CN100569650C - A kind of preparation method of nano crystal boehmite - Google Patents
A kind of preparation method of nano crystal boehmite Download PDFInfo
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- CN100569650C CN100569650C CNB2007100311640A CN200710031164A CN100569650C CN 100569650 C CN100569650 C CN 100569650C CN B2007100311640 A CNB2007100311640 A CN B2007100311640A CN 200710031164 A CN200710031164 A CN 200710031164A CN 100569650 C CN100569650 C CN 100569650C
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Abstract
The invention discloses a kind of preparation method of nano crystal boehmite, this method comprises the steps: (1) hydrolysis reaction: with distilled water and aluminum isopropylate by 50～150: 1 mixed in molar ratio, be heated to 70-90 ℃, reaction 1～2h, the filtering reaction product, 80-90 ℃ of dry 8-12h in baking oven; (2) hydro-thermal reaction is packed desciccate in the step (1) in the autoclave into, and as reaction medium, the reactor compactedness is 60%-80% with distilled water, and temperature of reaction is 150-200 ℃, and reaction times 4-12h makes nano crystal boehmite.The nano crystal boehmite product degree of crystallinity height of the present invention's preparation, regular crystal forms, even particle size, dispersion condition is simple, favorable dispersity.And have good water dispersible, its dispersion condition is simple, and particle size distribution is even, does not have obvious agglomeration.
Description
Technical field
The present invention relates to a kind of preparation method of boehmite, be specifically related to, handle the method for preparing nano crystal boehmite through hydrothermal method again by the hydrolysis aluminum alcoholate.
Background technology
Pseudo-boehmite and boehmite are preparation γ-Al
2O
3And α-Al
2O
3Deng two kinds of important presomas of crystal formation aluminum oxide, γ-Al
2O
3Extensively be used as support of the catalyst, catalyzer and sorbent material etc.; α-the Al of the final stable product of roasting
2O
3Use wide in fields such as pottery, electronic circuit substrate material and structured materials.Boehmite is except the presoma as aluminum oxide, because itself is at crystalline structure, crystal habit etc. are widely used in catalyzer and carrier to the characteristic that the aspect had, inorganic combustion inhibitor, papermaking filler, every field such as industrial chemicals.
The method for preparing at present boehmite mainly contains the inorganic salt hydrolysis method, organic coordination compound hydrolysis method, organic alkoxide hydrolysis, carborization, sol-gel method.
Traditional organic alkoxide hydrolysis prepares the pseudo-boehmite of normally low crystallization of products therefrom in the boehmite process or even amorphous state, but this product exist degree of crystallinity poor, easily reunite problem such as the irregular and size-grade distribution of morphology microstructure is inhomogeneous.
Summary of the invention
The objective of the invention is to overcome the problem that prior art exists, provide a kind of degree of crystallinity height that has, regular crystal forms, the preparation method of the nano crystal boehmite of favorable dispersity.
For addressing the above problem, the present invention takes following technical scheme:
A kind of preparation method of nano crystal boehmite comprises the steps:
(1) hydrolysis reaction: distilled water and aluminum isopropylate by 50～150: 1 mixed in molar ratio, are heated to 70-90 ℃, reaction 1～2h, filtering reaction product, 80-90 ℃ of dry 8-12h in baking oven;
(2) hydro-thermal reaction is packed desciccate in the step (1) in the autoclave into, stays water as reaction medium with steaming, and the reactor compactedness is 60%-80%, and temperature of reaction is 150-200 ℃, and reaction times 4-12h makes nano crystal boehmite.
For further realizing the object of the invention, the mol ratio of described distilled water and aluminum isopropylate is preferably 80～110: 1.
Described step (1) reaction times is preferably 1h.
Described oven temperature is preferably 90 ℃.
Described reactor compactedness is preferably 60%.
Described step (2) temperature of reaction is preferably 160-180 ℃.
