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Preparation method of high-purity benzoyl peroxide

A technology for the purity of benzoyl peroxide and benzoyl chloride, which is applied in the field of preparation of benzoyl peroxide, can solve the problems of low product purity, material punching, high production energy consumption, etc., and achieves high reaction safety and crystallization. Large particles, mild response effect

Inactive Publication Date: 2017-01-25
JIANGSU SINOBIOPHARMA
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] Most of the existing industrial production uses sodium hydroxide as the alkali, which is strong in alkalinity, and the reaction temperature needs to be controlled at -10-0°C. The production energy consumption is large, the reaction is not easy to control, and impurities are easily produced, and the product purity is not high; or carbonic acid is used. Sodium is used as alkali, it is easy to produce a large number of bubbles, and there is a risk of flushing; adding a surfactant for catalysis, such as sodium dodecyl sulfonate, the reaction will produce a large amount of foam, there may be overflow, and it is difficult to control

Method used

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  • Preparation method of high-purity benzoyl peroxide

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Embodiment 1

[0027] A preparation method of high-purity benzoyl peroxide, the preparation of high-purity benzoyl peroxide is completed through a synthesis process and a purification process; the specific steps are as follows:

[0028] (1) Synthesis process:

[0029] a. Add 15kg of 30% hydrogen peroxide into a 50L reactor, start stirring, then add 9.3kg of ammonium bicarbonate, slowly add 15kg of benzoyl chloride dropwise, the temperature in the reactor is 20 degrees Celsius, and the reaction time is 2.5 hours;

[0030] b. filter the reaction solution after the reaction, filter to obtain a filter cake, filter the cake in a mixed solvent of 15kg ethanol and 15kg of clear water and wash for 20 minutes, filter;

[0031] c. After beating and washing with 30kg of clear water for 10 minutes, repeat the beating and washing for 3 times;

[0032] d. Finally, rinse with 30kg of clear water, filter and dry to obtain 15.79kg of white benzoyl peroxide crude product;

[0033] (2) Purification process: ...

Embodiment 2

[0039] A preparation method of high-purity benzoyl peroxide, the preparation of high-purity benzoyl peroxide is completed through a synthesis process and a purification process; the specific steps are as follows:

[0040] (1) Synthesis process:

[0041] a. Add 22kg of 30% hydrogen peroxide into a 50L reactor, start stirring, then add 13.5kg of ammonium bicarbonate, slowly add 15kg of benzoyl chloride dropwise, the temperature in the reactor is 30 degrees Celsius, and the reaction time is 3.5 hours;

[0042] b. filter the reaction solution after the reaction, filter to obtain a filter cake, filter the cake in a mixed solvent of 30kg ethanol and 30kg of clear water and wash for 40 minutes, filter;

[0043] c. After beating and washing with 45kg of clear water for 20 minutes, repeat the beating and washing for 3 times;

[0044] d. finally rinse with 45kg of clear water, filter and dry, and obtain the white benzoyl peroxide crude product;

[0045] (2) Purification process:

[0...

Embodiment 3

[0051] A preparation method of high-purity benzoyl peroxide, the preparation of high-purity benzoyl peroxide is completed through a synthesis process and a purification process; the specific steps are as follows:

[0052] (1) Synthesis process:

[0053] a. Add 18kg of 30% hydrogen peroxide into a 50L reactor, start stirring, then add 10.2kg of ammonium bicarbonate, slowly add 15kg of benzoyl chloride dropwise, the temperature in the reactor is 25 degrees Celsius, and the reaction time is 3 hours;

[0054] b. filter the reaction solution after the reaction, filter to obtain a filter cake, and filter the filter cake in a mixed solvent of 22.5kg ethanol and 22.5kg of clear water for beating and washing for 30 minutes, and filter;

[0055] c. After beating and washing with 37.5kg of clear water for 15 minutes, repeat the beating and washing for 3 times;

[0056] d. finally rinse with 37.5kg of clear water, filter and dry to obtain 15.82kg of white benzoyl peroxide crude product; ...

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Abstract

The invention discloses a preparation method of high-purity benzoyl peroxide. The high-purity benzoyl peroxide is prepared through a synthesis process and a purification process. Alkali selected in the synthesis process is ammonium hydrogen carbonate, so that reaction safety is high, overall reaction is mild and control, and product purity can reach 99.5% and higher. A solvent selected in the purification process is safe and has lower toxicity than chloroform and methanol, operation is easy, and obtained crystal particles are large.

Description

technical field [0001] The invention relates to a preparation method of benzoyl peroxide, in particular to a preparation method of high-purity benzoyl peroxide. Background technique [0002] Benzoyl peroxide is also known as dibenzoyl peroxide, and its English name is: Dibenzoyl peroxide (BPO for short). Its molecular formula is: C14H10O4; molecular weight: 242.22; structural formula is: [0003] [0004] BPO is a widely used diacyl organic peroxide, which is white granular and has a slight smell of bitter almonds. It is a strong oxidizing agent. It is mainly used as a polymerization initiator for vinyl monomers and a curing agent for unsaturated resins. It can also be used as a cross-linking agent for silicone rubber and fluororubber, and an anti-oxidation and anti-corrosion additive in the feed industry. In addition, it can also be used as a bleaching agent and oxidizing agent for refining oil, whitening flour, decolorizing fiber, etc. Moreover, in the pharmaceutical...

Claims

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Application Information

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IPC IPC(8): C07C407/00C07C409/34
CPCC07C407/003C07C409/34
Inventor 黄乐群陈权
Owner JIANGSU SINOBIOPHARMA
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