CN102827101A - Purification method of rubber vulcanization accelerator MBT (2-mercaptobenzthiazole) - Google Patents
Purification method of rubber vulcanization accelerator MBT (2-mercaptobenzthiazole) Download PDFInfo
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- CN102827101A CN102827101A CN2012103620134A CN201210362013A CN102827101A CN 102827101 A CN102827101 A CN 102827101A CN 2012103620134 A CN2012103620134 A CN 2012103620134A CN 201210362013 A CN201210362013 A CN 201210362013A CN 102827101 A CN102827101 A CN 102827101A
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Abstract
The invention provides a purification method of a rubber vulcanization accelerator MBT (2-mercaptobenzthiazole), which comprises the following steps: pulverizing a crude product MBT synthesized under high pressure, and putting the pulverized MBT in a high-pressure kettle, wherein the mass percent of MBT in the crude product MBT is 80-90%; sealing the high-pressure kettle, vacuumizing, and charging a nitrogen protective atmosphere; pressing carbon bisulfide which is 2-5 times by weight of the crude product MBT into the reaction kettle; after sealing, starting stirring, heating to 120-180 DEG C, and keeping the temperature for 0.5-2 hours; cooling the reaction kettle to room temperature at the rate of 0.5-3 DEG C/min in a jacket cooling mode, filtering, washing, and drying to obtain the vulcanization accelerator MBT of which the content is higher than 98%; and distilling to recover the filtered mother liquor which can be circularly used in the reaction stage, wherein the recovery rate is up to higher than 96%. The method has the advantage of simple process, and the purity of the prepared high-content MBT is up to higher than 98%; no waste water is generated in the refinement process; and the extractant carbon bisulfide used as the reaction raw material has the advantage of low energy consumption for recovery, and can be returned to the reaction stage for circular use.
Description
Technical field
The present invention relates to the New Method of Purification of a kind of thiofide 2-mercaptobenzothiazole (MBT), belong to rubber vulcanization accelerant MBT purification techniques field.
Background technology
MBT (2-mercaptobenzothiazole) is the requisite a kind of primary accelerator of present rubber industry.Domestic production technique is an aniline legal system accelerant MBT at present.This kind technology products obtained therefrom yield is lower, is merely about 85%, needs after refining, can obtain specification product.Process for refining mainly contains acid-base method, solvent extration at present.Acid-base method technology is simple, easy handling, but generate the great amount of wastewater contaminate environment.Document (Northwest Institute for Ethnic Minorities newspaper, 21,4, P8-11) reported the method for refining MBT.To synthesize bullion M alkali under the certain pH value condition and dissolve, and after removing by filter a small amount of insolubles, obtain certain density M sodium salt solution.With dithiocarbonic anhydride the M sodium salt solution is extracted; After the standing separation; Oil phase returns building-up reactions with certain ratio. and water carries out reextraction with fresh dithiocarbonic anhydride, and oil phase all returns and is used for extraction for the first time after separating, and water is through acidifying, dehydration, dried product MBT.Though this method adopts solvent extration to make with extra care, but still can not avoid generating brine waste, environmental protection pressure is big.Patent CN 1300123C adopts toluene directly to extract bullion MBT as extraction agent, emit no waste water in the process, but the solvent recuperation power consumption is bigger, and operating process is bigger to hazard to person, contaminate environment.And the dithiocarbonic anhydride of one of reaction raw materials is low with its boiling point, and easy recovery becomes solvent-extracted optimal selection.
Summary of the invention
The object of the present invention is to provide a kind of New Method of Purification of rubber vulcanization accelerant MBT, for achieving the above object, the present invention realizes through following technical proposals: a kind of New Method of Purification of rubber vulcanization accelerant MBT is characterized in that comprising following process:
1. put into autoclave after high pressure synthetic bullion MBT being pulverized; The MBT massfraction is 80 ~ 90% among the bullion MBT;
2. with the autoclave sealing, charge into nitrogen protection after vacuumizing;
3. bullion MBT quality 2-5 dithiocarbonic anhydride doubly is pressed in the reaction kettle; Sealing back is opened to stir and is warming up to 120-180 ℃ and keep 0.5-2h;
4. adopt the chuck cooling to make reactor temperature be cooled to normal temperature with the speed of 0.5 ~ 3 ℃/min, filtration, washing, drying obtain content and are higher than 98% accelerator M BT;
5. filter mother liquid obtained distillation and reclaim, the recovery reaches more than 96%, the step of reaction that is used for capable of circulation.
