CN106186011A - Hydrated alumina and the preparation method of high temperature alumina - Google Patents
Hydrated alumina and the preparation method of high temperature alumina Download PDFInfo
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- CN106186011A CN106186011A CN201610572002.7A CN201610572002A CN106186011A CN 106186011 A CN106186011 A CN 106186011A CN 201610572002 A CN201610572002 A CN 201610572002A CN 106186011 A CN106186011 A CN 106186011A
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- CN
- China
- Prior art keywords
- preparation
- alumina
- hydrated alumina
- slurry
- high temperature
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- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 title claims abstract description 76
- 238000002360 preparation method Methods 0.000 title claims abstract description 30
- 239000002002 slurry Substances 0.000 claims abstract description 24
- WNROFYMDJYEPJX-UHFFFAOYSA-K aluminium hydroxide Chemical compound [OH-].[OH-].[OH-].[Al+3] WNROFYMDJYEPJX-UHFFFAOYSA-K 0.000 claims abstract description 23
- 229910021502 aluminium hydroxide Inorganic materials 0.000 claims abstract description 22
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 22
- 238000000034 method Methods 0.000 claims abstract description 21
- 238000009413 insulation Methods 0.000 claims abstract description 19
- 239000007788 liquid Substances 0.000 claims abstract description 9
- 238000000926 separation method Methods 0.000 claims abstract description 9
- 239000007787 solid Substances 0.000 claims abstract description 6
- 238000005406 washing Methods 0.000 claims description 5
- 238000002156 mixing Methods 0.000 claims description 2
- 239000012535 impurity Substances 0.000 abstract description 7
- 238000005265 energy consumption Methods 0.000 abstract description 4
- 230000007547 defect Effects 0.000 abstract description 3
- 238000010297 mechanical methods and process Methods 0.000 abstract description 3
- 239000000047 product Substances 0.000 description 11
- 239000012153 distilled water Substances 0.000 description 10
- 229910001648 diaspore Inorganic materials 0.000 description 5
- 238000001228 spectrum Methods 0.000 description 5
- 239000002245 particle Substances 0.000 description 4
- 239000002994 raw material Substances 0.000 description 4
- 239000013078 crystal Substances 0.000 description 3
- 238000007599 discharging Methods 0.000 description 3
- 238000005516 engineering process Methods 0.000 description 3
- 239000012065 filter cake Substances 0.000 description 3
- 229910052760 oxygen Inorganic materials 0.000 description 3
- 239000001301 oxygen Substances 0.000 description 3
- 238000005245 sintering Methods 0.000 description 3
- 229910052782 aluminium Inorganic materials 0.000 description 2
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 2
- 239000008367 deionised water Substances 0.000 description 2
- 229910021641 deionized water Inorganic materials 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 238000004137 mechanical activation Methods 0.000 description 2
- 239000000843 powder Substances 0.000 description 2
- 238000005215 recombination Methods 0.000 description 2
- 230000006798 recombination Effects 0.000 description 2
- 238000002441 X-ray diffraction Methods 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- 238000002425 crystallisation Methods 0.000 description 1
- 230000008025 crystallization Effects 0.000 description 1
- 230000001186 cumulative effect Effects 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 238000004821 distillation Methods 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 239000008187 granular material Substances 0.000 description 1
- 238000000227 grinding Methods 0.000 description 1
- 230000036571 hydration Effects 0.000 description 1
- 238000006703 hydration reaction Methods 0.000 description 1
- 238000003754 machining Methods 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 238000003701 mechanical milling Methods 0.000 description 1
- 238000010310 metallurgical process Methods 0.000 description 1
- 150000002926 oxygen Chemical class 0.000 description 1
- 239000011819 refractory material Substances 0.000 description 1
- 238000010025 steaming Methods 0.000 description 1
- 239000002023 wood Substances 0.000 description 1
Classifications
-
- 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
- C01F7/44—Dehydration of aluminium oxide or hydroxide, i.e. all conversions of one form into another involving a loss of water
- C01F7/441—Dehydration of aluminium oxide or hydroxide, i.e. all conversions of one form into another involving a loss of water by calcination
-
- 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
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2002/00—Crystal-structural characteristics
- C01P2002/70—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data
- C01P2002/72—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data by d-values or two theta-values, e.g. as X-ray diagram
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/01—Particle morphology depicted by an image
- C01P2004/03—Particle morphology depicted by an image obtained by SEM
-
- 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
- C01P2004/61—Micrometer sized, i.e. from 1-100 micrometer
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Life Sciences & Earth Sciences (AREA)
- Geology (AREA)
- Inorganic Chemistry (AREA)
- Compounds Of Alkaline-Earth Elements, Aluminum Or Rare-Earth Metals (AREA)
Abstract
The present invention provides the preparation method of a kind of hydrated alumina and high temperature alumina.The preparation method of the hydrated alumina of the present invention, comprises the steps: to mix industrial aluminium hydroxide with water, prepares slurry；By described slurry temperature be 150 300 DEG C, absolute pressure be 0.47 8.50MPa under conditions of carry out heat-insulation pressure keeping process；The slurry processed through described heat-insulation pressure keeping is carried out solid-liquid separation, and the solid obtaining solid-liquid separation washs, be dried, obtain hydrated alumina.The preparation method of the present invention reduces product granularity by non-mechanical means, thus overcomes conventional mechanical method energy consumption height, is easily introduced the defects such as impurity.
