CN109626406B - Preparation method of superfine ultra-white aluminum hydroxide micro powder - Google Patents
Preparation method of superfine ultra-white aluminum hydroxide micro powder Download PDFInfo
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- CN109626406B CN109626406B CN201811499951.2A CN201811499951A CN109626406B CN 109626406 B CN109626406 B CN 109626406B CN 201811499951 A CN201811499951 A CN 201811499951A CN 109626406 B CN109626406 B CN 109626406B
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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
- C01F7/04—Preparation of alkali metal aluminates; Aluminium oxide or hydroxide therefrom
- C01F7/14—Aluminium oxide or hydroxide from alkali metal aluminates
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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
- C01P2004/62—Submicrometer sized, i.e. from 0.1-1 micrometer
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- C—CHEMISTRY; METALLURGY
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- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
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Abstract
The invention relates to the technical field of aluminum hydroxide preparation, in particular to a method for preparing superfine and ultra-white aluminum hydroxide micropowder, which comprises the steps of injecting a sodium aluminate solution into a crystallization reactor, arranging six feeding pipes in the crystallization reactor, arranging a discharging port at the bottom of the crystallization reactor, and arranging a distributing groove at the top end of the crystallization reactor; the six feeding pipes are respectively communicated with the bottom of the distributing trough; the discharge port is communicated with the top end of the distributing trough through a circulating pump; six feeding pipes are uniformly distributed on the edge of the top of the crystallization reactor and are inclined towards the center of the crystallization reactor by 5-60 degrees, so that materials in the crystallization reactor are circularly distributed in multiple angles, and are distributed through the feeding pipes at different angles, so that the sodium aluminate solution is uniformly distributed, the particle size range of the obtained aluminum hydroxide micro powder is reduced, the change range of the whiteness is greatly reduced, the whiteness is improved, and the quality of the aluminum hydroxide micro powder is improved.
Description
Technical Field
The invention relates to the technical field of aluminum hydroxide preparation, in particular to a preparation method of superfine and ultra-white aluminum hydroxide micropowder.
Background
The aluminum hydroxide micro powder is widely applied to the fields of flame retardance, filling and the like; at present, for the preparation of aluminum hydroxide micropowder, a sodium aluminate solution is decomposed to obtain an aluminum hydroxide slurry, the aluminum hydroxide slurry is separated by a filter, and the aluminum hydroxide slurry is obtained by twice reverse washing with hot water, for example, in patent No. 201610171923.2, a carbonated sodium aluminate solution is adopted, aluminum hydroxide seed crystals are obtained and added into the sodium aluminate solution, the aluminum hydroxide seed crystals are decomposed by temperature-changing seed decomposition to obtain decomposed slurry, iron is removed, depolymerization is carried out, water is removed, and the micropowder aluminum hydroxide is obtained by scattering and classification; and carrying out carbonation treatment within the temperature range of 60-75 ℃, after adding seed crystals for 4-10h, controlling the temperature to be 45-60 ℃ for decomposition, and heating to 55-70 ℃ before discharging decomposed slurry, so that the prepared micro powder product has stable quality, the ferric oxide is less than or equal to 0.008 percent, the sodium oxide is between 0.083-0.100 percent, and the whiteness is between 96.9-98.8 percent.
Therefore, in the existing production process of the aluminum hydroxide micropowder, the prepared micropowder aluminum hydroxide needs to be scattered and graded to realize the preparation of the micropowder aluminum hydroxide, and the whiteness of the micropowder aluminum hydroxide is still not ideal, so that the application of the micropowder aluminum hydroxide is greatly influenced.
Disclosure of Invention
In order to solve the technical problems in the prior art, the invention provides a preparation method of ultrafine ultra-white aluminum hydroxide micropowder.
The method is realized by the following technical scheme:
the preparation method of the superfine ultra-white aluminum hydroxide micro powder comprises the following steps:
(1) adding 0.0001-0.003 times of active seed crystal solution into the sodium aluminate solution to obtain a mixed solution; the active seed crystal solution is prepared by mixing aluminum hydroxide and water according to equal mass ratio, operating according to a cell milling operation method, and grinding for 1.2-2.8h to obtain an aluminum hydroxide solution with the particle size of 1.8-2.2 mu m and the concentration of 330-380 g/L;
(2) placing the mixed solution in a crystallization reactor, performing circulation material distribution and mixing on the mixed solution in the crystallization reactor in a six-point material distribution mode, controlling the temperature of the mixed solution to be 50-70 ℃ for 10-14h, collecting crystals, filtering, and washing with water at 70-90 ℃ to obtain the superfine ultra-white aluminum hydroxide micropowder.
