CN115960389A - Method for preparing desulfurized rubber powder through self-friction heat generation - Google Patents
Method for preparing desulfurized rubber powder through self-friction heat generation Download PDFInfo
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- CN115960389A CN115960389A CN202310091333.9A CN202310091333A CN115960389A CN 115960389 A CN115960389 A CN 115960389A CN 202310091333 A CN202310091333 A CN 202310091333A CN 115960389 A CN115960389 A CN 115960389A
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- 229920001971 elastomer Polymers 0.000 title claims abstract description 73
- 239000005060 rubber Substances 0.000 title claims abstract description 73
- 239000000843 powder Substances 0.000 title claims abstract description 51
- 238000000034 method Methods 0.000 title claims abstract description 34
- 230000020169 heat generation Effects 0.000 title claims abstract description 12
- 239000000463 material Substances 0.000 claims abstract description 30
- 239000002699 waste material Substances 0.000 claims abstract description 23
- 238000006477 desulfuration reaction Methods 0.000 claims abstract description 20
- 230000023556 desulfurization Effects 0.000 claims abstract description 20
- 238000007599 discharging Methods 0.000 claims abstract description 15
- 238000003756 stirring Methods 0.000 claims abstract description 14
- 230000008569 process Effects 0.000 claims abstract description 13
- 230000009471 action Effects 0.000 claims abstract description 12
- 238000002156 mixing Methods 0.000 claims abstract description 8
- 230000008929 regeneration Effects 0.000 claims abstract description 7
- 238000011069 regeneration method Methods 0.000 claims abstract description 7
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 25
- 229910052757 nitrogen Inorganic materials 0.000 claims description 12
- 239000011295 pitch Substances 0.000 claims description 7
- 239000010920 waste tyre Substances 0.000 claims description 6
- 239000004902 Softening Agent Substances 0.000 claims description 5
- 238000007789 sealing Methods 0.000 claims description 5
- 239000010692 aromatic oil Substances 0.000 claims description 4
- 239000002245 particle Substances 0.000 claims description 4
- 239000011297 pine tar Substances 0.000 claims description 3
- 229940068124 pine tar Drugs 0.000 claims description 3
- 239000000126 substance Substances 0.000 claims description 3
- 229920005549 butyl rubber Polymers 0.000 claims description 2
- 239000003784 tall oil Substances 0.000 claims description 2
- 229910001873 dinitrogen Inorganic materials 0.000 claims 1
- 238000005265 energy consumption Methods 0.000 abstract description 8
- 238000001816 cooling Methods 0.000 abstract description 6
- 239000012492 regenerant Substances 0.000 abstract description 6
- 238000004064 recycling Methods 0.000 abstract description 3
- 238000013461 design Methods 0.000 abstract description 2
- 238000009775 high-speed stirring Methods 0.000 abstract 1
- 239000012299 nitrogen atmosphere Substances 0.000 abstract 1
- 238000006243 chemical reaction Methods 0.000 description 5
- 239000010426 asphalt Substances 0.000 description 3
- 239000003795 chemical substances by application Substances 0.000 description 3
- 230000000052 comparative effect Effects 0.000 description 3
- 230000000694 effects Effects 0.000 description 3
- 238000004519 manufacturing process Methods 0.000 description 3
- 229920003052 natural elastomer Polymers 0.000 description 3
- 229920001194 natural rubber Polymers 0.000 description 3
- 239000012466 permeate Substances 0.000 description 3
- 239000002994 raw material Substances 0.000 description 3
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 2
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 description 2
- 244000043261 Hevea brasiliensis Species 0.000 description 2
- 229910052799 carbon Inorganic materials 0.000 description 2
- 238000004134 energy conservation Methods 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 230000007613 environmental effect Effects 0.000 description 2
- 238000006386 neutralization reaction Methods 0.000 description 2
- 230000003647 oxidation Effects 0.000 description 2
- 238000007254 oxidation reaction Methods 0.000 description 2
- 239000000047 product Substances 0.000 description 2
- 229920003051 synthetic elastomer Polymers 0.000 description 2
- 239000005061 synthetic rubber Substances 0.000 description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 2
- 238000009825 accumulation Methods 0.000 description 1
- 230000003213 activating effect Effects 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 229910002092 carbon dioxide Inorganic materials 0.000 description 1
- 239000001569 carbon dioxide Substances 0.000 description 1
- 230000002860 competitive effect Effects 0.000 description 1
- 238000010924 continuous production Methods 0.000 description 1
