CN111348668A - Preparation method of aluminum oxide for heat-conducting filler - Google Patents
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- C01F7/00—Compounds of aluminium
- C01F7/02—Aluminium oxide; Aluminium hydroxide; Aluminates
- C01F7/46—Purification of aluminium oxide, aluminium hydroxide or aluminates
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- C01F7/00—Compounds of aluminium
- C01F7/02—Aluminium oxide; Aluminium hydroxide; Aluminates
- C01F7/021—After-treatment of oxides or hydroxides
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- C01F7/00—Compounds of aluminium
- C01F7/02—Aluminium oxide; Aluminium hydroxide; Aluminates
- C01F7/021—After-treatment of oxides or hydroxides
- C01F7/023—Grinding, deagglomeration or disintegration
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- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09C—TREATMENT OF INORGANIC MATERIALS, OTHER THAN FIBROUS FILLERS, TO ENHANCE THEIR PIGMENTING OR FILLING PROPERTIES ; PREPARATION OF CARBON BLACK ; PREPARATION OF INORGANIC MATERIALS WHICH ARE NO SINGLE CHEMICAL COMPOUNDS AND WHICH ARE MAINLY USED AS PIGMENTS OR FILLERS
- C09C1/00—Treatment of specific inorganic materials other than fibrous fillers; Preparation of carbon black
- C09C1/40—Compounds of aluminium
- C09C1/407—Aluminium oxides or hydroxides
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- C09C3/00—Treatment in general of inorganic materials, other than fibrous fillers, to enhance their pigmenting or filling properties
- C09C3/006—Combinations of treatments provided for in groups C09C3/04 - C09C3/12
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- C09C—TREATMENT OF INORGANIC MATERIALS, OTHER THAN FIBROUS FILLERS, TO ENHANCE THEIR PIGMENTING OR FILLING PROPERTIES ; PREPARATION OF CARBON BLACK ; PREPARATION OF INORGANIC MATERIALS WHICH ARE NO SINGLE CHEMICAL COMPOUNDS AND WHICH ARE MAINLY USED AS PIGMENTS OR FILLERS
- C09C3/00—Treatment in general of inorganic materials, other than fibrous fillers, to enhance their pigmenting or filling properties
- C09C3/04—Physical treatment, e.g. grinding, treatment with ultrasonic vibrations
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- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09C—TREATMENT OF INORGANIC MATERIALS, OTHER THAN FIBROUS FILLERS, TO ENHANCE THEIR PIGMENTING OR FILLING PROPERTIES ; PREPARATION OF CARBON BLACK ; PREPARATION OF INORGANIC MATERIALS WHICH ARE NO SINGLE CHEMICAL COMPOUNDS AND WHICH ARE MAINLY USED AS PIGMENTS OR FILLERS
- C09C3/00—Treatment in general of inorganic materials, other than fibrous fillers, to enhance their pigmenting or filling properties
- C09C3/04—Physical treatment, e.g. grinding, treatment with ultrasonic vibrations
- C09C3/043—Drying, calcination
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- C09C—TREATMENT OF INORGANIC MATERIALS, OTHER THAN FIBROUS FILLERS, TO ENHANCE THEIR PIGMENTING OR FILLING PROPERTIES ; PREPARATION OF CARBON BLACK ; PREPARATION OF INORGANIC MATERIALS WHICH ARE NO SINGLE CHEMICAL COMPOUNDS AND WHICH ARE MAINLY USED AS PIGMENTS OR FILLERS
- C09C3/00—Treatment in general of inorganic materials, other than fibrous fillers, to enhance their pigmenting or filling properties
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- C09K5/00—Heat-transfer, heat-exchange or heat-storage materials, e.g. refrigerants; Materials for the production of heat or cold by chemical reactions other than by combustion
- C09K5/08—Materials not undergoing a change of physical state when used
- C09K5/14—Solid materials, e.g. powdery or granular
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- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/60—Particles characterised by their size
- C01P2004/61—Micrometer sized, i.e. from 1-100 micrometer
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- 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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Abstract
The invention discloses a preparation method of alumina for a heat-conducting filler, which uses a byproduct dust collection powder produced in the process of producing and calcining alumina in a rotary kiln, wherein the content of alumina in the dust collection powder is 95-97%, and the laser granularity is D10: 10-15 μm, D50: 20-30 μm, D90: 40-50 um; adding pure water and a certain amount of inorganic acid into the dust collecting powder to prepare slurry with the concentration of 200-70 ℃ and the pH of 4-7, washing at 40-70 ℃, then carrying out filter pressing to obtain a filter cake, calcining at the temperature of 1200-1300 ℃, and crushing and screening by adopting a plastic roller pair or a polyurethane roller pair to obtain the raw material of alumina or spherical alumina which can be used as a heat-conducting filler. The invention can realize the comprehensive utilization of dust collection powder, prepare the heat-conducting alumina filler with typical particle size distribution characteristics, and has the advantages of low cost and excellent performance.
Description
Technical Field
The invention belongs to the field of inorganic non-metallic materials, and particularly relates to a comprehensive utilization technology of a byproduct, namely alumina dust collection powder.
