CN102963932A - Method for preparing ultrafine molybdenum trioxide - Google Patents
Method for preparing ultrafine molybdenum trioxide Download PDFInfo
- Publication number
- CN102963932A CN102963932A CN2012104511914A CN201210451191A CN102963932A CN 102963932 A CN102963932 A CN 102963932A CN 2012104511914 A CN2012104511914 A CN 2012104511914A CN 201210451191 A CN201210451191 A CN 201210451191A CN 102963932 A CN102963932 A CN 102963932A
- Authority
- CN
- China
- Prior art keywords
- crystal seed
- solution
- mass concentration
- sodium molybdate
- hydro
- Prior art date
- 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.)
- Granted
Links
- JKQOBWVOAYFWKG-UHFFFAOYSA-N molybdenum trioxide Chemical compound O=[Mo](=O)=O JKQOBWVOAYFWKG-UHFFFAOYSA-N 0.000 title claims abstract description 48
- 238000000034 method Methods 0.000 title claims abstract description 31
- TVXXNOYZHKPKGW-UHFFFAOYSA-N sodium molybdate (anhydrous) Chemical compound [Na+].[Na+].[O-][Mo]([O-])(=O)=O TVXXNOYZHKPKGW-UHFFFAOYSA-N 0.000 claims abstract description 61
- 239000013078 crystal Substances 0.000 claims abstract description 47
- 239000011684 sodium molybdate Substances 0.000 claims abstract description 42
- 235000015393 sodium molybdate Nutrition 0.000 claims abstract description 42
- 238000002360 preparation method Methods 0.000 claims abstract description 38
- 238000001027 hydrothermal synthesis Methods 0.000 claims abstract description 24
- 238000001914 filtration Methods 0.000 claims abstract description 15
- 239000000463 material Substances 0.000 claims abstract description 7
- 238000001704 evaporation Methods 0.000 claims abstract description 5
- 230000008020 evaporation Effects 0.000 claims abstract description 5
- 238000000926 separation method Methods 0.000 claims abstract description 5
- 238000004064 recycling Methods 0.000 claims abstract description 4
- 239000000243 solution Substances 0.000 claims description 44
- 239000012452 mother liquor Substances 0.000 claims description 40
- 239000012065 filter cake Substances 0.000 claims description 26
- 239000007864 aqueous solution Substances 0.000 claims description 17
- 238000005406 washing Methods 0.000 claims description 14
- 239000007788 liquid Substances 0.000 claims description 11
- 239000000203 mixture Substances 0.000 claims description 11
- 238000003756 stirring Methods 0.000 claims description 10
- 238000002425 crystallisation Methods 0.000 claims description 9
- 230000008025 crystallization Effects 0.000 claims description 9
- 239000010935 stainless steel Substances 0.000 claims description 9
- 229910001220 stainless steel Inorganic materials 0.000 claims description 9
- 229910000476 molybdenum oxide Inorganic materials 0.000 claims description 4
- 239000000047 product Substances 0.000 claims description 4
- 239000002253 acid Substances 0.000 claims description 3
- 229910052500 inorganic mineral Inorganic materials 0.000 claims description 2
- 235000010755 mineral Nutrition 0.000 claims description 2
- 239000011707 mineral Substances 0.000 claims description 2
- 150000007524 organic acids Chemical class 0.000 claims description 2
- PQQKPALAQIIWST-UHFFFAOYSA-N oxomolybdenum Chemical compound [Mo]=O PQQKPALAQIIWST-UHFFFAOYSA-N 0.000 claims description 2
- 230000035484 reaction time Effects 0.000 claims 3
- 238000010438 heat treatment Methods 0.000 claims 1
- 239000006210 lotion Substances 0.000 claims 1
- 239000002994 raw material Substances 0.000 abstract description 2
- 239000010413 mother solution Substances 0.000 abstract 2
- 239000002245 particle Substances 0.000 abstract 1
- 239000002002 slurry Substances 0.000 description 16
- 239000007795 chemical reaction product Substances 0.000 description 14
- 239000012141 concentrate Substances 0.000 description 7
- 238000005516 engineering process Methods 0.000 description 4
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 description 3