- 239000002826 coolant Substances 0.000 description 1
- 239000011258 core-shell material Substances 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 230000018109 developmental process Effects 0.000 description 1
- 230000003631 expected effect Effects 0.000 description 1
- 239000003292 glue Substances 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 230000008595 infiltration Effects 0.000 description 1
- 238000001764 infiltration Methods 0.000 description 1
- 229920000126 latex Polymers 0.000 description 1
- 239000004816 latex Substances 0.000 description 1
- 230000007246 mechanism Effects 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 239000003921 oil Substances 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 238000004321 preservation Methods 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 238000007670 refining Methods 0.000 description 1
- 238000010008 shearing Methods 0.000 description 1
- 230000008961 swelling Effects 0.000 description 1
- 238000012546 transfer Methods 0.000 description 1
- 230000009466 transformation Effects 0.000 description 1
- 239000002912 waste gas Substances 0.000 description 1
Classifications
-
- 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
Landscapes
- Separation, Recovery Or Treatment Of Waste Materials Containing Plastics (AREA)
Abstract
A method for preparing desulfurized rubber powder by self-friction heat generation, belonging to the field of waste rubber recycling. The method comprises the steps of adding waste rubber powder and a regenerant into a first high-speed stirrer by utilizing two serially-connected stirrers with different configurations, realizing uniform mixing, permeation and temperature rise of materials under the self-friction action of high-speed stirring, then butting and discharging the materials into a second stirrer, carrying out low-speed stirring under the nitrogen atmosphere to realize desulfurization and regeneration of the waste rubber, and finally discharging the waste rubber after cooling to obtain the desulfurized rubber powder. Through being provided with the mixer of two kinds of different functions, satisfied the control by temperature change demand of the different stages of desulfurization, simplified technical equipment, avoided the structural design that other methods are complicated, more can adapt to the trade demand. By optimizing the formula and the working procedures and reasonably designing the process flow, the energy consumption is greatly reduced.
Description
Technical Field
The invention belongs to the field of recycling of waste rubber, and particularly relates to a method for preparing desulfurized rubber powder by self-friction heat generation.
Background
As a strategic resource, the total yield of the imported natural and synthetic rubber (containing latex) in 2020 by China is 746.8 ten thousand tons, the total yield of the natural rubber in 2020 by China is only 69.3 ten thousand tons, the self-sufficiency rate is very low, and the requirement of the rubber industry in China can not be met. The reclaimed rubber is used as a resource disposal priority direction and a main force army, which is also determined by the national conditions of China. Reclaimed rubber is listed as a resource of the rubber industry in three war ages by the Ministry of industry and Ministry of industry of China together with synthetic rubber and natural rubber in 2012. Incomplete statistics shows that the yield of the regenerated rubber in China reaches 460 ten thousand tons in 2021.
Through development and technical innovation for many years, the reclaimed rubber industry forms a desulfurization regeneration process mainly based on high-temperature high-pressure dynamic desulfurization. The desulfurization reaction is completed in a desulfurization tank, a regenerant and water are added into the desulfurization tank together, the working pressure is about 2.2MPa, the working temperature is about 220 ℃, the desulfurization time is about 3 hours, the materials are taken after pressure relief and cooling to obtain desulfurized rubber powder, and then the desulfurized rubber powder is tabletted by 3 to 4 high-speed refiners to obtain reclaimed rubber. From the view of desulfurization reaction mechanism, the high-temperature high-pressure dynamic desulfurization belongs to chemical regeneration, namely under the action of external heat, an activating agent permeates and enters the waste rubber to react with the waste rubber under the assistance of a softening agent, and a cross-linked network is destroyed, so that the waste rubber becomes a quasi-linear and reprocessable process. However, the permeation of the regenerant into the waste rubber is completed within a long time at high temperature and high pressure by using the method, so that serious potential safety hazards exist, and the energy consumption is high.
