CN104045100A - Preparation method of aluminum hydroxide - Google Patents
Preparation method of aluminum hydroxide Download PDFInfo
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- CN104045100A CN104045100A CN201410293652.9A CN201410293652A CN104045100A CN 104045100 A CN104045100 A CN 104045100A CN 201410293652 A CN201410293652 A CN 201410293652A CN 104045100 A CN104045100 A CN 104045100A
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Abstract
The invention relates to a preparation method of aluminum hydroxide, particularly a preparation method of high-dispersity superfine aluminum hydroxide. The method is characterized by comprising the following steps: carrying out two-stage seed decomposition by using nano active aluminum hydroxide prepared by the reaction between a sodium aluminate solution and an aluminum sulfate solution as a seed, carrying out solid-liquid separation and washing on the obtained decomposition pulp, and carrying out mechanical stirring and grinding to prepare the superfine aluminum hydroxide. The superfine aluminum hydroxide prepared by the method has complete crystal form, effectively solves the problem of aggregation of the superfine aluminum hydroxide, and solves the problem of secondary granularity caused by aggregation; and the method enhances the dispersity of the superfine aluminum hydroxide, and lowers the oil absorption number of the superfine aluminum hydroxide to 28-32ml/100g.
Description
Technical field
A preparation method for aluminium hydroxide, relates to the ultrafine aluminium hydroxide preparation method that a kind of dispersiveness is high.
Background technology
At present, the production technique of ultrafine aluminium hydroxide mainly contains two kinds: a kind of be by ordinary hydrogen alumina lap to 2-5.0 μ m, directly as ultrafine aluminium hydroxide, use; Another kind of technique adopts crystal seed kind to divide decomposition technique exactly, the preparation of seed can often adopt acid-base neutralisation method, by preparation gel aluminium hydroxide as crystal seed, directly be dissolved in sodium aluminate solution, improve the degree of supersaturation of solution and carry out decomposition of crystal seed, the ultrafine aluminium hydroxide agglomeration that it decomposites is serious.Although the ultrafine aluminium hydroxide that ultrafine aluminium hydroxide application performance prepared by kind minute decomposition technique is prepared apparently higher than grinding technics, its oil-absorption(number) height is still very high.
Summary of the invention
Object of the present invention is exactly the deficiency existing for above-mentioned prior art, and a kind of preparation method that can effectively reduce agglomeration, reduce the ultrafine aluminium hydroxide of oil-absorption(number), good dispersity is provided.
The object of the invention is to be achieved through the following technical solutions.
A kind of preparation method of aluminium hydroxide, it is characterized in that its preparation process is that the nano active aluminium hydroxide that adopts sodium aluminate solution to react with alum liquor to prepare is as seed, carry out two sections of kind decomposition, the decomposition slurries of gained are carried out to solid-liquid separation, washing, through mechanical stirring mill, grind again, prepare ultra-fine aluminium hydroxide.
The preparation method of a kind of aluminium hydroxide of the present invention, it is characterized in that described sodium aluminate solution and alum liquor reaction process be by temperature at 40 ℃-80 ℃, concentration under the industrial sodium aluminate solution of 30g/L-180g/L and the alum liquor condition of 40-100g/L, carry out neutralization reaction, pH value is controlled at 10-14, reaction times 10-30 minute, prepares nano level active aluminium hydroxide crystal seed.
The preparation method of a kind of aluminium hydroxide of the present invention, it is characterized in that one section of decomposition reaction process in two sections of described kind decomposition is using the nano active aluminium hydroxide of preparation as seed, join and in sodium aluminate solution, carry out decomposition of crystal seed, decomposition temperature is controlled at 40 ℃ of-65 ℃ of temperature, one section of decomposition seed compares 10%-30%, decompose 2-10 hour, rate of decomposition is controlled at 40%-60%.
The preparation method of a kind of aluminium hydroxide of the present invention, it is characterized in that two sections of decomposition reaction processes in two sections of described kind decomposition are that one section of slurries after decomposition joins in sodium aluminate solution, temperature is controlled at 40 ℃-65 ℃, all seed compares 0.5%-5%, decompose 5-20 hour, rate of decomposition is controlled at 40%-60%, decomposes granularity and is controlled at 2.5-3.5 μ m.
The preparation method of a kind of aluminium hydroxide of the present invention, is characterized in that two sections of decomposition reactions have slurries through solid-liquid separation, washing, obtain water content at 30%-70% wet cake.
The preparation method of a kind of aluminium hydroxide of the present invention, is characterized in that filter cake adds dispersion agent, in wet srirred mill grinding distribution to particle diameter D (50) be 1.7-1.9 μ m.
