CN113060746A - Preparation method of large-particle-size alumina raw material and spherical alumina product thereof - Google Patents
Preparation method of large-particle-size alumina raw material and spherical alumina product thereof Download PDFInfo
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- CN113060746A CN113060746A CN202110398581.9A CN202110398581A CN113060746A CN 113060746 A CN113060746 A CN 113060746A CN 202110398581 A CN202110398581 A CN 202110398581A CN 113060746 A CN113060746 A CN 113060746A
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01F—COMPOUNDS OF THE METALS BERYLLIUM, MAGNESIUM, ALUMINIUM, CALCIUM, STRONTIUM, BARIUM, RADIUM, THORIUM, OR OF THE RARE-EARTH METALS
- 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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- C01F7/00—Compounds of aluminium
- C01F7/02—Aluminium oxide; Aluminium hydroxide; Aluminates
- C01F7/021—After-treatment of oxides or hydroxides
- C01F7/025—Granulation or agglomeration
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- C01F—COMPOUNDS OF THE METALS BERYLLIUM, MAGNESIUM, ALUMINIUM, CALCIUM, STRONTIUM, BARIUM, RADIUM, THORIUM, OR OF THE RARE-EARTH METALS
- C01F7/00—Compounds of aluminium
- C01F7/02—Aluminium oxide; Aluminium hydroxide; Aluminates
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- C01F7/026—Making or stabilising dispersions
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- C01P2004/30—Particle morphology extending in three dimensions
- C01P2004/32—Spheres
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- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
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- C01P2004/60—Particles characterised by their size
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- 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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Abstract
The invention provides a preparation method of a large-particle-size alumina raw material and a spherical alumina product thereof, wherein the preparation method comprises the following steps: crushing a part of the raw powder to obtain crushed fine powder; grading the crushed fine powder and the uncrushed raw powder according to the weight ratio, and stirring and uniformly mixing the crushed fine powder, the uncrushed raw powder, pure water and an adhesive to prepare slurry; and (3) carrying out spray granulation on the uniformly mixed slurry at a set drying temperature to obtain the large-particle-size alumina raw material. The large-particle-size alumina raw material can be made into spherical alumina products through flame melting and spheroidizing. The method sequentially processes the raw powder through crushing, grading and spray granulation, so that the large-particle-size alumina raw material can be prepared in batches, the production cost is low, the process is simple, and the spherical alumina product produced by the raw material is completely suitable for being used as a heat-conducting filler, has high yield and can meet the market demand for the large-particle-size spherical alumina product.
Description
Technical Field
The invention belongs to the technical field of spherical alumina preparation, and particularly relates to a preparation method of a large-particle-size alumina raw material and a spherical alumina product thereof.
Background
Along with the development of the 5G communication technology, the power of related electronic devices is greatly improved, the requirement on heat dissipation capacity is also improved, and the requirement on high-heat-conductivity heat dissipation filler is correspondingly increased. The heat conductivity of the thermal interface material is high or low, and the grain size of the spherical alumina filler plays an important role. The large-particle-size spherical alumina, particularly the heat-conducting gasket or the heat-conducting gel with the particle size of more than 90 mu m, which can prepare 7W/(m.K) is suitable for 5G base stations. However, the particle size of the alumina raw material for preparing the large-particle spherical alumina product is at least more than 100 μm, and the source of the alumina raw material with the particle size is very small, so that the production capacity of the large-particle spherical alumina is severely restricted.
At present, the average grain size of industrial alumina produced in the alumina industry is 70-80 μm, 90% of the yield is used in the electrolytic aluminum industry, and in addition, 10% of the yield is used in the chemical alumina industry, and calcined alumina is prepared by calcination processing and is used in the fields of refractory materials and alumina ceramics. The part of chemical alumina contains about 5 percent of alumina with large particle size of more than 100 mu m, and can be obtained by a screening process and used as a raw material of spherical alumina with large particle size. However, this sieving method requires a large amount of raw alumina to obtain a small amount of large-particle-size alumina, and the yield is low, and the by-product of the alumina sieved out is not easily digested. Another method for obtaining alumina raw material with particle size above 100 μm is to artificially synthesize large-particle-size aluminum hydroxide and further process it into alumina, but this method is expensive, usually more than four times as high as the sieving method, and has a small yield.
Disclosure of Invention
Aiming at the defects of the prior art, the invention aims to provide a preparation method of a large-particle-size alumina raw material and a spherical alumina product thereof.
