CN103102327A - Preparation method of rubber accelerator DZ (N,N-Dicyclohexyl-2-benzothiazolsulfene amide) - Google Patents

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

The rubber accelerator DZ preparation method

Technical field

The present invention relates to a kind of preparation method of rubber ingredients, be specially the rubber accelerator DZ preparation method.

Background technology

Rubber accelerator DZ (N, N-dicyclohexyl amine-2-[4-morpholinodithio sulphenamide, molecular formula is C19H26N2S2) be a kind of good late effect property time sulphonyl class promotor, be applicable in the sizing material of high reactivity strengthening agent large usage quantity, have mechanical property and dynamic property preferably.At present, its production technology adopts the highly basic such as sodium hydroxide or sodium methylate as acid binding agent usually, and the cost of acid binding agent raw material is higher, needs dissolving and dissolution rate slow, and long reaction time often has water to generate, and water is to reacting unfavorable, and abraum salt is difficult to wash away, and product yield is low.

Summary of the invention

For above-mentioned technical problem, the invention provides a kind of preparation method of cheap, rubber accelerator DZ that product yield is high, comprise the following steps:

Clorox is joined in dicyclohexyl amine, stir, Heating temperature to 35 degree centigrade, dicyclohexyl amine and clorox are according to weight ratio 1:1.1;

Reactant sedimentation layering divides except lower aqueous solution and middle cotton-shaped impurity, can make the chloro dicyclohexyl amine;

With 2,2'-dithio-bis-benzothiazole, dicyclohexyl amine and chloro dicyclohexyl amine add in reactor, three's weight ratio is that 1:1.2:1.2 adds the anhydrous methanol dissolving, stir, heating passes into ammonia under normal pressure, keep 60 ~ 65 degrees centigrade, react transparent to reaction system, stop logical ammonia, continue reaction 30min, be cooled to room temperature;

Suction filtration washes twice with methyl alcohol, washes twice;

Vacuum-drying gets the DZ product.

Ammonia solubleness in methyl alcohol is large, and dissolution rate is fast, has solved acid binding agent and dissolve this difficult problem of difficulty in solvent, has deducted acid binding agent dissolution process in suitability for industrialized production, has reduced investment cost and has improved throughput; React anhydrous generation, quality product is higher, and products therefrom need not other recrystallization or other purification operations.

Method provided by the invention adopts ammonia as acid binding agent, the low price of ammonia, and consumption is few, and speed of response is fast, and quality product is high, is fit to suitability for industrialized production, and the mother liquor that obtains and pure washing lotion can recycleds, and total recovery is near 100%.

Embodiment

Dicyclohexyl amine and 55kg clorox proportioning by 50kg are got the raw materials ready, dicyclohexyl amine is added in reactor with whipping appts, having reflux exchanger to heat on reactor stirred 2 hours, clorox is splashed in reactor, continue after dripping off to stir 1.5h, controlling temperature of reaction in whole process is 35 ~ 40 degrees centigrade again.

React complete, while hot with reactant sedimentation layering, emit lower aqueous solution and middle cotton-shaped impurity, can make the chloro dicyclohexyl amine.

With 2,2'-dithio-bis-benzothiazole, dicyclohexyl amine and chloro dicyclohexyl amine add in reactor, three's weight ratio is 1:1.2:1.2, add the anhydrous methanol dissolving, stirring and evenly mixing, heating, pass into ammonia under normal pressure, keep 60 ~ 65 degrees centigrade of reaction 5 ~ 10min, transparent to reaction system, stop logical ammonia, continue reaction 30min, be cooled to room temperature.

Suction filtration washes twice with methyl alcohol, washes twice.Vacuum-drying gets the DZ product.

Claims (1)

1. rubber accelerator DZ preparation method comprises the following steps:

Clorox is joined in dicyclohexyl amine, stir, Heating temperature to 35 degree centigrade, dicyclohexyl amine and clorox are according to weight ratio 1:1.1;

Reactant sedimentation layering divides except lower aqueous solution and middle cotton-shaped impurity, makes the chloro dicyclohexyl amine;

With 2,2'-dithio-bis-benzothiazole, dicyclohexyl amine and chloro dicyclohexyl amine add in reactor, three's weight ratio is that 1:1.2:1.2 adds the anhydrous methanol dissolving, stir, heating passes into ammonia under normal pressure, keep 60 ~ 65 degrees centigrade, react transparent to reaction system, stop logical ammonia, continue reaction 30min, be cooled to room temperature;

Suction filtration washes twice with methyl alcohol, washes twice;

Vacuum-drying gets the DZ product.