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Method for separating and purifying salt in 2,4,5-triamino-6-hydroxy pyrimidine sulfate production process

A technology for the production process of hydroxypyrimidine, which is applied in the field of synthesis of pharmaceutical intermediates, can solve the problems of high hazardous waste treatment and disposal costs, high operating costs, and expensive one-time investment, and achieve the elimination of hazardous waste generation, reduction of wastewater discharge, Favorable effect of biological treatment

Active Publication Date: 2016-05-04
NANCHANG UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

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

Method used

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  • Method for separating and purifying salt in 2,4,5-triamino-6-hydroxy pyrimidine sulfate production process
  • Method for separating and purifying salt in 2,4,5-triamino-6-hydroxy pyrimidine sulfate production process
  • Method for separating and purifying salt in 2,4,5-triamino-6-hydroxy pyrimidine sulfate production process

Examples

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Effect test

Embodiment 1

[0023] Put 330kg of guanidine nitrate into the dry 1000L jacketed condensation kettle, and then add 480kg of 30% sodium methoxide. When the jacket steam is heated to 45℃, 265kg of methyl cyanoacetate is added dropwise. When it reaches 1 / 3, watch the reflux, continue dripping without flushing, the dripping time is about half an hour, after dripping, the materials in the reactor will undergo condensation reaction at 67-70℃ to form the condensate 2.4-diamino -6-Hydroxypyrimidine. After refluxing for four hours, put the material into a closed centrifuge for solid-liquid separation. After the separation is completed, 150L methanol is used for centrifugal washing. The filtrate and washing liquid are pumped into the condensation kettle; the sodium nitrate filter cake washed with methanol is stirred and immersed with 300L methanol After centrifugal separation, the methanol solution is collected into the condensation kettle. Distill and condense the methanol in the recondensing kettle ...

Embodiment 2

[0025] In the 5000L nitrosation kettle with condensate, add 1100L of water and 300L of 50% sulfuric acid. When the temperature does not exceed 30℃, add 606L of dissolved 30% sodium nitrite to the nitrosation kettle for 0.5-1 hour. After the dripping is completed, after the end point is detected with a test paper, the temperature is kept for 1 hour, and the material is discharged and filtered to obtain the nitroso compound 2.4-diamino-5-nitroso-6-hydroxypyrimidine and the press filtrate. The filtrate was neutralized to neutrality with 30% sodium hydroxide 56L, clarified to remove solid impurities, evaporated, dried and dehydrated to obtain crude sodium sulfate; 200L methanol was used to stir and soak the crude sodium sulfate, and then centrifuged, methanol solution Collect the condensation kettle and the filtrate of Example 1 together with distillation and condensation to recover methanol and distillation residues; dry the centrifuged sodium sulfate, heat it to 65°C or more, and ...

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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 process optimization in the field of pharmaceutical intermediate synthesis, and specifically relates to the optimization of the process for preparing 2,4,5-triamino-6-hydroxypyrimidine sulfate, separation and purification of inorganic salts in intermediate products, and recovery as by-products, eliminating The amount of hazardous waste produced reduces the amount of wastewater discharged, eliminates the salt content in the wastewater, and is beneficial to the biological treatment of process wastewater. It is a cost-effective, green and environmentally friendly clean production process. Background technique [0002] 2,4,5-Triamino-6-hydroxypyrimidine sulfate (TAHMS) is an important intermediate for 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 raw materials of guanidine nitrate and ...

Claims

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Application Information

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IPC IPC(8): C07D239/50
CPCC07D239/50
Inventor 朱乐辉王深木朱衷榜
Owner NANCHANG UNIV
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