Waste liquid treatment method in guanine preparation process

Abstract

The invention belongs to the field of industrial waste liquid treatment, and particularly relates to a waste liquid treatment method in a guanine preparation process. Sulfuric acid and alcohol substances are added into a closed-loop reaction liquid generated in the process of producing the guanine step by step, the conversion between sodium formate and formic acid in the closed-loop reaction liquid is realized, the formate and salt substances obtained after conversion are recycled, so that the economic value of the wastewater in the production process of the guanine is effectively improved, and the pollution to the environment is reduced.

Description

Technical field

[0001] The invention belongs to the field of industrial waste liquid treatment, and is specifically a waste liquid treatment method in a guanine preparation process. Background technique

[0002] Guanine is an important substance in the synthesis of antivirals, such as the antiviral drugs acyclovir and gamma-aciclovir. Its chemical name is: 2-aminopurine, and its molecular formula is: C 5 H 5 N 5 O. Since guanine has very poor water solubility and ester solubility, in order to ensure the yield of guanine and the purity of the prepared guanine, the prior art adopts direct or indirect methods to obtain 2,4-diamino-6- Hydroxy-5nitrosopyrimidine (DAHNP) or 2,4,5-triamino-6-hydroxypyrimidine sulfate reacts with formic acid under the action of a catalyst, and the obtained product is washed with formic acid or inorganic acid to obtain a finished product.

[0003] The specific reaction principle is:

[0004] .

[0005] In this process, formic acid and inorganic acid are us...

Examples

Embodiment 1

[0035] The waste liquid treatment method in the guanine preparation process includes the following steps:

[0036] Put in formic acid (85%) 561.2g (10.363mol) in a 1500ml three-necked flask, add 249.6g (3.597mol) of sodium formate (98%) under stirring to dissolve it, then add 320g (1.338mol) of triamine, stir and heat up Reaction to reflux for 32 hours. 1.31 mol of formic acid was consumed during the reaction, and the total amount of residual formic acid was 12.65 mol.

[0037] Collect 1130.8g of the closed-loop reaction solution containing formic acid and sodium formate produced during the production of guanine; add 179.96g 98% concentrated sulfuric acid dropwise to the closed-loop reaction solution to convert the sodium formate in the closed-loop reaction solution into formic acid and sodium sulfate; Continue to put 8.82g of 98% concentrated sulfuric acid (0.025 times the amount of sodium formate) as a catalyst, and then add 425.57g of methanol (1.05 times the amount of total fo...

Embodiment 2

[0039] The waste liquid treatment method in the guanine preparation process includes the following steps:

[0040] Put in formic acid (85%) 561.2g (10.363mol) in a 1500ml three-necked flask, add 249.6g (3.597mol) of sodium formate (98%) under stirring to dissolve it, then add 320g (1.338mol) of triamine, stir and heat up Reaction to reflux for 32 hours. 1.31 mol of formic acid was consumed during the reaction, and the total amount of residual formic acid was 12.65 mol.

[0041] Collect 1130.8g of the closed-loop reaction solution containing formic acid and sodium formate produced during the production of guanine; add 179.96g 98% concentrated sulfuric acid dropwise to the closed-loop reaction solution to convert the sodium formate in the closed-loop reaction solution into formic acid and sodium sulfate; Continue to put in 98% concentrated sulfuric acid 176.4g (0.5 times the amount of sodium formate) as a catalyst, then add 506.65g methanol (1.25 times the amount of total formic aci...

Embodiment 3

[0043] The waste liquid treatment method in the guanine preparation process includes the following steps:

[0044] Put in formic acid (85%) 561.2g (10.363mol) in a 1500ml three-necked flask, add 249.6g (3.597mol) of sodium formate (98%) under stirring to dissolve it, then add 320g (1.338mol) of triamine, stir and heat up Reaction to reflux for 32 hours. 1.31 mol of formic acid was consumed during the reaction, and the total amount of residual formic acid was 12.65 mol.

