CN110002485B - Preparation method of high-purity barium carbonate - Google Patents

Preparation method of high-purity barium carbonate Download PDF

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CN110002485B
CN110002485B CN201910380497.7A CN201910380497A CN110002485B CN 110002485 B CN110002485 B CN 110002485B CN 201910380497 A CN201910380497 A CN 201910380497A CN 110002485 B CN110002485 B CN 110002485B
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barium
sulfide
barium sulfide
solution
gas
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CN110002485A (en
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张峰榛
张孝果
张伟
汤秀华
杨虎
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Sichuan University of Science and Engineering
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    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B17/00—Sulfur; Compounds thereof
    • C01B17/02—Preparation of sulfur; Purification
    • C01B17/04—Preparation of sulfur; Purification from gaseous sulfur compounds including gaseous sulfides
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B17/00—Sulfur; Compounds thereof
    • C01B17/22—Alkali metal sulfides or polysulfides
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B17/00—Sulfur; Compounds thereof
    • C01B17/69—Sulfur trioxide; Sulfuric acid
    • C01B17/74—Preparation
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01F—COMPOUNDS OF THE METALS BERYLLIUM, MAGNESIUM, ALUMINIUM, CALCIUM, STRONTIUM, BARIUM, RADIUM, THORIUM, OR OF THE RARE-EARTH METALS
    • C01F11/00—Compounds of calcium, strontium, or barium
    • C01F11/18—Carbonates
    • C01F11/186—Strontium or barium carbonate
    • C01F11/188—Barium carbonate
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2004/00—Particle morphology
    • C01P2004/60—Particles characterised by their size
    • C01P2004/61—Micrometer sized, i.e. from 1-100 micrometer
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2006/00—Physical properties of inorganic compounds
    • C01P2006/80—Compositional purity

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Inorganic Chemistry (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Geology (AREA)
  • Compounds Of Alkaline-Earth Elements, Aluminum Or Rare-Earth Metals (AREA)

Abstract

The invention discloses a preparation method of high-purity barium carbonate, which comprises the following steps: (1) crushing barite into powder, then carrying out alkali washing, acid washing and water washing, and finally drying to obtain barite powder; (2) adding barite powder into a reactor, introducing nitrogen to replace air in the reactor, continuously introducing nitrogen, heating to 1000-2000 ℃, introducing a mixed gas of sulfur vapor and nitrogen into the reactor, reacting for a period of time, and cooling to room temperature to obtain crude barium sulfide; (3) dissolving crude barium sulfide in deionized water, and filtering to obtain a barium sulfide clear solution; (4) introducing CO into the barium sulfide clear liquid at the temperature of 0-100 ℃ and the stirring speed of 0-1000 r/min2And gas or slowly adding a sodium carbonate solution to perform precipitation reaction to obtain the high-purity barium carbonate. The method has high conversion rate of raw materials, accords with the green production concept, and the purity of the prepared barium carbonate is more than 99.5 percent.

Description

Preparation method of high-purity barium carbonate
Technical Field
The invention relates to the field of chemical industry, in particular to a preparation method of high-purity barium carbonate.
Background
Barium carbonate is widely used in the fields of coatings, ceramics, optical glass, electronic chemical industry and the like as an important inorganic industrial raw material. The high-purity barium carbonate powder material has a wider application range, so that the preparation method of the high-purity barium carbonate is a research hotspot in recent years.
At present, the main methods for preparing high-purity barium carbonate at home and abroad are two: one is a liquid phase precipitation method, using high purity soluble barium salt (BaCl)2、Ba(NO3)2Etc.) in an aqueous solution with carbonate, which requires consumption of a large amount of water and generation of a large amount of waste water, while using BaCl2The introduced chloride ions are not easy to remove, and Ba (NO) is adopted3)2The prepared barium carbonate often deteriorates the electrical properties of the PTC element; the other is a carbonization method in the solid-phase synthesis method, which utilizes the oxidation and reduction of coal and barite at high temperatureAfter barium sulfide is generated by an original reaction, carbonate ions are introduced into a barium sulfide aqueous solution to prepare barium carbonate, and the method has the advantages that raw materials for preparing barium sulfide, namely coal and barite, are solid phases, so that the coal and the barite are not fully contacted in the reaction process, the utilization rate of the raw materials is low, and reaction tail gas contains a large amount of carbon dioxide and part of unreacted carbon monoxide, so that the method does not accord with the green environmental protection concept.
