CN109848431B - Preparation method of fine molybdenum powder - Google Patents
Preparation method of fine molybdenum powder Download PDFInfo
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Abstract
The invention discloses a preparation method of fine molybdenum powder, which comprises the steps of putting superfine molybdenum oxide and common molybdenum oxide into a double-cone mixer, uniformly mixing, then putting into a material boat, carrying out first-stage hydrogen reduction, then cooling to room temperature in a furnace, carrying out second-stage hydrogen reduction, filling nitrogen in a cooling area, cooling, and screening to obtain the fine molybdenum powder. According to the preparation method of the fine molybdenum powder, superfine molybdenum trioxide is added into common molybdenum trioxide according to the proportion and uniformly mixed to form a raw material, then two-stage hydrogen reduction is adopted, the first-stage reduction adopts the proper reduction temperature of the molybdenum trioxide, the reduction of large particle size and small particle size in the raw material is met, the molybdenum dioxide with uniform size is obtained, and the formation of regular superfine molybdenum powder is facilitated; the second stage reduction adopts proper reduction temperature and hydrogen flow rate, thus realizing the production of 0.8-2 μm fine molybdenum powder, not only having simple process and easy batch production, but also greatly reducing the production cost and having good practical value.
Description
Technical Field
The invention belongs to the technical field of molybdenum powder preparation methods, and particularly relates to a preparation method of fine molybdenum powder.
Background
At present, the method for producing molybdenum powder generally adopts ammonium molybdate or molybdenum trioxide as raw materials, and the molybdenum powder is obtained by hydrogen two-stage reduction. The granularity of the molybdenum powder obtained by the conventional method is more than 3.0. However, in order to prepare fine molybdenum powder with a particle size of less than 3 μm, it is common to ball mill the raw material or ball mill molybdenum dioxide obtained by reducing molybdenum trioxide once to obtain molybdenum oxide or molybdenum dioxide with uniform particle size, and finally obtain fine molybdenum powder with uniform size.
The superfine molybdenum powder prepared by the method for preparing molybdenum powder for ceramic metallization (application date: 2012.11.09, application number: 201210447145.7, publication number: 2014.05.21, publication number: 103801706A) is prepared by taking ammonium molybdate as a raw material and performing spray drying reduction on the ammonium molybdate to obtain molybdenum powder, but the molybdenum powder needs to be subjected to chemical decomposition, namely, a dilute nitric acid solution is used for performing chemical decomposition pretreatment on molybdenum powder aggregates to reduce or partially eliminate sintering necks among particles to improve the aggregates, and finally the monodisperse submicron nearly spherical molybdenum powder with narrow particle size distribution is obtained, wherein the particle size of the molybdenum powder is 0.5-2.0 mu m. Thus, although the agglomeration phenomenon of the molybdenum powder is improved and the proper ultra-fine molybdenum powder is obtained, the production cost is greatly increased.
The patent "preparation method of molybdenum powder with high surface activity" (application date: 2013.11.26, application number: 201310618960.X, published date: 2015.12.09, publication number: CN103639417B) discloses that molybdenum oxide is subjected to first-stage reduction to obtain molybdenum dioxide, and the molybdenum dioxide is sieved, ball-milled and then subjected to second-stage reduction to obtain molybdenum powder with the particle size of 2.0-4.0 μm.
In the patent "preparation method of submicron molybdenum powder" (application date: 2010.02.05, application number: 201010107245.6, publication number: 2011.07.20, publication number: CN101758241B), ammonium molybdate or molybdenum trioxide is put into a mechanical crusher to be crushed into fine particle raw materials, and the fine particle raw materials are put into a material boat to be subjected to two-stage reduction to obtain the molybdenum powder with the particle size of less than 1.0 μm.
The two molybdenum powder preparation methods have complex process and difficult control of operation process, and are difficult to produce in batches.
Disclosure of Invention
The invention aims to provide a preparation method of fine molybdenum powder, which solves the problems that the existing preparation method of molybdenum powder is complex in process, difficult to operate, high in production cost and incapable of realizing batch production.
