CN111285389A - Production method of superfine precipitated barium sulfate - Google Patents

Production method of superfine precipitated barium sulfate Download PDF

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Publication number
CN111285389A
CN111285389A CN201811489728.XA CN201811489728A CN111285389A CN 111285389 A CN111285389 A CN 111285389A CN 201811489728 A CN201811489728 A CN 201811489728A CN 111285389 A CN111285389 A CN 111285389A
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China
Prior art keywords
solution
barium sulfate
sodium
sodium sulfide
sulfate
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CN201811489728.XA
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Inventor
周新国
王泽云
王兰君
张超
尚方毓
李媛
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Shanxi Coking Coal Yuncheng Salinization Group Co.,Ltd.
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China Nafine Group Intenational Co ltd
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Priority to CN201811489728.XA priority Critical patent/CN111285389A/en
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    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01FCOMPOUNDS OF THE METALS BERYLLIUM, MAGNESIUM, ALUMINIUM, CALCIUM, STRONTIUM, BARIUM, RADIUM, THORIUM, OR OF THE RARE-EARTH METALS
    • C01F11/00Compounds of calcium, strontium, or barium
    • C01F11/46Sulfates
    • C01F11/462Sulfates of Sr or Ba
    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01PINDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2004/00Particle morphology
    • C01P2004/60Particles characterised by their size
    • C01P2004/61Micrometer sized, i.e. from 1-100 micrometer
    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01PINDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2004/00Particle morphology
    • C01P2004/60Particles characterised by their size
    • C01P2004/62Submicrometer sized, i.e. from 0.1-1 micrometer

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

Abstract

The invention provides a production method of ultrafine precipitated barium sulfate, wherein a barium sulfate solution (100-150 g/L) reacts with a sodium sulfate solution (280-320g/L) to generate precipitated barium sulfate and a sodium sulfide solution (the concentration is 4-5%), the sodium sulfide solution is precipitated, polysulfide is removed and then the sodium sulfide solution is reused in the sodium sulfate solution, and the solution (250 g/L of sodium sulfate 100-34.38 g/L and 4.28-34.38 g/L) is used as a next barium sulfate combination raw material to react with the barium sulfate solution to generate barium sulfate and sodium sulfide solution (4-5%). The concentration of the sodium sulfate solution is reduced, so that the concentration of barium sulfate generated in a reaction system is reduced, the nucleation and growth speed of barium sulfate is improved, the barium sulfate is prevented from agglomerating, the particle size of the generated barium sulfate is small, the whiteness is high, the quality is good, meanwhile, the concentration of the generated sodium sulfide solution is not reduced (4-5%), and the cost of subsequent evaporation production of 60 alkali is not increased.