The preparation method of nano crystal boehmite among the present invention was divided into for two steps, and the first step is a hydrolysis reaction; This step key be the control of the mol ratio and the temperature of reaction of distilled water and aluminum isopropylate.Second step was a hydro-thermal reaction, desciccate is added autoclave with distilled water carry out hydro-thermal reaction, increase with the pressure of the rising of temperature and the spontaneous formation of water vapour, prepare even particle size, good dispersity, do not have to reunite or few the reunion, the nm boehmite particle that degree of crystallinity is higher, this step most critical be the control in temperature of reaction and reaction times.
Than existing material and technology, the present invention has following advantage and beneficial effect:
(1) the nano crystal boehmite product degree of crystallinity height of the present invention's preparation, regular crystal forms, even particle size, dispersion condition is simple, favorable dispersity.
(2) the prepared nano crystal boehmite of the present invention has good water dispersible, and its dispersion condition is simple, and particle size distribution is even, does not have obvious agglomeration.
(3) the present invention on the basis of hydrolysis of alkoxide in conjunction with hydro-thermal synthesis process, hydrothermal synthesis method is a kind of main method for preparing high quality crystal, in High Temperature High Pressure solution, material has very high reactive behavior, the material that synthesizes stable chemical performance easily, under liquid condition, system is in the non-state that is forced to, and the crystalline habit can fully appear.
Description of drawings
Fig. 1 is the XRD figure of embodiment 1 products obtained therefrom.
Fig. 2 is the Ma Erwen sreen analysis figure after embodiment 1 products obtained therefrom disperses.
Embodiment
Below in conjunction with specific embodiment the present invention's preparation is further described, but the present invention's scope required for protection is not limited to the related scope of embodiment.
(1) hydrolysis reaction: aluminum isopropylate 10g, distilled water 80ml, 70 ℃ of reaction 1h filter, and 90 ℃ of dry 12h make hydrated aluminum oxide.
(2) hydro-thermal reaction: get the hydrated aluminum oxide 5g that step (1) makes, distilled water 60ml puts into band teflon-lined reactor, 60%, 150 ℃ of reaction of reactor compactedness 4h, and filtration drying gets nano crystal boehmite.
(3) disperse: get the nano crystal boehmite 1g that step (1) makes, distilled water 100ml, the high speed dispersion clarifixator disperseed one hour, and adding rare nitric acid to colloidal sol pH value is 3-4, obtains the homogeneous stable sols.
Nano particle diameter is little, and the surface energy height has the trend of spontaneous reunion, and the existence of reuniting will influence the performance of nano-powder advantage greatly, so dispersion and the stability of nano-powder in liquid phase medium is very important.After testing, the prepared nm boehmite of the present invention has good water dispersible, and dispersion condition is simple, and powder directly is evenly distributed, and does not have obvious agglomeration, and median size is about 100nm.The present invention is by synthetic this step of hydro-thermal, and the boehmite that makes has very high degree of crystallinity, and the prepared boehmite of traditional method is the pseudo-boehmite attitude, and degree of crystallinity is very low, even is metamict.
As can be seen from Figure 1, the diffraction peak peak shape of the boehmite of preparation is complete, and peak shape is narrow, and relative intensity is higher and sharp-pointed, illustrates that products obtained therefrom degree of crystallinity is higher, and crystallization is more complete.
As can be seen from Figure 2, grain diameter is normal distribution, and it is more even to distribute, and disperses relatively goodly, and it is existing not bright obviously not reunite, and median size is about 100nm.
This embodiment other with embodiment 1, change the adding distil water add-on, the mol ratio that makes water and aluminum isopropylate is 50: 1; Step (2) hydro-thermal reaction time lengthening makes nano crystal boehmite equally to 12h.
(1) hydrolysis reaction: aluminum isopropylate 10g, distilled water 80ml, 70 ℃ of reaction 1h filter 90 ℃ of dry 12h.
(2) hydro-thermal reaction: hydrated aluminum oxide 5g, distilled water 60ml, 60%, 200 ℃ of reaction of reactor compactedness 4h, filtration drying gets nano crystal boehmite.
(3) disperse: boehmite 1g, distilled water 100ml, the high speed dispersion clarifixator disperseed one hour, added rare nitric acid to colloidal sol pH value and was 3-4.