In conclusion, the high-purity barium carbonate prepared by the prior art has the problems of low conversion rate of raw materials, no resource utilization of byproducts, environmental protection and the like.
Disclosure of Invention
Aiming at the defects in the prior art, the invention aims to provide the preparation method of the high-purity barium carbonate, which has high conversion rate of raw materials, can realize the maximum value utilization of the raw materials, can realize the resource utilization of byproducts, and is green and environment-friendly.
The technical scheme of the invention is realized as follows:
a preparation method of high-purity barium carbonate specifically comprises the following steps:
(1) pretreatment: crushing barite into powder with the particle size of less than 50 mu m, then carrying out alkali washing, acid washing and water washing, and finally drying to obtain barite powder;
(2) thermal reduction reaction: adding the barite powder obtained in the step (1) into a thermal reduction reactor, introducing nitrogen to replace air in the reactor, continuously introducing nitrogen, heating to 1000-2000 ℃, introducing a mixed gas of sulfur vapor and nitrogen into the reactor, reacting for a period of time, cooling to room temperature to obtain crude barium sulfide, and collecting to obtain a gas containing a large amount of sulfur dioxide and a small amount of sulfur vapor;
(3) preparing a barium sulfide clear solution: dissolving the crude barium sulfide obtained in the step (2) in deionized water, and then filtering to obtain a barium sulfide clear solution;
(4) preparing high-purity barium carbonate: introducing CO into the barium sulfide clear liquid prepared in the step (3) at the temperature of 0-100 ℃ and the stirring speed of 0-1000 r/min2Gas or slowly adding sodium carbonate solution to perform precipitation reaction, and then performing solid-liquid separation, thereby obtainingAnd washing and drying the solid to obtain the high-purity barium carbonate.
Further, the alkali used in the step (1) is any one of a sodium hydroxide solution or a potassium hydroxide solution, and the acid used is a hydrochloric acid solution.
Further, in the step (2), the molar ratio of the barite powder to the sulfur vapor is 1: 2-10; the sulfur vapor in the mixed gas accounts for 5-95% of the total volume of the mixed gas, the flow of the mixed gas is controlled to be 0.1-2.5L/min, and the total reaction time is 0.5-2 h.
Furthermore, the sulfur vapor in the mixed gas accounts for 10-30% of the total volume of the mixed gas.
Further, the sulfur dioxide gas collected in step (2) is used for preparing sulfuric acid.
Further, in the step (3), the mass ratio of the crude barium sulfide to the deionized water is 5-500: 1000.
further, Ba in the clear barium sulfide solution in the step (4)2+With CO in sodium carbonate solution3 2-In a molar ratio of 1: 1; the molar concentration of the sodium carbonate solution is 0.05-0.5 mol/L.
Further, Ba in the clear barium sulfide solution in the step (4)2+With CO2The molar ratio of (A) to (B) is: 1: 0.8 to 1, control of CO2The gas flow rate of (1-10L/h).
And (3) further, carrying out precipitation reaction on sodium carbonate and the barium sulfide clear solution in the step (4), evaporating and concentrating the liquid obtained by solid-liquid separation to obtain a byproduct sodium sulfide, and circulating the condensed water obtained by evaporation to the step (3) for dissolving crude barium sulfide.
Further, CO in step (4)2Carrying out precipitation reaction on the gas and the barium sulfide clear solution to obtain hydrogen sulfide gas, reacting the hydrogen sulfide gas with part of sulfur dioxide collected in the step (2) to recover elemental sulfur, and then preparing sulfur vapor; and (4) directly reusing the liquid obtained by solid-liquid separation in the step (3) for dissolving the crude barium sulfide.
Compared with the prior art, the invention has the following beneficial effects:
1. barite and sulfur vapor are used as raw materials to prepare barium sulfide, the barite is a solid phase, and the sulfur vapor is a gas phase, so that the barite and the sulfur vapor are in full contact and full reaction, and the conversion rate of barium sulfate can be effectively improved.
2. Sulfur dioxide which is a product of the thermal reduction reaction can be directly used for preparing sulfuric acid, sodium sulfide solution generated by precipitation reaction of sodium carbonate and barium sulfide clear solution is evaporated and concentrated to obtain a sodium sulfide byproduct, and evaporated condensate water can be reused for dissolving crude barium sulfide; CO 22Hydrogen sulfide generated by precipitation reaction with the barium sulfide clear solution and part of sulfur dioxide generated by thermal reduction reaction are used for preparing elemental sulfur, so that the recovery of sulfur is realized, and the filtrate after solid-liquid separation can be reused for dissolving crude barium sulfide. Therefore, the reaction product of the whole process is recycled, and the maximum value utilization of the raw material is realized.