The invention has the advantages that: this procedure is simple, and prepared high-content MBT purity reaches more than 98%, fusing point is high, melting range is short, yield is high.Treating process does not produce waste water, and is few as the extraction agent dithiocarbonic anhydride recovery power consumption of reaction raw materials, can be back to the step of reaction recycle.
Embodiment
Embodiment 1:
Take by weighing bullion MBT500g, content is 90%, inserts after the pulverizing in the 1L seal pot.Pour nitrogen protection after vacuumizing.1000g dithiocarbonic anhydride is squeezed into seal pot with peristaltic pump.Open to stir the sealing back that finishes, and is warming up to 120 ℃ and keep 120min.Through chuck cooling with 1 ℃ //speed of min slowly is cooled to normal temperature.After filtration, washing, the drying product 440g, the mass content of this 2-mercaptobenzothiazole promotor is 98.5%, fusing point is 171.3 ° of C.Get dithiocarbonic anhydride 960g after the mother liquor distillation.
Embodiment 2:
Take by weighing bullion MBT500g, content is 85%, inserts after the pulverizing in the 1L seal pot.Pour nitrogen protection after vacuumizing.1500g dithiocarbonic anhydride is squeezed into seal pot with peristaltic pump.Open to stir the sealing back that finishes, and is warming up to 140 ℃ and keep 60min.Through chuck cooling with 2 ℃ //speed of min slowly is cooled to normal temperature.After filtration, washing, the drying product 421g, the mass content of this 2-mercaptobenzothiazole promotor is 99.1%, fusing point is 173.1 ° of C.Get dithiocarbonic anhydride 1447g after the mother liquor distillation.
Embodiment 3:
Take by weighing bullion MBT500g, content is 80%, inserts after the pulverizing in the 1L seal pot.Pour nitrogen protection after vacuumizing.2500g dithiocarbonic anhydride is squeezed into seal pot with peristaltic pump.Open to stir the sealing back that finishes, and is warming up to 180 ℃ and keep 30min.Through chuck cooling with 3 ℃ //speed of min slowly is cooled to normal temperature.After filtration, washing, the drying product 402g, the mass content of this 2-mercaptobenzothiazole promotor is 99.5%, fusing point is 177.1 ° of C.Get dithiocarbonic anhydride 2425g after the mother liquor distillation.
Embodiment 4:
Take by weighing bullion MBT500g, content is 80%, inserts after the pulverizing in the 1L seal pot.Pour nitrogen protection after vacuumizing.2500g dithiocarbonic anhydride is squeezed into seal pot with peristaltic pump.Open to stir the sealing back that finishes, and is warming up to 120 ℃ and keep 60min.Through chuck cooling with 0.5 ℃ //speed of min slowly is cooled to normal temperature.After filtration, washing, the drying product 408g, the mass content of this 2-mercaptobenzothiazole promotor is 98%, fusing point is 176 ° of C.Get dithiocarbonic anhydride 2420g after the mother liquor distillation.
Embodiment 5:
Take by weighing bullion MBT500g, content is 80%, inserts after the pulverizing in the 1L seal pot.Pour nitrogen protection after vacuumizing.2500g dithiocarbonic anhydride is squeezed into seal pot with peristaltic pump.Open to stir the sealing back that finishes, and is warming up to 150 ℃ and keep 120min.Through chuck cooling with 1 ℃ //speed of min slowly is cooled to normal temperature.After filtration, washing, the drying product 404g, the mass content of this 2-mercaptobenzothiazole promotor is 99%, fusing point is 176 ° of C.Get dithiocarbonic anhydride 2420g after the mother liquor distillation.
