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Production process of guanidine sulfate

A production process and technology of guanidine sulfate, applied in the field of preparation of guanidine-based compounds, can solve the problems of no mature guanidine sulfate production process, unstable sulfate ion, low product purity, etc., and achieve simple and controllable reaction principle, less impurities and purity high effect

Pending Publication Date: 2022-05-06
田雨
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] At present, the relatively mature technique of producing guanidine nitrate in the related art is to utilize ammonium nitrate and dicyandiamide to react, and when preparing guanidine sulfate, if adopt ammonium sulfate and dicyandiamide to react, because its sulfate ion is unstable, it is easy to make The reaction process produces side reactions and generates impurities, so that the purity of the product obtained is low, so there is no mature production process for guanidine sulfate

Method used

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  • Production process of guanidine sulfate
  • Production process of guanidine sulfate

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0047] Embodiment 1: Guanidine sulfate is prepared by the following method:

[0048] S1. Mix guanidine hydrochloride with a molar ratio of 2:1 and sulfuric acid with a mass fraction of 80%, place guanidine hydrochloride in sulfuric acid at a constant speed within 60s, and stir continuously at a stirring speed of 300r / min during this period, and then place it at a temperature of 0°C React 48h under condition, generate reaction product and hydrogen chloride gas;

[0049] S2. Suction filter the reaction product prepared in S1 while it is hot, take the filtrate and cool it down to 10°C at a cooling rate of 5°C / 10min, then let it stand for 2 hours, and obtain crude guanidine sulfate after filtration; pass hydrogen chloride gas into the hydrogen oxidizer In sodium aqueous solution, sodium chloride solution and water are generated;

[0050] S3, put the crude product guanidine sulfate prepared in S2 into water and stir and dissolve for 15min under the condition of 400r / min to obtain ...

Embodiment 2

[0052] Embodiment 2: Guanidine sulfate is prepared by the following method:

[0053] S1, mixing guanidine hydrochloride with a molar ratio of 2:1.2 and sulfuric acid with a mass fraction of 88%, placed guanidine hydrochloride in sulfuric acid at a uniform speed within 60s, during which it was constantly stirred at a stirring speed of 300r / min, and then heated at 50°C React 24h under condition, generate reaction product and hydrogen chloride gas;

[0054] S2. Suction filter the reaction product prepared in S1 while it is hot, take the filtrate and cool it down to 12°C at a cooling rate of 5°C / 10min, then let it stand for 2.5h, and obtain crude guanidine sulfate after filtration; pass hydrogen chloride gas into hydrogen In the aqueous solution of sodium oxide, sodium chloride solution and water are generated;

[0055] S3, put the crude product guanidine sulfate prepared in S2 into water and stir and dissolve under the condition of 450r / min for 18min to obtain a stirred liquid; ...

Embodiment 3

[0057] Embodiment 3: Guanidine sulfate is prepared by the following method:

[0058] S1, the guanidine hydrochloride that the molar ratio is 2:1.5 and the concentrated sulfuric acid that mass fraction is 98% are mixed, and guanidine hydrochloride is placed in the concentrated sulfuric acid at a constant speed within 60s, constantly stirs with the stirring speed of 300r / min during this period, then in 72 Under the condition of ℃, react for 8 hours to generate reaction product and hydrogen chloride gas;

[0059] S2. Suction filter the reaction product prepared in S1 while it is hot. Take the filtrate and cool it down to 50°C at a cooling rate of 5°C / 10min. Stir continuously at a speed of 450r / min during this period. Stop stirring when the temperature is lower than 50°C. Continue Cool down to 15°C at a cooling rate of 5°C / 10min, then stand still for 3 hours, and obtain crude guanidine sulfate after filtration; pass hydrogen chloride gas into aqueous sodium hydroxide solution to g...

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Abstract

The invention relates to the field of guanidyl compound preparation, and particularly discloses a guanidine sulfate production process which comprises the following steps: S1, mixing guanidine hydrochloride and sulfuric acid in a molar ratio of 2: (1-2), and reacting at 30-100 DEG C for 1-48 hours to generate a reaction product and hydrogen chloride gas; s2, cooling and crystallizing the reaction product prepared in S1, and filtering to obtain crude guanidine sulfate; introducing hydrogen chloride gas into the sodium hydroxide aqueous solution to generate a sodium chloride solution and water; s3, recrystallizing the crude guanidine sulfate prepared in S2 to prepare a guanidine sulfate finished product; the prepared guanidine sulfate finished product has the advantages of few impurities and high purity.

Description

technical field [0001] The application relates to the field of guanidine-based compound preparation, more specifically, it relates to a production process of guanidine sulfate. Background technique [0002] Guanidine is a nitrogen-containing organic compound, also known as "imide urea", "imide urea" and "carbamidine". It is a colorless crystal with strong hygroscopicity and is easily soluble in water; Positive charge, easy to adsorb and penetrate into microorganisms, destroying material and energy metabolism, killing or inhibiting microorganisms; guanidino group is easy to form hydrogen bonds, good stability and strong physiological activity, can be used as Antihypertensive drugs, etc. [0003] Common guanidine-based compounds include guanidine nitrate, guanidine hydrochloride, guanidine sulfate, and guanidine carbonate, etc.; guanidine sulfate is a white crystalline substance, which is safer and more environmentally friendly than guanidine nitrate and other guanidine salts...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C277/00C07C279/02C01C1/16
CPCC07C277/00C01C1/164C01P2006/80C07C279/02
Inventor 田雨赵法刚张愉岚
Owner 田雨
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