CN110902720A - Preparation method of nano antimony pentoxide - Google Patents
Preparation method of nano antimony pentoxide Download PDFInfo
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- CN110902720A CN110902720A CN201911315957.4A CN201911315957A CN110902720A CN 110902720 A CN110902720 A CN 110902720A CN 201911315957 A CN201911315957 A CN 201911315957A CN 110902720 A CN110902720 A CN 110902720A
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- antimony pentoxide
- antimony
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- 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
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y40/00—Manufacture or treatment of nanostructures
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- 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
- C01P2004/64—Nanometer sized, i.e. from 1-100 nanometer
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- 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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- Condensed Matter Physics & Semiconductors (AREA)
- General Physics & Mathematics (AREA)
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Abstract
The invention provides a preparation method of nano antimony pentoxide, which comprises the steps of introducing ozone into an acidic antimony trichloride solution, reacting at the temperature of 20-70 ℃, and aging after the reaction is finished to finally obtain the nano antimony pentoxide with the antimony pentoxide content of more than 96% and the particle size of 2-100 nm. The method belongs to an oxidation method, the process and the equipment are simple, the used oxidant is ozone, the oxidation efficiency is high, and the product purity is high.
Description
Technical Field
The invention relates to the technical field of preparation of nano compounds, in particular to a preparation method of nano antimony pentoxide.
Background
Antimony is a rare and precious metal, the antimony is mainly applied to a flame retardant at present, and antimony products used for the flame retardant mainly comprise antimony pentoxide, antimony trioxide, sodium antimonate and the like, wherein the colloidal antimony pentoxide has good performance and small using amount. The prior preparation methods mainly comprise an oxidation method, an ion exchange method, a mixing and stirring method and an electrodialysis method, but the prior preparation methods have the problems of low oxidation efficiency, low product purity or complex process and equipment.
Disclosure of Invention
The invention aims to provide a preparation method of nano antimony pentoxide, which has the characteristics of simple process and equipment, high oxidation efficiency and high product purity because the used oxidant is ozone.
The technical scheme of the invention is realized as follows:
the invention provides a preparation method of nano antimony pentoxide, which comprises the steps of introducing ozone into an acidic antimony trichloride solution, reacting at the temperature of 20-70 ℃, and aging after the reaction is finished to finally obtain the nano antimony pentoxide with the antimony pentoxide content of more than 96% and the particle size of 2-100 nm.
As a further improvement of the invention, the ozone is introduced in an amount of 10-100 g/h.
As a further improvement of the invention, Sb in the acidic antimony trichloride solution3+The content of ions is 40-60g/L, H+The content of ions is more than 1 mol/L.
As a further improvement of the invention, the temperature of the acidic antimony trichloride solution is 30-70 ℃ when ozone is introduced, and the temperature change is not more than +/-10 ℃.
As a further improvement of the invention, the reaction time is 1 to 50 hours.
As a further improvement of the invention, the aging method is to add an organic solvent and perform standing aging.
As a further improvement of the invention, the organic solvent is selected from one or more of ethyl acetate, ethanol, petroleum ether, n-hexane, cyclohexane, dichloromethane, toluene and acetonitrile.
As a further improvement of the invention, the aging time is 20-30 h.
As a further improvement of the invention, after aging for 5h, the medium is evaporated at low temperature.
As a further improvement of the invention, the low temperature is 35-75 ℃.
The invention has the following beneficial effects:
1. the method belongs to an oxidation method, and has simple process and equipment.
2. The oxidant used in the method is ozone, the oxidation efficiency is high, and the product purity is high.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Example 1
3L of antimony trichloride acidic aqueous solution (wherein [ Sb3+ ] -40 g/L and [ H + ] -2 mol/L) is added into a reactor with a stirrer, the temperature is raised to 20 ℃ by stirring, the temperature is maintained at +/-2 ℃, and ozone (50g/H) is continuously introduced for reaction for 3H. After the reaction is finished, adding petroleum ether, aging at room temperature for 24h, and then carrying out vacuum drying at 70 ℃, wherein the antimony in the antimony pentoxide in the obtained powder accounts for 96.58% of the total antimony. The efficiency of ozone oxidation of antimony trichloride in this process is about 50%.
Example 2
3L of antimony trichloride acidic aqueous solution (wherein [ Sb3+ ] -50 g/L and [ H + ] -2 mol/L) is added into a reactor with a stirrer, the temperature is raised to 20 ℃ by stirring, the temperature is maintained at +/-2 ℃, and ozone (50g/H) is continuously introduced for reaction for 4H. After the reaction is finished, ethyl acetate is added, the mixture is aged for 24 hours at room temperature and then is dried in vacuum at 70 ℃, and the proportion of antimony in the antimony pentoxide in the obtained powder accounts for 97.13 percent of the total antimony. The efficiency of ozone oxidation of antimony trichloride in this process is about 50%.
