CN104591278A - Preparation method of colloidal antimony pentoxide - Google Patents
Preparation method of colloidal antimony pentoxide Download PDFInfo
- Publication number
- CN104591278A CN104591278A CN201310520330.9A CN201310520330A CN104591278A CN 104591278 A CN104591278 A CN 104591278A CN 201310520330 A CN201310520330 A CN 201310520330A CN 104591278 A CN104591278 A CN 104591278A
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- CN
- China
- Prior art keywords
- antimony pentoxide
- preparation
- phosphoric acid
- colloidal antimony
- trolamine
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- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
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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
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/22—Rheological behaviour as dispersion, e.g. viscosity, sedimentation stability
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Inorganic Compounds Of Heavy Metals (AREA)
- Colloid Chemistry (AREA)
Abstract
The invention discloses a preparation method of colloidal antimony pentoxide. The preparation method comprises following steps, step1, triethanolamine is delivered into a beaker filled with water, phosphoric acid is added, and triethanolamine phosphate is obtained via 10min of ultrasonic treatment; step 2, the obtained triethanolamine phosphate is delivered into a three-mouth flask filled with antimonous oxide powder, an obtained mixture is stirred, is heated to 95 to 100 DEG C, and is subjected to constant temperature heating, wherein the three-mouth flask is provided with a magnetic stirring apparatus and a reflux condensing tube; step 3, oxidizing agent hydrogen peroxide is added dropwise using a constant-pressure funnel with full stirring, and after adding, an obtained mixed material is subjected to oxidation refluxing for 30min; and step 4, colloidal antimony pentoxide dry powder is obtained via evaporation, condensation, and drying of an obtained hydrosol. The preparation method is simple; production period is short; energy consumption is low; particle size distribution of the obtained antimony pentoxide colloid particles is uniform; and colloid particle dispersion degree is high.
Description
Technical field
The present invention relates to a kind of preparation method of compound, be specifically related to a kind of preparation method of colloidal antimony pentoxide.
Background technology
Colloidal antimony pentoxide has larger specific surface area, higher thermostability, stronger covering power and transparency and by as important fire retardant material, is widely used as the fire retardant of the products such as rubber.The production method production cycle of current colloidal antimony pentoxide is longer, and power consumption is comparatively large, and the Diantimony Pentoxide Colloid particle diameter produced is comparatively large, size distribution is uneven, colloidal particle degree of scatter is not high.
Summary of the invention
The object of the invention is to, provide a kind of preparation method of colloidal antimony pentoxide, technique is simple, with short production cycle, consumes energy low, and the Diantimony Pentoxide Colloid uniform particle produced.
The preparation method of described colloidal antimony pentoxide, it comprises the following steps:
One, trolamine is added fill in the beaker of water, add phosphoric acid, produce trolamine phosphoric acid salt through ultrasonic 10min;
Two, above-mentioned trolamine phosphoric acid salt is added antimonous oxide powder is housed, with in the there-necked flask of magnetic stirring apparatus and reflux condensing tube, stirs and be warming up to 95 DEG C-100 DEG C, thermostatically heating;
Three, under fully stirring, drip oxidant hydrogen peroxide by constant pressure funnel with the speed of 0.02ml/s, dropwise, continue oxidation back flow reaction 30min;
Four, the water-sol evaporated, concentrate, be drying to obtain colloidal antimony pentoxide dry powder.
The preparation method of colloidal antimony pentoxide provided by the invention, its beneficial effect is, technique is simple, with short production cycle, consumes energy low, and the Diantimony Pentoxide Colloid particle diameter produced is evenly distributed, and colloidal particle degree of scatter is high.
Embodiment
Below in conjunction with an embodiment, the preparation method of colloidal antimony pentoxide provided by the invention is described in detail.
