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Method for continuously producing vulcanization accelerator TBBS by taking liquid chlorine as oxidizing agent

A vulcanization accelerator and accelerator technology, applied in the field of rubber, can solve the problems of large loss in raw material purification process, poor storage safety of oxidant, high process risk, etc., and achieve the effects of controlling wastewater output, fast reaction speed, and avoiding large consumption

Pending Publication Date: 2019-08-09
KEMAI CHEM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0014] In view of the deficiencies in the prior art, the purpose of the present invention is to provide a method for continuously producing vulcanization accelerator TBBS using liquid chlorine as an oxidant, which overcomes the large loss and process risk in the raw material purification process when commercial MBT is used as raw material. At the same time, it avoids the problem of poor storage safety and high risk of explosion when sodium hypochlorite is used as the oxidant. The TBBS oxidation synthesis process produces a large amount of wastewater and low value-added sodium chloride, and the problem of high COD value in wastewater

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0067] The present embodiment provides a method for continuously producing the vulcanization accelerator TBBS with liquid chlorine as an oxidant, the method comprising the steps of:

[0068] (1) At 40°C, mix crude MBT and toluene with a mass ratio of 1:4.5 under stirring for 0.6h, then add a 12wt% NaOH solution at 40°C under stirring and continue mixing for 0.4h , the mass ratio of the crude product MBT and NaOH solution is 1:5, after standing for 1.5h, the phases are separated, the lower water phase is the salt solution of accelerator MBT, the upper organic phase is an organic solvent, and the upper organic phase is used as an organic solvent after separation for oxidation reactions;

[0069] (2) Pass the organic solvent and liquid chlorine obtained during the preparation of the salt solution of the accelerator MBT, tert-butylamine, and the salt solution of the accelerator MBT into the microchannel reactor, and carry out the oxidation reaction at 30 ° C to control the residen...

Embodiment 2

[0073] The present embodiment provides a method for continuously producing the vulcanization accelerator TBBS with liquid chlorine as an oxidant, the method comprising the steps of:

[0074] (1) At 45°C, mix the crude MBT with a mass ratio of 1:4 and the mixed solvent of toluene / ethyl acetate for 1h under stirring, and then add NaOH with a concentration of 20wt% at 45°C under stirring solution and continue to mix for 0.2h, the mass ratio of the crude product MBT and NaOH solution is 1:2, after standing for 1h, the phases are separated, the lower aqueous phase is the salt solution of the promotor MBT, the upper organic phase is an organic solvent, and the upper layer after separation The organic phase is used as an organic solvent for the oxidation reaction;

[0075] (2) The organic solution that separates when the saline solution of promotor MBT, t-butylamine, promotor MBT saline solution is configured and liquid chlorine are passed in the microchannel reactor, carry out oxida...

Embodiment 3

[0079] The present embodiment provides a method for continuously producing the vulcanization accelerator TBBS with liquid chlorine as an oxidant, the method comprising the steps of:

[0080] (1) At 20°C, mix the crude MBT with a mass ratio of 1:2.5 and the mixed solvent of ethyl acetate / isopropanol under stirring conditions for 0.8h, and then add a concentration of 5wt at 20°C under stirring conditions % NaOH solution and continue to mix for 1h, the mass ratio of the crude product MBT and NaOH solution is 1:9.6, after standing for 1h, the phase separation, the lower floor water phase is the salt solution of promotor MBT, and the upper organic phase is an organic solvent, separated Back upper organic phase is used for oxidation reaction as organic solvent;

[0081] (2) Pass the organic solvent and liquid chlorine that are separated when the salt solution of the accelerator MBT, tert-butylamine, and the salt solution of the accelerator MBT are configured into the microchannel re...

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Abstract

The method provides a method for continuously producing vulcanization accelerator TBBS by taking liquid chlorine as an oxidizing agent. The method comprises the following steps that a saline solutionof an accelerator MBT, tert-butylamine, an organic solvent and the liquid chlorine are introduced into reactors for an oxidation reaction, and a reaction product is post-treated to obtain a TBBS product; the reactors comprise a tubular reactor and / or a micro-channel reactor. The method for continuously producing the vulcanization accelerator MBT by taking the liquid chlorine as the oxidizing agenthas the advantages that the accelerator TBBS can be synthesized directly by taking crude MBT as a raw material, and the liquid chlorine is taken as the oxidizing agent for in-situ oxidation, which not only can avoid problem of large consumption of raw material lye and chlorine gas caused in the sodium hypochlorite production process, but also can effectively control the wastewater yield in the TBBS production process, and can greatly improve the overall benefit of the method, and the yield of the TBBS reaches up to 99.7%, so that the method has the advantage of industrial promotion.

Description

technical field [0001] The invention belongs to the technical field of rubber and relates to a method for producing a vulcanization accelerator TBBS, in particular to a method for continuously producing the vulcanization accelerator TBBS by using liquid chlorine as an oxidant. 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, rubber anti-aging agents, rubber vulcanization and vulcanization activators, processing rubber additives and Special functional additives. Among them, the rubber vulcanization accelerator is referred to as an accelerator, which is a substance that promotes vulcanization, which can shorten the vulcanization time, lower the vulcanization temperature, reduce the amount of vulcanization agent and improve the physical and mechanical properties of rubber. [0003] The rubber vulcanization acce...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D277/80
CPCC07D277/80
Inventor 孟庆森陈群陈海群朱军周维友张杰刘国卿窦东坡何明阳
Owner KEMAI CHEM