- KRKNYBCHXYNGOX-UHFFFAOYSA-N citric acid Chemical compound OC(=O)CC(O)(C(O)=O)CC(O)=O KRKNYBCHXYNGOX-UHFFFAOYSA-N 0.000 description 3
- VZCYOOQTPOCHFL-OWOJBTEDSA-N Fumaric acid Chemical compound OC(=O)\C=C\C(O)=O VZCYOOQTPOCHFL-OWOJBTEDSA-N 0.000 description 2
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 2
- MHAJPDPJQMAIIY-UHFFFAOYSA-N Hydrogen peroxide Chemical compound OO MHAJPDPJQMAIIY-UHFFFAOYSA-N 0.000 description 2
- APUPEJJSWDHEBO-UHFFFAOYSA-P ammonium molybdate Chemical compound [NH4+].[NH4+].[O-][Mo]([O-])(=O)=O APUPEJJSWDHEBO-UHFFFAOYSA-P 0.000 description 2
- 239000011609 ammonium molybdate Substances 0.000 description 2
- 235000018660 ammonium molybdate Nutrition 0.000 description 2
- 229940010552 ammonium molybdate Drugs 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 239000011541 reaction mixture Substances 0.000 description 2
- VZCYOOQTPOCHFL-UHFFFAOYSA-N trans-butenedioic acid Natural products OC(=O)C=CC(O)=O VZCYOOQTPOCHFL-UHFFFAOYSA-N 0.000 description 2
- 229910001182 Mo alloy Inorganic materials 0.000 description 1
- ZOKXTWBITQBERF-UHFFFAOYSA-N Molybdenum Chemical compound [Mo] ZOKXTWBITQBERF-UHFFFAOYSA-N 0.000 description 1
- 108010038629 Molybdoferredoxin Proteins 0.000 description 1
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 description 1
- OFOBLEOULBTSOW-UHFFFAOYSA-N Propanedioic acid Natural products OC(=O)CC(O)=O OFOBLEOULBTSOW-UHFFFAOYSA-N 0.000 description 1
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 1
- HBELESVMOSDEOV-UHFFFAOYSA-N [Fe].[Mo] Chemical compound [Fe].[Mo] HBELESVMOSDEOV-UHFFFAOYSA-N 0.000 description 1
- 229910045601 alloy Inorganic materials 0.000 description 1
- 239000000956 alloy Substances 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 230000003750 conditioning effect Effects 0.000 description 1
- 230000005611 electricity Effects 0.000 description 1
- 239000007772 electrode material Substances 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 239000001530 fumaric acid Substances 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- VZCYOOQTPOCHFL-UPHRSURJSA-N maleic acid Chemical compound OC(=O)\C=C/C(O)=O VZCYOOQTPOCHFL-UPHRSURJSA-N 0.000 description 1
- 239000011976 maleic acid Substances 0.000 description 1
- 235000012054 meals Nutrition 0.000 description 1
- 229910044991 metal oxide Inorganic materials 0.000 description 1
- 150000004706 metal oxides Chemical class 0.000 description 1
- MEFBJEMVZONFCJ-UHFFFAOYSA-N molybdate Chemical compound [O-][Mo]([O-])(=O)=O MEFBJEMVZONFCJ-UHFFFAOYSA-N 0.000 description 1
- 239000005078 molybdenum compound Substances 0.000 description 1
- 150000002752 molybdenum compounds Chemical class 0.000 description 1
- 239000002127 nanobelt Substances 0.000 description 1
- 239000002073 nanorod Substances 0.000 description 1
- 229910017604 nitric acid Inorganic materials 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 239000012716 precipitator Substances 0.000 description 1
- 239000002243 precursor Substances 0.000 description 1
- 230000001105 regulatory effect Effects 0.000 description 1
- 238000003980 solgel method Methods 0.000 description 1
- 239000001117 sulphuric acid Substances 0.000 description 1
- 235000011149 sulphuric acid Nutrition 0.000 description 1
Images
Landscapes
- Inorganic Compounds Of Heavy Metals (AREA)
Abstract
The invention relates to a method for preparing ultrafine molybdenum trioxide, which comprises the steps of crystal seed preparation, material proportioning, hydrothermal reaction, separation by filtration, low-temperature roasting, and mother solution evaporation and recycling. The invention has the advantages of short technical process, mild conditions and no need of complex equipment; the molybdenum trioxide product has high purity, and the particle size reaches nano level; and the mother solution recycling method can effectively enhance the utilization ratio of the sodium molybdate raw material.
