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Method for combined production of high purity crystalline calcium acetate and waterless calcium acetate

A calcium acetate, high-purity technology, applied in the fields of food, chemical industry, chemical reagents, and medicine, can solve the problem that it is difficult to produce high-purity calcium acetate and calcium hydroxide with high impurity content, and achieve increased yield, thorough impurity removal, The effect of the method is simple and easy

Inactive Publication Date: 2016-05-11
TIANJIN GUANGFU TECH DEV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] At present, there are two domestic production methods of calcium acetate, one is through the reaction of calcium carbonate and acetic acid, and the other is prepared by the reaction of calcium hydroxide and acetic acid. Due to the high impurity content of calcium hydroxide, it cannot be used as a high-purity product. The raw material of calcium acetate, calcium carbonate is used as raw material, and it is difficult to produce high-purity calcium acetate by general methods

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0025] A co-production method of high-purity crystalline calcium acetate and anhydrous calcium acetate, the steps are as follows:

[0026] (1) Weigh 1Kg of heavy calcium carbonate, then add 2.8L of 20wt% acetic acid, heat and dissolve until no CO 2 Escape, keep the temperature at 80°C for 20min;

[0027] (2) In the above solution, add a mixed impurity remover, the ratio of which is = 1:3, so that the pH is between 11-12, heat preservation and sedimentation for 1-2 hours, so that impurities are precipitated as hydroxides;

[0028] al 3+ +3OH - →Al(OH) 3

[0029] Mg 2+ +2OH - →Mg(OH) 2

[0030] Pb 2+ +2OH - →Pb(OH) 2

[0031] mn 2+ +2OH - →Mn(OH) 2

[0032] 2F - +Ca 2+ →CaF 2

[0033] SiO 3- +Ca 2+ →C a SiO 3

[0034] (3) Filtrate the precipitate, collect the filtrate, concentrate at 80-100°C, when concentrated to a specific gravity of 1.28-1.30g / cm3, cool to 60°C, filter out the precipitate to obtain monohydrate crystalline calcium acetate, dry at 60-70...

Embodiment 2

[0037] A co-production method of high-purity crystalline calcium acetate and anhydrous calcium acetate, the steps are as follows:

[0038] (1) Weigh 10Kg of heavy calcium carbonate, slowly add 20% acetic acid (30 liters), heat and stir at 80°C for about 30min

[0039] (2) In the above solution, add mixed impurity remover = 1:2, keep warm and settle for 1 hour, and filter;

[0040] (3) Concentrate the filtrate at 80°C. When the specific gravity is 1.18-1.28g / cm3, add 300-320ml of acetic acid, and a precipitate will precipitate out. Cool to 60-70°C, filter out the precipitate, and dry at 60-70°C to obtain a Hydrated crystalline calcium acetate, yield 55%;

[0041] (4) Collect the filtrate, continue to concentrate (80°C) until the solution is basically dry, and then discharge to obtain anhydrous calcium acetate with a yield of 45%

Embodiment 3

[0043] A co-production method of high-purity crystalline calcium acetate and anhydrous calcium acetate, the steps are as follows:

[0044] (1) Slowly add 1Kg of heavy calcium carbonate to 1L of 80% glacial acetic acid to make a suspension;

[0045] (2) Add 1Kg of glacial acetic acid in portions and stir until CO 2 escape completely;

[0046] (3) Add a mixed impurity remover to the solution, filter, concentrate the filtrate to a viscous shape, collect the precipitate at 80°C to obtain anhydrous calcium acetate, and the yield is 78%;

[0047] (4) Collect the filtrate, concentrate to a specific gravity of 1.3-1.4, cool at 20°C, precipitate crystals, filter the crystals, and dry naturally to obtain crystalline calcium acetate trihydrate with a yield of 15%.

[0048] Table 1 Solubility Product Difference Between Impurities and Calcium Hydroxide

[0049] KspAl(OH) 3

[0050] KspC 2

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PUM

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Abstract

The invention relates to a method for combined production of high purity crystalline calcium acetate and waterless calcium acetate. The method comprises 1, weighing heavy calcium carbonate, adding acetic acid into the heavy calcium carbonate, heating and dissolving the mixture until CO2 is not escaped, and keeping a temperature of 80 DEG C for 20min, 2, adding a mixed impurity removal agent into the solution according to a ratio of 1: 2-3, controlling pH in a range of 11-12 and carrying out thermal insulation and sedimentation for 1-2h so that the impurities are precipitated in a form of hydroxides, 3, filtering the precipitates, collecting the filtrate, concentrating the filtrate at a temperature of 80-100 DEG C until a concentrating proportion of 1.18-1.30g / cm<3>, carrying out cooling to a temperature of 60 DEG C, filtering the precipitates to obtain a crystalline calcium acetate monohydrate and carrying out drying at a temperature of 60-70 DEG C, and 4, collecting the filtrate, carrying out concentration until the solution is in a viscous solid form so that waterless calcium acetate is obtained, and carrying out drying at a temperature of 90 DEG C. Through use of the mixed impurity removal agent, impurity removal is thorough and all calcium acetate can be produced. The method improves a yield, realizes zero discharge and realizes eco-friendly production.

Description

technical field [0001] The invention belongs to the fields of chemical industry, food, medicine and chemical reagents, in particular to a co-production method of high-purity crystalline calcium acetate and anhydrous calcium acetate. technical background [0002] Crystalline calcium acetate is colorless transparent liquid, anhydrous calcium acetate loose fine powder, odorless, slightly bitter taste, easily soluble in water. Widely used in food, pharmaceutical industry and chemical reagents, used as mildew inhibitor, buffer, flavor enhancer, preservative, nutritional enhancer and processing aid. Calcium acetate is an ideal calcium supplement with a high absorption rate in the human body, and can be used to treat phosphate conjugates with excessive blood phosphate. [0003] At present, there are two domestic production methods of calcium acetate, one is through the reaction of calcium carbonate and acetic acid, and the other is prepared by the reaction of calcium hydroxide and...

Claims

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Application Information

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IPC IPC(8): C07C53/10C07C51/41
Inventor 赵鹏贾伟青
Owner TIANJIN GUANGFU TECH DEV
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