CN103723769A - Method for preparing potassium-doped molybdenum trioxide - Google Patents
Method for preparing potassium-doped molybdenum trioxide Download PDFInfo
- Publication number
- CN103723769A CN103723769A CN201310713108.0A CN201310713108A CN103723769A CN 103723769 A CN103723769 A CN 103723769A CN 201310713108 A CN201310713108 A CN 201310713108A CN 103723769 A CN103723769 A CN 103723769A
- Authority
- CN
- China
- Prior art keywords
- potassium
- molybdic oxide
- preparation
- saltpetre
- quality
- 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.)
- Pending
Links
Landscapes
- Inorganic Compounds Of Heavy Metals (AREA)
Abstract
The invention discloses a method for preparing potassium-doped molybdenum trioxide, which comprises the following steps: determining the quality of potassium nitrate to be added, preparing a potassium nitrate solution, carrying out spray addition, and preparing the potassium-doped molybdenum trioxide. The method solves the problem that the existing molybdenum trioxide preparation method lowers the content of the potassium element, and the problems of nonuniform potassium element content and unstable molybdenum powder quality in the molybdenum powder product due to the direct addition of the potassium element into the molybdenum trioxide finished product. The method has the advantages of controllable production technique and low implementation cost, is simple and safe to operate, and is suitable for large-scale production of molybdenum trioxide. The additive potassium nitrate and deionized water are low in price and harmless to the operating personnel, and do not pollute the working environment. The prepared molybdenum trioxide has high yield and favorable powder uniformity; and the method is short in preparation procedures and controllable in product performance, and can satisfy demands of different users in different industries.
Description
Technical field
The invention belongs to technical field of material, be specifically related to a kind of method of mixing potassium molybdic oxide of preparing.
Background technology
The emerging field of molybdenum mainly concentrates on electronics and automotive industry, molybdenum has obtained application widely as structured material and functional materials, relevant industries present the trend of growth for the demand of molybdenum, meanwhile, for molybdenum product alloying, also proposed new higher requirement.
The preparation of current molybdenum alloy normally utilizes infiltration, microstructure homogenization, alloying, the segregation-free that the volatile feature of potassium element is other alloying element that favourable condition is provided, and the high-purity molybdenum trioxide of therefore mixing potassium is the basic material of molybdenum product alloying.
At present domestic and international high-purity molybdenum trioxide is mainly by calcination production of molybdic ammonium, and ammonium molybdate aborning generally through overpickling or washing, ammonia soak, the removal of impurities means such as filtration, make the impurity elements such as sodium in molybdic oxide, calcium, magnesium, copper, nickel, iron change soluble salt into, through filtering, these impurity elements are removed again, but this method has also been removed a large amount of potassium elements useful to following process when removing impurity element, cause following process molybdenum powder product potassium content too low, can not meet customer requirement.And in order to improve the content of potassium element in molybdic oxide powder, conventionally directly in high-purity molybdenum trioxide, add potassium element, and can cause like this potassium element skewness in molybdic oxide, and then cause final molybdenum powder quality unstable.
Summary of the invention
The object of the present invention is to provide a kind of method of mixing potassium molybdic oxide of preparing, solved existing molybdic oxide preparation method and reduced the problem of Determination of Potassium and directly in molybdic oxide finished product, add potassium element and cause in molybdenum powder product that Determination of Potassium is inhomogeneous, the unsettled problem of molybdenum powder quality.
The technical solution adopted in the present invention is: the method that potassium molybdic oxide is mixed in preparation, comprises the steps:
The first step, determines the quality that needs the saltpetre adding
The content of potassium element and calculate the quality that needs the saltpetre adding in the molybdic oxide of preparation unit mass for the preparation of the content meter of potassium element in the ammonium molybdate of molybdic oxide in the molybdic oxide of unit mass of preparation as required;
Second step, prepares potassium nitrate solution
Get the saltpetre of the definite respective quality of the first step, and adopt deionized water that described saltpetre is fully dissolved, make potassium nitrate solution;
The 3rd step, spraying is added
The potassium nitrate solution that second step is made is added in ammonium molybdate by the mode of spraying, makes mixture;
The 4th step, potassium molybdic oxide is mixed in preparation
The mixture that the 3rd step is made carries out calcination, obtains the satisfactory potassium molybdic oxide of mixing.
