CN107089676A - A kind of preparation method of high-purity boehmite - Google Patents

A kind of preparation method of high-purity boehmite Download PDF

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Publication number
CN107089676A
CN107089676A CN201710367476.2A CN201710367476A CN107089676A CN 107089676 A CN107089676 A CN 107089676A CN 201710367476 A CN201710367476 A CN 201710367476A CN 107089676 A CN107089676 A CN 107089676A
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boehmite
preparation
purity
dispersion liquid
organic base
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CN107089676B (en
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刘亚
王宇湖
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Suzhou routao New Material Co.,Ltd.
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SUZHOU NANO DISPERSIONS CO Ltd
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    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01FCOMPOUNDS OF THE METALS BERYLLIUM, MAGNESIUM, ALUMINIUM, CALCIUM, STRONTIUM, BARIUM, RADIUM, THORIUM, OR OF THE RARE-EARTH METALS
    • C01F7/00Compounds of aluminium
    • C01F7/02Aluminium oxide; Aluminium hydroxide; Aluminates
    • C01F7/42Preparation of aluminium oxide or hydroxide from metallic aluminium, e.g. by oxidation
    • C01F7/428Preparation of aluminium oxide or hydroxide from metallic aluminium, e.g. by oxidation by oxidation in an aqueous solution
    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01PINDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2002/00Crystal-structural characteristics
    • C01P2002/70Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data
    • C01P2002/72Crystal-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
    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01PINDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2002/00Crystal-structural characteristics
    • C01P2002/80Crystal-structural characteristics defined by measured data other than those specified in group C01P2002/70
    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01PINDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2004/00Particle morphology
    • C01P2004/01Particle morphology depicted by an image
    • C01P2004/03Particle morphology depicted by an image obtained by SEM
    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01PINDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2006/00Physical properties of inorganic compounds
    • C01P2006/80Compositional purity

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  • 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 invention discloses a kind of preparation method of high-purity boehmite, including step:Pure water and high purity aluminum powder are mixed by a certain percentage, form dispersion liquid;Organic base is slowly added into above-mentioned dispersion liquid, until bubble-free is produced;Under the conditions of 130~250 DEG C, then 3~12h of hydro-thermal process both obtains boehmite through filtering, drying.Boehmite prepared by the present invention is free of harmful anion (such as SO4 2‑、Cl、NO3 ), metal ion content is extremely low, and post processing is cleaned without substantial amounts of pure water and alcohol, non-environmental-pollution.And preparation method reaction condition is gentle, operating procedure is simple, and production cost is low, and good product dispersibility, crystallinity are high, distribution of particles is narrow.