3. The barium carbonate prepared by the invention is a rod-shaped crystal with the diameter of about 1 mu m, the purity of the barium carbonate is more than 99.5 percent, and the barium carbonate is a high-purity barium carbonate product.
Drawings
Figure 1-process flow diagram of the route of the sodium carbonate according to the invention.
FIG. 2-CO of the invention2Process flow diagram of the route.
FIG. 3 scanning electron micrograph of high purity barium carbonate prepared in example 1.
Detailed Description
A preparation method of high-purity barium carbonate specifically comprises the following steps:
(1) pretreatment: crushing barite into powder with the particle size of less than 50 mu m, then carrying out alkali washing, acid washing and water washing, and finally drying to obtain barite powder;
in the step, alkali-soluble impurities in the barite can be effectively removed by alkali washing, acid-soluble impurities in the barite can be effectively removed by acid washing, the soluble impurities in the barite can be effectively removed by water washing, and barium sulfate in the barite is not dissolved in alkali nor acid. The alkali washing, the acid washing and the water washing can be carried out firstly, or the acid washing, the alkali washing and the water washing can be carried out firstly.
(2) Thermal reduction reaction: adding the barite powder obtained in the step (1) into a thermal reduction reactor, introducing nitrogen to replace air in the reactor, continuously introducing nitrogen, heating to 1000-2000 ℃, introducing a mixed gas of sulfur vapor and nitrogen into the reactor, reacting for a period of time, cooling to room temperature to obtain crude barium sulfide, and collecting a gas containing a large amount of sulfur dioxide and a small amount of sulfur vapor;
the reaction formula for this step is as follows:
BaSO4+2S＝BaS+2SO2
(3) preparing a barium sulfide clear solution: dissolving the crude barium sulfide obtained in the step (2) in deionized water, and then filtering to obtain a barium sulfide clear solution;
(4) preparing high-purity barium carbonate: introducing CO into the barium sulfide clear liquid prepared in the step (3) at the temperature of 0-100 ℃ and the stirring speed of 0-1000 r/min2And (3) gas or slowly adding a sodium carbonate solution for precipitation reaction, then carrying out solid-liquid separation, and washing and drying the solid to obtain the high-purity barium carbonate.
The solid-liquid separation in the step can be either centrifugal separation or filtration, and the reaction formula of the step is as follows:
BaS+CO2+H2O＝BaCO3↓+H2S
or BaS + Na2CO3＝BaCO3↓+Na2S
Wherein, the alkali adopted in the step (1) is any one of sodium hydroxide solution or potassium hydroxide solution, and the acid adopted is hydrochloric acid solution. Because the cost of potassium hydroxide is high, sodium hydroxide is preferred in order to save production cost.
Optimally, in the step (2), the temperature is raised to 1200-1500 ℃, the conversion rate of barium sulfate is low when the temperature is too low, and the energy consumption is high when the temperature is too high.
In the step (2), the molar ratio of the barite powder to the sulfur vapor is 1: 2-10; the sulfur vapor in the mixed gas accounts for 5-95% of the total volume of the mixed gas, the flow of the mixed gas is controlled to be 0.1-2.5L/min, and the total reaction time is 0.5-2 h.
Optimally, the sulfur vapor in the mixed gas accounts for 10-30% of the total volume of the mixed gas. Because too low a sulfur vapor fraction results in insufficient contact of the sulfur vapor with barium sulfate, the conversion of barium sulfate is low; too high sulfur vapor in turn results in lower sulfur vapor conversion, resulting in lower sulfur vapor utilization.
Wherein, the sulfur dioxide gas in the gas collected in the step (2) is used for preparing sulfuric acid. Therefore, the sulfur dioxide is recycled, and the pollution to the environment is reduced.
Wherein the mass ratio of the crude barium sulfide to the deionized water in the step (3) is 5-500: 1000.
wherein Ba in the barium sulfide clear liquid in the step (4)2+With CO in sodium carbonate solution3 2-In a molar ratio of 1: 1; the molar concentration of the sodium carbonate solution is 0.05-0.5 mol/L.
Wherein Ba in the barium sulfide clear liquid in the step (4)2+With CO2The molar ratio of (A) to (B) is: 1: 0.8 to 1, control of CO2The gas flow rate of (1-10L/h).
