CN115215372A - Preparation method of high-concentration antimony pentoxide colloid - Google Patents
Preparation method of high-concentration antimony pentoxide colloid Download PDFInfo
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- CN115215372A CN115215372A CN202210970673.4A CN202210970673A CN115215372A CN 115215372 A CN115215372 A CN 115215372A CN 202210970673 A CN202210970673 A CN 202210970673A CN 115215372 A CN115215372 A CN 115215372A
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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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- 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
- C01P2006/22—Rheological behaviour as dispersion, e.g. viscosity, sedimentation stability
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Abstract
The invention discloses a preparation method of high-concentration antimony pentoxide colloid, which comprises the following steps: adding 180-230g of antimony trioxide into 600-1000g of water, starting a stirring device for stirring, slowly adding 90-120g of hydrogen peroxide, heating to 90-110 ℃, reacting for 1-3 hours, adding 15-25g of a stabilizer, and completely reacting antimony pentoxide to obtain white antimony pentoxide colloid; and (2) cooling the white antimony pentoxide colloid obtained in the step two to 70-100 ℃, adding 3.8-5.6g of phosphoric acid, starting a vacuum device to start concentration, setting the vacuum degree to be-0.05-0.1 Mpa, concentrating until the mass fraction of the antimony pentoxide reaches 35-45%, adding 8-13g of triethanolamine, continuously concentrating until the concentration of the antimony pentoxide reaches 50-55%, adding 12-18g of triethanolamine, and adjusting the pH value to 4-7 to obtain the white high-concentration antimony pentoxide colloid. The invention has the advantages of low viscosity, good dispersibility in solvent, fine colloid particles, white color, wide application, simple and easily obtained raw materials, safe and controllable production process and the like.
Description
Technical Field
The invention belongs to the technical field of nano materials, and particularly relates to a preparation method of a high-concentration antimony pentoxide colloid.
Background
Antimony is a precious non-renewable resource, antimony pentoxide colloid developed at home at present is mainly used in the field of petroleum passivators, and antimony is used as an important component for passivating nickel, can be applied to an oil refining catalytic cracking device, and increases the yield of finished oil; antimony pentoxide colloid produced by the prior art at home at present is transparent colloid, organic acid and triethanolamine and the like are used as stabilizers, although the antimony pentoxide colloid has the advantage of high transparency, along with the increase of the antimony pentoxide content, the antimony pentoxide colloid is concentrated to about 42 percent of the antimony pentoxide content, the colloid viscosity is obviously increased, and the colloid loses fluidity, because the technology needs a large amount of triethanolamine as the stabilizer, the triethanolamine has strong hydrophilicity, the excessive consumption can cause overlarge intermolecular force and overlarge viscosity, the colloid is directly solidified at high concentration, the application range of the antimony pentoxide colloid is single, the antimony pentoxide colloid can only be used as a common water-soluble petroleum additive, the antimony pentoxide colloid is difficult to apply in a polar solvent system, and the antimony pentoxide colloid with high content cannot be used as a flame retardant to be filled into other materials: because the product prepared by the prior art can not be dispersed in a polar solvent, if acrylic fibers are prepared in a Dmac system, the product needs high content of antimony pentoxide, the color needs white and the like, the prior art can not be used as a flame retardant, the color is yellow after drying, the application of the product as the flame retardant influences the color of the product, and domestic research is not reported.
Disclosure of Invention
The invention aims to provide a preparation method of high-concentration antimony pentoxide colloid, which has the advantages of low viscosity, good dispersibility in a solvent, fine colloid particles, white color, wide application, simple and easily-obtained raw materials, safe and controllable production process and the like.
The technical scheme adopted by the invention for solving the technical problems is as follows: a preparation method of high-concentration antimony pentoxide colloid comprises the following steps:
(1) Adding 180-230g of antimony trioxide into 600-1000g of water, starting a stirring device for stirring, slowly adding 90-120g of hydrogen peroxide, heating to 90-110 ℃, reacting for 1-3 hours, adding 15-25g of a stabilizer, and completely reacting antimony pentoxide to obtain white antimony pentoxide colloid;
(2) And (2) cooling the white antimony pentoxide colloid obtained in the step two to 70-100 ℃, adding 3.8-5.6g of phosphoric acid, starting a vacuum device to start concentration, setting the vacuum degree to be-0.05-0.1 Mpa, concentrating until the mass fraction of the antimony pentoxide reaches 35-45%, adding 8-13g of triethanolamine, continuously concentrating until the concentration of the antimony pentoxide reaches 50-55%, adding 12-18g of triethanolamine, and adjusting the pH value to 4-7 to obtain the white high-concentration antimony pentoxide colloid.