Description
Technical field
The present invention relates to a kind of aluminium oxide metallurgical technology, be specifically related to the system of a kind of hydrated alumina and high temperature alumina
Preparation Method.
Background technology
In aluminium oxide metallurgical process, the hydrated alumina of institute's output is usually aluminium hydroxide, its median (D50)
As be about 100 μm.Aluminium hydroxide as thinner in obtained granularity is in addition to using sieve method and carrying out grading, the most logical
Cross and the method for coarse granule mechanical activation comminution is realized.But, the energy consumption of mechanical milling processes is the highest, and in mechanical activation comminution
During be readily incorporated impurity.
Aluminium oxide is a kind of widely used raw material of industry, and the aluminium oxide that purity is higher can be used to produce high-grade fire proofed wood
Material.In the production process of the high-grade refractory material aluminium oxide of tradition, first prepared aluminium hydroxide dry powder by needs, then by hydrogen-oxygen
Change aluminum dry powder high-temperature roasting and remove water of crystallization, thus produce high temperature alumina.The high temperature alumina that this traditional method is prepared
Granularity simply slightly refine in roasting process, overall particle size is more or less the same with the granularity of aluminium hydroxide raw material, median
About generally 100 μm.When high temperature alumina is processed further, it usually needs by levigate for its granularity, thus obtain
Less granularity.The general employing mechanical means such as ball mill or rod mill completes grinding processes, is requiring that product granularity is thinner
Time, machining process need to consume a large amount of electric energy, is readily incorporated impurity in the course of processing simultaneously.
Summary of the invention
The present invention provides the preparation method of a kind of hydrated alumina and high temperature alumina, and it is reduced by non-mechanical means
Product granularity, thus overcome conventional mechanical method energy consumption height, be easily introduced the defects such as impurity.
The present invention provides the preparation method of a kind of hydrated alumina, comprises the steps:
Industrial aluminium hydroxide is mixed with water, prepares slurry；
By described slurry temperature be 150-300 DEG C, absolute pressure be 0.47-8.50MPa under conditions of carry out insulation and protect
Pressure processes；
The slurry processed through described heat-insulation pressure keeping is carried out solid-liquid separation, and the solid obtaining solid-liquid separation is washed
Wash, be dried, obtain hydrated alumina.
The present inventor finds through numerous studies, is protected by the slurry that industrial aluminium hydroxide is prepared under high-temperature and high-pressure conditions
Temperature pressurize processes, it is possible to make the granularity refinement of product, thus it is speculated that reason may is that industrial aluminium hydroxide is under high-temperature and high-pressure conditions
Crystal lattice recombination reaction occurs, and during crystal lattice recombination, crystal internal stress makes the granularity refinement of product.Based on above-mentioned discovery, from
And complete the present invention.
The primary industry aluminium hydroxide used the most strictly is limited by the present invention, and its median can be 30-200 μ
M, such as 80 μm；Wherein, during median refers to product, cumulative particle sizes percentile reaches particle diameter corresponding when 50%.
