Method for synthesizing TD (thiourea dioxide) at low temperature

A technology of thiourea dioxide and thiourea dioxide, applied in the direction of organic chemistry, etc., can solve the problems of increasing product yield, reducing solubility of thiourea dioxide, etc., and achieves the effects of reducing side reactions, increasing yield, and increasing dispersibility.

Inactive Publication Date: 2015-12-16
UNIV OF JINAN
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Problems solved by technology

[0011] The present invention aims at the low yield of thiourea dioxide at present. By adding a dispersant to the reaction system, the dispersibility of the product is increased, the product is rapidly precipitated from the mother liquor, and the occurrence of side reactions is reduced. Reduced the solubility of thiourea dioxide in the mother liquor and increased the yield of the product

Method used

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  • Method for synthesizing TD (thiourea dioxide) at low temperature
  • Method for synthesizing TD (thiourea dioxide) at low temperature
  • Method for synthesizing TD (thiourea dioxide) at low temperature

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Embodiment Construction

[0017] 1. Add distilled water into the reactor, add catalyst in proportion, add ammonium bicarbonate to control pH4-5, and add dispersant cetyltrimethylammonium bromide at the same time, the amount added is 1.0‰ of the mass of thiourea, in batches Add thiourea, control the temperature of the reaction solution at -10°C, add hydrogen peroxide dropwise under stirring conditions to react, the ratio of hydrogen peroxide to thiourea is H 2 o 2 / CS(NH 2 ) 2 =2.0, left to stand for crystallization for 30 minutes after the completion of the reaction, suction filtered and dried to obtain the product, and the calculated product yield was 94%.

[0018] 2. Add distilled water to the reactor, add catalyst in proportion, add ammonium bicarbonate to control pH 4-5, and add dispersant cetyltrimethylammonium bromide at the same time, the amount added is 1.5‰ of the mass of thiourea, in batches Add thiourea, control the temperature of the reaction solution at -10°C, add hydrogen peroxide drop...

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Abstract

The invention discloses a method for synthesizing TD (thiourea dioxide) and belongs to the technical field of organic synthesis. The method comprises synthesis steps as follows: distilled water is added to a reactor, a catalyst is added in proportion, ammonium bicarbonate is added to control pH to range from 4 to 5, meanwhile, a dispersing agent is added, CS(NH2)2 is added in batches, the temperature of a reaction liquid is controlled, H2O2 is added dropwise under the stirring condition for a reaction, the ratio of the H2O2 to the CS(NH2)2 is 2.0, the mixture is left to stand for crystallization for 30 min after the reaction is finished, the TD is obtained through suction filtration and drying, and the yield of the TD is up to 95%. With the adoption of the method, over oxidation of the TD is reduced, the produced TD is separated out quickly, the reaction yield is increased, meanwhile, reaction steps are simple, and the method is suitable for industrial production.

Description

technical field [0001] The invention introduces a method for synthesizing thiourea dioxide at low temperature, which belongs to the field of organic synthesis. technical background [0002] Thioureadioxide, referred to as TD, is a new type of highly efficient organic reducing agent. It has the advantages of good thermal stability, strong reducing ability, and good safety performance. Thiourea dioxide has a wide range of uses. In addition to being used as a reducing agent for various metal ions in the field of inorganic chemistry, because its reducing ability is stronger than that of sodium hydrosulfite and its stability is good, it is more convenient and safe to transport, store and use. It is not easy to decompose and spontaneously ignite like hydrosulfite. It has become a substitute for hydrosulfite in the printing, dyeing and bleaching industries. And because the reduction potential of thiourea dioxide can reach up to 1230mv, it has excellent reducing ability. In addit...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C381/14
Inventor 孙国新司繁彬李建平刘瑶瑶曹胜光
Owner UNIV OF JINAN
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