CN1736880A - Ultra-fine alpha- molybdenum oxide production process - Google Patents
Ultra-fine alpha- molybdenum oxide production process Download PDFInfo
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- CN1736880A CN1736880A CN 200410073016 CN200410073016A CN1736880A CN 1736880 A CN1736880 A CN 1736880A CN 200410073016 CN200410073016 CN 200410073016 CN 200410073016 A CN200410073016 A CN 200410073016A CN 1736880 A CN1736880 A CN 1736880A
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Abstract
Disclosed is a process for manufacturing super fine alpha-molybdenum oxide which comprises, dissolving ammonium molybdate into water, obtaining cleaning solution of ammonium molybdate, formulating acetic acid solution, charging hydrogen peroxide solution to obtain acidified precipitant, heating the autoclave, slowly dripping acidified precipitant into ammonium molybdate solution and stirring, filtering the reaction liquid, obtaining yellow and white precipitate, drying to obtain block-shaped molybdenum trioxide, disintegrating and sieving to obtain molybdenum trioxide coarse powder, finally sintering and disintegrating with air flow to obtain ultra-fine alpha-molybdenum trioxide powder.
Description
Technical field
The present invention relates to a kind of production technique of ultra-fine alpha-molybdenum oxide.
Background technology
Alpha-molybdenum oxide is the molybdic oxide of laminated structure, the yellow-white powder, and molecular formula is MoO
1/1O
2/2O
3/3Being applied in the smoke-inhibiting flame retardant additive of PVC, cable etc., also is good Hydrobon catalyst, also can be used for photochromic, electrochromic display material etc.Its use properties is not only relevant with chemical purity, goes back and physical properties, and is relevant as size, aggregating state etc.
Industrial general method with the roasting ammonium molybdate is produced molybdenum oxide.Along with the continuous development of Materials science and utilisation technology, the molybdenum oxide that this method makes since particle thick, be aggregating state and can not satisfy service requirements.At present, carry out the micro mist research of molybdenum oxide both at home and abroad one after another.External Mohamed H Khan etc. improve the molybdic oxide electrothermal oven that distils, and develop nano oxidized molybdenum with distillation-quenching method; Maruyma Toshiro etc. prepares the molybdic oxide film with chemical Vapor deposition process.These methods are all high to equipment, ingredient requirement, and production technique is wayward, the production cost height, and productive rate is low.The Li Yadong of domestic Tsing-Hua University, Li Xiaolin have synthesized nano band of MoO 3 monocrystal with hydrothermal method in high temperature and high pressure kettle, but there are drawbacks such as poor stability, filtration difficulty in this method.The production method of above-mentioned molybdenum oxide all is difficult to realize scale operation.
Summary of the invention
The object of the present invention is to provide a kind of production technique of ultra-fine alpha-molybdenum oxide, it has solved background technology and has been difficult to realize scale operation; To equipment, ingredient requirement height, production technique is wayward, or the technical problem of poor stability, filtration difficulty.
Technical solution of the present invention is:
A kind of production technique of ultra-fine alpha-molybdenum oxide, its special character is: this production technique comprises:
1) in acid-resistant reacting kettle, adds deionized water; Get the analytical pure ammonium molybdate, be dissolved in the deionized water, obtain the ammonium molybdate clear liquor;
2) compound concentration is 35%～75% acetum, adds hydrogen peroxide, obtains the acid precipitation agent;
3) heating in water bath for reaction still to 60 ℃; Simultaneously, on one side the speed of acid precipitation agent with 1～10ml/min slowly is added drop-wise in the ammonium molybdate solution, stir on one side, reach 3.0～4.0 until the pH value of solution value;
4) filtering reacting liquid obtains Huang-white depositions;
5) Huang-white depositions is placed baking oven, oven dry obtains block molybdenum oxide;
6) block molybdenum oxide is pulverized, crossed 40 mesh sieves, obtain the molybdenum oxide meal;
7) with the molybdenum oxide meal at 400-600 ℃ of roasting kiln roasting 2-4h;
8), obtain the ultra-fine alpha-molybdenum oxide powder through comminution by gas stream.
