CN113735169A - Preparation method of high-purity antimony trioxide - Google Patents
Preparation method of high-purity antimony trioxide Download PDFInfo
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- CN113735169A CN113735169A CN202111103025.0A CN202111103025A CN113735169A CN 113735169 A CN113735169 A CN 113735169A CN 202111103025 A CN202111103025 A CN 202111103025A CN 113735169 A CN113735169 A CN 113735169A
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- ADCOVFLJGNWWNZ-UHFFFAOYSA-N antimony trioxide Chemical compound O=[Sb]O[Sb]=O ADCOVFLJGNWWNZ-UHFFFAOYSA-N 0.000 title claims abstract description 144
- 238000002360 preparation method Methods 0.000 title claims abstract description 17
- 238000003756 stirring Methods 0.000 claims abstract description 85
- 238000001914 filtration Methods 0.000 claims abstract description 43
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims abstract description 39
- 238000003723 Smelting Methods 0.000 claims abstract description 25
- 238000001035 drying Methods 0.000 claims abstract description 25
- 239000002244 precipitate Substances 0.000 claims abstract description 23
- 239000012535 impurity Substances 0.000 claims abstract description 11
- BVKZGUZCCUSVTD-UHFFFAOYSA-N carbonic acid Chemical compound OC(O)=O BVKZGUZCCUSVTD-UHFFFAOYSA-N 0.000 claims abstract description 10
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 7
- 239000012153 distilled water Substances 0.000 claims abstract description 6
- 238000000926 separation method Methods 0.000 claims abstract description 6
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims description 22
- 239000001301 oxygen Substances 0.000 claims description 22
- 229910052760 oxygen Inorganic materials 0.000 claims description 22
- 238000001816 cooling Methods 0.000 claims description 17
- 239000011261 inert gas Substances 0.000 claims description 14
- 238000000034 method Methods 0.000 claims description 13
- 238000007664 blowing Methods 0.000 claims description 10
- 239000007789 gas Substances 0.000 claims description 10
- 239000007788 liquid Substances 0.000 claims description 6
- 239000007787 solid Substances 0.000 claims description 5
- 239000004071 soot Substances 0.000 claims description 5
- 239000002699 waste material Substances 0.000 claims description 5
- 238000004519 manufacturing process Methods 0.000 claims description 3
- 239000000126 substance Substances 0.000 abstract description 9
- 239000003513 alkali Substances 0.000 abstract description 7
- 239000002253 acid Substances 0.000 abstract description 6
- 239000000243 solution Substances 0.000 description 22
- MYMOFIZGZYHOMD-UHFFFAOYSA-N Dioxygen Chemical compound O=O MYMOFIZGZYHOMD-UHFFFAOYSA-N 0.000 description 4
- 229910001882 dioxygen Inorganic materials 0.000 description 4
- 230000000694 effects Effects 0.000 description 4
- 238000009853 pyrometallurgy Methods 0.000 description 4
- 238000010438 heat treatment Methods 0.000 description 3
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 2
- FAPDDOBMIUGHIN-UHFFFAOYSA-K antimony trichloride Chemical compound Cl[Sb](Cl)Cl FAPDDOBMIUGHIN-UHFFFAOYSA-K 0.000 description 2
- 239000003795 chemical substances by application Substances 0.000 description 2
- 239000002131 composite material Substances 0.000 description 2
- 239000000843 powder Substances 0.000 description 2
- 238000005406 washing Methods 0.000 description 2
- KZBUYRJDOAKODT-UHFFFAOYSA-N Chlorine Chemical compound ClCl KZBUYRJDOAKODT-UHFFFAOYSA-N 0.000 description 1
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 1
- 239000003929 acidic solution Substances 0.000 description 1
- 239000012670 alkaline solution Substances 0.000 description 1
- 238000005915 ammonolysis reaction Methods 0.000 description 1
- 229910052787 antimony Inorganic materials 0.000 description 1
- WATWJIUSRGPENY-UHFFFAOYSA-N antimony atom Chemical compound [Sb] WATWJIUSRGPENY-UHFFFAOYSA-N 0.000 description 1
- DAMJCWMGELCIMI-UHFFFAOYSA-N benzyl n-(2-oxopyrrolidin-3-yl)carbamate Chemical compound C=1C=CC=CC=1COC(=O)NC1CCNC1=O DAMJCWMGELCIMI-UHFFFAOYSA-N 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 239000000428 dust Substances 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 230000003301 hydrolyzing effect Effects 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- 239000011259 mixed solution Substances 0.000 description 1
