CN109626406A - A kind of ultra-fine ultrawhite aluminum hydroxide micro mist preparation method - Google Patents
A kind of ultra-fine ultrawhite aluminum hydroxide micro mist preparation method Download PDFInfo
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- CN109626406A CN109626406A CN201811499951.2A CN201811499951A CN109626406A CN 109626406 A CN109626406 A CN 109626406A CN 201811499951 A CN201811499951 A CN 201811499951A CN 109626406 A CN109626406 A CN 109626406A
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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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- C—CHEMISTRY; METALLURGY
- 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
- C01P2004/62—Submicrometer sized, i.e. from 0.1-1 micrometer
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/60—Optical properties, e.g. expressed in CIELAB-values
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Abstract
The present invention relates to aluminium hydroxide preparation technical fields, especially a kind of ultra-fine ultrawhite aluminum hydroxide micro mist preparation method, by sodium aluminate solution is injected in crystallization reactor, and by six roots of sensation feed pipe will be provided in crystallization reactor, and one discharge port is set in crystallization reactor bottom, on crystallization reactor top, distributing trough is set；Six roots of sensation feed pipe is connected to the bottom of distributing trough respectively；Discharge port is connected to by circulating pump with distributing trough top；Six roots of sensation feed pipe is evenly distributed on crystallization reactor top edge, and to crystallization reactor center be in 5-60 ° of inclination, realize that the material in crystallization reactor obtains circulation multi-angle material distribution, and the cloth Jing Guo feed pipe different angle, being uniformly distributed for sodium aluminate solution is realized, so that the particle size range of the aluminium hydroxide micro powder obtained reduces, and whiteness variation range significantly reduces, whiteness is improved simultaneously, improves the quality of aluminium hydroxide micro powder.
Description
Technical field
The present invention relates to aluminium hydroxide preparation technical field, especially a kind of ultra-fine ultrawhite aluminum hydroxide micro mist preparation side
Method.
Background technique
Aluminium hydroxide micro powder is widely used in the fields such as fire-retardant, filler；It is at present by aluminium for aluminium hydroxide micro powder preparation
Acid sodium solution decomposes to obtain aluminum hydroxide slurry, is separated using filter, the secondary back flush of hot water and obtain, such as specially
Benefit number is to be disclosed in 201610171923.2 using carbonating sodium aluminate solution, obtains aluminium hydroxide crystal seed and is added to sodium aluminate
It in solution, and is decomposed by alternating temperature kind point, obtains decomposing slurry, remove iron, depolymerization removes moisture, and scattering and grading obtains micro mist hydrogen
Aluminium oxide；And carbonating processing is carried out within the scope of temperature range is 60-75 DEG C, after crystal seed 4-10h is added, controlled at
It is decomposed at 45-60 DEG C, is warming up to 55-70 DEG C of progress before decomposing stock discharge, so that the micro powder product quality of preparation is stablized, three oxygen
Change two iron≤0.008%, sodium oxide molybdena is between 0.083-0.100%, and whiteness is between 96.9-98.8%.
As it can be seen that at present in production of aluminium hydroxide micro-powder, needing to break up the aluminium hydroxide micropowder of preparation
Classification processing, realizes the preparation of aluminium hydroxide micropowder, and the whiteness of aluminium hydroxide micropowder is still undesirable, the shadow of high degree
The application of aluminium hydroxide micropowder is rung.
Summary of the invention
In order to solve the above technical problems existing in the prior art, it is micro- to provide a kind of ultra-fine ultrawhite aluminum hydroxide by the present invention
Powder, preparation method thereof.
It is achieved particular by following technical scheme:
Ultra-fine ultrawhite aluminum hydroxide micro mist preparation method, comprising the following steps:
(1) the 0.0001-0.003 times of active seed solution weighed is added into sodium aluminate solution, obtains mixed solution；Described
Active seed solution is to mix aluminium hydroxide according to equal mass ratioes with water, is operated, is passed through according to cell mill operating method
The grinding of 1.2-2.8h obtains the aluminum hydroxide solution that partial size is 1.8-2.2 μm, concentration is 330-380g/L；
(2) mixed solution is placed in crystallization reactor, by 6 distributing modes, by mixed solution in crystallization reactor
Middle progress circulating burden distribution is uniformly mixed, and the temperature for controlling mixed solution is circulating burden distribution 10-14h at 50-70 DEG C, collects crystallization
Body, filtering, uses temperature for 70-90 DEG C of water washing, obtains ultra-fine ultrawhite aluminum hydroxide micro mist.