The technical scheme adopted by the invention is that the preparation method of the fine molybdenum powder comprises the following steps:
step 1, mixing raw materials
Taking a proper amount of superfine molybdenum oxide and common molybdenum oxide, placing the superfine molybdenum oxide and the common molybdenum oxide in a double-cone mixer, and uniformly mixing to obtain a prefabricated raw material;
step 2, first stage hydrogen reduction
Loading the prefabricated raw materials obtained in the step (1) into a material boat, carrying out first-stage hydrogen reduction, then cooling the material boat to room temperature, and screening to obtain molybdenum dioxide;
step 3, two-stage hydrogen reduction
And (3) loading the molybdenum dioxide obtained in the step (2) into a material boat, carrying out two-stage hydrogen reduction, taking out, filling nitrogen into a cooling area, cooling to room temperature, and screening to obtain fine molybdenum powder.
The present invention is also characterized in that,
in the step 1, the weight ratio of the superfine molybdenum oxide to the common molybdenum oxide is (0-30%): (70-100%).
The granularity of the superfine molybdenum oxide is 0.1-1 mu m; the particle size of the common molybdenum oxide is 4-20 mu m.
The parameters of the material boat in the step 2 are as follows: loading the boat: 100-; boat pushing speed: 30-50 min/boat.
In the first stage of the step 2, dry hydrogen is used as hydrogen in the hydrogen reduction, and the hydrogen flow is 2-4m3/h。
In the step 2, the first section of hydrogen is reduced to four temperature areas, specifically: the first temperature zone 380-420 ℃; the second temperature zone is 420-480 ℃; the third temperature zone is 480-550 ℃; the fourth temperature zone is 500-530 ℃.
The parameters of the material boat in the step 3 are as follows: loading the boat: 150-: 40-60 min/boat.
The hydrogen flow rate of the two-stage hydrogen reduction in the step 3 is 2-4m3/h。
In the step 3, the two-stage hydrogen reduction is performed in four temperature areas, specifically: the first temperature zone 780-820 ℃; a second temperature zone 820-; the third temperature zone is 900-920 ℃; the fourth temperature zone 880-.
In step 3, the particle size of the fine molybdenum powder is 0.8-2 μm.
The preparation method of the fine molybdenum powder has the beneficial effects that: adding superfine molybdenum trioxide into common molybdenum trioxide according to the proportion of 0-30% and uniformly mixing to form a raw material, then adopting two-stage hydrogen reduction, wherein the reduction temperature of the molybdenum trioxide is suitable for the first-stage reduction, so that the reduction of large particle size and small particle size in the raw material is met, and molybdenum dioxide with uniform size is obtained, which is favorable for forming regular superfine molybdenum powder; the second stage reduction adopts proper reduction temperature and hydrogen flow rate, thus realizing the production of 0.8-2 μm fine molybdenum powder, not only having simple process and easy batch production, but also greatly reducing the production cost and having good practical value.
Drawings
FIG. 1 is an electron microscope scanning image of molybdenum dioxide obtained after a stage of hydrogen reduction in the preparation method of the present invention;
FIG. 2 is an electron microscope scanning image of the fine molybdenum powder obtained by the preparation method of the present invention.
Detailed Description
The present invention will be described in detail below with reference to the accompanying drawings and specific embodiments.
The invention relates to a preparation method of fine molybdenum powder, which comprises the following steps:
step 1, mixing raw materials
Taking a proper amount of superfine molybdenum oxide and common molybdenum oxide, placing the superfine molybdenum oxide and the common molybdenum oxide in a double-cone mixer, and uniformly mixing to obtain a prefabricated raw material;
the weight percentage of the superfine molybdenum oxide and the common molybdenum oxide is 100 percent, wherein the weight percentage of the superfine molybdenum oxide is 0 to 30 percent, and the balance is the common molybdenum oxide.
The granularity of the superfine molybdenum oxide is 0.1-1 mu m; the particle size of common molybdenum oxide is 4-20 μm.