Description
Technical field
The present invention relates to a kind of method for preparing molybdic oxide, particularly relate to a kind of crystal seed that utilizes and process sodium molybdate solution, prepare the method for ultra-fine molybdic oxide.Patent of the present invention belongs to the nonferrous metal oxides preparing technical field.
Background technology
Molybdic oxide is as the main raw material of producing molybdenum-iron and molybdenum compound, and the addition agent that also can be used as molybdenum element directly joins in the molybdenum alloy, improves the performance of alloy.The method of industrial general employing roasting ammonium molybdate is produced molybdic oxide, expansion along with the molybdic oxide Application Areas, especially in the application in optical material, electricity material field, existing industrial molybdenum trioxide more and more can not satisfy service requirements because granularity is too thick.
The method of the ultra-fine molybdic oxide of present domestic preparation is less, the application number production technique of ultra-fine alpha-molybdenum oxide that has been 200410073016.1 patent disclosure, the reagent such as this technology utilization ammonium molybdate, acetic acid, hydrogen peroxide, adopt the precipitator method to make the molybdic oxide meal, then obtain ultra-fine alpha-molybdenum oxide by comminution by gas stream; The application number preparation method of molybdenum trioxide laminated nanometer bar that has been 200510019381.9 patent disclosure as precursor, adopts sol-gel method to make the molybdenum trioxide nano rod with molybdenum oxide or molybdate powder; Application number a kind of method for preparing lithiumation molybdenum trioxide nano belt electrode material that has been 200710052368.2 patent disclosure, the method is utilized inorganic sol hydrothermal technique and ultrasonic technology, and making product is lithiumation molybdenum trioxide nano carrying material.So far, except above-mentioned patent, there is no how disclosed patented technology and patent of the present invention is similar, adopt crystal seed to prepare the report of ultra-fine molybdic oxide and mother liquor reuse.
Summary of the invention
The object of the invention is to provide a kind of technical process easy, ultra-fine molybdic oxide preparation method.
The present invention includes following steps:
(1) crystal seed preparation: the preparation mass concentration is 43%～45% sodium molybdate aqueous solution, in the scope with organic acid or mineral acid regulator solution pH to 4.5～8.0, hydro-thermal reaction is 8 hours in autoclave, and the gained throw out is filtered, concentrates and crystallization, obtains crystal seed;
(2) material proportion: be to add crystal seed in 10%～50% the sodium molybdate solution to mass concentration, the Sodium orthomolybdate mass ratio in crystal seed quality and the solution is 1:4.5～1:5;
(3) hydro-thermal reaction: the described sodium molybdate solution of step (2) and seed reaction mixture are placed the stainless steel autoclave, and under 180～200 ℃ of violent stirring conditions, hydro-thermal reaction was cooled to room temperature after 14～15 hours, obtained product slurry;
(4) filtering separation: with the filtration of the product slurry described in the step (3), carrying out washing treatment, obtain filter cake and mother liquor;
(5) low-temperature bake: the filter cake described in the step (4) is obtained ultra-fine molybdic oxide at 325 ℃ of low-temperature bakes;
(6) mother liquor is concentrated: the mother liquor described in the step (4) and filter cake washing liquid are merged, and to obtain the Sodium orthomolybdate mass concentration be 3%～20% mother liquor through concentrating;
(7) mother liquid recycling: step (6)) described concentrated mother liquor turns back to the molybdic oxide preparation process, is 10%～50% sodium molybdate solution for the preparation mass concentration.
Compare the production technique of traditional ultra-fine molybdic oxide, the present invention has shortened technical process, has reduced energy consumption, has alleviated the pollution to environment, and the molybdic oxide of preparation has the characteristics such as fine size, purity height, good stability.
Description of drawings
Fig. 1 is the process flow sheet of patent of the present invention " a kind of method for preparing ultra-fine molybdic oxide ".
Embodiment
Embodiment 1
The preparation mass concentration is 43% sodium molybdate aqueous solution, and with hydrochloric acid conditioning solution pH to 4.9, hydro-thermal reaction with the filtration of gained throw out, evaporation, crystallization, obtained crystal seed after 8 hours in autoclave.