Description

Production method of superfine precipitated barium sulfate
Technical Field
The invention discloses an industrial application of a production method of superfine precipitated barium sulfate in the barium sulfate production industry.
Background
The production process of precipitated barium sulfate by using mirabilite-black ash method in barium sulfate industry is characterized by that the barium sulfate solution produced after the black ash is leached is reacted with sodium sulfate solution to produce barium sulfate and sodium sulfide solution (concentration is 4-5%), and the sodium sulfide solution is precipitated, clarified and fed into evaporator to produce 60% alkali (sodium sulfide content is 60%). In the barium sulfate combination process, because the concentration of the sodium sulfate solution is high (280-320g/L) and the particle size of the generated barium sulfate is large, the sodium sulfate solution is treated and then reused in the sodium sulfate solution, and the solution (100-250 g/L of sodium sulfate and 4.28-34.38g/L of sodium sulfide) is used as the next barium sulfate combination raw material to react with the barium sulfate solution (100-150 g/L) to generate barium sulfate and sodium sulfide solution (4-5%). The concentration of the sodium sulfate solution is reduced, so that the concentration of the barium sulfate generated in the reaction system is reduced, the nucleation and growth speed of the barium sulfate is improved, the barium sulfate is prevented from agglomerating, the particle size of the generated barium sulfate is small, the whiteness is high, the quality is good, the concentration of the sodium sulfide solution entering the subsequent evaporation is ensured not to be reduced, and the production cost of 60 alkali is not increased.
Disclosure of Invention
The invention aims to develop a production method of superfine precipitated barium sulfate; meanwhile, the concentration of the sodium sulfide solution entering the subsequent evaporation is not reduced, and the production cost of 60 alkali is not increased.
In order to achieve the purpose, the invention adopts the scheme that the temperature of a sodium sulfide solution is reduced to 35-45 ℃, then the sodium sulfide solution is pumped into an air blowing device, air blowing is carried out for 4-6 hours in the sodium sulfide solution, the filtered sodium sulfide solution is reused in a sodium sulfate solution with the concentration of 280-320g/L, the solution (sodium sulfate 100-250g/L and sodium sulfide 4.28-34.38 g/L) is used as a next barium sulfate compound raw material to react with the barium sulfide solution to generate barium sulfate and sodium sulfide solution (4-5%), a barium sulfate product is obtained after the reaction solution is filtered, washed, acid-regulated, filtered, dried and scattered, and one part of the sodium sulfide solution is cooled, blown to remove polysulfide and then is reused, and one part of the sodium sulfide solution is used for producing 60 alkali.
The barium sulfate compound technology has the advantages that: the treated sodium sulfide solution is reused in a sodium sulfate solution, and the solution (100 g/L of sodium sulfate and 250g/L of sodium sulfide and 4.28-34.38g/L of sodium sulfide) is used as a next barium sulfate compound raw material to react with the barium sulfide solution to generate a barium sulfate and sodium sulfide solution (4-5%). The concentration of the sodium sulfate solution is reduced, so that the concentration of barium sulfate generated in a reaction system is reduced, the nucleation and growth speed of barium sulfate is improved, the barium sulfate is prevented from agglomerating, the particle size of the generated barium sulfate is small, the whiteness is high, the quality is good, the concentration of the sodium sulfide solution is not reduced (4-5%), and the cost of subsequent evaporation production of 60 alkali is not increased.
The specific implementation mode is as follows:
(1) reacting the barium sulfate solution (100-320 g/L) with the sodium sulfate solution (280-320g/L) to generate barium sulfate and sodium sulfide solution, filtering, washing, adjusting acid, filtering, drying and scattering the reaction solution to obtain a barium sulfate product, and precipitating and clarifying the sodium sulfide solution;
(2) cooling the clarified sodium sulfide solution to 35-45 ℃, and pumping into an air blowing device. Filtering after blowing air for 4-6 hours in the blowing device;
(3) dissolving a sodium sulfate solution by hot water, and preparing the sodium sulfate solution to be 320g/L after removing calcium and magnesium;
(4) the filtered sodium sulfide solution is reused in a sodium sulfate solution, and the solution (100 g/L of sodium sulfate and 250g/L of sodium sulfide, 4.28-34.38g/L of sodium sulfide) is used as a next barium sulfate compound raw material to react with the barium sulfide solution to generate barium sulfate and sodium sulfide solution (4-5%);
(5) filtering the reaction liquid, separating a barium sulfate solution and a sodium sulfide solution, precipitating and clarifying the sodium sulfide solution, pumping a part of the sodium sulfide solution into a four-effect evaporation device to produce 60 alkali, and cooling a part of the sodium sulfide solution to enter an air blowing device;