Embodiment
One, 306g trolamine is added in the beaker filling 1L water, add 79g phosphoric acid, produce trolamine phosphoric acid salt through ultrasonic 10min;
Two, above-mentioned trolamine phosphoric acid salt is added 1kg antimonous oxide powder is housed, with in the 2L there-necked flask of magnetic stirring apparatus and reflux condensing tube, stirs and be warming up to 95 DEG C-100 DEG C, thermostatically heating;
Three, under fully stirring, dripped the oxidant hydrogen peroxide 1.16kg of 30% with the speed of 0.02ml/s by constant pressure funnel, dropwise, continue oxidation back flow reaction 30min, along with antimonous oxide is become antimony peroxide by hydrogen peroxide oxidation, when the concentration of antimony peroxide is greater than its solubleness in water, antimony peroxide will be separated out from water with the form of solid phase, form initial glue core, adsorption zone charged particle, finally forms colloidal sol;
Four, the water-sol evaporated, concentrate, be drying to obtain colloidal antimony pentoxide dry powder.
Claims (1)
1. a preparation method for colloidal antimony pentoxide, is characterized in that: it comprises the following steps:
One, trolamine is added fill in the beaker of water, add phosphoric acid, produce trolamine phosphoric acid salt through ultrasonic 10min;
Two, above-mentioned trolamine phosphoric acid salt is added antimonous oxide powder is housed, with in the there-necked flask of magnetic stirring apparatus and reflux condensing tube, stirs and be warming up to 95 DEG C-100 DEG C, thermostatically heating;
Three, under fully stirring, drip oxidant hydrogen peroxide by constant pressure funnel with the speed of 0.02ml/s, dropwise, continue oxidation back flow reaction 30min;
Four, the water-sol evaporated, concentrate, be drying to obtain colloidal antimony pentoxide dry powder.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201310520330.9A CN104591278A (en) | 2013-10-30 | 2013-10-30 | Preparation method of colloidal antimony pentoxide |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201310520330.9A CN104591278A (en) | 2013-10-30 | 2013-10-30 | Preparation method of colloidal antimony pentoxide |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN104591278A true CN104591278A (en) | 2015-05-06 |
Family
ID=53117395
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201310520330.9A Pending CN104591278A (en) | 2013-10-30 | 2013-10-30 | Preparation method of colloidal antimony pentoxide |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN104591278A (en) |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104828866A (en) * | 2015-06-09 | 2015-08-12 | 锡矿山闪星锑业有限责任公司 | Colloidal antimony oxide powder low in volatility at high temperature and preparing method thereof |
| CN111153435A (en) * | 2020-01-06 | 2020-05-15 | 于淮旭 | Preparation method of antimony pentoxide crystal flame retardant |
| CN111977687A (en) * | 2020-09-08 | 2020-11-24 | 锡矿山闪星锑业有限责任公司 | Device and method for manufacturing colloidal antimony pentoxide |
| CN112960693A (en) * | 2021-04-16 | 2021-06-15 | 海宁恒爱新材料有限公司 | Preparation method of antimony pentoxide colloid for flame retardance of fabric |
| CN117756177A (en) * | 2024-01-23 | 2024-03-26 | 锡矿山闪星锑业有限责任公司 | Preparation method of powdery antimony pentoxide |
-
2013
- 2013-10-30 CN CN201310520330.9A patent/CN104591278A/en active Pending
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104828866A (en) * | 2015-06-09 | 2015-08-12 | 锡矿山闪星锑业有限责任公司 | Colloidal antimony oxide powder low in volatility at high temperature and preparing method thereof |
| CN111153435A (en) * | 2020-01-06 | 2020-05-15 | 于淮旭 | Preparation method of antimony pentoxide crystal flame retardant |
| CN111977687A (en) * | 2020-09-08 | 2020-11-24 | 锡矿山闪星锑业有限责任公司 | Device and method for manufacturing colloidal antimony pentoxide |
| CN111977687B (en) * | 2020-09-08 | 2024-03-26 | 锡矿山闪星锑业有限责任公司 | Device and method for preparing colloidal antimony pentoxide |
| CN112960693A (en) * | 2021-04-16 | 2021-06-15 | 海宁恒爱新材料有限公司 | Preparation method of antimony pentoxide colloid for flame retardance of fabric |
| CN117756177A (en) * | 2024-01-23 | 2024-03-26 | 锡矿山闪星锑业有限责任公司 | Preparation method of powdery antimony pentoxide |
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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: 20150506 |