CN105836770B - A kind of preparation method of high temperature resistant boehmite - Google Patents
A kind of preparation method of high temperature resistant boehmite Download PDFInfo
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- CN105836770B CN105836770B CN201610172756.3A CN201610172756A CN105836770B CN 105836770 B CN105836770 B CN 105836770B CN 201610172756 A CN201610172756 A CN 201610172756A CN 105836770 B CN105836770 B CN 105836770B
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- boehmite
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- C01F7/00—Compounds of aluminium
- C01F7/02—Aluminium oxide; Aluminium hydroxide; Aluminates
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Abstract
The invention discloses a kind of preparation method of high temperature resistant boehmite, aluminum contained compound and aquation are starched, add seed content and washing assisant, it is fitted into after well mixed in autoclave, it is 1~3 DEG C/min to control programming rate, at 150~250 DEG C, is cooled after reacting 2~6h, after separating, washing, drying, high temperature resistant boehmite is obtained.Preparation method of the present invention is simple, and production capacity is big, and production cost is low, and the boehmite conversion rate of preparation is high, and distribution of particles is concentrated, and 1% dehydration temperaturre reaches more than 350 DEG C, and chemical purity is high, the μ s/cm of electrical conductivity≤25.
Description
Technical field
The present invention relates to material to prepare synthesis technical field, and in particular to a kind of preparation method of high temperature resistant boehmite.
Background technology
Boehmite (Boehmite), also known as boehmite, boehmite etc., chemical formula are AlOOH or Al2O3·H2O,
It is not soluble in water, soda acid is insoluble in, its powder has very extensive application value.
The preparation method of boehmite, lot of domestic and international patent document are all reported, for example, described in US 4797139
Boehmite be that the method handled by seeding is formed, and be confined to boehmite particulate and adapt to be formed model in alumina abrasive
In enclosing, there is the spherical shape being especially desired to so that it is applied to abrasive application；R Bauers are in Publication No. CN 1942398A
Disclose a kind of seeded boehmite particulate material and preparation method, it is indicated that boeh-mite precursor and Bo Mu are provided in the form of suspension
Stone crystal seed, precursor is using conventional ATH (hibbsite), and crystal seed is pseudobochmite and acid-base modifier, then to it
It is heat-treated, so that boeh-mite precursor is converted into the boehmite particulate of various draw ratios；Cai Weiquan etc. is in Publication No. CN
A kind of preparation method of micrometre grade thin diaspore is disclosed in 1733607A, it is indicated that use H first2O2Precipitate certain alumina concentration
Sodium aluminate solution obtain boehmite crystal seed, then the sodium aluminate solution of itself and certain alumina concentration is carried out kind point, kind
Divide rate up to more than 50%；River fine jade is waited in ZL 200710031164.0, discloses a kind of preparation side of nano crystal boehmite
Method, i.e., using aluminium isopropoxide hydrolysate as precursor, the nm boehmite of good dispersion is then obtained by hydro-thermal reaction；CN
In 102249270A, the method that discloses a kind of big particle diameter boehmite of dry process, first by aluminium hydroxide in certain temperature and
Under pressure, boehmite is converted into, is then milled to certain particle diameter, nano silicon cladding processing is carried out finally by wet method,
Low oil absorbency is obtained, is widely used in the product of field of electronic materials；CN 102815733A disclose a kind of nm boehmite and
Its preparation method, i.e., the boehmite of certain component, inorganic acid/base, auxiliary agent, deionized water etc. stirs, and enters autoclave
Hydro-thermal reaction is carried out, is washed out, is spray-dried and obtains the nm boehmite of different-shape；CN 102092749A disclose one
The preparation method of kind boehmite, that is, use aluminium hydroxide as raw material, in hydrothermal treatment process, adds the crystal seed controls such as boehmite
The granule-morphology of product processed, adding acid or alkaline electrolyte reduces the sodium content of product, so as to obtain a kind of thin water of ultralow sodium
Aluminium stone and aluminum oxide；CN 101830491A disclose a kind of preparation method of high heat-resistant boehmite, i.e., aluminium hydroxide exist first
Boehmite is converted at >=350 DEG C, is then ground to certain particle diameter, then using progress nano surface dioxy under wet method high-speed stirred
The processing of SiClx cladding, is dried to obtain low oil absorbency, the boehmite product of high fluidity after edulcoration purification.
