CN104017239B - A kind of preparation method of sulfhydryl modified activated carbon for regenerating waste or used rubber - Google Patents
A kind of preparation method of sulfhydryl modified activated carbon for regenerating waste or used rubber Download PDFInfo
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- CN104017239B CN104017239B CN201410174003.7A CN201410174003A CN104017239B CN 104017239 B CN104017239 B CN 104017239B CN 201410174003 A CN201410174003 A CN 201410174003A CN 104017239 B CN104017239 B CN 104017239B
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- Prior art keywords
- activated carbon
- sulfhydryl modified
- rubber
- modified activated
- regenerating waste
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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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- Separation, Recovery Or Treatment Of Waste Materials Containing Plastics (AREA)
- Solid-Sorbent Or Filter-Aiding Compositions (AREA)
Abstract
The invention provides a kind of preparation method of the sulfhydryl modified activated carbon for regenerating waste or used rubber, by using the esterification between activated carbon and TGA, sulfhydryl modified activated carbon AC SH are prepared.Grafting sulfydryl can reach 3.12 more than mmol/g on the activated carbon, and reactivity is big, and preparation technology is simple, using common glue mill this sulfhydryl modified regenerating active carbon agent can be made to be used for the regeneration of waste old at room temperature.And reclaimed rubber adds wearability due to the addition of charcoal in regenerative process, the addition of carbon black can be reduced in post-production modifying process.This technique regenerant consumption is few, and regeneration cost is low, and reclaimed rubber is functional, there is good prospects for commercial application.
Description
Technical field
The invention belongs to regenerating technology for waste rubber, a kind of sulfhydryl modified work for regenerating waste or used rubber is specifically related to
The preparation method of property charcoal.
Technical background
There is the generation of millions of tons scrap rubber in the whole world every year, and quantity is so huge, how it is effectively treated into
For whole society's question of common concern.Therefore, in addition to the waste rubber product that pile up like a mountain is worked as into fuel and burned, being opened from 1910
Begin, scientists from all over the world study more efficiently scrap rubber regeneration treatment technology one after another.
Reclaimed rubber refers to that waste or used vulcanized rubber, by physical and chemical processes such as broken, heating, mechanical treatments, makes it from elasticity
State becomes with plasticity and rubber that is sticky, can vulcanizing again.The essence of regenerative process be heat, oxygen, mechanism and
The chemistry of regenerative agent is with the comprehensive function of physical action, being pyrolyzed vulcanizate Web Grafiti, the existing cross-bond of fracture position,
The crosslinking direct macromolecular key of key.Rubber regeneration method can generally be divided into two classes：Physics regenerates and chemical regeneration, physics
Regeneration use additional ability, such as power, Re-power, microwave, ultrasound, make crosslinking rubber three-dimensional network be crushed into it is low molecular
Fragment.In addition to microwave and ultrasound can cause real rubber regeneration, remaining physical method can only be a kind of crushing technology, that is, make
Make rubber powder.Chemical regeneration is using chemical assistant under Elevated Temperature Conditions, by means of mechanical force, to be destroyed crosslinking rubber,
Reach regeneration purpose.In chemical regeneration, it is nearly all unpleasant harmful for using these chemicals under a large amount of chemicals, HTHP
's.Scrap rubber regeneration is completed using activated carbon supported mercapto functional group, technique is easy, and favorable regeneration effect, use cost is low, the road
Line has no report.
The content of the invention
It is an object of the invention to overcome the shortcoming that prior art is present easy there is provided a kind of technique, favorable regeneration effect makes
It is low with cost, the sulfhydryl modified regenerating active carbon agent for regenerating waste or used rubber.
It is another object of the present invention to provide a kind of above-mentioned sulfhydryl modified activated carbon for regenerating waste or used rubber again
The preparation method of raw agent.
The present invention is adopted the following technical scheme that to achieve these goals：
The preparation method of a kind of sulfhydryl modified activated carbon for regenerating waste or used rubber, it is characterised in that including following step
Suddenly：By Powdered Activated Carbon（AC）Cleaned after pickling with distilled water to neutrality, with appropriate TGA, acetic anhydride and dense sulphur after drying
Acid is mixed, isothermal reaction certain time.Reaction product is filtered by vacuum, and the mercapto for regenerating waste or used rubber is dried to obtain after cleaning
Base modified activated carbon（AC-SH）.
The preparation method of the described sulfhydryl modified activated carbon for regenerating waste or used rubber, it is characterised in that described activity
Carbon granule footpath is 8-30 mesh.
The preparation method of the described sulfhydryl modified activated carbon for regenerating waste or used rubber, it is characterised in that described pickling
Reagent is dust technology, and concentration is 0.005-0.02mol/L.