- 239000003973 paint Substances 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 239000000049 pigment Substances 0.000 description 1
- 239000004033 plastic Substances 0.000 description 1
- 229920003023 plastic Polymers 0.000 description 1
- 238000000746 purification Methods 0.000 description 1
- 238000010791 quenching Methods 0.000 description 1
- 230000000171 quenching effect Effects 0.000 description 1
- 238000002791 soaking Methods 0.000 description 1
- 239000012463 white pigment Substances 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G30/00—Compounds of antimony
- C01G30/004—Oxides; Hydroxides; Oxyacids
- C01G30/005—Oxides
Abstract
The invention discloses a preparation method of high-purity antimony trioxide, which comprises the following steps: s1, dissolving: putting antimony trioxide in a container containing sodium hydroxide solution, adjusting the pH value to 9-10, and stirring for dissolving for the first time; s2, filtering: filtering undissolved impurities in the container for the first time by using a filter screen, then adding a carbonic acid solution into the container, and adjusting the pH value to 6-6.5; s3, stirring: then stirring the container for the second time, and continuously stirring until precipitates are separated out and ensuring complete separation; s4, filtering and drying: filtering the precipitated antimony trioxide for the second time, drying, adding distilled water, and repeatedly filtering and drying for three to four times to obtain a dried precipitate; s5, high-temperature smelting: and placing the precipitate in a smelting furnace. The preparation method of the high-purity antimony trioxide can be used for treating substances which are insoluble in alkali and soluble in acid and can also be used for removing impurities of other substances in an auxiliary manner.
Description
Technical Field
The invention belongs to the technical field of preparation and processing of antimony trioxide, and particularly relates to a preparation method of high-purity antimony trioxide.
Background
Antimony trioxide is a white powder and insoluble in water, soluble in sodium hydroxide solution and acid. It is used for white pigment, paint and plastics, and has functions of pigment and flame-retarding.
The Chinese patent document discloses a preparation method of high-purity antimony trioxide (application publication No. CN102020313A), which comprises the steps of rectifying antimony trichloride, hydrolyzing, ammonolysis, washing and the like, so as to prepare the high-purity antimony trioxide. The method has the advantages of simple process steps, higher production efficiency and low cost, and the antimony trioxide obtained by the method has high purity and low impurity content and can meet the urgent needs of the current market.
The Chinese patent document discloses a preparation method of high-purity antimony trioxide (application publication No. CN113277555A), which comprises the steps of adding crude antimony ore into a hydrochloric acid solution for soaking, introducing chlorine gas, adding iron powder into an obtained antimony chloride mixed solution, and reacting to obtain an antimony chloride solution; adding a proper amount of 4mol/L sodium hydroxide solution with the pH value of 8-9, stirring, filtering, washing, drying, and roasting in an air atmosphere to obtain antimony trioxide; and (3) gasifying the antimony trioxide into liquid, introducing compressed air and the composite lead removing agent, gasifying and quenching the prepared antimony trioxide powder, and obtaining the high-purity antimony trioxide. The method provided by the invention has the advantages of simple preparation, small usage amount of the composite lead removing agent, lower cost, recyclability, no burden on the environment, high purity of the prepared antimony trioxide up to 99.5%, nano-scale granularity and uniform particle size distribution.
The purification process of the antimony trioxide in the prior art is dissolved in acid and then dissolved in alkali, and the mode has weak impurity removal capability for substances which are easily dissolved in acid and are difficultly dissolved in alkali.
Therefore, in view of the current situation, the design and production of a preparation method of high-purity antimony trioxide are urgently needed to meet the requirement of practical use.
