CN101020239A - Low potassium molybdenum powder preparing process - Google Patents
Low potassium molybdenum powder preparing process Download PDFInfo
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- CN101020239A CN101020239A CN 200710020652 CN200710020652A CN101020239A CN 101020239 A CN101020239 A CN 101020239A CN 200710020652 CN200710020652 CN 200710020652 CN 200710020652 A CN200710020652 A CN 200710020652A CN 101020239 A CN101020239 A CN 101020239A
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Abstract
The low potassium molybdenum powder preparing process includes the following steps: the first hydrogen reduction of ammonium molybdate to produce molybdenum dioxide, sieving, water washing or acid pickling molybdenum dioxide, solid-liquid separation and/or stoving, the secondary hydrogen reduction to produce molybdenum powder, and sieving to obtain the molybdenum powder product. The technological process is simple and has obvious effect of eliminate potassium impurity.
Description
Technical field
The present invention relates to the preparation method of metal molybdenum, relate in particular to the process of removing potassium impurity in the molybdenum powder and preparing low-potassium molybdenum powder.
Background technology
Metal molybdenum has excellent physics and chemical properties such as high-melting-point, high-wearing feature, good heat-conductivity conducting performance and low-expansion coefficient because of it, have a wide range of applications on industrial production such as electronics, electric light source, metallurgy and metal processing industry.And molybdenum powder is a material of producing various molybdenum products, and many molybdenums and molybdenum powder require it to have higher purity on using.
Traditional molybdenum powder preparation technology is to be raw material with the ammonium molybdate, generates molybdenum dioxide through a low temperature hydrogen reduction, carries out the secondary high-temperature hydrogen reduction after the screening, criticizes out finished product molybdenum powder through screening, combined group again.The molybdenum powder quality that above-mentioned traditional handicraft method is produced, depend on the raw material quality of ammonium molybdate to a great extent, and potassium just is the highest impurity element of content in the ammonium molybdate product, and existing molybdenum powder production technology can not effectively be removed potassium impurity, and the residual ratio of its potassium is very high.
Because potassium is the low melting point alkali metal, its fusing point has only 63 ℃, 774 ℃ of boiling points; Potassium can be combined to potassium oxide with oxygen, dissolves readily in the water, and very easily moisture absorption generation has the very potassium hydroxide of severe corrosive in air, is one of the strongest alkali.Thereby in high temperature sintering (sintering temperature is more than the 1900 ℃) process of molybdenum or as electric source material the time, potassium can evaporate with gaseous state, is bonded on the devices such as high-temperature heating element or heating light-emitting component; Or influence the insulating properties of electrical equipment after the moisture absorption, or with the corrosion of highly basic form heater element, refractory material and insulation material, polluted product surface; Even if molybdenum is as the additive of alloy or stainless steel etc., because the molybdenum of high potassium content, can bring potassium in the materials such as alloy or stainless steel into, and potassium a kind of often harmful or people in these materials do not wish the element that its exists, and directly affect the machinery and the physical property of alloy or stainless steel etc.Therefore, be badly in need of low-potassium molybdenum powder on the market.
Summary of the invention
In order to overcome the existing existing above-mentioned deficiency of process, the technical problem to be solved in the present invention provides a kind of low-potassium molybdenum powder preparation technology that can remove potassium impurity in the molybdenum powder effectively.
In order to solve the problems of the technologies described above, the preparation technology of low-potassium molybdenum powder of the present invention, it comprises the following steps: that (1) generates molybdenum dioxide with hydrogen reducing of ammonium molybdate; (2) will reduce the molybdenum dioxide that generates sieves; (3) molybdenum dioxide after the screening is washed or pickling; (3) molybdenum dioxide Separation of Solid and Liquid and the oven dry after washing or the pickling; (4) molybdenum dioxide after Separation of Solid and Liquid and the oven dry is carried out the secondary hydrogen reducing and generate molybdenum powder; (5) molybdenum powder sieves the molybdenum powder that gets product.
