CN101347839A - Method for purifying molybdenum powder - Google Patents
Method for purifying molybdenum powder Download PDFInfo
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- CN101347839A CN101347839A CNA200810146534XA CN200810146534A CN101347839A CN 101347839 A CN101347839 A CN 101347839A CN A200810146534X A CNA200810146534X A CN A200810146534XA CN 200810146534 A CN200810146534 A CN 200810146534A CN 101347839 A CN101347839 A CN 101347839A
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Abstract
The invention discloses a purification method for molybdenum powder, which relates to a preparation method for high purity molybdenum. The invention is characterized in that the purification process comprises the steps as follows: (1) take common molybdenum powder as raw material; (2) the impurity in the raw material molybdenum powder is removed by water washing or acid washing; (3) the molybdenum power is dried after water washing or acid washing; (4) the impurity is removed by hydrogen shield or in vacuum at high temperature; (5) purity molybdenum powder is prepared by screening in vacuum. The method of the invention can not only decrease impurity content in the molybdenum powder, but also improve the physical properties of the molybdenum powder such as morphology, granularity, apparent density, etc. Compared with the common molybdenum powder, the production has the advantages of high purity and wide application range. The product of the invention is widely used in electronic processing industry, and has potential in the target field of LCD display particularly.
Description
Technical field
A kind of purification process of molybdenum powder relates to a kind of preparation method of high pure molybdenum powder.
Background technology
Molybdenum is a kind of have higher boiling and dystectic refractory metal, in fields such as steel and iron industry, nonferrous metallurgy, electronics, electric light source, chemical industry, agriculturals purposes is widely arranged.Molybdenum powder is the most important material of various molybdenum products, and molybdenum powder smelting Products Quality performance is had fundamental influence.Along with science and technology is constantly progressive, the molybdenum application constantly enlarges, and this just constantly proposes high-purity developing direction that changes into to each molybdenum powder production firm of higher requirement, particularly molybdenum powder to the quality of molybdenum powder.The technology of preparation high pure molybdenum powder is a lot, as being that predecessor prepares high pure molybdenum powder with high-purity molybdenum trioxide, high all-chloride, and ion-exchange method for refining, fused-salt electrolytic refining method etc.These method complex process, equipment required high, output is little to be difficult for industrialization, molybdenum powder granularity, apparent density, tap density and pattern are undesirable.
Summary of the invention
The present invention seeks to deficiency at above-mentioned prior art existence, provide that a kind of method is simple, purification effect good, cost is low, yield rate is high, easy realization of industrialization, and can effectively improve the purification process of the molybdenum powder of molybdenum powder granularity, apparent density, tap density and pattern.
The present invention is achieved by the following technical solutions.
A kind of purification process of molybdenum powder is characterized in that its purge process comprises:
(1) getting common molybdenum powder is raw material;
(2) the raw material molybdenum powder is through washing or pickling impurity removal;
(3) molybdenum powder after washing or the pickling is dried;
(4) high-temperature hydrogen protection removal of impurities or vacuum high-temperature removal of impurities;
(5) sieve the molybdenum powder that makes purifying through vacuum.
The purification process of a kind of molybdenum powder of the present invention, the temperature that it is characterized in that described raw material molybdenum powder water-washing process is 10～95 ℃, washing time 1～6h, the washing solid-to-liquid ratio is 1: 1～5, with pure water material is washed after the Separation of Solid and Liquid of washing back.
The purification process of a kind of molybdenum powder of the present invention, it is characterized in that described raw material molybdenum powder pickling impurity removal process can select hydrochloric acid or nitric acid, the mass concentration of washing lotion acid is 1%～10%, pickling temperature is 10～95 ℃, pickling time 1～6h, the pickling solid-to-liquid ratio is 1: 1～5, with pure water material is washed after the Separation of Solid and Liquid after the pickling.
The purification process of a kind of molybdenum powder of the present invention is characterized in that the molybdenum powder bake out temperature after described washing or the pickling is 50～200 ℃, and drying time is 1～6h.
