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Preparation method of sodium acetate

A technology of sodium acetate and glacial acetic acid, which is applied in the field of preparation of pharmaceutical excipients sodium acetate and pharmaceutical grade, food grade, and reagent grade sodium acetate, which can solve the problem that product purity cannot guarantee the quality requirements of pharmaceutical excipients and chemical reagents, and consumes energy Large, high operational risk and other problems, to achieve the effect of high yield, low equipment requirements, and uniform crystal particle size

Inactive Publication Date: 2014-06-04
TIANJIN KERMEL CHEM REAGENT
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

In the preparation process, the proportion of raw materials is usually controlled properly, resulting in the reaction solution being strongly alkaline and highly corrosive to various filter materials. If it is directly filtered, the operation risk is relatively large, and the concentration step in the preparation process is expensive. The energy is huge, and complex equipment is required to complete the preparation, and the purity of the prepared products often cannot guarantee the quality requirements of pharmaceutical excipients and chemical reagents

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0022] Dissolve 300g of glacial acetic acid in 300g of pure water to prepare an acetic acid solution with a mass percentage of 50%; then heat the solution to 50°C; pour the heated acetic acid solution into a three-necked flask, start stirring, and then pour into the solution Slowly add 200g of sodium hydroxide solid; after adding all the 200g of sodium hydroxide, continue to stir for 10 minutes to make the reaction complete; check the pH value with pH test paper, then adjust it to control the pH value at 7.7, and use the G3 funnel to complete the reaction. When filtering, the temperature is kept at 80°C; the filtrate is cooled and crystallized, and stirred during the crystallization process; when no crystals are precipitated in the solution, the supernatant is poured into a beaker, and the precipitated crystals are separated from solid and liquid, and shaken Dry to obtain sodium acetate, the product content is 100.71%, and the yield is 55%.

Embodiment 2

[0024] Dissolve 300g of glacial acetic acid in 300g of pure water to prepare an acetic acid solution with a mass percentage of 50%; then heat the solution to 60°C; pour the heated acetic acid solution into a three-necked flask, start stirring, and then pour into the solution Slowly add 200g of sodium hydroxide solid; after adding all the 200g of sodium hydroxide, continue to stir for 10 minutes to make the reaction complete; check the pH value with pH test paper, then adjust it to control the pH value at 8.2, and use the G3 funnel to complete the reaction. When filtering, the temperature is kept at 80°C; the filtrate is cooled and crystallized, and stirred during the crystallization process; when no crystals are precipitated in the solution, the supernatant is poured into a beaker, and the precipitated crystals are separated from solid and liquid, and shaken Dry to obtain sodium acetate, the product content is 99.97%, and the yield is 66.2%.

Embodiment 3

[0026] Dissolve 300g of glacial acetic acid in 300g of pure water to prepare an acetic acid solution with a mass percentage of 50%; then heat the solution to 60°C; pour the heated acetic acid solution into a three-necked flask, start stirring, and then pour into the solution Slowly add 200g of sodium hydroxide solid; after adding all the 200g of sodium hydroxide, continue to stir for 10 minutes to make it react completely; check the pH value with pH test paper, then adjust it to control the pH value at 7.4, and use the G 3 funnel to The reaction solution is filtered, and the temperature is maintained at 80°C during the filtration; the filtrate is cooled and crystallized, and stirred during the crystallization process; when no crystals are precipitated in the solution, the supernatant is poured into a beaker, and the precipitated crystals are separated into solids and liquids. Dried to obtain sodium acetate, the product content is 98.8%, and the yield is 60.3%.

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Abstract

The invention discloses a preparation method of sodium acetate. According to the preparation method, optimal reactant ratio is determined based on researches on sodium acetate synthesis and crystallization technology, strong alkaline liquid filtration is not needed, condensation or proportion adjustment is not needed, conventional sample equipment is adopted, heating is not needed by technical processes, technical conditions are mild and stable, and requirements on equipment are low. Quality of obtained products is capable of meeting with requirements of Chinese pharmacopoeia 2010 and reagent grade standards; crystal size is uniform; yield is high; the preparation method is suitable for GMP industrial production of pharmaceutic adjuvants, and food-grade and reagent-grade industrial production.

Description

technical field [0001] The invention relates to the field of chemical synthesis, in particular to a preparation method of sodium acetate as a medical auxiliary material and pharmaceutical grade, food grade and reagent grade sodium acetate. Background technique [0002] Sodium acetate, a colorless and odorless crystal, can be weathered in the air, flammable, soluble in water, slightly soluble in ethanol, insoluble in ether, loses crystal water at 123°C, alias: sodium acetate, crystalline sodium acetate, trihydrate Sodium acetate, molecular formula CH 3 COONa·3H 2 O, the pH value (50g / L, 25°C) is 7.5-9.0, the density is 1.45g / cm3, and the melting point is 58°C. [0003] The general production method of sodium acetate is to carry out metathesis reaction of calcium acetate and soda ash to become sodium acetate, concentrate the reaction solution to 26 ° Be, add activated carbon to decolorize, then carry out cooling crystallization, and centrifuge to obtain the finished product....

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C53/10C07C51/41
CPCC07C51/412
Inventor 秦汉超苏学松陈曙李刚林立成
Owner TIANJIN KERMEL CHEM REAGENT
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