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Synthesis method of tetrabutylurea

A synthesis method and technology of tetrabutylurea, applied in the field of fine chemical new material synthesis, can solve the problems of high equipment requirements, large amount of waste gas and low yield, and achieve the effects of low equipment requirements and avoiding three wastes

Inactive Publication Date: 2017-06-13
HUNAN GOFAR FINE CHEM IND TECH CO LDT
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0003] The traditional synthesis of tetrabutylurea mainly has the following methods: (1) Phosgene method: using highly toxic raw material phosgene, and a large amount of hydrogen chloride gas is generated during the production process, the amount of waste gas is large, and hydrogen chloride gas corrodes the equipment (2) Diphosgene and triphosgene methods: A large amount of waste water is generated in the production process, and hydrogen chloride gas is highly corrosive to equipment, which requires high equipment; (3) Carbonate method: Need to use high temperature and high pressure, high energy consumption, low yield; (4) carbonyl catalytic method: need to use metal catalyst, expensive and low yield

Method used

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Examples

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preparation example Construction

[0022] A kind of synthetic method of tetrabutylurea, comprises the following steps:

[0023] S110, dissolving the organic strong base catalyst and dimethyl carbonate in a solvent, and raising the temperature to 30° C. to 50° C. to obtain a mixed solution.

[0024] Wherein, the strong organic base catalyst is sodium methylate, potassium methylate, sodium ethylate, potassium ethylate, potassium tert-butyl alkoxide or sodium tert-butyl alkoxide. Preferably, the above-mentioned strong organic base catalyst is sodium methylate.

[0025] The solvent is chloroform, xylene, chlorobenzene, dimethylformamide, methanol or ethanol.

[0026] Since the by-product of the synthesis method of tetrabutylurea in the present application is methanol, the above-mentioned solvent is preferably methanol, which avoids the separation of follow-up products, by-products and solvents, and reduces production costs.

[0027] S120. Add di-n-butylamine dropwise to the above mixed solution at 50° C. to 80° C...

Embodiment 1

[0040] 2.14 g of sodium methoxide and 97 g of dimethyl carbonate were dissolved in 150 g of methanol, and the temperature was raised to 30° C. to obtain a mixed solution. Add 42.4 g of di-n-butylamine dropwise to the above mixture at 50° C. to 60° C. After the dropwise addition, the temperature is raised to reflux, and the mixture is kept for 5 hours to obtain a reaction liquid. Distill the reaction liquid under atmospheric pressure, collect 242g of condensate at 80°C~90°C (the mass content of methanol in the condensate is 66.6%, and the mass content of dimethyl carbonate is 33.4%), and the remaining liquid is rectified under reduced pressure. Collect 42.4g of condensate at 156°C~160°C, which is tetrabutylurea product.

[0041] After calculation, the mass content of tetrabutylurea in the tetrabutylurea product is 99.18%, and the yield is 90.9%.

Embodiment 2

[0043] 2 g of sodium methoxide and 97 g of dimethyl carbonate were dissolved in 150 g of methanol, and the temperature was raised to 50° C. to obtain a mixed solution. Add 42.4 g of di-n-butylamine dropwise to the above mixture at 50° C. to 60° C. After the dropwise addition, the temperature is raised to reflux, and the mixture is kept for 8 hours to obtain a reaction liquid. Distill the reaction liquid under atmospheric pressure, collect 238.4g of condensate at 80°C~90°C (the mass content of methanol in the condensate is 68.5%, and the mass content of dimethyl carbonate is 31.5%), and the remaining liquid is rectified under reduced pressure , Collect 35.1g of condensate at 156°C~160°C, which is tetrabutylurea product.

[0044] After calculation, the mass content of tetrabutylurea in the tetrabutylurea product is 99%, and the yield is 75.2%.

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Abstract

The invention provides a synthesis method of tetrabutylurea. The synthesis method comprises the following steps: dissolving an organic strong base catalyst and dimethyl carbonate into a solvent; raising temperature to 30 DEG C to 50 DEG C to obtain mixed liquid; dropwise adding dibutylamine into the mixed liquid at 50 DEG C to 80 DEG C; after dropwise adding, heating to reflux and keeping the heat and reacting for 5h to 8h to obtain reaction liquid; rectifying the reaction liquid under normal pressure to obtain condensed liquid containing the solvent and residual liquid; decompressing and rectifying the residual liquid to obtain a tetrabutylurea product and residues. According to the synthesis method of the tetrabutylurea, provided by the invention, a toxic raw material, namely phosgene, is not used and hydrogen chloride gas is not generated, so that equipment is not corroded and requirements on the equipment are relatively low; meanwhile, three wastes are avoided; the mass content of the tetrabutylurea in an obtained tetrabutylurea product is 99 percent or more and the yield is 75 percent or more.

Description

technical field [0001] The invention relates to the technical field of synthesis of fine chemical new materials, in particular to a synthesis method of tetrabutylurea. Background technique [0002] Tetrabutylurea is a widely used intermediate in organic synthesis, and can also be used as a solvent, extractant and catalyst in organic synthesis. In addition, because the solubility of hydrogenated anthraquinone in tetrabutyl urea is greater than that of trioctyl phosphate, the hydrogenation efficiency in the hydrogen peroxide production process is improved, and the distribution coefficient in the extraction process is increased. Therefore, it can replace trioctyl phosphate as hydrogen peroxide Solvents in production. [0003] The traditional synthesis of tetrabutylurea mainly has the following methods: (1) Phosgene method: using highly toxic raw material phosgene, and a large amount of hydrogen chloride gas is generated during the production process, the amount of waste gas is...

Claims

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Application Information

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IPC IPC(8): C07C275/06C07C273/18
CPCC07C273/18C07C275/06
Inventor 祝红福邓燕兰张敦河陈儒贵
Owner HUNAN GOFAR FINE CHEM IND TECH CO LDT
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