Further, the stabilizer is one or more of ammonium dihydrogen phosphate, diammonium hydrogen phosphate, sodium dihydrogen phosphate, disodium hydrogen phosphate, ethanolamine, diethanolamine, triethylamine, N-ethylmorpholine and N-methylmorpholine.
The invention has the following beneficial effects: the colloid prepared by the invention has the advantages of low viscosity, good dispersibility in a solvent, fine colloid particles, white color, wide application, simple and easily obtained raw materials, safe and controllable production process and the like.
Detailed Description
The following are specific examples of the present invention and further describe the technical solutions of the present invention, but the scope of the present invention is not limited to these examples. All changes, modifications and equivalents that do not depart from the spirit of the invention are intended to be included within the scope thereof.
Example 1
A preparation method of high-concentration antimony pentoxide colloid comprises the following steps:
(1) Adding 180g of antimony trioxide into 600g of water, starting a stirring device for stirring, slowly adding 90g of hydrogen peroxide, heating to 90 ℃, reacting for 1 hour, adding 15g of stabilizer, and completely reacting antimony pentoxide to obtain white antimony pentoxide colloid;
(2) And (3) cooling the white antimony pentoxide colloid obtained in the step two to 70 ℃, adding 3.8g of phosphoric acid, starting a vacuum device to start concentration, setting the vacuum degree to be 0.05Mpa, concentrating until the mass fraction of the antimony pentoxide reaches 35%, adding 8g of triethanolamine, continuously concentrating until the concentration of the antimony pentoxide reaches 50%, adding 12g of triethanolamine, and adjusting the pH value to 4 to obtain the white high-concentration antimony pentoxide colloid.
The stabilizer is ammonium dihydrogen phosphate.
Example 2
A preparation method of high-concentration antimony pentoxide colloid comprises the following steps:
(1) Adding 230g of antimony trioxide into 1000g of water, starting a stirring device for stirring, slowly adding 120g of hydrogen peroxide, heating to 110 ℃, reacting for 3 hours, adding 25g of a stabilizer, and completely reacting antimony pentoxide to obtain white antimony pentoxide colloid;
(2) And (3) cooling the white antimony pentoxide colloid obtained in the second step to 100 ℃, adding 5.6g of phosphoric acid, starting a vacuum device to start concentration, setting the vacuum degree to be-0.1 Mpa, concentrating until the mass fraction of the antimony pentoxide reaches 45%, adding 13g of triethanolamine, continuously concentrating until the concentration of the antimony pentoxide reaches 55%, adding 18g of triethanolamine, and adjusting the pH value to 7 to obtain the white high-concentration antimony pentoxide colloid.
The stabilizer is ammonium dihydrogen phosphate, diammonium hydrogen phosphate, sodium dihydrogen phosphate and disodium hydrogen phosphate.
Example 3
A preparation method of high-concentration antimony pentoxide colloid comprises the following steps:
(1) Adding 200g of antimony trioxide into 800g of water, starting a stirring device for stirring, slowly adding 107g of hydrogen peroxide, heating to 100 ℃, reacting for 2 hours, adding 20g of stabilizer, and completely reacting antimony pentoxide to obtain white antimony pentoxide colloid;
(2) And D, cooling the white antimony pentoxide colloid obtained in the step two to 80 ℃, adding 4.9g of phosphoric acid, starting a vacuum device to start concentration, setting the vacuum degree to be 0.08Mpa, concentrating until the mass fraction of the antimony pentoxide reaches 40%, adding 10.5g of triethanolamine, continuously concentrating until the concentration of the antimony pentoxide reaches 53%, adding 15g of triethanolamine, and adjusting the pH value to 6 to obtain the white high-concentration antimony pentoxide colloid.
The stabilizer is N-ethyl morpholine.
Example 4
A preparation method of high-concentration antimony pentoxide colloid comprises the following steps:
(1) Adding 190g of antimony trioxide into 700g of water, starting a stirring device for stirring, slowly adding 102g of hydrogen peroxide, heating to 96 ℃, reacting for 1.5 hours, adding 18g of stabilizer, and completely reacting the antimony pentoxide to obtain white antimony pentoxide colloid;
(2) And (3) cooling the white antimony pentoxide colloid obtained in the step two to 75 ℃, adding 4.3g of phosphoric acid, starting a vacuum device to start concentration, setting the vacuum degree to be 0.06MPa, concentrating until the mass fraction of the antimony pentoxide reaches 37%, adding 9.5g of triethanolamine, continuously concentrating until the concentration of the antimony pentoxide reaches 52%, adding 14g of triethanolamine, and adjusting the pH value to 5 to obtain the white high-concentration antimony pentoxide colloid.
The stabilizer is diammonium hydrogen phosphate, diethanolamine and triethylamine.
