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Process for preparing diphenyl sulphone formyl paraquinone dioxime

A technology for dibenzoyl-p-quinone dioxime and p-benzoyl-quinone dioxime is applied in the field of catalytic synthesis of dibenzoyl-p-quinone dioxime, which can solve the problems of serious pollution, non-compliance with greening, and high treatment cost, and can achieve raw material High utilization effect

Inactive Publication Date: 2012-05-09
EAST CHINA NORMAL UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[Refer to: Li Gang's "Synthetic Auxiliary Cleaner Production Process" Chemical Industry Press, August 2004, first edition] This method is due to the water reaction system used, the pollution is relatively serious, the treatment cost is high, and it does not meet the concept of greening

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0011] In the first step, put 2.0g of p-benzoquinone dioxime into the reactor, add 50ml of chloroform, stir evenly, and raise the temperature to 55°C, stir at constant temperature for 30min; then add 4.3g of benzoyl chloride dropwise to the reaction system within 10min In, reaction 4h.

[0012] In the second step, the reaction system is cooled to room temperature, then quickly filtered with suction, the filtrate is recovered into the reactor, the filtered solid is washed three times with 15ml of chloroform, and then recrystallized with chloroform to obtain the product dibenzoyl-p-quinonedioxime , all the chloroform consumed in this process is recycled to the reactor. The yield (calculated as p-benzoquinonedioxime) was 73.2%.

[0013] The recovery experiment was performed on the recovered solvent according to the above ratio, and the yield was 74.1%.

Embodiment 2

[0015] In the first step, put 2.0g of p-benzoquinone dioxime into the reactor, add 50ml of chloroform, stir evenly, and raise the temperature to 55°C, stir at constant temperature for 30min; then add 4.7g of benzoyl chloride dropwise to the reaction system within 10min In, reaction 4h.

[0016] In the second step, the reaction system is cooled to room temperature, then quickly filtered with suction, the filtrate is recovered into the reactor, the filtered solid is washed three times with 15ml of chloroform, and then recrystallized with chloroform to obtain the product dibenzoyl-p-quinonedioxime , all the chloroform consumed in this process is recycled to the reactor. The yield (calculated as p-benzoquinone dioxime) was 85.7%.

[0017] The recovery experiment was performed on the recovered solvent according to the above ratio, and the yield was 88.1%.

Embodiment 3

[0019] In the first step, put 2.0g of p-benzoquinone dioxime in the reactor, add 50ml of chloroform, stir evenly, and raise the temperature to 55°C, stir at constant temperature for 30min; then add 5.5g of benzoyl chloride dropwise to the reaction system within 10min In, react 3h.

[0020] In the second step, the reaction system is cooled to room temperature, then quickly filtered with suction, the filtrate is recovered into the reactor, the filtered solid is washed three times with 15ml of chloroform, and then recrystallized with chloroform to obtain the product dibenzoyl-p-quinonedioxime , all the chloroform consumed in this process is recycled to the reactor. The yield (calculated as p-benzoquinonedioxime) was 70.2%.

[0021] The recovery experiment was performed on the recovered solvent according to the above ratio, and the yield was 72.2%.

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PUM

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Abstract

The invention discloses a method for preparing dibenzoyl-p-quinonedioxime, particularly to a method for one-step synthesis of dibenzoyl-p-quinonedioxime from p-benzoquinone dioxime and benzoyl chloride in chloroform, belonging to the technology field of organic synthesis. The method has the advantages of high yield of dibenzoyl-p-quinonedioxime, mild reaction conditions, chloroform as solvent, complete solvent recycling, reduced production cost, and environmental friendliness.

Description

technical field [0001] The invention relates to a method for catalytically synthesizing dibenzoyl-p-quinone dioxime. To be precise, the method for synthesizing dibenzoyl-p-quinone dioxime with chloroform as a solvent and p-benzoyl quinone dioxime and benzoyl chloride as raw materials The method belongs to the technical field of organic synthesis. Background technique [0002] Dibenzoyl quinone dioxime is a rubber vulcanizing agent for natural rubber, butyl and styrene-butadiene synthetic rubber. The use is similar to p-quinonedioxime, but because of the benzoyl group in the structure, it has stronger vulcanization delay than p-quinonedioxime, and is not easy to scorch. Also used as an accelerator for oxide vulcanizing agents. [Refer to: Shanxi Chemical Research Institute "Plastic and Rubber Processing Auxiliaries" First Edition Page351-Page353, May 1983] It is especially suitable for butyl rubber, which is used to make inner tubes, water tires, vulcanizing bladders, insula...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C251/68C07C251/46C07C249/12
Inventor 单永奎贺峥孟静侯亚伟
Owner EAST CHINA NORMAL UNIV
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