Disclosure of Invention
The present invention aims to provide a method for preparing high-purity antimony trioxide, which solves the problems in the background art.
In order to achieve the purpose, the invention provides the following technical scheme: a preparation method of high-purity antimony trioxide comprises the following steps:
s1, dissolving: putting antimony trioxide in a container containing sodium hydroxide solution, adjusting the pH value to 9-10, and stirring for dissolving for the first time;
s2, filtering: filtering undissolved impurities in the container for the first time by using a filter screen, then adding a carbonic acid solution into the container, and adjusting the pH value to 6-6.5;
s3, stirring: then stirring the container for the second time, and continuously stirring until precipitates are separated out and ensuring complete separation;
s4, filtering and drying: filtering the precipitated antimony trioxide for the second time, drying, adding distilled water, and repeatedly filtering and drying for three to four times to obtain a dried precipitate;
s5, high-temperature smelting: placing the precipitate in a smelting furnace, raising the furnace temperature to 700-750 ℃ until the precipitate is melted into liquid, then introducing oxygen with a certain flow speed into the smelting furnace, and blowing away the unliquefied waste ash;
s6, cooling: and raising the temperature of the smelting furnace with soot blowing to 1600-1700 ℃, fully gasifying the liquefied antimony trioxide, introducing the gasified antimony trioxide into a cooling and settling device, introducing inert gas into the cooling and settling device, cooling the gasified antimony trioxide to liquefy, and finally solidifying into solid, thereby obtaining the high-purity antimony trioxide.
In a further embodiment, the stirring time of the first stirring is set to be 30-50 minutes, the stirring speed of the first stirring is set to be 100-200 rpm, and the stirring temperature of the first stirring is set to be 60-70 ℃.
In a further embodiment, the stirring time of the second stirring is set to be 50-60 minutes, the stirring speed of the second stirring is set to be 400-500 rpm, and the stirring temperature of the second stirring is set to be 20-30 ℃.
In a further embodiment, the temperature of the filter drying is set at 110-120 ℃.
In a further embodiment, the concentration of the sodium hydroxide solution is set to 4-6 moles per liter and the carbonation solution is set to 3-4 moles per liter.
In a further embodiment, the oxygen introducing direction and the gas outlet direction of the pyrometallurgical process are symmetrically arranged, and the height of the gas outlet direction is higher than that of the oxygen introducing direction.
In a further embodiment, the pyrometallurgical oxygen gas is introduced at a rate of 2-4 liters per minute and the inert gas is introduced at a rate of 0.1-0.2 liters per minute.
In a further embodiment, the temperature of the oxygen for pyrometallurgical treatment is set to 700-.
In a further embodiment, the mesh number of the filter screen for the first filtration is set to 500-600 mesh, and the mesh number of the filter screen for the second filtration is set to 800-900 mesh.
The invention has the technical effects and advantages that: according to the preparation method of the high-purity antimony trioxide, the alkaline solution is added to dissolve the antimony trioxide to treat substances which are difficult to dissolve in the alkali, and then the acidic solution destroys the alkaline environment, so that the antimony trioxide is separated out, and the treatment effect on the substances which are difficult to dissolve in the alkali can be ensured; the treatment effect of other ions in the solution can be ensured by multiple times of filtering and drying, so that the purity of the precipitated antimony trioxide is ensured, and the antimony trioxide is not accidentally reduced by the treatment of the introduced oxygen in the high-temperature smelting, and the unliquefied substances can be blown with dust to remove impurities; the preparation method of the high-purity antimony trioxide can be used for treating substances which are insoluble in alkali and soluble in acid and can also be used for removing impurities of other substances in an auxiliary manner.
Detailed Description
In the following description, numerous specific details are set forth in order to provide a more thorough understanding of the present invention. It will be apparent, however, to one skilled in the art, that the present invention may be practiced without one or more of these specific details. In other instances, well-known features have not been described in order to avoid obscuring the invention.