And (3) performing precipitation reaction on the sodium carbonate and the barium sulfide clear solution in the step (4), performing solid-liquid separation on the obtained liquid, evaporating and concentrating the obtained liquid to obtain a byproduct sodium sulfide, and circulating the evaporated condensed water to the step (3) for dissolving crude barium sulfide.
Wherein, in the step (4), CO2Carrying out precipitation reaction on the gas and the barium sulfide clear solution to obtain hydrogen sulfide gas, reacting the hydrogen sulfide gas with part of sulfur dioxide collected in the step (2) to recover elemental sulfur, and then preparing sulfur vapor; and (4) directly reusing the liquid obtained by solid-liquid separation in the step (3) for dissolving the crude barium sulfide.
The invention adopts barite and sulfur vapor as raw materials to prepare barium sulfide, and then the barium sulfide is mixed with sodium carbonate or CO2The technological process flow charts of the preparation of barium carbonate by the precipitation reaction are respectively shown in figure 1 and figure 2.
The present invention will be described in further detail with reference to the accompanying drawings and specific embodiments.
The space time in the following examples is the ratio of the reactor volume to the inlet flow of the mixed gas.
Example 1
Pulverizing to particle size smaller thanSequentially washing 50 mu m barite by a sodium hydroxide solution, a hydrochloric acid solution and deionized water, and drying for 24 hours in an environment at the temperature higher than 90 ℃; placing 30g of dried barite powder in a reactor, introducing nitrogen to replace air in the reactor, continuously introducing nitrogen, heating to 1400 ℃, then introducing a mixed gas of sulfur vapor and nitrogen, wherein the volume ratio of the sulfur vapor to the nitrogen is 1:4, the flow rate of the mixed gas is controlled to be 0.3-0.5L/min, the space time of the mixed gas in the reactor is 4.8-8 min, and reacting for 1.5h to obtain crude barium sulfide; dissolving the crude barium sulfide in 1L of deionized water, filtering to obtain a barium sulfide clear solution, and detecting and analyzing to obtain the barium sulfide molar concentration of 0.11mol/L in the barium sulfide clear solution; pouring 300mL of clear barium sulfide liquid into a crystallizer, slowly adding 330mL of sodium carbonate solution with the concentration of 0.1mol/L under the conditions of 25 ℃ and 300rad/min stirring speed, then obtaining solid and clear liquid through centrifugal separation, washing the separated solid with deionized water, and drying for 24 hours at 100 ℃ to obtain the high-purity barium carbonate. The filtrate is evaporated and concentrated under reduced pressure to obtain a by-product Na2And S, evaporating and concentrating the collected condensed water for dissolving the crude barium sulfide. The high purity barium carbonate thus prepared was analyzed to have a purity of 99.6%, and it was needle-shaped crystals having a diameter of about 1 μm, as shown in FIG. 3.
Example 2
Sequentially washing barite crushed to the particle size of less than 50 mu m by a sodium hydroxide solution, a hydrochloric acid solution and deionized water, and drying for 24 hours in an environment at the temperature of higher than 90 ℃; placing 50g of dried barite powder in a reactor, introducing nitrogen to replace air in the reactor, continuously introducing nitrogen, heating to 1200 ℃, then introducing a mixed gas of sulfur vapor and nitrogen, wherein the volume ratio of the sulfur vapor to the nitrogen is 1:5, controlling the flow of the mixed gas to be 0.25-0.4L/min, reacting the mixed gas in the reactor for 1h for 6-9.6 min to obtain crude barium sulfide, dissolving the crude barium sulfide in 1L of deionized water, filtering to obtain a barium sulfide clear solution, and detecting and analyzing to obtain the barium sulfide molar concentration in the barium sulfide clear solution to be 0.18 mol/L; pouring 200ml of barium sulfide clear solution into a crystallizer, and slowly adding the barium sulfide clear solution with the concentration of 0.15 at the temperature of 35 ℃ and the stirring speed of 300rad/minAnd after 240mL of a sodium carbonate solution of mol/L, filtering to obtain a solid and a filtrate, washing the separated solid with deionized water, and drying at 100 ℃ for 24 hours to obtain the high-purity barium carbonate. The filtrate is evaporated and concentrated under reduced pressure to obtain a by-product Na2And S, evaporating and concentrating the collected condensed water for dissolving the crude barium sulfide. The purity of the prepared high-purity barium carbonate is 99.5% by analysis.
