CN108502929A - A method of preparing electron level nanometer titanium dioxide molybdenum powder - Google Patents
A method of preparing electron level nanometer titanium dioxide molybdenum powder Download PDFInfo
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- CN108502929A CN108502929A CN201810413981.0A CN201810413981A CN108502929A CN 108502929 A CN108502929 A CN 108502929A CN 201810413981 A CN201810413981 A CN 201810413981A CN 108502929 A CN108502929 A CN 108502929A
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- Prior art keywords
- molybdenum
- powder
- titanium dioxide
- nanometer titanium
- electron level
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- 239000000843 powder Substances 0.000 title claims abstract description 32
- UQJSLVWCKFZHFO-UHFFFAOYSA-N molybdenum(4+) oxygen(2-) titanium(4+) Chemical compound [O-2].[O-2].[Ti+4].[Mo+4] UQJSLVWCKFZHFO-UHFFFAOYSA-N 0.000 title claims abstract description 14
- 238000000034 method Methods 0.000 title claims abstract description 13
- JKQOBWVOAYFWKG-UHFFFAOYSA-N molybdenum trioxide Chemical compound O=[Mo](=O)=O JKQOBWVOAYFWKG-UHFFFAOYSA-N 0.000 claims abstract description 40
- 239000000463 material Substances 0.000 claims abstract description 32
- QXYJCZRRLLQGCR-UHFFFAOYSA-N dioxomolybdenum Chemical compound O=[Mo]=O QXYJCZRRLLQGCR-UHFFFAOYSA-N 0.000 claims abstract description 26
- 239000001257 hydrogen Substances 0.000 claims abstract description 10
- 229910052739 hydrogen Inorganic materials 0.000 claims abstract description 10
- 229910052751 metal Inorganic materials 0.000 claims abstract description 9
- 239000002184 metal Substances 0.000 claims abstract description 9
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims abstract description 8
- 229910052581 Si3N4 Inorganic materials 0.000 claims description 9
- HQVNEWCFYHHQES-UHFFFAOYSA-N silicon nitride Chemical compound N12[Si]34N5[Si]62N3[Si]51N64 HQVNEWCFYHHQES-UHFFFAOYSA-N 0.000 claims description 9
- 239000012466 permeate Substances 0.000 claims description 6
- 239000012528 membrane Substances 0.000 claims description 4
- 238000000926 separation method Methods 0.000 claims description 4
- 238000005491 wire drawing Methods 0.000 claims description 4
- 230000006855 networking Effects 0.000 claims description 3
- 238000006243 chemical reaction Methods 0.000 abstract description 15
- 238000006722 reduction reaction Methods 0.000 abstract description 13
- 239000012535 impurity Substances 0.000 abstract description 5
- 238000002360 preparation method Methods 0.000 abstract description 4
- ZOKXTWBITQBERF-UHFFFAOYSA-N Molybdenum Chemical compound [Mo] ZOKXTWBITQBERF-UHFFFAOYSA-N 0.000 abstract description 3
- 229910052750 molybdenum Inorganic materials 0.000 abstract description 2
- 239000011733 molybdenum Substances 0.000 abstract description 2
- WFKWXMTUELFFGS-UHFFFAOYSA-N tungsten Chemical compound [W] WFKWXMTUELFFGS-UHFFFAOYSA-N 0.000 abstract description 2
- 229910052721 tungsten Inorganic materials 0.000 abstract description 2
- 239000010937 tungsten Substances 0.000 abstract description 2
- 150000002739 metals Chemical class 0.000 abstract 1
- WUAPFZMCVAUBPE-UHFFFAOYSA-N rhenium atom Chemical compound [Re] WUAPFZMCVAUBPE-UHFFFAOYSA-N 0.000 abstract 1
- 239000000047 product Substances 0.000 description 7
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 3
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 description 2
- 239000007795 chemical reaction product Substances 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- 150000002431 hydrogen Chemical class 0.000 description 2
- 229910018487 Ni—Cr Inorganic materials 0.000 description 1
- 239000000956 alloy Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 230000000536 complexating effect Effects 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 239000000686 essence Substances 0.000 description 1
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 description 1
- 239000010931 gold Substances 0.000 description 1
- 229910052737 gold Inorganic materials 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 229910000476 molybdenum oxide Inorganic materials 0.000 description 1
- 239000002086 nanomaterial Substances 0.000 description 1
- 229910052759 nickel Inorganic materials 0.000 description 1
- PQQKPALAQIIWST-UHFFFAOYSA-N oxomolybdenum Chemical compound [Mo]=O PQQKPALAQIIWST-UHFFFAOYSA-N 0.000 description 1
- 238000010791 quenching Methods 0.000 description 1
- 230000000171 quenching effect Effects 0.000 description 1
- 239000000376 reactant Substances 0.000 description 1
- 229910052710 silicon Inorganic materials 0.000 description 1
- 239000010703 silicon Substances 0.000 description 1
- -1 silicon nitrides Chemical class 0.000 description 1