Preferably, the sodium aluminate solution contains 180g/L of alumina 160-.
Preferably, after the washing and the liquid after the washing are returned to be mixed with aluminum hydroxide in equal mass ratio, the active seed crystal solution is prepared by adopting a cell milling method.
Preferably, the six-point material distribution is that six feeding pipes are arranged in a crystallization reactor, a discharge port is arranged at the bottom of the crystallization reactor, and a material distribution groove is arranged at the top end of the crystallization reactor; the six feeding pipes are respectively communicated with the bottom of the distributing trough; the discharge port is communicated with the top end of the distributing trough through a circulating pump; the six feeding pipes are uniformly distributed at the top edge of the crystallization reactor and are inclined towards the center of the crystallization reactor by 5-60 degrees.
Preferably, the adding amount of the active seed crystal solution accounts for 0.0015 to 0.0024 times of the weight of the sodium aluminate solution.
Preferably, the addition amount of the active seed crystal solution is 0.0019 times of the weight of the sodium aluminate solution.
Preferably, the concentration of the aluminum hydroxide in the active seed crystal solution is 350 g/L.
The superfine ultra-white aluminum hydroxide micro powder prepared by the preparation method has the granularity of 0.1-0.4 mu m and the whiteness of 98.9-99.2 percent.
Compared with the prior art, the invention has the technical effects that:
injecting a sodium aluminate solution into a crystallization reactor, arranging six feeding pipes in the crystallization reactor, arranging a discharging port at the bottom of the crystallization reactor, and arranging a distributing chute at the top end of the crystallization reactor; the six feeding pipes are respectively communicated with the bottom of the distributing trough; the discharge port is communicated with the top end of the distributing trough through a circulating pump; six feeding pipes are uniformly distributed on the edge of the top of the crystallization reactor and are inclined towards the center of the crystallization reactor by 5-60 degrees, so that materials in the crystallization reactor are circularly distributed in multiple angles, and are distributed through the feeding pipes at different angles, so that the sodium aluminate solution is uniformly distributed, the particle size range of the obtained aluminum hydroxide micro powder is reduced, the change range of the whiteness is greatly reduced, the whiteness is improved, and the quality of the aluminum hydroxide micro powder is improved.
Particularly, the mixed solution of aluminum hydroxide and water in equal proportion is ground by adopting a cell grinding method, so that the activity of the prepared seed crystal solution is greatly enhanced, the uniform precipitation of the aluminum hydroxide in the sodium aluminate solution is improved, the fast and slow time in the precipitation process of the aluminum hydroxide is avoided, the uniformity of the precipitation process of the aluminum hydroxide is also improved, the accumulation and precipitation are avoided, the particle size range of the prepared aluminum hydroxide micropowder is narrow, the particle size uniformity of the micropowder is improved, the whiteness range is narrowed, and the quality of the aluminum hydroxide micropowder is improved.
Through research, the particle size range of the prepared aluminum hydroxide micro powder is maintained between 0.1 and 0.4 mu m, the whiteness is between 98.9 and 99.2 percent, and the quality of the aluminum hydroxide micro powder is greatly improved.
Detailed Description
The technical solution of the present invention is further defined below with reference to the specific embodiments, but the scope of the claims is not limited to the description.
In the following examples, the present investigators installed six feeding pipes in the crystallization reactor, and installed a discharge port at the bottom of the crystallization reactor, and installed a distribution chute at the top of the crystallization reactor; the six feeding pipes are respectively communicated with the bottom of the distributing trough; the discharge port is communicated with the top end of the distributing trough through a circulating pump; six feeding pipes are uniformly distributed on the edge of the top of the crystallization reactor, and six-point material distribution treatment is carried out on equipment which is inclined towards the center of the crystallization reactor by 5-60 degrees.
Example 1
Adopting a sodium aluminate solution containing 160g/L of alumina as a raw material for preparing micro-powder aluminum hydroxide; adding 0.0001 times of active seed crystal solution to obtain mixed solution; the active seed crystal solution is prepared by mixing aluminum hydroxide and water according to equal mass ratio, operating according to a cell mill operating method, and grinding for 1.2h to obtain an aluminum hydroxide solution with the particle size of 1.8 mu m and the concentration of 330g/L, wherein the causticity ratio of the aluminum hydroxide solution is 0;
and injecting the mixed solution into a crystallization reactor, performing circulating material distribution and uniform mixing on the mixed solution in the crystallization reactor in a six-point material distribution mode, controlling the temperature of the mixed solution to be 50 ℃ and performing circulating material distribution for 10 hours, collecting crystals, filtering, and washing with water at the temperature of 70 ℃ to obtain the superfine ultra-white aluminum hydroxide micropowder.
