CN103373714A - Production method of tungsten selenide and production equipment thereof - Google Patents
Production method of tungsten selenide and production equipment thereof Download PDFInfo
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- CN103373714A CN103373714A CN2012101245863A CN201210124586A CN103373714A CN 103373714 A CN103373714 A CN 103373714A CN 2012101245863 A CN2012101245863 A CN 2012101245863A CN 201210124586 A CN201210124586 A CN 201210124586A CN 103373714 A CN103373714 A CN 103373714A
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Abstract
The invention provides a production method of tungsten selenide and production equipment thereof. The production method of tungsten selenide disclosed by the invention comprises the following steps of: vacuumizing tungsten powder to be reacted or introducing protective gas, heating till the temperature is 700-850 DEG C, introducing selenium steam to carry out chemical reaction and finally cooling to obtain tungsten selenide. The purity of tungsten selenide disclosed by the invention is above 99.95%. The corresponding production equipment runs in a hydraulic or mechanical pushing manner, therefore, the production process is continuous; and the production equipment is applied to large-scale industrial production.
Description
Technical field
The present invention relates to a kind of production method of selenizing tungsten;
The invention still further relates to a kind of production unit of selenizing tungsten.
Background technology
According to the current research report of the U.S., selenizing tungsten is the minimum material of thermal conductivity of finding at present.The thermal conductivity of material is lower, and the heat in the expression system more is difficult to scatter and disappear, and the turnover ratio of energy can be higher.Therefore, selenizing tungsten can be used as a kind of new thermal resistance material widespread adoption.Simultaneously, selenizing tungsten is again the minimum solid lubricant of frictional coefficient, is known as lubricated king.The application of this novel material will increase substantially the service efficiency of the energy, is China's energy-saving and emission-reduction, and the especially application in national defence and aerospace field will have the meaning of mileage board formula.
At present, external preparation and application thereof to selenizing tungsten there is no report.Domestic have Wuxi profit roc composite material company limited to apply for title in December, 2010: a kind of preparation method of two selenizing tungsten nanometer sheet, the patent of application number: CN201010572015.7, disclose a kind of preparation method: the mol ratio according to Se: W～2: 1 is got tungsten powder and selenium powder, under argon shield, carry out ball milling after grinding and mixing, then be packaged in the vitreosil pipe, obtain raw mix; Then the above-mentioned raw materials mixture is warming up to 600～700 ℃, is incubated cooling after 1 hour, obtain two selenizing tungsten nanometer sheet.Although this kind method technique is comparatively simple, also produces following defective: 1, the reaction of selenium and tungsten not exclusively has tin anhydride to produce, and production efficiency is low; 2, the inevitable virose tin anhydride that produces in the production process, to personnel and environment have very large infringement and broken outside, be not suitable for large-scale industrial production.
Summary of the invention
The defective that exists for overcoming above-mentioned preparation two selenizing tungsten (also claiming selenizing tungsten) method, a kind of production efficiency is high, the method for nontoxic large-scale industrial production but the object of the present invention is to provide.
Accordingly, but another object of the present invention is to provide that a kind of production efficiency is high, the production unit of nontoxic large-scale industrial production.
The production method of selenizing tungsten of the present invention, realize as follows:
(1) tungsten powder with question response vacuumizes or passes into shielding gas;
(2) keep vacuumizing or passing in the step (1) condition of shielding gas, the tungsten powder in the step (1) is heated to 700
850 ℃, pass into selenium steam and carry out chemical reaction, reaction equation is W+2Se=WSe
2, get selenizing tungsten;
(3) the selenizing tungsten that obtains in the step (2) is cooled to room temperature, namely gets this product.
Preferably, shielding gas is selected argon gas, nitrogen or helium described in the step (1);
The mass ratio of described tungsten powder and described selenium steam is 1: 1.5.