The preparation method of the described sulfhydryl modified activated carbon for regenerating waste or used rubber, it is characterised in that described activity
Charcoal is cleaned to neutrality through pickling, distilled water, and drying condition is 105-120oC constant pressure and dries.
The preparation method of the described sulfhydryl modified activated carbon for regenerating waste or used rubber, it is characterised in that described activity
Charcoal, TGA, acetic anhydride and concentrated sulfuric acid mass ratio are 1:1.1-1.4:0.8:0.1-0.3, in 60-100oReaction is stood under C
1~24 hour.
The preparation method of the described sulfhydryl modified activated carbon for regenerating waste or used rubber, it is characterised in that described gained
Product drying mode is 30-35oC is dried in vacuo.
The operating procedure that this regenerative agent is used for regenerating waste or used rubber is as follows：
Waste old is now ground into rubber powder, granularity is 20 ~ 150 mesh；Again by rubber powder and regenerative agent with mass ratio 100:5-
15 mix more than 5 minutes in kneading machine, and mill tabletting 3-4 obtains reclaimed rubber all over rear slice.In 140-150oNeed not under C
Vulcanizing system is being added to be sulfided into vulcanizate.
This synthesis for being used for the sulfhydryl modified activated carbon of regenerating waste or used rubber and regeneration mechanism are as follows：
Wherein, AC-S is sulfhydryl modified activated carbon（AC-SH）The free radical that regenerative agent is decomposed.
Beneficial effects of the present invention：
After tested, above-mentioned regenerative vulcanized obtained rubber, because carbon-carbon bond has obtained retaining well in regenerative process, makes
Obtain later vulcanization reclaimed rubber and maintain higher mechanical property, its mechanical property can return to the 60-75% of virgin rubber, and
Due to the addition of charcoal in regenerative process, wearability is added, the addition of carbon black can be reduced in post-production modifying process.This
Process route is easy, and favorable regeneration effect, use cost is low, there is good prospects for commercial application.
Grafting sulfydryl can reach 3.12 more than mmol/g on the activated carbon, and reactivity is big, and preparation technology is simple,
Embodiment：
In order to be better understood from the present invention, illustrated by following instance：
Embodiment 1：
Powdered Activated Carbon sample is placed in 0.01 mol/L HNO3In solution after the h of magnetic agitation 72, with distilled water repeatedly
Cleaning to filter liquor is neutrality, 105oC is dried to constant weight, is placed in saving backup in drier（AC）.In brown ground wide-mouth
6.5 g TGAs, 3.8 g acetic anhydrides and the 1.0 g concentrated sulfuric acids are separately added into bottle, 5 g AC are added after mixing, are fully mixed,
Seal, be placed in 80 in baking ovenoC constant temperature keeps 8 h.Finally the mixture is taken out, is filtered by vacuum, and it is anti-with distilled water
It is multiple to rinse to neutrality, 30~35oTo obtain this sulfhydryl modified regenerating active carbon agent standby for vacuum drying under C（AC-SH）.By element
Analysis-e/or determining sulfur content is 3.12 mmol/g.
Junked tire is removed into the fine powder that the wherein composition such as metal, fiber wears into 20 mesh or so with grater, pressed with AC-SH
According to mass ratio 100:8 ratios are mixed, and are mixed more than 5 minutes in kneading machine, and slice after mill tabletting 3 times produces reclaimed rubber
Finished product.The reclaimed rubber finished product can be directly 145 on vulcanizeroC vulcanizations obtain rubber.
Embodiment 2：
Powdered Activated Carbon sample is placed in 0.01 mol/L HNO3In solution after the h of magnetic agitation 72, with distilled water repeatedly
Cleaning to filter liquor is neutrality, 105oC is dried to constant weight, is placed in saving backup in drier（AC）.In brown ground wide-mouth
7.0 g TGAs, 4.1 g acetic anhydrides and the 1.1 g concentrated sulfuric acids are separately added into bottle, 5 g AC are added after mixing, are fully mixed,
Seal, be placed in 80 in baking ovenoC constant temperature keeps 8 h.Finally the mixture is taken out, is filtered by vacuum, and it is anti-with distilled water
It is multiple to rinse to neutrality, 30~35oTo obtain this sulfhydryl modified regenerating active carbon agent standby for vacuum drying under C（AC-SH）.By element
Analysis-e/or determining sulfur content is 3.01 mmol/g.