Above-mentioned analytical pure ammonium molybdate generally can adopt ammonium dimolybdate, ammonium tetramolybdate, Ammonium Heptamolybdate or ammonium octamolybdate.Wherein, with employing ammonium octamolybdate best results, but cost is higher; Actual production should be adopted Ammonium Heptamolybdate.
Above-mentioned acetum with add hydrogen peroxide ratio can be 100: 10～30.
The concentration of above-mentioned acetum is 36% o'clock, and acetum should adopt 100: 30 with the ratio of add of hydrogen peroxide; The concentration of above-mentioned acetum is 43% o'clock, and acetum should adopt 100: 20 with the ratio of add of hydrogen peroxide; The concentration of above-mentioned acetum is 50% o'clock, and acetum should adopt 100: 20 with the ratio of add of hydrogen peroxide; The concentration of above-mentioned acetum is 75% o'clock, and acetum should adopt 100: 10 with the ratio of add of hydrogen peroxide.
The speed of above-mentioned dropping acid precipitation agent can be 1～10ml/min.
The suitable speed of above-mentioned dropping acid precipitation agent can adopt 10ml/min, 5ml/min, 4ml/min or 1ml/min.
Above-mentioned the acid precipitation agent is added drop-wise in the ammonium molybdate solution, the pH value that reactor solution is reached is more suitable with 3.0 or 3.5.
Above-mentioned analytical pure ammonium molybdate is advisable with 0.04mol's, above-mentioned ammonium molybdate clear liquor being advisable with 0.4mol/l.
The temperature of above-mentioned roasted molybdenum oxide meal is more suitable with 400 ℃, 450 ℃ or 500 ℃.
Above-mentionedly place the bake out temperature of baking oven to can be 100～120 ℃ Huang-white depositions.
The present invention has the following advantages:
1. require low to raw materials for production.The raw material cheapness, be easy to get, ammonium molybdate and acidifying acetic acid generally can be adopted in the molybdenum source.
2. production unit is simple.Adopt common acid-resistant reacting kettle to get final product.
3. production technique is simple and easy to do, and working condition is normal temperature, normal pressure.Under the temperature about 60 ℃, drip ammonium molybdate solution and can produce synthetic.
4. production technique is easy to control, and is easy and simple to handle, safe, reliable.
5. process stabilizing, production cost is low, the productive rate height.
6. at normal temperatures and pressures, synthetic crystalline form even size distribution, and be powder granule, particle diameter generally about 1-0.5 μ m, good dispersity, purity height.
7. be suitable for scale operation.Can be widely used as smoke-inhibiting flame retardant additive, synthetic catalyst, and display material photochromic, electrochromic.
Description of drawings
Accompanying drawing is technological process of production figure of the present invention.
Embodiment
The present invention adopts the acidifying with acetic acid ammonium molybdate to produce alpha-molybdenum oxide, synthetic at normal temperatures and pressures crystalline form even size distribution powder granule.Referring to accompanying drawing, production technique of the present invention is as follows:
1. in acid-resistant reacting kettle, add the 100ml deionized water; Get 0.04mol analytical pure ammonium molybdate, be dissolved in the deionized water, obtain the ammonium molybdate clear liquor of 0.4mol/l;
2. compound concentration is 35%～75% acetum 100ml, adds 10～30ml hydrogen peroxide, obtains the acid precipitation agent;
3. heating in water bath for reaction still to 60 ℃; Simultaneously, on one side the speed of acid precipitation agent with 1～10ml/min slowly is added drop-wise in the ammonium molybdate solution, stir on one side, reach 3.0～4.0 until the pH value of solution value;
4. filtering reacting liquid obtains Huang-white depositions;
5. Huang-white depositions is placed baking oven, 100～120 ℃ of oven dry obtain block molybdenum oxide;
6. block molybdenum oxide is pulverized, crossed 40 mesh sieves, obtain the molybdenum oxide meal;
With the molybdenum oxide meal at 400-600 ℃ of roasting kiln roasting 2-4h;
8. through comminution by gas stream, obtain the ultra-fine alpha-molybdenum oxide powder.
