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Process for synthesizing biurea by adopting semicarbazide

A semicarbazide and biuret technology, applied in the field of biuret synthesis, can solve the problems of low utilization rate of raw materials, low product yield, long reaction time, etc., and achieve the effects of low acidity, high conversion rate and little equipment corrosion

Inactive Publication Date: 2015-08-19
HANGZHOU HI TECH FINE CHEM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Due to the high temperature required for the reaction, urea is easily decomposed to produce a large number of by-products during the reaction, so the amount of urea added is greatly excessive, the product yield is low, and the utilization rate of raw materials is low
Biurea can also be formed by direct condensation of urea and hydrazine hydrate, but the reaction time is longer, and the reaction needs to be carried out at 105-120°C. The by-product of the reaction is ammonia gas, and the subsequent input of ammonia recovery will increase the cost.

Method used

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  • Process for synthesizing biurea by adopting semicarbazide

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Effect test

Embodiment 1

[0031] First weigh 75g of semicarbazide, then weigh 66g of sodium cyanate, add both into a three-necked flask filled with 200mL of water, stir until the solution is clear, keep the solution temperature at 20°C, weigh 183g of 20% hydrochloric acid solution drop by drop Add it to the above mixture, stir while adding, and continue stirring for 5 minutes after the addition of hydrochloric acid is complete, then filter, wash and dry.

Embodiment 2

[0033] First weigh 75g of semicarbazide, then weigh 66g of sodium cyanate, add both into a three-necked flask filled with 200mL of water, stir until the solution is clear, keep the solution temperature at 40°C, weigh 184g of 20% hydrochloric acid solution drop by drop Add to the above mixture, stir while adding, and continue to stir for 7 minutes after the addition of hydrochloric acid is complete, then filter, wash and dry.

Embodiment 3

[0035] First weigh 75g of semicarbazide, then weigh 68g of sodium cyanate, add both into a three-necked flask filled with 200mL of water, stir until the solution is clear, keep the solution temperature at 50°C, weigh 185g of 20% hydrochloric acid solution drop by drop Add it to the above mixture, stir while adding, and continue stirring for 8 minutes after the addition of hydrochloric acid is complete, then filter, wash and dry.

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Abstract

The invention provides a process for synthesizing biurea by adopting semicarbazide. The process comprises the following steps: a, using semicarbazide and cyanate as raw materials, weighing solid according to the molar ratio of semicarbazide to cyanic acid radicals of 1: (1.01 to 1.05) and adding water; b, keeping the temperature of the mixed solution in a range of 0 to 80 DEG C; c, preparing an acid solution according to the molar ratio of the cyanic acid radical to H+ being 1: (1.01 to 1.05); d, dropwise adding the acid solution into the mixed solution while stirring, and finishing the reaction; and e, filtering, washing and drying. The process has the beneficial effects that firstly, a low temperature is adopted in the reaction, the semicarbazide is stable in property, is difficult to volatilize and is difficult to convert into other substances, the conversion rate is very high, and the yield of 100% can be reached; secondly, a reaction byproduct is sodium salt, has no pollution to the environment, and can be discharged without being post-processed; thirdly, the reaction is performed under a normal pressure and is easy to operate; and fourthly, the acidity is low in the reaction and the equipment is corroded a little.

Description

technical field [0001] The invention relates to the field of biurea synthesis, in particular to a process for synthesizing biurea by using semicarbazide. Background technique [0002] The chemical name of biurea is hydrazine dicarboxamide, the molecular formula is C2H6N4O2, the chemical formula is H2NCONH-NHCONH2, and the relative molecular mass is 118. It is mainly used in the production of ADC foaming agent (azodicarbonamide), and can also be used in the anti-skid of airstrips, high-grade highways, gears, and fire-proof and anti-melt of high-grade cables. [0003] Biurea is usually formed by the condensation reaction of hydrazine hydrate and urea under acidic conditions. This process produces biurea, and the reaction temperature is relatively high. Generally, the condensation reaction is carried out at 105-120°C to obtain the product biurea and ammonium salt. The by-product ammonium salt needs to be further evaporated and concentrated to recover ammonia. Due to the high ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C281/06
Inventor 陈海贤董梅倪彬鑫
Owner HANGZHOU HI TECH FINE CHEM
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