- 239000010935 stainless steel Substances 0.000 description 1
- 229910001220 stainless steel Inorganic materials 0.000 description 1
- GUVRBAGPIYLISA-UHFFFAOYSA-N tantalum atom Chemical compound [Ta] GUVRBAGPIYLISA-UHFFFAOYSA-N 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G39/00—Compounds of molybdenum
- C01G39/02—Oxides; Hydroxides
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F9/00—Making metallic powder or suspensions thereof
- B22F9/16—Making metallic powder or suspensions thereof using chemical processes
- B22F9/18—Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds
- B22F9/20—Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds starting from solid metal compounds
- B22F9/22—Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds starting from solid metal compounds using gaseous reductors
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/80—Compositional purity
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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Organic Chemistry (AREA)
- Nanotechnology (AREA)
- Inorganic Chemistry (AREA)
- Physics & Mathematics (AREA)
- General Chemical & Material Sciences (AREA)
- Composite Materials (AREA)
- Condensed Matter Physics & Semiconductors (AREA)
- General Physics & Mathematics (AREA)
- Materials Engineering (AREA)
- Crystallography & Structural Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Manufacture And Refinement Of Metals (AREA)
- Inorganic Compounds Of Heavy Metals (AREA)
Abstract
The present invention proposes a kind of method preparing electron level nanometer titanium dioxide molybdenum powder, includes the following steps：Step 1, by high-purity Nano-class molybdenum trioxide powder in material boat；Material boat equipped with molybdenum trioxide is passed sequentially through and is set in the reduction furnace there are five humidity province by step 2, and reverse direction is passed through hydrogen reducing processing.The present invention can greatly reduce the control temperature needed for reaction, improve the efficiency of whole reduction reaction, reduce the generation of impurity, be suitable for preparing high-purity molybdenum dioxide product, be also applied for the preparation method of common tungsten, molybdenum, rhenium powder and other metals.
Description
Technical field
The present invention relates to a kind of methods preparing electron level nanometer titanium dioxide molybdenum powder.
Background technology
Currently, during molybdenum trioxide is prepared molybdenum dioxide using reduction furnace, usually by molybdenum trioxide powder
It is sent in reduction furnace using 500 DEG C or more of high temperature.During reduction, since powder is stacking states, often in stacking
The temperature of the bottom molybdenum trioxide powder of portion or stacking is not achieved reaction temperature its internal reaction temperature that is not up to and does not restore
Reaction.Therefore, we just need to improve reaction temperature to promote yield rate.But after we improve high temperature, inside stacking or
When bottom reaches reaction temperature generation molybdenum dioxide, other reactions occur for the positions such as surface, often improve the yield of impurity.
Meanwhile during reduction reaction, stacking prevents in container, container generally uses nickel complexing gold, and inside occurs
The steam that reaction generates can not be excluded directly in time, formed water droplet and entered molybdenum dioxide (MoO2) formation caking phenomenon, drip material
Not only increase molybdenum dioxide oversize, but also influence follow-up molybdenum powder product quality, while reducing the purity of product.
Invention content
The present invention proposes a kind of method preparing electron level nanometer titanium dioxide molybdenum powder, can greatly reduce needed for reaction
Temperature is controlled, the efficiency of whole reduction reaction is improved, reduces the generation of impurity, is suitable for preparing high-purity molybdenum dioxide product,
It is also applied for the preparation of common tungsten, molybdenum, tantalum powder..
The technical proposal of the invention is realized in this way：
A method of preparing electron level nanometer titanium dioxide molybdenum powder, which is characterized in that include the following steps：
Step 1, by high-purity Nano-class molybdenum trioxide powder in material boat；
Material boat equipped with molybdenum trioxide is passed sequentially through and is set in the reduction furnace there are five humidity province by step 2, and reverse direction
It is passed through hydrogen reducing processing.
Preferably, expect that boat is using channel-shaped made of silicon nitride material described in step 1.
