CN102863648B - Method for multi-section desulfurization, regeneration and recovery of vulcanized butyl rubber - Google Patents
Method for multi-section desulfurization, regeneration and recovery of vulcanized butyl rubber Download PDFInfo
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- CN102863648B CN102863648B CN201110190095.4A CN201110190095A CN102863648B CN 102863648 B CN102863648 B CN 102863648B CN 201110190095 A CN201110190095 A CN 201110190095A CN 102863648 B CN102863648 B CN 102863648B
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- Prior art keywords
- desulfurization
- sections
- butyl rubber
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- 238000006477 desulfuration reaction Methods 0.000 title claims abstract description 125
- 230000023556 desulfurization Effects 0.000 title claims abstract description 125
- 238000000034 method Methods 0.000 title claims abstract description 27
- 229920005549 butyl rubber Polymers 0.000 title claims abstract description 24
- 238000011069 regeneration method Methods 0.000 title claims abstract description 20
- 230000008929 regeneration Effects 0.000 title claims abstract description 19
- 238000011084 recovery Methods 0.000 title abstract description 6
- 239000000463 material Substances 0.000 claims description 53
- 238000010792 warming Methods 0.000 claims description 26
- 238000003801 milling Methods 0.000 claims description 16
- 238000006243 chemical reaction Methods 0.000 claims description 15
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 13
- 238000007670 refining Methods 0.000 claims description 12
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims description 10
- 239000001301 oxygen Substances 0.000 claims description 10
- 229910052760 oxygen Inorganic materials 0.000 claims description 10
- 239000002994 raw material Substances 0.000 claims description 10
- 238000001125 extrusion Methods 0.000 claims description 9
- 230000004913 activation Effects 0.000 claims description 7
- 230000000694 effects Effects 0.000 claims description 7
- 238000001914 filtration Methods 0.000 claims 1
- 229920001971 elastomer Polymers 0.000 abstract description 20
- 125000000484 butyl group Chemical group [H]C([*])([H])C([H])([H])C([H])([H])C([H])([H])[H] 0.000 abstract description 12
- 238000005516 engineering process Methods 0.000 abstract description 7
- 241001441571 Hiodontidae Species 0.000 abstract description 2
- 238000004064 recycling Methods 0.000 abstract 1
- 238000001816 cooling Methods 0.000 description 8
- 230000006378 damage Effects 0.000 description 4
- 229910052799 carbon Inorganic materials 0.000 description 3
- 238000001514 detection method Methods 0.000 description 3
- 239000002245 particle Substances 0.000 description 3
- 239000000126 substance Substances 0.000 description 3
- 150000001721 carbon Chemical group 0.000 description 2
- GPRLSGONYQIRFK-UHFFFAOYSA-N hydron Chemical compound [H+] GPRLSGONYQIRFK-UHFFFAOYSA-N 0.000 description 2
- 230000001172 regenerating effect Effects 0.000 description 2
- 238000005987 sulfurization reaction Methods 0.000 description 2
- 239000004215 Carbon black (E152) Substances 0.000 description 1
- RWSOTUBLDIXVET-UHFFFAOYSA-N Dihydrogen sulfide Chemical compound S RWSOTUBLDIXVET-UHFFFAOYSA-N 0.000 description 1
- 244000043261 Hevea brasiliensis Species 0.000 description 1
- VHOQXEIFYTTXJU-UHFFFAOYSA-N Isobutylene-isoprene copolymer Chemical group CC(C)=C.CC(=C)C=C VHOQXEIFYTTXJU-UHFFFAOYSA-N 0.000 description 1
- UCKMPCXJQFINFW-UHFFFAOYSA-N Sulphide Chemical compound [S-2] UCKMPCXJQFINFW-UHFFFAOYSA-N 0.000 description 1
- 238000009825 accumulation Methods 0.000 description 1
- 239000006229 carbon black Substances 0.000 description 1
- -1 carbonium ion Chemical class 0.000 description 1
- 238000006555 catalytic reaction Methods 0.000 description 1
- 238000005336 cracking Methods 0.000 description 1
- 230000007423 decrease Effects 0.000 description 1
- 230000003009 desulfurizing effect Effects 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 239000003292 glue Substances 0.000 description 1
- 230000036571 hydration Effects 0.000 description 1
- 238000006703 hydration reaction Methods 0.000 description 1
- 229930195733 hydrocarbon Natural products 0.000 description 1
- 150000002430 hydrocarbons Chemical class 0.000 description 1
- 229910000037 hydrogen sulfide Inorganic materials 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- 239000000693 micelle Substances 0.000 description 1
- 229920003052 natural elastomer Polymers 0.000 description 1