The preparation method of a kind of aluminium hydroxide of the present invention, the slip that the it is characterized in that grinding distribution oven dry of spraying, obtains the ultrafine aluminium hydroxide of low oil-absorption(number), high degree of dispersion.
The preparation method of a kind of aluminium hydroxide of the present invention, efficiently solves the problem that ultrafine aluminium hydroxide is reunited, and makes the oil-absorption(number) of ultrafine aluminium hydroxide be reduced to 28-32ml/100g.The nano active aluminium hydroxide of preparing of usining is planted a minute decomposition as seed, improved the monocrystalline granularity of ultrafine aluminium hydroxide, make the granularity of the ultrafine aluminium hydroxide that decomposites be increased to 2.5-3.5 μ m, and then grind and make ultrafine aluminium hydroxide granularity reach 1.7-1.9 μ m, solved the secondary granularity of reuniting and causing, the dispersing property that improves ultrafine aluminium hydroxide, the product oil-absorption(number) of preparation reaches 28-32ml/100g.
Accompanying drawing explanation
The Electronic Speculum figure that Fig. 1 is the low oil-absorption(number) ultrafine aluminium hydroxide that adopts method of the present invention and prepare.
Embodiment
A kind of preparation method of aluminium hydroxide, its preparation process is that the nano active aluminium hydroxide that adopts sodium aluminate solution to react with alum liquor to prepare is as seed, carry out two sections of kind decomposition, the decomposition slurries of gained are carried out to solid-liquid separation, washing, through mechanical stirring mill, grind again, prepare ultra-fine aluminium hydroxide.The step of its preparation process comprises:
A. by temperature at 40 ℃-80 ℃, concentration under the industrial sodium aluminate solution of 30g/L-180g/L and the condition of alum liquor 40-100g/L, carry out neutralization reaction, pH value is controlled at 10-14, and reaction times 10-30 minute prepares nano level active aluminium hydroxide crystal seed.
B. the nano active aluminium hydroxide of being prepared by step a, as seed, joins in sodium aluminate solution and carries out decomposition of crystal seed, and decomposition temperature is controlled at 40 ℃ of-65 ℃ of temperature, one section of decomposition seed than 10%-30%, decomposes 2-10 hour, and rate of decomposition is controlled at 40%-60%.
C. one section of slurries after step b being decomposed join in sodium aluminate solution, and temperature is controlled at 40 ℃-65 ℃, all seed, than 0.5%-5%, decomposes 5-20 hour, and rate of decomposition is controlled at 40%-60%, decomposes granularity and is controlled at 2.5-3.5 μ m.
D. step c is decomposed to qualified slurries, through solid-liquid separation, washing, obtain water content at 30%-70% wet cake.
E. the filter cake of steps d is added to dispersion agent, grinding distribution certain hour in wet srirred mill, particle diameter D (5,0) is controlled at 1.7-1.9 μ m.
F. the qualified slip of grinding step e the being obtained oven dry of spraying, obtains the ultrafine aluminium hydroxide of low oil-absorption(number), high degree of dispersion.The product oil-absorption(number) of preparation reaches 28-32ml/100g.
Embodiment 1
(1) alum liquor is mixed according to a certain percentage with sodium aluminate solution under violent stirring, temperature of reaction is controlled to 80 ℃, pH value is 12, reacts 30 minutes, prepares nano level active aluminium hydroxide crystal seed.
(2) step (1) is joined in sodium aluminate solution and decomposed, decomposition temperature is controlled at 50 ℃, and seed is than 1%, decomposes 8h, and minute parsing aluminium hydroxide particle diameter is 3.00 μ m.
(3) step (2) is carried out to solid-liquid separation, filter cake washing.
(4) by washing, the filter cake water capacity after qualified is 50%, adds 1.5 ‰ dispersion agent to pull an oar, and then press the material ball ratio of 1:2, grinds 3 minutes in wet srirred mill, and grinding particle diameter is afterwards 1.70 μ m.
(5) after spraying is dried, the ultrafine aluminium hydroxide oil-absorption(number) obtaining is 30ml/100g.
Embodiment 2
(1) alum liquor is mixed according to a certain percentage with sodium aluminate solution under violent stirring, temperature of reaction is controlled to 70 ℃, pH value is 13, reacts 30 minutes, prepares nano level active aluminium hydroxide crystal seed.
(2) step (1) is joined in sodium aluminate solution and decomposed, decomposition temperature is controlled at 55 ℃, and seed is than 1.5%, decomposes 8h, and minute parsing aluminium hydroxide particle diameter is 2.80 μ m.
(3) step (2) is carried out to solid-liquid separation, filter cake washing.
