CN101928029A - Method for preparing aluminum oxide sol - Google Patents

Method for preparing aluminum oxide sol Download PDF

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Publication number
CN101928029A
CN101928029A CN 201010274945 CN201010274945A CN101928029A CN 101928029 A CN101928029 A CN 101928029A CN 201010274945 CN201010274945 CN 201010274945 CN 201010274945 A CN201010274945 A CN 201010274945A CN 101928029 A CN101928029 A CN 101928029A
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China
Prior art keywords
boehmite
pseudo
preparation
acid
suspension
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CN 201010274945
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Chinese (zh)
Inventor
张涛
蒋丹宇
陈家凡
冯涛
陆黎明
徐兵
毛晗君
黄德信
徐海芳
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Suzhou Chuangyuan New Materials Technology Co., Ltd.
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Suzhou Chuangyuan Investment Development Co ltd
Shanghai Institute of Ceramics of CAS
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Priority to CN 201010274945 priority Critical patent/CN101928029A/en
Publication of CN101928029A publication Critical patent/CN101928029A/en
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Abstract

The invention relates to a method for preparing aluminum oxide sol. In the method, pseudo-boehmite is taken as a raw material; and the method sequentially comprises the following steps of: (1) dispersing the pseudo-boehmite into de-ionized water, wherein the weight ratio of the pseudo-boehmite to the water is 1:2-20; (2) adding an acid to adjust pH to be 2 to 5, and stirring the mixed solution with a strong force for 0.5 to 2 hours by using a colloid mill to produce suspension; (3) placing the suspension into a baking oven of 80 to 90 DEG C, and ageing the suspension for 24 to 72 hours to produce aged slurry, and (4) taking the aged slurry out and removing precipitates on a lower layer to prepare the aluminum oxide sol. The method of the invention is simple and environmentally-friendly; and the prepared aluminum oxide sol has high performance and is suitable for large-scale industrial production.

