CN111730786A - Method for preparing tire rubber powder with porous structure by wet grinding - Google Patents

Method for preparing tire rubber powder with porous structure by wet grinding Download PDF

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Publication number
CN111730786A
CN111730786A CN202010520711.7A CN202010520711A CN111730786A CN 111730786 A CN111730786 A CN 111730786A CN 202010520711 A CN202010520711 A CN 202010520711A CN 111730786 A CN111730786 A CN 111730786A
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tire
rubber powder
porous structure
temperature
waste
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CN202010520711.7A
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Chinese (zh)
Inventor
高玉斌
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Beijing Klintyre Environmental Protection Technology Co ltd
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Beijing Klintyre Environmental Protection Technology Co ltd
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Publication of CN111730786A publication Critical patent/CN111730786A/en
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    • BPERFORMING OPERATIONS; TRANSPORTING
    • B29WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
    • B29BPREPARATION OR PRETREATMENT OF THE MATERIAL TO BE SHAPED; MAKING GRANULES OR PREFORMS; RECOVERY OF PLASTICS OR OTHER CONSTITUENTS OF WASTE MATERIAL CONTAINING PLASTICS
    • B29B17/00Recovery of plastics or other constituents of waste material containing plastics
    • B29B17/04Disintegrating plastics, e.g. by milling
    • B29B17/0404Disintegrating plastics, e.g. by milling to powder
    • B29B17/0408Disintegrating plastics, e.g. by milling to powder using cryogenic systems
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B29WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
    • B29BPREPARATION OR PRETREATMENT OF THE MATERIAL TO BE SHAPED; MAKING GRANULES OR PREFORMS; RECOVERY OF PLASTICS OR OTHER CONSTITUENTS OF WASTE MATERIAL CONTAINING PLASTICS
    • B29B13/00Conditioning or physical treatment of the material to be shaped
    • B29B13/10Conditioning or physical treatment of the material to be shaped by grinding, e.g. by triturating; by sieving; by filtering
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B29WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
    • B29BPREPARATION OR PRETREATMENT OF THE MATERIAL TO BE SHAPED; MAKING GRANULES OR PREFORMS; RECOVERY OF PLASTICS OR OTHER CONSTITUENTS OF WASTE MATERIAL CONTAINING PLASTICS
    • B29B17/00Recovery of plastics or other constituents of waste material containing plastics
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B29WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
    • B29BPREPARATION OR PRETREATMENT OF THE MATERIAL TO BE SHAPED; MAKING GRANULES OR PREFORMS; RECOVERY OF PLASTICS OR OTHER CONSTITUENTS OF WASTE MATERIAL CONTAINING PLASTICS
    • B29B17/00Recovery of plastics or other constituents of waste material containing plastics
    • B29B17/04Disintegrating plastics, e.g. by milling
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08JWORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
    • C08J11/00Recovery or working-up of waste materials
    • C08J11/02Recovery or working-up of waste materials of solvents, plasticisers or unreacted monomers
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B29WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
    • B29BPREPARATION OR PRETREATMENT OF THE MATERIAL TO BE SHAPED; MAKING GRANULES OR PREFORMS; RECOVERY OF PLASTICS OR OTHER CONSTITUENTS OF WASTE MATERIAL CONTAINING PLASTICS
    • B29B17/00Recovery of plastics or other constituents of waste material containing plastics
    • B29B2017/001Pretreating the materials before recovery
    • B29B2017/0015Washing, rinsing
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B29WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
    • B29BPREPARATION OR PRETREATMENT OF THE MATERIAL TO BE SHAPED; MAKING GRANULES OR PREFORMS; RECOVERY OF PLASTICS OR OTHER CONSTITUENTS OF WASTE MATERIAL CONTAINING PLASTICS
    • B29B17/00Recovery of plastics or other constituents of waste material containing plastics
    • B29B17/04Disintegrating plastics, e.g. by milling
    • B29B2017/0416Cooling the plastics before disintegration, e.g. freezing
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B29WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
    • B29BPREPARATION OR PRETREATMENT OF THE MATERIAL TO BE SHAPED; MAKING GRANULES OR PREFORMS; RECOVERY OF PLASTICS OR OTHER CONSTITUENTS OF WASTE MATERIAL CONTAINING PLASTICS
    • B29B17/00Recovery of plastics or other constituents of waste material containing plastics
    • B29B17/04Disintegrating plastics, e.g. by milling
    • B29B2017/0424Specific disintegrating techniques; devices therefor
    • B29B2017/0476Cutting or tearing members, e.g. spiked or toothed cylinders or intermeshing rollers
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08JWORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
    • C08J2389/00Characterised by the use of proteins; Derivatives thereof
    • YGENERAL 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
    • Y02TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02WCLIMATE CHANGE MITIGATION TECHNOLOGIES RELATED TO WASTEWATER TREATMENT OR WASTE MANAGEMENT
    • Y02W30/00Technologies for solid waste management
    • Y02W30/50Reuse, recycling or recovery technologies
    • Y02W30/52Mechanical processing of waste for the recovery of materials, e.g. crushing, shredding, separation or disassembly
    • YGENERAL 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
    • Y02TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02WCLIMATE CHANGE MITIGATION TECHNOLOGIES RELATED TO WASTEWATER TREATMENT OR WASTE MANAGEMENT
    • Y02W30/00Technologies for solid waste management
    • Y02W30/50Reuse, recycling or recovery technologies
    • Y02W30/62Plastics recycling; Rubber recycling