Feature of the present invention is also,
In the first step, need the method for calculation of the saltpetre quality C adding to be:
The content X of actual potassium element in the content A of potassium element and the ammonium molybdate of unit mass in the molybdic oxide of the unit mass of preparing as required, and following formula
Calculate the quality of mixing the saltpetre that potassium molybdic oxide need to add of preparation unit mass.
In second step, the mass ratio of saltpetre and deionized water is: 1:100～200.
In the 4th step, calcination adopts turbine rotary disc formula dryer, and the temperature of calcination is 510 ℃～530 ℃, and the time of calcination is 80～100min.
The invention has the beneficial effects as follows: the method for potassium molybdic oxide is mixed in preparation of the present invention, production technique is easy to control, implementation cost is low, easy and simple to handle, safety, be suitable for the scale operation of molybdic oxide, the additive saltpetre, the deionized water that use are cheap, to operator without injury, pollution-free to Working environment, the molybdic oxide yield rate prepared is high, powder high conformity; Production process is short, and product performance are easy to control, and can meet the demand of different industries different user.
Embodiment
Below in conjunction with embodiment, the present invention is described in detail.
Embodiment 1
The method that potassium molybdic oxide is mixed in preparation, comprises the steps:
The first step, determines the quality that needs the saltpetre adding
The quality of the saltpetre that the molybdic oxide that the content 90g of potassium element and for the preparation of the content 46g of potassium element in 1 ton of ammonium molybdate of molybdic oxide in the molybdic oxide of 1 ton of preparation, and following formula as required calculates 1 ton of preparation need to add is 51.3g:
Wherein C is the quality of the preparation molybdic oxide of the 1 ton saltpetre that need to add;
A is the content of potassium element in the molybdic oxide of 1 ton that needs to prepare;
X is the content of potassium element in 1 ton of ammonium molybdate;
Second step, prepares potassium nitrate solution
Get the saltpetre of the definite respective quality of the first step, and adopt deionized water that saltpetre is fully dissolved, make potassium nitrate solution, wherein the mass ratio of saltpetre and deionized water is 1:100;
The 3rd step, spraying is added
The potassium nitrate solution that second step is made is added in the ammonium molybdate of 1 ton by the mode of spraying, makes mixture;
The 4th step, potassium molybdic oxide is mixed in preparation
The mixture that the 3rd step is made carries out calcination, adopts turbine rotary disc formula dryer during calcination, and the temperature of calcination is 510 ℃, and the time of calcination is 100min, obtains the satisfactory potassium molybdic oxide of mixing.
In the molybdic oxide that the present embodiment prepares, the content of potassium element is 89.5ppm, and the quality that namely contains potassium element in 1 ton of molybdic oxide is 89.5g, and detects through Atomic Absorption Spectroscopy AAS, and the distribution of potassium element in molybdic oxide is very even.
Embodiment 2
The method that potassium molybdic oxide is mixed in preparation, comprises the steps:
The first step, determines the quality that needs the saltpetre adding
The quality of the saltpetre that the molybdic oxide that the content 75g of potassium element and for the preparation of the content 35g of potassium element in 1 ton of ammonium molybdate of molybdic oxide in the molybdic oxide of 1 ton of preparation, and following formula as required calculates 1 ton of preparation need to add is 53.1g:
Wherein C is the quality of the preparation molybdic oxide of the 1 ton saltpetre that need to add;
A is the content of potassium element in the molybdic oxide of 1 ton that needs to prepare;
X is the content of potassium element in 1 ton of ammonium molybdate;
Second step, prepares potassium nitrate solution
Get the saltpetre of the definite respective quality of the first step, and adopt deionized water that saltpetre is fully dissolved, make potassium nitrate solution, wherein the mass ratio of saltpetre and deionized water is 1:200;
The 3rd step, spraying is added
The potassium nitrate solution that second step is made is added in the ammonium molybdate of 1 ton by the mode of spraying, makes mixture;
The 4th step, potassium molybdic oxide is mixed in preparation
The mixture that the 3rd step is made carries out calcination, adopts turbine rotary disc formula dryer during calcination, and the temperature of calcination is 530 ℃, and the time of calcination is 80min, obtains the satisfactory potassium molybdic oxide of mixing.
In the molybdic oxide that the present embodiment prepares, the content of potassium element is 74.8ppm, and the quality that namely contains potassium element in 1 ton of molybdic oxide is 74.8g, and detects through Atomic Absorption Spectroscopy AAS, and the distribution of potassium element in molybdic oxide is very even.