Example 1
The invention provides a preparation method of high-purity antimony trioxide, which comprises the following steps:
s1, dissolving: putting antimony trioxide in a container containing sodium hydroxide solution, adjusting the pH value to 9, and stirring for dissolving for the first time;
s2, filtering: filtering undissolved impurities in the container for the first time by using a filter screen, then adding a carbonic acid solution into the container, and adjusting the pH value to 6;
s3, stirring: then stirring the container for the second time, and continuously stirring until precipitates are separated out and ensuring complete separation;
s4, filtering and drying: filtering the precipitated antimony trioxide for the second time, drying, adding distilled water, and repeatedly filtering and drying for four times to obtain a dried precipitate;
s5, high-temperature smelting: placing the precipitate in a smelting furnace, raising the furnace temperature to 700 ℃ until the precipitate is melted into liquid, then introducing oxygen with a certain flow speed into the smelting furnace, and blowing away the unliquefied waste ash;
s6, cooling: and (3) heating the smelting furnace with the soot blowing completed to 1600 ℃ to fully gasify the liquefied antimony trioxide, introducing the gasified antimony trioxide into a cooling and settling device, introducing inert gas into the cooling and settling device to cool and liquefy the gasified antimony trioxide, and finally solidifying the gasified antimony trioxide into a solid, thereby obtaining the high-purity antimony trioxide.
In a further embodiment, the stirring time of the first stirring is set to 30 minutes, the stirring speed of the first stirring is set to 100 revolutions per minute, and the stirring temperature of the first stirring is set to 60 degrees celsius.
In a further embodiment, the stirring time of the second stirring is set to 50 minutes, the stirring speed of the second stirring is set to 400 revolutions per minute, and the stirring temperature of the second stirring is set to 20 degrees celsius.
In a further embodiment, the temperature of the filter drying is set to 110 degrees celsius.
In a further embodiment, the concentration of the sodium hydroxide solution is set to 4 moles per liter and the carbonic acid solution is set to 3 moles per liter.
In a further embodiment, the oxygen introducing direction and the gas outlet direction of the pyrometallurgical process are symmetrically arranged, and the height of the gas outlet direction is higher than that of the oxygen introducing direction.
In a further embodiment, the pyrometallurgical oxygen gas introduction rate is set to 2 liters per minute and the inert gas introduction rate is set to 0.1 liters per minute.
In a further embodiment, the temperature of the pyrometallurgical oxygen is set to 700 degrees celsius and the temperature of the inert gas is set to ambient temperature.
In a further embodiment, the mesh number of the first-time filtering filter screen is set to be 500 meshes, and the mesh number of the second-time filtering filter screen is set to be 800 meshes.
Example 2
The invention provides a preparation method of high-purity antimony trioxide, which comprises the following steps:
s1, dissolving: putting antimony trioxide in a container containing sodium hydroxide solution, adjusting the pH value to 10, and stirring for dissolving for the first time;
s2, filtering: filtering undissolved impurities in the container for the first time by using a filter screen, then adding a carbonic acid solution into the container, and adjusting the pH value to 6.5;
s3, stirring: then stirring the container for the second time, and continuously stirring until precipitates are separated out and ensuring complete separation;
s4, filtering and drying: filtering the precipitated antimony trioxide for the second time, drying, adding distilled water, and repeatedly filtering and drying for four times to obtain a dried precipitate;
s5, high-temperature smelting: placing the precipitate in a smelting furnace, raising the furnace temperature to 750 ℃ until the precipitate is melted into liquid, then introducing oxygen with a certain flow speed into the smelting furnace, and blowing away the unliquefied waste ash;
s6, cooling: and (3) heating the smelting furnace with the soot blowing completed to 1700 ℃ to fully gasify the liquefied antimony trioxide, introducing the gasified antimony trioxide into a cooling and settling device, introducing inert gas into the cooling and settling device to cool and liquefy the gasified antimony trioxide, and finally solidifying the gasified antimony trioxide into a solid, thereby obtaining the high-purity antimony trioxide.
In a further embodiment, the stirring time of the first stirring is set to 50 minutes, the stirring speed of the first stirring is set to 200 revolutions per minute, and the stirring temperature of the first stirring is set to 70 degrees celsius.
