CN101759659A - Method for synthesizing thiofide MBT by liquid sulphur - Google Patents
Method for synthesizing thiofide MBT by liquid sulphur Download PDFInfo
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- CN101759659A CN101759659A CN200910228226A CN200910228226A CN101759659A CN 101759659 A CN101759659 A CN 101759659A CN 200910228226 A CN200910228226 A CN 200910228226A CN 200910228226 A CN200910228226 A CN 200910228226A CN 101759659 A CN101759659 A CN 101759659A
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Abstract
The invention discloses a method for synthesizing a thiofide MBT by liquid sulphur, comprising the following steps of: adding aniline, carbon disulfide and liquid sulphur to an oxidizing kettle according to the mole ratio of 1:1-2:1-3; reacting for 2-6 hours in a heat transfer oil heating way under the conditions that highest reaction pressure is 5-11 MPa, reaction temperature is 200-300 DEG C, stirring speed is 50-130 turns/minute, and then stopping reaction; and drying to obtain a thiofide MBT product, wherein the purity of the thiofide MBT is more than 92 percent. The method has simple process, easy industrialization, high safety, little pollution, liquid sulphur utilization, uniform reaction and good quality of the obtained thiofide MBT.
Description
Technical field
The present invention relates to a kind of method, belong to the rubber vulcanization accelerant MBT production technical field with liquid-state sulfur synthetic rubber vulcanization accelerator 2-benzothiazolyl mercaptan (MBT).
Background technology
Along with the development of rubber industry, the research of vulcanization accelerator more and more is subject to people's attention with production.Vulcanization accelerator plays important effect in vulcanization of rubber process, it can accelerate the reaction of rubber and vulcanizing agent greatly, boost productivity, also can improve the physical and mechanical properties of vulcanized rubber simultaneously, MBT is the requisite a kind of primary accelerator of present rubber industry.Document (Inner Mongol petrochemical complex, 2005,9:12) reported the method that orthogonal test is produced MBT.The mixture of oil of mirbane and aniline and dithiocarbonic anhydride and sulphur react under High Temperature High Pressure, make captax, and this method is polluted big, reacts inhomogeneous, and because of there being molten sulphur operation, hazard level height, product yield are not high, inefficiency.Document (petro-technology and application, 1996,14:48) reported the production method of accelerant MBT.Equally, this method is polluted greatly, and the hazard level height reacts inhomogeneous, and efficient is low, and the accelerant MBT of gained is of poor quality.
Summary of the invention
The object of the present invention is to provide a kind of method with liquid-state sulfur synthetic rubber accelerator M BT, this method is simple to operate, pollutes little, employing liquid-state sulfur, safe, and reaction is even, and the MBT quality of gained is good.
For achieving the above object, the present invention is realized by following technical proposals: a kind of method with liquid-state sulfur synthetic rubber accelerator M BT is characterized in that comprising following process:
1. with aniline: dithiocarbonic anhydride: liquid-state sulfur 1: 1 in molar ratio～2: 1～3 joins in the stills for air blowing, adopt the heat-conducting oil heating mode, at highest response pressure is that 5～11MPa, temperature of reaction are that 200～300 ℃, stirring velocity are under 50～130 rev/mins the condition, react after 2～6 hours, stopped reaction, get rubber accelerator MBT product after the drying, the purity of accelerant MBT reaches more than 92%.
The invention has the advantages that: this procedure is simple, is easy to industrialization, and is safe, pollute little, adopt liquid-state sulfur, reaction evenly, the MBT quality of gained is good.
Embodiment
Example 1:
465 gram aniline, 380 gram dithiocarbonic anhydride and 160 gram liquid-state sulfurs are joined in the stills for air blowing, adopt the heat-conducting oil heating mode, at highest response pressure is that 6MPa, temperature of reaction are that 200 ℃, stirring velocity are under 60 rev/mins the condition, react after 2 hours, stopped reaction, get rubber accelerator MBT product after the drying, the purity of this 2-benzothiazolyl mercaptan reaches 92.2%.