Preparation technology of the present invention utilized dexterously molybdenum dioxide powder fine size, specific surface big, in water or acid, do not dissolve; And the easy water-soluble or sour characteristics of potassium.After molybdenum dioxide forms, a washing or pickling process have been increased, like this in washing or acid cleaning process, potassium impurity in the titanium dioxide molybdenum powder, and other easy molten impurity will dissolve, thereby removed the impurity component in the titanium dioxide molybdenum powder effectively, improved the purity of molybdenum greatly, molybdenum powder is best in quality, and serviceability is better.On the other hand, because the activity of potassium in ammonium molybdate is very strong, it is generally acknowledged in the practice, potassium can quicken the fission of ammonium molybdate when reduction, thereby improves the reduction efficiency of ammonium molybdate, so the potassium process of removing of the present invention seems very reasonable, it is to go to remove potassium after ammonium molybdate fission reduction again, this had both made full use of the advantage of potassium in ammonium molybdate hydrogen reducing process, had reached the potassium impurity of removing in the finished product molybdenum powder again, had dual technique effect.
The further technical scheme of the present invention is that in described washing or pickling, the washing weight ratio of titanium dioxide molybdenum powder and water or watery hydrochloric acid is between 1: 2～5.Described pickling cleaning solution is that concentration is 0～10% watery hydrochloric acid.Adopt water or watery hydrochloric acid as washing agent, select suitable washing weight ratio simultaneously for use, make that not only washing procedure is simple and convenient, and have desirable detersive efficiency.
The further again technical scheme of the present invention is 40～95 ℃ of the washing reaction temperature of described washing or pickling, 1～10 hour washing reaction time.Help improving dust removal rate like this, stablize impurity-eliminating effect, improve the purity of molybdenum powder.
The specific embodiment
Embodiment 1
It is some to get ammonium molybdate, uses multi-tube furnace or four pipe reduction furnaces to carry out the low temperature hydrogen reduction, and 400-650 ℃ of reaction warm area, ammonium molybdate push away fast 3 boats/0.5 hour, 2.5 cubic metres/hour of every pipe hydrogen flowing quantities.The molybdenum dioxide that the reduction back generates sieves, by the screen cloth in 175um aperture.
Get above-mentioned titanium dioxide molybdenum powder 500kg again through a hydrogen reduction, be added in the reaction pot of the strap clamp cover that is placed with the 1500Kg pure water, under stirring condition, be heated to 90 ℃, kept 3 hours, emit suction filtration, behind pure water washing secondary, put into baking oven in 80 ℃ of oven dry 10 hours, screening is by the screen cloth in 350um aperture.Certainly except that oven dry, also can adopt other common solid-liquid separating method, or method such as adopt that Separation of Solid and Liquid is dried again.
Titanium dioxide molybdenum powder after using four pipe hydrogen reduction furnaces to washing carries out the secondary high temperature reduction, and 800-980 ℃ of reaction warm area, titanium dioxide molybdenum powder push away fast 1 boat/0.5 hour, 10.0 cubic meters/hours of every pipe hydrogen flowing quantities.The reduction back generates molybdenum powder, and the molybdenum powder screening is by the screen cloth in 60um aperture.Mixing equipment is the V-type batch mixer, and mixing time is 2 hours.Capable more at this moment molybdenum powder sample analysis, oxygen content 0.10%, potassium content 0.0025%.
Through above-mentioned technical process, the potassium major part in the molybdenum powder is removed, and molybdenum powder has reached higher purity, contains assorted declining to a great extent, thus the properties of product and the result of use of the molybdenum powder that improves greatly.