Embodiment one
1. in acid-resistant reacting kettle, add the 100ml deionized water; Take by weighing 0.04mol analytical pure Ammonium Heptamolybdate, be dissolved in the deionized water, obtain 0.4mol/l Ammonium Heptamolybdate clear liquor;
2. prepare 50% acetum 100ml, add the 20ml hydrogen peroxide, obtain the acid precipitation agent;
3. heating in water bath for reaction still to 60 ℃; Simultaneously, on one side the speed of acid precipitation agent with 5ml/min slowly is added drop-wise in the Ammoniun Heptamolybdate Solution, stir on one side, reach 3.5 until the pH value of solution value;
4. filtering reacting liquid obtains Huang-white depositions;
5. Huang-white depositions is placed baking oven, 100 ℃ of oven dry obtain block molybdenum oxide;
6. block molybdenum oxide is pulverized, crossed 40 mesh sieves, obtain the molybdenum oxide meal;
With the molybdenum oxide meal at 450 ℃ of roasting kiln roasting 3h;
8. through comminution by gas stream, obtain the ultra-fine alpha-molybdenum oxide powder.
Product is an alpha-molybdenum oxide through X-ray powder crystal diffraction XRD analysis, belongs to rhombic system; With scanning electron microscope sem testing product pattern, about particle diameter 1-0.5 μ m, be dispersion state.
Embodiment two
1. in acid-resistant reacting kettle, add the 100ml deionized water; Get 0.04mol analytical pure Ammonium Heptamolybdate, be dissolved in the deionized water, obtain the Ammonium Heptamolybdate clear liquor of 0.4mol/l;
2. prepare 36% acetum 100ml, add the 30ml hydrogen peroxide, obtain the acid precipitation agent;
3. heating in water bath for reaction still to 60 ℃; Simultaneously, on one side the speed of acid precipitation agent with 10ml/min slowly is added drop-wise in the Ammoniun Heptamolybdate Solution, stir on one side, reach 3.5 until the pH value of solution value;
4. filtering reacting liquid obtains Huang-white depositions;
5. Huang-white depositions is placed baking oven, 120 ℃ of oven dry obtain block molybdenum oxide;
6. block molybdenum oxide is pulverized, crossed 40 mesh sieves, obtain the molybdenum oxide meal;
With the molybdenum oxide meal at 500 ℃ of roasting kiln roasting 2h;
8. through comminution by gas stream, obtain the ultra-fine alpha-molybdenum oxide powder.
Product is an alpha-molybdenum oxide through X-ray powder crystal diffraction XRD analysis, belongs to rhombic system; Scanning electron microscope sem testing product pattern, about particle diameter 1-0.5 μ m or below, be dispersion state.
Embodiment three
1. in acid-resistant reacting kettle, add the 100ml deionized water; Get 0.04mol analytical pure Ammonium Heptamolybdate, be dissolved in the deionized water water, obtain the Ammonium Heptamolybdate clear liquor of 0.4mol/l;
2. prepare 75% acetum 100ml, add the 10ml hydrogen peroxide, obtain the acid precipitation agent;
3. heating in water bath for reaction still to 60 ℃; Simultaneously, on one side the speed of acid precipitation agent with 1ml/min slowly is added drop-wise in the Ammoniun Heptamolybdate Solution, stir on one side, reach 3.5 until the pH value of solution value;
4. filtering reacting liquid obtains Huang-white depositions;
5. Huang-white depositions is placed baking oven, 100 ℃ of oven dry obtain block molybdenum oxide;
6. block molybdenum oxide is pulverized, crossed 40 mesh sieves, obtain the molybdenum oxide meal;
With the molybdenum oxide meal at 400 ℃ of roasting kiln roasting 4h;
8. through comminution by gas stream, obtain the ultra-fine alpha-molybdenum oxide powder.