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  • Engineering & Computer Science (AREA)
  • Mechanical Engineering (AREA)
  • Environmental & Geological Engineering (AREA)
  • Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Medicinal Chemistry (AREA)
  • Polymers & Plastics (AREA)
  • Organic Chemistry (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Health & Medical Sciences (AREA)
  • Sustainable Development (AREA)
  • Disintegrating Or Milling (AREA)
  • Separation, Recovery Or Treatment Of Waste Materials Containing Plastics (AREA)

Abstract

The invention discloses a method for preparing tire rubber powder with a porous structure by wet grinding, which comprises the steps of swelling a coarsely ground waste tire block by using an organic solvent at normal temperature, performing active treatment under the action of ultrasonic waves, and then performing low-temperature grinding on the precooled waste tire block to obtain the porous tire rubber powder. The rubber powder is soaked in an organic solvent for swelling, small molecules of the solvent diffuse to gaps among large rubber molecules, and the three-dimensional crosslinked network of the large rubber molecules is gradually expanded, so that the glass transition temperature of the tire rubber is reduced, waste tire particles can be converted into an embrittled state in a short time, the crushing difficulty is reduced, and the production efficiency of fine rubber powder is improved; after the solvent is volatilized, rich pore structures are formed on the surface and inside of the rubber powder, the specific surface area is larger, and the performance of the rubber powder is improved.

