CN101638396A - Production process for rubber accelerator 2-thiol group benzothiazole - Google Patents
Production process for rubber accelerator 2-thiol group benzothiazole Download PDFInfo
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- CN101638396A CN101638396A CN200810140886A CN200810140886A CN101638396A CN 101638396 A CN101638396 A CN 101638396A CN 200810140886 A CN200810140886 A CN 200810140886A CN 200810140886 A CN200810140886 A CN 200810140886A CN 101638396 A CN101638396 A CN 101638396A
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Abstract
The invention relates to a production process for a rubber accelerator 2-thiol group benzothiazole, which belongs to the technical field of rubber accelerator production. The process comprises the following steps: adding carbon disulfide and sulfur into a reaction kettle; stirring the mixture for 2 to 4 hours under the condition that the temperature is between 25 and 30 DEG C and the rotating speed is 20 to 60 revolutions per minute; adding aniline into the mixture, wherein the mol ratio of the aniline to the carbon disulfide to the sulfur is 1:0.8-1.0:0.6-0.8; raising the temperature to between 150 and 300 DEG C, and performing reaction under the pressure of between 0.7 and 9.5 MPa for 60 to 120 minutes; extracting the mixture with methylbenzene for 5 to 25 minutes, then filtering the mixture to distil and reclaim the methylbenzene; and performing the extraction for 2 to 3 times repeatedly, and drying the product to obtain the 2-thiol group benzothiazole. The process does not need a great deal of acids and bases to perform 'neutralization' and 'water scrubbing', thereby avoiding the generation of a great deal of waste water, reducing environmental pollution, and avoiding corrosionto the devices.
Description
Technical field
The invention belongs to the production technical field of thiofide, be specifically related to a kind of production technique of rubber accelerator 2-thiol group benzothiazole.
Background technology
Vulcanization accelerator 2-thiol benzothiazole (M), be a kind of good thiazoles, half ultraaccelerator, has cure range widely, its curing temperature is low, in rubber, easily disperse, do not pollute, can improve the physical and mechanical property of rubber item, can be directly used in and make tire, adhesive tape, rubber overshoes and other industrial rubber articles, also being the intermediate of producing other vulcanization accelerator, is a kind of promotor product that has the call on the market.Produce captax at present both at home and abroad and mainly adopt acid-base method, as document (Inner Mongol petrochemical complex, 2005,9:12) Bao Dao orthogonal test production method and document (petro-technology and application, 1996,14:48) Bao Dao production method.The technological principle of acid-base method is: aniline, sulphur, dithiocarbonic anhydride generate M and by product resin after height is pressed into, add NaOH and M reaction and generate M-Na, after filtering out resin, generate M and saltcake with sulfuric acid and M-Na neutralization reaction, be washed to neutrality through repeated multiple times, remove the saltcake in the M material, after dehydration, drying, pulverizing, produce finished product M again.The characteristics of acid-base method technology are: technical qualification are less demanding, and working method is easily grasped, and cost is low, and disposable qualification rate is stable etc., therefore by the widespread use of domestic production producer.But there is also fatal shortcoming: be with a large amount of caustic soda and sulfuric acid reaction, neutralization, washing, the ton product produces the high-concentration waste water of 60-80 ton, seriously polluted, intractability is very big, the present domestic sophisticated treatment technology that also do not have, do not meet the environmental protection policy of country, and equipment corrosion is serious, the ratio of depreciation height.
Summary of the invention
The objective of the invention is to solve the post-processed that exists in the production technique of existing rubber accelerator 2-thiol group benzothiazole and produce a large amount of high-concentration waste waters, seriously polluted, intractability is very big, and equipment corrosion is serious, the technical problem that ratio of depreciation is high.Provide a kind of no waste water to produce, flow process is short, and schedule of operation is simple relatively, the production technique of free from corrosion rubber accelerator 2-thiol group benzothiazole.
