CN111646511A - Method for producing melt-blown chromium oxide by vacuum sintering - Google Patents
Method for producing melt-blown chromium oxide by vacuum sintering Download PDFInfo
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- CN111646511A CN111646511A CN202010547814.2A CN202010547814A CN111646511A CN 111646511 A CN111646511 A CN 111646511A CN 202010547814 A CN202010547814 A CN 202010547814A CN 111646511 A CN111646511 A CN 111646511A
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- chromium oxide
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- blown
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G37/00—Compounds of chromium
- C01G37/02—Oxides or hydrates thereof
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- F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
- F27—FURNACES; KILNS; OVENS; RETORTS
- F27D—DETAILS OR ACCESSORIES OF FURNACES, KILNS, OVENS, OR RETORTS, IN SO FAR AS THEY ARE OF KINDS OCCURRING IN MORE THAN ONE KIND OF FURNACE
- F27D17/00—Arrangements for using waste heat; Arrangements for using, or disposing of, waste gases
- F27D17/008—Arrangements for using waste heat; Arrangements for using, or disposing of, waste gases cleaning gases
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- F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
- F27—FURNACES; KILNS; OVENS; RETORTS
- F27D—DETAILS OR ACCESSORIES OF FURNACES, KILNS, OVENS, OR RETORTS, IN SO FAR AS THEY ARE OF KINDS OCCURRING IN MORE THAN ONE KIND OF FURNACE
- F27D7/00—Forming, maintaining, or circulating atmospheres in heating chambers
- F27D7/06—Forming or maintaining special atmospheres or vacuum within heating chambers
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- F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
- F27—FURNACES; KILNS; OVENS; RETORTS
- F27D—DETAILS OR ACCESSORIES OF FURNACES, KILNS, OVENS, OR RETORTS, IN SO FAR AS THEY ARE OF KINDS OCCURRING IN MORE THAN ONE KIND OF FURNACE
- F27D7/00—Forming, maintaining, or circulating atmospheres in heating chambers
- F27D7/06—Forming or maintaining special atmospheres or vacuum within heating chambers
- F27D2007/066—Vacuum
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- F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
- F27—FURNACES; KILNS; OVENS; RETORTS
- F27M—INDEXING SCHEME RELATING TO ASPECTS OF THE CHARGES OR FURNACES, KILNS, OVENS OR RETORTS
- F27M2003/00—Type of treatment of the charge
- F27M2003/04—Sintering
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P10/00—Technologies related to metal processing
- Y02P10/25—Process efficiency
Abstract
The invention belongs to the field of new materials, and particularly relates to a method for producing melt-blown chromium oxide by vacuum sintering, which comprises the following steps: homogenizing 325-mesh chromium oxide fine powder and an organic cementing material, adding purified water for humidification, briquetting by a hydraulic briquetting machine, drying at a low temperature of 80 ℃, and presintering and curing at a temperature of 500 ℃; step two, placing the presintered and solidified briquettes in a vacuum sintering furnace, gradually heating to 1300-1450 ℃, controlling the vacuum degree within 50Pa, keeping the temperature for 30-60 hours, cooling to 1000 ℃ naturally, filling argon into the vacuum sintering furnace to reach normal pressure or micro positive pressure, accelerating the cooling speed, opening a furnace door, cooling to room temperature, and discharging; and step three, carrying out coarse crushing, fine crushing, shaping and grading on the cooled agglomerated materials to obtain the melt-blown chromium oxide with different particle sizes. The invention can effectively solve the problem of low yield of finished products. Effectively solves the problem that the common kiln is difficult to realize at the temperature of more than 1650 ℃ for melting and spraying the chromium oxide puzzling the sintering of the chromium oxide at the normal temperature.
Description
Technical Field
The invention belongs to the field of new materials, and particularly relates to a method for producing melt-blown chromium oxide by vacuum sintering.