- 229920001194 natural rubber Polymers 0.000 description 1
- 239000008239 natural water Substances 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 238000010008 shearing Methods 0.000 description 1
- RWSOTUBLDIXVET-UHFFFAOYSA-O sulfonium Chemical compound [SH3+] RWSOTUBLDIXVET-UHFFFAOYSA-O 0.000 description 1
- 239000004636 vulcanized rubber Substances 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
The invention discloses a method for multi-section desulfurization, regeneration and recovery of vulcanized butyl rubber, which comprises from one to seven sections of desulfurization in sequence. The invention adopts seven-section desulfurization instead of the primary high-temperature desulfurization in a traditional desulfurization technology. The tensile strength of the obtained butyl regenerated rubber is 1.5MPa higher than that of the butyl rubber processed by the traditional technology; the elongation at break is 30% to 50% higher than that of the butyl rubber processed by the traditional technology; and the mooney point is 3 to 5 lower than that of the butyl rubber processed by the traditional technology. The recovery butyl rubber can essentially reach or exceed the indexes before the feeding, so that an aim of recycling the rubber with high quality can be achieved.
Description
Technical field
The present invention relates to a kind of desulfurization regeneration method of vulcanized butyl rubber.
Background technology
The regeneration techniques physics of vulcanized butyl rubber regeneration at present or chemical regeneration are substantially all to take its desulfurization degree of one section desulfurization not reach 50%, and the every physical and chemical index after its regeneration can only reach 80% of the index that feeds intake.
Summary of the invention
The invention provides a kind of vulcanized butyl rubber regenerative recovery method of implementing, end properties is good of being convenient to, can realize the recycle of high materialization rubber.
A kind of method that vulcanized butyl rubber multistage desulfurization regeneration restores, comprise one to seven section desulfurization successively, and the process of described one to seven section desulfurization is as follows:
One section desulfurization:
Raw material is warming up to 170~185 ℃, carries out the desulfurization of 1.5~4 minutes (preferably 2 minutes) at this temperature; Wherein temperature-rise period is generally at 4~8 minutes, preferably 6 minutes.
One section desulfurization can utilize existing milling machine to carry out, and in the milling machine with twin screw, the heat energy that twin screw can produce material cutting also improves pressure, and raw material is heated up, and wherein in temperature-rise period, material pressure rises gradually, the highest can be to 6.5 times of normal atmosphere.After raw material is warming up to 170~185 ℃, pressure decreases, can be in atmospheric pressure state.
Two sections desulfurization:
Add water in the material that completes one section desulfurization, 0.5~1.5% of the weight of the material that the weight of water has been one section desulfurization, preferably 0.8%, improve material pressure and make material be warming up to 220~230 ℃, resulting pressure can reach 6.5 times of normal atmosphere.This process time is about 20~40 seconds (preferably 30 seconds) generally, can in described milling machine, complete.
The hydration that the water utilized (preferably natural water) can play, catalysis, activation, ramollescence, rubber molecule is under the effect of mechanical force and middle high temperature, the motion aggravation, the molecular motion Showed Very Brisk that becomes, the sulfide linkage of being combined with rubber hydrocarbon absorbs the constraint that energy breaks away from carbon atom, become electronegative ion, make remaining carbon atom positively charged simultaneously, due to Sauerstoffatom in water molecules have lone-pair electron very easily with the carbonium ion set with unoccupied orbital, so just formed the unstable intermediate of water molecules and the set of macromole rubber chain, this unstable intermediate discharges the hydrogen ion of a positively charged, this hydrogen ion is combined with the electronegative sulfonium ion produced before and is generated hydrogen sulfide and separate, make most of cross-link bond fracture.This process produces HS and SO
2waste gas is by the environmental protecting device collection and treatment.