(4) by washing, the filter cake water capacity after qualified is 55%, adds 1.5 ‰ dispersion agent to pull an oar, and then press the material ball ratio of 1:2, grinds 5 minutes in wet srirred mill, and grinding particle diameter is afterwards 1.70 μ m.
(5) after spraying is dried, the ultrafine aluminium hydroxide oil-absorption(number) obtaining is 31ml/100g.
Embodiment 3
(1) alum liquor is mixed according to a certain percentage with sodium aluminate solution under violent stirring, temperature of reaction is controlled to 60 ℃, pH value is 14, reacts 30 minutes, prepares nano level active aluminium hydroxide crystal seed.
(2) step (1) is joined in sodium aluminate solution and decomposed, decomposition temperature is controlled at 60 ℃, and seed is than 1.5%, decomposes 8h, and minute parsing aluminium hydroxide particle diameter is 3.20 μ m.
(3) step (2) is carried out to solid-liquid separation, filter cake washing.
(4) by washing, the filter cake water capacity after qualified is 55%, adds 2.0 ‰ dispersion agent to pull an oar, and then press the material ball ratio of 1:2, grinds 3 minutes in wet srirred mill, and grinding particle diameter is afterwards 1.80 μ m.
(5) after spraying is dried, the ultrafine aluminium hydroxide oil-absorption(number) obtaining is 30ml/100g.
Embodiment 4
(1) alum liquor is mixed according to a certain percentage with sodium aluminate solution under violent stirring, temperature of reaction is controlled to 70 ℃, pH value is 14, reacts 30 minutes, prepares nano level active aluminium hydroxide crystal seed.
(2) step (1) is joined in sodium aluminate solution and decomposed, decomposition temperature is controlled at 60 ℃, and seed is than 2.0%, decomposes 8h, and minute parsing aluminium hydroxide particle diameter is 3.50 μ m.
(3) step (2) is carried out to solid-liquid separation, filter cake washing.
(4) by washing, the filter cake water capacity after qualified is 45%, adds 1.5 ‰ dispersion agent to pull an oar, and then press the material ball ratio of 1:2, grinds 5.0 minutes in wet srirred mill, and grinding particle diameter is afterwards 1.90 μ m.
(5) after spraying is dried, the ultrafine aluminium hydroxide oil-absorption(number) obtaining is 29ml/100g.
Claims (7)
1. the preparation method of an aluminium hydroxide, it is characterized in that its preparation process is that the nano active aluminium hydroxide that adopts sodium aluminate solution to react with alum liquor to prepare is as seed, carry out two sections of kind decomposition, the decomposition slurries of gained are carried out to solid-liquid separation, washing, through mechanical stirring mill, grind again, prepare ultra-fine aluminium hydroxide.
2. the preparation method of a kind of aluminium hydroxide according to claim 1, it is characterized in that described sodium aluminate solution and alum liquor reaction process be by temperature at 40 ℃-80 ℃, concentration under the industrial sodium aluminate solution of 30g/L-180g/L and the alum liquor condition of 40-100g/L, carry out neutralization reaction, pH value is controlled at 10-14, reaction times 10-30 minute, prepares nano level active aluminium hydroxide crystal seed.
3. the preparation method of a kind of aluminium hydroxide according to claim 1, it is characterized in that one section of decomposition reaction process in two sections of described kind decomposition is using the nano active aluminium hydroxide of preparation as seed, join and in sodium aluminate solution, carry out decomposition of crystal seed, decomposition temperature is controlled at 40 ℃ of-65 ℃ of temperature, one section of decomposition seed compares 10%-30%, decompose 2-10 hour, rate of decomposition is controlled at 40%-60%.
4. the preparation method of a kind of aluminium hydroxide according to claim 1, it is characterized in that two sections of decomposition reaction processes in two sections of described kind decomposition are that one section of slurries after decomposition joins in sodium aluminate solution, temperature is controlled at 40 ℃-65 ℃, all seed compares 0.5%-5%, decompose 5-20 hour, rate of decomposition is controlled at 40%-60%, decomposes granularity and is controlled at 2.5-3.5 μ m.
5. the preparation method of a kind of aluminium hydroxide according to claim 1, is characterized in that two sections of decomposition reactions have slurries through solid-liquid separation, washing, obtain water content at 30%-70% wet cake.
6. the preparation method of a kind of aluminium hydroxide according to claim 1, is characterized in that filter cake adds dispersion agent, in wet srirred mill grinding distribution to particle diameter D (50) be 1.7-1.9 μ m.
7. the preparation method of a kind of aluminium hydroxide according to claim 1, the slip that the it is characterized in that grinding distribution oven dry of spraying, obtains the ultrafine aluminium hydroxide of low oil-absorption(number), high degree of dispersion.