Description

A kind of preparation method of high-purity boehmite
Technical field
The present invention relates to technical field of chemistry, and in particular to a kind of preparation method of compound, more particularly to a kind of high-purity Spend the preparation method of boehmite.
Background technology
Boehmite (boehmite) is also known as boehmite, and white powder is presented in outward appearance, and molecular formula is γ-AlOOH.Bo Mu Stone can be used for the battery diaphragm and filling plastic of electric substrate, casting glue, coating, rubber, lithium battery as fire retardant in itself, Can also be using the blotting material for making high-end digital printing medium.And the most important purposes of boehmite is as preparation γ-Al2O3 With α-Al2O3The presoma of powder, boehmite is converted into γ-Al after 400-700 DEG C is calcined2O3It is widely used in catalyst load Body, catalyst and adsorbent etc.;α-Al are obtained after being calcined at 1100-1200 DEG C2O3It can be applied to high-grade ceramic, coating, efficiently urge Agent, micron/submicron grinding-material and polishing material and inorganic material film etc..
At present, the preparation method of boehmite mainly has sol-gel process, precipitation Hydrolyze method and hydro-thermal method.The precipitation method are synthesized Boehmite reaction is simple, but requirement is strict to some process parameter controls such as:PH, temperature and reactant concentration, are kept away with this Exempt from aluminium hydroxide Al (OH)3Generation.Sol-gel process, which prepares boehmite, has grain diameter small, bigger than surface and pore volume Feature, but its boehmite crystal degree prepared is poor, and also it is serious to reunite in last handling process, even if addition surface conditioning agent It is extremely difficult to preferable effect.Hydro-thermal method refers under certain temperature and pressure, and the reactive ion in solution has higher anti- Kinetic energy is answered, their mutual collision rifts easily break through solvation film, discharge lattice energy, and then it is low, constitutionally stable to synthesize energy Material.Higher with respect to hydro-thermal method synthesis boehmite efficiency for other method, the boehmite of preparation has crystallinity height, reunited Low, good dispersion, size be controllable and the features such as narrow particle diameter distribution;And hydro-thermal method prepares boehmite processing step simply, to temperature Degree and pressure requirements are relatively low.
There is series of advantages because hydro-thermal method prepares boehmite, the wide of domestic and international researchers has been caused in recent years General concern, wherein being mainly used as raw material using inorganic aluminate and organo-aluminium alcoholate.Inorganic aluminate is mainly aluminium chloride, aluminum sulfate, nitre Sour aluminium and sodium metaaluminate, the one or more using in them are as silicon source, and Hydrothermal Synthesiss prepare boehmite, Chinese patent CN103318931A discloses a kind of method by the use of composite inorganic aluminium salt as raw water hot preparation boehmite, is in this invention Removing the anion in aluminium salt needs to utilize substantial amounts of water eccentric cleaning;In addition, reunite for drying for reduction boehmite powder, need Dewater treatment is carried out using alcohol.Boehmite still purity prepared by the method is relatively low, contains the harmful the moon for not utilizing it to apply Ion, substantially, bad dispersibility, crystallinity is low for agglomeration.Method disclosed in Chinese patent CN103663519A is with meta-aluminic acid Sodium is silicon source, and urea is that precipitating reagent hydro-thermal prepares boehmite, though the method technique is simple, cost is low, post processing is also required to Using substantial amounts of water clean sodium ion, waste water resource, pollution environment, the boehmite finally prepared still containing more sodium from Son, it is impossible to meet high-purity demand.It can prepare the boehmite of high-purity using organo-aluminium alcoholate as silicon source hydro-thermal process, document (Shi Tao, The preparation of Guo Xingzhong, Yang Hui boehmites (γ-AlOOH) colloidal sol and sign rare metals and engineering, A20,2008,73-75) in Reaction is hydrolyzed by presoma of aluminium isopropoxide, then boehmite, the preparation side of this multistep reaction are prepared by hydro-thermal process Method, process is complicated, time-consuming, inefficient and higher by cost of material of aluminium isopropoxide, in addition, it is related to organic solvent, it is environmentally friendly Pressure is big.
The content of the invention
In view of the above-mentioned defect for preparing high-purity boehmite method, present invention offer one kind is prepared high-purity vigorous using hydro-thermal process The new method of nurse stone, boehmite prepared by this method is free of harmful anion (such as SO4 2-、Cl-、NO3 -), metal ion content pole Low, post processing is cleaned without substantial amounts of pure water and alcohol, non-environmental-pollution, and good product dispersibility, crystallinity are high, distribution of particles It is narrow.
In order to solve the above-mentioned technical problem, the preparation method for a kind of high-purity boehmite that the present invention is provided, including as follows Step:
(1) pure water and high purity aluminum powder are mixed by a certain percentage, are uniformly dispersed, form dispersion liquid;
(2) organic base is slowly added into above-mentioned dispersion liquid, the mol ratio of organic base and aluminium powder is 0.1~2, in 60- 1-6h is reacted under the conditions of 100 DEG C, until bubble-free is produced;
(3) by slurry obtained by above-mentioned reaction, under the conditions of 130~250 DEG C, 3~12h of hydro-thermal process, then through filtering, doing It is dry both to obtain boehmite.
In the optimal technical scheme of the present invention, the mol ratio of pure water and high purity aluminum powder is 1:3~12, preferably 1:5~ 10。
In the optimal technical scheme of the present invention, the organic base is selected from ethylenediamine or choline or triethylamine or tetramethyl hydrogen Mixtures more than one or both of amine-oxides or monoethanolamine.
In the optimal technical scheme of the present invention, in step (2), organic base is slowly dropped in dispersion liquid.