For realizing the production method of selenizing tungsten, the production unit of selenizing tungsten of the present invention comprises:
Opening for feed;
Can with the tungsten powder of question response that pack into reactor described feeding inlet;
Vacuum-pumping or pass into the protector that communicates with described reactor of shielding gas;
The heating unit that described reactor can be heated;
Can pass into the breather that selenium steam communicates with described reactor;
The refrigerating unit that described reactor can be cooled off;
Described reactor can be sent to successively the transport unit of described protector, heating unit, breather, refrigerating unit;
With discharge port.
Preferably, described protector is the vacuum pump that vacuumizes or the air delivery device that can pass into shielding gas;
Refrigerating unit is circulating water cooling device.
With respect to prior art, the production method of selenizing tungsten of the present invention and production unit, the advantage that has is as follows:
1, reduced batch mixing and encapsulation link, Chen Bengeng is low, and efficient is higher;
The technical parameters such as flow that 2, can be by selenium steam and temperature of reactor are controlled the particle size range of selenizing tungsten, and adapting to different use needs, and the selenizing tungsten particle of producing footpath is more even, and purity is higher;
3, the reaction more fully and completely, in the production process without poisonous tin anhydride γ-ray emission, more environmental protection;
4, travelling belt can adopt hydraulic pressure or machinery to push away the boat mode to produce and make the production process serialization, be fit to large-scale industrial production.
Description of drawings
Fig. 1 is production unit structural representation of the present invention.
Embodiment
Further understand the present invention below in conjunction with drawings and the specific embodiments, but they are not limitation of the invention, some nonessential variation and adjustment for those skilled in the art does according to the present invention all are considered as dropping in protection scope of the present invention.
Embodiment 1
Referring to Fig. 1, by opening for feed 1 tungsten powder of question response is packed in each reactor 2, the 1kg tungsten powder of packing in each reactor 2, each reactor 2 places on the travelling belt 7; Travelling belt 7 transmits reactor 2 to vacuum pump 3 places, after successively reactor 2 being vacuumized; Keep vacuum state, travelling belt 7 transmits reactor 2 to heating unit 4, and the tungsten powder in the reactor 2 is heated to 700 ℃; Keep vacuum state, travelling belt 7 transmits reactor 2 to breather 5, and each reactor 2 passes into selenium steam 1.5kg reaction, obtains the selenizing tungsten of high temperature; Travelling belt 7 transmits reactor 2 to refrigerating unit 6, be cooled with circulating water reactor 2, thereby the selenizing tungsten of cooling down high-temperature is to room temperature; Travelling belt 7 transmits reactor 2 to discharge port 8, namely makes this product.The purity that records this product reaches 99.96%.
Referring to Fig. 1, by opening for feed 1 tungsten powder of question response is packed in each reactor 2, the 2kg tungsten powder of packing in each reactor 2, each reactor 2 places on the travelling belt 7; Travelling belt 7 transmits reactor 2 to air delivery device 3 places, successively reactor 2 is passed into argon gas, behind the secluding air; Keep the argon shield state, travelling belt 7 transmits reactor 2 to heating unit 4, and the tungsten powder in the reactor 2 is heated to 800 ℃; Keep the argon shield state, travelling belt 7 transmits reactor 2 to breather 5, and each reactor 2 passes into selenium steam 3kg reaction, obtains the selenizing tungsten of high temperature; Travelling belt 7 transmits reactor 2 to refrigerating unit 6, be cooled with circulating water reactor 2, thereby the selenizing tungsten of cooling down high-temperature is to room temperature; Travelling belt 7 transmits reactor 2 to discharge port 8, namely makes this product.The purity that records this product reaches 99.98%.
