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Process for preparing N,N'-diphenyl sulfourea

A diphenylthiourea, a new type of technology, applied in the field of chemical raw materials, can solve the problems of uneconomical, inconvenient operation, low product yield, etc., and achieve the effects of saving water resources, improving production efficiency, and simple operation

Inactive Publication Date: 2004-05-26
JIANGSU UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The third is to add additives or surfactants, using the "one-pot synthesis method" of additive triethanolamine, although the yield of N,N'-diphenylthiourea has reached 98%, but the large use of expensive additive triethanolamine and water makes The law is not economical
[0003] The method for the synthesis of N,N'-diphenylthiourea reported in the literature has a low product yield, and in order to improve the yield, the reaction generally needs to be heated
Since carbon disulfide is a volatile gas with a boiling point of 46.5°C, heating will inevitably increase its dosage or the reaction needs to be carried out under higher pressure, which will cause inconvenience in operation

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0020] In a 150mL round bottom flask, add 15mL aniline (0.16mol), 6mL carbon disulfide (0.10mol) and 8.2% macroporous sulfonic acid resin solid strong acid catalyst (H type 20-40 mesh) of aniline consumption, the flask and a condensing cooler connected, stirred and refluxed at room temperature and pressure for 2 hours. After the reaction, the product was transferred to a Soxhlet extractor with 100 mL of ethanol for extraction and separation, and the macroporous sulfonic acid resin solid acid catalyst was recovered. After the extract was cooled to room temperature, a large amount of white flaky crystal N, N'-diphenylthiourea was crystallized in the extractor flask, and after vacuum drying at 80°C, 33.8 g of N, N'-diphenylthiourea was obtained by weighing. The yield is 89.9%, the purity measured by high performance liquid chromatography is 99.8%, and the melting point is 153.5-154°C.

Embodiment 2

[0022] In a 150mL round bottom flask, add 10mL aniline (0.11mol), 5mL carbon disulfide (0.08mol) and 9.3% macroporous sulfonic acid resin solid strong acid catalyst (H type 20-40 mesh) of aniline consumption, the flask and a condensing cooler connected, stirred and refluxed at normal temperature and pressure for 2 hours. After the reaction, the product was transferred to a Soxhlet extractor with 100 mL of ethanol for extraction and separation, and the macroporous sulfonic acid resin solid acid catalyst was recovered. After the extract was cooled to room temperature, a large amount of white flaky crystal N, N'-diphenylthiourea was crystallized in the extractor flask, and after vacuum drying at 80°C, 22.5 g of N, N'-diphenylthiourea was obtained by weighing. The yield is 90%, the purity measured by high performance liquid chromatography is 99.7%, and the melting point is 153.5-154°C.

Embodiment 3

[0024] Continuously add 30mL aniline (0.32mol), 10.1% macroporous sulfonic acid resin solid strong acid catalyst (H type 20-40) of 12mL carbon disulfide (0.20mol) and aniline consumption in a round bottom flask in a small single continuous stirring reaction pot order) and 200mL solvent ethanol, under normal temperature and pressure, adopt continuous process stirring reaction for 2 hours. After the reaction is finished, all the products are transferred to a Soxhlet extractor for extraction and separation, and the macroporous sulfonic acid resin solid acid catalyst is recovered. After the extract was cooled to room temperature, a large amount of white flaky crystal N, N'-diphenylthiourea was crystallized in the extractor flask, and after vacuum drying at 80°C, 42.6 g of N, N'-diphenylthiourea was obtained by weighing. The yield is 85.2%, the purity measured by high performance liquid chromatography is 99.6%, and the melting point is 153-154°C.

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Abstract

A process for preparing N,N'-diphenylthiourea is characterized by that the phenylamine, CS2, macroporous sulfonic resin and strong solid acid as catalyst are stirred for reacting at ordinary temp and pressure to obtain said product. It can be used as the intermediate of medicine and dye, thio-promoter of natural latex or chlorobutadiene latex product, thermal stabilizer for preparing polyvinyl chloride, etc.

Description

Technical field [0001] The invention relates to the field of chemical raw materials, in particular to a novel preparation method of N,N'-diphenylthiourea, the product can be used as an intermediate of medicine and dye, a thioaccelerator of natural latex and chloroprene latex products, and a polymer produced by emulsion method. Heat stabilizer for vinyl chloride, metal anti-corrosion and corrosion inhibitor and reagent for analysis and determination of elements such as ruthenium and osmium. Background technique [0002] There are several kinds of N, N'-diphenylthiourea synthesis methods reported in the existing literature. The first is to use sulfur and ammonia as catalysts, and at normal temperature, add 1% sulfur, 1% ammonium bicarbonate or ammonia water are used as catalysts, and the reaction is stirred and sealed. At room temperature, the reaction cycle is very long, about 15 days or more in summer. When the reaction temperature is controlled at about 40°C (close to the ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C335/16
Inventor 袁新华魏贤勇宗志敏
Owner JIANGSU UNIV
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