In the optimal technical scheme of the present invention, in step (3), under the conditions of 130~170 DEG C, 4~5h of hydro-thermal process Place.
The present invention is, using high purity aluminum powder and organic base as raw material, high-purity boehmite to be prepared using Hydrothermal Synthesiss, with current state Inside and outside conventional other method (sol-gel process, the hydro-thermal method of other raw materials) is compared, with following obvious advantage:
1. the present invention is using high purity aluminum powder and organic base as raw material, the boehmite purity of preparation is high, without harmful anion (such as SO4 2-、Cl-、NO3 -), metal ion content is extremely low, is to make catalyst or catalyst carrier γ-Al2O3Preferable presoma.
2. the post processing that the present invention prepares boehmite is simple, environmental protection, both need not using the cleaning of substantial amounts of water, with except The foreign ion gone in boehmite;Dewater treatment is carried out also without using alcohol, to reduce the reunion of boehmite.
3. the present invention prepares boehmite with Hydrothermal Synthesiss, reaction condition is gentle, and preparation efficiency is high, and operating procedure is simple, system Standby boehmite crystal degree is high, good dispersion.
4. the present invention is compared with being the high-purity boehmite of raw water hot preparation using organo-aluminium alcoholate, raw material is simple, and cost is low, closes It is simple into technique.
Brief description of the drawings
Below in conjunction with the accompanying drawings and embodiment the invention will be further described:
Fig. 1 is the boehmite powder X-ray diffraction analysis figure of the embodiment of the present invention 1;
Fig. 2 images picture for the boehmite powder electron scanning of the embodiment of the present invention 1;
Fig. 3 is the boehmite powder X-ray diffraction analysis figure of the embodiment of the present invention 2;
Fig. 4 images picture for the boehmite powder electron scanning of the embodiment of the present invention 2.
Embodiment
In order to facilitate the understanding of the purposes, features and advantages of the present invention, below in conjunction with the accompanying drawings to the present invention Embodiment be described in detail.Many details are elaborated in the following description to fully understand this hair It is bright.But the invention can be embodied in many other ways as described herein, those skilled in the art can be not Similar improvement is done in the case of running counter to intension of the present invention, therefore the present invention is not limited by following public specific embodiment.
Unless otherwise defined, all of technologies and scientific terms used here by the article is with belonging to technical field of the invention The implication that technical staff is generally understood that is identical.Term used in the description of the invention herein is intended merely to description tool The purpose of the embodiment of body, it is not intended that in the limitation present invention.Term as used herein " and/or " include one or more phases The arbitrary and all combination of the Listed Items of pass.
The specific embodiment of the invention is described below in conjunction with accompanying drawing.
Embodiment 1
Pure water and high purity aluminum powder (purity 99.99%) are pressed 1:5 mol ratio, is added in reactor, opens agitating paddle, Aluminium powder and water are uniformly dispersed, it is 1.5 choline (Choline) then to take with aluminium powder mol ratio, is slowly dropped in reactor, Heating response kettle obtains finely dispersed white slurry to 80 DEG C of insulation 4h, then improves temperature of reaction kettle to 150 DEG C, hydro-thermal 5h is reacted, reaction leads to cooling water temperature to room temperature, takes out slurry after terminating, high-purity boehmite powder is obtained after filtering, drying.
High-purity boehmite powder prepared by above step is the single crystalline phase of boehmite through X-ray diffraction analysis, and suddenly nurse Stone crystallinity is high, as shown in Figure 1;Powder microscopic appearance is as shown in Fig. 2 boehmite particles are tiny sheet-like morphology;Powder passes through After electron level acid is cleared up, metals content impurity such as following table is detected by ICP spectrometers:
Boehmite powder impurity content in the embodiment 1 of table 1:
Element Fe Mg Ca Cu Na K
Content <20ppm <10ppm <10ppm <5ppm <2ppm <2ppm
Other metals content impurities are below 1ppm.
Embodiment 2
Pure water and high purity aluminum powder (purity 99.99%) are pressed 1:10 mol ratio, is added in reactor, opens stirring Oar, is uniformly dispersed aluminium powder and water, and it is 0.5 TMAH (TMAH) then to take with aluminium powder mol ratio, is slowly added dropwise Into reactor, heating response kettle obtains finely dispersed white slurry, then improves temperature of reaction kettle to 100 DEG C of insulation 2h To 170 DEG C, hydro-thermal reaction 3h, reaction leads to cooling water temperature to room temperature after terminating, take out slurry, and height is obtained after filtering, drying Pure boehmite powder.
High-purity boehmite powder prepared by above step is the single crystalline phase of boehmite through X-ray diffraction analysis, and suddenly nurse Stone crystallinity is high, as shown in Figure 3;Powder microscopic appearance is as shown in figure 4, boehmite particles are sheet and fibrous mixed polymerization Bodily form looks;Powder detects metals content impurity such as following table after electron level acid is cleared up by ICP spectrometers:
Boehmite powder impurity content in the embodiment 2 of table 2:
Element Fe Mg Ca Cu Na K
Content <20ppm <10ppm <10ppm <5ppm <2ppm <2ppm
Other metals content impurities are below 1ppm.
General principle, principal character and the advantages of the present invention of the present invention has been shown and described above.The technology of the industry Personnel are not it should be appreciated that the present invention is limited by examples detailed above, and the simply explanation described in examples detailed above and specification is of the invention Principle, various changes and modifications of the present invention are possible without departing from the spirit and scope of the present invention, these change and Improvement all fall within the protetion scope of the claimed invention.The claimed scope of the invention is by appended claims and its is equal Thing is defined.

