Preparation technology of tetrabutyl urea

Abstract

The invention provides a preparation technology of tetrabutyl urea synthetized by a phosgene method. The tetrabutyl urea is synthetized from dibutylamine and carbonyl chloride as main materials in an alkaline organic solvent. The technology comprises the following steps: (1) adding dibutylamine, carbonyl chloride and the organic solvent according to a ratio to a reaction container; (2) adjusting the temperature of an acylation reaction, and controlling the time of the acylation reaction so as to obtain a tetrabutyl urea crude product; and (3) enabling the tetrabutyl urea crude product to be subjected to standing, separation, distillation, and purification so as to obtain the finished product of the tetrabutyl urea. The preparation method disclosed by the invention is simple in operation steps, the raw materials are low in price and easy to obtain, products are high in quality, the reaction yield reaches 90% or above, and the purity reaches 99% or above.

Description

Technical field [0001] The invention relates to the field of organic chemistry, and specifically relates to a preparation process of organic compound tetrabutylurea. Background technique [0002] Tetrabutylurea (C 17 H 36 N 2 0), is a widely used organic synthesis intermediate. It can also be used as a solvent, extraction agent and catalyst in organic chemistry, especially as a solvent in the production process of hydrogen peroxide. The methods for synthesizing tetrabutylurea are generally divided into phosgene method and non-phosgene method. The phosgene method includes the monophosgene method, the diphosgene method, the triphosgene method, etc.; the diphosgene method and the triphosgene method require the use of solvents in the process of preparing tetrabutylurea, but the monophosgene method is not applicable during the reaction. Solvent, but in subsequent processing, benzene or toluene needs to be used for extraction. According to relevant reports, the yield of the fi...

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Problems solved by technology

Phosgene method includes monophosgene method, diphosgene method, triphosgene method, etc.; diphosgene method and triphosgene method need to use solvent in the process of preparing tetrabutylurea, although monophosgene method is not applicable during reaction Solvent, but in the follow-up treatment, benzene or toluene needs to be used for extraction. According to related reports, the yield of finished product is only 80%-85%. Non-phosgene methods include carbon monoxide method, carbon dioxide method, acetanilide method, etc.; carbon monoxide method needs to use oxygen Or auxiliary reagents such as potassium iodide, reaction under pressurized condition, yield is low, and by-product is many, use dibutylamide lithium and di-n-butylamine and carbon monoxide reaction then be difficult to industrialization; Acetanilide method reacts with di-n-butylamine, Although less toxic, the product is an equal amount of tetrabutylurea and by-products

At present, there are basically no enterprises producing tetrabutylurea in China, and most of the market demand depends on foreign imports.