Background
The technology for producing the melt-blown chromium oxide has the following technical problems:
problem 1: the fine powder of the chromium sesquioxide is not compact in molding in the production process of the melt-blown chromium oxide sintering method, and the yield of finished products is too low;
problem 2: the preparation of melt-blown chromium oxide by sintering chromium oxide at normal temperature at a temperature of over 1650 ℃ is difficult to realize in a common kiln;
problem 3: the vacuum sintering furnace used for sintering the tantalum-niobium alloy has the performance of bearing high temperature and high pressure, and the furnace of the sintering furnace needs to be vacuumized before the sintering furnace is started. The vacuum-pumping system of the vacuum sintering furnace generally uses a vacuum-pumping pump to directly pump out air, and no filter device is arranged before the air enters the vacuum pump, so that impurities such as flying dust are easily brought into the vacuum pump to damage the vacuum pump. The filter screen is added into the vacuum-pumping pipeline of the vacuum sintering furnace, so that high-temperature heat in the furnace is easily transferred to the filter screen along the vacuum-pumping pipeline during sintering, the filter screen is damaged, and heat loss is also caused.
Disclosure of Invention
In order to solve the problems in the prior art, the invention provides a method for producing melt-blown chromium oxide by vacuum sintering.
The technical scheme adopted by the invention for solving the technical problems is as follows:
a method for producing melt-blown chromium oxide by vacuum sintering comprises the following steps:
homogenizing chromium oxide fine powder and an organic cementing material, adding purified water for humidification, briquetting by a hydraulic briquetting machine, drying at low temperature, pre-sintering and curing;
step two, placing the presintered and solidified briquettes in a vacuum sintering furnace, gradually heating, keeping the temperature in vacuum, naturally cooling, filling argon into the vacuum sintering furnace, opening a furnace door, cooling to room temperature, and discharging;
and step three, carrying out coarse crushing, fine crushing, shaping and grading on the cooled agglomerated materials to obtain the melt-blown chromium oxide with different particle sizes.
Compared with the prior art, the invention has the advantages that:
the method has the advantages that: the method can effectively solve the problems of non-compact formation of the chromium oxide fine powder and low finished product yield in the production process of the melt-blown chromium oxide sintering method.
The method has the advantages that: the method effectively solves the problem that the ordinary kiln is difficult to realize at the temperature of over 1650 ℃ for melt-blown chromium oxide prepared by sintering the chromium oxide at normal temperature, and the method is a pure physical sintering process without participation of chemical reaction.
The method has the advantages that: the method has the advantages of replacing the traditional high-pollution electric melting method, titanium dioxide sintering method, thermit method and chemical mixed sintering method, and can be widely applied.
The advantages are that: according to the invention, the opening and closing pipe joints are arranged, so that the passage between the vacuum sintering furnace and the vacuum pumping pipe body is conveniently closed by opening and closing the pipe joints, high-temperature heat in the furnace is not easy to enter a pipeline of the vacuum pumping pipe body, a filter screen in the filter pipe joints is not easy to be damaged by high temperature, and the service life is prolonged.
The advantages are that: the valve plate is provided with the 0-90-degree rotating device, the valve plate, the valve rod and the opening and closing pipe section form a butterfly valve type structure, and the right end of the valve rod is in transmission connection with the motor through the first bevel gear and the second bevel gear, so that the valve plate can be opened and closed conveniently.
The method has the advantages that: according to the invention, the cross section of the valve plate is circular, the longitudinal section of the valve plate is elliptical, and the exterior of the valve plate is wrapped with the coating layer made of high-temperature-resistant heat-insulating cotton, so that the heat-insulating effect is improved.
The method has the advantages that: the invention has the advantages of simple structure, difficult damage to the filter screen, long service life, convenient opening and closing and good heat insulation effect.
Drawings
FIG. 1 is a schematic view of a vacuum sintering furnace according to the present invention;
FIG. 2 is a schematic view of a partial structure of a vacuum sintering furnace according to the present invention;
FIG. 3 is a schematic cross-sectional structure diagram of a valve plate of the vacuum sintering furnace of the present invention.
