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A kind of preparation method of di-(3,5,5-trimethylhexanoyl) peroxide

A technology of trimethylhexanoyl and bis-peroxide, which is applied in the field of preparation of bis-peroxide, can solve the problems of time-consuming, side reactions, reduction in the occurrence rate of side reactions, etc., and achieves simplified process flow and reduced water phase The effect of shortening the content and reaction cycle

Active Publication Date: 2022-02-25
鄂尔多斯市瀚博科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

This preparation method simplifies the technological process, overcomes the complex requirements for the reaction equipment, enables the reaction to be carried out in a mild and safe environment, greatly improves the product content and yield, and the yield is as high as 96%. Increase the space, while the incidence of side reactions still needs to be reduced
[0006] In view of this, aiming at problems such as time-consuming and side reactions in the prior art, the present invention provides a high-efficiency preparation method of di-(3,5,5-trimethylhexanoyl) peroxide, by introducing synergistic Retaining the advantages of simple operation and high conversion rate, while greatly shortening the reaction time, reducing the incidence of side reactions, and solving the shortcomings of the existing technology

Method used

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  • A kind of preparation method of di-(3,5,5-trimethylhexanoyl) peroxide
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Examples

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Embodiment 1

[0048] A high-efficiency preparation method of di-(3,5,5-trimethylhexanoyl) peroxide, comprising the steps of:

[0049] (1) According to the mass ratio of 1:0.002, add polyethylene glycol 200 dropwise to 12.5% ​​sodium hydroxide lye, dropwise for 5 minutes, and stir for 15 minutes to obtain a reaction solution;

[0050] (2) According to the mass ratio of 1:0.25, add 27.5% hydrogen peroxide solution dropwise to the reaction solution obtained in step (1), dropwise for 15 minutes, temperature 2°C, stir and react for 30 minutes to obtain solution 1;

[0051] (3) According to the mass ratio of 1:0.25, add 99% isononanoyl chloride dropwise to the solution 1 obtained in step (2), dropwise time 45min, reaction temperature 5°C, stir for 75min, let stand for 30min, divide water , to get the crude product;

[0052] (4) washing the crude product obtained in step (3), stirring for 30 minutes, standing for 30 minutes, and separating water to obtain the product;

[0053] The washing soluti...

Embodiment 2

[0055] A high-efficiency preparation method of di-(3,5,5-trimethylhexanoyl) peroxide, comprising the steps of:

[0056] (1) According to the mass ratio of 1:0.001, polyethylene glycol 600 was added dropwise to 12.5% ​​sodium hydroxide lye solution for 5 minutes, and stirred for 15 minutes to obtain a reaction solution;

[0057] (2) According to the mass ratio of 1:0.35, add 27.5% hydrogen peroxide solution dropwise to the reaction solution obtained in step (1), dropwise for 15 minutes, temperature 5°C, stir and react for 30 minutes to obtain solution 1;

[0058] (3) According to the mass ratio of 1:0.35, add 99% isononanoyl chloride dropwise to the solution 1 obtained in step (2), dropwise time 60min, reaction temperature 15°C, stir for 60min, let stand for 30min, divide water , to get the crude product;

[0059] (4) washing the crude product obtained in step (3), stirring for 30 minutes, standing for 30 minutes, and separating water to obtain the product;

[0060] The washi...

Embodiment 3

[0062] A high-efficiency preparation method of di-(3,5,5-trimethylhexanoyl peroxide), comprising the steps of:

[0063] (1) According to the mass ratio of 1:0.006, add polyethylene glycol 400 dropwise to 12.5% ​​sodium hydroxide lye, dropwise for 5 minutes, and stir for 15 minutes to obtain a reaction solution;

[0064] (2) According to the mass ratio of 1:0.3, add 27.5% hydrogen peroxide solution dropwise to the reaction solution obtained in step (1), dropwise for 15 minutes, temperature 3°C, stir and react for 30 minutes to obtain solution 1;

[0065] (3) According to the mass ratio of 1:0.3, add 99% isononanoyl chloride dropwise to the solution 1 obtained in step (2), dropwise time 50min, reaction temperature 10°C, stir for 70min, let stand for 30min, divide water , to get the crude product;

[0066] (4) washing the crude product obtained in step (3), stirring for 30 minutes, standing for 30 minutes, and separating water to obtain the product;

[0067] The washing solutio...

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Abstract

The invention discloses a high-efficiency preparation method of di-(3,5,5-trimethylhexanoyl) peroxide, relates to the technical field of organic peroxide initiators, and comprises the following steps: (1) dripping Add hydrogen peroxide solution and react to obtain solution 1; the reaction solution is a mixed solution of synergist and lye; (2) add isononanoyl chloride dropwise to the solution 1 obtained in step (1), react, leave standstill, and divide water to obtain the crude product; (3) the crude product obtained in step (2) is washed, left to stand, and separated from water to obtain di-(3,5,5-trimethylhexanoyl) peroxide; in the washing The washing solution used is a mixed solution of synergist, pH buffer and deionized water. The present invention improves the mass transfer effect of isononanoyl chloride and aqueous sodium peroxide by introducing a synergist, increases the reaction rate, shortens the reaction time, reduces product decomposition loss, reduces the selectivity of side reactions, and improves the conversion rate of the target product , Improve product purity.

Description

technical field [0001] The invention relates to the technical field of organic peroxide initiators, in particular to a preparation method of di-(3,5,5-trimethylhexanoyl) peroxide. Background technique [0002] PVC resin is a general-purpose resin with large output and excellent comprehensive performance. Its products have excellent mechanical properties, flame retardancy, transparency, chemical resistance, etc., and are widely used in industry, construction, agriculture, daily life, packaging It plays a very important role in balancing the chlorine gas by-product of caustic soda, an important chemical raw material. [0003] Di-(3,5,5-trimethylhexanoyl peroxide) is a low-activity chain initiator used in domestic PVC resin production. It is used in combination with tert-butyl acid, used alone or in combination with other low-activity chain initiators in the production of ultra-low polymerization PVC resin. It has the characteristics of uniform reaction speed, easy control, un...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C407/00C07C409/34
CPCC07C407/00C07C407/003C07C409/34
Inventor 赵长森牛强张强王会昌
Owner 鄂尔多斯市瀚博科技有限公司