In a further embodiment, the stirring time of the second stirring is set to 60 minutes, the stirring speed of the second stirring is set to 500 revolutions per minute, and the stirring temperature of the second stirring is set to 30 degrees celsius.
In a further embodiment, the temperature of the filter drying is set to 120 degrees celsius.
In a further embodiment, the concentration of the sodium hydroxide solution is set at 6 moles per liter and the carbonic acid solution is set at 4 moles per liter.
In a further embodiment, the oxygen introducing direction and the gas outlet direction of the pyrometallurgical process are symmetrically arranged, and the height of the gas outlet direction is higher than that of the oxygen introducing direction.
In a further embodiment, the pyrometallurgical oxygen gas introduction rate is set to 4 liters per minute and the inert gas introduction rate is set to 0.2 liters per minute.
In a further embodiment, the temperature of the pyrometallurgical oxygen is set to 750 degrees celsius and the temperature of the inert gas is set to ambient temperature.
In a further embodiment, the mesh number of the first-time filtering filter screen is set to 600 meshes, and the mesh number of the second-time filtering filter screen is set to 900 meshes.
Example 3
The invention provides a preparation method of high-purity antimony trioxide, which comprises the following steps:
s1, dissolving: putting antimony trioxide in a container containing sodium hydroxide solution, adjusting the pH value to 9.5, and stirring for dissolving for the first time;
s2, filtering: filtering undissolved impurities in the container for the first time by using a filter screen, then adding a carbonic acid solution into the container, and adjusting the pH value to 6.25;
s3, stirring: then stirring the container for the second time, and continuously stirring until precipitates are separated out and ensuring complete separation;
s4, filtering and drying: filtering the precipitated antimony trioxide for the second time, drying, adding distilled water, and repeatedly filtering and drying for three times to obtain a dried precipitate;
s5, high-temperature smelting: placing the precipitate in a smelting furnace, raising the furnace temperature to 725 ℃ until the precipitate is melted into liquid, introducing oxygen with a certain flow speed into the smelting furnace, and blowing away the unliquefied waste ash;
s6, cooling: and (3) heating the smelting furnace with the soot blowing completed to 1650 ℃ to fully gasify the liquefied antimony trioxide, introducing the gasified antimony trioxide into a cooling and settling device, introducing inert gas into the cooling and settling device to cool the gasified antimony trioxide to liquefy, and finally solidifying into solid, thereby obtaining the high-purity antimony trioxide.
In a further embodiment, the stirring time of the first stirring is set to 40 minutes, the stirring speed of the first stirring is set to 1500 revolutions per minute, and the stirring temperature of the first stirring is set to 65 degrees celsius.
In a further embodiment, the stirring time of the second stirring is set to 55 minutes, the stirring speed of the second stirring is set to 450 revolutions per minute, and the stirring temperature of the second stirring is set to 25 degrees celsius.
In a further embodiment, the temperature of the filter drying is set to 1150 degrees celsius.
In a further embodiment, the concentration of the sodium hydroxide solution is set at 5 moles per liter and the carbonic acid solution is set at 3.5 moles per liter.
In a further embodiment, the oxygen introducing direction and the gas outlet direction of the pyrometallurgical process are symmetrically arranged, and the height of the gas outlet direction is higher than that of the oxygen introducing direction.
In a further embodiment, the pyrometallurgical oxygen gas introduction rate is set to 3 liters per minute and the inert gas introduction rate is set to 0.15 liters per minute.
In a further embodiment, the temperature of the pyrometallurgical oxygen is set to 725 degrees celsius and the temperature of the inert gas is set to ambient temperature.
In a further embodiment, the mesh number of the first-time filtering filter screen is set to be 550 meshes, and the mesh number of the second-time filtering filter screen is set to be 850 meshes.
Through multiple experiments of workers, the substances which are easily soluble in acid and alkali can be treated in the examples 1, 2 and 3, and the effect of the example 3 is the best.