In the figure: the vacuum tube comprises a vacuum-pumping tube body 1, a vacuum sintering furnace 2, a vacuum pump 3, a filtering tube joint 4, an opening-closing tube joint 5, a valve plate 6, a valve rod 7, a first bevel gear 8, a second bevel gear 9, a motor 10, a motor mounting seat 11 and a coating layer 601.
Detailed Description
Exemplary embodiments of the present disclosure will be described in more detail below with reference to the accompanying drawings, in order that the present disclosure may be more fully understood and fully conveyed to those skilled in the art. While the exemplary embodiments of the present disclosure are shown in the drawings, it should be understood that the invention is not limited to the embodiments set forth herein.
A method for producing melt-blown chromium oxide by vacuum sintering comprises the following steps:
homogenizing 325-mesh chromium oxide fine powder and an organic cementing material, adding purified water for humidification, briquetting by a hydraulic briquetting machine, drying at a low temperature of 80 ℃, and presintering and curing at a temperature of 500 ℃;
step two, placing the presintering solidified pressing block in a vacuum sintering furnace, gradually heating to 1300-1450 ℃, controlling the vacuum degree within 50Pa, keeping the temperature for 30-60 hours, then filling argon in the vacuum sintering furnace after the natural temperature is reduced to 1000 ℃, achieving normal pressure or micro positive pressure, accelerating the cooling speed, opening a furnace door, cooling to room temperature, and then discharging;
and step three, carrying out coarse crushing, fine crushing, shaping and grading on the cooled agglomerated materials to obtain the melt-blown chromium oxide with different particle sizes.
Example 1
A method for preparing melt-blown chromium oxide by vacuum sintering comprises the following steps:
step one, the chromium oxide is named as chromium oxide and chromium oxide green, wherein, Cr is2O3The content is more than 99.5 percent, and the content of impurities such as iron, silicon, aluminum and the like is less than 0.03 percent. Homogenizing the 325-mesh chromium oxide fine powder and the organic cementing material, adding purified water for humidification, briquetting by a hydraulic briquetting machine, drying at a low temperature of 80 ℃, and presintering and curing at a temperature of 500 ℃. Wherein the median diameter D50 of the 325-mesh chromium oxide fine powder is preferably 5-7 μm; the organic cementing material is one or more of self-hardening furan resin, phenolic resin or starch; preferably selecting self-hardening furan resin, and the adding amount is 0.5-1.5% of the total material; the purified water is humidified, the pressure of the press is mainly related, and if a 250-ton oil press is selected, the water content is preferably 7-9%; the low-temperature drying at the temperature of 80 ℃ adopts forced circulation drying of hot air and temperature control of the hot airPreparing at 80 ℃; the presintering and curing at the temperature of 500 ℃ is mainly related to the selected organic cementing material, and if furan resin is selected, the presintering at the temperature of 500 ℃ can achieve the optimal hardness index.
And step two, placing the presintered and solidified briquettes in a vacuum sintering furnace, gradually heating to 1300-1450 ℃, controlling the vacuum degree within 50Pa, continuously preserving heat for 30-60 hours, naturally cooling to 300 ℃, opening a furnace door, cooling to room temperature, and discharging. The sintered, solidified and molded pressing blocks are placed in a vacuum sintering furnace, and a gap of 5-10mm is reserved when the pressing blocks are placed, so that the uniform thorough burning of the temperature is ensured; gradually heating to 1300-1450 ℃, controlling the vacuum degree within 50Pa, determining the end point temperature of 1300-1450 ℃ according to the particle size of the required product, and if a product with large particle size is required, selecting high end point temperature and keeping the vacuum degree within 50 Pa; the continuous heat preservation is carried out for 30-60h, the proper heat preservation time is selected mainly according to the particle size of the finished product and the selected end point temperature, the same effect is achieved when the temperature is long and the temperature is short, and the effect of low-temperature long-time particle forming is superior to that of high-temperature short-time particle forming.