Description

A kind of preparation method of alumina sol
Technical field
The present invention relates to a kind of preparation method of alumina sol.
Background technology
Sol-gel method is to have developed one of material synthesis method rapidly in the Materials science since this century, has been widely used in superconducting material electronic ceramics, composite organic-inorganic material, ceramic ultrafine powder, crystalline state and noncrystalline membrane and coating every field.The alumina sol gel application is the most extensive in actual production, is mainly used in preparation carrier, porous-film and thermofin, is the emphasis of field of inorganic materials research.Its, character of alumina sol played decisive role for the structure and the performance of the finished product mid-early stage, so the preparation of colloidal sol is worth our further investigation.
In the prior art, alumina sol to mainly contain with organic salt such as aluminum isopropylate be organic salt raw material method, inorganic salt raw material method and the powder dispersion method of raw material.The inorganic salt raw material method be with the metallic aluminium digestion in hydrochloric acid or AlCl3 solution, obtain the aluminium colloidal sol of clear, colorless, also can analytical pure aluminum nitrate and citric acid is soluble in water according to a certain ratio, with concentrated nitric acid or strong aqua regulator solution value, get colourless transparent solution, after the filtration,, can obtain having certain viscosity and mobile faint yellow vitreosol with the slowly evaporation at a certain temperature of this solution; Perhaps the method that need not evaporate after the precipitation and centrifugal separation that obtains, adds nitric acid by a certain percentage, and effect can obtain aluminium colloidal sol in ultrasonic water bath.It is raw material that the powder dispersion method directly adopts existing Industrial products such as SB powder or aluminum oxide powder, gets colloidal sol by the powder decentralized system.The SB powder is a kind of boehmite powder, and main component is a gama-alumina, and content is 76.2%, and all the other are moisture.Allow SB powder and distilled water be mixed into certain density suspension liquid earlier, be heated to 85 ℃ after high degree of agitation, add a certain amount of nitric acid, the certain hour that refluxes under high degree of agitation and 85 ℃ of conditions promptly gets γ-AlOOH colloidal sol.The preparation process of this method need be carried out under comparatively high temps, is unfavorable for energy-conservation and operation.
Summary of the invention
Technical problem to be solved by this invention provides a kind of preparation method of new alumina sol.
For solving above technical problem, the present invention takes following technical scheme:
A kind of preparation method of alumina sol, this method is raw material with the pseudo-boehmite, comprises the following steps of carrying out successively:
(1), pseudo-boehmite is dispersed in the deionized water, wherein, the weight ratio of pseudo-boehmite and water is 1: 2~20;
(2), add acid for adjusting pH to 2~5, adopt colloidal mill powerful stirred 0.5~2 hour suspension;
(3), described suspension put into 80 ℃~90 ℃ oven ageing obtain aging slurry, the aged time is 24~72 hours;
(4), described aging slurry is taken out, remove the precipitation of sub-cloud, promptly get described alumina sol.
According to an aspect of the present invention, as the purity of the pseudo-boehmite of raw material more than or equal to 98.5wt%.
The weight ratio of pseudo-boehmite and water is preferably 1: 4~and 8, and adding acid, to regulate described pH be 2~4.Described acid is for can be for being selected from nitric acid, hydrochloric acid, oxalic acid and the hydrofluoric acid one or more.These acid can be for directly buying the technical grade acid or the acid through diluting of gained.Those skilled in the art can select the concentration of suitable acid in order to regulate the purpose of pH.
In the step (3), described aging preferably under 84 ℃~86 ℃ of temperature, carry out.
Because adopt technique scheme, the present invention compared with prior art has the following advantages:
Technology of the present invention is simple, environmental protection, and gained alumina sol excellent property is suitable for large-scale industrial production.
Embodiment
The present invention is according to powder dispersive principle, has proposed a kind of raw material that adopts nontoxic pseudo-boehmite as the preparation alumina sol, the novel method of disperseing pseudo-boehmite is prepared into colloidal sol by brute force.
Pseudo-boehmite has another name called monohydrate alumina, and molecular formula AlOOH is nontoxic, tasteless, odorless, white colloidal (wet product) or powder (dry product), and crystalline phase purity height, peptization performance are good, and cohesiveness is strong, has the characteristics of thixotropy gel.
The present invention will be further described in detail below in conjunction with specific embodiments:
Embodiment 1
Preparation process according to the alumina sol of present embodiment is: the pseudo-boehmite of purity greater than 98.5wt% is dispersed in the deionized water, and the weight ratio of boehmite and water is 1: 10; Add hydrochloric acid and regulate pH to 2, the powerful stirring of colloidal mill obtained suspension in 0.5 hour; Then, suspension is put into 85 ℃ of baking ovens, leave standstill and obtained aging slurry in aging 72 hours, the slurry that should wear out at last takes out, and removes the precipitation of sub-cloud, promptly gets translucent alumina sol, and the viscosity of surveying under its 25 ℃ is 5MPa/s.
Embodiment 2
Preparation process according to the alumina sol of present embodiment is: the pseudo-boehmite of purity greater than 98.5wt% is dispersed in the deionized water, and the weight ratio of boehmite and water is 1: 5; Add oxalic acid and regulate pH to 2, the powerful stirring of colloidal mill obtained suspension in 0.5 hour; Then, suspension is put into 85 ℃ of baking ovens, leave standstill and obtained aging slurry in aging 72 hours, the slurry that should wear out at last takes out, and removes the precipitation of sub-cloud, promptly gets translucent alumina sol, and the viscosity of surveying under its 25 ℃ is 5MPa/s.
Embodiment 3
Preparation process according to the alumina sol of present embodiment is: the pseudo-boehmite of purity greater than 98.5wt% is dispersed in the deionized water, and the weight ratio of boehmite and water is 1: 8; Add hydrochloric acid and regulate pH to 4, the powerful stirring of colloidal mill obtained suspension in 1.5 hours; Then, suspension is put into 85 ℃ of baking ovens, leave standstill and obtained aging slurry in aging 60 hours, the slurry that should wear out at last takes out, and removes the precipitation of sub-cloud, promptly gets translucent alumina sol, and the viscosity of surveying under its 25 ℃ is 4MPa/s.
The foregoing description only is explanation technical conceive of the present invention and characteristics; its purpose is to allow the personage who is familiar with this technology can understand content of the present invention and enforcement according to this; can not limit protection scope of the present invention with this; all equivalences that spirit is done according to the present invention change or modify, and all should be encompassed within protection scope of the present invention.

