CN106277003A - A kind of preparation method of high pure and ultra-fine nano-aluminum hydroxide - Google Patents
A kind of preparation method of high pure and ultra-fine nano-aluminum hydroxide Download PDFInfo
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- CN106277003A CN106277003A CN201610613630.5A CN201610613630A CN106277003A CN 106277003 A CN106277003 A CN 106277003A CN 201610613630 A CN201610613630 A CN 201610613630A CN 106277003 A CN106277003 A CN 106277003A
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- preparation
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- high pure
- aluminum hydroxide
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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
- C01F7/42—Preparation of aluminium oxide or hydroxide from metallic aluminium, e.g. by oxidation
- C01F7/426—Preparation of aluminium oxide or hydroxide from metallic aluminium, e.g. by oxidation by applying mechanical energy to solid aluminium at a low temperature
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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
- C01P2006/80—Compositional purity
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- Organic Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Mechanical Engineering (AREA)
- Life Sciences & Earth Sciences (AREA)
- Geology (AREA)
- Inorganic Chemistry (AREA)
- Compounds Of Alkaline-Earth Elements, Aluminum Or Rare-Earth Metals (AREA)
Abstract
The invention belongs to high pure and ultra-fine nano-aluminum hydroxide preparation field, in particular it relates to the preparation method of a kind of high pure and ultra-fine nano-aluminum hydroxide.The preparation method of high pure and ultra-fine nano-aluminum hydroxide of the present invention, comprises the following steps: 1) activated aluminum powder that granularity D50 is 15 30 μm is mixed with water；2) using the purity of granularity D50≤1 μm more than 99.995% aluminium oxide as crystal seed, be added into step 1) acquisition mixture in；3) use ultrasound wave to step 2) obtain mixed material disperse, after reaction, prepare high pure and ultra-fine nano-aluminum hydroxide.Present invention introduces alumina in Nano level as crystal seed, reaction efficiency can be improved when reaction, make the material of 80% can be converted into aluminium hydroxide in the short time.The reactor paddle reciprocation cycle stirring of the present invention, is possible to prevent the reunion of large granular materials.The application of the ultra-high frequency ultrasonic wave of the present invention, makes aluminium hydroxide molecule be constantly in kinestate, plays good peptizaiton.
Description
Technical field
The invention belongs to high pure and ultra-fine nano-aluminum hydroxide preparation field, in particular it relates to a kind of high pure and ultra-fine nanometer hydrogen
The preparation method of aluminium oxide.
Background technology
The technique of domestic production aluminium hydroxide has alkoxide process, improvement Bayer process, direct hydrolysis method etc. at present.Alkoxide process produces
Cost is high, is unfavorable for the market competition；The product purity that improvement Bayer process produces only up to reach 99.99%, does not prepares super
Cross 99.99% aluminium hydroxide；It is big that the aluminum hydroxide particles that direct hydrolysis method produces depends on that early stage prepares the granule of activated aluminum powder
Little, the relatively big so later stage aluminum hydroxide particles of early stage activated aluminum powder granule also can become big, is unfavorable for producing nano-aluminum hydroxide；Again
Needed for person's direct hydrolysis method, the cycle is taken 3-5 days time aluminium powder just can be made to be fully converted to aluminium hydroxide, and reaction time is long, efficiency
Low.
Summary of the invention
It is an object of the invention to, not enough for prior art, it is provided that the preparation side of a kind of high pure and ultra-fine nano-aluminum hydroxide
Method.Technique is adjusted on the Process ba-sis of direct hydrolysis method by the present invention, produces purity higher, and granule is little, produces week
The aluminium hydroxide that phase is short.
The preparation method of the high pure and ultra-fine nano-aluminum hydroxide of the present invention, comprises the following steps:
1) activated aluminum powder that granularity D50 is 15-30 μm is mixed with water；
2) using the purity of granularity D50≤1um more than 99.995% aluminium oxide as crystal seed, be added into step 1) obtain
Mixture in；
3) use ultrasound wave to step 2) obtain mixed material disperse, after reaction, prepare high pure and ultra-fine nanometer hydrogen-oxygen
Change aluminum.
Preparation in accordance with the present invention, wherein, step 1) mass ratio of described activated aluminum powder and water is 1:8-1:12.
Preparation in accordance with the present invention, wherein, step 2) quality of described addition crystal seed is activated aluminum powder quality
1%-5%.
Preparation in accordance with the present invention, the most preferably, step 3) described supersonic frequency controls at 40-100kHz.
Preparation in accordance with the present invention, as preferably, step 3) described reaction temperature between 85-95 DEG C, reaction
Time 24-48h.