Be to add crystal seed in 45% the sodium molybdate solution to mass concentration, obtain the mixture of sodium molybdate solution and crystal seed, the Sodium orthomolybdate mass ratio in crystal seed quality and the solution is 1:5.The mixture of above-mentioned sodium molybdate solution and crystal seed is placed the stainless steel autoclave, and under 200 ℃ of violent stirring conditions, hydro-thermal reaction is after 15 hours, stops to stir, and obtains the reaction product slurry after being cooled to room temperature.The reaction product slurries filtration is obtained filter cake and mother liquor, and filter cake obtains ultra-fine molybdic oxide at 325 ℃ of low-temperature bakes.
Above-mentioned mother liquor and filter cake washing liquid are merged concentrated, obtain the Sodium orthomolybdate mass concentration and be 11.5% mother liquor, mother liquor is back to use in the molybdic oxide preparation process, is used for the preparation mass concentration and is 45% sodium molybdate aqueous solution.
Embodiment 2
The preparation mass concentration is 43% sodium molybdate aqueous solution, and in the scope with oxysuccinic acid regulator solution pH to 7.5, hydro-thermal reaction is 8 hours in autoclave, and the gained throw out is filtered, concentrates and crystallization, obtains crystal seed.
Be to add crystal seed in 32% the sodium molybdate solution to mass concentration, the Sodium orthomolybdate mass ratio in crystal seed quality and the solution is 1:5.The reaction mixture of above-mentioned sodium molybdate solution and crystal seed is placed the stainless steel autoclave, and under 180 ℃ of intensively stirred conditions, hydro-thermal reaction is after 14 hours, stops to stir, and obtains the reaction product slurry after being cooled to room temperature.The reaction product slurries filtration is obtained filter cake and mother liquor, and filter cake obtains ultra-fine molybdic oxide at 325 ℃ of low-temperature bakes.
Above-mentioned mother liquor and filter cake washing liquid are merged concentrated, obtain the Sodium orthomolybdate mass concentration and be 7% mother liquor, again mother liquor is turned back in the molybdic oxide preparation process, be used for the preparation mass concentration and be 32% sodium molybdate aqueous solution.
Embodiment 3
The preparation mass concentration is 44% sodium molybdate aqueous solution, and with rare nitric acid regulator solution pH to 5.0, hydro-thermal reaction is 8 hours in autoclave, and the gained throw out is filtered, concentrates and crystallization, obtains crystal seed.
Be to add crystal seed in 41% the sodium molybdate solution to mass concentration, obtain the mixture of sodium molybdate solution and crystal seed, the Sodium orthomolybdate mass ratio in crystal seed quality and the solution is 1:4.7.The mixture of above-mentioned sodium molybdate solution and crystal seed is placed the stainless steel autoclave, and under 180 ℃ of intensively stirred conditions, hydro-thermal reaction was cooled to room temperature and obtains the reaction product slurry after 15 hours.The reaction product slurries filtration is obtained filter cake and mother liquor, and filter cake obtains ultra-fine molybdic oxide at 325 ℃ of low-temperature bakes.
Above-mentioned mother liquor and filter cake washing liquid are merged concentrated, obtain the Sodium orthomolybdate mass concentration and be 9.6% mother liquor, again mother liquor is turned back in the molybdic oxide preparation process, be used for the preparation mass concentration and be 41% sodium molybdate aqueous solution.
Embodiment 4
The preparation mass concentration is 43% sodium molybdate solution, and in the scope with dilute sulphuric acid regulator solution pH to 5.1, hydro-thermal reaction is 8 hours in autoclave, and the gained throw out is filtered, concentrates and crystallization, obtains crystal seed.
Be to add crystal seed in 25% the sodium molybdate solution to mass concentration, the Sodium orthomolybdate mass ratio in control crystal seed quality and the solution is at 1:5.The mixture of above-mentioned sodium molybdate solution and crystal seed is placed the stainless steel autoclave, and under 180 ℃ of violent stirring conditions, hydro-thermal reaction is after 14 hours, obtains the reaction product slurry after being cooled to room temperature.With reaction product slurries filtration, carrying out washing treatment, obtain filter cake and mother liquor, filter cake obtains ultra-fine molybdic oxide through 325 ℃ of low-temperature bakes, the mother liquor reuse.
Above-mentioned mother liquor and filter cake washing liquid are merged concentrated, obtain the Sodium orthomolybdate mass concentration and be 17% mother liquor, again mother liquor is turned back in the molybdic oxide preparation process, be used for the preparation mass concentration and be 25% sodium molybdate aqueous solution.