Three sections desulfurization:
The material that completes two sections desulfurization contacts with air, and hot oxygen desulphurization reaction occurs, and material is warming up to 240~250 ℃ under the reaction heat effect, and hot oxygen desulphurization reaction carries out under normal pressure.
The time of three sections desulfurization is about 20~40 seconds (preferably 30 seconds) generally.In front two-stage desulfurization process, if use milling machine, this stage has been that the material of two sections desulfurization delivers from godown after (discharge milling machine) and contacts with air, and hot oxygen desulphurization reaction occurs.The natural rubber particle of 1-2% in these stage processing sulfuration butyl rubber goods.
Four sections desulfurization:
The material that completes three sections desulfurization was cooled to 120 ℃ at 2~5 minutes in (preferably 2 minutes).
Four sections desulfurization can be carried out in mill, can utilize in automation process and realize, the milling machine tipping bucket that delivers from godown touching conveying belt is switch activated, material is delivered to automatically can force the cooling rapid cooling down of boring cylinder mill, and under the middle condition of high temperature in mill prompt drop temperature process, desulfurization is restored.Because be that automatization control just makes each processing action consistent, thereby make the process quality index stable uniform.
Be cooled to middle low-temp desulfurization in mill, heat energy impels the molecular motion aggravation, cause the molecule chain break, 1 times of 10 ℃ of thermo-cracking Speed Reduction often fall, during to 80 ℃, unsettled radical tends towards stability, it is further to make the cross-link bond fracture of not rupturing that this stage will complete purpose in the short period of time, and the destruction of will as far as possible reduce-C-C-.
Five sections desulfurization:
The material that completes four sections desulfurization is naturally cooled to normal temperature by 120 ℃, standing 3~6 hours (preferably 4 hours) under normal temperature (20~25 ℃), atmospheric pressure state.
Standing is in order to complete activation, this process can make leading portion accumulation shearing can and chemical energy play one's part to the full and can not only make associative key further disconnect, and the molecule long-chain substantially do not rupture and do not degrade, thereby improved desulfurization recovery degree.
Six sections desulfurization:
The material that completes five sections desulfurization is warming up at 90~110 ℃ (preferably 100 ℃), carries out refining.
The time of six sections desulfurization is 10~15 minutes, 8~12 minutes heating-up times wherein, continues refining 2~3 minutes after being warming up to 90~110 ℃.
This stage can be utilized refiner, and the material under the normal temperature state heats up in the effect of mechanical mill, also makes residual rubber molecule and the association particle on carbon black particle surface separate.
Seven sections desulfurization:
By the material that completes six sections desulfurization under 130~140 ℃ of conditions, filtered, extrusion, then normal temperature is placed 36~60 hours (preferably 48 hours) of activation, obtains finished product.
Seven sections desulfurization can utilize that extruder is filtered, extrusion, filter, extrusion generally can complete in 4~7 minutes, and in six sections desulfurization, the material of refiner output is delivered to extruder by automatic delivering belt and concentrated under 3 normal atmosphere and carry out the limbs unification and restore processing.The main technical point of this process is that after opening refining (four sections desulfurization) still residual sulfuration micelle of failing the desulphurization, disaggregation reduction has become residual meticulous vulcanized rubber powder through refiner low temperature refining glue major part, and under the medium temperature and medium pressure condition of the butyl rubber that this part does not restore in extruder again intensifying regenerating restore.
