Looking for breakthrough ideas for innovation challenges? Try Patsnap Eureka!

Continuous production method for vulcanization accelerator DCBS

A technology of vulcanization accelerator and production method, which is applied in the field of rubber additives, can solve the problems of long reaction residence time, unguaranteed purity of reaction products, no enlightenment effect, etc., and achieve the effect of shortening reaction residence time

Inactive Publication Date: 2018-09-28
KEMAI CHEM
View PDF4 Cites 7 Cited by
  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Although this method provides a kind of continuous method for preparing rubber vulcanization accelerator CBS, this method does not have enlightenment effect to utilizing microchannel reactor to prepare DCBS, and reason is as follows: this method adopts excess cyclohexylamine as the solvent of product CBS, No solids are produced during the entire reaction process, and the reaction can proceed smoothly
However, dicyclohexylamine, the raw material of DCBS, cannot dissolve the product DCBS, and a large amount of solids will be produced during the synthesis process, which will block the pipeline and make the reaction impossible.
And the reaction residence time in the microchannel reactor is too long in this method, and the maximum flux of single reactor is only 15L / h, makes this technology do not possess industrialization capability at all, and reaction yield is relatively low (only in 87 %-95%), the purity of the reaction product cannot be guaranteed

Method used

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
View more

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0070] A continuous production method of vulcanization accelerator DCBS, comprising the following steps:

[0071] (1) configure M-Na salt solution: the accelerator MBT of 400g is mixed with the NaOH solution of 32wt% with 360g concentration, stir 2h at 50 ℃, make M-Na salt solution;

[0072] Configure the hydrochloric acid solution of cyclohexylamine: mix 567g of dicyclohexylamine and 376g of industrial hydrochloric acid with a concentration of 31wt%, add 567g of water, and stir at 35°C to obtain the hydrochloric acid solution of cyclohexylamine;

[0073] (2) the sodium hypochlorite solution that the hydrochloric acid solution of M-Na salt solution, dicyclohexylamine, solvent toluene and available chlorine content are 17% according to the hydrochloric acid solution 136mL / min of M-Na salt solution 69mL / min, dicyclohexylamine , toluene 130mL / min and sodium hypochlorite solution 49mL / min speed into the microchannel reactor for oxidation reaction, the reaction residence time is 2s...

Embodiment 2

[0077] A continuous production method of vulcanization accelerator DCBS, comprising the following steps:

[0078] (1) configure M-Na salt solution: the accelerator MBT of 400g is mixed with the NaOH solution of 32wt% with 360g concentration, stir 2h at 50 ℃, make M-Na salt solution;

[0079] (2) Configure the hydrochloric acid solution of dicyclohexylamine: mix 567g of dicyclohexylamine and 376g of industrial hydrochloric acid with a concentration of 31wt%, add 567g of water, and stir at 35°C to obtain the hydrochloric acid solution of dicyclohexylamine;

[0080] (3) the sodium hypochlorite solution that the hydrochloric acid solution of M-Na salt solution, dicyclohexylamine, solvent ethyl acetate and available chlorine content is 17% according to the hydrochloric acid solution 116mL / min of M-Na salt solution 59mL / min, cyclohexylamine Min, ethyl acetate 167mL / min and sodium hypochlorite solution 42mL / min are passed into the tower reactor for oxidation reaction, the reaction re...

Embodiment 3

[0084] A continuous production method of vulcanization accelerator DCBS, comprising the following steps:

[0085] (1) configure M-Na salt solution: the accelerator MBT of 400g is mixed with the NaOH solution of 1wt% with 11520g concentration, stir 2h at 50 ℃, make M-Na salt solution;

[0086] (2) Configure the hydrochloric acid solution of dicyclohexylamine: mix 567g of dicyclohexylamine and 376g of industrial hydrochloric acid with a concentration of 31wt%, add 567g of water, and stir at 35°C to obtain the hydrochloric acid solution of dicyclohexylamine;

[0087] (3) the mixture of M-Na salt solution, the hydrochloric acid solution of dicyclohexylamine, the solvent ethyl acetate and toluene (the mass ratio of ethyl acetate and toluene is 1:4) and the sodium hypochlorite solution that the available chlorine content is 17% According to M-Na salt solution 266mL / min, hydrochloric acid solution of cyclohexylamine 34mL / min, ethyl acetate 48mL / min and sodium hypochlorite solution 12...

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
Login to View More

PUM

No PUM Login to View More

Abstract

The invention provides a continuous production method for vulcanization accelerator DCBS. The continuous production method includes the steps that an MBT alkali solution, a dicyclohexylamine acid solution, solvent and oxidizing agent are subjected to an oxidizing reaction in a continuous flow reactor, then reacted materials are after-treated, and the vulcanization accelerator DCBS is obtained. According to the method, the MBT conversion percent is high, and the purity of the product is high; the continuous production method has the advantages of being high in reaction speed, high in product yield, low in wastewater COD (reacted wastewater is subjected to atmospheric distillation, residual solvent is recycled, and then the COD in residual water can be reduced to be 8,000 ppm or below), capable of facilitating treatment and the like, and is a new technology having the higher industry value.

Description

technical field [0001] The invention belongs to the field of rubber additives and relates to a continuous production method of a vulcanization accelerator DCBS. Background technique [0002] In the process of using rubber to produce various rubber products such as tires, hoses and rubber shoes, five types of additives must be used, which are rubber vulcanization accelerators (referred to as accelerators), rubber antioxidants, rubber vulcanization and vulcanization activators, processing Type rubber additives and special functional additives. [0003] The vulcanization accelerator is called accelerator for short. Substances that promote vulcanization. It can shorten the vulcanization time, lower the vulcanization temperature, reduce the amount of vulcanizing agent and improve the physical and mechanical properties of rubber. [0004] Accelerator DCBS (Chinese name N, N-dicyclohexyl-2-benzothiazole sulfenamide) is an aftereffect accelerator, which has good dispersion perfor...

Claims

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
Login to View More

Application Information

Patent Timeline
no application Login to View More
IPC IPC(8): C07D277/80
CPCC07D277/80
Inventor 孟庆森
Owner KEMAI CHEM
Who we serve
  • R&D Engineer
  • R&D Manager
  • IP Professional
Why Patsnap Eureka
  • Industry Leading Data Capabilities
  • Powerful AI technology
  • Patent DNA Extraction
Social media
Patsnap Eureka Blog
Learn More
PatSnap group products