Background
The heat conduction material is widely applied to various fields of national economy and national defense industry, and with the rapid development of the 5G era and the field of new energy, higher requirements are also put forward on the heat conduction material. Along with the high integration of electronic components, in order to ensure the reliability of the operation of components, the excellent heat conduction material with high heat conduction performance and high stability is required to replace the common material used in the occasion, so that the heat generated by the heating element can be rapidly, timely and effectively transferred to the heat dissipation equipment, and the normal operation of the electronic equipment is ensured. At present, the market demand of heat conduction materials is more and more large, the mainstream heat conduction filler is mainly alumina, and the heat conduction materials are prepared by compounding spherical, quasi-spherical and angular heat conduction alumina with different particle sizes.
Fraction D50 for current thermal conductive materials: the alumina which is 20-30 microns and is a narrowly distributed heat-conducting filler is mainly spherical and spheroidal alumina, but is produced by grading other granular spherical or spheroidal aluminas, so that the problems of high cost, high impurity and electric conductivity, large abrasion on equipment of a melting furnace and the like exist; the angular alumina mainly adopts corundum, and has the defects of high impurity content and high conductivity, so that the wide application of the alumina with the particle size in the heat conduction material industry is limited to a certain extent.
Disclosure of Invention
Aiming at the defects of the prior art, the invention provides a preparation method of alumina for a heat-conducting filler.
The invention is realized by the following technical scheme.
The preparation method of the alumina for the heat-conducting filler is characterized in that the used raw materials are dust collecting powder which is a byproduct in the process of producing and calcining the alumina by a rotary kiln, wherein the content of the alumina in the dust collecting powder is 95-97%, and the laser granularity is D10: 10-15 μm, D50: 20-30 μm, D90: 40-50 um; adding pure water and a certain amount of inorganic acid into dust collection powder, preparing into slurry with the concentration of 200-70 ℃ and the pH of 4-7, washing at 40-70 ℃, then carrying out filter pressing to obtain a filter cake, calcining at the temperature of 1200-1300 ℃, crushing and screening by using a plastic roller pair or a polyurethane roller pair, and crushing equipment with a grinding function such as a ball mill cannot be adopted to keep the particle morphology and the particle size distribution of the powder from being damaged, and finally obtaining the alumina capable of being used as a heat-conducting filler.
The source of the dust collecting powder in the invention is a byproduct of alumina production by calcining in a rotary kiln, and the raw material of the rotary kiln is industrial alumina with purity of national first-grade product.
The pH value in the washing process of the invention is 4-7, and the optimal condition is 5-6.
The calcination process in the invention is in a tunnel kiln or a shuttle kiln, and the kiln is a ceramic sagger or a clay sagger.
The calcination temperature in the present invention is preferably 1200-1250 ℃.
The invention has the beneficial technical effects that: the invention can realize the comprehensive utilization of dust collection powder, prepare the alumina for the heat-conducting filler with typical particle size distribution characteristics, reduce the production cost by more than 30 percent compared with other types of alumina, and the alumina obtained by the invention has narrower particle size distribution and low conductivity, is superior to the existing marketized products, and has the advantages of low cost and excellent performance.
Drawings
Fig. 1 is a flow chart of a process for preparing alumina for a heat conductive filler.
Detailed Description
The present invention will be described in detail with reference to the following embodiments.
As shown in fig. 1, a method for preparing alumina for a heat-conducting filler uses a dust-collecting powder which is a byproduct of a process of producing calcined alumina by a rotary kiln, wherein the content of alumina in the dust-collecting powder is 95-97%, and the laser particle size is D10: 10-15 μm, D50: 20-30 μm, D90: 40-50 um; adding pure water and a certain amount of inorganic acid into the dust collecting powder to prepare slurry with the concentration of 200-70 ℃ and the pH of 4-7, washing at 40-70 ℃, then carrying out filter pressing to obtain a filter cake, calcining at the temperature of 1200-1300 ℃, and crushing and screening by adopting a plastic roller pair or a polyurethane roller pair to obtain the aluminum oxide which can be used as a heat-conducting filler. The calcination process in the invention is in a tunnel kiln or a shuttle kiln, and the kiln furniture is a ceramic sagger or a clay sagger; the calcination temperature in the invention is preferably 1200-1250 ℃; the dust collecting powder is obtained from a byproduct generated in the process of calcining the alumina in the rotary kiln, the raw material of the rotary kiln is industrial alumina, the purity of the industrial alumina is a national first-grade product, the comprehensive utilization of the byproduct is realized through the development of the method, the method has a strong cost advantage, the cost is 30% lower than that of a product with the same index in the market, and the method is mainly reflected in the raw material and processing cost (the marketized product is obtained by grinding, crushing and grading coarse particles, and has low yield and high cost).
