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CN-121990600-A - Preparation method of high-purity barium carbonate

CN121990600ACN 121990600 ACN121990600 ACN 121990600ACN-121990600-A

Abstract

The invention belongs to the technical field of inorganic materials, and particularly relates to a preparation method of high-purity barium carbonate. The invention adopts a barium chloride solution and an ammonium bicarbonate solution to prepare high-purity barium carbonate by a coprecipitation method, adds a crystal form control agent into the barium chloride solution in advance, adds a surfactant into the ammonium bicarbonate solution to enable an auxiliary agent to be adsorbed on potential crystal nucleus sites in advance, reduces the interfacial tension of a liquid phase, ensures the uniformity of a barium carbonate precipitation reaction, adopts hyperbranched polycarboxylic acid and tartaric acid to compound the crystal form control agent, adopts polyacrylic acid and citric acid to compound the crystal form control agent, adopts a compound dispersion system, and controls the pH value in the reaction process to enable the prepared barium carbonate to have higher purity, sphericity and narrower particle size distribution.

Inventors

  • JIA DAOFENG
  • CHANG GUANGXI
  • ZHOU ZHENGMING

Assignees

  • 青岛红蝶新材料有限公司

Dates

Publication Date
20260508
Application Date
20260123

Claims (10)

  1. 1. The preparation method of the high-purity barium carbonate is characterized by comprising the following steps of: s1, dissolving high-purity barium chloride in deionized water to prepare a solution with the concentration of 0.5-1.0mol/L, adding a crystal form control agent, and filtering to obtain a barium chloride solution; S2, dissolving ammonium bicarbonate in deionized water to prepare a solution with the concentration of 0.5-1.0mol/L, adding a surfactant, and filtering to obtain an ammonium bicarbonate solution; S3, dissolving the composite dispersing agent in deionized water to prepare an aqueous solution with the mass percent of 1% -5% so as to obtain a composite dispersing agent solution; S4, adding deionized water into a reaction kettle, adding the composite dispersing agent solution prepared in the step S3, adding ammonia water under stirring to adjust the pH value of a reaction system to 9.8-10.2, heating to 25-35 ℃, simultaneously adding the barium chloride solution prepared in the step S1 and the ammonium bicarbonate solution prepared in the step S2 to react for 1-2h, keeping the pH value of the reaction system in the reaction process to 9.8-10.2, aging, filtering, washing, drying and crushing to obtain high-purity barium carbonate; The crystal form control agent consists of hyperbranched polycarboxylic acid and tartaric acid according to the mass ratio of (8-11) to (3-5).
  2. 2. The preparation method of the high-purity barium carbonate according to claim 1, wherein the preparation method of the hyperbranched polycarboxylic acid is characterized in that maleic anhydride and propylene glycol are put into a reaction kettle according to a molar ratio of 1:1, heated to 60-70 ℃ for reaction for 2-3 hours under the protection of nitrogen to obtain an active monomer, maleic anhydride and benzoyl peroxide are continuously added, ethylene glycol diethyl ether is added after stirring for 15-20min, heated to 80-85 ℃ for stirring for reaction for 6-8 hours, and reduced pressure distillation is carried out to obtain the hyperbranched polycarboxylic acid.
  3. 3. The method for preparing high-purity barium carbonate according to claim 2, wherein the mass of the continuously added maleic anhydride in the method for preparing hyperbranched polycarboxylic acid is 2-3 times of the mass of the active monomer, the mass of benzoyl peroxide is 3% -5% of the mass of the active monomer, and the mass of ethylene glycol diethyl ether is 5-8 times of the mass of the active monomer.
  4. 4. The method for preparing high-purity barium carbonate according to claim 1, wherein the crystal form control agent consists of hyperbranched polycarboxylic acid and tartaric acid according to a mass ratio of 9:4.
  5. 5. The method for preparing high purity barium carbonate according to claim 1, wherein the addition amount of the crystal form control agent in step S1 is 4% -7% of the mass of the barium chloride solution.
  6. 6. The method for preparing high-purity barium carbonate according to claim 1, wherein the addition amount of the surfactant in the step S2 is 0.2% -0.4% of the mass of the ammonium bicarbonate solution, and the surfactant is a nonionic surfactant.
  7. 7. The method for preparing high purity barium carbonate according to claim 6, wherein the surfactant is one of polysorbate, sorbitan fatty acid and alkyl polyglucoside.
  8. 8. The method for preparing high purity barium carbonate according to claim 1, wherein the composite dispersant in step S3 is composed of polyacrylic acid and citric acid in a mass ratio of (1-5): 1.
  9. 9. The method for preparing high purity barium carbonate according to claim 1, wherein the amount of the complex dispersant solution in step S4 is 0.4% -1% of the theoretical barium carbonate mass.
  10. 10. The method for preparing high purity barium carbonate according to claim 1, wherein the flow rates of the barium chloride solution and the ammonium bicarbonate solution in step S4 are set according to the molar ratio of 1 (1.1-1.4) of barium chloride to ammonium bicarbonate.