In order to achieve the purpose, the invention adopts the technical scheme that:
the invention firstly discloses a preparation method of a large-particle-size alumina raw material, which comprises the following steps:
s1, crushing a part of the raw powder to obtain crushed fine powder;
s2, grading the crushed fine powder and the uncrushed raw powder according to the weight ratio, and stirring and uniformly mixing the crushed fine powder, the uncrushed raw powder, the pure water and the adhesive to prepare slurry;
and S3, carrying out spray granulation on the uniformly mixed slurry at the set drying temperature to obtain the large-particle-size alumina raw material.
In one embodiment disclosed herein, the raw powder is industrial alumina or calcined alumina.
In one embodiment disclosed in the present application, the average particle size of the crushed fine powder is 0.5 to 20 μm.
In one embodiment disclosed herein, the weight ratio of the materials in the gradation is as follows:
the weight ratio of the crushed fine powder to the uncrushed raw powder is 1: 9-7: 3;
the weight ratio of the total weight of the crushed fine powder and the uncrushed raw powder to the pure water is 3: 7-7: 3;
the addition amount of the binder is 1-10% of the total weight of the powder.
In one embodiment of the present disclosure, in step S2, pure water, binder, crushed fine powder and uncrushed raw powder are fed in this order.
In one embodiment disclosed in the present application, the binder is one or more of polyvinyl alcohol, polyethylene glycol, alumina sol, and polyacrylic acid.
In one embodiment disclosed herein, the set drying temperature is > 200 ℃.
In one embodiment disclosed in the application, the crushing processing is completed in powder crushing equipment, the grading is completed in a stirring kettle, and the spray granulation is completed in spray granulation equipment; the powder crushing equipment, the stirring kettle and the spray granulation equipment are sequentially arranged according to the working procedures to form the preparation device of the large-particle-size alumina raw material.
The invention also discloses a spherical alumina product, which is prepared by preparing the alumina raw material by the preparation method of the alumina raw material with large particle size and spheroidizing the alumina raw material by flame melting.
In one embodiment disclosed herein, the flame melt spheroidization is accomplished at a spheroidization temperature of greater than or equal to 2000 ℃ in a spheroidization furnace disposed downstream of the spray granulation apparatus.
The beneficial effects of the invention can be concluded from the above technical solution:
the method is characterized in that industrial alumina or calcined alumina which is easy to obtain and low in cost is used as raw powder, and a large-particle-size alumina raw material with the particle size of more than 100 mu m is prepared by crushing, grading and spray granulation, so that the method is low in production cost and simple in process, can be used for preparing the raw material in batches, and further can be used for producing spherical alumina products with the particle size of 90 mu m or more, is completely suitable for being used as a heat-conducting filler, is high in yield, and can meet the market demand for the large-particle-size spherical alumina products.
Drawings
In order to more clearly illustrate the embodiments of the present application or the technical solutions in the prior art, the drawings used in the description of the embodiments or the prior art will be briefly described below, it is obvious that the drawings in the following description are only some embodiments of the present application, and for those skilled in the art, other drawings can be obtained according to the drawings without creative efforts.
FIG. 1 is a schematic diagram of the operation steps of the preparation method disclosed by the present invention.
Detailed Description
In the following, only certain exemplary embodiments are briefly described. As those skilled in the art will recognize, the described embodiments may be modified in various different ways, all without departing from the spirit or scope of the present invention. Accordingly, the drawings and description are to be regarded as illustrative in nature, and not as restrictive.
The following disclosure provides many different embodiments or examples for implementing the invention. To simplify the disclosure of the present invention, the steps of a specific example are described below. Of course, they are merely examples and are not intended to limit the present invention.
Embodiments of the present invention will be described in detail below with reference to the accompanying drawings.
Referring to fig. 1, a method for preparing a large-particle-size alumina raw material disclosed in the embodiments of the present application includes the following steps:
s1, crushing a part of the raw powder to obtain crushed fine powder.
The method is characterized in that industrial alumina or calcined alumina which is easy to obtain and low in cost is used as raw powder, and the micro-morphology of alumina particles in the raw powder is angular; and (3) taking a part of the raw powder to carry out crushing processing in powder crushing equipment such as a ball mill, an air flow mill and the like to obtain small-particle-size crushed fine powder with the average particle size of 0.5-20 mu m.
And S2, grading the crushed fine powder and the uncrushed raw powder according to the weight ratio, stirring and uniformly mixing the crushed fine powder, the uncrushed raw powder, the pure water and the adhesive to prepare slurry.
Grading the crushed fine powder and the uncrushed raw powder according to the weight ratio of 1: 9-7: 3 so as to improve the strength and compaction degree of the granulation ball; the weight ratio of the total weight of the crushed fine powder and the uncrushed raw powder to the pure water is 3: 7-7: 3; the binder can be one or more of polyvinyl alcohol, polyethylene glycol, alumina sol and polyacrylic acid, and the addition amount of the binder is 1-10% of the total weight of the powder; grading is completed in a stirring kettle, pure water, a binder, crushed fine powder and uncrushed raw powder are sequentially fed into the stirring kettle, and stirring is kept for at least half an hour after feeding is completed, so that slurry is fully and uniformly mixed.
