Method for separation and purification of salt during production of 2,4,5-triamino-6-hydroxypyrimidine sulfate

A technology for the production process of hydroxypyrimidine, applied in the field of synthesis of pharmaceutical intermediates, can solve the problems of high cost of hazardous waste treatment, large amount of hazardous waste, expensive one-time investment, etc., to eliminate the amount of hazardous waste generated and reduce the content of waste water Salt content, beneficial effect of biological treatment

Active Publication Date: 2019-04-16
NANCHANG UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

At present, the desalination method of wastewater mainly adopts multi-effect evaporation (mainly three-effect) or MVR (mechanical secondary vapor recompression) technology. These two evaporation technologies have the disadvantages of high one-time investment, high energy consumption and hazardous waste. Large volume and high cost of hazardous waste treatment and disposal
(1) One-time investment: due to the high salt content and strong corrosion of wastewater, the evaporation equipment needs to be made of titanium steel as the main material, and the equipment is expensive to manufacture; (2) Operation energy consumption: three-effect evaporation of 1 ton of water requires about 0.4 steam tons, MVR needs 60 to 100 degrees of electricity to evaporate 1 ton of water, high energy consumption and high operating costs; (3) The residue after the two kinds of evaporation technology evaporates waste water is water-containing waste salt slag, based on a moisture content of 20%, With an annual output of 2,000 tons of 2,4,5-triamino-6-hydroxypyrimidine sulfate, 2,067 tons of waste salt slag is produced, which is disposed of as hazardous waste, and the disposal cost is high

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  • Method for separation and purification of salt during production of 2,4,5-triamino-6-hydroxypyrimidine sulfate
  • Method for separation and purification of salt during production of 2,4,5-triamino-6-hydroxypyrimidine sulfate
  • Method for separation and purification of salt during production of 2,4,5-triamino-6-hydroxypyrimidine sulfate

Examples

Experimental program
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Effect test

Embodiment 1

[0023] Put 330kg of guanidine nitrate into the dried 1000L jacketed condensation kettle, and then drop into 480kg of 30% sodium methoxide. See the reflux at one-third of the time, continue to drop without flushing, the dropping time is about half an hour, after the dropping is completed, the materials in the reactor undergo condensation reaction at a temperature of 67-70°C to form the condensate 2.4-diamino -6-Hydroxypyrimidine. After four hours of reflux, feed the material into a closed centrifuge for solid-liquid separation. After the separation, use 150L methanol for centrifugal washing, and pump the filtrate and washing liquid into the condensation kettle; the sodium nitrate filter cake washed with methanol is stirred and soaked with 300L methanol , and then centrifuged, and the methanol solution was collected into the condensation tank. Distill and condense the methanol in the condensation kettle under normal pressure above 65°C. After the methanol is recovered, add 500L...

Embodiment 2

[0025]Add 1100L of water and 300L of 50% sulfuric acid to the 5000L nitrosation kettle where the condensate is added. When the temperature does not exceed 30°C, add 606L of dissolved 30% sodium nitrite dropwise to the nitrosation kettle for 0.5-1 hour After the dropwise addition is completed, after the end point is detected with test paper, keep warm for 1 hour, discharge and press filter to obtain the nitroside 2.4-diamino-5-nitroso-6-hydroxypyrimidine and the press-filtrate. Neutralize the filtrate to neutral with 56L of 30% sodium hydroxide, clarify and remove solid impurities, and obtain crude sodium sulfate by evaporation, drying and dehydration; stir and soak the crude sodium sulfate with 200L of methanol, then perform centrifugation, methanol solution Collected into the condensation tank and the filtrate of Example 1 to distill and condense to recover methanol and distillation residue; dry the sodium sulfate separated by centrifugation, and heat it to above 65°C. Methano...

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Abstract

The invention provides a method for separating and purifying salts in the 2,4,5-triamino-6-hydroxy pyrimidine sulfate production process. The method comprises the following steps that: guanidine nitrate, ethyl cyanoacetate and sodium methoxide serving as raw materials are subjected to a condensation reaction to generate condensate 2,4-diamino-6-hydroxypyrimidine, methanol and sodium nitrate; the condensate 2,4-diamino-6-hydroxypyrimidine, sodium nitrate and sulfuric acid serving as raw materials are subjected to a nitrosation reaction to generate a nitrosified substance 2,4-diamino-5-nitroso-6-hydroxypyrimidine, sodium sulfate and water. According to the method, firstly, after the condensation reaction, sodium nitrate is separated, and purification is carried out; then, sodium sulfate is separated in the nitrosation reaction, and purification is carried out; and byproducts of industrial sodium nitrate and industrial sodium sulfate meeting the national standard are reclaimed, so that hazard waste output is eliminated, wastewater drainage is reduced, salt content in wastewater is reduced, and process wastewater biological treatment is benefited.

Description

technical field [0001] The invention belongs to the process optimization in the field of synthesis of pharmaceutical intermediates, in particular to the optimization of the process for preparing 2,4,5-triamino-6-hydroxypyrimidine sulfate, the separation and purification of inorganic salts in intermediate products, and recovery as by-products, eliminating The amount of hazardous waste generated reduces the amount of wastewater discharged and eliminates the salt content in wastewater, which is beneficial to the biological treatment of process wastewater. It is an economical, effective, green and environmentally friendly clean production process. Background technique [0002] 2,4,5-Triamino-6-hydroxypyrimidine sulfate (TAHMS) is an important intermediate in the synthesis of broad-spectrum antiviral drug acyclovir and anti-anemia drug folic acid. The preparation process is divided into the following steps: [0003] (1) Condensation (cyclization): Put the guanidine nitrate and ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07D239/50
CPCC07D239/50
Inventor 朱乐辉王深木朱衷榜
Owner NANCHANG UNIV
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