CN115385369A - Preparation method of high-purity barium hydroxide - Google Patents

Preparation method of high-purity barium hydroxide Download PDF

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Publication number
CN115385369A
CN115385369A CN202110568854.XA CN202110568854A CN115385369A CN 115385369 A CN115385369 A CN 115385369A CN 202110568854 A CN202110568854 A CN 202110568854A CN 115385369 A CN115385369 A CN 115385369A
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Prior art keywords
barium hydroxide
barium
temperature
octahydrate
mineral powder
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CN202110568854.XA
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Chinese (zh)
Inventor
王经镇
焦安浩
卢丙学
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Shandong Xinke Huanhua Co ltd
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Shandong Xinke Huanhua Co ltd
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Priority to CN202110568854.XA priority Critical patent/CN115385369A/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
    • C01F11/02Oxides or hydroxides
    • C01F11/04Oxides or hydroxides by thermal decomposition
    • C01F11/06Oxides or hydroxides by thermal decomposition of carbonates
    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01PINDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2006/00Physical properties of inorganic compounds
    • C01P2006/80Compositional purity

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Physics & Mathematics (AREA)
  • Thermal Sciences (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Geology (AREA)
  • Inorganic Chemistry (AREA)
  • Manufacture And Refinement Of Metals (AREA)

Abstract

The invention discloses a preparation method of high-purity barium hydroxide, which comprises the following steps; s1, grinding: grinding the mineral containing barium carbonate into mineral powder by using a grinder; s2, calcining and reducing: calcining the mineral powder obtained in the step S1 at a high temperature, wherein the mineral powder is in a suspension fluidization state during the high-temperature calcination, and roasting the mineral powder at the high temperature to obtain roasted ore containing barium oxide; in the high-temperature roasting, the temperature of the high-temperature roasting is controlled to be 900-1500 ℃, and the time of the high-temperature roasting is 45-90 s; s3, immersing the roasted ore obtained in the S2 into water, fully stirring, and obtaining a barium hydroxide solution after barium oxide in the roasted ore fully reacts with the water; s4, heating the barium hydroxide solution obtained in the S3 to 76-90 ℃; and S5, spraying the barium hydroxide solution obtained in the step S4 to treat barium hydroxide octahydrate with the particle size of less than 4000 micrometers. The barium hydroxide solution is cooled by using purified air, so that the purity of the barium hydroxide can be effectively improved.