The traditional desulfurization mode is actively improved in the industry at present, high temperature high pressure dynamic digester is gradually eliminated by the market, and partial technology is in the mode of simulating the working of digester, and through changing the external form and trying to obtain a substitute, such as fedli et al (CN 210314088U, a reclaimed rubber desulfurization machine) including the shell body, rotate the interior casing of installing inside the shell body and set up the (mixing) shaft in the interior casing inside. The inner shell drives the regenerated rubber to rotate in the inner shell, and the outer shell still comprises a controller, a heating device, a temperature sensor and a cooling device. The essence of the method is to simulate the working principle of a dynamic devulcanizer: the materials are stirred in the tank body and a series of reactions are carried out under the action of an external heater. The problem that it had to be solved is "avoided prior art to lead to reclaimed rubber at the desulfurization machine bottom accumulation, stirs inadequately" problem, and the stirring effect of its setting is also in order to "avoid useless reclaimed rubber to glue the conglomeration. Zhang gang et al (CN 102977404B, a method for continuously preparing reclaimed rubber by using double-stage double-screw extruder) pretreats waste rubber powder and a reclaiming agent in a stirrer, stands at high temperature to enable the reclaiming agent to fully permeate the swelling rubber powder, and then adds a counter-rotating double-screw extruder to replace the traditional high-temperature high-pressure dynamic reaction tank, and desulfurized rubber powder enters a co-rotating double-screw extruder to exert high shearing action at low temperature to replace a refiner. The viscosity of the regenerant is still high under the condition of 50-100 ℃, the infiltration can be completed only by standing for 12h-36h, the intermittent operation production efficiency is low, the heat preservation time at high temperature is long, and the energy consumption is large; the heat in the incongruous twin-screw is still transferred from the outside of the rubber powder to the inside, and a core-shell structure is inevitably existed, so that the mechanical property is poor, and the energy consumption in the refining process of the same-direction twin-screw is still large.
The carbon dioxide emission in China strives to reach a peak value 2030 years ago, and strives to achieve carbon neutralization 2060 years ago. At present, both the produced product and the production method are in the important stage of upgrading transformation. The energy conservation and consumption reduction are realized in the process of recycling the waste rubber, the carbon neutralization index is met, and the new situation can be more competitive.
Disclosure of Invention
In order to solve the defects existing in the background, the invention aims to provide a method for preparing desulfurized rubber powder by utilizing self-friction heat generation, and the method has the advantages of continuous process, environmental protection, simple operation and outstanding high-efficiency and energy-saving effects.
In order to achieve the purpose, the technical solution of the invention is as follows:
a method for preparing desulfurized rubber powder by self-friction heat generation comprises the following steps: quantifying by an automatic metering device to obtain a mass ratio of 100: adding the rubber powder and a softening agent into a first stirrer, stirring and mixing the materials within 2 to 3min, raising the temperature of the materials to 180 to 250 ℃ under the action of self-friction heat generation, discharging volatile low-molecular substances at the temperature to obtain a primarily desulfurized material, directly discharging the primarily desulfurized material into a second stirrer through a continuous sealing device, continuously injecting nitrogen into the second stirrer through an air inlet hole formed in the stirrer in the stirring process, preserving the heat for 10 to 20min to realize desulfurization regeneration of the waste rubber, and finally discharging the material after the temperature of the material is reduced to below 50 ℃ to obtain the desulfurized rubber powder.
The preferable rubber powder is waste tire rubber powder or waste butyl rubber powder, and the particle size is 20 to 60 meshes.
Preferably, the softening agent is one or a mixture of more of pine tar pitch, tall oil pitch or aromatic oil pitch.
Preferably, the speed of the first stirrer is 400 to 800 revolutions per minute, and the speed of the second stirrer is 20 to 50 revolutions per minute.
The preferable injected nitrogen is normal pressure, and the mass ratio of the injected nitrogen to rubber powder is 0.001-0.003%.
The preferable Mooney viscosity of the desulfurized rubber powder after being discharged is 80 to 150.
Advantageous effects
1. The invention mixes the regenerant and the waste rubber powder at a proper temperature, realizes uniform mixing in the stirring process of a first high-speed stirrer, simultaneously fully permeates the regenerant into the waste rubber powder, simultaneously removes low components of the waste rubber powder fully, takes away waste gas generated by desulfurization while introducing nitrogen continuously to isolate oxygen after the fully swelled mixed oil rubber powder enters a second low-speed stirrer, mixes the materials again under the control of proper rotating speed, further improves the uniformity, and finally slowly and uniformly cools under the action of a cooling medium to finally obtain the required desulfurized rubber powder. In combination with the production practice of rubber powder in the industry, the waste rubber powder with different particle sizes is selected as a raw material, and under the action of a first high-speed stirrer, the uniform mixing, permeation and temperature rise of materials can be realized, so that the oxidation of the materials caused by overlong time is avoided; the second stirrer controls the rotation speed, temperature and time to ensure the macro and micro desulfurization uniformity of the waste rubber powder.