The method that vulcanized butyl rubber multistage desulfurization regeneration of the present invention restores, changed a high temperature desulfurizing in traditional desulfurization technology, and adopted seven sections desulfurization, and the butyl renewable rubber obtained is than the high 1.5Mpa of butyl renewable rubber tensile strength of traditional technology processing; Tensile yield is high by 30~50%; Mooney point low 3~5.The index that basically can meet or exceed before feeding intake is recovery isoprene-isobutylene rubber truly, thereby reaches the purpose of high materialization rubber recycle.
Embodiment
Embodiment 1
The method that the present embodiment vulcanized butyl rubber multistage desulfurization regeneration restores comprises one to seven section desulfurization:
One section desulfurization:
Raw material is inserted in the milling machine with twin screw, and the heat energy that twin screw can produce material cutting also improves pressure, and raw material is heated up, and within 6 minutes, is warming up to 185 ℃, maintains 2 minutes and carry out desulfurization in the time of 185 ℃.
Two sections desulfurization:
Add water in milling machine, 0.8% of the weight of the material that the weight of water has been one section desulfurization, improve material pressure and make material be warming up to 220 ℃ in 30 seconds, makes most of cross-link bond fracture.
Three sections desulfurization:
The material discharge milling machine that completes two sections desulfurization contacts with air, and hot oxygen desulphurization reaction occurs, and material is warming up to 250 ℃ under the reaction heat effect, and hot oxygen desulphurization reaction maintains 30 seconds.
Four sections desulfurization:
The material that completes three sections desulfurization is automatically delivered to and can be forced the cooling rapid cooling down of boring cylinder mill, be cooled to 120 ℃ in 2 minutes, further make the cross-link bond fracture of not rupturing, and the destruction of will as far as possible reduce-C-C-.
Five sections desulfurization:
Will complete the material of four sections desulfurization discharge mill, under normal temperature, atmospheric pressure state standing 4 hours.
Six sections desulfurization:
The mass transport that completes five sections desulfurization, to refiner, is warming up to 100 ℃, carries out refining, 10 minutes heating-up times wherein, continue refining 2 minutes after being warming up to 100 ℃.
Seven sections desulfurization:
The material that completes six sections desulfurization is sent to extruder by refiner, is filtered under 135 ℃ of conditions, extrusion, then normal temperature is placed activation 48 hours, obtains finished product.
The butyl renewable rubber of the finished product that obtains and prior art processing is carried out to Performance Detection and contrast:
The butyl renewable rubber that the visible the present invention of upper table obtains obviously improves according to the butyl renewable rubber performance by prior art processing.
Embodiment 2
The method that the present embodiment vulcanized butyl rubber multistage desulfurization regeneration restores comprises one to seven section desulfurization:
One section desulfurization:
Raw material is inserted in the milling machine with twin screw, and the heat energy that twin screw can produce material cutting also improves pressure, and raw material is heated up, within 5 minutes, be warming up to 180 ℃, in temperature-rise period, material pressure rises gradually, the highest can be to 6.5 times of normal atmosphere, carry out desulfurization to maintaining 2 minutes after 180 ℃.
Two sections desulfurization:
Add water in milling machine, 0.6% of the weight of the material that the weight of water has been one section desulfurization, improve material pressure (the highest can to 6.5 times of normal atmosphere), makes material be warming up to 225 ℃ in 30 seconds, makes most of cross-link bond fracture.
Three sections desulfurization:
The material discharge milling machine that completes two sections desulfurization contacts with air, and hot oxygen desulphurization reaction occurs, and material is warming up to 245 ℃ under the reaction heat effect, and hot oxygen desulphurization reaction maintains 40 seconds.
Four sections desulfurization:
The material that completes three sections desulfurization is automatically delivered to and can be forced the cooling rapid cooling down of boring cylinder mill, be cooled to 120 ℃ in 2 minutes, further make the cross-link bond fracture of not rupturing, and the destruction of will as far as possible reduce-C-C-.
Five sections desulfurization:
Will complete the material of four sections desulfurization discharge mill, under normal temperature, atmospheric pressure state standing 4 hours.