[0045] Collect 1130.8g of the closed-loop reaction solution containing formic acid and sodium formate produced during the production of guanine; add 179.96g 98% concentrated sulfuric acid dropwise to the closed-loop reaction solution to convert the sodium formate in the closed-loop reaction solution into formic acid and sodium sulfate; Continue to put 92.60g of 98% concentrated sulfuric acid (0.2625 times the amount of sodium formate) as a catalyst, then add 466.10g of methanol (1.15 times the amount of total form...

Technical field

[0001] The invention belongs to the field of industrial waste liquid treatment, and is specifically a waste liquid treatment method in a guanine preparation process. Background technique

[0002] Guanine is an important substance in the synthesis of antivirals, such as the antiviral drugs acyclovir and gamma-aciclovir. Its chemical name is: 2-aminopurine, and its molecular formula is: C 5 H 5 N 5 O. Since guanine has very poor water solubility and ester solubility, in order to ensure the yield of guanine and the purity of the prepared guanine, the prior art adopts direct or indirect methods to obtain 2,4-diamino-6- Hydroxy-5nitrosopyrimidine (DAHNP) or 2,4,5-triamino-6-hydroxypyrimidine sulfate reacts with formic acid under the action of a catalyst, and the obtained product is washed with formic acid or inorganic acid to obtain a finished product.

[0003] The specific reaction principle is:

[0004] .

[0005] In this process, formic acid and inorganic acid are us...

Examples

Embodiment 1

[0035] The waste liquid treatment method in the guanine preparation process includes the following steps:

[0036] Put in formic acid (85%) 561.2g (10.363mol) in a 1500ml three-necked flask, add 249.6g (3.597mol) of sodium formate (98%) under stirring to dissolve it, then add 320g (1.338mol) of triamine, stir and heat up Reaction to reflux for 32 hours. 1.31 mol of formic acid was consumed during the reaction, and the total amount of residual formic acid was 12.65 mol.

[0037] Collect 1130.8g of the closed-loop reaction solution containing formic acid and sodium formate produced during the production of guanine; add 179.96g 98% concentrated sulfuric acid dropwise to the closed-loop reaction solution to convert the sodium formate in the closed-loop reaction solution into formic acid and sodium sulfate; Continue to put 8.82g of 98% concentrated sulfuric acid (0.025 times the amount of sodium formate) as a catalyst, and then add 425.57g of methanol (1.05 times the amount of total fo...

Embodiment 2

[0039] The waste liquid treatment method in the guanine preparation process includes the following steps:

[0040] Put in formic acid (85%) 561.2g (10.363mol) in a 1500ml three-necked flask, add 249.6g (3.597mol) of sodium formate (98%) under stirring to dissolve it, then add 320g (1.338mol) of triamine, stir and heat up Reaction to reflux for 32 hours. 1.31 mol of formic acid was consumed during the reaction, and the total amount of residual formic acid was 12.65 mol.

[0041] Collect 1130.8g of the closed-loop reaction solution containing formic acid and sodium formate produced during the production of guanine; add 179.96g 98% concentrated sulfuric acid dropwise to the closed-loop reaction solution to convert the sodium formate in the closed-loop reaction solution into formic acid and sodium sulfate; Continue to put in 98% concentrated sulfuric acid 176.4g (0.5 times the amount of sodium formate) as a catalyst, then add 506.65g methanol (1.25 times the amount of total formic aci...

Embodiment 3

[0043] The waste liquid treatment method in the guanine preparation process includes the following steps:

[0044] Put in formic acid (85%) 561.2g (10.363mol) in a 1500ml three-necked flask, add 249.6g (3.597mol) of sodium formate (98%) under stirring to dissolve it, then add 320g (1.338mol) of triamine, stir and heat up Reaction to reflux for 32 hours. 1.31 mol of formic acid was consumed during the reaction, and the total amount of residual formic acid was 12.65 mol.

[0045] Collect 1130.8g of the closed-loop reaction solution containing formic acid and sodium formate produced during the production of guanine; add 179.96g 98% concentrated sulfuric acid dropwise to the closed-loop reaction solution to convert the sodium formate in the closed-loop reaction solution into formic acid and sodium sulfate; Continue to put 92.60g of 98% concentrated sulfuric acid (0.2625 times the amount of sodium formate) as a catalyst, then add 466.10g of methanol (1.15 times the amount of total form...