The above description is only for the preferred embodiment of the present invention, but the scope of the present invention is not limited thereto, and any person skilled in the art should be considered to be within the technical scope of the present invention, and the technical solutions and the inventive concepts thereof according to the present invention should be equivalent or changed within the scope of the present invention.
Claims (9)
1. A preparation method of high-purity antimony trioxide is characterized by comprising the following steps: the method comprises the following steps:
s1, dissolving: putting antimony trioxide in a container containing sodium hydroxide solution, adjusting the pH value to 9-10, and stirring for dissolving for the first time;
s2, filtering: filtering undissolved impurities in the container for the first time by using a filter screen, then adding a carbonic acid solution into the container, and adjusting the pH value to 6-6.5;
s3, stirring: then stirring the container for the second time, and continuously stirring until precipitates are separated out and ensuring complete separation;
s4, filtering and drying: filtering the precipitated antimony trioxide for the second time, drying, adding distilled water, and repeatedly filtering and drying for three to four times to obtain a dried precipitate;
s5, high-temperature smelting: placing the precipitate in a smelting furnace, raising the furnace temperature to 700-750 ℃ until the precipitate is melted into liquid, then introducing oxygen with a certain flow speed into the smelting furnace, and blowing away the unliquefied waste ash;
s6, cooling: and raising the temperature of the smelting furnace with soot blowing to 1600-1700 ℃, fully gasifying the liquefied antimony trioxide, introducing the gasified antimony trioxide into a cooling and settling device, introducing inert gas into the cooling and settling device, cooling the gasified antimony trioxide to liquefy, and finally solidifying into solid, thereby obtaining the high-purity antimony trioxide.
2. The method for preparing high-purity antimony trioxide according to claim 1, characterized in that: the stirring time of the first stirring is set to be 30-50 minutes, the stirring speed of the first stirring is set to be 100-200 revolutions per minute, and the stirring temperature of the first stirring is set to be 60-70 ℃.
3. The method for preparing high-purity antimony trioxide according to claim 1, characterized in that: the stirring time of the second stirring is set to be 50-60 minutes, the stirring speed of the second stirring is set to be 400-500 rpm, and the stirring temperature of the second stirring is set to be 20-30 ℃.
4. The method for preparing high-purity antimony trioxide according to claim 1, characterized in that: the temperature of the filtration drying is set to 110-120 ℃.
5. The method for preparing high-purity antimony trioxide according to claim 1, characterized in that: the concentration of the sodium hydroxide solution is set to be 4-6 mol/L, and the concentration of the carbonic acid solution is set to be 3-4 mol/L.
6. The method for preparing high-purity antimony trioxide according to claim 1, characterized in that: the oxygen introducing direction and the gas outlet direction of the high-temperature smelting are symmetrically arranged, and the height of the gas outlet direction is higher than that of the oxygen introducing direction.
7. The method for preparing high-purity antimony trioxide according to claim 1, characterized in that: the introduction rate of oxygen for pyrometallurgical operation is set to 2-4 liters per minute and the introduction rate of inert gas is set to 0.1-0.2 liters per minute.
8. The method for producing high-purity antimony trioxide according to claim 7, wherein: the temperature of the oxygen for high-temperature smelting is set to 700-750 ℃, and the temperature of the inert gas is set to normal temperature.
9. The method for preparing high-purity antimony trioxide according to claim 1, characterized in that: the mesh number of the filter screen for the first filtration is set to be 500-600 meshes, and the mesh number of the filter screen for the second filtration is set to be 800-900 meshes.
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CN115305361A (en) * | 2022-08-26 | 2022-11-08 | 山东恒邦冶炼股份有限公司 | High-purity antimony rod and high-purity antimony white combined preparation process |
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CN115305361A (en) * | 2022-08-26 | 2022-11-08 | 山东恒邦冶炼股份有限公司 | High-purity antimony rod and high-purity antimony white combined preparation process |
CN115305361B (en) * | 2022-08-26 | 2023-05-09 | 山东恒邦冶炼股份有限公司 | High-purity antimony rod and high-purity antimony white combined preparation process |
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