Six sections desulfurization:
The mass transport that completes five sections desulfurization, to refiner, is warming up to 100 ℃, carries out refining, 10 minutes heating-up times wherein, continue refining 3 minutes after being warming up to 100 ℃.
Seven sections desulfurization:
The material that completes six sections desulfurization is sent to extruder by refiner, is filtered under 130 ℃ of conditions, extrusion, then normal temperature is placed activation 60 hours, obtains finished product.
The butyl renewable rubber of the finished product that obtains and prior art processing is carried out to Performance Detection and contrast:
The butyl renewable rubber that the visible the present invention of upper table obtains obviously improves according to the butyl renewable rubber performance by prior art processing.
Embodiment 3
The method that the present embodiment vulcanized butyl rubber multistage desulfurization regeneration restores comprises one to seven section desulfurization:
One section desulfurization:
Raw material is inserted in the milling machine with twin screw, and the heat energy that twin screw can produce material cutting also improves pressure, and raw material is heated up, and within 6 minutes, is warming up to 170 ℃, maintains 3 minutes and carry out desulfurization in the time of 170 ℃.
Two sections desulfurization:
Add water in milling machine, 1.0% of the weight of the material that the weight of water has been one section desulfurization, improve material pressure and make material be warming up to 230 ℃ in 40 seconds, makes most of cross-link bond fracture.
Three sections desulfurization:
The material discharge milling machine that completes two sections desulfurization contacts with air, and hot oxygen desulphurization reaction occurs, and material is warming up to 240 ℃ under the reaction heat effect, and hot oxygen desulphurization reaction maintains 35 seconds.
Four sections desulfurization:
The material that completes three sections desulfurization is automatically delivered to and can be forced the cooling rapid cooling down of boring cylinder mill, be cooled to 120 ℃ in 3 minutes, further make the cross-link bond fracture of not rupturing, and the destruction of will as far as possible reduce-C-C-.
Five sections desulfurization:
Will complete the material of four sections desulfurization discharge mill, under normal temperature, atmospheric pressure state standing 5 hours.
Six sections desulfurization:
The mass transport that completes five sections desulfurization, to refiner, is warming up to 110 ℃, carries out refining, 8 minutes heating-up times wherein, continue refining 3 minutes after being warming up to 100 ℃.
Seven sections desulfurization:
The material that completes six sections desulfurization is sent to extruder by refiner, is filtered under 132 ℃ of conditions, extrusion, then normal temperature is placed activation 50 hours, obtains finished product.
The butyl renewable rubber of the finished product that obtains and prior art processing is carried out to Performance Detection and contrast:
The butyl renewable rubber that the visible the present invention of upper table obtains obviously improves according to the butyl renewable rubber performance by prior art processing.
Claims (7)
1. the method that vulcanized butyl rubber multistage desulfurization regeneration restores, is characterized in that, comprise successively one to seven section desulfurization, the process of described one to seven section desulfurization is as follows:
One section desulfurization: raw material is warming up to 170~185 ℃, carries out the desulfurization of 1.5~4 minutes at this temperature;
Two sections desulfurization: add water in the material that completes one section desulfurization, 0.5~1.5% of the weight of the material that the weight of water has been one section desulfurization, make material be warming up to 220~230 ℃, and the time of described two sections desulfurization is 20~40 seconds;
Three sections desulfurization: the material that completes two sections desulfurization contacts with air, and hot oxygen desulphurization reaction occurs, and material is warming up to 240~250 ℃ under the reaction heat effect, and the time of described three sections desulfurization is 20~40 seconds;
Four sections desulfurization: the material that will complete three sections desulfurization was cooled to 120 ℃ in 2~5 minutes;
Five sections desulfurization: the material that will complete four sections desulfurization naturally cools to normal temperature by 120 ℃, under normal temperature, atmospheric pressure state standing 3~6 hours;
Six sections desulfurization: the material that will complete five sections desulfurization is warming up at 90~110 ℃ and carries out refining, and the time of described six sections desulfurization is 10~15 minutes;
Seven sections desulfurization: the material that will complete six sections desulfurization is filtered under 130~140 ℃ of conditions, extrusion, and then normal temperature is placed activation 36~60 hours, obtains finished product.
