CN103524454A

CN103524454A - Method for producing rubber vulcanization accelerant DZ by solvent method

Info

Publication number: CN103524454A
Application number: CN201310468637.9A
Authority: CN
Inventors: 朱军
Original assignee: Kemai Chemical Co Ltd
Current assignee: Kemai Chemical Co Ltd
Priority date: 2013-09-30
Filing date: 2013-09-30
Publication date: 2014-01-22

Abstract

The invention discloses a method for producing a rubber vulcanization accelerant DZ by a solvent method. With methanol as a solvent, hydrogen peroxide as an oxidant and an M-Na salt as raw material, the method is characterized by comprising the steps: adding 50 g of a 24% sulfuric acid into a reactor containing 43 g of dicyclohexylamine and 200-800 ml of methanol, under conditions of the temperature of 30-60 DEG C and the rotating speed of 800 rpm, fully undergoing a reaction of sulfuric acid with dicyclohexylamine, then dropwise adding 98 g of the M-Na salt, next adding the oxidant hydrogen peroxide with the content of 8-12% at the flowing speed of 5 ml/min, at the same time, controlling the pH of the reaction solution to 8-11 and the dropwise adding time of 2 h, after completing the reaction, carrying out suction filtration, washing with water, filtering, and drying to obtain the rubber accelerant DZ product. The purity of the product reaches 99% or more, and the yield of the product reaches 95%. The method has simple process, and is easy for industrialized production.

Description

Solvent method is produced the method for rubber vulcanization accelerator DZ

Technical field

The present invention relates to a kind of thiofide N, the production method of N-dicyclohexyl-2-[4-morpholinodithio sulphenamide (DZ), belongs to rubber vulcanization accelerator DZ production technical field.

Background technology

Along with the development of rubber industry, the research of vulcanization accelerator more and more comes into one's own with production.DZ is delayed action accelerator, is the requisite a kind of primary accelerator of current rubber industry.Be specially adapted to radial, there is sulfuration and promote and adhesive effect.Patent (patent No. 200810053774.5) the method process of delivering on July 8th, 2008 comprises: Virahol and dicyclohexyl amine are joined in stills for air blowing, under the condition stirring, make dicyclohexyl amine fully be dissolved in Virahol, add again sulfuric acid, control pH value simultaneously, then drip M-Na salt, drip oxygenant clorox simultaneously, in reaction process, control pH value, after completion of the reaction suction filtration, washing, filtration, the dry rubber accelerator DZ product that to obtain.Although the DZ quality that the method for this patent obtains has reached 99%, yield does not have concrete numerical value, and needs three kinds of raw materials to drip in operation simultaneously, operation more complicated.Document (scientific and technical information, 2005,7:23) reported the method for the synthetic DZ of large proportioning oxidation style.Captax, dicyclohexyl amine, Virahol are added in reactor and stirred, make its salify; With clorox, as oxygenant, react cooling, suction filtration, washing, filtration, the dry product that to obtain.The dicyclohexyl amine amount that this method is used is large, and the yield of accelerator DZ is not high.Document (China Synthetic Rubber Industry, 1996,19:317) reported the fast synthesis method of accelerator DZ.Captax, dicyclohexyl amine, Virahol are added in reactor and stirred, make its salify; With hydrogen peroxide, as oxygenant, react cooling, suction filtration, washing, filtration, the dry product that to obtain.This method accelerator DZ yield is low.Aforesaid method solvent all adopts Virahol, and can produce a large amount of brine wastes, to environment.

Summary of the invention

The object of the present invention is to provide a kind of take methyl alcohol as solvent, hydrogen peroxide be oxygenant, the method for M-Na salt as raw material production rubber vulcanization accelerator DZ of take, the method is simple to operate, do not produce a large amount of brine wastes, the DZ yield, the quality that synthesize are all higher, and solvent methanol is lower one times than the unit price of Virahol, so production cost is also low.

For achieving the above object, the present invention is realized by following technical proposals: a kind ofly take methyl alcohol as solvent, hydrogen peroxide are the method that oxygenant, the M-Na salt of take are raw material production rubber vulcanization accelerator DZ, it is characterized in that comprising following process:

The method process comprises: 24% sulfuric acid 50g joins in the reactor of existing 43 grams of dicyclohexyl amines and 200～800ml methyl alcohol, at 30-60 ℃, rotating speed, be under the condition of 800 revs/min, make sulfuric acid fully and dicyclohexyl amine react, drip again 98g M-Na salt, the flow velocity of then take 5ml/ minute adds the oxidant hydrogen peroxide that content is 8-12%, control the flat pH8-11 of reaction soln, time for adding is 2 hours simultaneously, after completion of the reaction suction filtration, washing, filtration, the dry rubber accelerator DZ product that to obtain.

The invention has the advantages that: the method process is simple, what oxygenant was used is that environment is not had to the hydrogen peroxide polluting, and reaction does not produce a large amount of brine wastes, and the methyl alcohol comparatively cheap by price is solvent, and the purity of the accelerator DZ synthesizing reaches more than 99%.Yield has reached more than 95%.

Embodiment

Example 1:

24% sulfuric acid 50g joins in the reactor of existing 43 grams of dicyclohexyl amines and 200ml methyl alcohol, at 30 ℃, rotating speed, be under the condition of 800 revs/min, make sulfuric acid fully and dicyclohexyl amine react, dripping 98g M-Na salt, the flow velocity of then take 5ml/ minute adds the oxidant hydrogen peroxide that content is 12%, control the pH8-11 of reaction soln, time for adding is 2 hours simultaneously, after completion of the reaction suction filtration, washing, filtration, the dry rubber accelerator DZ product that to obtain.

Example 2:

24% sulfuric acid 50g joins in the reactor of existing 43 grams of dicyclohexyl amines and 500ml methyl alcohol, at 45 ℃, rotating speed, be under the condition of 800 revs/min, make sulfuric acid fully and dicyclohexyl amine react, dripping 98g M-Na salt, the flow velocity of then take 5ml/ minute adds the oxidant hydrogen peroxide that content is 10%, control the pH8-11 of reaction soln, time for adding is 2 hours simultaneously, after completion of the reaction suction filtration, washing, filtration, the dry rubber accelerator DZ product that to obtain.

Example 3:

24% sulfuric acid 50g joins in the reactor of existing 43 grams of dicyclohexyl amines and 800ml methyl alcohol, at 60 ℃, rotating speed, be under the condition of 800 revs/min, make sulfuric acid fully and dicyclohexyl amine react, dripping 98g M-Na salt, the flow velocity of then take 5ml/ minute adds the oxidant hydrogen peroxide that content is 8%, control the pH8-11 of reaction soln, time for adding is 2 hours simultaneously, after completion of the reaction suction filtration, washing, filtration, the dry rubber accelerator DZ product that to obtain.

Claims

1. a solvent method is produced the method for rubber vulcanization accelerator DZ, take methyl alcohol as solvent, hydrogen peroxide is oxygenant, take M-Na salt as raw material, it is characterized in that 24% sulfuric acid 50g to join in the reactor of existing 43 grams of dicyclohexyl amines and 200～800ml methyl alcohol, at 30-60 ℃, rotating speed is under the condition of 800 revs/min, make sulfuric acid fully and dicyclohexyl amine react, drip again the flow velocity that then 98g M-Na salt take 5ml/ minute and add the oxidant hydrogen peroxide that content is 8-12%, control the pH8-11 of reaction soln simultaneously, time for adding is 2 hours, suction filtration after completion of the reaction, washing, filter, be dried to obtain rubber accelerator DZ product.