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Method for preparing 3,4-dichlorobenzoperoxide

A technology of dichlorobenzoyl peroxide and dichlorobenzoyl chloride, which is applied in 3 fields, can solve problems such as low decomposition temperature and increased unsafe factors, achieve high decomposition temperature, use equipment and process requirements that are not harsh, and have high purity high effect

Active Publication Date: 2010-06-16
江苏强盛功能化学股份有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the thermal decomposition temperature of Shuang24 is only 60°C, and the decomposition temperature is low, which increases the unsafe factors in the process of production, storage, transportation and use.

Method used

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  • Method for preparing 3,4-dichlorobenzoperoxide
  • Method for preparing 3,4-dichlorobenzoperoxide
  • Method for preparing 3,4-dichlorobenzoperoxide

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0015] Put 8.362mol of sodium hydroxide solution, 5.537mol of hydrogen peroxide, 3000g of water, 96g of sodium dodecylsulfonate, and 960g of toluene into the reaction kettle, stir, adjust the temperature to 0°C, and dropwise add industrial grade 3,4-dichlorobenzene Formyl chloride 5.65mol (1200g), the dropping temperature is maintained at 0-5°C, the dropping time is 15min, and after the dropwise addition is completed, the reaction is kept at 35°C for 200min to obtain the reactant, which is filtered and washed to obtain 3,4- The wet product of benzoyl dichloroperoxide (wet product), the wet product was dried in a desiccator at 35°C for 5h to obtain 1989.6g of a light yellow solid, with a yield of 92.7%, and a liquid chromatography area normalized purity of 98.6%, decomposed The temperature is 131.6°C.

Embodiment 2

[0017] Put 9.605mol of sodium hydroxide solution, 7.062mol of hydrogen peroxide, 3600g of water, 180g of sodium dodecylbenzenesulfonate, and 1440g of hexane into the reaction kettle, stir, adjust the temperature to 12°C, and dropwise add industrial grade 3,4-di Chlorobenzoyl chloride 5.65mol (1200g), the dropping temperature is maintained at 10-15°C, the dropping time is 55min, and after the dropwise addition is completed, the reaction is kept at 15°C for 110min to obtain the reactant, which is filtered and washed to obtain 3,4 -Dichlorobenzoyl peroxide wet product, dry the wet product in a desiccator at 40°C for 5h, obtain 2024.5g of light yellow solid, yield 94.3%, liquid chromatography area normalized purity 98.9%, decomposition temperature 131.9°C .

Embodiment 3

[0019] Put 10.735mol of sodium hydroxide solution, 6.215mol of hydrogen peroxide, 5040g of water, 204g of sodium lauryl sulfate, and 3000g of dichloroethane into the reaction kettle, stir, adjust the temperature to 20°C, and dropwise add industrial grade 3,4-dichloroethane Chlorobenzoyl chloride 5.65mol (1200g), the dropping temperature was maintained at 20-24°C, the dropping time was 92min, and after the dropwise addition was completed, the reaction was kept at 28°C for 42min to obtain the reactant, which was filtered and washed to obtain 3,4 - Dichlorobenzoyl peroxide wet product, dry the wet product in a desiccator below 38°C for 5 hours to obtain 2011.0 g of light yellow solid, yield 93.6%, liquid chromatography area normalized purity 99.1%, decomposition temperature 131.9 ℃.

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Abstract

A preparation process of 3, 4-dichlorobenzoyl peroxide belongs to the organic peroxide preparation technology field, which comprises firstly putting caustic soda solution, hydrogen dioxide solution, water surface activator and solvent into a reaction device to stirring, regulating temperature, adding 3, 4-dichloro benzoyl chloride, insulating to obtain reactant, then filtering reactant to obtain filter cake, finally scouring and drying filter cake to obtain 3, 4-dichlorobenzoyl peroxide. The invention has short preparation technology steps, wider range of usage device and technology, high decomposition temperature (131 DEG C), safer production, storage, transport and usage, which can obtain high purity 3, 4-dichlorobenzoyl peroxide (>=98%), and can guarantee the rubber which is vulcanizeddoes not peculiar smell, has excellent transparency and high rubber strength.

Description

technical field [0001] The invention belongs to the technical field of preparation of organic peroxides, and in particular relates to a preparation method of 3,4-dichlorobenzoyl peroxide. Background technique [0002] The English name of 3,4-dichlorobenzoyl peroxide is: 3,4-dichloro benzoyl peroxide. Its molecular formula is: C 14 h 6 Cl 4 o 4 ; Molecular weight: 380.10; Structural formula: [0003] [0004] 3,4-Dichlorobenzoyl peroxide, abbreviated as DSQ, is a diacyl organic peroxide, a free radical donor, used as a polymer chemical additive, and also used as a vulcanizing agent for silicone rubber. Diacyl organic peroxides commonly used at present include 2,4-dichlorobenzoyl peroxide (abbreviated as bis-2-4), dibenzoyl peroxide (BPO), etc., wherein bis-2-4 is an excellent extruded Silicone rubber vulcanizing agent is produced, the product has high strength, good transparency, low service temperature and fast vulcanization speed. However, the thermal decompositio...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C409/34C07C407/00
Inventor 应立陈国华应志耀
Owner 江苏强盛功能化学股份有限公司
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