Claims (6)

1. the preparation method of an alumina sol, it is characterized in that: this method is a raw material with the pseudo-boehmite, comprises the following steps of carrying out successively:
(1), pseudo-boehmite is dispersed in the deionized water, wherein, the weight ratio of pseudo-boehmite and water is 1: 2~20;
(2), add acid for adjusting pH to 2~5, adopt colloidal mill powerful stirred 0.5~2 hour suspension;
(3), described suspension put into 80 ℃~90 ℃ oven ageing obtain aging slurry, the aged time is 24~72 hours;
(4), described aging slurry is taken out, remove the precipitation of sub-cloud, promptly get described alumina sol.
2. preparation method according to claim 1 is characterized in that: as the purity of the described pseudo-boehmite of raw material more than or equal to 98.5wt%.
3. preparation method according to claim 1 is characterized in that: in the step (1), the weight ratio of pseudo-boehmite and water is 1: 4~8.
4. preparation method according to claim 1 is characterized in that: in the step (2), described acid is to be selected from nitric acid, hydrochloric acid, oxalic acid and the hydrofluoric acid one or more.
5. according to claim 1 or 4 described preparation methods, it is characterized in that: in the step (2), regulate pH to 3~4.
6. preparation method according to claim 1 is characterized in that: in the step (3), described wearing out carried out under 84 ℃~86 ℃ of temperature.
CN 201010274945 2010-09-08 2010-09-08 Method for preparing aluminum oxide sol Pending CN101928029A (en)

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Cited By (14)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103183501A (en) * 2013-03-13 2013-07-03 湖南大学 Micro-nano spherical SG corundum abrasive and preparation method thereof
CN103288111A (en) * 2013-06-28 2013-09-11 河南省格林沃特净化器股份有限公司 Fast stabilization preparation method of alumina sol
CN103496724A (en) * 2013-08-30 2014-01-08 航天特种材料及工艺技术研究所 Preparation method of nano alumina sol and gel
CN105347373A (en) * 2015-11-20 2016-02-24 中石化催化剂(北京)有限公司 Preparation method of pseudo-boehmite
CN105347375A (en) * 2015-11-20 2016-02-24 中石化催化剂(北京)有限公司 Production device of pseudo-boehmite and method thereof
CN106477607A (en) * 2016-10-13 2017-03-08 沈阳工业大学 A kind of preparation method of high solids content alumina sol
CN106687412A (en) * 2014-06-13 2017-05-17 Ifp 新能源公司 Gel with high dispersibility and method for preparing same
CN110037053A (en) * 2019-05-13 2019-07-23 无锡市妇幼保健院 High-efficiency antimicrobial liquid and preparation method thereof
CN110950365A (en) * 2019-12-20 2020-04-03 大连理工大学 Low-acid-content high-purity alumina sol and preparation method thereof
CN115140753A (en) * 2022-08-03 2022-10-04 中国科学院广州地球化学研究所 Method for preparing boehmite by using pseudo-boehmite and application thereof
CN115172059A (en) * 2022-08-09 2022-10-11 西安稀有金属材料研究院有限公司 Method for preparing aluminum electrolytic capacitor anode foil by combining aerosol spraying method
CN115957798A (en) * 2021-10-09 2023-04-14 中国石油化工股份有限公司 Catalytic cracking catalyst with rich mesoporous structure and preparation method thereof
CN115990496A (en) * 2021-10-18 2023-04-21 中国石油化工股份有限公司 Catalytic cracking auxiliary agent containing large-particle-size sol and preparation method thereof
CN115990505A (en) * 2021-10-18 2023-04-21 中国石油化工股份有限公司 Catalytic cracking auxiliary agent containing large-particle-size sol and preparation method thereof