Additionally, the content of other impurity reaches industry product prescription in industrial aluminium hydroxide.
In the present invention, the mass ratio of industrial aluminium hydroxide during described mixing with water is the most strictly limited, the most permissible
For 1:(1-100)；For the easy to operate and consideration of economy, generally could be arranged to 1:(3.0-5.0).Additionally, water is permissible
Use distilled water or deionized water.
It is possible to further by described slurry temperature be 180-220 DEG C, absolute pressure be the condition of 1.00-2.30MPa
Under carry out heat-insulation pressure keeping process.The time that described heat-insulation pressure keeping is processed by the present invention the most strictly limits, such as, can be 30-
300min, is 60-180min further.
In the present invention, distilled water or deionized water can be used to carry out described washing；Further, to the consumption of described water not
Make strict restriction, such as, the water of 3-10 times of described solid weight can be used to carry out described washing.
Further, described dry temperature is the most strictly limited, such as, can carry out at a temperature of 100-110 DEG C
Described dry.
In the present invention, can carry out by the holding temperature of slurry, dwell pressure and heat-insulation pressure keeping being processed the time
Control, thus obtain the hydrated alumina of different median；Wherein, the median of hydrated alumina is 1-10 μm；
Additionally, this hydrated alumina is pure phase one diaspore.
Further, it is also possible to described hydrated alumina is carried out grading process, thus obtains particle size distribution more
Narrow hydrated alumina product.
The present invention also provides for the preparation method of a kind of high temperature alumina, to prepare according to any of the above-described described preparation method
Hydrated alumina carries out roasting, obtains high temperature alumina.
In the present invention, can use this area conventional method that hydrated alumina is made high temperature alumina；Particularly,
The temperature that can control described roasting is 1300-1400 DEG C, and the time is 0.5-1.5h.
Further, the median of described high temperature alumina is 1-10 μm.
The preparation method of the present invention uses non-mechanical means to reduce product granularity, thus overcomes conventional mechanical method energy consumption
High, be easily introduced the defects such as impurity；The median of the hydrated alumina prepared is 1-10 μm, and it can be directly as product
Product, it is possible to as the raw materials for production of high temperature alumina, have wide range of applications.
Accompanying drawing explanation
The scanning electron microscope (SEM) photograph of the industrial aluminium hydroxide that Fig. 1 is used by the embodiment of the present invention 1；
The X ray diffracting spectrum of the industrial aluminium hydroxide that Fig. 2 is used by the embodiment of the present invention 1；
Fig. 3 is the process chart of the preparation method of the embodiment of the present invention 1；
Fig. 4 is the scanning electron microscope (SEM) photograph of the hydrated alumina of the embodiment of the present invention 1 preparation；
Fig. 5 is the X ray diffracting spectrum of the hydrated alumina of the embodiment of the present invention 1 preparation；
Fig. 6 is the scanning electron microscope (SEM) photograph of the hydrated alumina of the embodiment of the present invention 2 preparation.
Detailed description of the invention
For making the object, technical solutions and advantages of the present invention clearer, below in conjunction with embodiments of the invention, to this
Technical scheme in inventive embodiments is clearly and completely described, it is clear that described embodiment is that a part of the present invention is real
Execute example rather than whole embodiments.Based on the embodiment in the present invention, those of ordinary skill in the art are not making creation
The every other embodiment obtained under property work premise, broadly falls into the scope of protection of the invention.
Embodiment 1
The present embodiment uses industrial aluminium hydroxide to prepare hydrated alumina as raw material, its scanning electron microscope collection of illustrative plates such as Fig. 1
Shown (Fig. 1 shows that its median D50 is about 80 μm), (Fig. 2 shows that it is pure phase three to X ray diffracting spectrum as shown in Figure 2
, there is not other miscellaneous peak in diaspore), other impurity content reaches industry product prescription.
As it is shown on figure 3, the preparation method of the hydrated alumina of the present embodiment comprises the steps:
1, slurrying
Above-mentioned industrial aluminium hydroxide is mixed homogeneously with distilled water, makes slurry；Wherein, distilled water and industry hydrogen-oxygen are controlled
The mass ratio changing aluminum is about 4.0.
