CN104512926A - Preparation method of rhombic antimony (III) trioxide - Google Patents
Preparation method of rhombic antimony (III) trioxide Download PDFInfo
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- CN104512926A CN104512926A CN201310444555.0A CN201310444555A CN104512926A CN 104512926 A CN104512926 A CN 104512926A CN 201310444555 A CN201310444555 A CN 201310444555A CN 104512926 A CN104512926 A CN 104512926A
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- antimony
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- rhombic
- trioxide
- iii
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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
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/30—Particle morphology extending in three dimensions
- C01P2004/39—Particle morphology extending in three dimensions parallelepiped-like
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Inorganic Compounds Of Heavy Metals (AREA)
Abstract
The invention discloses a preparation method of rhombic antimony (III) trioxide. The preparation method comprises the following steps: step one, preparing antimony trichloride, a sodium hydroxide solution, and triethanolamine, dissolving antimony trichloride into waterless ethanol, and then saving the solution for later use; step two, adding the sodium hydroxide solution and triethanolamine into the obtained ethanol solution, and then dropwise adding a waterless ethanol solution of antimony trichloride under stirring; step three, after reaction, allowing the system to stand still to precipitate, then pouring the supernate so as to obtain an antimony hydroxide-triethanolamine precursor, and then dropwise adding the precursor into deionized water under stirring; step four, adjusting the temperature to 60 DEG C, carrying out aging, then performing centrifugal separation, and finally drying so as to obtain the nano crystal powder of rhombic antimony (III) trioxide. The provided preparation method has the advantages that the raw materials are cheap, the impurities can be easily removed, the obtained product particles are spherical, the particles are evenly distributed, the crystallization is complete, and thus the prepared rhombic antimony (III) trioxide can be better dispersed in paints and plastic and attached on fibers.
Description
Technical field
The present invention relates to a kind of preparation method of inorganic Sb system fire retardant, be specifically related to a kind of preparation method of antimonous oxide.
Background technology
Sb system fire retardant is one of most important inorganic combustion inhibitor, and when they are used alone, fire retardation is very little, but with halogenated flame retardant and the used time, greatly can improve the usefulness of halogen flame.
Antimonous oxide is one of Sb system fire retardant principal item, to add in plastics, coating and fiber after antimonous oxide nanometer, form inorganic organic polymer nano composite material, the fire-resistant synergistic of antimonous oxide and the flame retardant resistance of flame retardant resistance and whole material will be significantly improved on the one hand, also can improve the physicochemical property of matrix material on the other hand significantly.
At present, the preparation method of antimonous oxide powder has dry method and wet method two class, and all dry method all need some specific installation, and wet method is easy to carry out, and what wet method was conventional is alkoxide hydrolysis, but expensive starting materials.
Summary of the invention
For solving the problem, the object of the invention is to, a kind of preparation method of oblique side's antimonous oxide is provided, while reduction production cost, obtain oblique side's antimonous oxide that particle distribution is even, crystallization is complete nanocrystalline.
A preparation method for oblique side's antimonous oxide, it comprises the following steps:
One, 1:3:2 gets butter of antimony, sodium hydroxide solution and trolamine in molar ratio, and butter of antimony is dissolved in dehydrated alcohol, for subsequent use;
Two, sodium hydroxide solution and trolamine are added in ethanol, then under agitation instill the ethanol solution of butter of antimony;
Three, after having reacted, place precipitation 0.5-1h, incline and supernatant liquid, obtain antimony hydroxide-trolamine presoma, then this presoma is under agitation instilled in deionized water;
Four, temperature adjustment to 60 DEG C, ageing, centrifugation, dry, obtain tiltedly square antimonous oxide nanocrystalline powder.
The preparation method of oblique side's antimonous oxide provided by the invention, its beneficial effect is, raw material is cheap, impurity easily removes, and the product pellet obtained is spherical, and particle distribution is even, crystallization is complete, is more conducive to the dispersion in plastics, coating and the attachment on fiber.
Embodiment
Below in conjunction with an embodiment, the preparation method of oblique side's antimonous oxide provided by the invention is described in detail.
Embodiment
One, 1:3:2 gets butter of antimony, sodium hydroxide solution and trolamine in molar ratio, and butter of antimony is dissolved in dehydrated alcohol, for subsequent use;
Two, sodium hydroxide solution and trolamine are added in ethanol, then under agitation instill the ethanol solution of butter of antimony, see that rapidly white depositions is produced;
Three, react 30min, place, precipitation 1h, incline and supernatant liquid, obtain antimony hydroxide-trolamine presoma, then under agitation instilled in deionized water by this presoma, and control pH is in acid range, flocks is separated out rapidly from presoma;
Four, temperature adjustment to 60 DEG C, ageing 4h, centrifugation, product drying, obtains tiltedly square antimonous oxide nanocrystalline powder.
Claims (1)
1. a preparation method for oblique side's antimonous oxide, is characterized in that: it comprises the following steps:
One, 1:3:2 gets butter of antimony, sodium hydroxide solution and trolamine in molar ratio, and butter of antimony is dissolved in dehydrated alcohol, for subsequent use;
Two, sodium hydroxide solution and trolamine are added in ethanol, then under agitation instill the ethanol solution of butter of antimony;
Three, after having reacted, place precipitation 0.5-1h, incline and supernatant liquid, obtain antimony hydroxide-trolamine presoma, then this presoma is under agitation instilled in deionized water;
Four, temperature adjustment to 60 DEG C, ageing, centrifugation, dry, obtain tiltedly square antimonous oxide nanocrystalline powder.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201310444555.0A CN104512926A (en) | 2013-09-27 | 2013-09-27 | Preparation method of rhombic antimony (III) trioxide |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201310444555.0A CN104512926A (en) | 2013-09-27 | 2013-09-27 | Preparation method of rhombic antimony (III) trioxide |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN104512926A true CN104512926A (en) | 2015-04-15 |
Family
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Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201310444555.0A Pending CN104512926A (en) | 2013-09-27 | 2013-09-27 | Preparation method of rhombic antimony (III) trioxide |
Country Status (1)
| Country | Link |
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| CN (1) | CN104512926A (en) |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106904943A (en) * | 2017-03-16 | 2017-06-30 | 贵州理工学院 | A kind of method for preparing oxidation Sb film in situ |
| CN112499680A (en) * | 2020-12-17 | 2021-03-16 | 南昌大学 | Preparation method of spherical nano antimony trioxide |
-
2013
- 2013-09-27 CN CN201310444555.0A patent/CN104512926A/en active Pending
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106904943A (en) * | 2017-03-16 | 2017-06-30 | 贵州理工学院 | A kind of method for preparing oxidation Sb film in situ |
| CN106904943B (en) * | 2017-03-16 | 2020-07-14 | 贵州理工学院 | Method for in-situ preparation of antimony oxide film |
| CN112499680A (en) * | 2020-12-17 | 2021-03-16 | 南昌大学 | Preparation method of spherical nano antimony trioxide |
| CN112499680B (en) * | 2020-12-17 | 2021-06-29 | 南昌大学 | Preparation method of spherical nano antimony trioxide |
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Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| WD01 | Invention patent application deemed withdrawn after publication |
Application publication date: 20150415 |
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| WD01 | Invention patent application deemed withdrawn after publication |