Description

Preparation method of high-purity barium hydroxide
Technical Field
The invention relates to the technical field of barium hydroxide preparation, in particular to a preparation method of high-purity barium hydroxide.
Background
Barium hydroxide is an inorganic substance of the formula Ba (OH) 2 Colorless transparent crystals or white powder. The hydrate can lose 7 molecules of crystal water in a sulfuric acid dryer, and all crystal water is lost at about 78 ℃. It is soluble in water and methanol, slightly soluble in ethanol and hardly soluble in acetone. If carbon dioxide is rapidly absorbed from the air and converted into carbonate, it cannot be completely dissolved in water. Relative density 2.188, melting point 78 ℃ (octahydrate, greater than 408 ℃ in the case of pure barium hydroxide), refractivityThe rate is 1.471, high toxicity and strong corrosivity. The method is used for measuring carbon dioxide in air, quantifying chlorophyll, refining sugar and animal and vegetable oil, cleaning water for boilers, pesticides and rubber industry.
However, the conventional method for preparing barium hydroxide is to react barium sulfide with hydrochloric acid to prepare barium chloride, and then to perform a double decomposition reaction with sodium hydroxide. Cooling, crystallizing, separating, washing and packaging to obtain the finished product. In order to ensure the reaction to be carried out well, the reaction is carried out at a higher temperature and under the condition of excessive sodium hydroxide; although the preparation method of barium hydroxide is short in process and simple in operation, the finally prepared barium hydroxide contains impurities such as barium chloride, sodium chloride and sodium hydroxide.
Disclosure of Invention
The invention aims to provide a preparation method of high-purity barium hydroxide, which aims to improve the traditional preparation method of barium hydroxide. Cooling, crystallizing, separating, washing and packaging to obtain the finished product. In order to ensure the reaction to be carried out well, the reaction needs to be carried out at a higher temperature and under the condition of excessive sodium hydroxide; although the preparation method of the barium hydroxide is short in process and simple in operation, the finally prepared barium hydroxide contains impurities such as barium chloride, sodium hydroxide and the like.
The invention is realized by the following steps:
a preparation method of high-purity barium hydroxide comprises the following steps;
s1, grinding: grinding the mineral containing barium carbonate into mineral powder by using a grinder;
s2, calcining and reducing: calcining the mineral powder obtained in the step S1 at a high temperature, wherein the mineral powder is in a suspension fluidization state during the high-temperature calcination, and roasting the mineral powder at the high temperature to obtain roasted ore containing barium oxide; in the high-temperature roasting, the temperature of the high-temperature roasting is controlled to be 900-1500 ℃, and the time of the high-temperature roasting is 45-90 s;
s3, immersing the roasted ore obtained in the S2 into water, fully stirring, and obtaining a barium hydroxide solution after barium oxide in the roasted ore fully reacts with the water;
s4, heating the barium hydroxide solution obtained in the S3 to 76-90 ℃;
and S5, spraying the barium hydroxide solution obtained in the step S4 to treat barium hydroxide octahydrate with the particle size of less than 4000 microns, cooling the barium hydroxide octahydrate to room temperature by using air to obtain an anti-caking barium hydroxide octahydrate product, cooling and crystallizing the barium hydroxide octahydrate product, and drying precipitated crystals to obtain a barium hydroxide product.
Preferably, in the S1, the granularity of the ore powder is controlled to be less than 0.6mm, and the ore powder is aligned and dried during the grinding process, so that the water content of the ore powder is less than 2%.
Preferably, in the calcining reduction, the mineral powder is in a suspension fluidization state by continuously introducing neutral or weak reducing high-temperature flue gas, and the solid-gas ratio of the mineral powder during high-temperature roasting to the introduced high-temperature flue gas is 0.3-0.8 kg/Nm < 3 >; the high-temperature calcination time is 45-90 s; the high-temperature flue gas source in roasting mainly comes from a hot blast stove, the hot blast stove takes coal, coal gas, natural gas or petroleum and the like as fuels, and the mixed gas in the hot blast stove comes from fresh air blown by a blower used by the hot blast stove.
Preferably, in S4, the barium hydroxide octahydrate with the particle size of less than 4000 microns is placed on a mesh belt, the thickness of a material layer is controlled to be less than 10mm, the advancing speed of the mesh belt is controlled to be 800-1000 mm/min, and the barium hydroxide solution obtained in S4 is sprayed on the barium hydroxide octahydrate in a region of 150-250mm in the advancing direction of the mesh belt.
Compared with the prior art, the invention has the beneficial effects that:
(1) The preparation method of the invention firstly finely grinds the mineral containing barium carbonate into mineral powder, and the mineral powder is roasted at high temperature under the suspension fluidization state, thereby effectively improving the combustion efficiency, leading the heat and mass transfer speed of the mineral and gas to be extremely high, leading the time required by the reaction of the mineral containing barium carbonate to be within a few minutes, greatly shortening the time required by the reaction and improving the volume utilization rate of equipment.
(2) The barium hydroxide solution is cooled by using the purified air, so that the purity of the barium hydroxide can be effectively improved.
Detailed Description