Description

Method for preparing tire rubber powder with porous structure by wet grinding
Technical Field
The invention relates to the technical field of tire rubber powder preparation, in particular to a method for preparing tire rubber powder with a porous structure by wet grinding.
Background
Along with the improvement of the living standard of people, more and more families or individuals buy automobiles, the using amount of the automobiles is increased year by year, meanwhile, the scrapping amount of the automobiles is increased year by year, corresponding waste tires are also generated in large quantity, the tires are mainly made of rubber, if the tires are directly discarded, on one hand, the rubber material is difficult to degrade, and great harm is caused to the environment, on the other hand, the production of the natural rubber is increasingly restricted by forest resources, and the development requirements of the existing industry cannot be met. Therefore, the recycling of the waste tires is significant.
At present, there are two technical methods for crushing waste rubber tires without pollution at home and abroad, namely: the normal-temperature mechanical crushing method has the defects that high heat is generated in the process of grinding rubber particles, the higher the grinding temperature is along with the thinner the rubber powder required to be ground, the higher the temperature generated by the friction between a grinding head and the rubber particles with strong elasticity is, and the coking phenomenon of the rubber powder is often generated, so that products become waste products; in addition, the low-temperature mechanical pulverization method is a method in which a rubber is embrittled by a pulverizer at a low temperature of about-120 ℃ to a glass transition temperature and then pulverized by a mechanical force. The crushing method has low brittle temperature, large energy consumption, low production of fine rubber powder and poor economic benefit, and influences the service life of the crusher hammer head.
Disclosure of Invention
The invention aims to provide a method for preparing tire rubber powder with a porous structure by wet grinding, which reduces the grinding difficulty of waste tires, obtains the tire rubber powder with the porous structure and improves the service performance of the tire rubber powder.
The invention is realized by adopting the following technical scheme:
a method for preparing tire rubber powder with a porous structure by wet grinding comprises the steps of swelling coarsely ground waste tire blocks by using an organic solvent at normal temperature, performing active treatment under the action of ultrasonic waves, and then grinding precooled waste tire blocks at low temperature to obtain the porous tire rubber powder.
The method specifically comprises the following steps:
(1) cleaning and drying the waste tires, primarily crushing the waste tires into particles with the size of 30-50 meshes, then placing the waste tire blocks into an organic solvent, and swelling the waste tire blocks for 10-18 h under the conditions of normal temperature and normal pressure;
(2) carrying out ultrasonic activation treatment for 4-12 h at 40-60 ℃, and after stopping ultrasonic treatment, continuing standing and swelling for 12-36 h;
(3) rapidly cooling the swelled waste tire blocks in a short time by adopting a liquid nitrogen cooling mode;
(4) then placing the pre-cooled waste tire blocks into crushing equipment for low-temperature fine crushing treatment, and inputting compressed cold air into the crushing equipment while crushing to keep the internal temperature of the crushing equipment at-10 ℃ to-5 ℃;
(5) sieving and drying the crushed waste tire rubber powder to obtain the tire rubber powder with the particle size of 150-200-mesh porous structure.
Further, the mass ratio of the waste tire blocks to the organic solvent in the step (1) is 1: (10-20).
Further, the organic solvent is one or more of n-heptane, n-octane, cyclohexane, toluene, xylene, ethyl acetate or dibutyl phthalate.
Furthermore, the organic solvent is toluene, and the using amount of the organic solvent is 1-1.2 times of the mass of the waste tire blocks.
Further, after the waste tire block is subjected to swelling-activating-swelling treatment, the swollen tire block is expanded to 4 to 8 times.
Further, in the liquid nitrogen cooling treatment in the step (3), the swelled tire block is frozen for 3-10s in a liquid nitrogen environment to obtain a pre-cooled tire block.
Further, before the low-temperature fine grinding in the step (4), the pre-cooled tire particles are rolled by using a roller and ground to obtain uniform cold and brittle tire particles, and then the low-temperature fine grinding treatment is performed.
Further, preparation of compressed cold air in step (4): the air is compressed by an air compressor, enters an air storage tank, is filtered by an air filter, is dried by an air dryer, and is refrigerated by a turbine refrigerator to obtain low-temperature air with the temperature of-5 to-15 ℃.
Compared with the prior art, the invention has the following advantages:
1. the waste tire rubber is soaked in the organic solvent for swelling, the small molecules of the solvent diffuse to the gaps of the large molecules of the rubber, and the three-dimensional crosslinked network of the large molecules of the rubber is gradually expanded, so that the waste tire rubber particles are expanded, the glass transition temperature of the tire rubber is reduced, the cost and the difficulty of low-temperature crushing treatment are reduced, and the crushing efficiency is improved.