Product is an alpha-molybdenum oxide through X-ray powder crystal diffraction XRD analysis, belongs to rhombic system; Scanning electron microscope sem testing product pattern, about particle diameter 1-0.5 μ m or below, be dispersion state.
Embodiment four
1. in acid-resistant reacting kettle, add the 100ml deionized water; Get 0.04mol analytical pure Ammonium Heptamolybdate, be dissolved in the water, obtain the Ammonium Heptamolybdate clear liquor of 0.4mol/l;
2. prepare 43% acetum 100ml, add the 20ml hydrogen peroxide, obtain the acid precipitation agent;
3. heating in water bath for reaction still to 60 ℃ keeps about 1h; Simultaneously, on one side the speed of acid precipitation agent 4ml/min slowly is added drop-wise in the Ammoniun Heptamolybdate Solution, stir on one side, reach 3.5 until the pH value of solution value;
4. filtering reacting liquid obtains Huang-white depositions;
5. Huang-white depositions is placed baking oven, 120 ℃ of oven dry obtain block molybdenum oxide;
6. block molybdenum oxide is pulverized, crossed 40 mesh sieves, obtain the molybdenum oxide meal;
With the molybdenum oxide meal at 400 ℃ of roasting kiln roasting 4h;
8. through comminution by gas stream, obtain the ultra-fine alpha-molybdenum oxide powder.
Product is an alpha-molybdenum oxide through X-ray powder crystal diffraction XRD analysis, belongs to rhombic system; Scanning electron microscope sem testing product pattern about particle diameter 1-0.5 μ m, is dispersion state.
Claims (10)
1. the production technique of a ultra-fine alpha-molybdenum oxide, it is characterized in that: this production technique comprises:
1) in acid-resistant reacting kettle, adds deionized water; Get the analytical pure ammonium molybdate, be dissolved in the deionized water, obtain the ammonium molybdate clear liquor;
2) compound concentration is 35%～75% acetum, adds hydrogen peroxide, obtains the acid precipitation agent;
3) heating in water bath for reaction still to 60 ℃; Simultaneously, on one side the speed of acid precipitation agent with 1～10ml/min slowly is added drop-wise in the ammonium molybdate solution, stir on one side, reach 3.0～4.0 until the pH value of solution value;
4) filtering reacting liquid obtains Huang-white depositions;
5) Huang-white depositions is placed baking oven, oven dry obtains block molybdenum oxide;
6) block molybdenum oxide is pulverized, crossed 40 mesh sieves, obtain the molybdenum oxide meal;
7) with the molybdenum oxide meal at 400-600 ℃ of roasting kiln roasting 2-4h;
8), obtain the ultra-fine alpha-molybdenum oxide powder through comminution by gas stream.
2. the production technique of ultra-fine alpha-molybdenum oxide according to claim 1, it is characterized in that: described analytical pure ammonium molybdate is ammonium dimolybdate, ammonium tetramolybdate, Ammonium Heptamolybdate, ammonium octamolybdate.
3. the production technique of ultra-fine alpha-molybdenum oxide according to claim 1 and 2 is characterized in that: described acetum is 100: 10～30 with the ratio of add of hydrogen peroxide.
4. the production technique of ultra-fine alpha-molybdenum oxide according to claim 3, it is characterized in that: the concentration of described acetum is respectively 36%, 43%, 50% or 75%; Corresponding with described acetum concentration, described acetum was respectively 100: 30 with the ratio that adds hydrogen peroxide, and 100: 20,100: 20 or 100: 10.
5. the production technique of ultra-fine alpha-molybdenum oxide according to claim 3, it is characterized in that: the speed of described dropping acid precipitation agent is 1～10ml/min.
6. the production technique of ultra-fine alpha-molybdenum oxide according to claim 5, it is characterized in that: the speed of described dropping acid precipitation agent is 10ml/min, 5ml/min, 4ml/min or 1ml/min.
7. the production technique of ultra-fine alpha-molybdenum oxide according to claim 5 is characterized in that: described the acid precipitation agent is added drop-wise in the ammonium molybdate solution, the pH value that reactor solution is reached is 3.0 or 3.5.