It is preferred that salic 160-180g/L in the sodium aluminate solution.
It is preferred that the washing, after liquid return is mixed with mass ratioes such as aluminium hydroxides after washing, using cell mill method preparation
Active seed solution.
It is preferred that 6 clothes are will to be provided with six roots of sensation feed pipe in crystallization reactor, and at crystallization reactor bottom
A discharge port is arranged in portion, and distributing trough is arranged on crystallization reactor top；Six roots of sensation feed pipe is connected to the bottom of distributing trough respectively；
Discharge port is connected to by circulating pump with distributing trough top；Six roots of sensation feed pipe is evenly distributed on crystallization reactor top edge, and to
Crystallization reactor center is in 5-60 ° of inclination.
It is preferred that the active seed solution additional amount accounts for 0.0015-0.0024 times of sodium aluminate solution and weighs.
It is preferred that the active seed solution additional amount accounts for 0.0019 times of weight of sodium aluminate solution.
It is preferred that the concentration of aluminium hydroxide is 350g/L in the active seed solution.
The ultra-fine ultrawhite aluminum hydroxide micro mist of above-mentioned preparation method preparation, powder size are 0.1-0.4 μm, and whiteness exists
98.9-99.2%.
Compared with prior art, the technical effect of the invention is embodied in:
By sodium aluminate solution is injected in crystallization reactor, and by six roots of sensation charging will be provided in crystallization reactor
Pipe, and one discharge port is set in crystallization reactor bottom, on crystallization reactor top, distributing trough is set；Six roots of sensation feed pipe difference
It is connected to the bottom of distributing trough；Discharge port is connected to by circulating pump with distributing trough top；Six roots of sensation feed pipe is evenly distributed on crystallization
Reactor head edge, and realize that the material in crystallization reactor is followed in 5-60 ° of inclination to crystallization reactor center
Ring multi-angle material distribution, and the cloth Jing Guo feed pipe different angle, realize being uniformly distributed for sodium aluminate solution, so that obtain
The particle size range of aluminium hydroxide micro powder reduces, and whiteness variation range significantly reduces, while improving whiteness, improves
The quality of aluminium hydroxide micro powder.
In particular by the mixed liquor of cell mill grinding method grinding aluminium hydroxide and water same-size ratio, so that be prepared
The activity of seed-solution significantly enhances, and the aluminium hydroxide uniformity improved in sodium aluminate solution is precipitated, and avoids hydroxide
Aluminium precipitation process is sometimes fast and sometimes slow, but also can be improved the uniformity of aluminium hydroxide precipitation process, and accumulation is avoided to be precipitated, so that system
The particle size range of standby obtained aluminium hydroxide micro powder is narrow, improves the particle size uniformity of micro mist, while but also whiteness range becomes
It is narrow, improve the quality of aluminium hydroxide micro powder.
After study, so that the particle size range of the aluminium hydroxide micro powder of preparation maintains between 0.1-0.4 μm, and whiteness
Between 98.9-99.2%, the quality for improving aluminium hydroxide micro powder of high degree.
Specific embodiment
It is limited below with reference to specific embodiment technical solution of the present invention is further, but claimed
Range is not only limited to made description.
In the examples below, this researcher, which uses, will be provided with six roots of sensation feed pipe in crystallization reactor, and anti-in crystallization
It answers device bottom that one discharge port is set, distributing trough is set on crystallization reactor top；Six roots of sensation feed pipe respectively with the bottom of distributing trough
Portion's connection；Discharge port is connected to by circulating pump with distributing trough top；Six roots of sensation feed pipe is evenly distributed on crystallization reactor top sides
Edge, and 6 cloth processing are carried out in 5-60 ° of inclined equipment to crystallization reactor center.
Embodiment 1
The raw material prepared using the sodium aluminate solution of salic 160g/L as aluminium hydroxide micropowder；It is added 0.0001 times
The active seed solution of weight, obtains mixed solution；Active seed solution is to mix aluminium hydroxide according to equal mass ratioes with water, according to
Cell mill operating method is operated, and by the grinding of 1.2h, obtains the aluminium hydroxide that partial size is 1.8 μm, concentration is 330g/L
Solution, the Crater corrosion of the aluminum hydroxide solution are 0；
Above-mentioned mixed solution is injected in crystallization reactor, by 6 distributing modes, by mixed solution in crystallization reaction
It carries out circulating burden distribution in device to be uniformly mixed, the temperature for controlling mixed solution is circulating burden distribution 10h at 50 DEG C, collects crystalline solid, mistake
Filter, uses temperature for 70 DEG C of water washing, obtains ultra-fine ultrawhite aluminum hydroxide micro mist.