2. Through the mixer of two kinds of different functions of reasonable matching, satisfied intensification and heat retaining demand, the equipment that relates adopts present or slightly revise on the market can use, has simplified current waste rubber desulfurization regeneration technology equipment, has avoided the structural design that other methods are complicated, more can adapt to the trade demand. By optimizing the formula and the working procedures and reasonably designing the process flow, the whole preparation flow is completed under a closed condition, and the energy consumption is greatly reduced. Has the advantages of safe, simple and continuous operation, energy conservation and environmental protection.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments.
In the description of the present invention, it is to be understood that the terms "disposed," "mounted," "connected," and "fixed" are used broadly herein, and may be, for example, either fixedly or removably connected, unless otherwise specifically stated or limited; may be a mechanical connection; may be directly connected or indirectly connected through an intermediate. The specific meanings of the above terms in the present invention can be understood according to specific situations by those of ordinary skill in the art.
Furthermore, the terms "first", "second" and "first" are used for descriptive purposes only and are not to be construed as indicating or implying relative importance or implicitly indicating the number of technical features indicated. Thus, a feature defined as "first" or "second" may explicitly or implicitly include one or more of that feature, and in the description of the invention, "plurality" means two or more unless explicitly defined otherwise.
According to the invention, the waste rubber powder with different particle sizes is selected as a raw material, and under the action of the first high-speed stirrer, uniform mixing, permeation and temperature rise of materials can be realized, so that the oxidation of the materials caused by overlong time is avoided; the second stirrer controls the rotating speed, temperature and time to ensure the macroscopic and microscopic desulfurization uniformity of the waste rubber powder, and simultaneously, the addition of nitrogen effectively improves the problem of mass and heat transfer in the traditional desulfurization regeneration process, the performance of the desulfurized rubber powder is excellent, the selected equipment is conventional equipment in the field, or the selected equipment is slightly improved so as to meet the reaction conditions of the invention without specific limitation.
Example 1
Quantitatively adding 100phr of waste tire tread rubber powder at room temperature and 15phr of aromatic oil asphalt at 120 ℃ into a first stirrer through an automatic metering device, setting the rotating speed to be 500 revolutions per minute, directly discharging the materials into a second stirrer through a continuous sealing device when the temperature of the materials reaches 180 ℃ under the action of self-friction heat generation within 2 minutes, continuously injecting nitrogen at normal pressure through an air inlet arranged on the stirrer in the stirring process of the second stirrer, wherein the mass ratio of the nitrogen introduction amount to the rubber powder is 0.001%, stirring the materials for 10 minutes by the second stirrer at 20 revolutions per minute, then cooling, and discharging the desulfurized rubber powder with the Mooney viscosity of 140 when the temperature reaches 53 ℃.
Example 2
Quantitatively adding 100phr of waste tire tread rubber powder at room temperature and 10phr of 80 ℃ pine tar pitch into a first stirrer by an automatic metering device, setting the rotating speed to 600 revolutions per minute, directly discharging the materials into a second stirrer by a continuous sealing device when the temperature reaches 200 ℃ under the action of self-friction heat generation in 2.5 minutes, continuously injecting nitrogen at normal pressure through an air inlet arranged on the stirrer in the stirring process of the second stirrer, wherein the mass ratio of the nitrogen introduction amount to the rubber powder is 0.003 percent, stirring the materials by the second stirrer for 15 minutes at 50 revolutions per minute, then cooling, and discharging desulfurized rubber powder with Mooney viscosity of 90 when the temperature reaches 43 ℃.
Example 3
Quantitatively adding 100phr of waste tire tread rubber powder at room temperature and 2phr of 90 ℃ Tuell asphalt into a first stirrer through an automatic metering device, setting the rotating speed to be 800 revolutions per minute, directly discharging the materials into a second stirrer through a continuous sealing device when the temperature of the materials reaches 220 ℃ under the action of self-friction heat generation within 3 minutes, continuously injecting nitrogen at normal pressure through an air inlet arranged on the stirrer in the stirring process of the second stirrer, wherein the mass ratio of the nitrogen introduction amount to the rubber powder is 0.002 percent, stirring the materials for 20 minutes by the second stirrer at 30 revolutions per minute, then cooling, and discharging the materials to obtain the desulfurized rubber powder with the Mooney viscosity of 100 when the temperature reaches 30 ℃.