Preparation in accordance with the present invention, wherein, step 3) reaction carries out in a kettle., described reactor paddle with
40-80 turns/and min, 1-5min be a cycle reciprocation cycle stirring.
Preparation in accordance with the present invention, step 1) described water is preferably deionized water.
Granularity D50 of the high pure and ultra-fine nano-aluminum hydroxide that the present invention prepares up to 500nm-1 μm, purity up to
More than 99.99%.
The invention have the advantages that
1, present invention introduces alumina in Nano level as crystal seed, reaction efficiency can be improved when reaction, make material front
During phase reaction more acutely more rapidly, the material of 80% is made can be converted into aluminium hydroxide in the short time.
2, the reactor paddle reciprocation cycle stirring of the present invention, can make the material in still collide with each other, cut, prevent
The reunion of large granular materials.
3, the application of the ultra-high frequency ultrasonic wave of the present invention, makes aluminium hydroxide molecule be constantly in kinestate, plays very well
Peptizaiton.
Detailed description of the invention
The present invention is expanded on further by the following examples, and these embodiments are only used for the purpose illustrated, not
Limit the scope of the present invention.The test method of unreceipted actual conditions in the following example, generally according to normal condition.
Embodiment 1
With the activated aluminum powder of direct hydrolysis method prepared sizes D50:20 μm as the raw material of the aluminium hydroxide produced, according to aluminum
Powder and pure water mass ratio 1:10 mixing are put in reactor, the oxygen more than 99.995% by granularity D50:500nm and purity
Change aluminum is as crystal seed, and it is 4% that crystal seed adds the ratio of quality and aluminium powder quality.Reactor paddle with 70 turns/min, 4min be
One cycle reciprocation cycle stirring, reactor heating-up temperature 85 DEG C；The ultrasound wave of use high-power high-frequency rate meanwhile is to molten
Liquid disperses, and supersonic frequency controls at 85kHz.Material starts after reaction after 24h, to separate the most permissible through solid-liquid filtration device
Obtain the granularity D50 aluminium hydroxide at 700nm.
Embodiment 2
With the activated aluminum powder of direct hydrolysis method prepared sizes D50:25 μm as the raw material of the aluminium hydroxide produced, according to aluminum
Powder and pure water mass ratio 1:8 mixing are put in reactor, the oxidation more than 99.995% by granularity D50:800nm and purity
Aluminum is as crystal seed, and it is 2% that crystal seed adds the ratio of quality and aluminium powder quality.Reactor paddle with 50 turns/min, 2min be for one
Cycle reciprocation cycle stirs, reactor heating-up temperature 95 DEG C；The ultrasound wave of use high-power high-frequency rate meanwhile is to solution
Disperseing, supersonic frequency controls at 60kHz.Material starts after reaction after 24h, to separate through solid-liquid filtration device and just can obtain
To granularity D50 at the aluminium hydroxide of 900nm.
Embodiment 3
With the activated aluminum powder of direct hydrolysis method prepared sizes D50:15 μm as the raw material of the aluminium hydroxide produced, according to aluminum
Powder and pure water mass ratio 1:8 mixing are put in reactor, the oxidation more than 99.995% by granularity D50:900nm and purity
Aluminum is as crystal seed, and it is 1% that crystal seed adds the ratio of quality and aluminium powder quality.Reactor paddle with 40 turns/min, 5min be for one
Cycle reciprocation cycle stirs, reactor heating-up temperature 90 DEG C；The ultrasound wave of use high-power high-frequency rate meanwhile is to solution
Disperseing, supersonic frequency controls at 40kHz.Material starts after reaction after 36h, to separate through solid-liquid filtration device and just can obtain
To granularity D50 at the aluminium hydroxide of 1000nm.
Embodiment 4
With the activated aluminum powder of direct hydrolysis method prepared sizes D50:30 μm as the raw material of the aluminium hydroxide produced, according to aluminum
Powder and pure water mass ratio 1:12 mixing are put in reactor, the oxygen more than 99.995% by granularity D50:500nm and purity
Change aluminum is as crystal seed, and it is 5% that crystal seed adds the ratio of quality and aluminium powder quality.Reactor paddle with 80 turns/min, 1min be
One cycle reciprocation cycle stirring, reactor heating-up temperature 85 DEG C；The ultrasound wave of use high-power high-frequency rate meanwhile is to molten
Liquid disperses, and supersonic frequency controls at 100kHz.Material starts after reaction after 48h, to separate through solid-liquid filtration device and just may be used
To obtain the granularity D50 aluminium hydroxide at 600nm.
Certainly, the present invention can also have various embodiments, in the case of without departing substantially from present invention spirit and essence thereof, is familiar with
Those skilled in the art can make various corresponding change and deformation according to disclosure of the invention, but these change accordingly and
Deformation all should belong to the scope of the claims of the present invention.