2. The temperature requirement for low-temperature crushing of the waste tires after swelling treatment is reduced, liquid nitrogen is adopted for rapid cooling, waste tire particles can be converted into an embrittled state in a short time, the production efficiency of fine rubber powder is improved through treatment of a crusher, the production capacity of the fine rubber powder is greatly improved, low-temperature air is used as a cold source during treatment of the crusher, the tire particles are kept in the embrittled state, a large amount of liquid nitrogen is not required for ultralow-temperature cooling, and the crushing difficulty and the production cost are reduced.
3. After swelling treatment, the micromolecular solvent is uniformly dispersed in the tire rubber block, and after crushing and drying treatment, the solvent is volatilized to form rich pore structures on the surface and inside of the rubber powder, so that the specific surface area is larger, the performance of the rubber powder is improved, and the bonding with other rubber materials is facilitated.
4. Under the action of ultrasound, the uniform diffusion of the solvent is promoted, the swelling time is shortened, and the problem of poor activity of tire rubber powder is solved by activating the rubber powder by using ultrasound.
Detailed Description
The technical solution of the present patent will be described in further detail with reference to the following embodiments.
The following detailed description of embodiments of the present patent is, therefore, to be construed as merely illustrative, and not limitative of the remainder of the disclosure.
Example 1
A method for preparing tire rubber powder with a porous structure by wet grinding specifically comprises the following steps:
(1) cleaning and drying waste tires, primarily crushing the waste tires into particles with the size of 30-50 meshes, then putting the waste tire blocks into an organic solvent, and swelling the waste tire blocks for 12 hours under the conditions of normal temperature and normal pressure;
wherein the organic solvent is toluene, and the using amount of the organic solvent is 1.2 times of the mass of the waste tire blocks;
(2) carrying out ultrasonic activation for 8 hours at the temperature of 40-60 ℃, stopping ultrasonic treatment, and continuing standing and swelling for 24 hours;
wherein, after the waste tire blocks are subjected to swelling-activating-swelling treatment, the swollen tire blocks are expanded to 4 to 8 times;
(3) rapidly cooling the swelled waste tire blocks in a short time by adopting a liquid nitrogen cooling mode, and freezing the swelled tire blocks for 3-10s in a liquid nitrogen environment to obtain pre-cooled tire blocks;
(4) rolling the precooled tire particles by using a rolling shaft, crushing the precooled tire particles to obtain cold and brittle tire particles with uniform particles, and then performing low-temperature fine crushing treatment; placing the cold and brittle tire particles into crushing equipment, performing low-temperature fine crushing treatment, and inputting compressed cold air into the crushing equipment while crushing to keep the internal temperature of the crushing equipment at-10 ℃ to-5 ℃;
wherein, the air enters the air storage tank after being compressed by the air compressor, is filtered by the air filter, is dried by the air dryer, and is refrigerated by the turbine refrigerator to obtain the low-temperature cold air with the temperature of minus 5 to minus 15 ℃.
(5) Sieving and drying the crushed waste tire rubber powder to obtain the tire rubber powder with the particle size of 150-200-mesh porous structure.
Example 2
A method for preparing tire rubber powder with a porous structure by wet grinding specifically comprises the following steps:
(1) cleaning and drying the waste tires, primarily crushing the waste tires into particles with the size of 30-50 meshes, then placing the waste tire blocks into toluene, wherein the using amount of the waste tire blocks is 1.2 times of the mass of the waste tire blocks, and swelling the waste tire blocks for 12 hours under the conditions of normal temperature and normal pressure;
(2) carrying out ultrasonic activation for 4 hours at the temperature of 40-60 ℃, stopping ultrasonic treatment, and continuing standing and swelling for 24 hours;
(3) freezing the swelled tire block in a liquid nitrogen environment for 3-10s to obtain a pre-cooled tire block;
(4) placing the cold and brittle tire particles into crushing equipment, performing low-temperature fine crushing treatment, and inputting compressed cold air into the crushing equipment while crushing to keep the internal temperature of the crushing equipment at-10 ℃ to-5 ℃;
wherein, the air enters the air storage tank after being compressed by the air compressor, is filtered by the air filter, is dried by the air dryer, and is refrigerated by the turbine refrigerator to obtain the low-temperature cold air with the temperature of minus 5 to minus 15 ℃.
(5) Sieving and drying the crushed waste tire rubber powder to obtain the tire rubber powder with the particle size of 150-200-mesh porous structure.
Example 3
Directly mechanically crushing the waste tires, and sieving to obtain 150-200-mesh tire rubber powder.
The rubber powders prepared in examples 1, 2 and 3 were tested, and example 3 was used as a control.
The internal pore size distribution and specific surface area are shown in the following table:
Figure BDA0002531934370000041
the foregoing is a more detailed description of the invention in connection with specific preferred embodiments and it is not intended that the invention be limited to these specific details. For those skilled in the art to which the invention pertains, several equivalent substitutions or obvious modifications can be made without departing from the spirit of the invention, and all the properties or uses are considered to be within the scope of the invention.