2. the method that vulcanized butyl rubber multistage desulfurization regeneration as claimed in claim 1 restores, is characterized in that, utilizes milling machine to carry out described one section desulfurization and two sections desulfurization.
3. the method that vulcanized butyl rubber multistage desulfurization regeneration as claimed in claim 2 restores, is characterized in that, 8~12 minutes heating-up times in described six sections desulfurization, continues refining 2~3 minutes after being warming up to 90~110 ℃.
4. the method that vulcanized butyl rubber multistage desulfurization regeneration as claimed in claim 3 restores, is characterized in that, in described seven sections desulfurization, filtration, extrusion completed in 4~7 minutes.
5. the method that vulcanized butyl rubber multistage desulfurization regeneration as described as claim 1~4 any one restores is characterized in that described four sections desulfurization are carried out in mill.
6. the method that vulcanized butyl rubber multistage desulfurization regeneration as claimed in claim 5 restores is characterized in that described six sections desulfurization utilize refiner to carry out.
7. the method that vulcanized butyl rubber multistage desulfurization regeneration as claimed in claim 6 restores, is characterized in that, utilizes in described seven sections desulfurization that extruder is filtered, extrusion.
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CN201110190095.4A CN102863648B (en) | 2011-07-07 | 2011-07-07 | Method for multi-section desulfurization, regeneration and recovery of vulcanized butyl rubber |
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CN103467864A (en) * | 2013-08-12 | 2013-12-25 | 随州市普康橡塑有限公司 | Preparation technology for regenerating waste butyl rubber |
CN111204000B (en) * | 2020-01-15 | 2022-01-11 | 福建中宏新材料科技有限公司 | Two-stage plasticizing process of butyl reclaimed rubber |
Citations (4)
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CN1754904A (en) * | 2004-09-28 | 2006-04-05 | 南通回力橡胶有限公司 | High-temperature continuous reproduction process of butyl rubber |
CN101066617A (en) * | 2007-04-09 | 2007-11-07 | 辽宁万来轮胎有限公司 | Process of producing inner tube material with waste butyl rubber inner tube |
CN101508795A (en) * | 2009-03-16 | 2009-08-19 | 江苏强维橡塑科技有限公司 | Method for desulfurization regeneration of vulcanized rubber by employing double-screw extruder |
CN101591451A (en) * | 2008-05-30 | 2009-12-02 | 天津市亚腾达橡塑制品发展有限公司 | A kind of method for regenerating waste butyl vulcanized rubber by radiation and desulfuration |
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2011
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Patent Citations (4)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN1754904A (en) * | 2004-09-28 | 2006-04-05 | 南通回力橡胶有限公司 | High-temperature continuous reproduction process of butyl rubber |
CN101066617A (en) * | 2007-04-09 | 2007-11-07 | 辽宁万来轮胎有限公司 | Process of producing inner tube material with waste butyl rubber inner tube |
CN101591451A (en) * | 2008-05-30 | 2009-12-02 | 天津市亚腾达橡塑制品发展有限公司 | A kind of method for regenerating waste butyl vulcanized rubber by radiation and desulfuration |
CN101508795A (en) * | 2009-03-16 | 2009-08-19 | 江苏强维橡塑科技有限公司 | Method for desulfurization regeneration of vulcanized rubber by employing double-screw extruder |
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Effective date of registration: 20180410 Address after: 300499 Beichen City Economic Development Zone, Beichen District, double Chen East Road, No. 29, No. Patentee after: Tianjin Dongzhen Rubber Co., Ltd. Address before: 300381 No. 1, building 4, gambling house, Shi Ying Road, Nankai District, Tianjin. Patentee before: Zhang Dalu |
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CF01 | Termination of patent right due to non-payment of annual fee | ||
CF01 | Termination of patent right due to non-payment of annual fee |
Granted publication date: 20140108 Termination date: 20180707 |