Step 2, first stage hydrogen reduction
Loading the prefabricated raw materials obtained in the step (1) into a material boat, carrying out first-stage hydrogen reduction, then cooling the material boat to room temperature, and screening the material boat by using a 80-mesh sieve to obtain molybdenum dioxide;
the material boat parameters are as follows: loading the boat: 100-400 g/boat; boat pushing speed: 30-50 min/boat.
The hydrogen gas in the first-stage hydrogen reduction uses dry hydrogen, and the hydrogen flow is 2-4m3/h。
One section of hydrogen is original four warm areas, specifically: the first temperature zone 380-; the second temperature zone is 420-480 ℃; the third temperature zone is 480-550 ℃; the fourth temperature zone is 500-530 ℃.
The first-stage hydrogen reduction adopts the proper reduction temperature of the molybdenum trioxide, meets the requirements of the first-stage hydrogen reduction of large-particle size and small-particle size, and obtains regular uniform flaky molybdenum dioxide as shown in figure 1, thereby being beneficial to the formation of regular ultrafine molybdenum powder.
Step 3, two-stage hydrogen reduction
And (3) loading the molybdenum dioxide obtained in the step (2) into a material boat, carrying out two-stage hydrogen reduction, taking out, filling nitrogen into a cooling area, cooling to room temperature, and screening by using a 200-mesh sieve, wherein fine molybdenum powder with the particle size of 0.8-2 mu m is obtained as shown in figure 2.
The parameters of the material boat are as follows: loading the boat: 150-: 40-60 min/boat.
The hydrogen flow rate of the two-stage hydrogen reduction is 2-4m3/h。
The two-stage hydrogen reduction method comprises the following four temperature regions: the first temperature zone 780-820 ℃; a second temperature zone 820-; the third temperature zone is 900-920 ℃; the fourth temperature zone 880-.
Example 1
Adding the superfine molybdenum oxide with the particle size of 0.5 mu m into the common molybdenum oxide with the particle size of 20 mu m according to the proportion of 10 percent by weight, and uniformly mixing the superfine molybdenum oxide and the common molybdenum oxide by adopting a double-cone mixer; loading into a material boat, performing hydrogen reduction at a temperature of 420 deg.C, 480 deg.C, 520 deg.C, 550 deg.C, and hydrogen flow rate of 3m3Adding 300g of molybdenum trioxide into the material boat per boat, pushing the material boat at a boat pushing speed of 45min per boat, cooling the material boat in a furnace to room temperature after the boat pushing speed is finished, and then sieving the material boat with a 80-mesh sieve; the product of the first stage reduction is regular uniform flaky molybdenum dioxide. Then, two-stage hydrogen reduction is carried out, the process reduction temperature is 780 ℃, 880 ℃, 920 ℃, 900 ℃, the loading quantity is 200 g/boat, and the hydrogen flow is 4m3And h, pushing the boat for 40 min/boat to realize two-stage reduction, placing the boat in a cooling area after the two-stage reduction is finished, filling nitrogen for cooling, sieving by a 200-mesh sieve, detecting and packaging.
The Fisher size of the molybdenum powder was measured to be 1.6. mu.m.
Example 2
Adding the superfine molybdenum oxide with the particle size of 0.5 mu m into common molybdenum oxide with the particle size of 4 mu m according to the proportion of 30 percent by weight, and uniformly mixing the mixture by adopting a double-cone mixer; loading into a material boat, performing hydrogen reduction at 400 deg.C, 450 deg.C, 480 deg.C, 520 deg.C, and hydrogen flow rate of 3m3And h, adding 200g of molybdenum trioxide into the material boat, pushing the material boat at a boat pushing speed of 40 min/boat, placing the material boat into a furnace after the boat pushing speed is finished, cooling the material boat to room temperature, sieving the material boat by using a 80-mesh sieve, and obtaining a first-stage reduction product which is regular uniform sheet-shaped molybdenum dioxide. Then, two-stage reduction is carried out, the process reduction temperature is 780 ℃, 830 ℃, 900 ℃, 880 ℃, the boat loading amount is 200 g/boat, and the hydrogen flow is 2m3And h, pushing the boat for 40 min/boat to realize two-stage reduction, placing the boat in a cooling area after the two-stage reduction is finished, filling nitrogen for cooling, sieving by a 200-mesh sieve, detecting and packaging.