And S3, carrying out spray granulation on the uniformly mixed slurry at the set drying temperature to obtain the large-particle-size alumina raw material.
Carrying out spray granulation on the uniformly mixed slurry by adopting spray granulation equipment, firstly starting the spray granulation equipment, preheating to a set drying temperature of more than 200 ℃, and then pumping the uniformly mixed slurry into a feeding system of the spray granulation equipment for spray granulation; by adjusting spray granulation parameters, the large-particle-size alumina raw material with the average particle size of more than 100 mu m can be prepared, and the micro-morphology is spherical; the spray granulation apparatus may be a centrifugal spray granulation tower or a pressure spray granulation tower.
The powder crushing equipment, the stirring kettle and the spray granulation equipment are arranged in sequence according to the working procedures to form the preparation device of the large-particle-size alumina raw material.
The spherical alumina product disclosed by the embodiment of the invention is prepared by melting and spheroidizing the obtained alumina raw material with large particle size by flame.
Specifically, a spheroidizing furnace arranged downstream of the spray granulation equipment is used as flame melting spheroidizing equipment, and the large-particle-size alumina raw material obtained by spray granulation is put into the spheroidizing furnace to be melted to prepare the spherical alumina. The spheroidizing furnace is a flame furnace, uses natural gas as fuel, uses oxygen to support combustion, and makes the flame burn downwards, and the furnace chamber temperature is greater than 2000 deg.C. The powder is put into the device from a feed inlet at the top end of the device and is melted into balls in the process of downwards passing through the flame, so that the spherical alumina product is prepared. And then, after the spherical alumina product is cooled and packaged, bagging the product by taking a 25Kg bag as a standard, wherein the inner layer is a plastic bag, and the outer layer is a kraft paper bag.
The average particle size of the large-particle-size alumina raw material is more than 100 mu m, and the particle size is shrunk by about 10% in the melting process, so that the final alumina product can reach more than 90 mu m and can be used for preparing a heat-conducting gasket or heat-conducting gel of 7W/(m.K). Meanwhile, the large-particle-size alumina raw material is formed by mixing crushed fine powder and uncrushed raw powder in a grading manner, so that the gaps inside the large-particle-size alumina raw material are smaller, and the sphericity of the large-particle-size alumina raw material cannot be influenced by the collapse of the inner gaps in the melting and shrinking process of alumina. The spray granulation ensures that the large-particle-size alumina raw material has better sphericity and good foundation, and is beneficial to finally obtaining spherical alumina products.
According to the preparation method of the large-particle-size alumina raw material and the spherical alumina product thereof, disclosed by the invention, the large-particle-size alumina raw material is prepared by taking industrial alumina or calcined alumina as raw powder through crushing, grading and spray granulation methods, the production cost is low, the process is simple, the raw material can be prepared in batches, and then the spherical alumina product is produced from the raw material, so that the preparation method is completely suitable for being used as a heat-conducting filler, the yield is high, and the market demand on the large-particle-size spherical alumina product can be met.
The present invention will be explained and illustrated in further detail with reference to specific examples, which are not intended to limit the scope of the present invention in any way.
The first embodiment is as follows: preparing a large-particle-size alumina raw material with the particle size of 120 mu m, and firing to obtain a spherical alumina product with the particle size of 90 mu m.
1. 500Kg of raw industrial alumina powder having an average particle size of 76 μm was prepared, and 150Kg thereof was pulverized by a ball mill into a fine powder having an average particle size of 10 μm.
2. And opening the stirring kettle, injecting 400L of pure water, adding 5Kg of polyvinyl alcohol, stirring uniformly, sequentially adding 150Kg of 10 μm fine powder and the rest 350Kg of industrial alumina raw powder, and keeping stirring for more than half an hour to prepare the slurry.
3. Starting a spray granulation tower, preheating, pumping the slurry in the stirring kettle into a feed system of the spray granulation tower by using a diaphragm pump, and starting spray granulation to obtain a large-particle-size alumina raw material; the temperature in the tower of the granulation tower is maintained above 200 ℃, and the average grain diameter of the granulated product is 119 mu m by a laser particle sizer.
4. Starting the spheroidizing furnace, preheating for 2 hours, and starting to add the large-particle-size alumina raw material for flame melting spheroidization when the furnace temperature is increased to 2000 ℃.
5. The average grain diameter of the spheroidized product is 90 mu m through the inspection of a laser particle sizer, the heat conductivity coefficient is 7.5W/(m.K), and the preparation of the spherical alumina product is finished.