Although above the preferred embodiments of the present invention are described; But the present invention is not limited to above-mentioned embodiment, and above-mentioned embodiment only is schematically, is not restrictive; Those of ordinary skill in the art is under enlightenment of the present invention; Not breaking away under the scope situation that aim of the present invention and claim protect, can also make the concrete conversion of a lot of forms, these all belong within protection scope of the present invention.
Claims (1)
1. the method for purification of a rubber vulcanization accelerant MBT is characterized in that comprising following process:
1) with putting into autoclave after the high pressure synthetic bullion MBT pulverizing, wherein MBT content is 80%-90%;
2) with the autoclave sealing, charge into nitrogen protection after vacuumizing;
3) bullion MBT quality 2-5 dithiocarbonic anhydride doubly is pressed in the reaction kettle; The sealing back is opened to stir and is risen
120-180 ℃ and keep 0.5-2h;
4) adopt the chuck cooling to be cooled to normal temperature with the cooling rate of 0.5 ℃/min-3 ℃/min, filtration, washing, drying obtain content and are higher than 98% accelerator M BT;
5) filter mother liquid obtained distillation and reclaim, the recovery reaches more than 96%, the step of reaction that is used for capable of circulation.
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| CN2012103620134A CN102827101A (en) | 2012-09-25 | 2012-09-25 | Purification method of rubber vulcanization accelerator MBT (2-mercaptobenzthiazole) |
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| CN2012103620134A CN102827101A (en) | 2012-09-25 | 2012-09-25 | Purification method of rubber vulcanization accelerator MBT (2-mercaptobenzthiazole) |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103965137A (en) * | 2014-05-07 | 2014-08-06 | 镇江苏秦环保科技有限公司 | Method for refining accelerant M(2-mercaptobenzothiazole) by using non-aqueous polarity method |
| CN110615772A (en) * | 2019-09-09 | 2019-12-27 | 山东尚舜化工有限公司 | Novel process for purifying rubber accelerator MBT |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102070562A (en) * | 2010-12-21 | 2011-05-25 | 天津大学 | Method for preparing 2-mercaptobenzothiazole |
| CN102391205A (en) * | 2011-09-20 | 2012-03-28 | 科迈化工股份有限公司 | Method for synthesizing rubber vulcanization accelerant 2-mercaptobenzothiazole |
| CN102408393A (en) * | 2011-10-18 | 2012-04-11 | 中国石油化工集团公司 | Method for continuously purifying vulcanization accelerator 2-mercaptobenzothiazole |
-
2012
- 2012-09-25 CN CN2012103620134A patent/CN102827101A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102070562A (en) * | 2010-12-21 | 2011-05-25 | 天津大学 | Method for preparing 2-mercaptobenzothiazole |
| CN102391205A (en) * | 2011-09-20 | 2012-03-28 | 科迈化工股份有限公司 | Method for synthesizing rubber vulcanization accelerant 2-mercaptobenzothiazole |
| CN102408393A (en) * | 2011-10-18 | 2012-04-11 | 中国石油化工集团公司 | Method for continuously purifying vulcanization accelerator 2-mercaptobenzothiazole |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103965137A (en) * | 2014-05-07 | 2014-08-06 | 镇江苏秦环保科技有限公司 | Method for refining accelerant M(2-mercaptobenzothiazole) by using non-aqueous polarity method |
| CN103965137B (en) * | 2014-05-07 | 2015-11-18 | 镇江苏秦环保科技有限公司 | Non-aqueous polar method refines the method for captax (2-mercaptobenzothiazole) |
| CN110615772A (en) * | 2019-09-09 | 2019-12-27 | 山东尚舜化工有限公司 | Novel process for purifying rubber accelerator MBT |
| CN110615772B (en) * | 2019-09-09 | 2022-03-18 | 山东尚舜化工有限公司 | Novel process for purifying rubber accelerator MBT |
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Application publication date: 20121219 |