Embodiment 5
The preparation mass concentration is 43% sodium molybdate aqueous solution, and with citric acid regulating solution pH to 7.5, hydro-thermal reaction is 8 hours in autoclave, and the gained throw out is filtered, concentrates and crystallization, obtains crystal seed.
Be to add crystal seed in 20% the sodium molybdate solution to mass concentration, the Sodium orthomolybdate mass ratio in control crystal seed quality and the solution is at 1:4.5.The mixture of above-mentioned sodium molybdate solution and crystal seed is placed the stainless steel autoclave, and under 220 ℃ of violent stirring conditions, hydro-thermal reaction is after 15 hours, obtains the reaction product slurry after being cooled to room temperature.With reaction product slurries filtration, carrying out washing treatment, obtain filter cake and mother liquor, the mother liquor reuse, filter cake obtains ultra-fine molybdic oxide through 325 ℃ of low-temperature bakes.
Above-mentioned mother liquor and filter cake washing liquid are merged concentrated, obtain the Sodium orthomolybdate mass concentration and be 5% mother liquor and be back in the molybdic oxide preparation process, be used for the preparation mass concentration and be 20% sodium molybdate solution.
Embodiment 6
The preparation mass concentration is 43% sodium molybdate aqueous solution, and with maleic acid regulator solution pH to 6.5, hydro-thermal reaction is 8 hours in autoclave, and the gained throw out is filtered, concentrates and crystallization, obtains crystal seed.
Be to add crystal seed in 42% the sodium molybdate solution to mass concentration, the Sodium orthomolybdate mass ratio in control crystal seed quality and the solution is 1:5.The mixture of above-mentioned sodium molybdate solution and crystal seed is placed the stainless steel autoclave, and under 190 ℃ of violent stirring conditions, hydro-thermal reaction is after 15 hours, obtains the reaction product slurry after being cooled to room temperature.With reaction product slurries filtration, carrying out washing treatment, obtain filter cake and mother liquor, the mother liquor reuse, filter cake obtains ultra-fine molybdic oxide through 325 ℃ of low-temperature bakes.
Above-mentioned mother liquor and filter cake washing liquid are merged concentrated, obtain the Sodium orthomolybdate mass concentration and be 14% mother liquor, be back in the molybdic oxide preparation process, be used for the preparation mass concentration and be 42% sodium molybdate aqueous solution.
Embodiment 7
The preparation mass concentration is 44% sodium molybdate aqueous solution, and with FUMARIC ACID TECH GRADE regulator solution pH to 5.0, hydro-thermal reaction is 8 hours in autoclave, and the gained throw out is filtered, concentrates and crystallization, obtains crystal seed.
Be to add crystal seed in 30% the sodium molybdate solution to mass concentration, the Sodium orthomolybdate mass ratio in control crystal seed quality and the solution is 1:5.The mixture of above-mentioned sodium molybdate solution and crystal seed is placed the stainless steel autoclave, and under 180 ℃ of violent stirring conditions, hydro-thermal reaction is after 14 hours, obtains the reaction product slurry after being cooled to room temperature.With reaction product slurries filtration, carrying out washing treatment, obtain filter cake and mother liquor, the mother liquor reuse, filter cake obtains ultra-fine molybdic oxide through 325 ℃ of low-temperature bakes.
Above-mentioned mother liquor and filter cake washing liquid are merged concentrated, obtain the Sodium orthomolybdate mass concentration and be 5.3% circulating mother liquor, again circulating mother liquor is turned back in the molybdic oxide preparation process, be used for the preparation mass concentration and be 30% sodium molybdate aqueous solution.