Preferably, expect that the bottom surface of boat is that ventilative structure is made using silicon nitride material described in step 1.
Preferably, the bottom surface of the material boat forms highly dense silk net using metal wire-drawing networking, and gap can permeate moisture
Son, impermeable molybdenum trioxide powder and molybdenum dioxide powder.
Preferably, the bottom surface of the material boat is made arc-shaped of metal membrane separation technique, and gap can permeate hydrone,
Impermeable molybdenum trioxide powder and molybdenum dioxide powder.
Preferably, the temperature of five humidity provinces is followed successively by step 2：300~320 DEG C, 320~340 DEG C, 340~375
DEG C, 340~375 DEG C, 300~330 DEG C.
What the present invention generated has the beneficial effect that：Expect that boat is made of silicon nitride material in the present invention, and expects boat be made can
Ventilating structure, such as high desnity metal wire drawing are molded at web frame, metal membrane separation technique, and hydrogen reducing shape can be passed through with high temperature
At molybdenum dioxide.Compare and the prior art, material boat uses silicon nitride material, use than in the prior art Ni-Cr stainless steel or
For other materials, under the conditions of identical technical parameter, reaction temperature can be reduced, avoids the generation of impurity, is suitable for making
The preparation of standby electron level nanometer titanium dioxide molybdenum.
Description of the drawings
In order to more clearly explain the embodiment of the invention or the technical proposal in the existing technology, to embodiment or will show below
There is attached drawing needed in technology description to be briefly described, it should be apparent that, the accompanying drawings in the following description is only this
Some embodiments of invention for those of ordinary skill in the art without creative efforts, can be with
Obtain other attached drawings according to these attached drawings.
Fig. 1 is a kind of embodiment schematic diagram of present invention material boat.
Fig. 2 is another embodiment schematic diagram of present invention material boat.
Specific implementation mode
Following will be combined with the drawings in the embodiments of the present invention, and technical solution in the embodiment of the present invention carries out clear, complete
Site preparation describes, it is clear that described embodiments are only a part of the embodiments of the present invention, instead of all the embodiments.It is based on
Embodiment in the present invention, it is obtained by those of ordinary skill in the art without making creative efforts every other
Embodiment shall fall within the protection scope of the present invention.
A kind of method preparing electron level nanometer titanium dioxide molybdenum powder as shown in Figs. 1-2, includes the following steps：
Step 1, by high-purity Nano-class molybdenum trioxide powder in material boat；
Material boat equipped with molybdenum trioxide is passed sequentially through and is set in the reduction furnace there are five humidity province by step 2, and reverse direction
It is passed through hydrogen reducing processing.
Expect that boat is using channel-shaped made of silicon nitride material, directly by existing high temperature resistant described in the present embodiment step 1
The alloy material of corrosion is changed to silicon nitride, improves degree of being heated evenly and the thermal efficiency；It is ventilative structure that bottom surface, which can also be used, material
The ontology material of boat is 316L or 2520, and bottom surface is two kinds of forms：One is bottom surfaces 2 to form highly dense silk using metal wire-drawing networking
Knitmesh (such as Fig. 1)；Can also arc-shaped (such as Fig. 2) be made using metal membrane separation technique, gap can permeate hydrone, cannot
Permeate molybdenum trioxide powder and molybdenum dioxide powder.
Wherein, the temperature of five humidity provinces is followed successively by step 2：300~320 DEG C, 320~340 DEG C, 340~375 DEG C,
340~375 DEG C, 300~330 DEG C.Wherein molybdenum trioxide powder passes sequentially through above-mentioned temperature range, between 300~320 DEG C
The energy of molybdenum trioxide outer-shell electron can be supplemented；Between 320~340 DEG C, mainly first preceding article is provided for reduction reaction
Part, while a part participates in reduction reaction；In 340~375 DEG C, 340~375 DEG C when, molybdenum trioxide total overall reaction become two
Molybdenum oxide；It is mainly cooling section in 300~330 DEG C, avoids quenching from generating steam or impurity, influence the purity of product.
The invention firstly uses silicon nitrides to the superconductivity of heat so that and entire molybdenum trioxide powder heap can be heated evenly,
The reaction temperature for needing to control can greatly be reduced；Second is sufficiently stable under silicon nitride high temperature resistant, hydrogen atmosphere, in material boat
The especially active high electron level nanoscale material of reaction mass does not generate any secondary pollution, ensure that the purity of product,
Improve product quality.