Claims (4)

1. a kind of preparation method of high-purity boehmite, comprises the following steps:
(1) pure water and high purity aluminum powder are mixed by a certain percentage, are uniformly dispersed, form dispersion liquid;
(2) organic base is slowly added into above-mentioned dispersion liquid, the mol ratio of organic base and aluminium powder is 0.1~2, at 60-100 DEG C Under the conditions of react 1-6h, until bubble-free produce;
(3) by slurry obtained by above-mentioned reaction, under the conditions of 130~250 DEG C, 3~12h of hydro-thermal process, then through filtering, drying both Obtain boehmite.
2. the preparation method of high-purity boehmite according to claim 1, it is characterised in that pure water and high purity aluminum powder are rubbed You are than being 1:3~12.
3. the preparation method of high-purity boehmite according to claim 1, it is characterised in that the organic base is selected from second two Mixture more than amine or choline or triethylamine or one or both of TMAH or monoethanolamine.
4. the preparation method of high-purity boehmite according to claim 1, it is characterised in that in step (2), by organic base It is slowly dropped in dispersion liquid.
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Cited By (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN113860342A (en) * 2021-11-05 2021-12-31 中化学科学技术研究有限公司 Method for preparing high-purity parallelepipedal boehmite and high-purity parallelepipedal boehmite
CN113955782A (en) * 2021-09-06 2022-01-21 湖北金泉新材料有限公司 Morphology-controllable boehmite preparation method
CN114477253A (en) * 2022-03-15 2022-05-13 青海万加环保新材料有限公司 Method for producing high-purity boehmite by hydrothermal method
CN114804170A (en) * 2021-06-30 2022-07-29 上交赛孚尔(包头)新材料有限公司 Adsorbent, method for preparing aluminum hydroxide and application
CN115448342A (en) * 2022-08-26 2022-12-09 雅安百图高新材料股份有限公司 Boehmite powder and preparation method thereof

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Cited By (9)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN114804170A (en) * 2021-06-30 2022-07-29 上交赛孚尔(包头)新材料有限公司 Adsorbent, method for preparing aluminum hydroxide and application
CN114873620A (en) * 2021-06-30 2022-08-09 上交赛孚尔(包头)新材料有限公司 Adsorbent, method for preparing aluminum hydroxide and application
CN114804170B (en) * 2021-06-30 2023-11-17 上交赛孚尔(包头)新材料有限公司 Adsorbent, method for preparing aluminum hydroxide and application
CN114873620B (en) * 2021-06-30 2024-05-10 上交赛孚尔(包头)新材料有限公司 Adsorbent, method for preparing aluminum hydroxide and application
CN113955782A (en) * 2021-09-06 2022-01-21 湖北金泉新材料有限公司 Morphology-controllable boehmite preparation method
CN113860342A (en) * 2021-11-05 2021-12-31 中化学科学技术研究有限公司 Method for preparing high-purity parallelepipedal boehmite and high-purity parallelepipedal 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
CN114477253A (en) * 2022-03-15 2022-05-13 青海万加环保新材料有限公司 Method for producing high-purity boehmite by hydrothermal method
CN115448342A (en) * 2022-08-26 2022-12-09 雅安百图高新材料股份有限公司 Boehmite powder and preparation method thereof

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