CN101100460A

CN101100460A - Method for producing rubber vulcanization accelerator

Info

Publication number: CN101100460A
Application number: CNA2007100585689A
Authority: CN
Inventors: 王树华; 洪学斌; 王树领; 王树恒; 孟庆保
Original assignee: TIANJIN KEMAI CHEMICAL CO Ltd
Current assignee: TIANJIN KEMAI CHEMICAL CO Ltd
Priority date: 2007-08-02
Filing date: 2007-08-02
Publication date: 2008-01-09

Abstract

Production of rubber vulcanization accelerator CZ is carried out by mixing water with cyclohexylamine in proportion of 1:0.8-1.2 mol, adding mixed liquor into oxidizing kettle, adding into 80-90 wt% accelerator M slurry 20-100 ml at 20-70 deg. C and 200-1200 rotation/ min by 20-50 ml/min, dripping 10-30 wt% sodium hypochlorite into solution by 40-90 ml/min for 1-10 mins, dripping 80-90 wt% accelerator M slurry into solution by 50-110 ml/min for 10-30 mins, sampling, stopping dripping sodium hypochlorite and accelerator M while changing material into gray or white, pump filtering, washing by water, filtering and drying to obtain final product. CZ accelerator yield reaches above 99%. It's easy and saves resources and can be used for industrial production.

Description

The production method of rubber vulcanization accelerant CZ

Technical field

The present invention relates to the production method of a kind of thiofide N cyclohexyl 2 benzothiazole sulfenamide (CZ), belong to the rubber vulcanization accelerant CZ 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, CZ is the requisite a kind of primary accelerator of present rubber industry.Accelerant CZ is active aftereffect half ultra fast accelerator of a kind of height, and scorching quality is good, process safety, and curing time is short.Document (fine chemistry industry, 2006,23:923) reported the method that catalytic oxidation synthesizes CZ.With stirring in captax, hexahydroaniline, catalyzer, the water adding reactor, make its salify; React cooling, suction filtration, washing, filtration, the dry product that gets as oxygenant with hydrogen peroxide.The hexahydroaniline amount that this method is used is big, and the yield of accelerant CZ is not high.Document (the Guangxi chemical industry, 1994,23:58) reported the fast synthesis method of accelerant CZ.With stirring in captax, hexahydroaniline, catalyzer, the water adding reactor, make its salify; React suction filtration, washing, filtration, the dry product that gets as oxygenant with clorox.This method accelerant CZ yield is low.

Summary of the invention

The object of the present invention is to provide a kind of production method of rubber vulcanization accelerant CZ, this method is simple to operate, and the hexahydroaniline consumption is little, yield is high.

For achieving the above object, the present invention is realized by following technical proposals: a kind of production method of rubber vulcanization accelerant CZ is characterized in that comprising following process:

1. the volume ratio by water and hexahydroaniline is 1: 0.8～1.2, water and hexahydroaniline mixing liquid are joined in the stills for air blowing, at 20～70 ℃, rotating speed is under 200～1200 rev/mins the condition, flow velocity with 20～50ml/ minute, the adding mass content is captax slip 20～100ml of 80～90%, then with 40～90ml/ minute flow velocity, the dropping mass content is 10～30% chlorine bleach liquor in solution, after 1～10 minute with 50～110ml/ minute flow velocity, the dropping mass content is 80～90% captax slip in solution, after 10～30 minutes, the material color is observed in sampling, when the material color is grey or white, stops to drip clorox and captax, suction filtration, washing, filter, the dry rubber accelerator CZ product that gets, the yield of accelerant CZ reaches more than 99%.

The invention has the advantages that: this procedure is simple, is easy to industrialization, and the hexahydroaniline of use is few, and the yield of accelerant CZ reaches more than 99%.

Embodiment

Example 1:

At 270～280 ℃, carry out condensation reaction under pressure 9～10Mpa condition with aniline and curing charcoal, sulphur, generate mass content and be 92% MBT.100ml water and 80ml hexahydroaniline mixing liquid are joined in the stills for air blowing, at 25 ℃, rotating speed is under 300 rev/mins the condition, flow velocity with 20ml/ minute, the adding mass content is 80% captax slip 20ml, then with 40ml/ minute flow velocity, the dropping mass content is 10% chlorine bleach liquor in solution, after 2 minutes with 50ml/ minute flow velocity, the dropping mass content is 80% captax slip in solution, after 15 minutes, the material color is observed in sampling, when the material color is grey or white, stop to drip clorox and captax, suction filtration, washing, filter, drying obtains rubber accelerator CZ product.The yield of this N cyclohexyl 2 benzothiazole sulfenamide is 99.2%.

Example 2:

The MBT that present embodiment adopted is identical with embodiment 1,150ml water and 150ml hexahydroaniline mixing liquid are joined in the stills for air blowing, at 50 ℃, rotating speed is under 600 rev/mins the condition, flow velocity with 35ml/ minute, the adding mass content is 85% captax slip 30ml, then with 45ml/ minute flow velocity, the dropping mass content is 15% chlorine bleach liquor in solution, after 5 minutes with 60ml/ minute flow velocity, the dropping mass content is 85% captax slip in solution, after 20 minutes, the material color is observed in sampling, when the material color is grey or white, stop to drip clorox and captax, suction filtration, washing, filter, drying obtains rubber accelerator CZ product.The yield of this N cyclohexyl 2 benzothiazole sulfenamide is 99.3%.

Example 3:

The technology of the synthetic MBT that present embodiment adopted is identical with embodiment 1.100ml water and 120ml hexahydroaniline mixing liquid are joined in the stills for air blowing, at 70 ℃, rotating speed is under 1000 rev/mins the condition, flow velocity with 50ml/ minute, the adding mass content is 85% captax slip 30ml, then with 75ml/ minute flow velocity, the dropping mass content is 15% chlorine bleach liquor in solution, after 10 minutes with 80ml/ minute flow velocity, the dropping mass content is 85% captax slip in solution, after 30 minutes, the material color is observed in sampling, when the material color is grey or white, stop to drip clorox and captax, suction filtration, washing, filter, drying obtains rubber accelerator CZ product.The yield of this N cyclohexyl 2 benzothiazole sulfenamide is 99.6%.

Claims

1. the production method of a rubber vulcanization accelerant CZ, it is characterized in that comprising following process: the volume ratio by water and hexahydroaniline is 1: 0.8～1.2, water and hexahydroaniline mixing liquid are joined in the stills for air blowing, at 20～70 ℃, rotating speed is under 200～1200 rev/mins the condition, flow velocity with 20～50ml/ minute, the adding mass content is captax slip 20～100ml of 80～90%, then with 40～90ml/ minute flow velocity, the dropping mass content is 10～30% chlorine bleach liquor in solution, after 1～10 minute with 50～110ml/ minute flow velocity, the dropping mass content is 80～90% captax slip in solution, after 10～30 minutes, the material color is observed in sampling, when the material color is grey or white, stop to drip clorox and captax, suction filtration, washing, filter, the dry rubber accelerator CZ product that gets, the yield of accelerant CZ reaches more than 99%.