The purification process of a kind of molybdenum powder of the present invention is characterized in that the temperature of described high-temperature hydrogen protection reduction removal of impurities is 1100 ℃～1500 ℃, and temperature retention time is 1～6h.
The purification process of a kind of molybdenum powder of the present invention is characterized in that described high-temperature vacuum removal of impurities temperature is 1100～1500 ℃, and temperature retention time is 1～6h, and vacuum is higher than 10
-3Pa.
The purification process of a kind of molybdenum powder of the present invention is characterized in that it is 200 mesh standard sieves that the described molybdenum powder that makes purifying through vacuum screening is crossed grit number, gets sieve and is product down.
The method applied in the present invention at first utilizes molybdenum powder characteristics water insoluble, that be insoluble to weak acid to remove soluble impurity in the molybdenum powder.Utilize the high characteristics of molybdenum powder fusing point again, at high temperature remove volatile impurity.Make molybdenum powder obtain purifying through above two main removal of impurities means.The purification process of a kind of molybdenum powder of the present invention is raw material with common molybdenum powder, and is low to ingredient requirement, the commercially available molybdenum powder of ordinary production all can be used as raw material of the present invention, and production technology is easy to control, and is easy and simple to handle, safe, reliable, be suitable for large-scale production, low, the high conformity of product cost.Method of the present invention not only can reduce the impurity content in the molybdenum powder, also can improve the physical property such as pattern, granularity, apparent density of molybdenum powder.Molybdenum powder that makes and common molybdenum powder are compared, and product has purity height, applied widely, have widely to use in the electronics processing industry, especially have more potentiality in LCD display target field.
Description of drawings
Fig. 1 is a method process chart of the present invention.
The specific embodiment
A kind of purification process of molybdenum powder, its purge process comprises: (1) gets common molybdenum powder is raw material; (2) washing of raw material molybdenum powder or pickling impurity removal; (3) the molybdenum powder oven dry after washing or the pickling; (4) high-temperature hydrogen protection removal of impurities or vacuum high-temperature removal of impurities; (5) sieve the molybdenum powder that makes purifying through vacuum.
During operation, be raw material with common molybdenum powder; The temperature of washing is 10～95 ℃, washing time 1～6h, and the washing solid-to-liquid ratio is 1: 1～5; Pickling can be washed and be selected hydrochloric acid or nitric acid, and concentration is 1～10%, and pickling temperature is 10～95 ℃, pickling time 1～6h, and the pickling solid-to-liquid ratio is 1: 1～5; According to the degree of wishing to get the molybdenum powder purifying, but repeating step (2)～(4) are repeatedly washed or pickling; Separation of Solid and Liquid after washing or the pickling is washed material with pure water, dries 1～10h afterwards under 10～95 ℃ of temperature, and the residual moisture content in oven dry back is no more than 2%; Adopt high-temperature hydrogen protection removal of impurities, temperature is 1100～1500 ℃, and temperature retention time is 1～6h, and hydrogen flowing quantity is 0.5～2.0m
3/ h; Adopt the high-temperature vacuum removal of impurities, temperature is 1100～1500 ℃, and temperature retention time is 1～6h, and vacuum is higher than 10
-3Pa, last vacuum state descended 200 mesh standard sieves, got sieve and was product down.
Embodiment 1
Take by weighing the 1000kg molybdenum powder and put into the reactor that fills the 1000kg industrial pure water with heating jacket and agitating device, be heated to 50 ℃ and wash removal of impurities under stirring condition, insulation 60min emits filtration, with the industrial pure water washing once, filter cake is dried 8h under 90 ℃ of conditions.
Above molybdenum powder is carried out high temperature deoxidation and removal of impurities in single warm area Muffle furnace, temperature is 1350 ℃, temperature retention time 4h, thickness of feed layer 3cm, hydrogen flowing quantity 1.0m
3/ h.Come out of the stove when material is cooled to room temperature,, obtain molybdenum powder of the present invention behind the test package through the vacuum screening.
