CN104592155A - Preparation method of rubber promoter 2,2'-dithiobis(benzothiazole) - Google Patents
Preparation method of rubber promoter 2,2'-dithiobis(benzothiazole) Download PDFInfo
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- CN104592155A CN104592155A CN201310520621.8A CN201310520621A CN104592155A CN 104592155 A CN104592155 A CN 104592155A CN 201310520621 A CN201310520621 A CN 201310520621A CN 104592155 A CN104592155 A CN 104592155A
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- dithiobis
- benzothiazole
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07D—HETEROCYCLIC COMPOUNDS
- C07D277/00—Heterocyclic compounds containing 1,3-thiazole or hydrogenated 1,3-thiazole rings
- C07D277/60—Heterocyclic compounds containing 1,3-thiazole or hydrogenated 1,3-thiazole rings condensed with carbocyclic rings or ring systems
- C07D277/62—Benzothiazoles
- C07D277/68—Benzothiazoles with hetero atoms or with carbon atoms having three bonds to hetero atoms with at the most one bond to halogen, e.g. ester or nitrile radicals, directly attached in position 2
- C07D277/70—Sulfur atoms
- C07D277/76—Sulfur atoms attached to a second hetero atom
- C07D277/78—Sulfur atoms attached to a second hetero atom to a second sulphur atom
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Thiazole And Isothizaole Compounds (AREA)
Abstract
The invention discloses a preparation method of rubber promoter 2,2'-dithiobis(benzothiazole). The preparation method comprises following steps: step 1, refined 2-mercaptobenzothiazole and an organic solvent are delivered into a four-mouth flask provided with an electric stirrer, a condenser pipe, a dropping funnel, and a thermometer, the four-mouth flask is subjected to thermostatic waterbath, the temperature of an obtained reaction system is kept at 40 DEG C, stirring is carried out, solution pH is adjusted to 7, a mixture of a solvent with hydrogen peroxide is added dropwise for 1h, and reaction is carried out for 3h; and step 2, after reaction, 2,2'-dithiobis(benzothiazole) is obtained via filtering, water washing, and drying. According to the preparation method of rubber promoter 2,2'-dithiobis(benzothiazole), oxidation of 2-mercaptobenzothiazole is carried out directly; the preparation method is simple; yield is high; quality of obtained products is reliable; solvents can be recycled; and no environmental pollution is caused.
Description
Technical field
The present invention relates to a kind of preparation method of rubber accelerator, be specifically related to a kind of preparation method of dibenzothiazyl disulfide.
Background technology
Dibenzothiazyl disulfide have that sulfuration promoter action is fast, sulfuration flatness is low and mixing time without features such as scorchings, being widely used in Rubber processing industry, is the universal vulcanization accelerator of natural rubber, synthetic rubber and regenerated rubber.Conventional method is that raw material consumption is many by 2-benzothiazolyl mercaptan through oxidizing preparation, and production cost is high, and causes environmental pollution.
Summary of the invention
The object of the invention is to, provide a kind of preparation method of rubber accelerator dibenzothiazyl disulfide, technique is simple, and yield is high, products obtained therefrom reliable in quality, and solvent can be recycled, and can not pollute environment.
The preparation method of described rubber accelerator dibenzothiazyl disulfide, it comprises the following steps:
One, the di-mercaptobenzothiazolby after refining, organic solvent are added in the four-hole boiling flask with electric stirring, prolong, dropping funnel, thermometer, flask being placed in water bath with thermostatic control keeps temperature of reaction system to be 40 DEG C, start stirring, regulator solution pH to 7, drip the mixture of solvent and hydrogen peroxide, 1h dropwises, reaction 3h;
Two, react complete, filter, washing, is drying to obtain dibenzothiazyl disulfide.
The preparation method of rubber accelerator dibenzothiazyl disulfide provided by the invention, its beneficial effect is, is directly oxidized di-mercaptobenzothiazolby solid, technique is simple, and yield is high, products obtained therefrom reliable in quality, solvent can be recycled, and can not pollute environment.