Example 1
Adding 0.5m into a plastic stirring tank with the volume of 1 cubic meter3Adding hot pure water with conductivity of 30 mu S/cm and temperature of 55 ℃, adding 100kg of dust collecting powder, adding a certain amount of industrial hydrochloric acid to adjust the initial pH value of the slurry to 6, stirring for 4 hours, removing the upper clear water after settling, and adding again 0.5m of clear water3Stirring the pure water at normal temperature, repeating the operation for 2-3 times, performing filter pressing by a plate-and-frame filter press, filling the obtained filter cake into a sagger, placing the sagger in a shuttle kiln, calcining for 6 hours at 1200 ℃, crushing the obtained powder by using a polyurethane pair roller, and then sieving to obtain the calcined alumina with concentrated product granularity and complete particle appearance. The technical indexes of the obtained alumina are as follows: purity 99.5%, laser particle size distribution D10: 14 μm, D50: 24 μm, D90: 43 um.
Example 2
Adding 0.5m into a plastic stirring tank with the volume of 1 cubic meter3Adding hot pure water with conductivity of 30 μ S/cm and temperature of 60 deg.C, adding 150kg of dust collecting powder, adding a certain amount of industrial hydrochloric acid to adjust initial pH of the slurry to 5, stirring for 4 hr, removing upper clear water after settling, and adding 0.5m3Stirring the pure water at normal temperature, and repeating the operation for 2 to 3 timesAnd performing filter pressing by using a plate-and-frame filter press, loading the obtained filter cake into a sagger, placing the sagger in a shuttle kiln, calcining for 6 hours at 1230 ℃, crushing the obtained powder by using a polyurethane pair roller, and then screening to obtain calcined alumina with concentrated product granularity and complete particle appearance. The technical indexes of the obtained alumina are as follows: purity 99.3%, laser particle size distribution D10: 12 μm, D50: 26 μm, D90: 48 um.
Example 3
Adding 0.5m into a plastic stirring tank with the volume of 1 cubic meter3Adding hot pure water with conductivity of 30 μ S/cm and temperature of 65 deg.C, adding 200kg of dust collecting powder, adding a certain amount of industrial hydrochloric acid to adjust initial pH of the slurry to 4, stirring for 4 hr, removing upper clear water after settling, and adding 0.5m3Stirring the pure water at normal temperature, repeating the operation for 2-3 times, performing filter pressing by a plate-and-frame filter press, putting the obtained filter cake into a sagger, placing the sagger in a shuttle kiln, calcining for 6 hours at 1250 ℃, crushing the obtained powder by using a polyurethane pair roller, and then sieving to obtain the calcined alumina with concentrated product granularity and complete particle appearance. The technical indexes of the obtained alumina are as follows: the purity is 99.6%, the laser particle size distribution is D10: 15 μm, D50: 26.5 μm, D90: 44 um.
The above description is only for the purpose of illustrating the preferred embodiments of the present invention and is not to be construed as limiting the invention. It should be noted that other equivalent modifications can be made by those skilled in the art in light of the teachings of the present invention, and all such modifications can be made as are within the scope of the present invention.
Claims (5)
1. The preparation method of the alumina for the heat-conducting filler is characterized in that the used raw materials are dust collecting powder which is a byproduct in the process of producing and calcining the alumina by a rotary kiln, wherein the content of the alumina in the dust collecting powder is 95-97%, and the laser granularity is D10: 10-15 μm, D50: 20-30 μm, D90: 40-50 um; adding pure water and a certain amount of inorganic acid into the dust collecting powder to prepare slurry with the concentration of 200-70 ℃ and the pH of 4-7, washing at 40-70 ℃, then carrying out filter pressing to obtain a filter cake, calcining at the temperature of 1200-1300 ℃, and crushing and screening by adopting a plastic roller pair or a polyurethane roller pair to obtain the aluminum oxide which can be used as a heat-conducting filler.
2. The method for preparing alumina as heat-conducting filler according to claim 1, wherein the source of the dust is a byproduct of alumina production by calcination in a rotary kiln, and the raw material of the rotary kiln is industrial alumina with purity of national first-grade standard.
3. The method of preparing alumina for a heat conductive filler according to claim 1, wherein the PH of washing is 5 to 6.
4. The method of preparing alumina for a heat conductive filler according to claim 1, wherein the calcination process is in a tunnel kiln or a shuttle kiln, and the kiln furniture is a ceramic sagger or a clay sagger.
5. The method for producing alumina for a heat conductive filler according to claim 1 or 2, characterized in that the calcination temperature is 1200-1250 ℃.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN116161686A (en) * | 2022-12-27 | 2023-05-26 | 联瑞新材(连云港)有限公司 | Preparation method of high-heat-conductivity alumina powder for communication PKG |
| CN116462213A (en) * | 2023-05-10 | 2023-07-21 | 中铝郑州有色金属研究院有限公司 | Method for preparing submicron spherical alumina by recycling dust collection powder |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN116161686A (en) * | 2022-12-27 | 2023-05-26 | 联瑞新材(连云港)有限公司 | Preparation method of high-heat-conductivity alumina powder for communication PKG |
| CN116462213A (en) * | 2023-05-10 | 2023-07-21 | 中铝郑州有色金属研究院有限公司 | Method for preparing submicron spherical alumina by recycling dust collection powder |
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