To sum up, the preparation method of high temperature resistant boehmite, related data are seldom.
The content of the invention
In view of the deficiencies of the prior art, the present invention provides a kind of preparation method of high temperature resistant boehmite.
To achieve the above object, the technical solution adopted by the present invention is：
A kind of preparation method of high temperature resistant boehmite, aluminum contained compound and aquation are starched, add seed content and washing assisant,
It is fitted into after well mixed in autoclave, it is 1~3 DEG C/min to control programming rate, at 150~250 DEG C, is dropped after reacting 2~6h
Temperature, after separating, washing, drying, obtain high temperature resistant boehmite.
Further, the mass ratio of the aluminum contained compound, seed content and washing assisant is 1：0.05~0.5：0.005~
0.1。
Further, the aluminum contained compound, including soda lime sintering process aluminium hydroxide, boehmite, ρ-aluminum oxide
Or the one or more in bayerite.
Further, the water includes distilled water, high purity water, deionized water or reverse osmosis water.
Further, the slurries liquid-solid ratio of the aluminum contained compound and aquation slurry is 1~10.
Further, one kind or more in the seed content, including unformed aluminium glue, alumina sol or boehmite
Kind.
Further, 0.1~95%wt of moisture content of the seed content.
Further, the washing assisant is the carbonate of ammonium, the pH value of slurries is controlled between 7~13.
Further, the drying temperature is 100~220 DEG C.
Further, reaction temperature is 180~210 DEG C, and programming rate is 1.5~3 DEG C/min, and the reaction time is 2~4h.
A kind of preparation method of high temperature resistant boehmite provided by the invention, obtained boehmite conversion rate is high, distribution of particles
Concentrate, 1% dehydration temperaturre reaches more than 350 DEG C, and chemical purity is high, the μ s/cm of electrical conductivity≤25；And preparation method is simple, production
Can be big, production cost is low, is widely used as preparing high purity aluminium oxide, high performance catalyst and carrier, high effect nontoxic fire retardant and
The fields such as electronic material.
Embodiment
The embodiment of the present invention provides a kind of preparation method of high temperature resistant boehmite, and aluminum contained compound and aquation are starched, and adds
Seed content and washing assisant, it is fitted into after well mixed in autoclave, it is 1~3 DEG C/min to control programming rate, at 150~250 DEG C
Under, cool after reacting 2~6h, after separating, washing, drying, obtain high temperature resistant boehmite.
The mass ratio of the aluminum contained compound, seed content and washing assisant is 1：0.05~0.5：0.005~0.1.It is described
The slurries liquid-solid ratio of aluminum contained compound and aquation slurry is 1~10, preferably 1.5~4.The moisture content 0.1~95% of the seed content
Wt, preferably 30~80%wt.
The aluminum contained compound includes soda lime sintering process aluminium hydroxide, boehmite, ρ-aluminum oxide or/and Bayer
Stone, aluminum contained compound can be that one kind can also be a variety of while adds, and not limit its additional proportion.
The seed content, including unformed aluminium glue, alumina sol and boehmite, seed content can be that one kind can also
It is a variety of to add simultaneously, its additional proportion is not limited.
One or more in the washing assisant, including the carbonate of the ammonium such as ammonium carbonate, ammonium hydrogen carbonate, make the pH of slurries
Value control is 7~13.
The drying, the filter cake after separating, washing is qualified, using baking oven, expansion drying or spray drying, dry temperature
Spend for 100~220 DEG C, preferably 150~210 DEG C.
The creativeness of the present invention is, contains aluminium using the soda lime sintering process aluminium hydroxide of low cost and its intermediate product etc.
Compound is raw material, by adding seed content and washing assisant, can obtain high heat-resistant boehmite (the 1% dehydration temperature of high-purity
Degree reaches more than 350 DEG C).Wherein, seed content can effectively control the crystal morphology of boehmite and granularity and distribution, washing assisant to have
Soluble sodium salt is converted into beneficial to by the sodium in raw material, is easy to washing and removes.Preparation method provided by the invention is simple, production capacity
Greatly, production cost is low, and this product is widely used as preparing high purity aluminium oxide, and high performance catalyst and carrier, high effect nontoxic are fire-retardant
The field such as agent and electronic material.