Embodiment
Below in conjunction with an embodiment, the preparation method of rubber accelerator dibenzothiazyl disulfide provided by the invention is described in detail.
Embodiment
One, the di-mercaptobenzothiazolby after refining, organic solvent are added in the four-hole boiling flask with electric stirring, prolong, dropping funnel, thermometer, flask being placed in water bath with thermostatic control keeps temperature of reaction system to be 40 DEG C, start stirring, regulator solution pH to 7, drip the mixture of solvent and hydrogen peroxide, 1h dropwises, reaction 3h;
Two, react complete, filter, washing, is drying to obtain dibenzothiazyl disulfide.
Claims (1)
1. a preparation method for rubber accelerator dibenzothiazyl disulfide, is characterized in that: it comprises the following steps:
One, the di-mercaptobenzothiazolby after refining, organic solvent are added in the four-hole boiling flask with electric stirring, prolong, dropping funnel, thermometer, flask being placed in water bath with thermostatic control keeps temperature of reaction system to be 40 DEG C, start stirring, regulator solution pH to 7, drip the mixture of solvent and hydrogen peroxide, 1h dropwises, reaction 3h;
Two, react complete, filter, washing, is drying to obtain dibenzothiazyl disulfide.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201310520621.8A CN104592155A (en) | 2013-10-30 | 2013-10-30 | Preparation method of rubber promoter 2,2'-dithiobis(benzothiazole) |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201310520621.8A CN104592155A (en) | 2013-10-30 | 2013-10-30 | Preparation method of rubber promoter 2,2'-dithiobis(benzothiazole) |
Publications (1)
| Publication Number | Publication Date |
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| CN104592155A true CN104592155A (en) | 2015-05-06 |
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| Application Number | Title | Priority Date | Filing Date |
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| CN201310520621.8A Pending CN104592155A (en) | 2013-10-30 | 2013-10-30 | Preparation method of rubber promoter 2,2'-dithiobis(benzothiazole) |
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| CN (1) | CN104592155A (en) |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105801911A (en) * | 2016-04-22 | 2016-07-27 | 宁波硫华聚合物有限公司 | Rubber accelerator dibenzothiazyl disulfide pre-dispersed rubber master batch particle and preparation method thereof |
| CN107365281A (en) * | 2017-08-28 | 2017-11-21 | 青岛科技大学 | A kind of synthetic method of diphenyl disulfide a pair of horses going side by side thiazole |
| CN108218810A (en) * | 2018-01-18 | 2018-06-29 | 清华大学 | A kind of micro- reaction method for synthesizing 2,2 '-dithio-bis-benzothiazole |
-
2013
- 2013-10-30 CN CN201310520621.8A patent/CN104592155A/en active Pending
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105801911A (en) * | 2016-04-22 | 2016-07-27 | 宁波硫华聚合物有限公司 | Rubber accelerator dibenzothiazyl disulfide pre-dispersed rubber master batch particle and preparation method thereof |
| CN107365281A (en) * | 2017-08-28 | 2017-11-21 | 青岛科技大学 | A kind of synthetic method of diphenyl disulfide a pair of horses going side by side thiazole |
| CN107365281B (en) * | 2017-08-28 | 2021-02-19 | 青岛科技大学 | Synthesis method of dibenzothiazole disulfide |
| CN108218810A (en) * | 2018-01-18 | 2018-06-29 | 清华大学 | A kind of micro- reaction method for synthesizing 2,2 '-dithio-bis-benzothiazole |
| CN108218810B (en) * | 2018-01-18 | 2020-09-11 | 清华大学 | Micro-reaction method for synthesizing 2,2' -dithiodibenzothiazole |
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| C06 | Publication | ||
| PB01 | Publication | ||
| WD01 | Invention patent application deemed withdrawn after publication |
Application publication date: 20150506 |