The objective of the invention is to be achieved through the following technical solutions:
The production technique of rubber accelerator 2-thiol group benzothiazole of the present invention, in reactor, add dithiocarbonic anhydride and sulphur, at 25～30 ℃, rotating speed is to stir 2～4 hours under 20～60 rev/mins the condition, add aniline, the mol ratio of aniline, dithiocarbonic anhydride and sulphur is 1: 0.8～1.0: 0.6～0.8, be warming up to 150～300 ℃, at pressure is to react under 0.7～9.5Mpa 60～120 minutes, with toluene extraction 5～25 minutes, to filter, toluene is reclaimed in distillation, re-extract 2～3 times obtains the 2-thiol benzothiazole after the drying.
The add-on of toluene is 0.8～1.2 times of raw material gross weight when extracting with toluene.Pressure when toluene is reclaimed in distillation is 0.25～0.35MPa, and distillation temperature is no more than 128 ℃.
Compare with prior art, the present invention directly extracts the 2-thiol benzothiazole with toluene behind Synthetic 2-thiol benzothiazole, toluene is reclaimed in distillation then, do not need to carry out " neutralization " and " washing " with a large amount of soda acids, thereby avoided the generation of a large amount of waste water, reduced environmental pollution, and equipment has not been had corrosion; Technical process of the present invention in addition is short.Utilize the toluene soluble resin and be beneficial to the principle of recovery, reclaim toluene, and logical toluene cyclic utilization system carries out 2～3 extractions, resin is all discharged, obtain 2-thiol benzothiazole quality product height with the distillatory method.
Embodiment
Embodiment 1
300Kg dithiocarbonic anhydride and 100Kg sulphur are added reactor, are to stir 2 hours under 20 rev/mins the condition at 25 ℃, rotating speed, add 400Kg aniline, when being warming up to 150 ℃, pressure rises to 7.0Mpa, reacts after 60 minutes, with 700Kg toluene extraction 5 minutes, filtering, is 0.25MPa at pressure, and temperature is no more than 128 ℃ of distillation recovery toluene down, re-extract 2 times, obtain vulcanization accelerator 2-thiol benzothiazole after the drying, yield reaches 90%, and the main performance index fusing point reaches 180.1 ℃.
Embodiment 2
350Kg dithiocarbonic anhydride and 130Kg sulphur are added reactor, are to stir 2.5 hours under 30 rev/mins the condition at 26 ℃, rotating speed, add 500Kg aniline, when being warming up to 200 ℃, pressure rises to 7.5Mpa, reacts after 70 minutes, with 784Kg toluene extraction 10 minutes, filtering, is 0.30MPa at pressure, and temperature is no more than 128 ℃ of distillation recovery toluene down, re-extract 3 times, obtain accelerator M after the drying, yield reaches 90.5%, and the main performance index fusing point reaches 180.4 ℃.
Embodiment 3
400Kg dithiocarbonic anhydride and 150Kg sulphur are added reactor, are to stir 3 hours under 40 rev/mins the condition at 27 ℃, rotating speed, add 550Kg aniline, when being warming up to 240 ℃, pressure rises to 8.0Mpa, reacts after 80 minutes, with 1320Kg toluene extraction 15 minutes, filtering, is 0.35MPa at pressure, and temperature is no more than 128 ℃ of distillation recovery toluene down, re-extract 3 times, obtain accelerator M after the drying, yield reaches 91%, and the main performance index fusing point reaches 181.2 ℃.
Embodiment 4
500Kg dithiocarbonic anhydride and 180Kg sulphur are added reactor, are to stir 3.5 hours under 50 rev/mins the condition at 28 ℃, rotating speed, add 700Kg aniline, when being warming up to 260 ℃, pressure rises to 8.5Mpa, reacts after 100 minutes, with toluene extraction 20 minutes, filtering, is 0.32MPa at pressure, and temperature is no more than 128 ℃ of distillation recovery toluene down, re-extract 3 times, obtain accelerator M after the drying, yield reaches 92%, and the main performance index fusing point reaches 180.8 ℃.