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US4676928A (en) * 1986-01-30 1987-06-30 Vista Chemical Company Process for producing water dispersible alumina
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CN1477059A (en) * 2003-06-05 2004-02-25 上海大学 Preparation method of nano alumina material
CN101200297A (en) * 2007-12-24 2008-06-18 天津大学 Method for preparing integral macroporous alumina

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KR20020044683A (en) * 2000-12-06 2002-06-19 김충섭 Method of preparing alumina sols from aluminium chloride solution
CN1445167A (en) * 2003-03-20 2003-10-01 淄博市临淄正华助剂有限公司 Technique for preparing aluminium sol
CN1454963A (en) * 2003-05-13 2003-11-12 昆明理工大学 Quasi-thin empholite crystal-inoculating rare earth light-emitting material preparing process
CN1477059A (en) * 2003-06-05 2004-02-25 上海大学 Preparation method of nano alumina material
CN101200297A (en) * 2007-12-24 2008-06-18 天津大学 Method for preparing integral macroporous alumina

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Cited By (20)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103183501B (en) * 2013-03-13 2015-01-07 湖南大学 Micro-nano spherical SG corundum abrasive and preparation method thereof
CN103183501A (en) * 2013-03-13 2013-07-03 湖南大学 Micro-nano spherical SG corundum abrasive and preparation method thereof
CN103288111A (en) * 2013-06-28 2013-09-11 河南省格林沃特净化器股份有限公司 Fast stabilization preparation method of alumina sol
CN103288111B (en) * 2013-06-28 2014-12-10 河南省格林沃特净化器股份有限公司 Fast stabilization preparation method of alumina sol
CN103496724A (en) * 2013-08-30 2014-01-08 航天特种材料及工艺技术研究所 Preparation method of nano alumina sol and gel
CN103496724B (en) * 2013-08-30 2016-03-30 航天特种材料及工艺技术研究所 The preparation method of a kind of nano alumina sol and gel
CN106687412A (en) * 2014-06-13 2017-05-17 Ifp 新能源公司 Gel with high dispersibility and method for preparing same
CN106687412B (en) * 2014-06-13 2018-03-13 Ifp 新能源公司 Gel with polymolecularity and preparation method thereof
CN105347373A (en) * 2015-11-20 2016-02-24 中石化催化剂(北京)有限公司 Preparation method of pseudo-boehmite
CN105347375A (en) * 2015-11-20 2016-02-24 中石化催化剂(北京)有限公司 Production device of pseudo-boehmite and method thereof
CN106477607A (en) * 2016-10-13 2017-03-08 沈阳工业大学 A kind of preparation method of high solids content alumina sol
CN110037053A (en) * 2019-05-13 2019-07-23 无锡市妇幼保健院 High-efficiency antimicrobial liquid and preparation method thereof
CN110037053B (en) * 2019-05-13 2021-08-24 无锡市妇幼保健院 Efficient antibacterial liquid and preparation method thereof
CN110950365A (en) * 2019-12-20 2020-04-03 大连理工大学 Low-acid-content high-purity alumina sol and preparation method thereof
CN115957798A (en) * 2021-10-09 2023-04-14 中国石油化工股份有限公司 Catalytic cracking catalyst with rich mesoporous structure and preparation method thereof
CN115990496A (en) * 2021-10-18 2023-04-21 中国石油化工股份有限公司 Catalytic cracking auxiliary agent containing large-particle-size sol and preparation method thereof
CN115990505A (en) * 2021-10-18 2023-04-21 中国石油化工股份有限公司 Catalytic cracking auxiliary agent containing large-particle-size sol and preparation method thereof
CN115140753A (en) * 2022-08-03 2022-10-04 中国科学院广州地球化学研究所 Method for preparing boehmite by using pseudo-boehmite and application thereof
CN115140753B (en) * 2022-08-03 2023-11-03 中国科学院广州地球化学研究所 Method for preparing boehmite by pseudo-boehmite and application thereof
CN115172059A (en) * 2022-08-09 2022-10-11 西安稀有金属材料研究院有限公司 Method for preparing aluminum electrolytic capacitor anode foil by combining aerosol spraying method

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