Embodiment 4
This embodiment other with embodiment 3, change the adding distil water add-on, the mol ratio that makes water and aluminum isopropylate is 150: 1; Step (2) hydro-thermal reaction time lengthening makes nano crystal boehmite equally to 8h.
Can better implement the present invention as mentioned above.
Claims (6)
1, a kind of preparation method of nano crystal boehmite is characterized in that comprising the steps:
(1) hydrolysis reaction: distilled water and boundary's Tripropoxyaluminum by 50～150: 1 mixed in molar ratio, are heated to 70-90 ℃, reaction 1～2h, filtering reaction product, 80-90 ℃ of dry 8-12h in baking oven;
(2) hydro-thermal reaction is packed desciccate in the step (1) in the autoclave into, stays water as reaction medium with steaming, and the reactor compactedness is 60%-80%, and temperature of reaction is 150-200 ℃, and reaction times 4-12h makes nano crystal boehmite.
2, the preparation method of nano crystal boehmite according to claim 1, the mol ratio that it is characterized in that described distilled water and aluminum isopropylate is 80～110: 1.
3, the preparation method of nano crystal boehmite according to claim 1 is characterized in that described step (1) reaction times is 1h.
4,, it is characterized in that oven temperature is 90 ℃ in the described step (1) according to the preparation method of each described nano crystal boehmite of claim 1～3.
5,, it is characterized in that described reactor compactedness is 60% according to the preparation method of each described nano crystal boehmite of claim 1～3.
6, the preparation method of nano crystal boehmite according to claim 1 is characterized in that described step (2) temperature of reaction is 160-180 ℃.
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| CNB2007100311640A CN100569650C (en) | 2007-10-30 | 2007-10-30 | A kind of preparation method of nano crystal boehmite |
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| CNB2007100311640A CN100569650C (en) | 2007-10-30 | 2007-10-30 | A kind of preparation method of nano crystal boehmite |
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| CN101177290A CN101177290A (en) | 2008-05-14 |
| CN100569650C true CN100569650C (en) | 2009-12-16 |
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Families Citing this family (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102815732A (en) * | 2012-09-20 | 2012-12-12 | 天津碧海蓝天水性高分子材料有限公司 | Nanometer boehmite having high dispersion performance, and preparation method and application of nanometer boehmite |
| TWI555704B (en) * | 2013-12-26 | 2016-11-01 | Univ Kun Shan | Method of manufacturing montmorillonite composite material |
| CN104944453B (en) * | 2015-06-12 | 2017-04-19 | 安徽壹石通材料科技股份有限公司 | Preparation method of boehmite coated alumina material |
| CN105836770B (en) * | 2016-03-24 | 2017-11-21 | 中铝山东有限公司 | A kind of preparation method of high temperature resistant boehmite |
| CN106903765B (en) * | 2017-03-07 | 2018-01-26 | 东北林业大学 | The fire retarding wood that a kind of method for improving fire-retarding of wood performance and this method obtain |
| CN111217382B (en) * | 2018-11-25 | 2021-10-08 | 中国科学院大连化学物理研究所 | Nanowire-type spherical alumina with large length-diameter ratio and preparation method thereof |
| CN111453751B (en) * | 2020-04-08 | 2021-09-10 | 安徽壹石通新能源材料有限公司 | Preparation method of high-purity nano boehmite |
| CN112062145B (en) * | 2020-09-09 | 2021-09-10 | 中国科学院过程工程研究所 | Alumina and preparation method and application 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 |
| CN113620328B (en) * | 2021-08-17 | 2023-07-11 | 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 nanocrystalline |
-
2007
- 2007-10-30 CN CNB2007100311640A patent/CN100569650C/en not_active Expired - Fee Related
Non-Patent Citations (2)
| Title |
|---|
| 常压制备针状勃姆石(r-AlOOH)超微粒子. 吴永祥等.上海师范大学学报(自然科学版)，第27卷第4期. 1998 |
| 常压制备针状勃姆石(r-AlOOH)超微粒子. 吴永祥等.上海师范大学学报(自然科学版)，第27卷第4期. 1998 * |
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