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Preparation method for co-producing high-purity crystalline calcium acetate and anhydrous calcium acetate

A calcium acetate, high-purity technology, applied in the direction of carboxylate preparation, carboxylate preparation, chemical instruments and methods, etc.

Inactive Publication Date: 2015-11-04
TIANJIN GUANGFU TECH DEV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] In view of this, the main purpose of the present invention is to provide a co-production preparation method of high-purity crystalline calcium acetate and anhydrous calcium acetate, which can solve the problem of existing calcium acetate preparation The purity of calcium acetate prepared by the method is relatively low, and the co-production of crystalline calcium acetate and anhydrous calcium acetate cannot be realized

Method used

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Examples

Experimental program
Comparison scheme
Effect test

specific Embodiment approach 1

[0021] Specific embodiment one: a kind of high-purity crystalline calcium acetate and anhydrous calcium acetate co-production preparation method described in this embodiment are realized through the following steps:

[0022] Step 1. Weigh 1~10Kg of heavy calcium carbonate, first add 0.8Kg of heavy calcium carbonate to the reaction vessel, then add 2.8~30L of 20% ethanol, heat and dissolve until no CO2 escapes, and then put the remaining heavy Calcium carbonate was added to the reaction vessel and kept at a constant temperature of 80°C for 20 minutes;

[0023] Step 2. Add a mixed impurity remover to the solution in step 1. The ratio is calcium oxide:ammonia water=1:2~3, keep the pH of the solution between 11~12, and keep it warm for 1~2 hours. The reaction formula is :

[0024] al 3+ + 3OH - → Al(OH) 3

[0025] Mg 2+ + 2OH - → Mg(OH) 2

[0026] Pb 2+ + 2OH - → Pb(OH) 2

[0027] mn 2+ + 2OH - → Mn(OH) 2

[0028] 2F - ...

specific Embodiment approach 2

[0034] Specific embodiment 2: In step 3 of the co-production method of high-purity crystalline calcium acetate and anhydrous calcium acetate described in this embodiment, 80% acetic acid is added at any time during the concentration process, and the acetic acid is 26-30ml in total. Other components and connections are the same as those in the first embodiment.

[0035]

Embodiment 1

[0037] Step 1. Weigh 1Kg of heavy calcium carbonate, first add 0.8Kg of heavy calcium carbonate to the reaction vessel, then add 2.8L of 20% ethanol, heat and dissolve until no CO2 escapes, then add the remaining heavy calcium carbonate In the reaction vessel, keep a constant temperature of 80°C for 20 minutes;

[0038] Step 2, add a mixed impurity remover to the solution in step 1, the ratio is calcium oxide: ammonia water = 1: 3, keep the pH of the solution between 11 and 12, keep the temperature and settle for 1 to 2 hours;

[0039] Step 3, filter the precipitate, collect the filtrate, concentrate at 80-100°C, remove excess ammonia, and concentrate to a specific gravity of 1.28-1.30;

[0040] Step 4, cooling the solution to 60°C, filtering out the precipitate to obtain crystalline calcium acetate monohydrate;

[0041] Step 5: Collect the filtrate in step 4, and continue to concentrate the filtrate until the solution is in the form of a viscous solid to obtain anhydrous cal...

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PUM

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Abstract

The invention provides a preparation method for co-producing high-purity crystalline calcium acetate and anhydrous calcium acetate, aiming to solve the problem that calcium acetate prepared by existing calcium acetate preparation methods has lower purity. The preparation method comprises the following steps: firstly adding 0.8Kg of heavy calcium carbonate to a reaction vessel, then adding 2.8-30L of 20% ethanol, heating to dissolve heavy calcium carbonate until no CO2 escapes, then adding remaining heavy calcium carbonate to the reaction vessel and maintaining the constant temperature of 80 DEG C for 20 minutes; adding a mixed impurity removal agent to the solution and carrying out insulation and precipitation for 1-2 hours; filtering a precipitate, collecting filtrate, concentrating the filtrate at 80-100 DEG C, removing excessive ammonia and concentrating the filtrate until the proportion is 1.18-1.30; cooling the solution to 60 DEG C and filtering out a precipitate, thus obtaining crystalline calcium acetate monohydrate; collecting filtrate and continuously concentrating the filtrate until the solution is a thick solid, thus obtaining anhydrous calcium acetate. The preparation method is used in the field of chemical reagents.

Description

technical field [0001] The invention relates to a method for co-producing high-purity crystalline calcium acetate and anhydrous calcium acetate, belonging to the field of chemical reagents. Background technique [0002] Crystalline calcium acetate is a colorless transparent liquid, anhydrous calcium acetate is a loose fine powder, odorless, slightly bitter taste, easily soluble in water. It is widely used in food and pharmaceutical industries, and can also be used as a 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. 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 impurit...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C53/10C07C51/41C07C51/42C07C51/487
Inventor 赵鹏贾伟青
Owner TIANJIN GUANGFU TECH DEV