Embodiment 2
The raw material prepared using the sodium aluminate solution of salic 180g/L as aluminium hydroxide micropowder；It is added 0.003 times
The active seed solution of weight, obtains mixed solution；Active seed solution be after washing in aluminium hydroxide and embodiment 1 liquid according to etc.
Mass ratio mixing is operated according to cell mill operating method, by the grinding of 2.8h, obtains that partial size is 2.2 μm, concentration is
The aluminum hydroxide solution of 380g/L, the Crater corrosion of the aluminum hydroxide solution are 0.3；
Above-mentioned mixed solution is injected in crystallization reactor, by 6 distributing modes, by mixed solution in crystallization reaction
It carries out circulating burden distribution in device to be uniformly mixed, the temperature for controlling mixed solution is circulating burden distribution 14h at 70 DEG C, collects crystalline solid, mistake
Filter, using water washing at a temperature of 90 °C, obtains ultra-fine ultrawhite aluminum hydroxide micro mist.
Embodiment 3
The raw material prepared using the sodium aluminate solution of salic 170g/L as aluminium hydroxide micropowder；It is added 0.0015 times
The active seed solution of weight, obtains mixed solution；Active seed solution be after washing in aluminium hydroxide and embodiment 1 liquid according to etc.
Mass ratio mixing is operated according to cell mill operating method, by the grinding of 1.7h, obtains that partial size is 1.9 μm, concentration is
The aluminum hydroxide solution of 350g/L, the Crater corrosion of the aluminum hydroxide solution are 1.2；
Above-mentioned mixed solution is injected in crystallization reactor, by 6 distributing modes, by mixed solution in crystallization reaction
It carries out circulating burden distribution in device to be uniformly mixed, the temperature for controlling mixed solution is circulating burden distribution 13h at 60 DEG C, collects crystalline solid, mistake
Filter, uses temperature for 80 DEG C of water washing, obtains ultra-fine ultrawhite aluminum hydroxide micro mist.
Embodiment 4
The raw material prepared using the sodium aluminate solution of salic 168g/L as aluminium hydroxide micropowder；It is added 0.0025 times
The active seed solution of weight, obtains mixed solution；Active seed solution be after washing in aluminium hydroxide and embodiment 1 liquid according to etc.
Mass ratio mixing is operated according to cell mill operating method, by the grinding of 2.3h, obtains that partial size is 2.1 μm, concentration is
The aluminum hydroxide solution of 367g/L, the Crater corrosion of the aluminum hydroxide solution are 0.9；
Above-mentioned mixed solution is injected in crystallization reactor, by 6 distributing modes, by mixed solution in crystallization reaction
It carries out circulating burden distribution in device to be uniformly mixed, the temperature for controlling mixed solution is circulating burden distribution 12h at 58 DEG C, collects crystalline solid, mistake
Filter, uses temperature for 88 DEG C of water washing, obtains ultra-fine ultrawhite aluminum hydroxide micro mist.
Embodiment 5
The raw material prepared using the sodium aluminate solution of salic 176g/L as aluminium hydroxide micropowder；It is added 0.0019 times
The active seed solution of weight, obtains mixed solution；Active seed solution be after washing in aluminium hydroxide and embodiment 1 liquid according to etc.
Mass ratio mixing is operated according to cell mill operating method, by the grinding of 1.6h, obtains that partial size is 2.2 μm, concentration is
The aluminum hydroxide solution of 330g/L, the Crater corrosion of the aluminum hydroxide solution are 1.5；
Above-mentioned mixed solution is injected in crystallization reactor, by 6 distributing modes, by mixed solution in crystallization reaction
It carries out circulating burden distribution in device to be uniformly mixed, the temperature for controlling mixed solution is circulating burden distribution 10h at 70 DEG C, collects crystalline solid, mistake
Filter, using water washing at a temperature of 90 °C, obtains ultra-fine ultrawhite aluminum hydroxide micro mist.