Claims (8)
1. a preparation method for high pure and ultra-fine nano-aluminum hydroxide, comprises the following steps:
1) activated aluminum powder that granularity D50 is 15-30 μm is mixed with water；
2) using the purity of the granularity D50≤1 μm aluminium oxide more than 99.995% as crystal seed, be added into step 1) obtain mixed
In compound；
3) use ultrasound wave to step 2) obtain mixed material disperse, after reaction, prepare high pure and ultra-fine nano-aluminum hydroxide.
Preparation method the most according to claim 1, it is characterised in that step 1) described activated aluminum powder and the mass ratio of water
For 1:8-1:12.
Preparation method the most according to claim 1, it is characterised in that step 2) quality of described addition crystal seed is activated aluminum
The 1%-5% of opaque amount.
Preparation method the most according to claim 1, it is characterised in that step 3) described supersonic frequency controls at 40-
100kHz。
Preparation method the most according to claim 1, it is characterised in that step 3) described reaction temperature between 85-95 DEG C,
Response time 24-48h.
6. according to the arbitrary described preparation method of claim 1-5, it is characterised in that step 3) reaction carries out in a kettle.,
Described reactor paddle with 40-80 turn/min, 1-5min be one cycle reciprocation cycle stirring.
7. according to the arbitrary described preparation method of claim 1-6, it is characterised in that step 1) described water is deionized water.
8. according to the arbitrary described preparation method of claim 1-6, it is characterised in that step 3) the high pure and ultra-fine nanometer hydrogen for preparing
Granularity D50 of aluminium oxide is in 500nm-1 μm.
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| CN201610613630.5A CN106277003A (en) | 2016-07-29 | 2016-07-29 | A kind of preparation method of high pure and ultra-fine nano-aluminum hydroxide |
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| CN201610613630.5A CN106277003A (en) | 2016-07-29 | 2016-07-29 | A kind of preparation method of high pure and ultra-fine nano-aluminum hydroxide |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113620328A (en) * | 2021-08-17 | 2021-11-09 | 苏瓷纳米技术(苏州)有限公司 | Preparation method of nano alumina seed crystal and preparation method of high-purity alumina nanocrystal |
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| CN1394807A (en) * | 2002-07-09 | 2003-02-05 | 刘明 | Preparation method of high-purity superfine alumina powder body |
| CN101362604A (en) * | 2007-08-11 | 2009-02-11 | 陈勇 | High purity alumina powder preparation method |
| CN102107899A (en) * | 2011-01-11 | 2011-06-29 | 上海理工大学 | Preparation method of lamellar gamma-phase nano aluminum oxide |
| CN103787395A (en) * | 2014-01-21 | 2014-05-14 | 江苏大学 | Method for preparing micron-sized ultra-high-purity aluminum oxide powder by virtue of full-process regulation control |
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| CN105347378A (en) * | 2015-10-13 | 2016-02-24 | 刘冠华 | Preparation method for alumina powder, and alumina powder |
| RU2577832C1 (en) * | 2014-12-15 | 2016-03-20 | Федеральное государственное бюджетное учреждение науки Институт химии и технологии редких элементов и минерального сырья им. И.В. Тананаева Кольского научного центра Российской академии наук (ИХТРЭМС КНЦ РАН) | Method for producing aluminum hydroxide |
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2016
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| CN101362604A (en) * | 2007-08-11 | 2009-02-11 | 陈勇 | High purity alumina powder preparation method |
| CN102107899A (en) * | 2011-01-11 | 2011-06-29 | 上海理工大学 | Preparation method of lamellar gamma-phase nano aluminum oxide |
| CN103787395A (en) * | 2014-01-21 | 2014-05-14 | 江苏大学 | Method for preparing micron-sized ultra-high-purity aluminum oxide powder by virtue of full-process regulation control |
| CN104386723A (en) * | 2014-11-07 | 2015-03-04 | 南京福皓晶体材料科技有限公司 | Preparation method of high-purity aluminum oxide |
| RU2577832C1 (en) * | 2014-12-15 | 2016-03-20 | Федеральное государственное бюджетное учреждение науки Институт химии и технологии редких элементов и минерального сырья им. И.В. Тананаева Кольского научного центра Российской академии наук (ИХТРЭМС КНЦ РАН) | Method for producing aluminum hydroxide |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113620328A (en) * | 2021-08-17 | 2021-11-09 | 苏瓷纳米技术(苏州)有限公司 | Preparation method of nano alumina seed crystal and preparation method of high-purity alumina nanocrystal |
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