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Preparation method of high-purity vaterite type calcium carbonate microspheres

A technology of vaterite and calcium carbonate, applied in the direction of calcium carbonate/strontium/barium, etc., can solve the problems of adding crystal form control agent, complicated preparation process and high cost of raw materials, and achieves low dosage, low preparation cost and low equipment investment. Effect

Pending Publication Date: 2020-10-16
SOUTHWEAT UNIV OF SCI & TECH
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  • Abstract
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  • Claims
  • Application Information

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Problems solved by technology

[0006] In summary, the existing vaterite type calcium carbonate microsphere preparation process has problems such as high raw material cost, complex preparation process, and the need to add a crystal form control agent, so the present invention is aimed at the above preparation method of vaterite type calcium carbonate microsphere Deficiency Invented a new method for preparing high-purity vaterite-type calcium carbonate microspheres at low temperature and normal pressure without adding a crystal form control agent as raw material of calcium sulfate

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  • Preparation method of high-purity vaterite type calcium carbonate microspheres
  • Preparation method of high-purity vaterite type calcium carbonate microspheres

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preparation example Construction

[0021] A preparation method of high-purity vaterite type calcium carbonate microspheres of the present invention comprises the following steps.

[0022] 1) Grinding the calcium sulfate raw material to obtain calcium sulfate powder with an average particle size of 60-180 mesh.

[0023] Wherein, the calcium sulfate raw material described in the above step 1) is mainly natural gypsum, gypsum tailings and industrial by-product gypsum, etc.

[0024] 2) Mix the calcium sulfate powder obtained in step 1) with the leaching aid, place in a stirred reaction vessel, and react for 30-120 minutes under normal pressure and 30-120 °C to obtain the reaction product.

[0025] Wherein, the leaching aid in step 2) is one or more of ammonium acetate, ammonium chloride and ammonium sulfate; the concentration of the leaching aid is 2-12 mol / L; the amount of the leaching aid is 5-20 mL / g.

[0026] 3) Suction filter, wash, and dry the reaction product obtained in step 2) to obtain a filtrate rich i...

example 1

[0033] The calcium sulfate raw material in the present embodiment selects phosphogypsum, and the main chemical composition of phosphogypsum is, by weight percentage: SO 3 38%, CaO32%, SiO 2 7%, other 23%; the specific process is as follows:

[0034] 1) Take 50g of the above-mentioned phosphogypsum powder, prepare 650 mL of 9.5 mol / L ammonium chloride solution, then pour the phosphogypsum powder into the ammonium chloride solution, stir and react at 90°C for 110 min, and suction filter after the reaction is completed Obtain filtrate and solid reactant;

[0035] 2) Take 500 mL of the above filtrate, add 29.4 g of calcium chloride powder and 45 mL of ammonia water to the solution, and pass through CO 2 gas, stirred at 85 °C for 95 min, CO 2 The flow rate is 210 mL / min, and the stirring speed is 400 r / min; after the reaction is completed, stop feeding CO 2 gas, the reaction product is suction filtered, washed and dried to obtain the calcium carbonate microsphere product;

[0...

example 2

[0038] Calcium sulfate raw material in the present embodiment selects gypsum tailings for use, and the main chemical composition of gypsum tailings is, by weight percentage: SO 3 24%, CaO20%, SiO 2 23%, Al 2 o 3 6%, Fe 2 o 3 3%, other 24%; the specific process is as follows:

[0039] 1) Take 20 g of the above gypsum tailings powder, prepare 240 mL of 4.5 mol / L ammonium acetate solution, then pour the gypsum tailings powder into the ammonium acetate solution, stir and react at 75 °C for 55 min, and suction filter after the reaction is completed Obtain filtrate and solid reactant;

[0040] 2) Take 200 mL of the above filtrate, add 3.6 g of calcium chloride powder and 18 mL of ammonia water to the solution, and pass in CO 2 gas, stirred the reaction at 55 °C for 70 min, CO 2 The flow rate was 85 mL / min, and the stirring speed was 250 r / min; after the reaction was completed, stop feeding CO 2 gas, the reaction product is suction filtered, washed and dried to obtain the cal...

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Abstract

The invention relates to a method for preparing high-purity vaterite type calcium carbonate microspheres from a calcium sulfate raw material. The method comprises the following steps of: 1) grinding the calcium sulfate raw material to obtain a powder raw material; 2) proportioning the powder raw material obtained in the step 1) and a leaching aid, putting the mixture into a reaction container witha stirring function for reaction, and carrying out solid-liquid separation on a reaction product after the reaction is finished so as to obtain filtrate rich in calcium ions and a solid product; and3) burdening the filtrate obtained in the step 2) and ammonia water, introducing CO2 gas, carrying out reaction in a reaction container with a stirring function, controlling process conditions to obtain the high-purity vaterite type calcium carbonate microspheres, and further recycling the filtrate for leaching the calcium sulfate raw material. The calcium carbonate microsphere material is non-toxic, safe and fine in particles, has the characteristics of high whiteness, good fluidity and the like, and can be applied to the industries of rubber, plastics, chemical engineering and the like.

Description

technical field [0001] The invention relates to a method for preparing high-purity vaterite-type calcium carbonate microspheres, in particular to a method for preparing high-purity vaterite-type calcium carbonate microspheres from calcium sulfate raw materials without adding a crystal form control agent, and belongs to the field of inorganic functional materials and chemical materials. Background technique [0002] Calcium carbonate is an important inorganic chemical filler, which is widely used in rubber, plastics, coatings, paper, ink, sealant and other industries, and can also be used in toothpaste, food, medicine, building materials, chemical industry and other industries. Calcium carbonate has three crystal forms: calcite, aragonite and vaterite, among which calcite has the most stable structure, followed by aragonite, and vaterite is the most unstable. [0003] Compared with ordinary calcium carbonate, spherical calcium carbonate has special properties such as large su...

Claims

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Application Information

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IPC IPC(8): C01F11/18
CPCC01F11/18C01P2004/32C01P2004/61C01P2004/62C01P2006/80C01P2002/72C01P2004/03
Inventor 丁文金陈秋菊孙红娟彭同江
Owner SOUTHWEAT UNIV OF SCI & TECH
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