8. the production technique of ultra-fine alpha-molybdenum oxide according to claim 7, it is characterized in that: described analytical pure ammonium molybdate is 0.04mol, described ammonium molybdate clear liquor is 0.4mol/l.
9. the production technique of ultra-fine alpha-molybdenum oxide according to claim 8, it is characterized in that: the temperature of described roasted molybdenum oxide meal is 400 ℃, 450 ℃ or 500 ℃.
10. the production technique of ultra-fine alpha-molybdenum oxide according to claim 9 is characterized in that: described Huang-white depositions is placed the bake out temperature of baking oven is 100～120 ℃.
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101590529B (en) * | 2009-06-29 | 2011-08-10 | 金堆城钼业股份有限公司 | Method for preparing high bulk density molybdenum powder |
| CN101780981B (en) * | 2009-01-14 | 2011-11-23 | 新疆教育学院 | Hydro-thermal synthesis method of molybdenum dioxide nano particle |
| CN102126757B (en) * | 2010-01-19 | 2012-11-14 | 中国环境科学研究院 | Method for pollution-free production of molybdenum oxide |
| CN105819509A (en) * | 2016-03-11 | 2016-08-03 | 金堆城钼业股份有限公司 | Preparation method of pure molybdenum trioxide for catalyst |
| CN105836802A (en) * | 2016-03-29 | 2016-08-10 | 河南师范大学 | MoO3 wet catalyst for degradation of dye wastewater and preparation method thereof |
Family Cites Families (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4273745A (en) * | 1979-10-03 | 1981-06-16 | Amax Inc. | Production of molybdenum oxide from ammonium molybdate solutions |
| CN1155524C (en) * | 2002-03-15 | 2004-06-30 | 清华大学 | Process for synthesizing nano band of MoO3 monocrystal |
-
2004
- 2004-08-16 CN CNB2004100730161A patent/CN1314596C/en active Active
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101780981B (en) * | 2009-01-14 | 2011-11-23 | 新疆教育学院 | Hydro-thermal synthesis method of molybdenum dioxide nano particle |
| CN101590529B (en) * | 2009-06-29 | 2011-08-10 | 金堆城钼业股份有限公司 | Method for preparing high bulk density molybdenum powder |
| CN102126757B (en) * | 2010-01-19 | 2012-11-14 | 中国环境科学研究院 | Method for pollution-free production of molybdenum oxide |
| CN105819509A (en) * | 2016-03-11 | 2016-08-03 | 金堆城钼业股份有限公司 | Preparation method of pure molybdenum trioxide for catalyst |
| CN105819509B (en) * | 2016-03-11 | 2017-09-12 | 金堆城钼业股份有限公司 | A kind of preparation method of the pure molybdenum trioxide of catalyst |
| CN105836802A (en) * | 2016-03-29 | 2016-08-10 | 河南师范大学 | MoO3 wet catalyst for degradation of dye wastewater and preparation method thereof |
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Address after: Technology center of Shaanxi province Xi'an 710068 South Second Ring Road West, No. 5 building 17 layer Generay Jinduicheng Molybdenum Group Co. Ltd. Patentee after: Jinduicheng Molybdenum Group Co., Ltd. Address before: Technology center of Shaanxi province Xi'an 710068 South Second Ring Road West, No. 5 building 17 layer Generay Jinduicheng Molybdenum Mining Corporation Patentee before: Jinduicheng Molybdenum Industry Corp. |
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Effective date of registration: 20071214 Address after: The western part of Shaanxi province Xi'an City, South Second Ring Road No. 5 building 17 layer Generay Jinduicheng Molybdenum Limited by Share Ltd technical center zip code: 710068 Patentee after: Jinduicheng Molybdenum Industry Co., Ltd. Address before: Technology center of Shaanxi province Xi'an City West South Second Ring Road No. 5 building 17 layer Generay Jinduicheng Molybdenum Group Co. Ltd. postcode: 710068 Patentee before: Jinduicheng Molybdenum Group Co., Ltd. |