Embodiment 2
In the present embodiment, the process of preparation titanium dioxide molybdenum powder is same as the previously described embodiments.After a hydrogen reduction makes the titanium dioxide molybdenum powder, the titanium dioxide molybdenum powder 500kg of a hydrogen reduction learns from else's experience, be added in the reaction pot of the strap clamp cover that is placed with 1500Kg pure water and 100Kg hydrochloric acid, under stirring condition, be heated to 90 ℃, kept 3 hours, emit suction filtration, after pure water washing four times, water lotion PH=4.Put into baking oven in 80 ℃ of oven dry 10 hours, screening is by the screen cloth in 350um aperture.
Titanium dioxide molybdenum powder after using four pipe hydrogen reduction furnaces to washing carries out the secondary high temperature reduction and generates molybdenum powder, and 800-980 ℃ of reaction warm area, titanium dioxide molybdenum powder push away fast 1 boat/0.5 hour, 10 cubic meters/hours of every pipe hydrogen flowing quantities.The screening of reduction molybdenum powder is by the screen cloth in 60um aperture.Mixing equipment is the V-type batch mixer, and mixing time is 2 hours.Carry out the molybdenum powder sample analysis, oxygen content 0.08%, potassium content 0.0022%.
Above-mentionedly enumerated two embodiments of the present invention, but above-mentioned embodiment of the present invention can only think all can not limit the present invention to explanation of the present invention, claims have been pointed out scope of the present invention.Therefore, under the situation of basic thought of the present invention,, all should think to fall within the scope of protection of the present invention as long as adopted washing or pickling process.
Claims (6)
1, a kind of preparation technology of low-potassium molybdenum powder is characterized in that: it comprises the following steps: that (1) generates molybdenum dioxide with hydrogen reducing of ammonium molybdate; (2) will reduce the molybdenum dioxide that generates sieves; (3) molybdenum dioxide after the screening is washed or pickling; (3) molybdenum dioxide Separation of Solid and Liquid and the oven dry after washing or the pickling; (4) molybdenum dioxide after Separation of Solid and Liquid and the oven dry is carried out the secondary hydrogen reducing and generate molybdenum powder; (5) molybdenum powder sieves the molybdenum powder that gets product.
2, the preparation technology of low-potassium molybdenum powder according to claim 1 is characterized in that: in described washing or the pickling, the washing weight ratio of titanium dioxide molybdenum powder and water or watery hydrochloric acid is between 1: 2～5.
3, the preparation technology of low-potassium molybdenum powder according to claim 1 is characterized in that: described pickling cleaning solution is that concentration is 0～10% watery hydrochloric acid.
4, according to the preparation technology of claim 1,2 or 3 described low-potassium molybdenum powders, it is characterized in that: 40～95 ℃ of the washing reaction temperature of described washing or pickling, 1～10 hour washing reaction time.
5, the preparation technology of low-potassium molybdenum powder according to claim 1 is characterized in that: 400～650 ℃ of the reaction warm areas of a described hydrogen reducing.
6, the preparation technology of low-potassium molybdenum powder according to claim 1 is characterized in that: 800～980 ℃ of the reaction warm areas of described secondary hydrogen reducing.
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| CN 200710020652 CN101020239A (en) | 2007-03-19 | 2007-03-19 | Low potassium molybdenum powder preparing process |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
| 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 |
| CN108118148A (en) * | 2017-12-13 | 2018-06-05 | 金堆城钼业股份有限公司 | The control method of potassium content in a kind of ammonium molybdate solution |
| CN110919020A (en) * | 2019-12-10 | 2020-03-27 | 河南科技大学 | Preparation method of molybdenum powder with large particle size |
-
2007
- 2007-03-19 CN CN 200710020652 patent/CN101020239A/en active Pending
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
| 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 |
| CN108118148A (en) * | 2017-12-13 | 2018-06-05 | 金堆城钼业股份有限公司 | The control method of potassium content in a kind of ammonium molybdate solution |
| CN110919020A (en) * | 2019-12-10 | 2020-03-27 | 河南科技大学 | Preparation method of molybdenum powder with large particle size |
| CN110919020B (en) * | 2019-12-10 | 2022-10-11 | 河南科技大学 | Preparation method of molybdenum powder with large particle size |
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