CN101182040A - Method for producing ultra-fine tungsten oxide - Google Patents
Method for producing ultra-fine tungsten oxide Download PDFInfo
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- CN101182040A CN101182040A CNA2007101955429A CN200710195542A CN101182040A CN 101182040 A CN101182040 A CN 101182040A CN A2007101955429 A CNA2007101955429 A CN A2007101955429A CN 200710195542 A CN200710195542 A CN 200710195542A CN 101182040 A CN101182040 A CN 101182040A
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- tungsten oxide
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- fine tungsten
- ammonium tungstate
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Abstract
The invention relates to a production method of superfine tungsten oxide, in particular to a method for producing colloidal powder by a hydrometallurgical technique. The method is characterized in that the invention has the producing processes that ammonium tungstate solution which is used as raw material is added into hot salpeter solution and then yellow tungstic acid sedimentation is obtained by stirring; the superfine tungsten oxide is generated after the processes of filtration, sedimentation, drying, calcination and comminution by gas stream. The method of the invention has cheap and easily available raw material, simple production technique and equipment, low production cost, high productivity and small particle size and high purity of products.
Description
Technical field
A kind of production method of ultra-fine tungsten oxide relates to a kind of method that adopts hydrometallurgy to produce ultrafine powder.
Background technology
As transistion metal compound, tungstic oxide has characteristic of semiconductor, is a kind of very potential sensitive material, and multiple gases is had susceptibility; Then because have bigger specific surface area, surface effects is remarkable for ultra-fine tungstic oxide, and it has very strong receptivity to hertzian wave, can do good solar absorptive material and recessive material.Except good photochromic properties and air-sensitive performance are arranged, tungstic oxide also has special catalytic performance, have a wide range of applications in chemical industry and petrochemical complex, become formaldehyde, propylene oxidation to become propenal etc. as methanol oxidation, its particle diameter is mostly at micron or submicron order.
Industrial general method with the roasting ammonium paratungstate is produced Tungsten oxide 99.999, and this technology is difficult to obtain the Tungsten oxide 99.999 of particle diameter below 1 micron, can not satisfy the properties for follow requirement.The method that prepare at present oxide micropowder mainly contains: solid phase method, liquid phase method (comprising the precipitator method, hydrothermal method, sol-gel method etc.), vapor phase process, these methods exist all that productive rate is low, cost is high, production is difficult to shortcomings such as control, should not carry out suitability for industrialized production.
Summary of the invention
The objective of the invention is to the deficiency of depositing, provide a kind of and can effectively solve, poor stability wayward, be difficult to realize the production method of the ultra-fine tungsten oxide of suitability for industrialized production problem equipment, ingredient requirement height, production technique at above-mentioned prior art.
The objective of the invention is to be achieved through the following technical solutions.
A kind of production method of ultra-fine tungsten oxide, it is characterized in that production process is is raw material to adopt ammonium tungstate solution, with ammonium tungstate solution add heat to salpeter solution in, stir and obtain yellow wolframic acid precipitation, precipitate after filtration, oven dry, roasting, comminution by gas stream obtain ultra-fine tungsten oxide.
The production method of a kind of ultra-fine tungsten oxide of the present invention is characterized in that its described ammonium tungstate solution, WO
3Content 20%～25% is that industrial ammonium tungstate solution that obtains after ion-exchange or wolframic acid are dissolved in the ammonium tungstate solution that disposes in the ammoniacal liquor and get.
The production method of a kind of ultra-fine tungsten oxide of the present invention is characterized in that its described salpeter solution is that volumetric concentration is 50% salpeter solution, ammonium tungstate solution and salpeter solution volume ratio 1: 1;
The production method of a kind of ultra-fine tungsten oxide of the present invention is characterized in that described process is that ammonium tungstate solution is heated in 80～100 ℃ the salpeter solution, and when the pH value of solution value reached 3.0～4.0, filtering reacting solution obtained yellow wolframic acid precipitation.
The production method of a kind of ultra-fine tungsten oxide of the present invention is characterized in that its yellow wolframic acid that obtains is dry dewatered under 80～90 ℃ of temperature.
The production method of a kind of ultra-fine tungsten oxide of the present invention is characterized in that its dry dewatered yellow wolframic acid is under 500～600 ℃ of temperature, roasting 2～4h.
The production method of a kind of ultra-fine tungsten oxide of the present invention is characterized in that roasting process is at 200 ℃, 400 ℃, 600 ℃ each section insulation 40min～1h.
Method of the present invention requires lowly to raw materials for production, the raw material cheapness, be easy to get; Production unit is simple, adopts common acid-resistant reacting kettle to get final product; Production technique is simple and easy to do, carries out under the normal pressure; Production technique is easy to control, and is easy and simple to handle, safe, reliable; Process stabilizing, production cost is low, the productive rate height; The synthetic powder granularity is evenly distributed, and Fisher particle size is at 1～0.3 μ m, good dispersity, purity height; Be suitable for suitability for industrialized production.