In order to make the objects, technical solutions and advantages of the embodiments of the present invention more apparent, the embodiments of the present invention will be described in detail and completely with reference to the examples of the present invention, and it is apparent that the described embodiments are some, but not all embodiments of the present invention. All other embodiments obtained by a person of ordinary skill in the art based on the embodiments of the present invention without any creative effort belong to the protection scope of the present invention. Thus, the following detailed description of embodiments of the invention is not intended to limit the scope of the invention as claimed, but is merely representative of selected embodiments of the invention. All other embodiments, which can be obtained by a person skilled in the art without any inventive step based on the embodiments of the present invention, are within the scope of the present invention.
Example 1
A preparation method of high-purity barium hydroxide comprises the following steps;
s1, grinding: grinding the mineral containing barium carbonate into mineral powder by using a grinder;
s2, calcining and reducing: performing high-temperature calcination on the mineral powder obtained in the step S1, wherein the mineral powder is in a suspended fluidized state during the high-temperature calcination, and obtaining a roasted ore containing barium oxide after the high-temperature calcination is completed; in the high-temperature roasting, the temperature of the high-temperature roasting is controlled to be 900-1500 ℃, and the time of the high-temperature roasting is 45-90 s;
s3, immersing the roasted ore obtained in the S2 into water, fully stirring, and obtaining a barium hydroxide solution after barium oxide in the roasted ore fully reacts with the water;
s4, heating the barium hydroxide solution obtained in the S3 to 76-90 ℃;
and S5, spraying the barium hydroxide solution obtained in the step S4 to treat barium octahydrate with the particle size of less than 4000 micrometers, cooling the barium hydroxide octahydrate to room temperature by using air to obtain an anti-caking barium octahydrate product, cooling and crystallizing the barium hydroxide octahydrate product, and drying precipitated crystals to obtain a barium hydroxide product.
Further, in the S1, the particle size of the ore powder is controlled below 0.6mm, and the ore powder is aligned and dried during the grinding process, so that the water content of the ore powder is less than 2%.
Furthermore, in the calcination reduction, the mineral powder is in a suspension fluidization state by continuously introducing neutral or weak-reducing high-temperature flue gas, and the solid-gas ratio of the mineral powder during high-temperature roasting to the introduced high-temperature flue gas is 0.3-0.8 kg/Nm3; the high-temperature calcination time is 45-90 s; the high-temperature flue gas source in roasting mainly comes from a hot blast stove, the hot blast stove takes coal, coal gas, natural gas or petroleum and the like as fuels, and the mixed gas in the hot blast stove comes from fresh air blown by a blower used by the hot blast stove.
Further, in S4, barium octahydrate with the particle size of less than 4000 micrometers is placed on a mesh belt, the thickness of a material layer is controlled to be less than 10mm, the advancing speed of the mesh belt is controlled to be 800-1000 mm/min, and the barium hydroxide solution obtained in S4 is sprayed on the barium hydroxide octahydrate in an area of 150-250mm in the advancing direction of the mesh belt.
Example 2
A preparation method of high-purity barium hydroxide comprises the following steps;
s1, grinding: grinding the mineral containing barium carbonate into mineral powder by using a grinder;
s2, calcining and reducing: calcining the mineral powder obtained in the step S1 at a high temperature, wherein the mineral powder is in a suspension fluidization state during the high-temperature calcination, and roasting the mineral powder at the high temperature to obtain roasted ore containing barium oxide; in the high-temperature roasting, the temperature of the high-temperature roasting is controlled to be 1600 ℃, and the time of the high-temperature roasting is 100s;
s3, immersing the roasted ore obtained in the S2 into water, fully stirring, and obtaining a barium hydroxide solution after barium oxide in the roasted ore fully reacts with the water;
s4, heating the barium hydroxide solution obtained in the S3 to 95 ℃;
and S5, spraying the barium hydroxide solution obtained in the step S4 to treat barium hydroxide octahydrate with the particle size of less than 3000 microns, cooling the barium hydroxide octahydrate to room temperature by using air to obtain an anti-caking barium hydroxide octahydrate product, cooling and crystallizing the barium hydroxide octahydrate product, and drying precipitated crystals to obtain a barium hydroxide product.
Further, in the S1, the granularity of the ore powder is controlled to be 0.4mm, and the ore powder is aligned and dried during the grinding process, so that the water content of the ore powder is less than 2%.
Furthermore, in the calcination reduction, the mineral powder is in a suspension fluidization state by continuously introducing neutral or weak-reducing high-temperature flue gas, and the solid-gas ratio of the mineral powder during high-temperature roasting to the introduced high-temperature flue gas is 0.3-0.8 kg/Nm3; the high-temperature calcination time is 45-90 s; the high-temperature flue gas source in roasting mainly comes from a hot blast stove, the hot blast stove takes coal, coal gas, natural gas or petroleum and the like as fuels, and the mixed gas in the hot blast stove comes from fresh air blown by a blower used by the hot blast stove.
Further, in S4, barium hydroxide octahydrate with the particle size of less than 4000 microns is placed on a mesh belt, the thickness of a material layer is controlled to be less than 10mm, the advancing speed of the mesh belt is controlled to be 800-1000 mm/min, and the barium hydroxide solution obtained in S4 is sprayed on the barium hydroxide octahydrate in a region of 150-250mm of the advancing direction of the mesh belt.
The above description is only a preferred embodiment of the present invention, and is not intended to limit the present invention, and various modifications and changes may be made to the present invention by those skilled in the art. Any modification, equivalent replacement, or improvement made within the spirit and principle of the present invention should be included in the protection scope of the present invention.