Claims (10)
1. a method for preparing ultra-fine molybdenum oxide is characterized in that, comprises the steps:
(1) crystal seed preparation: the preparation mass concentration is 5%～48% sodium molybdate aqueous solution, in the scope with organic acid or mineral acid regulator solution pH to 4.5～8.0, hydro-thermal reaction is 4～15 hours in autoclave, with the filtration of gained throw out, evaporation, crystallization, obtains crystal seed;
(2) material proportion: the preparation mass concentration is 10%～50% sodium molybdate solution, adds crystal seed in solution, and the Sodium orthomolybdate mass ratio in crystal seed quality and the solution is in 1:3～1:9.5 scope;
(3) reaction under high pressure: the mixture of sodium molybdate solution and crystal seed is placed the stainless steel autoclave, under 80～250 ℃ temperature of reaction and intensively stirred condition, hydro-thermal reaction is carried out in stirring, after the hydro-thermal reaction 4～20 hours, stop to stir, autoclave is cooled to the solidliquid mixture that takes out after the room temperature wherein;
(4) filtering separation: the solidliquid mixture filtering separation slip described in the step (3) is obtained ultra-fine molybdic oxide filter cake and mother liquor;
(5) low-temperature bake: ultra-fine molybdic oxide filter cake is carried out low-temperature bake obtain ultra-fine molybdic oxide product in stoving oven;
(6) mother liquid evaporation: with the washing lotion heating evaporation of mother liquor with the filtering separation stage, make the Sodium orthomolybdate mass concentration and be 3%～20% circulating mother liquor;
(7) mother liquid recycling: circulating mother liquor is turned back to the crystal seed preparation process, is 5%～45% sodium molybdate aqueous solution for the preparation mass concentration.
2. the method for claim 1, it is characterized in that: the mass concentration of sodium molybdate aqueous solution is 35%～48% described in " crystal seed preparation " step.
3. method as claimed in claim 2, it is characterized in that: the mass concentration of sodium molybdate aqueous solution is 43～45% described in " crystal seed preparation " step.
4. the method for claim 1, it is characterized in that: the hydro-thermal reaction time described in " crystal seed preparation " step is 8 hours.
5. the method for claim 1, it is characterized in that: the Sodium orthomolybdate mass ratio in " material proportion " process crystal seed quality and the solution is 1:4.5～1:5.
6. the method for claim 1, it is characterized in that: the described reaction under high pressure temperature of " reaction under high pressure " step is 180～200 ℃.
7. the method for claim 1, it is characterized in that: the temperature of the described low-temperature bake of " low-temperature bake " step is 250～400 ℃.
8. the method for claim 1, it is characterized in that: the described hydro-thermal reaction time of " reaction under high pressure " step is 12～16 hours.
9. method as claimed in claim 7, it is characterized in that: the temperature of described low-temperature bake is 325 ℃.
10. method as claimed in claim 8, it is characterized in that: the described hydro-thermal reaction time of " reaction under high pressure " step is 14～15 hours.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201210451191.4A CN102963932B (en) | 2012-11-13 | 2012-11-13 | Method for preparing ultrafine molybdenum trioxide |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201210451191.4A CN102963932B (en) | 2012-11-13 | 2012-11-13 | Method for preparing ultrafine molybdenum trioxide |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN102963932A true CN102963932A (en) | 2013-03-13 |
| CN102963932B CN102963932B (en) | 2014-06-18 |
Family
ID=47794409
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201210451191.4A Expired - Fee Related CN102963932B (en) | 2012-11-13 | 2012-11-13 | Method for preparing ultrafine molybdenum trioxide |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN102963932B (en) |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104276605A (en) * | 2014-10-23 | 2015-01-14 | 江苏华伦化工有限公司 | Preparation method of monoclinic-phase molybdenum trioxide |
| CN104310481A (en) * | 2014-10-13 | 2015-01-28 | 杭州聚力氢能科技有限公司 | Porous molybdenum trioxide as well as preparation method, hydrogenation catalyst and dehydrogenation catalyst thereof |
| CN105129853A (en) * | 2015-09-28 | 2015-12-09 | 蚌埠学院 | Method for synthesizing MoO3 powder in hexagonal prism shape by utilizing citric acid induction |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101381106A (en) * | 2007-09-05 | 2009-03-11 | 西南交通大学 | Method for preparing nano tungsten trioxide powder |