Comparative example 1
Using 22-mesh waste tire tread rubber powder and aromatic oil asphalt and mixing the raw materials according to the proportion of 100: adding 15 parts by mass and 0.6 part by mass of water into a devulcanizer, reacting for 2.7 hours at the working pressure of 2.2MPa and the working temperature of 220 ℃, and discharging to obtain the devulcanized rubber powder with the Mooney viscosity of 140.
The data for the results of examples 1, 2, 3 and comparative example 1 above are shown in the following table:
comparison of product and energy consumption under the same productivity condition
| Mooney viscosity ML100 ℃ (1 +4 min) | Tensile strength MPa | Elongation at break% | Ton energy consumption | |
| Example 1 | 140 | 13.6 | 470 | 190 |
| Example 2 | 90 | 11.4 | 380 | 181 |
| Example 3 | 100 | 9.5 | 325 | 175 |
| Comparative example 1 | 140 | 13.5 | 461 | 200 |
The above-mentioned embodiments are provided only for illustrating the technical idea and features of the present invention, and the purpose thereof is to enable those skilled in the art to understand the content of the present invention and to implement the present invention, and not to limit the protection scope of the present invention by this, and all equivalent changes or modifications made according to the spirit of the present invention should be covered in the protection scope of the present invention.
In conclusion, the invention achieves the expected effect.
Claims (6)
1. A method for preparing desulfurized rubber powder by self-friction heat generation is characterized by comprising the following steps: quantifying by an automatic metering device to obtain a mass ratio of 100: adding the rubber powder and a softening agent into a first stirrer, stirring and mixing the materials within 2 to 3min, raising the temperature of the materials to 180 to 250 ℃ under the action of self-friction heat generation, discharging volatile low-molecular substances at the temperature to obtain a primarily desulfurized material, directly discharging the primarily desulfurized material into a second stirrer through a continuous sealing device, continuously injecting nitrogen into the second stirrer through an air inlet hole formed in the stirrer in the stirring process, preserving the heat for 10 to 20min to realize desulfurization regeneration of the waste rubber, and finally discharging the material after the temperature of the material is reduced to below 50 ℃ to obtain the desulfurized rubber powder.
2. The method as claimed in claim 1, wherein the rubber powder is waste tire rubber powder or waste butyl rubber powder, and the particle size is 20-60 meshes.
3. The method of claim 1, wherein the softening agent is one or more selected from the group consisting of pine tar pitch, tall oil pitch, and aromatic oil pitch.
4. The method according to claim 1, wherein the first mixer is operated at a speed of 400 to 800 rpm and the second mixer is operated at a speed of 20 to 50 rpm.
5. The method as claimed in claim 1, wherein the nitrogen gas is injected under normal pressure and has a mass ratio of 0.001% to 0.003% with respect to the rubber powder.
6. The method according to claim 1, wherein the Mooney viscosity of the desulfurized rubber powder after being discharged is 80 to 150.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202310091333.9A CN115960389A (en) | 2023-02-09 | 2023-02-09 | Method for preparing desulfurized rubber powder through self-friction heat generation |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202310091333.9A CN115960389A (en) | 2023-02-09 | 2023-02-09 | Method for preparing desulfurized rubber powder through self-friction heat generation |
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| CN115960389A true CN115960389A (en) | 2023-04-14 |
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| CN202310091333.9A Pending CN115960389A (en) | 2023-02-09 | 2023-02-09 | Method for preparing desulfurized rubber powder through self-friction heat generation |
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| Country | Link |
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101173059A (en) * | 2007-10-11 | 2008-05-07 | 回振有 | Atmospheric cryochemistry ageing effect desulfurizing method and device for waste and old vulcanized rubber |
| CN102134330A (en) * | 2011-04-20 | 2011-07-27 | 丰城向华水基科学技术有限公司 | Reclaimed rubber desulfuration and carbon protection process and equipment |
| US20120184634A1 (en) * | 2009-09-30 | 2012-07-19 | Huihong Chen | Thermal Regeneration Method of Waste Rubber |
-
2023
- 2023-02-09 CN CN202310091333.9A patent/CN115960389A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101173059A (en) * | 2007-10-11 | 2008-05-07 | 回振有 | Atmospheric cryochemistry ageing effect desulfurizing method and device for waste and old vulcanized rubber |
| US20120184634A1 (en) * | 2009-09-30 | 2012-07-19 | Huihong Chen | Thermal Regeneration Method of Waste Rubber |
| CN102134330A (en) * | 2011-04-20 | 2011-07-27 | 丰城向华水基科学技术有限公司 | Reclaimed rubber desulfuration and carbon protection process and equipment |
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