CN102689913B - Method for preparing gamma-Al2O3 through molecular self-assembly - Google Patents
Method for preparing gamma-Al2O3 through molecular self-assembly Download PDFInfo
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- CN102689913B CN102689913B CN201110068751.3A CN201110068751A CN102689913B CN 102689913 B CN102689913 B CN 102689913B CN 201110068751 A CN201110068751 A CN 201110068751A CN 102689913 B CN102689913 B CN 102689913B
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Abstract
Belonging to the field of preparation techniques of material chemistry, the invention relates to a method for preparing gamma-Al2O3 through molecular self-assembly. The method comprises: taking a different aluminum source as a reactant, adding a surfactant, controlling the reaction temperature for a period of reaction, conducting sufficient mixing to form a clarified solution, carrying out heating to a certain temperature, adding an alkaline solution for a period of reaction, then performing aging, washing, hydrothermal treatment, drying, calcination and other processes, thus obtaining gamma-Al2O3. The invention provides a new raw material and method for preparation of gamma-Al2O3.
Description
Technical field
The present invention relates to one utilizes molecular self-assembling to prepare γ-Al
2o
3method, belong to materials chemistry preparing technical field.
Background technology
γ-Al
2o
3it is the most widely used support of the catalyst of modern oil-refining chemical technical field, also directly can be used as the binding agent of producing olefin hydrocarbon with alcohols dehydration catalyzer, car tail gas purificant, petroleum cracking catalyzer, molecular sieve and environment heavy metal absorbent etc., be used widely in industries such as petrochemical complex, fine ceramics, refractory materials, microelectronics, environmental protection at present.
At present, the preparation method of aluminum oxide is more, and CN1323741A adopts sodium hydroxide alkali fusion bauxite technique to prepare aluminum oxide; CN1243101A prepares γ-Al by adopting Alumina gel preparation, thermal treatment and the step such as oven dry, roasting
2o
3; CN1401575A describes and adopts sol-gel method and supercritical fluid drying, prepares γ-Al through 900 DEG C of roastings
2o
3particle; CN1420082A adopts sodium metaaluminate to be aluminium source, passes into CO
2gas mixture prepares aluminum oxide; CN101880050A describes and adopts sodium hydroxide, water, catalyzer, Trimethylamine 99 and aluminium flake after 120 ~ 180 DEG C of reactions, obtains aluminium sesquioxide through high-temperature roasting; It is aluminium source that CN101829552A describes with aluminum nitrate, adopts sluggish precipitation to prepare aluminum oxide.
But different raw materials, Method and process route can prepare the γ-Al of different in kind
2o
3.Molecular self-assembling method, mainly utilize the structure-directing effect of block nonionogenic tenside, the weak force non-chemically set up by the hydrogen bond, Van der Waals force etc. that are formed between target molecule and automatic synthesizing ordered organized product, control the molecular structure of final product with this.
The present invention utilizes this principle of molecular self-assembling just, adopts molecular self-assembling method to prepare γ-Al
2o
3, and then the controlled orderly γ-Al of implementation structure
2o
3, be γ-Al
2o
3preparation provide a kind of feasible method.
Summary of the invention
One is the object of the present invention is to provide to utilize molecular self-assembling to prepare γ-Al
2o
3method.For γ-Al
2o
3preparation provide a kind of new method and raw material, widened the range of application of polymeric aluminum chlorides solution in the field such as material, catalysis simultaneously.
Main technical content of the present invention is: using aluminium source as reactant, add tensio-active agent, control temperature of reaction and react for some time, be thoroughly mixed to form clear soln, be heated to certain temperature, add basic solution, after reaction for some time, obtain γ-Al through processes such as overaging, washing, hydrothermal treatment consists, drying, roastings
2o
3product.
Aluminium source of the present invention can be the homemade polymerize aluminum chloride in laboratory, Al
bcontent is 50 ~ 90%; Also can be AlCl
3, Al (NO
3)
3, Al
2(SO
4)
3etc. different aluminium sources, the concentration range 0.1 ~ 0.5mol/L of aluminum solutions.
Tensio-active agent of the present invention is the nonionogenic tensides such as L64, L65, F68, and concentration is 0.1 ~ 0.7%.
Range of reaction temperature of the present invention is 20 ~ 45 DEG C.
Reaction times of the present invention is 24 ~ 48h.
Basic solution of the present invention can be ammoniacal liquor or sodium hydroxide solution, and concentration of lye is 2 ~ 6%.
Digestion time of the present invention is 6 ~ 24h.
According to method provided by the invention, described in be separated into the known technology of this area, as filtered or the method for centrifugation.
According to method provided by the invention, described washing, drying and roasting method are for preparing pseudo-boehmite conventional process.As can oven dry, air blast and cryodesiccated method be used.Maturing temperature is 450 ~ 750 DEG C.
γ-the Al that method provided by the invention is prepared
2o
3can be used as sorbent material and support of the catalyst.