Example 3
Sequentially washing barite crushed to the particle size of less than 50 mu m by a sodium hydroxide solution, a hydrochloric acid solution and deionized water, and drying for 24 hours in an environment at the temperature of higher than 90 ℃; placing 30g of dried barite powder in a reactor, introducing nitrogen to replace air in the reactor, continuously introducing nitrogen, heating to 1400 ℃, then introducing a mixed gas of sulfur vapor and nitrogen, wherein the volume ratio of the sulfur vapor to the nitrogen is 1:9, controlling the flow of the mixed gas to be 0.2-0.4L/min, reacting the mixed gas in the reactor for 6-12 min to obtain crude barium sulfide, dissolving the crude barium sulfide in 1L of deionized water, filtering to obtain a barium sulfide clear solution, and detecting and analyzing to obtain the barium sulfide molar concentration of 0.10mol/L in the barium sulfide clear solution; pouring 200mL of clear barium sulfide liquid into a crystallizer, slowly adding 200mL of sodium carbonate solution with the concentration of 0.10mol/L under the conditions of 35 ℃ and the stirring speed of 200rad/min, then obtaining solid and clear liquid through centrifugal separation, washing the separated solid with deionized water, and drying for 24 hours at the temperature of 100 ℃ to obtain the high-purity barium carbonate. The filtrate is evaporated and concentrated under reduced pressure to obtain a by-product Na2And S, evaporating and concentrating the collected condensed water for dissolving the crude barium sulfide. The purity of the prepared high-purity barium carbonate is 99.5% by analysis.
Example 4
Sequentially washing barite crushed to the particle size of less than 50 mu m by a sodium hydroxide solution, a hydrochloric acid solution and deionized water, and drying for 24 hours in an environment at the temperature of higher than 90 ℃; putting 45g of dried barite powder into a reactor, introducing nitrogen to replace air in the reactor, continuously introducing nitrogen, heating to 1450 ℃, then introducing a mixed gas of sulfur vapor and nitrogen, wherein the volume ratio of the sulfur vapor to the nitrogen is 1:4, the flow rate of the mixed gas is controlled to be 0.45-0.6L/min, the space time of the mixed gas in the reactor is 4-4.8 min, and reacting for 1.5h to obtain crude barium sulfide; dissolving the crude barium sulfide in 1L of deionized water, filtering to obtain a barium sulfide clear solution, and detecting and analyzing to obtain the barium sulfide molar concentration of 0.18mol/L in the barium sulfide clear solution; pouring 300ml of barium sulfide clear liquid into a crystallizer, slowly introducing carbon dioxide gas at the temperature of 40-80 ℃ and the stirring speed of 300rad/min for 15min, filtering to obtain solid and filtrate, washing the separated solid with deionized water, and drying at the temperature of 100 ℃ for 24h to obtain the high-purity barium carbonate. The hydrogen sulfide gas after the precipitation reaction reacts with partial thermal reduction gas phase product sulfur dioxide to generate elemental sulfur, and then the elemental sulfur is reused for preparing sulfur vapor, and the filtrate is reused for dissolving crude barium sulfide. The purity of the prepared high-purity barium carbonate is 99.6 percent by analysis.
Example 5
Sequentially washing barite crushed to the particle size of less than 50 mu m by a sodium hydroxide solution, a hydrochloric acid solution and deionized water, and drying for 24 hours in an environment at the temperature of higher than 90 ℃; putting 32g of dried barite powder into a reactor, introducing nitrogen to replace air in the reactor, continuously introducing nitrogen, heating to 1200 ℃, then introducing a mixed gas of sulfur vapor and nitrogen, wherein the volume ratio of the sulfur vapor to the nitrogen is 1:7, the flow rate of the mixed gas is controlled to be 0.2-0.4L/min, the space time of the mixed gas in the reactor is 6-12 min, and reacting for 1h to obtain crude barium sulfide; dissolving the crude barium sulfide in 1L of deionized water, filtering to obtain a barium sulfide clear solution, and detecting and analyzing to obtain the barium sulfide molar concentration of 0.11mol/L in the barium sulfide clear solution; pouring 400ml of barium sulfide clear liquid into a crystallizer, slowly introducing carbon dioxide gas at the flow rate of 3L/h and the introduction time of 20min under the conditions of 40-80 ℃ and 200rad/min stirring speed, filtering to obtain solid and filtrate, washing the separated solid with deionized water, and drying for 24h at 100 ℃ to obtain the high-purity barium carbonate. The hydrogen sulfide gas after the precipitation reaction reacts with partial thermal reduction gas phase product sulfur dioxide to generate elemental sulfur, and then the elemental sulfur is reused for preparing sulfur vapor, and the filtrate is reused for dissolving crude barium sulfide. The purity of the prepared high-purity barium carbonate is 99.5% by analysis.