Claims (4)

1. A preparation method of high-purity barium hydroxide comprises the following steps;
s1, grinding: grinding the mineral containing barium carbonate into mineral powder by using a grinder;
s2, calcining and reducing: performing high-temperature calcination on the mineral powder obtained in the step S1, wherein the mineral powder is in a suspended fluidized state during the high-temperature calcination, and obtaining a roasted ore containing barium oxide after the high-temperature calcination is completed; in the high-temperature roasting, the temperature of the high-temperature roasting is controlled to be 900-1500 ℃, and the time of the high-temperature roasting is 45-90 s;
s3, immersing the roasted ore obtained in the S2 into water, fully stirring, and obtaining a barium hydroxide solution after barium oxide in the roasted ore fully reacts with the water;
s4, heating the barium hydroxide solution obtained in the S3 to 76-90 ℃;
and S5, spraying the barium hydroxide solution obtained in the step S4 to treat barium octahydrate with the particle size of less than 4000 micrometers, cooling the barium octahydrate to room temperature by using air to obtain an anti-caking barium octahydrate product, cooling and crystallizing the barium octahydrate product, and drying precipitated crystals to obtain a barium hydroxide product.
2. The method according to claim 1, wherein in the step S1, the particle size of the ore powder is controlled to be less than 0.6mm, and the ore powder is dried in alignment during the grinding process, so that the water content of the ore powder is less than 2%.
3. The method for preparing high-purity barium hydroxide according to claim 1, wherein during the calcination reduction, the mineral powder is in a suspended fluidized state by continuously introducing neutral or weakly reducing high-temperature flue gas, and the solid-gas ratio of the mineral powder during high-temperature roasting to the introduced high-temperature flue gas is 0.3-0.8 kg/Nm3..
4. The method according to claim 1, wherein in S4, barium hydroxide octahydrate having a particle size of less than 4000 microns is placed on a mesh belt, the thickness of a material layer is controlled to be less than 10mm, the advancing speed of the mesh belt is controlled to be 800-1000 mm/min, and the barium hydroxide octahydrate is sprayed with the barium hydroxide solution obtained in S4 in a region of 150-250mm in the advancing direction of the mesh belt.
CN202110568854.XA 2021-05-25 2021-05-25 Preparation method of high-purity barium hydroxide Pending CN115385369A (en)

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Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
GB191003649A (en) * 1910-02-14 1910-09-15 Peder Farup Improvements in Manufacture of Colouring Matters of Great Covering Power and Polishing Powders from Titaniferous Iron Minerals.
US2651563A (en) * 1947-09-24 1953-09-08 Delia J Rentschler Method of preparing pure barium and strontium hydroxides
CN102923748A (en) * 2012-11-30 2013-02-13 长沙矿冶研究院有限责任公司 Method for preparing barium hydroxide by using barium carbonate
CN103387252A (en) * 2013-07-31 2013-11-13 贵州红星发展股份有限公司 Anti-caking high-purity barium hydroxide and preparation method thereof

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
GB191003649A (en) * 1910-02-14 1910-09-15 Peder Farup Improvements in Manufacture of Colouring Matters of Great Covering Power and Polishing Powders from Titaniferous Iron Minerals.
US2651563A (en) * 1947-09-24 1953-09-08 Delia J Rentschler Method of preparing pure barium and strontium hydroxides
CN102923748A (en) * 2012-11-30 2013-02-13 长沙矿冶研究院有限责任公司 Method for preparing barium hydroxide by using barium carbonate
CN103387252A (en) * 2013-07-31 2013-11-13 贵州红星发展股份有限公司 Anti-caking high-purity barium hydroxide and preparation method thereof

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Application publication date: 20221125