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Vulcanizing accelerator MBT and preparation method thereof

A vulcanization accelerator and catalyst technology, applied in the field of rubber additives, can solve problems such as high safety risk, high equipment investment, and product quality impact, and achieve the effects of stable process parameters, improved purification effect, and reduced process risk

Inactive Publication Date: 2019-01-18
KEMAI CHEM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] To sum up, the main problems currently plaguing MBT production enterprises are mainly centered on the following three points: First, batch reactors are used for batch production, which requires high equipment investment under high temperature and high pressure conditions, difficulty in industrialization, and high safety risks in the production process; The 2nd, there are too many by-products in the MBT synthetic process, and the product yield is on the low side (industrialization average yield is only about 90%), and though adopting catalyzer can improve yield, catalyzer can't reclaim, and also can produce certain to the quality of product The third is that the product requires a refining process, and the waste liquid or waste resin obtained from the refining process is difficult to handle, which greatly increases the cost of the enterprise and the environmental risk

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0022] A new synthetic method of sulfur accelerator MBT. The method includes using aniline, carbon disulfide and sulfur as raw materials, using DNW type temperature-resistant strong acid cation exchange resin as a catalyst, and catalyzing the synthesis of the promoter MBT.

[0023] First, mix the raw material sulfur and carbon disulfide, stir and prepare the sulfur carbon disulfide solution, and control the mass ratio of sulfur and carbon disulfide to 1:2.6;

[0024] Secondly, the carbon disulfide solution of aniline and prepared sulfur is pumped into the fixed bed reactor at a mass ratio of 1:1.7, and the feed mass space velocity is controlled to 0.4h -1 , Carry out continuous feeding; control the temperature during the reaction to be 190-200°C, and the reaction pressure to be 7.5-8.0Mpa.

[0025] The product flowing out of the reactor enters the toluene solution for extraction, the crude MBT obtained by suction filtration is washed twice with toluene, and the finished product MBT i...

Embodiment 2

[0028] A new synthetic method of sulfur accelerator MBT. The method includes using aniline, carbon disulfide and sulfur as raw materials, using DNW type temperature-resistant strong acid cation exchange resin as a catalyst, and catalyzing the synthesis of the promoter MBT.

[0029] First, mix the raw material sulfur and carbon disulfide, stir and prepare the sulfur carbon disulfide solution, and control the mass ratio of sulfur and carbon disulfide to 1:2;

[0030] Secondly, the carbon disulfide solution of aniline and the configured sulfur is pumped into the fixed bed reactor according to the mass ratio of 1:2, and the feed mass space velocity is controlled to 1h -1 , Carry out continuous feeding; control the temperature during the reaction to be 190-200°C, and the reaction pressure to be 8.0-8.5Mpa.

[0031] The product flowing out of the reactor enters the toluene solution for extraction, the crude MBT obtained by suction filtration is washed twice with toluene, and the finished p...

Embodiment 3

[0034] A new synthetic method of sulfur accelerator MBT. The method includes using aniline, carbon disulfide and sulfur as raw materials, using DNW type temperature-resistant strong acid cation exchange resin as a catalyst, and catalyzing the synthesis of the promoter MBT.

[0035] First, mix the raw material sulfur and carbon disulfide, stir and prepare the sulfur carbon disulfide solution, and control the mass ratio of sulfur and carbon disulfide to 1:2.6;

[0036] Secondly, the carbon disulfide solution of aniline and prepared sulfur is pumped into the fixed bed reactor at a mass ratio of 1:1.2, and the feed mass space velocity is controlled to 0.11h -1 , Carry out continuous feeding; control the temperature during the reaction to be 190-200°C, and the reaction pressure to be 8.0-8.5Mpa.

[0037] The product flowing out of the reactor enters the toluene solution for extraction, the crude MBT obtained by suction filtration is washed twice with toluene, and the finished product MBT ...

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PUM

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Abstract

The invention belongs to the field of rubber aids, and particularly relates to a vulcanizing accelerator MBT and a preparation method thereof. The preparation method adopts phenylamine, sulfur and carbon disulfide as raw materials to prepare the vulcanizing accelerator MBT under the action of a catalyst and under the conditions of 150 to 240 DEG C and 5 to 15 MPa. The preparation method comprisesthe following steps: mixing raw materials sulfur and carbon disulfide, stirring, preparing a carbon disulfide solution of sulfur, controlling a mass ratio of sulfur to carbon disulfide at 1: (0.7 to 4.8); and then pumping the raw material phenylamine and the prepared carbon disulfide solution of sulfur into a reactor according to a mass ratio of 1: (1.0 to 6.0), and controlling a feeding air rateat 0.08 to 3h<-1>. By adopting the non-homogenous catalyst, the synthetic condition of the MBT can be milder, and the product yield is increased compared with a catalyst-free direct synthesis method and is basically equivalent to the catalytic effect using organic strong acid such as salicylic acid.

Description

Technical field [0001] The invention belongs to the field of rubber additives, and specifically relates to a vulcanization accelerator MBT and a preparation method thereof. Background technique [0002] In the 1920s, BedFord CW et al. discovered that MBT (2-mercaptobenzothiazole) can be used as a vulcanization accelerator in rubber processing, namely accelerator MBT, which is a milestone in the history of accelerator development. The accelerator MBT is not only an important vulcanization accelerator in the rubber industry, but also the parent material of most sulfenamide accelerators, and an indispensable intermediate for the production of thiazole vulcanization accelerators. After further synthesis and processing, it can produce accelerators DM, CBS, DCBS, TBBS and other accelerators, whose output occupies the first place among various rubber additives, are the "leading products" in the vulcanization accelerator industry. In addition, the promoter MBT can also be used as a mine...

Claims

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Application Information

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IPC IPC(8): C07D277/72
CPCC07D277/72
Inventor 孟庆森孟庆宝
Owner KEMAI CHEM
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