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Series production technology of biurea

A production process, the technology of biurea, applied in the field of continuous production of biurea, can solve the problems of high chemical oxygen consumption, high cost, and difficult post-treatment of wastewater, and achieve fast reaction speed, high cost, and difficult post-treatment big effect

Active Publication Date: 2008-07-30
JIANGSU SOPO GRP
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, when the acidic condensation process is adopted, since a large amount of ammonium salts are generated in the reaction process, the ammonia nitrogen (NH3) in the mother liquor and washing liquid after the reaction is finished 3 -N) content is extremely high, chemical oxygen demand (COD) is very large, resulting in difficult and expensive post-treatment of wastewater

Method used

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  • Series production technology of biurea

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0038] Get 500ml hydrazine hydrate solution and 125g urea, wherein the content of hydrazine hydrate in the middle of the hydrazine hydrate solution is 10% (referring to " weight percent content ", the same below), be placed in the 1000ml four of heating, electric stirring, thermometer and reflux device In the flask, the temperature was raised to 102°C, and part of the condensed water was refluxed. The content of urea and hydrazine hydrate in the reaction solution was detected every half hour, and after 13 hours, the content of hydrazine hydrate was 0.9%.

[0039] Another 400ml of hydrazine hydrate solution (10% hydrazine hydrate content) was added to 100ml of mother liquor (0.9% hydrazine hydrate content), and the control conditions were as above. After 11.5 hours, the hydrazine hydrate content was 0.9%.

[0040] The comparison of the above results shows that the reuse of mother liquor can accelerate the reaction speed.

Embodiment 2

[0042] The three-pot process shown in Figure 1 is adopted. The volume of the first reactor R01 is 400 liters, and the volumes of the second reactor R02 and the third reactor R03 are both 350 liters. The hydrazine hydrate solution with a hydrazine hydrate content of 10% is used as a raw material, and the urea consumption is determined according to the material ratio of "hydrazine hydrate: urea = 1: 6". In addition, the mother liquor is added to form a mixed solution with a hydrazine hydrate content of 5.8%. The first reactor R01 is then fed with a feed rate of 250 liters per hour. The bottom material of R01 enters R02 continuously, the bottom material of R02 continuously enters the solid-liquid separation device, the mother liquor separated by X01 continuously enters R03, the mother liquor produced by the separation of R03 bottom material by X02 returns to M01, and the solid separated by X01 and X02 is combined Diurea. The reaction temperatures of R01, R02, and R03 are all gr...

Embodiment 3

[0044] Still using the three-pot process shown in Figure 1. The volume of the first reactor R01 is 400 liters, and the volumes of the second reactor R02 and the third reactor R03 are both 350 liters. The material ratio of hydrazine hydrate and urea is 1: 3.9, the content of hydrazine hydrate in the middle of the raw material hydrazine hydrate solution is 10%, and the concentration of hydrazine hydrate in the mixed solution made after adding the mother liquor is 6.5%, and the first reaction kettle R01 per hour The total feed volume is 180 liters. The bottom material of R01 enters R02 continuously, the bottom material of R02 continuously enters the solid-liquid separation device, the mother liquor separated by X01 continuously enters R03, the mother liquor produced by the separation of R03 bottom material by X02 returns to M01, and the solid separated by X01 and X02 is combined Diurea. The reaction temperatures of R01, R02, and R03 are all greater than 100°C, and the reaction ...

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Abstract

The invention provides a continuous production process for biurea, which comprises a step that the hydrazine hydrate solution and urea serving as main reaction raw materials reacts with each other to generate the biurea by condensation reaction. The invention is characterized in that: the urea is mixed with the hydrazine hydrate solution to prepare the mixed solution continusouly going into a reaction vessel; The biurea produced in the reaction together with the mother liquor containing the hydrazine hydrate and urea that do not participate in the reaction is discharged from the bottom of reaction vessel, and continuously goes into a solid-liquid separation unit; after being subject to a separation in a solid-liquid separation unit, the biurea solid substance and mother liquid are respectively obtained, and all of the mother liquid is used in circulation. The ammonia and water vapor generated in the reaction escape from the top of reaction vessel and are separated from each other after condensation, At least part of the formed liquor condensate is discharged from reaction system directly. The method shows not only short reaction time and great production capacity but realizes full circulation utilization of mother liquid and biurea washing water. The invention has less wastewater and simple components, and is suitable for comprehensive treatment.

Description

technical field [0001] The present invention relates to the production of biurea, especially the method for continuously producing biurea through condensation reaction under alkaline conditions. Background technique [0002] Biurea (NH 2 CONHNHCONH 2 ) is an important intermediate for the production of ADC foaming agent (azodicarbonamide), and can also be used for anti-skid of airstrips, anti-skid of gears, fireproof and anti-solvent of high-grade cables, etc. In the chemical industry, the traditional method for preparing biurea is to use hydrazine hydrate (N 2 h 4 ·H 2 O) and urea (NH 2 CONH 2 ) as a raw material, which is condensed under acidic or alkaline conditions to generate biurea. Its overall reaction formula is: [0003] N 2 h 4 +2NH 2 CONH 2 →NH 2 CONHNHCONH 2 +2NH 3 [0004] In the prior art, biurea production devices basically adopt batch production process. The practical application shows that the acidic condensation process is used, the reactio...

Claims

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Application Information

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IPC IPC(8): C07C281/06C07C273/18
Inventor 宋勤华胡宗贵邵守言朱晓新孙云霞凌晨陆锡峰周月荣曹宏兵
Owner JIANGSU SOPO GRP
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