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Preparation method of solvent type tert-butyl peroxyneo-caprate (BNP)

A new technology of tert-butyl decanoate and peroxidation, which is applied in the direction of preparation of peroxide compounds, preparation of organic compounds, chemical instruments and methods, etc., can solve the problems affecting the product quality, high toxicity and activity of high polymers such as polyvinyl chloride Low and other problems, to achieve stable product quality and high activity, increase product content and yield, and overcome the effects of low activity

Active Publication Date: 2013-11-06
LINZIZHENGHUA ACCESSORY INGREDIENT ZIBO
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, azo initiators have insurmountable disadvantages such as low activity and high toxicity, which affect the quality of high polymers such as polyvinyl chloride products, and the toxic substances in the production process are seriously harmful to the human body.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0012] Example 1: The preparation steps of solvent-based tert-butyl peroxyneodecanoate (BNP) are as follows:

[0013] (1) In a 500ml flask, add 22.5 grams of sodium hydroxide with a mass content of 90%, 40 grams of water, stir and cool down to 5°C, and make a sodium hydroxide alkaline solution with a concentration of about 32%;

[0014] (2) 28 grams of tert-butyl hydroperoxide with a purity of 70.5% were added dropwise to the solution prepared in step (1), reacted for 30 minutes, and the temperature was controlled at 25° C.;

[0015] (3) After stirring evenly, slowly add 50 grams of neodecanoyl chloride solution with a concentration of 80% in the flask dropwise, the reaction temperature is controlled at 25°C to 30°C, and the addition is completed within 1.5 hours to 2 hours. After adding the neodecanoyl chloride solution Stir the reaction for 60 minutes;

[0016] (4) Stop stirring after the reaction is over, let it stand, separate the reaction mother liquor, and wash the reac...

Embodiment 2

[0019] Example 2: The preparation steps of solvent-based tert-butyl peroxyneodecanoate (BNP) are as follows:

[0020] (1) In a 500ml flask, add 22.5 grams of sodium hydroxide with a mass content of 90%, 40 grams of water, stir and cool down to 5°C, and make a sodium hydroxide alkaline solution with a concentration of about 32%;

[0021] (2) 28 grams of tert-butyl hydroperoxide with a purity of 70.5% were added dropwise to the solution prepared in step (1), reacted for 30 minutes, and the temperature was controlled at 25° C.;

[0022] (3) After stirring evenly, slowly add 50 grams of neodecanoyl chloride solution with a concentration of 80% in the flask dropwise, the reaction temperature is controlled at 25°C to 35°C, and the addition is completed within 1.5 hours to 2 hours. After adding the neodecanoyl chloride solution Stir the reaction for 60 minutes;

[0023] (4) Stop stirring after the reaction is over, let it stand, separate the reaction mother liquor, and wash the reac...

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Abstract

The invention relates to a preparation method of an initiator for synthesizing a high polymer, in particular to a preparation method of solvent type tert-butyl peroxyneo-caprate (BNP). According to the technical scheme of the invention, the preparation method of the solvent type BNP comprises the following steps of: mixing octyl decanoyl chloride with an alkaline solution and tert-butyl hydrogen peroxide, stirring and reacting at the temperature of 10-40 DEG C; separating a mother liquor; and washing a reaction product to the neutral state and adding an alkane solvent to obtain the solvent type BNP. Due to the adoption of the method for preparing the solvent type BNP provided by the invention, the process flow is simplified, the complex requirements on reaction equipment are eliminated, a reaction is undergone in the mild and safe environment, the product content and yield are increased greatly, and the yield can be over 95 percent.

Description

technical field [0001] The invention relates to a preparation method of an initiator for high polymer synthesis, in particular to a preparation method of solvent-based tert-butyl peroxyneodecanoate (BNP). Background technique [0002] With the rapid development of the domestic polymer synthesis industry, the quality and demand of initiators for polymer synthesis have increased rapidly. As we all know, azo initiators, such as azobisisobutyronitrile and azobisisoheptanonitrile (ABVN), have long been used as initiators for the synthesis of high polymers such as polyvinyl chloride. However, azo initiators have insurmountable shortcomings such as low activity and high toxicity, which affect the quality of high polymers such as polyvinyl chloride products, and the toxic substances in the production process are seriously poisonous to the human body. [0003] Solvent-based tert-butyl peroxyneodecanoate (BNP), as a high-efficiency initiator for polymer synthesis, compared with commo...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C409/38C07C407/00
Inventor 侯永正翟少华倪啟化许淑女
Owner LINZIZHENGHUA ACCESSORY INGREDIENT ZIBO
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