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Refining method for preparing high-purity non-caking fine-particle citric acid crystals

A refining method, citric acid technology, applied in the separation/purification of carboxylic acid compounds, organic chemistry, etc., can solve the problems of affecting the quality of citric acid-containing reagents, reducing the yield of citric acid, and reducing the strength of tablets, etc. , to achieve the effects of increased chloride and sulfate content, stable and feasible process, and extended shelf life

Active Publication Date: 2020-09-18
湖南新绿方药业有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Because the solubility difference of citric acid at different temperatures is less, directly adopt recrystallization operation to reduce the yield of citric acid, and the citric acid product particle size distribution that described method obtains is extensive, easily causes the reduction of tablet strength, And it is easy to agglomerate, which is easy to cause powder cohesion and affects the quality of medicines containing citric acid reagents

Method used

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  • Refining method for preparing high-purity non-caking fine-particle citric acid crystals
  • Refining method for preparing high-purity non-caking fine-particle citric acid crystals
  • Refining method for preparing high-purity non-caking fine-particle citric acid crystals

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Effect test

Embodiment 1

[0025] This embodiment provides a kind of refining method for preparing high-purity, non-caking fine-grained citric acid crystals:

[0026] S1. Dissolution and decolorization: Dissolve 100g of citric acid monohydrate and 35mL of water, add 0.4g of powdered medicinal activated carbon, heat up to 85°C, stir at a speed of 60-65r / min for 10-20min to decolorize.

[0027] S2. Filtration: Reduce the stirring speed to 10-12r / min, open the discharge valve, the liquid enters the 20um titanium rod filter for coarse filtration, and then enters the 0.5um titanium rod filter for fine filtration;

[0028] S3. Concentration and crystallization: Concentrate the substance liquid filtered in step S2 until the specific gravity of the concentrated solution is 1.35-1.45g / mL, the temperature is 60°C, the vacuum degree is -0.07MPa, and the concentration is concentrated to a relative density of 1.35g / mL. Reduce the stirring speed to 5-8r / min, slowly add 1.75g ​​of citric acid seed crystals, continue t...

Embodiment 2

[0031] This embodiment provides a kind of refining method for preparing high-purity, non-caking fine-grained citric acid crystals:

[0032] S1. Dissolution and decolorization: Dissolve 100g of citric acid monohydrate and 40mL of water, add 0.3g of powdered medicinal activated carbon, heat up to 90°C, and stir at a speed of 60-65r / min for 10-20min.

[0033] S2. Filtration: Reduce the stirring speed to 10-12r / min, open the discharge valve, and the liquid enters the 20um titanium rod filter for coarse filtration, and then enters the 0.5um titanium rod filter for fine filtration.

[0034] S3. Concentration and crystallization: Concentrate the substance liquid filtered in step S2 until the specific gravity of the concentrated solution is 1.35-1.45g / mL, the temperature is 50°C, the vacuum degree is -0.07MPa, and the concentration is concentrated to a relative density of 1.40g / mL. Reduce the stirring speed to 5-8r / min, slowly add 1.70g of citric acid seed crystals, continue to stir f...

Embodiment 3

[0037] This embodiment provides a kind of refining method for preparing high-purity, non-caking fine-grained citric acid crystals:

[0038] S1. Dissolution and decolorization: Dissolve 100g of citric acid monohydrate and 45mL of water, add 0.5g of activated carbon, heat up to 95°C, stir at a speed of 60-65r / min for 10-20min to decolorize.

[0039] S2. Filtration: Reduce the stirring speed to 10-12r / min, open the discharge valve, the liquid enters the 20um titanium rod filter for coarse filtration, and then enters the 0.5um titanium rod filter for fine filtration;

[0040] S3. Concentration and crystallization: Concentrate the liquid filtered in step S2 until the specific gravity of the concentrated solution is 1.35-1.45g / mL, the temperature is 50°C, the vacuum degree is -0.07MPa, and the relative density is 1.45g / mL. Reduce the stirring speed to 5-8r / min, slowly add 1.82g of citric acid seed crystals, continue to stir for 30min, pass in cooling water to cool to 20°C, crystalli...

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Abstract

The invention discloses a refining method for preparing high-purity non-caking fine-particle citric acid crystals, wherein the refining method comprises the steps: by using a citric acid crude productas a raw material, dissolving, decolorizing, filtering, concentrating, crystallizing, separating and drying to obtain refined citric acid. The method provided by the invention is simple and easy to implement and mild in condition, and overcomes the defects that a citric acid product obtained by an existing edible citric acid production method contains more impurities and is easy to cake. The method is stable, feasible, accurate, controllable and stable in quality, the content of citric acid and the impurity removal effect are remarkably improved, the purity of the obtained citric acid productis more than or equal to 99.5%, particularly, the particle size, the chloride content, the sulfate content and the like of the product are greatly improved, and the pharmaceutical grade standard is completely met.

Description

technical field [0001] The invention relates to the technical field of citric acid, in particular to a refining method for preparing high-purity, non-caking fine-grained citric acid crystals. Background technique [0002] Citric acid is colorless translucent crystal, white granule or white crystalline powder; odorless, very sour taste, easily soluble in water and ethanol. Citric acid monohydrate loses water of crystallization in dry air or when heated to about 40°C, and slightly deliquesces in humid air, dilute citric acid aqueous solution can be fermented when standing still. As an organic acid, citric acid has been widely used in food, beverage, medicine and other industries, and its application scope is still expanding. [0003] Citric acid is obtained by fermenting potato, corn and other plant materials with Aspergillus niger. The mature fermented product contains not only the main product citric acid, but also residual sugar, bacteria, protein, pigment, colloidal subst...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C59/265C07C51/42C07C51/43C07C51/47
CPCC07C51/42C07C51/43C07C51/47C07C59/265
Inventor 唐波彭立辉
Owner 湖南新绿方药业有限公司
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