And after the heat preservation time reaches the set requirement, the natural temperature is reduced to 1000 ℃, argon is filled in the furnace, the normal pressure or micro-positive pressure is reached, the cooling speed is accelerated, and the material can be discharged when the temperature is reduced to 300 ℃ and the furnace door can be opened to naturally cool to below 80 ℃.
And step three, carrying out coarse crushing, fine crushing, shaping and grading on the cooled agglomerated materials to obtain melt-blown chromium oxide products with different particle sizes of 10-32 microns, 16-45 microns and the like. The products with different grain size grades are mainly obtained by adjusting a sintering process. The special stainless steel equipment is adopted for the breakage-fine crushing-shaping-grading equipment, so that the nodulizing rate of the product reaches over 75 percent.
Example 2
The vacuum sintering furnace comprises a vacuum pumping pipe body 1, a vacuum sintering furnace 2, a vacuum pump 3, a filtering pipe joint 4, an opening and closing pipe joint 5, a valve plate 6, a valve rod 7, a first bevel gear 8, a second bevel gear 9, a motor 10, a motor mounting seat 11 and a coating layer 601; the front end of the vacuumizing tube body 1 is connected with a hearth of the vacuum sintering furnace 2, and the rear end of the vacuumizing tube body 1 is connected with a vacuum pump 3; a filter pipe joint 4 and an opening and closing pipe joint 5 are arranged on a pipeline of the vacuum tube body 1, and the filter pipe joint 4 and the opening and closing pipe joint 5 are fixedly connected with the vacuum tube body 1 through flanges; the opening and closing pipe joint 5 is arranged at one end of the vacuum-pumping pipe body 1 close to the vacuum sintering furnace 2, and a valve plate 6 is embedded in the inner side of the opening and closing pipe joint 5; the valve plate 6 is in clearance fit with the opening and closing pipe joint 5, and a coating layer 601 is wrapped outside the valve plate 6; the right side key of the valve plate 6 is connected with a valve rod 7, the right end of the valve rod 7 penetrates through the pipe wall of the opening and closing pipe joint 5 to the outside, and the valve rod 7 is rotatably connected with the opening and closing pipe joint 5; the right end key of the valve rod 7 is connected with a first bevel gear 8, and a second bevel gear 9 is meshed above the first bevel gear 8; the second bevel gear 9 is connected on an output shaft of the motor 10 in a key mode, and the motor 10 is fixed on the motor mounting seat 11 through bolts; the motor mounting seat 11 is welded on the outer pipe wall of the vacuum tube body 1.
Referring to fig. 1, a filter screen is embedded in the filter pipe section 4.
Referring to fig. 2, the valve plate 6 is provided with a 0-90 degree rotating device, the valve plate 6, the valve rod 7 and the opening and closing pipe joint 5 form a butterfly valve type structure, the valve rod 7 is rotated by ninety degrees, so that the axial lead of the valve plate 6 is perpendicular to the axial lead of the opening and closing pipe joint 5, the vacuum pumping pipe body 1 is communicated with the vacuum sintering furnace 2, the valve rod 7 is rotated by ninety degrees in the reverse direction, the axial lead of the valve plate 6 is collinear with the axial lead of the opening and closing pipe joint 5, and the passage between the vacuum pumping pipe body 1 and the vacuum sintering furnace 2 is cut off.
Referring to fig. 2, the coating layer 601 is made of high temperature resistant heat insulation cotton, and the high temperature resistant heat insulation cotton is made by molding silicide fibers in a non-woven mold, has the characteristics of stability, high and low temperature resistance, heat insulation, and easy assembly and processing.
Referring to fig. 3, the opening and closing pipe section 5 is in a circular pipe shape, and referring to fig. 2, circular mounting flanges are welded to both ends of the opening and closing pipe section 5.
Referring to fig. 3, the valve plate 6 has a circular cross-section, and referring to fig. 2, the valve plate 6 has an elliptical longitudinal cross-section.
