 268 degrees Celsius in step (3), and screw speed is 88 revs/min.
Embodiment 4
A kind of preparation method of sole regnerated rubber powder, includes the following steps；
(1) it by after waste old sole clean and reuse, send to pulverizer and is crushed to 18 mesh, wherein with the removal of strong magnetic magnetic separator de-ironing
Iron filings impurity, obtains waste and old rubber particle；
(2) cleaning agent, polypropylene glycerol ether, epoxidized soybean oil and water are added into waste and old rubber particle to be uniformly mixed
Afterwards, it is placed in ball mill and carries out ground and cleaned, until more than waste and old rubber particle as low as 80 mesh greatly, filtering cleans 6 with clear water repeatedly
After, until being dried to moisture content lower than 5% in 88 degrees Celsius of baking oven；
(3) product of step (2) and initiator, second comonomer, maleic anhydride, age resister are added in high-speed mixer
56 degrees Celsius are warming up to after 18 minutes with the speed of 10 degrees celsius/minutes, extruding pelletization are added twin-screw extrude, through sink
It is granulated on pelleter after cooling；
(4) after pellet being cleaned 3 times with deionized water, under 89 degrees Celsius, after 20 hours dry, powder is sent into pulverizer
Pellet is broken to 260 mesh to get the sole reclaiming rubber powder.
The dosage quality of waste and old rubber particle, cleaning agent, polypropylene glycerol ether, epoxidized soybean oil and water in step (2)
It is formed than being mixed for 100:3:0.5:0.8:100.
The product of step (2) in the step (3) and the quality of initiator, second comonomer, maleic anhydride, age resister
Than for 100:3.5:4.4:7:2.8.
Initiator is that benzoyl peroxide and methyl ethyl ketone peroxide are formed according to mass ratio 1:1 mixing.
Second comonomer is at least one of triallyl isocyanurate and triallyl cyanurate.
Age resister is that antioxidant and ultra-violet stabilizer are formed according to mass ratio 3:1 mixing.
Antioxidant is three (2,4- di-tert-butyl-phenyl) phosphites.
Ultra-violet stabilizer is group-substituted acrylonitrile.
Double screw extruder extrusion temperature is 268 degrees Celsius in step (3), and screw speed is 88 revs/min.
Sole reclaiming rubber powder is made in embodiment 1-4 and carries out service check, test result such as table 1
Table 1
| Inspection project | Standard value | Embodiment 1 | Embodiment 2 | Embodiment 3 | Embodiment 4 |
| Ash content, % | ≤8 | 7.2 | 6.8 | 6.5 | 6.9 |
| Rubber hydrocarbon content, % | ≥42 | 57 | 62 | 59 | 63 |
| Bulk density, kg/m3 | 260-460 | 328 | 334 | 331 | 329 |
| Tensile strength, MPa； | ≥15 | 21 | 19 | 22 | 24 |
| Elongation rate of tensile failure, % | ≥500 | 583 | 579 | 591 | 596 |
In conclusion the invention has the following advantages that
(1) present invention is grafted waste old by maleic anhydride, improves the mechanical property of waste old, improves waste old
Crack resistance and stretch-resistance, increase the recycling property of waste old, solve the problems, such as the recycling of waste old sole, save money
Source, it is environmentally protective.
(2) second comonomer triallyl isocyanurate and triallyl cyanurate contain the double bond there are three allyl,
Thus during rubber cross, it can play a part of increasing the degree of cross linking, i.e., under the initiation for crossing initiator, the two can increase
The effect for adding the degree of cross linking increases substantially the grafting rate of maleic anhydride, improves the flexibility and mechanical shock resistance of waste old,
Improve poor, the easy to crack disadvantage of waste old flexibility.
(3) present invention cleans waste old using cleaning agent, polypropylene glycerol ether, epoxidized soybean oil and water mixed grinding
Grain, can be enhanced the clean type of waste and old rubber particle, while softening waste and old rubber particle, improves the comprehensive of waste and old rubber particle
Energy.