Example 2:
930 gram aniline, 836 gram dithiocarbonic anhydride and 320 gram liquid-state sulfurs are joined in the stills for air blowing, adopt the heat-conducting oil heating mode, at highest response pressure is that 7MPa, temperature of reaction are that 220 ℃, stirring velocity are under 70 rev/mins the condition, react after 3 hours, stopped reaction, get rubber accelerator MBT product after the drying, the purity of this 2-benzothiazolyl mercaptan reaches 92.3%.
Example 3:
1450 gram aniline, 1368 gram dithiocarbonic anhydride and 640 gram liquid-state sulfurs are joined in the stills for air blowing, adopt the heat-conducting oil heating mode, at highest response pressure is that 8MPa, temperature of reaction are that 240 ℃, stirring velocity are under 80 rev/mins the condition, react after 4 hours, stopped reaction, get rubber accelerator MBT product after the drying, the purity of this 2-benzothiazolyl mercaptan reaches 92.8%.
Example 4:
1450 gram aniline, 1368 gram dithiocarbonic anhydride and 640 gram liquid-state sulfurs are joined in the stills for air blowing, adopt the heat-conducting oil heating mode, at highest response pressure is that 10MPa, temperature of reaction are that 270 ℃, stirring velocity are under 130 rev/mins the condition, react after 5 hours, stopped reaction, get rubber accelerator MBT product after the drying, the purity of this 2-benzothiazolyl mercaptan reaches 92.5%.
Claims (1)
1. method with liquid-state sulfur synthetic rubber accelerator M BT, it is characterized in that comprising following process: with aniline: dithiocarbonic anhydride: liquid-state sulfur 1: 1 in molar ratio～2: 1～3 joins in the stills for air blowing, adopt the heat-conducting oil heating mode, at highest response pressure is that 5～11MPa, temperature of reaction are that 200～300 ℃, stirring velocity are under 50～130 rev/mins the condition, react after 2～6 hours, stopped reaction, get rubber accelerator MBT product after the drying, the purity of accelerant MBT reaches more than 92%.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN200910228226A CN101759659A (en) | 2009-11-16 | 2009-11-16 | Method for synthesizing thiofide MBT by liquid sulphur |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN200910228226A CN101759659A (en) | 2009-11-16 | 2009-11-16 | Method for synthesizing thiofide MBT by liquid sulphur |
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| Publication Number | Publication Date |
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| CN101759659A true CN101759659A (en) | 2010-06-30 |
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| CN200910228226A Pending CN101759659A (en) | 2009-11-16 | 2009-11-16 | Method for synthesizing thiofide MBT by liquid sulphur |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104151263A (en) * | 2014-08-08 | 2014-11-19 | 东营市晨宏橡胶助剂有限公司 | Anhydrous preparation technology for vulcanization promoter M |
| CN104592161A (en) * | 2014-12-29 | 2015-05-06 | 内蒙古科迈化工有限公司 | Method for producing rubber vulcanization accelerator CBS by crude product MBT |
| CN104610193A (en) * | 2014-12-29 | 2015-05-13 | 内蒙古科迈化工有限公司 | Preparation method of rubber vulcanizing accelerator TBBS |
| CN116120258A (en) * | 2022-12-21 | 2023-05-16 | 彤程化学（中国）有限公司 | Purification method of accelerator M |
-
2009
- 2009-11-16 CN CN200910228226A patent/CN101759659A/en active Pending
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104151263A (en) * | 2014-08-08 | 2014-11-19 | 东营市晨宏橡胶助剂有限公司 | Anhydrous preparation technology for vulcanization promoter M |
| CN104151263B (en) * | 2014-08-08 | 2016-03-16 | 东营市晨宏橡胶助剂有限公司 | The anhydrous preparation technology of 2 Mercaptobenzothiazole (MBT) |
| CN104592161A (en) * | 2014-12-29 | 2015-05-06 | 内蒙古科迈化工有限公司 | Method for producing rubber vulcanization accelerator CBS by crude product MBT |
| CN104610193A (en) * | 2014-12-29 | 2015-05-13 | 内蒙古科迈化工有限公司 | Preparation method of rubber vulcanizing accelerator TBBS |
| CN116120258A (en) * | 2022-12-21 | 2023-05-16 | 彤程化学（中国）有限公司 | Purification method of accelerator M |
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Application publication date: 20100630 |