Embodiment 3
The method that potassium molybdic oxide is mixed in preparation, comprises the steps:
The first step, determines the quality that needs the saltpetre adding
The quality of the saltpetre that the molybdic oxide that the content 120g of potassium element and for the preparation of the content 60g of potassium element in 1 ton of ammonium molybdate of molybdic oxide in the molybdic oxide of 1 ton of preparation, and following formula as required calculates 1 ton of preparation need to add is 72.5g:
Wherein C is the quality of the preparation molybdic oxide of the 1 ton saltpetre that need to add;
A is the content of potassium element in the molybdic oxide of 1 ton that needs to prepare;
X is the content of potassium element in 1 ton of ammonium molybdate;
Second step, prepares potassium nitrate solution
Get the saltpetre of the definite respective quality of the first step, and adopt deionized water that saltpetre is fully dissolved, make potassium nitrate solution, wherein the mass ratio of saltpetre and deionized water is 1:150;
The 3rd step, spraying is added
The potassium nitrate solution that second step is made is added in the ammonium molybdate of 1 ton by the mode of spraying, makes mixture;
The 4th step, potassium molybdic oxide is mixed in preparation
The mixture that the 3rd step is made carries out calcination, adopts turbine rotary disc formula dryer during calcination, and the temperature of calcination is 520 ℃, and the time of calcination is 90min, obtains the satisfactory potassium molybdic oxide of mixing.
In the molybdic oxide that the present embodiment prepares, the content of potassium element is 120.1ppm, and the quality that namely contains potassium element in 1 ton of molybdic oxide is 120.1g, and detects through Atomic Absorption Spectroscopy AAS, and the distribution of potassium element in molybdic oxide is very even.
By the way, the method that potassium molybdic oxide is mixed in preparation of the present invention has solved existing molybdic oxide preparation method and has reduced the problem of Determination of Potassium and directly in molybdic oxide finished product, add potassium element and cause in molybdenum powder product Determination of Potassium inhomogeneous, the unsettled problem of molybdenum powder quality, and the method production technique is easy to control, implementation cost is low, easy and simple to handle, safety, be suitable for the scale operation of molybdic oxide, the additive saltpetre using, deionized water is cheap, to operator without injury, pollution-free to Working environment, the molybdic oxide yield rate of preparing is high, powder high conformity, production process is short, and product performance are easy to control, and can meet the demand of different industries different user.
Claims (4)
1. the method that potassium molybdic oxide is mixed in preparation, is characterized in that, comprises the steps:
The first step, determines the quality that needs the saltpetre adding
The content of potassium element and calculate the quality that needs the saltpetre adding in the molybdic oxide of preparation unit mass for the preparation of the content meter of potassium element in the ammonium molybdate of molybdic oxide in the molybdic oxide of unit mass of preparation as required;
Second step, prepares potassium nitrate solution
Get the saltpetre of the definite respective quality of the first step, and adopt deionized water that described saltpetre is fully dissolved, make potassium nitrate solution;
The 3rd step, spraying is added
The potassium nitrate solution that second step is made is added in ammonium molybdate by the mode of spraying, makes mixture;
The 4th step, potassium molybdic oxide is mixed in preparation
The mixture that the 3rd step is made carries out calcination, obtains the satisfactory potassium molybdic oxide of mixing.
2. the method for potassium molybdic oxide is mixed in preparation as claimed in claim 1, it is characterized in that, needs the method for calculation of the saltpetre quality C adding to be in the first step:
The content X of actual potassium element in the content A of potassium element and the ammonium molybdate of unit mass in the molybdic oxide of the unit mass of preparing as required, and following formula
Calculate the quality of mixing the saltpetre that potassium molybdic oxide need to add of preparation unit mass.
3. the method for potassium molybdic oxide is mixed in preparation as claimed in claim 1, it is characterized in that, in second step, the mass ratio of saltpetre and deionized water is: 1:100～200.