The foregoing is only a preferred embodiment of the present invention, is not intended to restrict the invention, although referring to aforementioned reality
Applying example, invention is explained in detail, for those skilled in the art, still can be to aforementioned each implementation
Technical solution documented by example is modified or equivalent replacement of some of the technical features.It is all in essence of the invention
Within mind and principle, any modification, equivalent replacement, improvement and so on be should all be included in the protection scope of the present invention.
Claims (10)
1. a kind of preparation method of sole reclaiming rubber powder, which comprises the following steps:
(1) it by after waste old sole clean and reuse, send to pulverizer and is crushed to 10-20 mesh, wherein with the removal of strong magnetic magnetic separator de-ironing
Iron filings impurity, obtains waste and old rubber particle；
(2) after into waste and old rubber particle, addition cleaning agent, polypropylene glycerol ether, epoxidized soybean oil and water are uniformly mixed,
Ground and cleaned is carried out in merging ball mill, until more than waste and old rubber particle as low as 80 mesh greatly, filtering cleans 4-6 with clear water repeatedly
After, until being dried to moisture content lower than 5% in 80-90 degrees Celsius of baking oven；
(3) product of step (2) and initiator, second comonomer, maleic anhydride, age resister are added in high-speed mixer with 10
After the speed of degrees celsius/minute is warming up to 50-60 degrees Celsius of 15-20 minutes, extruding pelletization is added twin-screw extrude, through water
It is granulated on pelleter after slot is cooling；
(4) after pellet being cleaned 3 times with deionized water, under 85-90 degrees Celsius, after 20 hours dry, powder is sent into pulverizer
Pellet is broken to 150-300 mesh to get the sole reclaiming rubber powder.
2. the preparation method of sole reclaiming rubber powder according to claim 1, which is characterized in that the step (2)
In waste and old rubber particle, cleaning agent, polypropylene glycerol ether, epoxidized soybean oil and water dosage mass ratio be 100:3:0.5:
0.8:100 mixing composition.
3. the preparation method of sole reclaiming rubber powder according to claim 1, which is characterized in that the step (3)
In step (2) product and initiator, second comonomer, maleic anhydride, age resister mass ratio be 100:3-5:3-5:6-
8:2-4。
4. the preparation method of sole reclaiming rubber powder according to claim 3, which is characterized in that the step (3)
In step (2) product and initiator, second comonomer, maleic anhydride, age resister mass ratio be 100:3.5:4.4:7:
2.8。
5. the preparation method of sole reclaiming rubber powder according to claim 3, which is characterized in that the initiator is
One or more of ammonium persulfate, potassium peroxydisulfate, benzoyl peroxide, benzoyl peroxide and methyl ethyl ketone peroxide
In conjunction with.
6. the preparation method of sole reclaiming rubber powder according to claim 3, which is characterized in that second comonomer three
At least one of allyl chlorinated isocyanurates and triallyl cyanurate.
7. the preparation method of sole reclaiming rubber powder according to claim 3, which is characterized in that the age resister
It mixes and forms according to mass ratio 3:1 for antioxidant and ultra-violet stabilizer.
8. the preparation method of sole reclaiming rubber powder according to claim 7, which is characterized in that the antioxidant
For three (2,4- di-tert-butyl-phenyl) phosphites, β-(3,5- di-tert-butyl-hydroxy phenyl) propionate, β-
One or more of (3,5- di-tert-butyl-hydroxy phenyl) propionic acid octadecanol ester combines.
9. the preparation method of sole reclaiming rubber powder according to claim 7, which is characterized in that the ultraviolet light is steady
Determining agent is one or more of salicylic acid esters, benzophenone, benzotriazole, group-substituted acrylonitrile and triazines knot
It closes.
10. the preparation method of sole reclaiming rubber powder according to claim 1, which is characterized in that the step (3)
Middle double screw extruder extrusion temperature is 265-272 degrees Celsius, and screw speed is 80-90 revs/min.
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| CN111961268A (en) * | 2020-09-04 | 2020-11-20 | 石家庄硕若科技有限公司 | Preparation process of rubber powder with good wear resistance |
| CN112140606A (en) * | 2020-09-09 | 2020-12-29 | 瑞安市匡泰鞋业有限公司 | Sole production process |
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