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Preparation method of tert-butyl peroxybenzoate

A technology for tert-butyl peroxybenzoate and tert-butanol peroxide is applied in the field of preparation of tert-butyl peroxybenzoate, and can solve the problems of large amount of waste water, low impurity conversion rate, easy decomposition and deterioration, etc.

Inactive Publication Date: 2020-10-27
TIANJIN CHENGJIAN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0007] In the above method, there are many impurities, low conversion rate and large amount of waste water; at the same time, it is easy to decompose and deteriorate during product storage and transportation.

Method used

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  • Preparation method of tert-butyl peroxybenzoate
  • Preparation method of tert-butyl peroxybenzoate
  • Preparation method of tert-butyl peroxybenzoate

Examples

Experimental program
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Embodiment 1

[0027] Embodiment 1: the preparation of tert-butyl peroxybenzoate

[0028] Add 144g of 5% sodium hydroxide (0.18mol) solution into the reaction flask, cool down to 5-10°C, slowly add 21.8g (0.15mol) of 70% tert-butanol peroxide dropwise, and the dropwise addition completes the reaction 1 hour; keep the temperature at 5-10°C and add 21g (0.15mol) benzoyl chloride dropwise, and keep stirring for 1 hour after the dropwise addition; after standing for 0.5 hours, separate the liquid, collect the high-salt wastewater in the lower layer for three-effect evaporation treatment, and the organic The phase was stirred and washed twice with 30ml / time of purified water; then the lower layer product was added with 0.2g of stabilizer and 1g of anhydrous magnesium sulfate, dried and suction filtered to obtain 28.5g of tert-butyl peroxybenzoate with a content of 99.4%. , yield 98.15%.

Embodiment 2

[0029] Embodiment 2: the preparation of tert-butyl peroxybenzoate

[0030] Add 45g of 8% sodium hydroxide (0.09mol) solution into the reaction flask, cool down to 10-15°C, slowly add 11.9g (0.075mol) of 70% tert-butanol peroxide dropwise, and the dropwise addition completes the reaction 1 hour; keep the temperature at 5-10°C and add 10.7g (0.077mol) benzoyl chloride dropwise, and keep stirring for 1 hour after the dropwise addition; after standing for 0.5 hours, separate the liquid, collect the high-salt wastewater in the lower layer for three-effect evaporation treatment, and the upper layer The organic phase is stirred and washed twice with 15ml / time of purified water; then the lower layer product is added with 0.1g of stabilizer and 0.5g of anhydrous magnesium sulfate, dried, and suction filtered to obtain tert-butyl peroxybenzoate with a content of 99.2%. 14.30 g, yield 98.22%.

Embodiment 3

[0031] Embodiment 3: the preparation of tert-butyl peroxybenzoate

[0032] Add 72g of 10% sodium hydroxide (0.18mol) solution into the reaction flask, cool down to 15-20°C, slowly add 23.2g (0.16mol) of 70% tert-butanol peroxide dropwise, and the dropwise addition completes the reaction 1 hour; keep the temperature at 10-15°C and add 24.7g (0.176mol) benzoyl chloride dropwise, and keep stirring for 1 hour after the dropwise addition; after standing for 0.5 hours, separate the liquid, collect the high-salt wastewater in the lower layer for three-effect evaporation treatment, and the upper layer The organic phase was stirred and washed twice with 30ml / time of purified water, and the lower layer product was added with 0.2g of stabilizer and 1g of anhydrous magnesium sulfate, dried, and suction filtered to obtain tert-butyl peroxybenzoate 30.4 with a content of 99.08%. g, yield 98.3%.

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Abstract

The invention discloses a preparation method of tert-butyl peroxybenzoate, specifically comprising the following steps of: salifying tert-butyl hydroperoxide and caustic soda liquid; then dropwise adding benzoyl chloride into sodium tert-butoxide peroxide for coupling, and washing a coupling product twice after liquid separation; and adding a stabilizer into the product, drying, dewatering and carrying out suction filtration to obtain the tert-butyl peroxybenzoate product. The preparation method comprises the following steps of: dropwise adding benzoyl chloride into sodium tert-butoxide peroxide; and after liquid separation, washing with water twice, adding a stabilizer into the upper product phase, adding anhydrous magnesium sulfate for drying, and carrying out suction filtration to obtain tert-butyl peroxybenzoate with the yield of not less than 95% and the content of not less than 99%, so that the product can be stored in a dark place and transported for a long distance.

Description

technical field [0001] The invention relates to a preparation method of tert-butyl peroxybenzoate, which belongs to the field of organic chemistry. Background technique [0002] Tert-butyl peroxybenzoate is an important chemical raw material. Tert-butyl peroxybenzoate is widely used in the polymerization process of ethylene, styrene, propylene, vinyl acetate, diallyl phthalate and isobutylene. as an initiator. In the curing process of unsaturated polyester, it is widely used in molding processes such as SMC, BMC, DMC, etc. At the same time, it can also be used in two-component curing systems with higher activity such as MEPK, BPO or TBPO. . [0003] US 2567615 discloses the preparation of peroxyesters by reacting acid chlorides or carboxylic anhydrides with tertiary alkyl hydroperoxides in the presence of alkali metal hydroxides, when using a concentration of 10% sodium carbonate and washing the organic phase obtained in the reaction with water , to obtain a product compr...

Claims

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Application Information

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IPC IPC(8): C07C407/00C07C409/24
CPCC07C407/00C07C409/24
Inventor 谷迎春李滢费学宁李征
Owner TIANJIN CHENGJIAN UNIV
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