Embodiment 5
600Kg dithiocarbonic anhydride and 200Kg sulphur are added reactor, are to stir 4 hours under 60 rev/mins the condition at 30 ℃, rotating speed, add 800Kg aniline, when being warming up to 300 ℃, pressure rises to 9.0Mpa, reacts after 120 minutes, with toluene extraction 25 minutes, filtering, is 0.28MPa at pressure, and temperature is no more than 128 ℃ of distillation recovery toluene down, re-extract 3 times, obtain accelerator M after the drying, yield reaches 91.5%, and the main performance index fusing point reaches 181.6 ℃.
Claims (3)
1, a kind of production technique of rubber accelerator 2-thiol group benzothiazole, in reactor, add dithiocarbonic anhydride and sulphur, at 25～30 ℃, rotating speed is to stir 2～4 hours under 20～60 rev/mins the condition, add aniline, the mol ratio of aniline, dithiocarbonic anhydride and sulphur is 1: 0.8～1.0: 0.6～0.8, be warming up to 150～300 ℃, at pressure is to react under 0.7～9.5Mpa 60～120 minutes, with toluene extraction 5～25 minutes, to filter, toluene is reclaimed in distillation, re-extract 2～3 times obtains the 2-thiol benzothiazole after the drying.
2, the production technique of rubber accelerator 2-thiol group benzothiazole according to claim 1 is characterized in that: the add-on of toluene is 0.8～1.2 times of raw material gross weight when extracting with toluene.
3, the production technique of rubber accelerator 2-thiol group benzothiazole according to claim 1 and 2 is characterized in that: the pressure when toluene is reclaimed in distillation is 0.25～0.35MPa, and distillation temperature is no more than 128 ℃.
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| Application Number | Priority Date | Filing Date | Title |
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| CN200810140886A CN101638396A (en) | 2008-08-01 | 2008-08-01 | Production process for rubber accelerator 2-thiol group benzothiazole |
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| CN200810140886A CN101638396A (en) | 2008-08-01 | 2008-08-01 | Production process for rubber accelerator 2-thiol group benzothiazole |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102304099A (en) * | 2011-07-11 | 2012-01-04 | 南开大学 | Improved method for synthesizing 2-mercaptobenzothiazole derivative |
| 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 |
| CN102850292A (en) * | 2011-06-30 | 2013-01-02 | 鹤壁市恒瑞橡塑材料有限公司 | Totally enclosed clean production system for rubber vulcanization accelerator 2-mercaptobenzothiazole |
| CN106432133A (en) * | 2016-09-30 | 2017-02-22 | 王显权 | Preparation method of 2-mercaptobenzothiazole |
| JP2018531286A (en) * | 2015-10-09 | 2018-10-25 | 聖奥化学科技有限公司Ｓｅｎｎｉｃｓ Ｃｏ．，Ｌｔｄ． | Method for preparing 2-mercaptobenzothiazole |
-
2008
- 2008-08-01 CN CN200810140886A patent/CN101638396A/en active Pending
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102850292A (en) * | 2011-06-30 | 2013-01-02 | 鹤壁市恒瑞橡塑材料有限公司 | Totally enclosed clean production system for rubber vulcanization accelerator 2-mercaptobenzothiazole |
| CN102850292B (en) * | 2011-06-30 | 2014-05-07 | 鹤壁市恒瑞橡塑材料有限公司 | Totally enclosed clean production system for rubber vulcanization accelerator 2-mercaptobenzothiazole |
| CN102304099A (en) * | 2011-07-11 | 2012-01-04 | 南开大学 | Improved method for synthesizing 2-mercaptobenzothiazole derivative |
| 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 |
| JP2018531286A (en) * | 2015-10-09 | 2018-10-25 | 聖奥化学科技有限公司Ｓｅｎｎｉｃｓ Ｃｏ．，Ｌｔｄ． | Method for preparing 2-mercaptobenzothiazole |
| CN106432133A (en) * | 2016-09-30 | 2017-02-22 | 王显权 | Preparation method of 2-mercaptobenzothiazole |
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