The vacuum sintering furnace comprises the following specific implementation steps: the during operation of motor 10, its output shaft drives second bevel gear 9 and rotates, second bevel gear 9 drives first bevel gear 8 and rotates, first bevel gear 8 drives valve rod 7 and rotates, after valve rod 7 rotates ninety degrees, the axial lead of valve plate 6 is perpendicular with the axial lead of opening and close tube coupling 5, evacuation pipe body 1 and vacuum sintering stove 2 intercommunication, the evacuation operation can be carried out this moment, the back is accomplished in the evacuation, reverse rotation valve rod 7 ninety degrees, make the axial lead of valve plate 6 and the axial lead collineation of opening and close tube coupling 5, cut the route of evacuation pipe body 1 and vacuum sintering stove 2, the difficult vacuum tube body 1 that gets into of high temperature heat in the vacuum sintering stove 2 this moment, make the filter screen in the filter tube coupling 4 difficult damaged by high temperature.
Claims (9)
1. A method for producing melt-blown chromium oxide by vacuum sintering is characterized by comprising the following steps:
homogenizing chromium oxide fine powder and an organic cementing material, adding purified water for humidification, briquetting by a hydraulic briquetting machine, drying at low temperature, pre-sintering and curing;
step two, placing the presintered and solidified briquettes in a vacuum sintering furnace, gradually heating, keeping the temperature in vacuum, naturally cooling, filling argon into the vacuum sintering furnace, opening a furnace door, cooling to room temperature, and discharging;
and step three, carrying out coarse crushing, fine crushing, shaping and grading on the cooled agglomerated materials to obtain the melt-blown chromium oxide with different particle sizes.
2. The method for producing melt-blown chromium oxide by vacuum sintering according to claim 1, comprising the steps of:
homogenizing 325-mesh chromium oxide fine powder and an organic cementing material, adding purified water for humidification, briquetting by a hydraulic briquetting machine, drying at a low temperature of 80 ℃, and presintering and curing at a temperature of 500 ℃;
step two, placing the presintering solidified pressing block in a vacuum sintering furnace, gradually heating to 1300-1450 ℃, controlling the vacuum degree within 50Pa, keeping the temperature for 30-60 hours, then filling argon in the vacuum sintering furnace after the natural temperature is reduced to 1000 ℃, achieving normal pressure or micro positive pressure, accelerating the cooling speed, opening a furnace door, cooling to room temperature, and then discharging;
and step three, carrying out coarse crushing, fine crushing, shaping and grading on the cooled agglomerated materials to obtain the melt-blown chromium oxide with different particle sizes.
3. The method for producing melt-blown chromium oxide by vacuum sintering according to claim 1 or 2, wherein in the first step, the median diameter D50 of the 325-mesh chromium oxide fine powder is 5-7 μm; the organic cementing material is one or more of self-hardening furan resin, phenolic resin or starch; the adding amount of the organic cementing material is 0.5-1.5% of the total material; drying at low temperature of 80 ℃ by adopting forced circulation of hot air.
4. The method for producing melt-blown chromium oxide by vacuum sintering according to claim 1 or 2, wherein in step one, the content of chromium sesquioxide is more than 99.5%, and the content of impurities is less than 0.03%.
5. The method for producing the melt-blown chromium oxide by vacuum sintering according to claim 1 or 2, wherein in the second step, the sintered, solidified and formed compact is placed in a vacuum sintering furnace, and a gap of 5-10mm is reserved when the compact is placed.
6. The process of claim 1 or 2, wherein in step three, the particle size of the melt-blown chromium oxide is 10-32 μm or 16-45 μm.
7. The method for producing the melt-blown chromium oxide by vacuum sintering according to claim 1 or 2, wherein the equipment for rough breaking, fine breaking, shaping and grading adopts stainless steel special equipment, and the nodularity of the melt-blown chromium oxide is more than 75 percent.