The Fisher size of the molybdenum powder was measured to be 1.2 μm.
Example 3
Adding the superfine molybdenum oxide with the particle size of 0.2 mu m into the common molybdenum oxide with the particle size of 20 mu m according to the proportion of 30 percent by weight, and uniformly mixing the superfine molybdenum oxide and the common molybdenum oxide by adopting a double-cone mixer; loading into a material boat, performing a first-stage hydrogen reduction, and performing reduction in four temperature regions at 380 deg.C, 430 deg.C, 550 deg.C, 500 deg.C and hydrogen flow rate of 3m3And h, adding 100g of molybdenum trioxide into the material boat, pushing the material boat at a boat pushing speed of 30 min/boat, placing the material boat into a furnace after the boat pushing speed is finished, cooling to room temperature, and then sieving the material boat by using a 80-mesh sieve, wherein the first-stage reduction product is regular uniform flaky molybdenum dioxide. Then, two-stage reduction is carried out, the process reduction temperature is 820 ℃, 880 ℃, 920 ℃, 900 ℃, the loading amount of the boat is 150 g/boat, and the hydrogen flow is 4m3And h, pushing the boat for 30 min/boat to realize two-stage reduction, placing the boat in a cooling area after the two-stage reduction is finished, filling nitrogen for cooling, sieving by a 200-mesh sieve, detecting and packaging.
The Fisher size of the molybdenum powder was measured to be 0.9. mu.m.
Example 4
Adding the superfine molybdenum oxide with the particle size of 1.0 mu m into common molybdenum oxide with the particle size of 4 mu m according to the proportion of 20 percent by weight, and uniformly mixing the superfine molybdenum oxide with the common molybdenum oxide by adopting a double-cone mixer; loading into a material boat, performing hydrogen reduction at 400 deg.C, 460 deg.C, 500 deg.C, 530 deg.C, and hydrogen flow rate of 2m3And h, adding 400g of molybdenum trioxide into the material boat, pushing the material boat at a boat pushing speed of 40 min/boat, placing the material boat into a furnace after the boat pushing speed is finished, cooling to room temperature, and then sieving the material boat with an 80-mesh sieve to obtain a first-stage reduction product which is regular uniform flaky molybdenum dioxide. Then, two-stage reduction is carried out, the process reduction temperature is 820 ℃, 880 ℃, 900 ℃, 880 ℃, the boat loading amount is 400 g/boat, and the hydrogen flow is 4m3And h, the boat pushing speed is 50 min/boat to realize two-stage reduction, after that, the material boat is placed in a cooling area to be filled with nitrogen for cooling, and is sieved by a 200-mesh sieve, detected and packaged.
The Fisher size of the molybdenum powder was measured to be 2.0. mu.m.
Example 5
Adding superfine molybdenum oxide with the particle size of 0.8 mu m into common molybdenum oxide with the weight percentage of 20 percent, uniformly mixing the superfine molybdenum oxide and the common molybdenum oxide by a double-cone mixer, loading the mixture into a material boat, carrying out first-stage hydrogen reduction, and dividing into four partsReducing in each temperature zone at 420 deg.C, 470 deg.C, 480 deg.C, 530 deg.C, and hydrogen flow rate of 4m3And h, adding 400g of molybdenum trioxide into the material boat, pushing the material boat at a boat pushing speed of 40 min/boat, placing the material boat into a furnace after the boat pushing speed is finished, cooling the material boat to room temperature, and then sieving the material boat by using a 80-mesh sieve, wherein the first-stage reduction product is regular uniform flaky molybdenum dioxide. Then, two-stage reduction is carried out, the process reduction temperature is 780 ℃, 820 ℃, 900 ℃, 880 ℃, the boat loading amount is 200 g/boat, and the hydrogen flow is 4m3And h, pushing the boat for 40 min/boat to realize two-stage reduction, placing the boat in a cooling area after the two-stage reduction is finished, filling nitrogen for cooling, sieving by a 200-mesh sieve, detecting and packaging.