(6) and washing, adjusting acid, filtering, drying and scattering the barium sulfate cake to obtain a barium sulfate product.
The process flow chart is as follows: as in fig. 1.
Example 1:
reacting a barium sulfide solution (120 g/L) with a sodium sulfate solution (300g/L) to generate a barium sulfate solution and a sodium sulfide solution, precipitating and clarifying the generated sodium sulfide solution, cooling a part of the sodium sulfide solution to 45 ℃, and pumping the cooled sodium sulfide solution into an air blowing device. Blowing air in an air blowing device for 4 hours, filtering, dissolving a sodium sulfate solution with hot water to obtain a sodium sulfide solution with the concentration of 41.43g/L, and blending the sodium sulfate solution to 300g/L after removing calcium and magnesium; after the filtered sodium sulfide solution is reused in a sodium sulfate solution, the concentration of sodium sulfate is 125g/L, the solution is combined with a barium sulfide solution (120 g/L) to react to generate a barium sulfate solution and a sodium sulfide solution, the reaction solution is filtered to separate the barium sulfate solution and the sodium sulfide solution, after the sodium sulfide solution is settled, part of the sodium sulfide solution is pumped into a four-effect evaporator to produce 60 alkali, and the other part of the sodium sulfide solution is cooled and enters an air blowing device; and washing, adjusting acid, filtering, drying and scattering the barium sulfate cake to obtain a barium sulfate product.
Reacting the barium sulfide solution (120 g/L) with the sodium sulfate solution (300g/L) to generate a sodium sulfide solution with the concentration: the concentration of the sodium hydroxide is 41.43g/L,
the barium sulfate particle size D50:1.24 μm, D90:2.77 μm (FIG. 1)
After the sodium sulfide solution is reused in the sodium sulfate solution, the concentration of sodium sulfide is as follows: 24.17 g/L;
the reaction ratio of the sodium sulfate solution to the barium sulfide solution is as follows: 1: 1.24;
the concentration of the sodium sulfide solution generated by the reaction is as follows: 41.44 g/L;
the particle size of barium sulfate D50:0.81 μm and D90:1.59 μm (FIG. 2);
the sodium sulfate solution of the recycled sodium sulfide solution reacts with the barium sulfide solution to generate barium sulfate and sodium sulfide solution, the generated barium sulfate has small particle size, high whiteness and good quality, the concentration of the sodium sulfide solution is not changed greatly, and the subsequent production of 60 alkali (the content of sodium sulfide is 60%) is not influenced.
Example 2:
reacting a barium sulfide solution (140 g/L) with a sodium sulfate solution (310g/L) to generate a barium sulfate solution and a sodium sulfide solution, precipitating and clarifying the generated sodium sulfide solution, cooling a part of the sodium sulfide solution to 40 ℃, and pumping the cooled sodium sulfide solution into an air blowing device. Blowing air in an air blowing device for 5 hours, filtering, dissolving a sodium sulfate solution with hot water, and blending the sodium sulfate solution to 310g/L after removing calcium and magnesium, wherein the concentration of the filtered sodium sulfide solution is 46.86 g/L; after the filtered sodium sulfide solution is reused in a sodium sulfate solution, the concentration of the sodium sulfate solution is 130g/L, the solution is combined with a barium sulfide solution (140 g/L) to react to generate a barium sulfate solution and a sodium sulfide solution, the reaction solution is filtered to separate the barium sulfate solution and the sodium sulfide solution, after the sodium sulfide solution is settled, part of the sodium sulfide solution is pumped into a four-effect evaporator to produce 60 alkali, and the other part of the sodium sulfide solution is cooled to enter an air blowing device; and washing, adjusting acid, filtering, drying and scattering the barium sulfate cake to obtain a barium sulfate product.
Reacting the barium sulfide solution (140 g/L) with the sodium sulfate solution (310g/L) to generate a sodium sulfide solution with the concentration: 46.86g/L of the total weight of the oil,
the particle size of barium sulfate is D50:1.28 μm and D90:2.84 μm;
after the sodium sulfide solution is reused in the sodium sulfate solution, the concentration of sodium sulfide is as follows: 27.21 g/L;
the reaction ratio of the sodium sulfate solution to the barium sulfide solution is as follows: 1: 1.08;
the concentration of the sodium sulfide solution generated by the reaction is as follows: 46.63 g/L;
the particle size of barium sulfate; d50:0.87 μm, D90:2.21 μm;
the sodium sulfate solution of the recycled sodium sulfide solution reacts with the barium sulfide solution to generate barium sulfate and sodium sulfide solution, the generated barium sulfate has small particle size, high whiteness and good quality, the concentration of the sodium sulfide solution is not changed greatly, and the subsequent production of 60 alkali (the content of sodium sulfide is 60%) is not influenced.
Description of the drawings: FIG. 1 is a flow chart of the production process of ultra-fine precipitated barium sulfate.
FIG. 2 is a particle size distribution diagram of barium sulfate.
FIG. 3 is a graph showing a distribution of barium sulfate particle diameters.

