Preparation method of high-purity barium carbonate

A high-purity barium carbonate and sodium carbonate technology, which is applied in the preparation/purification of barium carbonate and sulfur, calcium carbonate/strontium/barium, etc., can solve the problem that by-products are not resourced and utilized, are environmentally friendly, consume a lot, and chloride ions are not easy to remove and other issues to achieve maximum value utilization and increase conversion rate

Active Publication Date: 2019-07-12
SICHUAN UNIVERSITY OF SCIENCE AND ENGINEERING
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Problems solved by technology

[0003] At present, there are two main methods for preparing high-purity barium carbonate at home and abroad: one is liquid phase precipitation method, using high-purity soluble barium salt (BaCl 2 , Ba(NO 3 ) 2 etc.) carry out precipitation reaction with carbonate radical in aqueous solution, this method needs to consume a large amount of water, and produces a large amount of waste water, adopts BaCl simultaneously 2 The introduced chloride ions are not easy to remove, and Ba(NO 3 ) 2 The prepared barium carbonate often deteriorates the electrical properties of PTC components; the other is the carbonization method in the solid-phase synthesis method, which uses the oxidation-reduction reaction of coal and barite at high temperature to generate barium sulfide, and then introduces it into the barium sulfide aqueous solution. Carbonate ions are used to prepare barium carbonate. In this method, because the raw coal and barite used in the preparation of barium sulfide are in solid phase, the coal and barite are not in sufficient contact during the reaction process, resulting in low raw material utilization, and the reaction tail gas contains A large amount of carbon dioxide and some unreacted carbon monoxide do not conform to the concept of green environmental protection
[0004] In summary, the use of existing technologies to prepare high-purity barium carbonate has problems such as low conversion rate of raw materials, failure of by-products to be utilized as resources, and environmental protection.

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  • Preparation method of high-purity barium carbonate

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[0028] A preparation method of high-purity barium carbonate, specifically comprising the following steps:

[0029] (1) Pretreatment: crush the barite into a powder with a particle size of less than 50 μm, then wash with alkali, pickle and water, and finally dry to obtain barite powder;

[0030] In this step, alkali washing can effectively remove the alkali-soluble impurities in the barite, acid washing can effectively remove the acid-soluble impurities in the barite, washing with water can effectively remove the barite soluble impurities, and the barite in the barite Barium sulfate is neither soluble in alkali nor acid. It can be washed with alkali first, then pickled, and finally washed with water, or it can be acid washed first, then washed with alkali, and finally washed with water.

[0031] (2) Thermal reduction reaction: Add the barite powder obtained in step (1) into the thermal reduction reactor, and after introducing nitrogen gas to replace the air in the reactor, con...

Embodiment 1

[0053] The barite crushed to a particle size of less than 50 μm is washed sequentially with sodium hydroxide solution, hydrochloric acid solution and deionized water, and then dried at an environment higher than 90 ° C for 24 hours; take 30 g of dried barite powder Put it in the reactor, pass in nitrogen to replace the air in the reactor, continue to pass in nitrogen, raise the temperature to 1400°C, and then pass in the mixed gas of sulfur vapor and nitrogen, the volume ratio of sulfur vapor and nitrogen is 1:4, and the mixture is controlled The gas flow rate is 0.3-0.5L / min, the space time of the mixed gas in the reactor is 4.8-8min, and the crude barium sulfide is produced after 1.5h of reaction; then the crude barium sulfide is dissolved in 1L deionized water, and the barium sulfide is produced after filtering Supernatant liquid, the molar concentration of barium sulfide in the barium sulfide clear liquid obtained by detection and analysis is 0.11mol / L; Get 300ml of barium ...

Embodiment 2

[0055] The barite crushed to a particle size of less than 50 μm is washed sequentially with sodium hydroxide solution, hydrochloric acid solution and deionized water, and then dried at an environment higher than 90°C for 24 hours; take 50g of dried barite powder Put it in the reactor, pass in nitrogen to replace the air in the reactor, continue to pass in nitrogen, raise the temperature to 1200°C, and then pass in the mixed gas of sulfur vapor and nitrogen, the volume ratio of sulfur vapor and nitrogen is 1:5, and the mixture is controlled The gas flow rate is 0.25 ~ 0.4L / min, the space time of the mixed gas in the reactor is 6 ~ 9.6min, and the crude barium sulfide is produced after 1 hour of reaction, then the crude barium sulfide is dissolved in 1L deionized water, and the barium sulfide is produced after filtration Supernatant liquid, the molar concentration of barium sulfide in the barium sulfide clear liquid obtained by detection and analysis is 0.18mol / L; Get 200ml of ba...

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Abstract

The invention discloses a preparation method of high-purity barium carbonate. The preparation method comprises the following steps: (1) crushing barite into powder, carrying out alkali washing, acid washing and water washing, and finally carrying out drying to obtain barite powder; (2) adding the barite powder into a reactor, introducing nitrogen to replace air in the reactor, continuously introducing nitrogen, carrying out heating to 1000-2000 DEG C, then introducing a mixed gas of sulfur vapor and nitrogen into the reactor, carrying out reacting for a period of time, and carrying out coolingto room temperature to obtain crude barium sulfide; (3) dissolving the crude barium sulfide in deionized water, and then carrying out filtering to obtain a barium sulfide clear solution; and (4) under the condition of 0-100 DEG C and a stirring rotating speed of 0-1000 r/min, introducing CO2 gas into the barium sulfide clear solution or slowly adding a sodium carbonate solution to carry out a precipitation reaction to obtain the high-purity barium carbonate. The preparation method disclosed by the invention is high in raw material conversion rate and meets the green production idea, and purity of the prepared barium carbonate is higher than 99.5%.

Description

technical field [0001] The invention relates to the field of chemical industry, in particular to a preparation method of high-purity barium carbonate. Background technique [0002] As an important inorganic industrial raw material, barium carbonate is widely used in coatings, ceramics, optical glass, electronic chemicals and other fields. The high-purity barium carbonate powder material has a wider range of applications, so the preparation method of high-purity barium carbonate is a research hotspot in recent years. [0003] At present, there are two main methods for preparing high-purity barium carbonate at home and abroad: one is liquid phase precipitation method, using high-purity soluble barium salt (BaCl 2 , Ba(NO 3 ) 2 etc.) carry out precipitation reaction with carbonate radical in aqueous solution, this method needs to consume a large amount of water, and produces a large amount of waste water, adopts BaCl simultaneously 2 The introduced chloride ions are not eas...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01F11/18C01B17/74C01B17/22C01B17/04
CPCC01B17/04C01B17/22C01B17/74C01F11/188C01P2004/61C01P2006/80
Inventor 张峰榛张孝果张伟汤秀华杨虎
Owner SICHUAN UNIVERSITY OF SCIENCE AND ENGINEERING
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