Embodiment 1
A kind of preparation method for high temperature resistant boehmite that the embodiment of the present invention 1 provides, it is specific as follows：Take 0.7kg soda lime
Sintering process aluminium hydroxide and 0.3kg ρ-aluminum oxide, aluminum contained compound and aquation slurry uniform with 2.5kg distilled water stirring slurrying
Slurries liquid-solid ratio is 2.5, adds the unformed aluminium glues of seed content 0.5kg (moisture content 65%), and after 5g scrubbing with ammonium carbonate auxiliary agents,
Slurries pH is about 7.5, is fitted into autoclave, and the speed of 1.5 DEG C/min of control rises to 180 DEG C, is incubated 2.5 hours.Mistake after cooling
Filter separation, with water washing is distilled, dried at 180 DEG C of baking oven.Product boehmite conversion rate is 98%, 1% 381 DEG C of dehydration temperaturre,
The μ s/cm of electrical conductivity 24.
Embodiment 2
A kind of preparation method for high temperature resistant boehmite that the embodiment of the present invention 2 provides, it is specific as follows：Take 0.5kg soda lime
Sintering process aluminium hydroxide and 0.5kg bayerites, the slurry that slurrying is uniform, and aluminum contained compound is starched with aquation is stirred with 1.5kg high purity waters
Liquid-liquid-solid ratio is 1.5, adds seed content 0.4kg boehmites (moisture content 50%), and after 50g scrubbing with ammonium carbonate auxiliary agents, slurries
PH is about 11.5, is fitted into autoclave, and the speed of 1.5 DEG C/min of control rises to 190 DEG C, is incubated 2 hours.Filtering point after cooling
From with high-purity water washing, being dried at 150 DEG C of baking oven.Product boehmite conversion rate is 97.5%, 1% 352 DEG C of dehydration temperaturre, electricity
The μ s/cm of conductance 20.
Embodiment 3
A kind of preparation method for high temperature resistant boehmite that the embodiment of the present invention 3 provides, it is specific as follows：1.0kg bayerites are taken,
Uniform with 2.5kg deionized waters stirring slurrying, the slurries liquid-solid ratio of aluminum contained compound and aquation slurry is 2.5, adds seed content
After 0.25kg alumina sols (moisture content 80%) and 10g ammonium hydrogen carbonate washing assisants, slurries pH is about 8, is fitted into autoclave,
The speed of 1.8 DEG C/min of control rises to 198 DEG C, is incubated 3 hours.It is separated by filtration, is washed with deionized after cooling, spraying is dry
Dried at dry 198 DEG C of device.Product boehmite conversion rate is 98.5%, 1% 358 DEG C of dehydration temperaturre, the μ s/cm of electrical conductivity 20.
Embodiment 4
A kind of preparation method for high temperature resistant boehmite that the embodiment of the present invention 4 provides, it is specific as follows：1kg ρ-aluminum oxide is taken,
Uniform with 2kg reverse osmosis waters stirring slurrying, the slurries liquid-solid ratio of aluminum contained compound and aquation slurry is 2.0, adds seed content
After 0.75kg boehmites (moisture content 0.5%), and 100g ammonium hydrogen carbonate washing assisants, slurries pH is about 13, loads high pressure
In kettle, the speed of 2.0 DEG C/min of control rises to 205 DEG C, is incubated 2 hours.It is separated by filtration after cooling, is washed with reverse osmosis water, is dodged
Steam and dried at 220 DEG C of drier.Product boehmite conversion rate is 97.8%, 1% 365 DEG C of dehydration temperaturre, the μ s/cm of electrical conductivity 21.