Description of drawings
Accompanying drawing is technological process of production figure of the present invention.
Embodiment
A kind of production method of ultra-fine tungsten oxide, its step comprises:
1) preparation salpeter solution (volume ratio 1: 1), stand for standby use;
2) configuration ammonium tungstate solution, wherein WO
3Content 20～25%, ammonium tungstate solution and salpeter solution volume ratio 1: 1;
3) heating salpeter solution to 80～100 ℃;
4) on one side with 2) slowly be added drop-wise to 1) in, Yi Bian stir fast, reach 3.0～4.0 until the pH value of solution value; Filtering reacting solution obtains yellow mercury oxide;
5) yellow mercury oxide is placed baking oven, 80～90 ℃ of dryings are removed moisture;
6) as 5) in caking phenomenon is arranged, yellow is dried thing pulverizes, cross 40 mesh sieves;
7) with 6) at the roasting kiln roasting, at 200 ℃, 400 ℃, 600 ℃ each section insulation 40min～1h;
8), obtain the ultra-fine tungsten oxide powder through comminution by gas stream.
Embodiment 1
Raw material: the ammonium tungstate solution (WO that obtains after the ion-exchange
3Content 20%), nitric acid (1: 1) is measured the 200ml salpeter solution and put into clean beaker, and is standby.
Measure the 200ml ammonium tungstate solution, standby.
Heating in water bath salpeter solution to 100 ℃ slowly is added drop-wise to ammonium tungstate solution in the hot nitric acid, stirs fast simultaneously, reaches 4.0 until the pH value of solution value.Filter, yellow mercury oxide is placed baking oven, 80～90 ℃ of dryings are again at 600 ℃ of roasting kiln roastings 2, in the roasting process, at 200 ℃, 400 ℃, 600 ℃ each section insulation 40min.After comminution by gas stream obtains the ultra-fine tungsten oxide powder.
Product is a tungstic oxide through X-ray powder crystal diffraction analysis, with scanning electron microscopic observation product pattern, Fisher particle size 1～0.3 μ m, dispersion state.
Embodiment 2
Raw material: wolframic acid, nitric acid, ammoniacal liquor
Measure 200ml salpeter solution (1: 1) and put into clean beaker, standby.
Take by weighing 50 gram wolframic acids, be dissolved in 80ml ammoniacal liquor (28%), add the 70ml deionized water again, obtain ammonium tungstate solution (WO
3Content 23%) 200ml is standby.
Heating in water bath salpeter solution to 80 ℃ slowly is added drop-wise to ammonium tungstate solution in the hot nitric acid, stirs fast simultaneously, reaches 3.5 until the pH value of solution value; Filter, yellow mercury oxide is placed baking oven, 80～90 ℃ of dryings are again at 500 ℃ of roasting kiln roasting 3h, in the roasting process, at 200 ℃, 400 ℃, 600 ℃ each section insulation 50min.After comminution by gas stream obtains the ultra-fine tungsten oxide powder.
Product is a Tungsten oxide 99.999 through X-ray powder crystal diffraction analysis, scanning electron microscopic observation product pattern, Fisher particle size 1～0.3 μ m, dispersion state.
Embodiment 3
Raw material: ammonium tungstate solution (WO
3Content 25%), nitric acid (1: 1)
Measure the 200ml salpeter solution and put into clean beaker, standby.
Measure the 200ml ammonium tungstate solution, standby.
Heating in water bath salpeter solution to 90 ℃ slowly is added drop-wise to ammonium tungstate solution in the hot nitric acid, stirs fast simultaneously, reaches 4.0 until the pH value of solution value.Filter, yellow mercury oxide is placed baking oven, 80～90 ℃ of dryings are again at 550 ℃ of roasting kiln roasting 3h, in the roasting process, at 200 ℃, 400 ℃, 600 ℃ each section insulation 1h.After comminution by gas stream obtains the ultra-fine tungsten oxide powder.
Product is a tungstic oxide through X-ray powder crystal diffraction analysis, with scanning electron microscopic observation product pattern, Fisher particle size 1～0.3 μ m, dispersion state.
Claims (7)
1. the production method of a ultra-fine tungsten oxide, it is characterized in that production process is is raw material to adopt ammonium tungstate solution, with ammonium tungstate solution add heat to salpeter solution in, stir and obtain yellow wolframic acid precipitation, precipitate after filtration, oven dry, roasting, comminution by gas stream obtain ultra-fine tungsten oxide.
2. the production method of ultra-fine tungsten oxide according to claim 1 is characterized in that its described ammonium tungstate solution, WO
3Content 20%～25% is that industrial ammonium tungstate solution that obtains after ion-exchange or wolframic acid are dissolved in the ammonium tungstate solution that disposes in the ammoniacal liquor and get.