Table 1 molybdenum powder impurity content of the present invention (ppm)
Embodiment 2
Take by weighing 500kg molybdenum powder (impurity content sees Table 1) and put into the reactor that fills the 2500kg industrial pure water with heating jacket and agitating device, room temperature washing 180min under stirring condition, emit filtration, with the industrial pure water washing leaching cake once, filter cake is dried 8h under 90 ℃ of conditions.
Above molybdenum powder is carried out high temperature deoxidation and removal of impurities in single warm area Muffle furnace, temperature is 1100 ℃, temperature retention time 4h, thickness of feed layer 3cm, hydrogen flowing quantity 1.0m
3/ h.Come out of the stove when material is cooled to room temperature,, obtain molybdenum powder of the present invention behind the test package through the vacuum screening.
Table 2 molybdenum powder impurity content of the present invention (ppm)
Embodiment 3
Take by weighing 500kg molybdenum powder (impurity content sees Table 1) and put into the reactor that fills the 2500kg industrial pure water with heating jacket and agitating device, add technical hydrochloric acid 500kg again, under stirring condition, be heated to 90 ℃, emit filtration after stirring insulation 120min, with industrial pure water washing leaching cake secondary, filter cake is dried 5h under 150 ℃ of conditions.
Above molybdenum powder is carried out high temperature deoxidation and removal of impurities in single warm area Muffle furnace, temperature is 1500 ℃, temperature retention time 3h, thickness of feed layer 3.5cm, hydrogen flowing quantity 1.0m
3/ h.Come out of the stove when material is cooled to room temperature,, obtain molybdenum powder of the present invention behind the test package through the vacuum screening.
Table 3 molybdenum powder impurity content of the present invention (ppm)
Embodiment 4
Take by weighing 500kg molybdenum powder (impurity content sees Table 1) and put into the reactor that fills the 2500kg industrial pure water with heating jacket and agitating device, add industrial nitric acid 200kg again, under stirring condition, be heated to 50 ℃, emit filtration after stirring insulation 150min, with industrial pure water washing leaching cake secondary, filter cake is dried 3h under 200 ℃ of conditions.
Above molybdenum powder is carried out high temperature deoxidation and removal of impurities in vacuum drying oven, vacuum is 1 * 10
-4Pa, temperature is 1200 ℃, temperature retention time 4h, thickness of feed layer 2.5cm.Come out of the stove when material is cooled to room temperature,, obtain molybdenum powder of the present invention behind the test package through the vacuum screening.
Table 4 molybdenum powder impurity content of the present invention (ppm)
Claims (7)
1. the purification process of a molybdenum powder is characterized in that its purge process comprises:
(1) getting common molybdenum powder is raw material;
(2) the raw material molybdenum powder is through washing or pickling impurity removal;
(3) molybdenum powder after washing or the pickling is dried;
(4) high-temperature hydrogen protection removal of impurities or vacuum high-temperature removal of impurities;
(5) sieve the molybdenum powder that makes purifying through vacuum.
2. the purification process of a kind of molybdenum powder according to claim 1, the temperature that it is characterized in that described raw material molybdenum powder water-washing process is 10～95 ℃, washing time 1～6h, the washing solid-to-liquid ratio is 1: 1～5, with pure water material is washed after the Separation of Solid and Liquid of washing back.
3. the purification process of a kind of molybdenum powder according to claim 1, it is characterized in that described raw material molybdenum powder pickling impurity removal process can select hydrochloric acid or nitric acid, the mass concentration of washing lotion acid is 1%～10%, pickling temperature is 10～95 ℃, pickling time 1～6h, the pickling solid-to-liquid ratio is 1: 1～5, with pure water material is washed after the Separation of Solid and Liquid after the pickling.
4. the purification process of a kind of molybdenum powder according to claim 1 is characterized in that the molybdenum powder bake out temperature after described washing or the pickling is 50～200 ℃, and drying time is 1～6h.