Embodiment 5
A kind of preparation method for high temperature resistant boehmite that the embodiment of the present invention 5 provides, it is specific as follows：0.6kg is taken to intend thin water
Aluminium stone and 0.4kg soda lime sintering process aluminium hydroxides, aluminum contained compound and aquation slurry uniform with 4kg high purity waters stirring slurrying
Slurries liquid-solid ratio is 4.0, adds seed content 1.65kg alumina sols (moisture content 70%), and the washing of 100g ammonium hydrogen carbonate helps
After agent, slurries pH is about 13, is fitted into autoclave, and the speed of 2 DEG C/min of control rises to 205 DEG C, is incubated 3 hours.Mistake after cooling
Filter separation, with high-purity water washing, dried at 190 DEG C of spray dryer.Product boehmite conversion rate is 98.5%, 1% dehydration temperature
358 DEG C of degree, the μ s/cm of electrical conductivity 18.
Embodiment 6
A kind of preparation method for high temperature resistant boehmite that the embodiment of the present invention 6 provides, it is specific as follows：Take 0.6kg bayerites,
0.2kg ρ-aluminum oxide and 0.2kg soda lime sintering process aluminium hydroxides, aluminum contained compound uniform with 3kg deionized waters stirring slurrying
Slurries liquid-solid ratio with aquation slurry is 3.0, adds the unformed aluminium glue of 0.5kg seed contents (moisture content 80%) and 70g ammonium carbonates
After washing assisant, slurries pH is about 9, is fitted into autoclave, and the speed of 2.0 DEG C/min of control rises to 198 DEG C, is incubated 4 hours.
It is separated by filtration, is washed with deionized after cooling, is dried at 205 DEG C of flash distillation dryer.Product boehmite conversion rate is 98.3%,
1% 355 DEG C of dehydration temperaturre, the μ s/cm of electrical conductivity 15.
Comparative example 1
A kind of preparation method for high temperature resistant boehmite that comparative example 1 of the present invention provides, it is specific as follows：Take and visitd with 1kg
Ear method aluminium hydroxide, addition 3kg high purity water stirrings slurrying is uniform, and the slurries liquid-solid ratio of aluminum contained compound and aquation slurry is 3.0, is filled
Enter in autoclave, the speed of 3.5 DEG C/min of control rises to 190 DEG C, is incubated 2 hours.It is separated by filtration, washs, 120 DEG C after cooling
Lower drying.Product boehmite conversion rate is 94.3%, 1% 281 DEG C of dehydration temperaturre, the μ s/cm of electrical conductivity 215.
Comparative example 2
A kind of preparation method for high temperature resistant boehmite that comparative example 2 of the present invention provides, it is specific as follows：Take and visitd with 1kg
Otolith, addition 4kg high purity water stirrings slurrying is uniform, and the slurries liquid-solid ratio of aluminum contained compound and aquation slurry is 4.0, loading autoclave
In, the speed of 3.5 DEG C/min of control rises to 200 DEG C, is incubated 3 hours.It is separated by filtration, washs after cooling, is dried at 120 DEG C.Production
Product boehmite conversion rate is 97.6%, 1% 272 DEG C of dehydration temperaturre, the μ s/cm of electrical conductivity 198.
Comparative example 3
A kind of preparation method for high temperature resistant boehmite that comparative example 3 of the present invention provides, it is specific as follows：Take and visitd with 1kg
Ear method aluminium hydroxide, addition 3kg high purity water stirrings slurrying is uniform, and the slurries liquid-solid ratio of aluminum contained compound and aquation slurry is 3.0, is added
Enter 100g seed content boehmites, be fitted into together in autoclave, the speed of 3.5 DEG C/min of control rises to 190 DEG C, and insulation 2 is small
When.It is separated by filtration, washs after cooling, is dried at 120 DEG C.Product boehmite conversion rate is 95.3%, 1% 275 DEG C of dehydration temperaturre,
The μ s/cm of electrical conductivity 208.
It should be noted last that above embodiment is merely illustrative of the technical solution of the present invention and unrestricted,
Although the present invention is described in detail with reference to example, it will be understood by those within the art that, can be to the present invention
Technical scheme modify or equivalent substitution, without departing from the spirit and scope of technical solution of the present invention, it all should cover
Among scope of the presently claimed invention.
