Study on Synthesis Process of Bis(2,4-dichlorobenzoyl)peroxide |
Received:November 08, 2021 Revised:November 08, 2021 |
DOI:10.12136/j.issn.1000-890X.2023.04.0300 |
Key Words: bis(2,4-dichlorobenzoyl)peroxide;synthesis process;cooling crystallization;dissolution crystallization;yield;purity |
Author Name | Affiliation | E-mail | YU Lei* | Shandong Yanggu Huatai Chemical Co.,Ltd | 18363569583@163.com | LI Qingchao | Shandong Yanggu Huatai Chemical Co.,Ltd | | MA Zhenyu | Shandong Yanggu Huatai Chemical Co.,Ltd | | HUANG Cunying | Shandong Yanggu Huatai Chemical Co.,Ltd | | LI Yuanjie | Shandong Academy of Sciences | | LIU Xilin | Shandong Yanggu Huatai Chemical Co.,Ltd | |
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Abstract: |
The synthesis process of bis(2,4-dichlorobenzoyl)peroxide(DCBP) was studied. The
synthesis reaction was carried out at a certain temperature by using sodium hydroxide,hydrogen peroxide
and 2,4-dichlorobenzoyl chloride as the main raw materials,and using chloroform as the solvent. After the
reaction was completed,high purity powder DCBP could be obtained through the recrystallization process
which included dissolution crystallization and cooling crystallization steps by using methanol as the inert
solvent of the product. The optimum process conditions of DCBP synthesis were as follows:the molar
ratio of sodium hydroxide/hydrogen peroxide/2,4-dichlorobenzoyl chloride was 2. 4/1. 2/2,the reaction
temperature was 5 ~ 10 ℃,the mass ratio of chloroform/2,4-dichlorobenzoyl chloride was 4/1,the mass
ratio of methanol/2,4-dichlorobenzoyl chloride was 2. 5/1,and the cooling crystallization temperature
was - 15 ℃ . Under the optimum process conditions,the yield of DCBP was 85. 83%,the purity reached
99. 78%,and the particle size was less than 50 μm. |
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