CN101367776A - Novel production method of rubber vulcanization accelerant MBT - Google Patents
Novel production method of rubber vulcanization accelerant MBT Download PDFInfo
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- CN101367776A CN101367776A CNA200810052073XA CN200810052073A CN101367776A CN 101367776 A CN101367776 A CN 101367776A CN A200810052073X A CNA200810052073X A CN A200810052073XA CN 200810052073 A CN200810052073 A CN 200810052073A CN 101367776 A CN101367776 A CN 101367776A
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- state sulfur
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- thiofide
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Abstract
The present invention discloses a novel production method of thiofide MBT. The method comprises the following steps: 200 to 2200 grams of aniline and 50 to 100 grams of carbon bisulfide are added into an oxidization reactor with a catalyst KM-02; under the conditions with the temperature between 100 DEG C and 550 DEG C and the rotating speed of 100 to 4000 rounds per minute, liquid sulfur is added at a flow rate between 10 ml/m and 220 ml/m and is stopped to be added after the reaction lasts for 10 to 150 minutes, the prepared mixture is pumped, washed, filtered and dried to produce the thiofide MBT product, the yield rate of the thiofide MBT reaches above 79 percent, and the melting point of the thiofide MBT is above 179 DEG C. The present invention has the advantages that the process is simple, the industrialization of the process can be easily realized, the security is high, the pollution is less, the liquid sulfur is used, the yield rate is high, and the quality of the MBT is high.
Description
Technical field
The present invention relates to the new process for producing of a kind of thiofide 2-benzothiazolyl mercaptan (MBT), belong to the rubber vulcanization accelerant MBT production technical field.
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, and yield is not high.Document (petro-technology and application, 1996,14:48) reported the production method of accelerant MBT.Equally, this method is polluted greatly, 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 new process for producing of rubber vulcanization accelerant MBT, this method is simple to operate, pollute little, adopt the MBT quality of liquid-state sulfur, yield height, gained good.
For achieving the above object, the present invention is realized by following technical proposals: a kind of new process for producing of rubber vulcanization accelerant MBT is characterized in that comprising following process:
1. 200～2200 gram aniline and 50～100 gram dithiocarbonic anhydride are joined in the stills for air blowing that catalyzer KM-02 is housed, be under 100～4000 rev/mins the condition at 100～550 ℃, rotating speed, flow velocity with 10～220ml/ minute, add liquid-state sulfur, react after 10～150 minutes, stop to add liquid-state sulfur, suction filtration, washing, filtration, the dry rubber accelerator MBT product that gets, the yield of accelerant MBT reaches more than 79%, and fusing point reaches more than 179 ℃.
The invention has the advantages that: this procedure is simple, is easy to industrialization, and is safe, pollute little, adopt the MBT quality of liquid-state sulfur, yield height, gained good.
Embodiment
Example 1:
200 gram aniline and 50 gram dithiocarbonic anhydride are joined in the stills for air blowing that catalyzer KM-02 is housed, be under 100 rev/mins the condition at 200 ℃, rotating speed, flow velocity with 10ml/ minute, add liquid-state sulfur, react after 50 minutes, stop to add liquid-state sulfur, suction filtration, washing, filtration, the dry rubber accelerator MBT product that gets, the yield of this 2-benzothiazolyl mercaptan reaches 80%, and fusing point reaches 179.2 ℃.
Example 2:
400 gram aniline and 60 gram dithiocarbonic anhydride are joined in the stills for air blowing that catalyzer KM-02 is housed, be under 400 rev/mins the condition at 400 ℃, rotating speed, flow velocity with 20ml/ minute, add liquid-state sulfur, react after 40 minutes, stop to add liquid-state sulfur, suction filtration, washing, filtration, the dry rubber accelerator MBT product that gets, the yield of this 2-benzothiazolyl mercaptan reaches 81%, and fusing point reaches 179.0 ℃.
Example 3:
600 gram aniline and 70 gram dithiocarbonic anhydride are joined in the stills for air blowing that catalyzer KM-02 is housed, be under 1000 rev/mins the condition at 300 ℃, rotating speed, flow velocity with 100ml/ minute, add liquid-state sulfur, react after 10 minutes, stop to add liquid-state sulfur, suction filtration, washing, filtration, the dry rubber accelerator MBT product that gets, the yield of this 2-benzothiazolyl mercaptan reaches 86%, and fusing point reaches 179.9 ℃.
Example 4:
800 gram aniline and 80 gram dithiocarbonic anhydride are joined in the stills for air blowing that catalyzer KM-02 is housed, be under 500 rev/mins the condition at 276 ℃, rotating speed, flow velocity with 60ml/ minute, add liquid-state sulfur, react after 20 minutes, stop to add liquid-state sulfur, suction filtration, washing, filtration, the dry rubber accelerator MBT product that gets, the yield of this 2-benzothiazolyl mercaptan reaches 90%, and fusing point reaches 179.4 ℃.
Example 5:
1000 gram aniline and 100 gram dithiocarbonic anhydride are joined in the stills for air blowing that catalyzer KM-02 is housed, be under 600 rev/mins the condition at 241 ℃, rotating speed, flow velocity with 30ml/ minute, add liquid-state sulfur, react after 100 minutes, stop to add liquid-state sulfur, suction filtration, washing, filtration, the dry rubber accelerator MBT product that gets, the yield of this 2-benzothiazolyl mercaptan reaches 88%, and fusing point reaches 179.1 ℃.
Claims (1)
1. the new process for producing of a rubber vulcanization accelerant MBT, it is characterized in that comprising following process: 200～2200 gram aniline and 50～100 gram dithiocarbonic anhydride are joined in the stills for air blowing that catalyzer KM-02 is housed, be under 100～4000 rev/mins the condition at 100～550 ℃, rotating speed, flow velocity with 10～220ml/ minute, add liquid-state sulfur, react after 10～150 minutes, stop to add liquid-state sulfur, suction filtration, washing, filtration, the dry rubber accelerator MBT product that gets, the yield of accelerant MBT reaches more than 79%, and fusing point reaches more than 179 ℃.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNA200810052073XA CN101367776A (en) | 2008-01-16 | 2008-01-16 | Novel production method of rubber vulcanization accelerant MBT |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNA200810052073XA CN101367776A (en) | 2008-01-16 | 2008-01-16 | Novel production method of rubber vulcanization accelerant MBT |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN101367776A true CN101367776A (en) | 2009-02-18 |
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Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
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| CNA200810052073XA Pending CN101367776A (en) | 2008-01-16 | 2008-01-16 | Novel production method of rubber vulcanization accelerant MBT |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN101367776A (en) |
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2008
- 2008-01-16 CN CNA200810052073XA patent/CN101367776A/en active Pending
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| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C02 | Deemed withdrawal of patent application after publication (patent law 2001) | ||
| WD01 | Invention patent application deemed withdrawn after publication |
Open date: 20090218 |