The Fisher size of the molybdenum powder was measured to be 1.8. mu.m.
From the above examples, the invention adopts two-stage hydrogen reduction, the reduction temperature of the first stage meets the reduction of large particle size and small particle size in the raw materials, and molybdenum dioxide with uniform size is obtained, which is beneficial to the formation of regular ultrafine molybdenum powder; the second stage realizes the production of 0.8-2 μm fine molybdenum powder, and has simple process, easy mass production and greatly reduced production cost.
Claims (5)
1. A method for preparing fine molybdenum powder is characterized by comprising the following steps:
step 1, mixing raw materials
Taking a proper amount of superfine molybdenum oxide and common molybdenum oxide, placing the superfine molybdenum oxide and the common molybdenum oxide in a double-cone mixer, and uniformly mixing to obtain a prefabricated raw material;
in the step 1, the weight ratio of the superfine molybdenum oxide to the common molybdenum oxide is (0-30%): (70-100%);
step 2, first stage hydrogen reduction
Loading the prefabricated raw materials obtained in the step (1) into a material boat, carrying out first-stage hydrogen reduction, then cooling the material boat to room temperature, and screening to obtain molybdenum dioxide;
the material boat parameters in the step 2 are as follows: loading the boat: 100-; boat pushing speed: 30-50 min/boat;
the step 2 is that the first section of hydrogen reduces the original four temperature areas, and specifically comprises the following steps: the first temperature zone 380-; the second temperature zone is 420-480 ℃; the third temperature zone is 480-550 ℃; the fourth temperature zone is 500-530 ℃;
step 3, two-stage hydrogen reduction
Loading the molybdenum dioxide obtained in the step (2) into a material boat, carrying out two-stage hydrogen reduction, taking out, filling nitrogen into a cooling area, cooling to room temperature, and screening to obtain fine molybdenum powder;
the parameters of the material boat in the step 3 are as follows: loading the boat: 150-: 40-60 min/boat;
the two-stage hydrogen reduction in the step 3 comprises four temperature zones: the first temperature zone is 780-820 ℃; a second temperature zone 820-; the third temperature zone is 900-920 ℃; the fourth temperature zone 880-920 ℃.
2. The method of claim 1, wherein the ultra-fine molybdenum oxide has a particle size of 0.1 to 1 μm; the particle size of the common molybdenum oxide is 4-20 mu m.
3. The method of claim 1, wherein dry hydrogen is used as hydrogen in the first stage hydrogen reduction in step 2, and the hydrogen flow rate is 2-4m3/h。
4. The method for preparing fine molybdenum powder as claimed in claim 1, wherein the hydrogen flow rate in the two-stage hydrogen reduction in the step 3 is 2 to 4m3/h。
5. The method of claim 1, wherein the fine molybdenum powder in step 3 has a particle size of 0.8 to 2 μm.
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| CN111069620A (en) * | 2020-01-15 | 2020-04-28 | 金堆城钼业股份有限公司 | Preparation method of uniform approximately spherical molybdenum powder |
| CN112077333B (en) * | 2020-09-18 | 2022-09-02 | 成都新世佳材料科技有限公司 | Method for preparing metal powder and energy-saving push boat type hydrogen reduction furnace for preparing metal powder |
| CN114411006A (en) * | 2021-12-24 | 2022-04-29 | 海特信科新材料科技有限公司 | Production process of high-homogeneity molybdenum-copper alloy with low molybdenum content |
| CN114657404B (en) * | 2022-03-24 | 2022-10-21 | 金堆城钼业股份有限公司 | High-density ultrafine-grained molybdenum-lanthanum alloy and preparation method thereof |
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