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Cited By (10)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN104760979A (en) * | 2015-03-20 | 2015-07-08 | 河南能源化工集团研究院有限公司 | Preparation technology of highly pure alumina powder |
| CN107265487A (en) * | 2017-06-15 | 2017-10-20 | 郑州中绿环保新材料有限公司 | A kind of method that use solid sodium aluminate produces special aluminium hydroxide product |
| CN108341422A (en) * | 2018-05-16 | 2018-07-31 | 洛阳中超新材料股份有限公司 | Rodlike β-aluminium hydroxide and its preparation method and application |
| CN108569714A (en) * | 2018-04-17 | 2018-09-25 | 郝亚明 | It improves and decomposes aluminium hydroxide micro powder resolution ratio method |
| CN108862341A (en) * | 2018-09-06 | 2018-11-23 | 中铝矿业有限公司 | A kind of technique of two-stage method production ultrafine aluminium hydroxide |
| CN109422285A (en) * | 2017-08-30 | 2019-03-05 | 洛阳中超新材料股份有限公司 | Low oil factor aluminium hydroxide and its preparation method and application |
| CN114655974A (en) * | 2022-04-01 | 2022-06-24 | 中铝中州铝业有限公司 | Preparation method of submicron small primary crystal alpha aluminum oxide for CMP (chemical mechanical polishing) polishing solution |
| CN115818681A (en) * | 2022-12-12 | 2023-03-21 | 洛阳中超新材料股份有限公司 | Method for preparing single crystal large-particle aluminum hydroxide by one-stage method |
| CN116102041A (en) * | 2023-01-30 | 2023-05-12 | 中铝山东有限公司 | Preparation method of low-sodium low-oil-absorption superfine aluminum hydroxide |
| CN116143152A (en) * | 2022-12-23 | 2023-05-23 | 清远市普塞呋磷化学有限公司 | Superfine aluminum hydroxide and preparation method and application thereof |
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Cited By (14)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104760979B (en) * | 2015-03-20 | 2016-08-17 | 河南能源化工集团研究院有限公司 | A kind of preparation technology of high-purity alumina powder |
| CN104760979A (en) * | 2015-03-20 | 2015-07-08 | 河南能源化工集团研究院有限公司 | Preparation technology of highly pure alumina powder |
| CN107265487A (en) * | 2017-06-15 | 2017-10-20 | 郑州中绿环保新材料有限公司 | A kind of method that use solid sodium aluminate produces special aluminium hydroxide product |
| CN107265487B (en) * | 2017-06-15 | 2019-04-19 | 郑州中绿环保新材料有限公司 | A method of special aluminium hydroxide product is produced using solid sodium aluminate |
| CN109422285A (en) * | 2017-08-30 | 2019-03-05 | 洛阳中超新材料股份有限公司 | Low oil factor aluminium hydroxide and its preparation method and application |
| CN108569714A (en) * | 2018-04-17 | 2018-09-25 | 郝亚明 | It improves and decomposes aluminium hydroxide micro powder resolution ratio method |
| CN108341422A (en) * | 2018-05-16 | 2018-07-31 | 洛阳中超新材料股份有限公司 | Rodlike β-aluminium hydroxide and its preparation method and application |
| CN108341422B (en) * | 2018-05-16 | 2020-07-03 | 洛阳中超新材料股份有限公司 | Rod-shaped β -aluminum hydroxide and preparation method and application thereof |
| CN108862341A (en) * | 2018-09-06 | 2018-11-23 | 中铝矿业有限公司 | A kind of technique of two-stage method production ultrafine aluminium hydroxide |
| CN114655974A (en) * | 2022-04-01 | 2022-06-24 | 中铝中州铝业有限公司 | Preparation method of submicron small primary crystal alpha aluminum oxide for CMP (chemical mechanical polishing) polishing solution |
| CN115818681A (en) * | 2022-12-12 | 2023-03-21 | 洛阳中超新材料股份有限公司 | Method for preparing single crystal large-particle aluminum hydroxide by one-stage method |
| CN115818681B (en) * | 2022-12-12 | 2024-01-23 | 洛阳中超新材料股份有限公司 | Method for preparing large-particle monocrystalline aluminum hydroxide by one-stage method |
| CN116143152A (en) * | 2022-12-23 | 2023-05-23 | 清远市普塞呋磷化学有限公司 | Superfine aluminum hydroxide and preparation method and application thereof |
| CN116102041A (en) * | 2023-01-30 | 2023-05-12 | 中铝山东有限公司 | Preparation method of low-sodium low-oil-absorption superfine aluminum hydroxide |
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Application publication date: 20140917 |