Finally, it should be noted that the above-mentioned examples of the present invention are only examples for illustrating the present invention, and are not intended to limit the embodiments of the present invention. Variations and modifications in other variations will occur to those skilled in the art upon reading the foregoing description. Not all embodiments are exhaustive. All obvious changes and modifications of the present invention are within the scope of the present invention.

Claims (10)

1. The preparation method of the high-purity barium carbonate is characterized by comprising the following steps:
(1) pretreatment: crushing barite into powder with the particle size of less than 50 mu m, then carrying out alkali washing, acid washing and water washing, and finally drying to obtain barite powder;
(2) thermal reduction reaction: adding the barite powder obtained in the step (1) into a thermal reduction reactor, introducing nitrogen to replace air in the reactor, continuously introducing nitrogen, heating to 1000-2000 ℃, introducing a mixed gas of sulfur vapor and nitrogen into the reactor, reacting for a period of time, cooling to room temperature to obtain crude barium sulfide, and collecting to obtain a gas containing a large amount of sulfur dioxide and a small amount of sulfur vapor;
(3) preparing a barium sulfide clear solution: dissolving the crude barium sulfide obtained in the step (2) in deionized water, and then filtering to obtain a barium sulfide clear solution;
(4) preparing high-purity barium carbonate: introducing CO into the barium sulfide clear liquid prepared in the step (3) at the temperature of 0-100 ℃ and the stirring speed of 0-1000 r/min2And (3) gas or slowly adding a sodium carbonate solution for precipitation reaction, then carrying out solid-liquid separation, and washing and drying the solid to obtain the high-purity barium carbonate.
2. The method for preparing high purity barium carbonate according to claim 1, wherein the base used in step (1) is any one of sodium hydroxide solution or potassium hydroxide solution, and the acid used is hydrochloric acid solution.
3. The method for preparing high-purity barium carbonate according to claim 1, wherein in the step (2), the molar ratio of the barite powder to the sulfur vapor is 1: 2-10; the sulfur vapor in the mixed gas accounts for 5-95% of the total volume of the mixed gas, the flow of the mixed gas is controlled to be 0.1-2.5L/min, and the total reaction time is 0.5-2 h.
4. The method for preparing high purity barium carbonate according to claim 3, wherein the sulfur vapor in the mixed gas accounts for 10-30% of the total volume of the mixed gas.
5. The method for preparing high purity barium carbonate according to claim 1, wherein the sulfur dioxide gas collected in step (2) is used for preparing sulfuric acid.
6. The preparation method of high-purity barium carbonate according to claim 1, wherein the mass ratio of the crude barium sulfide to the deionized water in the step (3) is 5-500: 1000.
7. the method for preparing high purity barium carbonate according to claim 1, wherein Ba in the clear barium sulfide solution in step (4)2+With CO in sodium carbonate solution3 2-In a molar ratio of 1: 1; the molar concentration of the sodium carbonate solution is 0.05-0.5 mol/L.
8. The method for preparing high purity barium carbonate according to claim 1, wherein Ba in the clear barium sulfide solution in step (4)2+With CO2The molar ratio of (A) to (B) is: 1: 0.8 to 1, control of CO2The gas flow rate of (1-10L/h).
9. The method for preparing high-purity barium carbonate according to claim 1, wherein the liquid obtained by solid-liquid separation after the precipitation reaction of sodium carbonate and the barium sulfide clear solution in step (4) is evaporated and concentrated to obtain a by-product sodium sulfide, and the condensed water obtained by evaporation is recycled to step (3) for dissolving crude barium sulfide.
10. The method for preparing high purity barium carbonate according to claim 1, wherein in the step (4), CO is added2Carrying out precipitation reaction on the gas and the barium sulfide clear solution to obtain hydrogen sulfide gas, reacting the hydrogen sulfide gas with part of sulfur dioxide collected in the step (2) to recover elemental sulfur, and then preparing sulfur vapor; and (4) directly reusing the liquid obtained by solid-liquid separation in the step (3) for dissolving the crude barium sulfide.
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