Example 2
Adopting a sodium aluminate solution containing 180g/L of alumina as a raw material for preparing micro-powder aluminum hydroxide; adding 0.003 times of active seed crystal solution to obtain a mixed solution; the active seed crystal solution is prepared by mixing aluminum hydroxide and the washed solution obtained in the embodiment 1 according to the equal mass ratio, operating according to a cell milling operation method, and grinding for 2.8 hours to obtain an aluminum hydroxide solution with the particle size of 2.2 mu m and the concentration of 380g/L, wherein the causticity ratio of the aluminum hydroxide solution is 0.3;
and injecting the mixed solution into a crystallization reactor, performing circulating material distribution and uniform mixing on the mixed solution in the crystallization reactor in a six-point material distribution mode, controlling the temperature of the mixed solution to be 70 ℃ and performing circulating material distribution for 14 hours, collecting crystals, filtering, and washing with water at the temperature of 90 ℃ to obtain the superfine ultra-white aluminum hydroxide micropowder.
Example 3
Adopting a sodium aluminate solution containing 170g/L of alumina as a raw material for preparing micro-powder aluminum hydroxide; adding 0.0015 times of active seed crystal solution to obtain a mixed solution; the active seed crystal solution is prepared by mixing aluminum hydroxide and the washed solution obtained in the embodiment 1 according to the equal mass ratio, operating according to a cell milling operation method, and grinding for 1.7h to obtain an aluminum hydroxide solution with the particle size of 1.9 mu m and the concentration of 350g/L, wherein the causticity ratio of the aluminum hydroxide solution is 1.2;
and injecting the mixed solution into a crystallization reactor, performing circulating material distribution and uniform mixing on the mixed solution in the crystallization reactor in a six-point material distribution mode, performing circulating material distribution for 13 hours at the temperature of 60 ℃, collecting crystals, filtering, and washing with water at the temperature of 80 ℃ to obtain the superfine ultrawhite aluminum hydroxide micropowder.
Example 4
Adopting a sodium aluminate solution containing 168g/L of alumina as a raw material for preparing micro-powder aluminum hydroxide; adding 0.0025 times of active seed crystal solution to obtain mixed solution; the active seed crystal solution is prepared by mixing aluminum hydroxide and the washed solution obtained in the embodiment 1 according to the equal mass ratio, operating according to a cell milling operation method, and grinding for 2.3h to obtain an aluminum hydroxide solution with the particle size of 2.1 mu m and the concentration of 367g/L, wherein the causticity ratio of the aluminum hydroxide solution is 0.9;
and injecting the mixed solution into a crystallization reactor, performing circulating material distribution and uniform mixing on the mixed solution in the crystallization reactor in a six-point material distribution mode, controlling the temperature of the mixed solution to be 58 ℃ and performing circulating material distribution for 12 hours, collecting crystals, filtering, and washing with water at 88 ℃ to obtain the superfine ultra-white aluminum hydroxide micropowder.
Example 5
Adopting a sodium aluminate solution containing 176g/L alumina as a raw material for preparing micro-powder aluminum hydroxide; adding 0.0019 times of active seed crystal solution to obtain a mixed solution; the active seed crystal solution is prepared by mixing aluminum hydroxide and the washed solution obtained in the embodiment 1 according to the equal mass ratio, operating according to a cell milling operation method, and grinding for 1.6h to obtain an aluminum hydroxide solution with the particle size of 2.2 mu m and the concentration of 330g/L, wherein the causticity ratio of the aluminum hydroxide solution is 1.5;
and injecting the mixed solution into a crystallization reactor, performing circulating material distribution and uniform mixing on the mixed solution in the crystallization reactor in a six-point material distribution mode, controlling the temperature of the mixed solution to be 70 ℃ and performing circulating material distribution for 10 hours, collecting crystals, filtering, and washing with water at the temperature of 90 ℃ to obtain the superfine ultra-white aluminum hydroxide micropowder.