2, heat-insulation pressure keeping processes
Proceeding in high-pressure reactor by above-mentioned slurry, liter high-temperature is to 210 DEG C, and now absolute pressure reaches a 1.9MPa left side
The right side, slurry 210 DEG C, heat-insulation pressure keeping processes about 60min under conditions of 1.9MPa；After process completes, high-pressure reactor is dropped
Temperature is to normal pressure discharging.
3, separate, wash, be dried
The slurry processed through above-mentioned heat-insulation pressure keeping is carried out solid-liquid separation, collects solid (i.e. filter cake), with the steaming of about 6 times
Distilled water washing after, be dried at about 105 DEG C, obtain hydrated alumina, its scanning electron microscope collection of illustrative plates as shown in Figure 4, X-ray
Diffracting spectrum is as shown in Figure 5.
As shown in Figure 4, the median D50 of this hydrated alumina is about 3 μm；As shown in Figure 5, this alumina hydration
Thing is pure phase one diaspore, there is not other miscellaneous peak.
It is possible to further the above-mentioned hydrated alumina prepared is carried out roasting, wherein sintering temperature is 1350
DEG C, the time is 1h, obtains high temperature alumina.After testing, the median of this high temperature alumina is about 3 μm.
Embodiment 2
The preparation method of the hydrated alumina of the present embodiment comprises the steps:
1, slurrying
The industrial aluminium hydroxide of embodiment 1 is mixed homogeneously with distilled water, makes slurry；Wherein, distilled water and work are controlled
The mass ratio of industry aluminium hydroxide is about 5.0.
2, heat-insulation pressure keeping processes
Proceeding in high-pressure reactor by above-mentioned slurry, liter high-temperature is to 180 DEG C, and now absolute pressure reaches a 1.0MPa left side
The right side, slurry 180 DEG C, heat-insulation pressure keeping processes about 60min under conditions of 1.0MPa；After process completes, high-pressure reactor is dropped
Temperature is to normal pressure discharging.
3, separate, wash, be dried
The slurry processed through above-mentioned heat-insulation pressure keeping is carried out solid-liquid separation, collects filter cake, with the distilled water wash of about 4 times
After, be dried at about 100 DEG C, obtain hydrated alumina, its scanning electron microscope collection of illustrative plates as shown in Figure 6, it will be appreciated from fig. 6 that should
The median D50 of hydrated alumina is about 10 μm；Additionally, X ray diffracting spectrum shows that this hydrated alumina is pure
, there is not other miscellaneous peak in a diaspore mutually.
It is possible to further the above-mentioned hydrated alumina prepared is carried out roasting, wherein sintering temperature is 1300
DEG C, the time is 1.5h, obtains high temperature alumina.After testing, the median of this high temperature alumina is about 10 μm.
Embodiment 3
The preparation method of the hydrated alumina of the present embodiment comprises the steps:
1, slurrying
The industrial aluminium hydroxide of embodiment 1 is mixed homogeneously with distilled water, makes slurry；Wherein, distilled water and work are controlled
The mass ratio of industry aluminium hydroxide is about 3.0.
2, heat-insulation pressure keeping processes
Proceeding in high-pressure reactor by above-mentioned slurry, liter high-temperature is to 200 DEG C, and now absolute pressure reaches a 1.55MPa left side
The right side, slurry 200 DEG C, heat-insulation pressure keeping processes about 100min under conditions of 1.55MPa；After process completes, by high-pressure reactor
It is cooled to normal pressure discharging.
3, separate, wash, be dried
The slurry processed through above-mentioned heat-insulation pressure keeping is carried out solid-liquid separation, collects filter cake, wash with the distillations of about 10 times
After washing, it is dried at about 110 DEG C, obtains hydrated alumina, scanned Electronic Speculum and X-ray diffraction detection and understand, this oxygen
The median D50 changing aluminum hydrate is about 5 μm, and is pure phase one diaspore, there is not other miscellaneous peak.
It is possible to further the above-mentioned hydrated alumina prepared is carried out roasting, wherein sintering temperature is 1400
DEG C, the time is 0.5h, obtains high temperature alumina.After testing, the median of this high temperature alumina is about 5 μm.