Referring to Fig. 1, by opening for feed 1 tungsten powder of question response is packed in each reactor 2, the 3kg tungsten powder of packing in each reactor 2, each reactor 2 places on the travelling belt 7; Travelling belt 7 transmits reactor 2 to air delivery device 3 places, successively reactor 2 is passed into nitrogen, behind the secluding air; Keep the nitrogen protection state, travelling belt 7 transmits reactor 2 to heating unit 4, and the tungsten powder in the reactor 2 is heated to 850 ℃; Keep the nitrogen protection state, travelling belt 7 transmits reactor 2 to breather 5, and each reactor 2 passes into selenium steam 4.5kg reaction, obtains the selenizing tungsten of high temperature; Travelling belt 7 transmits reactor 2 to refrigerating unit 6, be cooled with circulating water reactor 2, thereby the selenizing tungsten of cooling down high-temperature is to room temperature; Travelling belt 7 transmits reactor 2 to discharge port 8, namely makes this product.The purity that records this product reaches 99.97%.
Claims (6)
1. the production method of a selenizing tungsten is characterized in that: comprise the steps:
(1) tungsten powder with question response vacuumizes or passes into shielding gas;
(2) keep vacuumizing or passing in the step (1) condition of shielding gas, the tungsten powder in the step (1) is heated to 700
850 ℃, pass into selenium steam and carry out chemical reaction, reaction equation is W+2Se=WSe
2, get selenizing tungsten;
(3) the selenizing tungsten that obtains in the step (2) is cooled to room temperature, namely gets this product.
2. the production method of selenizing tungsten as claimed in claim 1, it is characterized in that: shielding gas is selected argon gas, nitrogen or helium described in the step (1).
3. the production method of selenizing tungsten as claimed in claim 1, it is characterized in that: the mass ratio of described tungsten powder and described selenium steam is 1: 1.5.
4. production unit of be used for realizing the described selenizing tungsten of claim 1 production method is characterized in that:
Comprise opening for feed;
Can with the tungsten powder of question response that pack into reactor described feeding inlet;
Vacuum-pumping or pass into the protector that communicates with described reactor of shielding gas;
The heating unit that described reactor can be heated;
Can pass into the breather that selenium steam communicates with described reactor;
The refrigerating unit that described reactor can be cooled off;
Described reactor can be sent to successively the transport unit of described protector, heating unit, breather, refrigerating unit;
With discharge port.
5. production unit as claimed in claim 4, it is characterized in that: described protector is the vacuum pump that vacuumizes or the air delivery device that can pass into shielding gas.
6. production unit as claimed in claim 4, it is characterized in that: refrigerating unit is circulating water cooling device.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
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| CN2012101245863A CN103373714A (en) | 2012-04-24 | 2012-04-24 | Production method of tungsten selenide and production equipment thereof |
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| Application Number | Priority Date | Filing Date | Title |
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| CN2012101245863A CN103373714A (en) | 2012-04-24 | 2012-04-24 | Production method of tungsten selenide and production equipment thereof |
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| CN2012101245863A Pending CN103373714A (en) | 2012-04-24 | 2012-04-24 | Production method of tungsten selenide and production equipment thereof |
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4676969A (en) * | 1986-06-23 | 1987-06-30 | Eastman Kodak Company | Method of synthesis of inorganic chalcogenides |
| CN101150151A (en) * | 2007-11-08 | 2008-03-26 | 北京科技大学 | A making method of copper, indium and selenium film for solar battery |
| CN102092690A (en) * | 2010-12-03 | 2011-06-15 | 无锡润鹏复合新材料有限公司 | Method for preparing tungsten diselenide nano sheets |
-
2012
- 2012-04-24 CN CN2012101245863A patent/CN103373714A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4676969A (en) * | 1986-06-23 | 1987-06-30 | Eastman Kodak Company | Method of synthesis of inorganic chalcogenides |
| CN101150151A (en) * | 2007-11-08 | 2008-03-26 | 北京科技大学 | A making method of copper, indium and selenium film for solar battery |
| CN102092690A (en) * | 2010-12-03 | 2011-06-15 | 无锡润鹏复合新材料有限公司 | Method for preparing tungsten diselenide nano sheets |
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Application publication date: 20131030 |