Junked tire is removed into the fine powder that the wherein composition such as metal, fiber wears into 20 mesh or so with grater, pressed with AC-SH
According to mass ratio 100:10 ratios are mixed, and are mixed more than 5 minutes in kneading machine, and slice after mill tabletting 4 times produces reclaimed rubber
Finished product.The reclaimed rubber finished product can be directly 145 on vulcanizeroC vulcanizations obtain rubber.
Claims (4)
1. a kind of application of sulfhydryl modified activated carbon in regenerating waste or used rubber, it is characterised in that:The system of sulfhydryl modified activated carbon
Preparation Method comprises the following steps：To be cleaned after Powdered Activated Carbon pickling with distilled water to neutrality, after drying and appropriate TGA,
Acetic anhydride and the concentrated sulfuric acid are mixed, isothermal reaction certain time, and reaction product vacuum filtration is dried to obtain for waste and old after cleaning
The sulfhydryl modified activated carbon of rubber regeneration；Described activated carbon particle size is 8-30 mesh；Described activated carbon, TGA, acetic acid
Acid anhydride and concentrated sulfuric acid mass ratio are 1:1.1-1.4:0.8:0.1-0.3, stands reaction 1-24 hours at 60-100 DEG C；
Sulfhydryl modified activated carbon prepared by the above method is used in regenerating waste or used rubber.
2. application of the sulfhydryl modified activated carbon according to claim 1 in regenerating waste or used rubber, it is characterised in that described
Pickling reagent be dust technology, concentration is 0.005-0.02mol/L.
3. application of the sulfhydryl modified activated carbon according to claim 1 in regenerating waste or used rubber, it is characterised in that described
Activated carbon cleaned through pickling, distilled water to neutrality, drying condition is 105-120 DEG C of constant pressure and dry.
4. application of the sulfhydryl modified activated carbon according to claim 1 in regenerating waste or used rubber, it is characterised in that described
Products therefrom drying mode for 30-35 DEG C vacuum drying.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201410174003.7A CN104017239B (en) | 2014-04-28 | 2014-04-28 | A kind of preparation method of sulfhydryl modified activated carbon for regenerating waste or used rubber |
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|---|---|---|---|
| CN201410174003.7A CN104017239B (en) | 2014-04-28 | 2014-04-28 | A kind of preparation method of sulfhydryl modified activated carbon for regenerating waste or used rubber |
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| Publication Number | Publication Date |
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| CN104017239A CN104017239A (en) | 2014-09-03 |
| CN104017239B true CN104017239B (en) | 2017-08-01 |
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| CN201410174003.7A Expired - Fee Related CN104017239B (en) | 2014-04-28 | 2014-04-28 | A kind of preparation method of sulfhydryl modified activated carbon for regenerating waste or used rubber |
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| CN109616233A (en) * | 2018-11-19 | 2019-04-12 | 中核二七二铀业有限责任公司 | A kind of middle low-level radioactivity rubber and plastic waste recovery recycling processing method |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5359007A (en) * | 1990-07-26 | 1994-10-25 | Relastomer S/A | Thermoplastic rubber obtention method |
| CN1666999A (en) * | 2005-02-21 | 2005-09-14 | 株洲时代新材料科技股份有限公司 | Process for preparing in-situ graft modified rubber by using general rubber preparing device and its modifier |
| CN101613496A (en) * | 2009-07-13 | 2009-12-30 | 扬州大学 | A kind of modified glue powder and blend rubber cross-linked rubber and preparation method thereof |
| CN103265744A (en) * | 2013-06-06 | 2013-08-28 | 中胶橡胶资源再生（青岛）有限公司 | Environment-friendly regenerated rubber and preparation method |
-
2014
- 2014-04-28 CN CN201410174003.7A patent/CN104017239B/en not_active Expired - Fee Related
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5359007A (en) * | 1990-07-26 | 1994-10-25 | Relastomer S/A | Thermoplastic rubber obtention method |
| CN1666999A (en) * | 2005-02-21 | 2005-09-14 | 株洲时代新材料科技股份有限公司 | Process for preparing in-situ graft modified rubber by using general rubber preparing device and its modifier |
| CN101613496A (en) * | 2009-07-13 | 2009-12-30 | 扬州大学 | A kind of modified glue powder and blend rubber cross-linked rubber and preparation method thereof |
| CN103265744A (en) * | 2013-06-06 | 2013-08-28 | 中胶橡胶资源再生（青岛）有限公司 | Environment-friendly regenerated rubber and preparation method |
Non-Patent Citations (1)
| Title |
|---|
| "巯基改性活性炭对水溶液中汞的吸附性能研究";王静 等;《环境工程学报》;中国学术期刊电子出版社;20090228;第3卷(第2期);第219-222页 * |
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