It will expect that boat bottom makes the form of ventilative structure into simultaneously, traditional reduction reaction is hydrogen from the top down into boat
It is permeated in reaction mass, reduction reaction occurs, reaction product water vapour is inversely gone from bottom to top, with hydrogen, leans on high concentration
It is spread into hydrogen, material boat bottom of the invention is ventilative, and reaction product water vapour is since molecule is heavier, with hydrogen movement side
To unanimously being flowed out from bottom, reduce pollution of the material of material boat to product itself, especially reactant purity is electron level grain
Diameter is nano level reaction mass, and pollution level may be implemented and reach zero.
The foregoing is merely illustrative of the preferred embodiments of the present invention, is not intended to limit the invention, all essences in the present invention
With within principle, any modification, equivalent replacement, improvement and so on should all be included in the protection scope of the present invention god.
Claims (6)
1. a kind of method preparing electron level nanometer titanium dioxide molybdenum powder, which is characterized in that include the following steps：
Step 1, by high-purity Nano-class molybdenum trioxide powder in material boat；
Material boat equipped with molybdenum trioxide is passed sequentially through and is set in the reduction furnace there are five humidity province by step 2, and reverse direction is passed through
Hydrogen reducing processing.
2. a kind of method preparing electron level nanometer titanium dioxide molybdenum powder as described in claim 1, which is characterized in that in step 1
The material boat is using channel-shaped made of silicon nitride material.
3. a kind of method preparing electron level nanometer titanium dioxide molybdenum powder as described in claim 1, which is characterized in that in step 1
The bottom surface of the material boat is that ventilative structure is made using silicon nitride material.
4. a kind of method preparing electron level nanometer titanium dioxide molybdenum powder as claimed in claim 3, which is characterized in that the material boat
Bottom surface highly dense silk net is formed using metal wire-drawing networking, gap can permeate hydrone, impermeable molybdenum trioxide powder
With molybdenum dioxide powder.
5. a kind of method preparing electron level nanometer titanium dioxide molybdenum powder as claimed in claim 3, which is characterized in that the material boat
Bottom surface be made of metal membrane separation technique arc-shaped, gap can permeate hydrone, impermeable molybdenum trioxide powder and
Molybdenum dioxide powder.
6. a kind of method preparing electron level nanometer titanium dioxide molybdenum powder as described in claim 1, which is characterized in that in step 2
The temperature of five humidity provinces is followed successively by：300~320 DEG C, 320~340 DEG C, 340~375 DEG C, 340~375 DEG C, 300~330
℃。
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201810413981.0A CN108502929A (en) | 2018-05-03 | 2018-05-03 | A method of preparing electron level nanometer titanium dioxide molybdenum powder |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201810413981.0A CN108502929A (en) | 2018-05-03 | 2018-05-03 | A method of preparing electron level nanometer titanium dioxide molybdenum powder |
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| CN108502929A true CN108502929A (en) | 2018-09-07 |
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| CN201810413981.0A Pending CN108502929A (en) | 2018-05-03 | 2018-05-03 | A method of preparing electron level nanometer titanium dioxide molybdenum powder |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109368700A (en) * | 2018-12-13 | 2019-02-22 | 郑州大学 | A kind of non-laminar molybdenum dioxide of two dimension and preparation method thereof |
| CN109399721A (en) * | 2018-12-25 | 2019-03-01 | 金堆城钼业股份有限公司 | A kind of preparation method of molybdenum dioxide |
| CN112222419A (en) * | 2020-12-07 | 2021-01-15 | 西安稀有金属材料研究院有限公司 | Method for preparing nano molybdenum powder by regulating nucleation and growth processes and application |
| CN114653945A (en) * | 2022-02-23 | 2022-06-24 | 江西理工大学 | Preparation method of porous copper with ultrahigh porosity |
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109368700A (en) * | 2018-12-13 | 2019-02-22 | 郑州大学 | A kind of non-laminar molybdenum dioxide of two dimension and preparation method thereof |
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| CN112222419A (en) * | 2020-12-07 | 2021-01-15 | 西安稀有金属材料研究院有限公司 | Method for preparing nano molybdenum powder by regulating nucleation and growth processes and application |
| CN114653945A (en) * | 2022-02-23 | 2022-06-24 | 江西理工大学 | Preparation method of porous copper with ultrahigh porosity |
| CN114653945B (en) * | 2022-02-23 | 2023-12-15 | 江西理工大学 | Preparation method of porous copper with ultrahigh porosity |
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Application publication date: 20180907 |