Claims (1)
- A kind of 1. preparation method of high temperature resistant boehmite, it is characterised in that：Aluminum contained compound and aquation are starched, add seed content and Washing assisant, it is fitted into after well mixed in autoclave, it is 1.5~3 DEG C/min to control programming rate, at 180~210 DEG C, instead Cool after answering 2~4h, after separating, washing, drying, obtain high temperature resistant boehmite；The mass ratio of the aluminum contained compound, seed content and washing assisant is 1：0.05~0.5：0.005~0.1；One in the aluminum contained compound, including soda lime sintering process aluminium hydroxide, boehmite, ρ-aluminum oxide or bayerite Kind is a variety of；The water includes distilled water, high purity water, deionized water or reverse osmosis water；The slurries liquid-solid ratio of the aluminum contained compound and aquation slurry is 1.5~4；One or more in the seed content, including unformed aluminium glue, alumina sol or boehmite；30~80%wt of moisture content of the seed content；The washing assisant is the carbonate of ammonium, the pH value of slurries is controlled between 7~13；The drying temperature is 150~210 DEG C.
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Families Citing this family (12)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN106517273B (en) * | 2016-11-02 | 2017-12-05 | 齐鲁工业大学 | A kind of production technology for preparing low sodium boehmite |
| CN107298453A (en) * | 2017-07-03 | 2017-10-27 | 中国科学院青海盐湖研究所 | The nanocrystalline preparation method of boehmite |
| CN112062144B (en) * | 2020-09-19 | 2021-05-18 | 河津市炬华铝业有限公司 | A kind of macropore volume pseudo-boehmite and preparation method thereof |
| CN112551563B (en) * | 2020-12-30 | 2024-02-02 | 宣城晶瑞新材料有限公司 | Preparation method of boehmite liquid |
| CN113479919A (en) * | 2021-08-24 | 2021-10-08 | 安徽壹石通材料科技股份有限公司 | Low-conductivity boehmite and preparation method thereof |
| CN113860341B (en) * | 2021-10-28 | 2023-10-27 | 中化学科学技术研究有限公司 | High-purity platy boehmite and preparation method thereof |
| CN113860340B (en) * | 2021-10-28 | 2023-10-27 | 中化学科学技术研究有限公司 | Method for preparing high-purity granular boehmite by dry method and boehmite |
| CN113955779B (en) * | 2021-11-05 | 2023-10-27 | 中化学科学技术研究有限公司 | Method for preparing high-purity boehmite by dry method and high-purity boehmite |
| CN113860342B (en) * | 2021-11-05 | 2023-08-08 | 中化学科学技术研究有限公司 | Method for preparing high-purity parallelepiped boehmite and high-purity parallelepiped boehmite |
| CN114560482A (en) * | 2022-02-08 | 2022-05-31 | 中铝山东有限公司 | Pseudo-boehmite powder, forming carrier and preparation method thereof |
| CN115245798B (en) * | 2022-07-20 | 2024-08-16 | 山东大学 | A kind of γ-AlOOH sol and its preparation method and application |
| CN115353133B (en) * | 2022-09-02 | 2023-12-26 | 宁波大浦新材料科技有限公司 | Preparation method of high-purity boehmite |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| JPH02239113A (en) * | 1989-03-14 | 1990-09-21 | Mitsubishi Kasei Corp | Boehmite manufacturing method |
| JP4181777B2 (en) * | 2002-01-29 | 2008-11-19 | 河合石灰工業株式会社 | Boehmite production method |
| US20050227000A1 (en) * | 2004-04-13 | 2005-10-13 | Saint-Gobain Ceramics & Plastics, Inc. | Surface coating solution |
| CN1286725C (en) * | 2004-05-14 | 2006-11-29 | 山东铝业股份有限公司 | Method for preparing high-pruity alumina powder |
| CN100569650C (en) * | 2007-10-30 | 2009-12-16 | 华南理工大学 | A kind of preparation method of nano crystal boehmite |
| CN101830491A (en) * | 2010-05-14 | 2010-09-15 | 上海百图高新材料科技有限公司 | Preparation method of high heat-resistant boehmite |
| CN102092749A (en) * | 2010-12-15 | 2011-06-15 | 中国铝业股份有限公司 | Preparation method of boehmite |
| CN102807244A (en) * | 2012-07-27 | 2012-12-05 | 中国铝业股份有限公司 | Method for preparing boehmite |
| CN102942199B (en) * | 2012-10-17 | 2014-04-09 | 河南科技大学 | Preparation method of boehmite nanocrystallines or nanowhiskers |
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