Preparation method of rubber accelerator DZ (N,N-Dicyclohexyl-2-benzothiazolsulfene amide)

A technology of rubber accelerator and dicyclohexylamine, which is applied in the field of preparation of rubber additives, can solve the problems of difficult washing of waste salt, slow dissolution speed, and long reaction time, and achieve high solubility, fast reaction speed, and dissolution speed fast effect

Inactive Publication Date: 2013-05-15
JIANGSU GUOLI CHEM TECH
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  • Summary
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  • Application Information

AI Technical Summary

Problems solved by technology

At present, its production technology usually uses strong bases such as sodium hydroxide or sodium methoxide as acid-binding agents. The cost of raw materials for acid-binding agents is high, it needs to be dissolved and the dissolution rate is slow, the reaction time is long, and water is often formed, which is not good for the reaction. , the waste salt is difficult to wash off, and the product yield is low

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment Construction

[0011] Prepare materials according to the ratio of 50kg of dicyclohexylamine and 55kg of sodium hypochlorite, add dicyclohexylamine into a reactor with a stirring device, and there is a reflux condenser on the reactor to heat and stir for 2 hours, then drip sodium hypochlorite into the reactor, Continue to stir for 1.5 h after dropping, and control the reaction temperature at 35-40 degrees Celsius during the whole process.

[0012] After the reaction is completed, the reactants are precipitated and separated while they are hot, and the aqueous solution of the lower layer and the flocculent impurities in the middle are released to obtain dicyclohexyl chloride.

[0013] Add 2, 2'-dithiodibenzothiazole, dicyclohexylamine and chlorinated dicyclohexylamine into the reaction kettle, the weight ratio of the three is 1:1.2:1.2, add anhydrous methanol to dissolve, stir and mix well , heat, feed ammonia gas under normal pressure, maintain 60-65 degrees Celsius and react for 5-10 minutes...

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Abstract

The invention relates to a preparation method of a rubber auxiliary, in particular to a preparation method of a rubber accelerator DZ (N,N-Dicyclohexyl-2-benzothiazolsulfene amide). An accelerator DM (dibenzothiazole disulfide) and dicyclohexylamine are adopted as raw materials, ammonia gas is taken as an acid-binding agent and methyl alcohol is taken as a solvent for synthesizing a rubber vulcanization accelerator DZ. According to the preparation method, the ammonia gas is adopted as the acid-binding agent, the ammonia gas is cheap, dosage of the ammonia gas is low, a reaction speed is high, and product quality is high, so that the prepared method provided by the invention is applicable to industrial production; and the obtained mother liquor and alcohol lotion can be recycled, and the total yield is close to 100%.

Description

technical field [0001] The invention relates to a method for preparing a rubber auxiliary agent, in particular to a method for preparing a rubber accelerator DZ. Background technique [0002] Rubber accelerator DZ (N,N-dicyclohexylamine-2-benzothiazole sulfenamide, molecular formula C19H26N2S2) is an excellent slow-acting sulfenyl accelerator, suitable for high active reinforcing agent dosage Among the larger rubber compounds, it has better mechanical properties and dynamic properties. At present, its production technology usually uses strong bases such as sodium hydroxide or sodium methoxide as acid-binding agents. The cost of raw materials for acid-binding agents is high, it needs to be dissolved and the dissolution rate is slow, the reaction time is long, and water is often formed, which is not good for the reaction. , the waste salt is difficult to wash off, and the product yield is low. Contents of the invention [0003] For above-mentioned technical problem, the pr...

Claims

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Application Information

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Patent Type & AuthorityApplications(China)
IPC IPC(8): C07D277/80
Inventor胡立新郎旭东宗红兴
OwnerJIANGSU GUOLI CHEM TECH