Example 5
A preparation method of high-concentration antimony pentoxide colloid is disclosed, which comprises the following steps:
(1) Adding 215g of antimony trioxide into 950g of water, starting a stirring device for stirring, slowly adding 116g of hydrogen peroxide, heating to 106 ℃, reacting for 2.6 hours, adding 22g of stabilizer, and completely reacting antimony pentoxide to obtain white antimony pentoxide colloid;
(2) And D, cooling the white antimony pentoxide colloid obtained in the step two to 94 ℃, adding 5.3g of phosphoric acid, starting a vacuum device to start concentration, setting the vacuum degree to be 0.09Mpa, concentrating until the mass fraction of the antimony pentoxide reaches 42%, adding 11.5g of triethanolamine, continuously concentrating until the concentration of the antimony pentoxide reaches 53%, adding 16g of triethanolamine, and adjusting the pH value to 6 to obtain the white high-concentration antimony pentoxide colloid.
The stabilizer is disodium hydrogen phosphate, ethanolamine, diethanolamine or triethylamine.
Claims (2)
1. A preparation method of high-concentration antimony pentoxide colloid is characterized by comprising the following steps:
(1) Adding 180-230g of antimony trioxide into 600-1000g of water, starting a stirring device for stirring, slowly adding 90-120g of hydrogen peroxide, heating to 90-110 ℃, reacting for 1-3 hours, adding 15-25g of a stabilizer, and completely reacting the antimony pentoxide to obtain white antimony pentoxide colloid;
(2) And (2) cooling the white antimony pentoxide colloid obtained in the step two to 70-100 ℃, adding 3.8-5.6g of phosphoric acid, starting a vacuum device to start concentration, setting the vacuum degree to be-0.05-0.1 Mpa, concentrating until the mass fraction of the antimony pentoxide reaches 35-45%, adding 8-13g of triethanolamine, continuously concentrating until the concentration of the antimony pentoxide reaches 50-55%, adding 12-18g of triethanolamine, and adjusting the pH value to 4-7 to obtain the white high-concentration antimony pentoxide colloid.
2. The method for preparing a high concentration antimony pentoxide colloid according to claim 1, wherein: the stabilizer is one or more of ammonium dihydrogen phosphate, diammonium hydrogen phosphate, sodium dihydrogen phosphate, disodium hydrogen phosphate, ethanolamine, diethanolamine, triethylamine, N-ethylmorpholine and N-methylmorpholine.
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| CN202210970673.4A CN115215372A (en) | 2022-08-13 | 2022-08-13 | Preparation method of high-concentration antimony pentoxide colloid |
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| CN202210970673.4A CN115215372A (en) | 2022-08-13 | 2022-08-13 | Preparation method of high-concentration antimony pentoxide colloid |
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Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4026819A (en) * | 1976-04-09 | 1977-05-31 | N L Industries, Inc. | Production of hydrous pentavalent antimony oxide sol composition, dry powder prepared therefrom, and production of said dry powder |
| US5800740A (en) * | 1996-10-25 | 1998-09-01 | Nyacol Products, Inc. | Antimony pentoxide dispersions and method of making |
| US20080038187A1 (en) * | 2004-09-21 | 2008-02-14 | Nissan Chemical Industries, Ltd. | Process for Producing Antimony Pentaoxide |
| CN101798112A (en) * | 2010-03-25 | 2010-08-11 | 中南大学 | Method for preparing antimony pentoxide hydrosol and dry powder thereof by using composite stabilizer |
| CN111748231A (en) * | 2020-06-28 | 2020-10-09 | 四川硅迪新材料有限公司 | Synthesis method of antimony oxide sol and flame-retardant auxiliary |
-
2022
- 2022-08-13 CN CN202210970673.4A patent/CN115215372A/en active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4026819A (en) * | 1976-04-09 | 1977-05-31 | N L Industries, Inc. | Production of hydrous pentavalent antimony oxide sol composition, dry powder prepared therefrom, and production of said dry powder |
| US5800740A (en) * | 1996-10-25 | 1998-09-01 | Nyacol Products, Inc. | Antimony pentoxide dispersions and method of making |
| US20080038187A1 (en) * | 2004-09-21 | 2008-02-14 | Nissan Chemical Industries, Ltd. | Process for Producing Antimony Pentaoxide |
| CN101798112A (en) * | 2010-03-25 | 2010-08-11 | 中南大学 | Method for preparing antimony pentoxide hydrosol and dry powder thereof by using composite stabilizer |
| CN111748231A (en) * | 2020-06-28 | 2020-10-09 | 四川硅迪新材料有限公司 | Synthesis method of antimony oxide sol and flame-retardant auxiliary |
Non-Patent Citations (1)
| Title |
|---|
| 田春明;石俊瑞;薛恩钰;: "胶态五氧化二锑制备及其稳定性", 化学世界, no. 10 * |
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