3. the production method of a kind of ultra-fine tungsten oxide according to claim 1 is characterized in that its described salpeter solution is that volumetric concentration is 50% salpeter solution, ammonium tungstate solution and salpeter solution volume ratio 1: 1.
4. the production method of ultra-fine tungsten oxide according to claim 1, it is characterized in that described process is that ammonium tungstate solution is added temperature is in 80～100 ℃ the salpeter solution, when the pH value of solution value reached 3.0～4.0, filtering reacting solution obtained yellow wolframic acid precipitation.
5. the production method of ultra-fine tungsten oxide according to claim 1 is characterized in that its yellow wolframic acid that obtains is dry dewatered under 80～90 ℃ of temperature.
6. the production method of ultra-fine tungsten oxide according to claim 1 is characterized in that its dry dewatered yellow wolframic acid is at 500～600 ℃ of roasting temperature 2～4h.
7. the production method of ultra-fine tungsten oxide according to claim 1 is characterized in that in the roasting process, at 200 ℃, 400 ℃, 600 ℃ each section insulation 40min～1h.
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| Application Number | Priority Date | Filing Date | Title |
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| CNA2007101955429A CN101182040A (en) | 2007-12-07 | 2007-12-07 | Method for producing ultra-fine tungsten oxide |
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105948129A (en) * | 2016-06-12 | 2016-09-21 | 南昌航空大学 | Controllable synthesis method for different nanocrystalline types of WO3 and application of method to wastewater |
| CN108862391A (en) * | 2018-08-07 | 2018-11-23 | 厦门钨业股份有限公司 | A kind of low Fei Shi tungsten oxide and preparation method thereof |
| CN108941598A (en) * | 2018-08-09 | 2018-12-07 | 蓬莱市超硬复合材料有限公司 | A kind of soilless sticking body, uniformly, crystallize complete ultra-fine and nano-tungsten powder preparation method |
| CN109680178A (en) * | 2018-12-05 | 2019-04-26 | 盐城工学院 | A kind of preparation method and application of tungsten base nanometer floral material |
| CN109987632A (en) * | 2019-04-29 | 2019-07-09 | 江西省科学院应用物理研究所 | A kind of method that chemical precipitation method prepares ultra-fine ammonium paratungstate |
| CN114835164A (en) * | 2022-03-21 | 2022-08-02 | 厦门钨业股份有限公司 | Treatment method of tungsten oxide oversize product |
| CN116119719A (en) * | 2023-04-18 | 2023-05-16 | 崇义章源钨业股份有限公司 | Superfine platy tungsten oxide and preparation method thereof |
-
2007
- 2007-12-07 CN CNA2007101955429A patent/CN101182040A/en active Pending
Cited By (12)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105948129A (en) * | 2016-06-12 | 2016-09-21 | 南昌航空大学 | Controllable synthesis method for different nanocrystalline types of WO3 and application of method to wastewater |
| CN108862391A (en) * | 2018-08-07 | 2018-11-23 | 厦门钨业股份有限公司 | A kind of low Fei Shi tungsten oxide and preparation method thereof |
| CN108862391B (en) * | 2018-08-07 | 2020-07-10 | 厦门钨业股份有限公司 | Low-Fischer tungsten oxide and preparation method thereof |
| CN108941598A (en) * | 2018-08-09 | 2018-12-07 | 蓬莱市超硬复合材料有限公司 | A kind of soilless sticking body, uniformly, crystallize complete ultra-fine and nano-tungsten powder preparation method |
| CN109680178A (en) * | 2018-12-05 | 2019-04-26 | 盐城工学院 | A kind of preparation method and application of tungsten base nanometer floral material |
| CN109680178B (en) * | 2018-12-05 | 2020-12-01 | 盐城工学院 | Preparation method and application of tungsten-based nanoflower material |
| CN109987632A (en) * | 2019-04-29 | 2019-07-09 | 江西省科学院应用物理研究所 | A kind of method that chemical precipitation method prepares ultra-fine ammonium paratungstate |
| CN109987632B (en) * | 2019-04-29 | 2020-08-07 | 江西省科学院应用物理研究所 | Method for preparing superfine ammonium paratungstate by chemical precipitation method |
| CN114835164A (en) * | 2022-03-21 | 2022-08-02 | 厦门钨业股份有限公司 | Treatment method of tungsten oxide oversize product |
| CN114835164B (en) * | 2022-03-21 | 2023-11-28 | 厦门钨业股份有限公司 | Method for treating tungsten oxide oversize material |
| CN116119719A (en) * | 2023-04-18 | 2023-05-16 | 崇义章源钨业股份有限公司 | Superfine platy tungsten oxide and preparation method thereof |
| CN116119719B (en) * | 2023-04-18 | 2023-06-27 | 崇义章源钨业股份有限公司 | Superfine platy tungsten oxide and preparation method thereof |
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Open date: 20080521 |