Description

Preparation method of high-purity barium carbonate Technical Field The invention belongs to the technical field of inorganic materials, and particularly relates to a preparation method of high-purity barium carbonate. Background The high-purity barium carbonate is used as a key inorganic fine chemical material, and takes up an irreplaceable position in the high-end manufacturing fields of electronic information, optical glass, new energy sources and the like by virtue of the excellent chemical stability and physical properties of the high-purity barium carbonate. The core application scene of the material comprises liquid crystal substrate glass, electronic ceramics, solid battery electrolyte precursors, high refractive index optical materials and the like, can obviously improve the transmittance, the electricity storage performance and the structural stability of downstream products, and is an important basic raw material for supporting the upgrade of strategic emerging industries. The nano barium carbonate has better performance than the common barium carbonate, and the nano technology is gradually rising, and based on the unique structure, the nano material has the advantages of surface effect, quantum size effect, small size effect and the like, so that compared with a large-scale material, the nano barium carbonate has the advantages of high magnetic conductivity, low loss, saturation magnetization and the like. The main method for industrial production of barium carbonate at present is a liquid phase method by using soluble barium salt and carbonate to react, and the method has the advantages of easily available raw materials, simple process, low production cost and the like. However, in practical production, the method also exposes one side of the defect that the particle size of the barium carbonate crystal cannot be effectively controlled, the quality is not stable enough, the impurity content of the product is high, especially the impurity content of chlorine, sodium, potassium, calcium, iron, sulfur and the like is high, certain special requirements of the microelectronics industry cannot be met, the particle size of the nano barium carbonate cannot be effectively controlled in the preparation process, and in addition, the specific surface area of the obtained nano barium carbonate product cannot meet the current increasingly miniaturized electronic device manufacturing requirements. The Chinese patent application publication No. CN110002485A discloses a preparation method of high-purity barium carbonate, which comprises (1) crushing barite into powder, then carrying out alkali washing, acid washing and water washing, finally drying to obtain barite powder, (2) adding the barite powder into a reactor, introducing nitrogen to replace air in the reactor, continuously introducing nitrogen, heating to 1000-2000 ℃, introducing mixed gas of sulfur vapor and nitrogen into the reactor, reacting for a period of time, cooling to room temperature to obtain coarse barium sulfide, (3) dissolving the coarse barium sulfide into deionized water, filtering to obtain barium sulfide clear liquid, and (4) introducing CO 2 gas into the barium sulfide clear liquid or slowly adding sodium carbonate solution to carry out precipitation reaction under the conditions of 0-100 ℃ and stirring rotation speed of 0-1000r/min to obtain the high-purity barium carbonate. Although the barium carbonate prepared by the method has higher purity (> 99.5%), barium sulfide particles are sintered and agglomerated to form blocks or large-size aggregates under a high-temperature environment, and even though the barium sulfide particles are subjected to a dissolution and filtration process, incompletely dispersed agglomerated cores still possibly remain, and in a precipitation reaction, the cores become crystal nucleus growth base points, large-particle impurities are induced, and dispersing agents, crystal nucleus inhibitors, crystal form regulators and the like are not added in the process, so that the prepared barium carbonate particles have large particle size span, irregular morphology and lack of spherical regulation capability. Disclosure of Invention The invention aims to solve the technical problems of uneven particle size distribution, low purity, poor sphericity and the like in the prior art, and provides a preparation method of high-purity barium carbonate. In order to achieve the above object, the technical scheme of the present invention is as follows: The preparation method of the high-purity barium carbonate comprises the following steps: s1, dissolving high-purity barium chloride in deionized water to prepare a solution with the concentration of 0.5-1.0mol/L, adding a crystal form control agent, and filtering to obtain a barium chloride solution; S2, dissolving ammonium bicarbonate in deionized water to prepare a solution with the concentration of 0.5-1.0mol/L, adding a surfactant, and filtering to obtain an ammonium bicarbo