8. The method for producing the melt-blown chromium oxide by vacuum sintering according to claim 1 or 2, wherein in the vacuum sintering furnace, the front end of the vacuum tube body (1) is connected with the hearth of the vacuum sintering furnace (2), and the rear end of the vacuum tube body (1) is connected with the vacuum pump (3); a filter pipe joint (4) and an opening and closing pipe joint (5) are arranged on a pipeline of the vacuum pipe body (1), and the filter pipe joint (4) and the opening and closing pipe joint (5) are fixedly connected with the vacuum pipe body (1) through flanges; the opening and closing pipe joint (5) is arranged at one end of the vacuumizing pipe body (1) close to the vacuum sintering furnace (2), and a valve plate (6) is embedded in the inner side of the opening and closing pipe joint (5); the valve plate (6) is in clearance fit with the opening and closing pipe joint (5), and a coating layer (601) is wrapped outside the valve plate (6); the right side key of the valve plate (6) is connected with a valve rod (7), the right end of the valve rod (7) penetrates through the pipe wall of the opening and closing pipe joint (5) to the outside, and the valve rod (7) is rotatably connected with the opening and closing pipe joint (5); the right end key of the valve rod (7) is connected with a first bevel gear (8), and a second bevel gear (9) is meshed above the first bevel gear (8); the second bevel gear (9) is connected to an output shaft of the motor (10) in a key mode, and the motor (10) is fixed on the motor mounting seat (11) through bolts; the motor mounting seat (11) is welded on the outer pipe wall of the vacuum pipe body (1).
9. The method for producing the melt-blown chromium oxide by vacuum sintering according to claim 8, wherein the opening and closing pipe joint (5) is in a circular pipe shape, and mounting flanges in a circular shape are welded at two ends of the opening and closing pipe joint (5); the cross section of the valve plate (6) is circular, and the longitudinal section of the valve plate (6) is oval; the valve plate (6) is provided with a 0-90-degree rotating device, and the valve plate (6), the valve rod (7) and the opening and closing pipe section (5) form a butterfly valve type structure; the coating layer (601) is made of high-temperature-resistant heat-preservation heat-insulation cotton; a filter screen is embedded in the filter pipe joint (4).
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|---|---|---|---|---|
| JPS62167219A (en) * | 1986-01-20 | 1987-07-23 | Awamura Kinzoku Kogyo Kk | Production of thermal spraying powder of sintered chromium oxide |
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| CN109622979A (en) * | 2019-01-11 | 2019-04-16 | 湘潭大学 | A kind of preparation method of pre-alloyed high-entropy alloy porous material |
| CN210739396U (en) * | 2019-07-22 | 2020-06-12 | 温州福莱特阀门有限公司 | Manual hard seal butterfly valve convenient to adjust |
-
2020
- 2020-06-16 CN CN202010547814.2A patent/CN111646511A/en active Pending
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|---|---|---|---|---|
| JPS62167219A (en) * | 1986-01-20 | 1987-07-23 | Awamura Kinzoku Kogyo Kk | Production of thermal spraying powder of sintered chromium oxide |
| CN203881112U (en) * | 2014-06-16 | 2014-10-15 | 四川盛马粉末冶金科技有限公司 | Metal powder vacuum sintering furnace |
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| CN208171034U (en) * | 2018-02-28 | 2018-11-30 | 炎陵县今成钽铌有限公司 | A kind of vacuum lead of vacuum sintering furnace |
| CN108264089A (en) * | 2018-04-03 | 2018-07-10 | 苏州化联高新陶瓷材料有限公司 | A kind of production technology of sintering process chromium trioxide powder used for hot spraying |
| CN109622979A (en) * | 2019-01-11 | 2019-04-16 | 湘潭大学 | A kind of preparation method of pre-alloyed high-entropy alloy porous material |
| CN210739396U (en) * | 2019-07-22 | 2020-06-12 | 温州福莱特阀门有限公司 | Manual hard seal butterfly valve convenient to adjust |
Non-Patent Citations (1)
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