Claims (1)

1. The production method of the superfine precipitated barium sulfate mainly comprises the following three aspects:
① cooling to 35-45 deg.C, pumping into an air blowing device, blowing air in the air blowing device for 4-6 hr, and filtering;
② the filtered sodium sulfide solution is reused in the sodium sulfate solution, and the solution (sodium sulfate 100-250g/L, sodium sulfide 4.28-34.38 g/L) is used as the next barium sulfate raw material to react with the barium sulfide solution (100-150 g/L) to generate barium sulfate and sodium sulfide solution (4-5%);
③ filtering the reaction solution, separating barium sulfate and sodium sulfide solution, precipitating and clarifying the sodium sulfide solution, pumping part of the sodium sulfide solution into a four-effect evaporator to produce 60 alkali, cooling part of the sodium sulfide solution, and introducing the cooled part of the sodium sulfide solution into an air blowing device.
CN201811489728.XA 2018-12-06 2018-12-06 Production method of superfine precipitated barium sulfate Pending CN111285389A (en)

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN113307297A (en) * 2021-06-18 2021-08-27 竹山县秦巴钡盐有限公司 Barium sulfate and zinc sulfide cyclic production system and process

Citations (7)

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Publication number Priority date Publication date Assignee Title
RU95111420A (en) * 1995-07-03 1997-06-20 К.В. Ткачев Method of producing sodium sulfide
US20040126320A1 (en) * 2001-03-08 2004-07-01 Tsuyoshi Miyamoto Barium sulfate based poder and cosmetics containing the same
WO2007096383A1 (en) * 2006-02-21 2007-08-30 Sachtleben Chemie Gmbh Method for carrying out chemical and physical processes and reaction cells
CN101332998A (en) * 2008-07-04 2008-12-31 竹山县秦巴钡盐有限公司 Method for preparing barium sulfate
CN102167386A (en) * 2011-03-16 2011-08-31 清华大学 Method for preparing barium sulfate nanoparticles
CN104326499A (en) * 2014-10-13 2015-02-04 南风化工集团股份有限公司 Method for improving sodium sulfide solution concentration by leaching black ash for three times
CN106186027A (en) * 2016-07-01 2016-12-07 深州嘉信化工有限责任公司 A kind of microgranule footpath blanc fixe production method

Patent Citations (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
RU95111420A (en) * 1995-07-03 1997-06-20 К.В. Ткачев Method of producing sodium sulfide
US20040126320A1 (en) * 2001-03-08 2004-07-01 Tsuyoshi Miyamoto Barium sulfate based poder and cosmetics containing the same
WO2007096383A1 (en) * 2006-02-21 2007-08-30 Sachtleben Chemie Gmbh Method for carrying out chemical and physical processes and reaction cells
CN101332998A (en) * 2008-07-04 2008-12-31 竹山县秦巴钡盐有限公司 Method for preparing barium sulfate
CN102167386A (en) * 2011-03-16 2011-08-31 清华大学 Method for preparing barium sulfate nanoparticles
CN104326499A (en) * 2014-10-13 2015-02-04 南风化工集团股份有限公司 Method for improving sodium sulfide solution concentration by leaching black ash for three times
CN106186027A (en) * 2016-07-01 2016-12-07 深州嘉信化工有限责任公司 A kind of microgranule footpath blanc fixe production method

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尚方毓等: "1.1芒硝-硫酸钠法", 《无机盐工业》 *
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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN113307297A (en) * 2021-06-18 2021-08-27 竹山县秦巴钡盐有限公司 Barium sulfate and zinc sulfide cyclic production system and process

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Address after: 044099 No. 376, Hongqi East Street, Yanhu District, Yuncheng City, Shanxi Province

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Application publication date: 20200616