Last it is noted that various embodiments above is only in order to illustrate technical scheme, it is not intended to limit；To the greatest extent
The present invention has been described in detail by pipe with reference to foregoing embodiments, it will be understood by those within the art that: it depends on
So the technical scheme described in foregoing embodiments can be modified, or the most some or all of technical characteristic is entered
Row equivalent；And these amendments or replacement, do not make the essence of appropriate technical solution depart from various embodiments of the present invention technology
The scope of scheme.
Claims (10)
1. the preparation method of a hydrated alumina, it is characterised in that comprise the steps:
Industrial aluminium hydroxide is mixed with water, prepares slurry；
By described slurry temperature be 150-300 DEG C, absolute pressure be 0.47-8.50MPa under conditions of carry out at heat-insulation pressure keeping
Reason；
The slurry processed through described heat-insulation pressure keeping is carried out solid-liquid separation, and the solid obtaining solid-liquid separation washs, dry
Dry, obtain hydrated alumina.
Preparation method the most according to claim 1, it is characterised in that the median of described industrial aluminium hydroxide is 30-
200μm。
Preparation method the most according to claim 1, it is characterised in that described mixing time, control industrial aluminium hydroxide with
The mass ratio of water is 1:(1-100).
Preparation method the most according to claim 1, it is characterised in that the time controlling the process of described heat-insulation pressure keeping is 30-
300min。
Preparation method the most according to claim 1, it is characterised in that use the water of 3-10 times of described solid weight to carry out institute
State washing.
Preparation method the most according to claim 1, it is characterised in that carry out described being dried at a temperature of 100-110 DEG C.
Preparation method the most according to claim 1, it is characterised in that the median of described hydrated alumina is 1-10
μm。
8. the preparation method of a high temperature alumina, it is characterised in that to according to the arbitrary described preparation method of claim 1 to 7
The hydrated alumina of preparation carries out roasting, obtains high temperature alumina.
Preparation method the most according to claim 8, it is characterised in that the temperature of described roasting is 1300-1400 DEG C, the time
For 0.5-1.5h.
Preparation method the most according to claim 8, it is characterised in that the median of described high temperature alumina is 1-10 μ
m。
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610572002.7A CN106186011A (en) | 2016-07-18 | 2016-07-18 | Hydrated alumina and the preparation method of high temperature alumina |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610572002.7A CN106186011A (en) | 2016-07-18 | 2016-07-18 | Hydrated alumina and the preparation method of high temperature alumina |
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| CN106186011A true CN106186011A (en) | 2016-12-07 |
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| CN201610572002.7A Pending CN106186011A (en) | 2016-07-18 | 2016-07-18 | Hydrated alumina and the preparation method of high temperature alumina |
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20100040536A1 (en) * | 2008-08-18 | 2010-02-18 | Fujimi Incorporated | Method for producing boehmite particles and method for producing alumina particles |
| CN102320638A (en) * | 2011-08-04 | 2012-01-18 | 中国铝业股份有限公司 | Preparation method of low-sodium fine grain alumina |
| US20120289653A1 (en) * | 2004-09-07 | 2012-11-15 | Nissan Motor Co., Ltd. | Alumina particle composite, method of manufacturing the alumina particle composite, resin composition and method of manufacturing the resin composition |
| CN104944454A (en) * | 2015-06-12 | 2015-09-30 | 安徽壹石通材料科技股份有限公司 | Granularity-controllable boehmite preparation method |
-
2016
- 2016-07-18 CN CN201610572002.7A patent/CN106186011A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20120289653A1 (en) * | 2004-09-07 | 2012-11-15 | Nissan Motor Co., Ltd. | Alumina particle composite, method of manufacturing the alumina particle composite, resin composition and method of manufacturing the resin composition |
| US20100040536A1 (en) * | 2008-08-18 | 2010-02-18 | Fujimi Incorporated | Method for producing boehmite particles and method for producing alumina particles |
| CN102320638A (en) * | 2011-08-04 | 2012-01-18 | 中国铝业股份有限公司 | Preparation method of low-sodium fine grain alumina |
| CN104944454A (en) * | 2015-06-12 | 2015-09-30 | 安徽壹石通材料科技股份有限公司 | Granularity-controllable boehmite preparation method |
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