Claims (9)

1. A method for preparing tire rubber powder with a porous structure by wet grinding is characterized in that under the condition of normal temperature, organic solvent is used for carrying out swelling treatment on waste tire blocks after coarse grinding, meanwhile, activation treatment is carried out under the action of ultrasonic waves, and then, precooled waste tire blocks are subjected to low-temperature grinding treatment to obtain the porous tire rubber powder.
2. The method for preparing the tire rubber powder with the porous structure by wet grinding as claimed in claim 1, is characterized by comprising the following steps:
(1) cleaning and drying the waste tires, primarily crushing the waste tires into particles with the size of 30-50 meshes, then placing the waste tire blocks into an organic solvent, and swelling the waste tire blocks for 10-18 h under the conditions of normal temperature and normal pressure;
(2) carrying out ultrasonic activation treatment for 4-12 h at 40-60 ℃, and after stopping ultrasonic treatment, continuing standing and swelling for 12-36 h;
(3) rapidly cooling the swelled waste tire blocks in a short time by adopting a liquid nitrogen cooling mode;
(4) then placing the pre-cooled waste tire blocks into crushing equipment for low-temperature fine crushing treatment, and inputting compressed cold air into the crushing equipment while crushing to keep the internal temperature of the crushing equipment at-10 ℃ to-5 ℃;
(5) sieving and drying the crushed waste tire rubber powder to obtain the tire rubber powder with the particle size of 150-200-mesh porous structure.
3. The method for preparing the tire rubber powder with the porous structure by wet grinding as claimed in claim 2, wherein the mass ratio of the waste tire blocks to the organic solvent in the step (1) is 1: (10-20).
4. The method for preparing the tire rubber powder with the porous structure by wet grinding as claimed in claim 2 or 3, wherein the organic solvent is one or more of n-heptane, n-octane, cyclohexane, toluene, xylene, ethyl acetate or dibutyl phthalate.
5. The method for preparing the tire rubber powder with the porous structure by wet grinding as claimed in claim 4, wherein the organic solvent is toluene, and the use amount of the toluene is 1-1.2 times of the mass of the waste tire blocks.
6. The method for preparing the tire rubber powder with the porous structure by wet grinding as claimed in claim 2, wherein the swollen tire block is expanded to 4-8 times after the swelling-activating-swelling treatment of the waste tire block.
7. The method for preparing the tire rubber powder with the porous structure by wet grinding as claimed in claim 2, wherein in the step (3) of liquid nitrogen cooling treatment, the swollen tire block is frozen in a liquid nitrogen environment for 3-10s to obtain a pre-cooled tire block.
8. The method for preparing the tire rubber powder with the porous structure by wet grinding as claimed in claim 7, wherein before the step (4) of low-temperature fine grinding, the precooled tire particles are rolled by a roller to be ground to obtain cold and brittle tire particles with uniform particles, and then the low-temperature fine grinding treatment is carried out.
9. The method for preparing the tire rubber powder with the porous structure by wet grinding as claimed in claim 2, wherein the preparation of the compressed cold air in the step (4): the air is compressed by an air compressor, enters an air storage tank, is filtered by an air filter, is dried by an air dryer, and is refrigerated by a turbine refrigerator to obtain low-temperature air with the temperature of-5 to-15 ℃.
CN202010520711.7A 2020-06-10 2020-06-10 Method for preparing tire rubber powder with porous structure by wet grinding Pending CN111730786A (en)

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN113583524A (en) * 2021-09-16 2021-11-02 金川集团股份有限公司 Preparation method of coating-grade chlorinated polyvinyl chloride resin
WO2022221780A3 (en) * 2021-04-12 2022-12-08 Illinois Tool Works Inc. Solutions for solvent swelling and solvent bonding

Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1215651A (en) * 1997-10-23 1999-05-05 烟台思可达高新技术中试有限公司 Method and apparatus for treatment of waste steel wire tyre and recovery of fine rubber powder by air refrigerating
CN1325917A (en) * 2000-05-29 2001-12-12 刘扬生 Process for regenerating waste or used rubber
CN104151598A (en) * 2014-07-25 2014-11-19 南京红太阳新材料有限公司 Method for preparing porous microspheres from waste rubber
CN107234748A (en) * 2017-06-29 2017-10-10 安徽中宏橡塑有限公司 A kind of method that normal temperature prepares junked tire fine glue powder with low-temperature phase combination crushing

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1215651A (en) * 1997-10-23 1999-05-05 烟台思可达高新技术中试有限公司 Method and apparatus for treatment of waste steel wire tyre and recovery of fine rubber powder by air refrigerating
CN1325917A (en) * 2000-05-29 2001-12-12 刘扬生 Process for regenerating waste or used rubber
CN104151598A (en) * 2014-07-25 2014-11-19 南京红太阳新材料有限公司 Method for preparing porous microspheres from waste rubber
CN107234748A (en) * 2017-06-29 2017-10-10 安徽中宏橡塑有限公司 A kind of method that normal temperature prepares junked tire fine glue powder with low-temperature phase combination crushing

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2022221780A3 (en) * 2021-04-12 2022-12-08 Illinois Tool Works Inc. Solutions for solvent swelling and solvent bonding
CN113583524A (en) * 2021-09-16 2021-11-02 金川集团股份有限公司 Preparation method of coating-grade chlorinated polyvinyl chloride resin

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