Example two: preparing 150 mu m of large-particle-size alumina raw material, and firing to obtain a 120 mu m spherical alumina product.
1. 500Kg of calcined alumina raw powder having an average particle size of 82 μm was prepared, and 300Kg thereof was pulverized by a ball mill into a fine powder having an average particle size of 5 μm.
2. Opening the stirring kettle, injecting 500L of pure water, adding 5Kg of polyvinyl alcohol and 5Kg of polyethylene glycol, stirring uniformly, sequentially adding 300Kg of 5 μm fine powder and the rest 200Kg of calcined alumina raw powder, and stirring for more than half an hour to obtain the slurry.
3. Starting a spray granulation tower, preheating, pumping the slurry in the stirring kettle into a feed system of the spray granulation tower by using a diaphragm pump, and starting spray granulation to obtain a large-particle-size alumina raw material; the temperature in the tower of the granulation tower is maintained above 200 ℃, and the average grain diameter of the granulated product is 155 mu m by a laser particle sizer.
4. Starting the spheroidizing furnace, preheating for 2 hours, and starting to add the large-particle-size alumina raw material for flame melting spheroidization when the furnace temperature is increased to 2000 ℃.
5. The average grain diameter of the spheroidized product is 121 mu m through the inspection of a laser particle sizer, the heat conductivity coefficient is 7.1W/(m.K), and the preparation of the spherical alumina product is finished.
From the results of the above examples it can be seen that: no matter industrial alumina raw powder or calcined alumina raw powder is adopted, after crushing, grading and spray granulation, alumina raw materials with the particle size of more than 100 mu m can be prepared, so that spherical alumina products with the particle size of 90 mu m and above can be further prepared, the method is completely suitable for being used as heat-conducting fillers, the process is simple, the yield is high, the production cost is low, and the market demand on large-particle-size spherical alumina products can be met.
The above embodiments are only preferred embodiments of the present invention, and are not intended to limit the technical solutions of the present invention, so long as the technical solutions can be realized on the basis of the above embodiments without creative efforts, which should be considered to fall within the protection scope of the patent of the present invention.
Claims (10)
1. A preparation method of a large-particle-size alumina raw material is characterized by comprising the following steps of:
s1, crushing a part of the raw powder to obtain crushed fine powder;
s2, grading the crushed fine powder and the uncrushed raw powder according to the weight ratio, and stirring and uniformly mixing the crushed fine powder, the uncrushed raw powder, the pure water and the adhesive to prepare slurry;
and S3, carrying out spray granulation on the uniformly mixed slurry at the set drying temperature to obtain the large-particle-size alumina raw material.
2. The method of producing a large-particle-size alumina starting material according to claim 1, wherein the raw powder is industrial alumina or calcined alumina.
3. The method of producing a large-particle-size alumina starting material according to claim 1, wherein the average particle size of the finely pulverized powder is 0.5 to 20 μm.
4. The method for preparing a large-particle-size alumina raw material according to any one of claims 1 to 3, wherein the weight ratio of each material in the gradation is as follows:
the weight ratio of the crushed fine powder to the uncrushed raw powder is 1: 9-7: 3;
the weight ratio of the total weight of the crushed fine powder and the uncrushed raw powder to the pure water is 3: 7-7: 3;
the addition amount of the binder is 1-10% of the total weight of the powder.
5. The method of preparing a large-particle-size alumina starting material according to claim 4, wherein in step S2, pure water, a binder, a crushed fine powder, and an uncrushed raw powder are fed in this order.
6. The method for preparing the large-particle-size alumina raw material according to claim 5, wherein the binder is one or more of polyvinyl alcohol, polyethylene glycol, alumina sol and polyacrylic acid.
7. The method of producing a large-particle-size alumina starting material according to claim 1, wherein the set drying temperature is > 200 ℃.
8. The method for preparing a large-particle-size alumina starting material according to claim 1, wherein the pulverization processing is performed in a powder pulverization device, the gradation is performed in a stirred tank, and the spray granulation is performed in a spray granulation device.
9. A spherical alumina product, which is characterized in that,
preparing an alumina raw material by using the method for preparing the large-particle-size alumina raw material according to any one of claims 1 to 8, and performing flame melting and spheroidizing on the alumina raw material to obtain a spherical alumina product;
the average particle size of the spherical alumina product is more than 90 μm.
10. The spherical alumina product according to claim 9, wherein the flame fusion spheroidization temperature is not less than 2000 ℃.
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| WO2023040599A1 (en) * | 2021-09-14 | 2023-03-23 | 江苏联瑞新材料股份有限公司 | Preparation method for spherical alumina having low viscosity and high thermal conductivity |
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