Particle size and whiteness measurements:
the particle size measuring method comprises the following steps: a laser scattering type particle size distribution measuring device in the prior art is used; adding a sample to a 0.2 mass% sodium hexametaphosphate aqueous solution, adjusting the concentration to a measurable concentration, irradiating with ultrasonic waves having an output of 25W for 120 seconds, and measuring with the number of samples being 2; further, a particle size distribution curve is obtained, a particle size distribution range is obtained from the curve, and the particle size results of the micro-powder aluminum hydroxide products prepared in the above examples 1 to 5 are specifically determined as shown in the following table 1:
whiteness measurement the whiteness measurement was carried out according to the whiteness measurement method of the aluminum hydroxide fine powder in the prior art, and the results are shown in table 1.
TABLE 1
| Example 1 | Example 2 | Example 3 | Example 4 | Example 5 | |
| Particle size range (μm) | 0.25-0.37 | 0.28-0.40 | 0.31-0.38 | 0.12-0.36 | 0.16-0.39 |
| Average particle diameter (μm) | 0.28 | 0.36 | 0.34 | 0.27 | 0.24 |
| Whiteness (%) | 99.2 | 98.9 | 99.0 | 99.1 | 98.9 |
As can be seen from Table 1, the particle size range of the prepared aluminum hydroxide micropowder is narrow, the average particle size and the maximum particle size are both lower than 0.5 μm, the micropowder yield of the ultrafine aluminum hydroxide is improved, and the whiteness of the ultrafine aluminum hydroxide is improved to a certain extent.
The above description is only for the preferred embodiment of the present invention, but the scope of the present invention is not limited thereto, and any person skilled in the art should be considered to be within the technical scope of the present invention, and the technical solutions and the inventive concepts thereof according to the present invention should be equivalent or changed within the scope of the present invention.
Claims (7)
1. A preparation method of superfine ultra-white aluminum hydroxide micropowder is characterized by comprising the following steps:
(1) adding 0.0001-0.003 times of active seed crystal solution into the sodium aluminate solution to obtain a mixed solution; the active seed crystal solution is prepared by mixing aluminum hydroxide and water according to equal mass ratio, operating according to a cell milling operation method, and grinding for 1.2-2.8h to obtain an aluminum hydroxide solution with the particle size of 1.8-2.2 mu m and the concentration of 330-380 g/L;
(2) placing the mixed solution in a crystallization reactor, performing circulating material distribution and mixing on the mixed solution in the crystallization reactor in a six-point material distribution mode, controlling the temperature of the mixed solution to be 50-70 ℃ and performing circulating material distribution for 10-14h, collecting crystals, filtering, and washing with water at 70-90 ℃ to obtain superfine ultra-white aluminum hydroxide micropowder;
the six-point material distribution is characterized in that six feeding pipes are arranged in a crystallization reactor, a discharge port is arranged at the bottom of the crystallization reactor, and a material distribution groove is arranged at the top end of the crystallization reactor; the six feeding pipes are respectively communicated with the bottom of the distributing trough; the discharge port is communicated with the top end of the distributing trough through a circulating pump; the six feeding pipes are uniformly distributed at the top edge of the crystallization reactor and are inclined towards the center of the crystallization reactor by 5-60 degrees.
2. The method for preparing ultra-fine ultra-white aluminum hydroxide micropowder as claimed in claim 1, wherein the sodium aluminate solution contains alumina 160-180 g/L.
3. The method for preparing ultra-fine ultra-white aluminum hydroxide micropowder of claim 1, wherein the active seed crystal solution is prepared by cell milling after washing and returning the washed solution to mix with aluminum hydroxide in equal mass ratio.
4. The method for preparing ultra-fine ultra-white aluminum hydroxide micropowder of claim 1, wherein the amount of the active seed crystal solution added is 0.0015 to 0.0024 times the weight of the sodium aluminate solution.
5. The method for preparing ultra-fine ultra-white aluminum hydroxide micropowder according to claim 1 or 4, wherein the amount of the active seed solution added is 0.0019 times the weight of the sodium aluminate solution.
6. The method for preparing ultra-fine ultra-white aluminum hydroxide micropowder according to claim 1 or 4, wherein the concentration of aluminum hydroxide in the active seed solution is 350 g/L.
7. The ultra-fine ultra-white aluminum hydroxide micropowder prepared by the preparation method according to any one of claims 1 to 6, characterized in that the micropowder has a particle size of 0.1 to 0.4 μm and a whiteness of 98.9 to 99.2%.
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