Example 3
50L of antimony trichloride acidic aqueous solution (wherein [ Sb3+ ] -60g/L and [ H + ] -2 mol/L) is added into a reactor with a stirrer, the temperature is raised to 40 ℃ by stirring, the temperature is maintained at +/-2 ℃, and ozone (50g/H) is continuously introduced for reaction for 40H. After the reaction is finished, adding ethanol, aging at room temperature for 24h, and vacuum drying at 70 ℃ to obtain powder with the particle size of 2-100nm, wherein the antimony in the antimony pentoxide in the powder accounts for 97.32% of the total antimony. The efficiency of ozone oxidation of antimony trichloride in this process was about 70%.
Compared with the prior art, the method belongs to an oxidation method, the process and the equipment are simple, the used oxidant is ozone, the oxidation efficiency is high, and the product purity is high.
The above description is only for the purpose of illustrating the preferred embodiments of the present invention and is not to be construed as limiting the invention, and any modifications, equivalents, improvements and the like that fall within the spirit and principle of the present invention are intended to be included therein.
Claims (10)
1. A preparation method of nanometer antimony pentoxide is characterized in that ozone is introduced into an acidic antimony trichloride solution, reaction is carried out at the temperature of 20-70 ℃, and after the reaction is finished, the nanometer antimony pentoxide with the antimony pentoxide content of more than 96% and the particle size of 2-100nm is finally obtained through aging.
2. The method for preparing nano antimony pentoxide according to claim 1, wherein the ozone is introduced in an amount of 10-100 g/h.
3. The method for preparing nano antimony pentoxide according to claim 1, wherein Sb in the acidic antimony trichloride solution is Sb3+The content of ions is 40-60g/L, H+The content of ions is more than 1 mol/L.
4. The method for preparing nano antimony pentoxide according to claim 1, wherein the temperature of the acidic antimony trichloride solution is 30-70 ℃ when ozone is introduced, and the temperature change is not more than ± 10 ℃.
5. The method for preparing nano antimony pentoxide according to claim 1, wherein the reaction time is 1-50 h.
6. The method for preparing nano antimony pentoxide according to claim 1, wherein the aging method comprises adding an organic solvent, standing and aging.
7. The method for preparing nano antimony pentoxide according to claim 6, wherein the organic solvent is one or more selected from ethyl acetate, ethanol, petroleum ether, n-hexane, cyclohexane, dichloromethane, toluene and acetonitrile.
8. The method for preparing nano antimony pentoxide according to claim 6, wherein the aging time is 20-30 h.
9. The method for preparing nano antimony pentoxide according to any one of claims 1-8, wherein after aging for 5h, the medium is evaporated at low temperature.
10. The method as claimed in claim 9, wherein the low temperature is 35-75 ℃.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
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| CN201911315957.4A CN110902720A (en) | 2019-12-19 | 2019-12-19 | Preparation method of nano antimony pentoxide |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201911315957.4A CN110902720A (en) | 2019-12-19 | 2019-12-19 | Preparation method of nano antimony pentoxide |
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| CN110902720A true CN110902720A (en) | 2020-03-24 |
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| CN201911315957.4A Pending CN110902720A (en) | 2019-12-19 | 2019-12-19 | Preparation method of nano antimony pentoxide |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113060763A (en) * | 2021-03-18 | 2021-07-02 | 刘明钢 | Preparation method of powdery antimony pentoxide applied to optical glass |
Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1074945A (en) * | 1992-01-28 | 1993-08-04 | 锡矿山矿务局 | Chlorinolysis is produced colloidal antimony pentoxide |
| CN101509080A (en) * | 2009-03-24 | 2009-08-19 | 中南大学 | Method for comprehensively processing stibium smelt arsenic alkaline residue and producing colloid antimony peroxide |
| CN104355333A (en) * | 2014-10-31 | 2015-02-18 | 嘉兴职业技术学院 | Preparation method of antimony pentoxide composite powder |
| CN105858724A (en) * | 2016-05-16 | 2016-08-17 | 中南大学 | Method of using solution atomization method to prepare superfine Sb oxide |
| CN109534396A (en) * | 2018-12-26 | 2019-03-29 | 浙江工业大学 | A kind of transition state sb oxide and preparation method thereof |
-
2019
- 2019-12-19 CN CN201911315957.4A patent/CN110902720A/en active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1074945A (en) * | 1992-01-28 | 1993-08-04 | 锡矿山矿务局 | Chlorinolysis is produced colloidal antimony pentoxide |
| CN101509080A (en) * | 2009-03-24 | 2009-08-19 | 中南大学 | Method for comprehensively processing stibium smelt arsenic alkaline residue and producing colloid antimony peroxide |
| CN104355333A (en) * | 2014-10-31 | 2015-02-18 | 嘉兴职业技术学院 | Preparation method of antimony pentoxide composite powder |
| CN105858724A (en) * | 2016-05-16 | 2016-08-17 | 中南大学 | Method of using solution atomization method to prepare superfine Sb oxide |
| CN109534396A (en) * | 2018-12-26 | 2019-03-29 | 浙江工业大学 | A kind of transition state sb oxide and preparation method thereof |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113060763A (en) * | 2021-03-18 | 2021-07-02 | 刘明钢 | Preparation method of powdery antimony pentoxide applied to optical glass |
| CN113060763B (en) * | 2021-03-18 | 2022-11-29 | 刘明钢 | Preparation method of powdery antimony pentoxide applied to optical glass |
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