| US20090311169A1 (en) * | 2008-05-12 | 2009-12-17 | Krishnan Rajeshwar | Combustion synthesis and doping of oxide semiconductors |
| CN101774643A (en) * | 2010-01-12 | 2010-07-14 | 中南大学 | Process for preparing tungstic oxide hydrate from sodium tungstate solution |
-
2012
- 2012-11-13 CN CN201210451191.4A patent/CN102963932B/en not_active Expired - Fee Related
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101381106A (en) * | 2007-09-05 | 2009-03-11 | 西南交通大学 | Method for preparing nano tungsten trioxide powder |
| US20090311169A1 (en) * | 2008-05-12 | 2009-12-17 | Krishnan Rajeshwar | Combustion synthesis and doping of oxide semiconductors |
| CN101774643A (en) * | 2010-01-12 | 2010-07-14 | 中南大学 | Process for preparing tungstic oxide hydrate from sodium tungstate solution |
Non-Patent Citations (2)
| Title |
|---|
| 《中国优秀硕士学位论文全文数据库 工程科技Ⅰ辑》 20120115 喻晓剑 "水热合成法制备焦绿石型三氧化钨的研究" 第13-16、20-23、31-34、38-42页 1-10 , 第01期 * |
| 喻晓剑: ""水热合成法制备焦绿石型三氧化钨的研究"", 《中国优秀硕士学位论文全文数据库 工程科技Ⅰ辑》, no. 01, 15 January 2012 (2012-01-15) * |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104310481A (en) * | 2014-10-13 | 2015-01-28 | 杭州聚力氢能科技有限公司 | Porous molybdenum trioxide as well as preparation method, hydrogenation catalyst and dehydrogenation catalyst thereof |
| CN104310481B (en) * | 2014-10-13 | 2016-09-28 | 杭州聚力氢能科技有限公司 | Porous molybdenum trioxide and preparation method thereof, hydrogenation catalyst and dehydrogenation |
| CN104276605A (en) * | 2014-10-23 | 2015-01-14 | 江苏华伦化工有限公司 | Preparation method of monoclinic-phase molybdenum trioxide |
| CN105129853A (en) * | 2015-09-28 | 2015-12-09 | 蚌埠学院 | Method for synthesizing MoO3 powder in hexagonal prism shape by utilizing citric acid induction |
Also Published As
| Publication number | Publication date |
|---|---|
| CN102963932B (en) | 2014-06-18 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN103539210B (en) | A kind of preparation method of cobalt molybdate crystallite | |
| CN105417570B (en) | Method for preparing spinel-type complex oxide through co-precipitation, homogenization and spray drying | |
| CN101508464B (en) | Process for preparing anatase type nano-titanium dioxide | |
| CN103203455B (en) | Method for manufacturing molybdenum powder | |
| CN101555038B (en) | Method for preparing titanium pigment by hydrolysis | |
| CN103606694A (en) | Preparation method for commercial vanadium battery electrolyte | |
| CN102101697A (en) | Rapid preparation method of high-dispersible TiO2 nano crystal sol | |
| CN107601561B (en) | The preparation method of nanometer pucherite yellow uitramarine | |
| CN102786095B (en) | Method for preparing manganous manganic oxide | |
| CN102910683A (en) | Production method for synthesizing nanoscale oxide iron red through full-wet method | |
| CN102963932B (en) | Method for preparing ultrafine molybdenum trioxide | |
| CN108046311A (en) | The preparation method of high-purity gallium oxide | |
| CN107827153B (en) | A kind of preparation method of nanometer of silver vanadate | |
| CN105016371A (en) | Preparation method of electronic grade ceric sulfate | |
| CN110339843B (en) | Preparation method of magnetic bismuth oxide/bismuth vanadate composite photocatalyst | |
| CN102676817A (en) | Method for preparing calciferous vanadium oxide from vanadate | |
| CN103539183A (en) | Acid method for preparing aluminum polychlorid and high-purity nanoscale white carbon black through ash of oil shale | |
| CN102069001B (en) | Preparation process for preparing photocatalyst from blast furnace slag serving as raw material | |
| CN202968150U (en) | Device combination for preparing superfine molybdenum trioxide | |
| CN103447024B (en) | The preparation method of a kind of bismuthino strontium magnetic photocatalyst and bismuthino strontium magnetic photocatalyst thereof | |
| CN105129834B (en) | A kind of nanometer level RE oxide raw powder's production technology | |
| CN103332711B (en) | Deep desilicication method of high-alumina fly ash | |
| CN102701240A (en) | Method for preparing silicon-steel-grade magnesium oxide from magnesium sulfate waste liquor | |
| CN102275997A (en) | Porous ferric oxide constructed by nanocrystalline and preparation method thereof | |
| CN102963935A (en) | Method for preparing ultrafine tungsten trioxide |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C14 | Grant of patent or utility model | ||
| GR01 | Patent grant | ||
| CF01 | Termination of patent right due to non-payment of annual fee |
Granted publication date: 20140618 |
|
| CF01 | Termination of patent right due to non-payment of annual fee |