Method for continuous neutralization and continuous water separation of polycondensation reaction solution during production of antioxidant TMQ

A polycondensation reaction and production process technology, applied in the field of green and environmentally friendly preparation technology, can solve problems such as affecting product stability, restricting process continuity, TMQ product blackening, etc. The effect of blending

Inactive Publication Date: 2018-04-03
CHINA PETROLEUM & CHEM CORP +1
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0007] (1) The process is semi-continuous. Even if the process enters the DCS system, it is still necessary to manually switch between the reactor and the neutralization tank. The steps include: feeding the polycondensation reaction liquid in the neutralization tank, The preparation and dripping of liquid caustic soda, stirring neutralization, standing still after neutralization and water separation (including TMQ crude product discharge and TMQ waste water discharge), etc., seriously affect production efficiency
[0008] (2) The control of the pH value in the process adopts manual on-site sampling and analysis, which brings a certain amount of tediousness to production management and increases labor costs
[0010] The above three points are cumbersome to operate, which restricts the continuity of the process, increases the labor cost of production, and seriously affects the stability of the product. TMQ products sometimes appear black.

Method used

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  • Method for continuous neutralization and continuous water separation of polycondensation reaction solution during production of antioxidant TMQ

Examples

Experimental program
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Effect test

Embodiment 1

[0035] (1) In the production process of anti-aging agent TMQ, aniline and acetone are condensed and polymerized under acidic conditions to obtain TMQ polycondensation reaction liquid, which is placed in the TMQ polycondensation reaction liquid storage tank for buffer storage;

[0036] (2) Use the distributed control system (DCS system) according to pH=7, control the flow meter and the regulating valve to initially mix the TMQ polycondensation reaction liquid and the liquid caustic soda (sodium hydroxide solution), and then import it into a set of static mixers for mixing. to obtain a mixed solution;

[0037] (3) After the mixed solution comes out of the static mixer, the online pH meter shows pH = 8, and the water is continuously divided through the primary water separator. The oil phase on the water separator overflows continuously to collect TMQ crude product, and the bottom water phase is continuous. Collect TMQ waste water. After testing, the pH of the anti-aging agent TM...

Embodiment 2

[0040] (1) In the production process of anti-aging agent TMQ such as "two-step method" or "one-step method", aniline and mesityl oxide are condensed and polymerized under acidic conditions to obtain the polycondensation reaction liquid of TMQ, which is placed in a storage tank, buffer storage;

[0041] (2) Use the distributed control system (DCS system) to preliminarily mix the TMQ polycondensation reaction liquid and liquid caustic soda (mixed solution of 10% sodium hydrogen phosphate and 25% sodium hydroxide) according to pH=8, control the flow meter and the regulating valve Then import four sets of static mixer groups to mix to obtain a mixed solution;

[0042] (3) Due to the polycondensation process in the previous production process of TMQ, the concentration of hydrochloric acid in the polycondensation reaction solution is too high. After the mixed solution comes out of the static mixer, the online pH meter shows pH = 6, and the DCS automatically adjusts the parameters th...

Embodiment 3

[0044] (1) In the production process of anti-aging agent TMQ such as "two-step method" or "one-step method", aniline and acetone are condensed and polymerized under acidic conditions to obtain the polycondensation reaction solution of TMQ, which is placed in a storage tank for buffer storage;

[0045] (2) Using the distributed control system (DCS system) according to pH=8, control the flow meter and the regulating valve to initially mix the TMQ polycondensation reaction solution and the liquid caustic soda (sodium bicarbonate solution) and then import it into four sets of static mixers for mixing , to obtain a mixed solution;

[0046] (3) Due to the polycondensation process in the previous production process of TMQ, the concentration of hydrochloric acid in the polycondensation reaction solution is too low. After the mixed solution comes out of the static mixer, the online pH meter shows pH = 12, and the DCS automatically adjusts the parameters through the set ratio to reduce ...

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Abstract

The invention belongs to the technical field of fine chemicals, and is a continuous treatment method for neutralization and water separation of a polycondensation reaction solution during production of antioxidant TMQ, wherein the method can improve the stability and improve the efficiency and effect of neutralization and water separation. The method utilizes combination of a static mixer and a water separator to achieve continuous neutralization and continuous water separation during production of TMQ, continuously obtains a TMQ crude product and TMQ wastewater, replaces intermittent kettle reaction operation, realizes automatic operation of neutralization and water separation during TMQ production, can greatly reduce labor intensity and save labor cost, and improve the stability of the antioxidant TMQ production process.

Description

technical field [0001] The invention belongs to the technical field of fine chemicals, relates to a treatment method for continuous neutralization and continuous water separation of TMQ polycondensation reaction liquid in the production process of anti-aging agent TMQ, and is a green and environment-friendly preparation process. Background technique [0002] Antiaging agent TMQ is the two, three, and tetrapolymers of 2,2,4-trimethyl-1,2-dihydroquinoline, also known as antiaging agent RD. It is a ketamine antiaging agent, which is light yellow to Xubo color granules or flakes are mainly used as rubber anti-aging agent, and it is one of the most demanded rubber anti-aging agent products in the domestic and foreign markets. [0003] The synthesis of anti-aging agent TMQ is to generate 2,2,4-trimethyl-1,2-dihydroquinoline monomer through condensation reaction with aniline and acetone (or its derivatives) under the action of acid catalyst, and then obtain Under the action of an ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D215/06
CPCC07D215/06
Inventor 韦志强付春黄伟孙阿沁黄天慧
Owner CHINA PETROLEUM & CHEM CORP
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