Partial size and measuring brightness:
Particle Size Determination Method: laser scattering type particle size distribution analyzer in the prior art is used；Sample is added to
It in 0.2 mass % hempa acid sodium aqueous solution, adjusts to the concentration that can be measured, the ultrasonic wave 120 that irradiation output is 25W
Second, then it is measured with sample number for 2；And then obtain grading curve, particle size distribution range is obtained by curve, specifically
The aluminium hydroxide micropowder product of above-described embodiment 1-5 preparation is measured, particle size results are as shown in table 1 below:
Measuring brightness is detected according to aluminium hydroxide micro powder whiteness detection method in the prior art, result such as table 1
It is shown.
Table 1
| Embodiment 1 | Embodiment 2 | Embodiment 3 | Embodiment 4 | Embodiment 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 grain diameter (μm) | 0.28 | 0.36 | 0.34 | 0.27 | 0.24 |
| Whiteness (%) | 99.2 | 98.9 | 99.0 | 99.1 | 98.9 |
Seen from table 1, the particle size range of the aluminium hydroxide micro powder prepared is relatively narrow, and average grain diameter and maximum particle diameter
It is below 0.5 μm, improves the micro mist rate of ultrafine aluminium hydroxide, but also improves aluminium hydroxide micropowder to a certain extent
Whiteness.
The foregoing is only a preferred embodiment of the present invention, but scope of protection of the present invention is not limited thereto,
Anyone skilled in the art in the technical scope disclosed by the present invention, according to the technique and scheme of the present invention and its
Inventive concept is subject to equivalent substitution or change, should be covered by the protection scope of the present invention.
Claims (8)
1. a kind of ultra-fine ultrawhite aluminum hydroxide micro mist preparation method, which comprises the following steps:
(1) the 0.0001-0.003 times of active seed solution weighed is added into sodium aluminate solution, obtains mixed solution；The activity
Seed-solution is to mix aluminium hydroxide according to equal mass ratioes with water, is operated according to cell mill operating method, by 1.2-
The grinding of 2.8h obtains the aluminum hydroxide solution that partial size is 1.8-2.2 μm, concentration is 330-380g/L；
(2) mixed solution is placed in crystallization reactor, by 6 distributing modes, by mixed solution in crystallization reactor into
Row circulating burden distribution is uniformly mixed, and the temperature for controlling mixed solution is circulating burden distribution 10-14h at 50-70 DEG C, collects crystalline solid, mistake
Filter, uses temperature for 70-90 DEG C of water washing, obtains ultra-fine ultrawhite aluminum hydroxide micro mist.
2. ultra-fine ultrawhite aluminum hydroxide micro mist preparation method as described in claim 1, which is characterized in that the sodium aluminate solution
Salic 160-180g/L in liquid.
3. ultra-fine ultrawhite aluminum hydroxide micro mist preparation method as described in claim 1, which is characterized in that the washing is washed
It washs after the return of rear liquid mixes with mass ratioes such as aluminium hydroxides, method is ground using cell and prepares active seed solution.
4. ultra-fine ultrawhite aluminum hydroxide micro mist preparation method as described in claim 1, which is characterized in that 6 clothes
It is six roots of sensation feed pipe will to be provided in crystallization reactor, and one discharge port is set in crystallization reactor bottom, in crystallization reaction
Distributing trough is arranged in device top；Six roots of sensation feed pipe is connected to the bottom of distributing trough respectively；Discharge port is by circulating pump and cloth groove top
End connection；Six roots of sensation feed pipe is evenly distributed on crystallization reactor top edge, and inclines to crystallization reactor center in 5-60 °
Tiltedly.
5. ultra-fine ultrawhite aluminum hydroxide micro mist preparation method as described in claim 1, which is characterized in that the active seed
Solution additional amount accounts for 0.0015-0.0024 times of sodium aluminate solution and weighs.
6. ultra-fine ultrawhite aluminum hydroxide micro mist preparation method as claimed in claim 1 or 5, which is characterized in that the activity
Seed-solution additional amount accounts for 0.0019 times of weight of sodium aluminate solution.
7. ultra-fine ultrawhite aluminum hydroxide micro mist preparation method as claimed in claim 1 or 5, which is characterized in that the activity
The concentration of aluminium hydroxide is 350g/L in seed-solution.
8. such as the ultra-fine ultrawhite aluminum hydroxide micro mist of the described in any item preparation method preparations of claim 1-7, which is characterized in that
Powder size is 0.1-0.4 μm, and whiteness is in 98.9-99.2%.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN110357134A (en) * | 2019-08-16 | 2019-10-22 | 山东省化工研究院 | A kind of aluminium hydroxide synthesis process size controlling method |
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