5. the purification process of a kind of molybdenum powder according to claim 1 is characterized in that the temperature of described high-temperature hydrogen protection reduction removal of impurities is 1100 ℃～1500 ℃, and temperature retention time is 1～6h.
6. the purification process of a kind of molybdenum powder according to claim 1 is characterized in that described high-temperature vacuum removal of impurities temperature is 1100～1500 ℃, and temperature retention time is 1～6h, and vacuum is higher than 10
-3Pa.
7. the purification process of a kind of molybdenum powder according to claim 1 is characterized in that it is 200 mesh standard sieves that the described molybdenum powder that makes purifying through the vacuum screening is crossed grit number, gets sieve and is product down.
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| CNA200810146534XA CN101347839A (en) | 2008-09-02 | 2008-09-02 | Method for purifying molybdenum powder |
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101518865B (en) * | 2009-03-25 | 2010-08-04 | 盛华伟 | High-purity molybdenum filament production method |
| CN102284704A (en) * | 2011-07-30 | 2011-12-21 | 金堆城钼业股份有限公司 | Preparation method of small-granularity potassium-doped molybdenum alloy powder |
| CN102632249A (en) * | 2012-03-29 | 2012-08-15 | 洛阳开拓者投资管理有限公司 | Method for preparing metal molybdenum powder |
| CN103255288A (en) * | 2012-02-17 | 2013-08-21 | 苏州艾默特材料技术有限公司 | Purification method of industrial molybdenum powder |
| CN104707994A (en) * | 2015-03-19 | 2015-06-17 | 金堆城钼业股份有限公司 | Impurity removal method for seepage refractory metal powder |
| CN105200231A (en) * | 2015-09-28 | 2015-12-30 | 昆明理工大学 | Method for preparing molybdenum powder and sulfur from molybdenite concentrate |
| CN106735193A (en) * | 2016-12-23 | 2017-05-31 | 西安瑞福莱钨钼有限公司 | A kind of preparation method of low potassium content molybdenum plate blank |
-
2008
- 2008-09-02 CN CNA200810146534XA patent/CN101347839A/en active Pending
Cited By (11)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101518865B (en) * | 2009-03-25 | 2010-08-04 | 盛华伟 | High-purity molybdenum filament production method |
| CN102284704A (en) * | 2011-07-30 | 2011-12-21 | 金堆城钼业股份有限公司 | Preparation method of small-granularity potassium-doped molybdenum alloy powder |
| CN102284704B (en) * | 2011-07-30 | 2013-08-21 | 金堆城钼业股份有限公司 | Preparation method of small-granularity potassium-doped molybdenum alloy powder |
| CN103255288A (en) * | 2012-02-17 | 2013-08-21 | 苏州艾默特材料技术有限公司 | Purification method of industrial molybdenum powder |
| CN103255288B (en) * | 2012-02-17 | 2014-11-26 | 苏州艾默特材料技术有限公司 | Purification method of industrial molybdenum powder |
| CN102632249A (en) * | 2012-03-29 | 2012-08-15 | 洛阳开拓者投资管理有限公司 | Method for preparing metal molybdenum powder |
| CN102632249B (en) * | 2012-03-29 | 2013-07-31 | 洛阳开拓者投资管理有限公司 | Method for preparing metal molybdenum powder |
| CN104707994A (en) * | 2015-03-19 | 2015-06-17 | 金堆城钼业股份有限公司 | Impurity removal method for seepage refractory metal powder |
| CN104707994B (en) * | 2015-03-19 | 2017-03-15 | 金堆城钼业股份有限公司 | A kind of impurity-removing method of sepage refractory metal powder |
| CN105200231A (en) * | 2015-09-28 | 2015-12-30 | 昆明理工大学 | Method for preparing molybdenum powder and sulfur from molybdenite concentrate |
| CN106735193A (en) * | 2016-12-23 | 2017-05-31 | 西安瑞福莱钨钼有限公司 | A kind of preparation method of low potassium content molybdenum plate blank |
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Open date: 20090121 |