4. the method for potassium molybdic oxide is mixed in preparation as claimed in claim 1, it is characterized in that, calcination described in the 4th step adopts turbine rotary disc formula dryer, and the temperature of calcination is 510 ℃～530 ℃, and the time of calcination is 80～100min.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201310713108.0A CN103723769A (en) | 2013-12-20 | 2013-12-20 | Method for preparing potassium-doped molybdenum trioxide |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201310713108.0A CN103723769A (en) | 2013-12-20 | 2013-12-20 | Method for preparing potassium-doped molybdenum trioxide |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN103723769A true CN103723769A (en) | 2014-04-16 |
Family
ID=50448116
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201310713108.0A Pending CN103723769A (en) | 2013-12-20 | 2013-12-20 | Method for preparing potassium-doped molybdenum trioxide |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN103723769A (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105789467A (en) * | 2016-04-19 | 2016-07-20 | Tcl集团股份有限公司 | Preparation method of In-doped MoO3 thin film and application of thin film in QLED |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101487093A (en) * | 2009-03-05 | 2009-07-22 | 株洲硬质合金集团有限公司 | Doped high temperature molybdenum alloy bar and wire, and preparation thereof |
| CN101643874B (en) * | 2009-09-15 | 2011-08-17 | 金堆城钼业光明（山东）股份有限公司 | Rare earth ammonium tetramolybdate preparation method |
-
2013
- 2013-12-20 CN CN201310713108.0A patent/CN103723769A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101487093A (en) * | 2009-03-05 | 2009-07-22 | 株洲硬质合金集团有限公司 | Doped high temperature molybdenum alloy bar and wire, and preparation thereof |
| CN101643874B (en) * | 2009-09-15 | 2011-08-17 | 金堆城钼业光明（山东）股份有限公司 | Rare earth ammonium tetramolybdate preparation method |
Non-Patent Citations (2)
| Title |
|---|
| 向铁根: "《钼冶金》", 31 December 2009, 中南大学出版社 * |
| 雷宁宁等: "纯三氧化钼在氨水中溶解现象的分析研究", 《中国钼业》 * |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105789467A (en) * | 2016-04-19 | 2016-07-20 | Tcl集团股份有限公司 | Preparation method of In-doped MoO3 thin film and application of thin film in QLED |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN108067242B (en) | A kind of recycling and reusing method of hydrogenation catalyst dead meal | |
| CN102660706A (en) | Lanthanum-doped molybdenum alloy wire for thermal spraying and preparation method thereof | |
| CN102719856B (en) | Method for removing alkali metal via electrolytic aluminum liquid | |
| CN104946912A (en) | Rear earth high-entropy alloy of close-packed hexagonal structure | |
| CN106430334A (en) | Preparation method of palladium nitrate solution | |
| CN102616826A (en) | Pyrolysis method for preparing trivalent rare earth oxide | |
| CN106807383A (en) | A kind of method for preparing catalyst of ammonia and preparation method thereof and the catalyst preparation ammonia | |
| CN102633291B (en) | Preparation method for basic copper nitrate | |
| CN103723769A (en) | Method for preparing potassium-doped molybdenum trioxide | |
| CN108101121A (en) | A kind of resource recycling method of iron content waste sulfuric acid solution | |
| CN102701293A (en) | Production method of basic cobalt carbonate | |
| CN102949996A (en) | Preparation method of unsaturated fat nickel hydrogenation catalyst | |
| CN102643990B (en) | Method for removing trace Cu in high-purity Ni by chelate resin | |
| CN110983091B (en) | Method for preparing nano tungsten-based powder material by doping yttrium oxide in liquid-liquid manner | |
| CN102251121A (en) | Method for preparing industrial molybdenum trioxide by roasting ammonia leaching residue | |
| CN102633290A (en) | Preparation method for basic copper nitrate | |
| CN105271288A (en) | Method for preparing molecular sieve by taking oxidized stone as raw material | |
| CN106179388A (en) | A kind of preparation method of hydrotreating catalyst | |
| CN107337491A (en) | A kind of method for preparing siliceous fertilizer using solar energy crystalline silicon Buddha's warrior attendant wire cutting waste slurry | |
| CN107262100B (en) | Preparation method of oil hydrogenation nano catalyst with improved catalytic activity | |
| CN108620083A (en) | A kind of recycling method of hydrogenation catalyst dead meal | |
| CN107497429B (en) | A kind of preparation method and application of Ag doping tungsten oxide photcatalyst | |
| CN105617939A (en) | Synthetic process of high self-sharpening diamond | |
| CN103877914A (en) | High-strength fine-particle cubic boron nitride monocrystal as well as synthesizing method thereof and application | |
| CN107217186B (en) | A kind of preparation method of modified metal based composites |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C12 | Rejection of a patent application after its publication | ||
| RJ01 | Rejection of invention patent application after publication |
Application publication date: 20140416 |