Embodiment
Below in conjunction with preparation method of the present invention, the specific embodiment of the present invention is described.
Example 1:
In 0.2mol/L polymeric aluminum chlorides solution, add L64 tensio-active agent at constant temperature 40 DEG C, reaction 36h, obtains clear soln, then 0.5mol/L ammoniacal liquor is dripped, produce white precipitate, leave standstill aging 15h, filtration centrifugal with refrigerated centrifuge, and use deionized water wash filter cake, then filter cake is put into 100 DEG C of loft drier and dries 6h, then at 500 DEG C roasting 8h, obtain γ-Al
2o
3product.
Example 2:
In 0.3mol/L alum liquor, add L64 tensio-active agent at constant temperature 40 DEG C, reaction 36h, obtains clear soln, then 0.5mol/L ammoniacal liquor is dripped, produce white precipitate, leave standstill aging 15h, filtration centrifugal with refrigerated centrifuge, and use deionized water wash filter cake, then filter cake is put into 100 DEG C of loft drier and dries 6h, then at 500 DEG C roasting 8h, obtain γ-Al
2o
3product.
Example 3:
In 0.3mol/L polymeric aluminum chlorides solution, add L65 tensio-active agent at constant temperature 45 DEG C, reaction 40h, obtains clear soln, then 0.5mol/L ammoniacal liquor is dripped, produce white precipitate, leave standstill aging 20h, filtration centrifugal with refrigerated centrifuge, and use deionized water wash filter cake, then filter cake is put into 100 DEG C of loft drier and dries 6h, then at 600 DEG C roasting 8h, obtain γ-Al
2o
3product.
Example 4:
In 0.2mol/L polymeric aluminum chlorides solution, add F68 tensio-active agent at constant temperature 40 DEG C, reaction 36h, obtains clear soln, then 0.5mol/L ammoniacal liquor is dripped, produce white precipitate, leave standstill aging 15h, filtration centrifugal with refrigerated centrifuge, and use deionized water wash filter cake, then filter cake is put into 100 DEG C of loft drier and dries 6h, then at 500 DEG C roasting 8h, obtain γ-Al
2o
3product.
Example 5:
In 0.1mol/L liquor alumini chloridi, add L65 tensio-active agent at constant temperature 30 DEG C, reaction 48h, obtains clear soln, then 0.5mol/L sodium hydroxide solution is dripped, produce white precipitate, leave standstill aging 20h, with centrifuge, filtration, and use deionized water wash filter cake, then filter cake is put into seasoning 24h, then at 600 DEG C roasting 8h, obtain γ-Al
2o
3product.
Example 6:
In 0.1mol/L aluminum nitrate solution, add F68 tensio-active agent at constant temperature 30 DEG C, reaction 48h, obtains clear soln, then 0.5mol/L sodium hydroxide solution is dripped, produce white precipitate, leave standstill aging 20h, with centrifuge, filtration, and use deionized water wash filter cake, then filter cake is put into seasoning 24h, then at 600 DEG C roasting 8h, obtain γ-Al
2o
3product.
Claims (2)
1. one kind utilizes molecular self-assembling to prepare γ-Al
2o
3method, it is characterized in that: using aluminium source as reactant, add tensio-active agent, controlling temperature of reaction is 20 ~ 45 DEG C of reaction 24 ~ 48h, be thoroughly mixed to form clear soln, be heated to certain temperature, add basic solution, after reaction 24 ~ 48h, obtain through overaging 6 ~ 24h, washing, hydrothermal treatment consists, drying, 450 ~ 750 DEG C of roastings the γ-Al being used as sorbent material and support of the catalyst
2o
3product, wherein, described aluminium source be laboratory from preparing polymeric aluminium chloride, Al
bcontent is 50 ~ 90% or AlCl
3, Al (NO
3)
3, Al
2(SO
4)
3; Described tensio-active agent is L64, L65 or F68, and concentration is 0.1 ~ 0.7%; Described basic solution is ammoniacal liquor or sodium hydroxide solution, and concentration is 2 ~ 6%.
2. one according to claim 1 utilizes molecular self-assembling to prepare γ-Al
2o
3method, it is characterized in that, the concentration range 0.1 ~ 0.5mol/L of aluminum solutions.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201110068751.3A CN102689913B (en) | 2011-03-22 | 2011-03-22 | Method for preparing gamma-Al2O3 through molecular self-assembly |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201110068751.3A CN102689913B (en) | 2011-03-22 | 2011-03-22 | Method for preparing gamma-Al2O3 through molecular self-assembly |
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|---|---|
| CN102689913A CN102689913A (en) | 2012-09-26 |
| CN102689913B true CN102689913B (en) | 2015-01-28 |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103359765A (en) * | 2013-07-10 | 2013-10-23 | 华南理工大学 | Preparation method of micron gamma aluminum oxide with controllable morphology and mesoporous structure |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1803618A (en) * | 2005-01-11 | 2006-07-19 | 中国科学院大连化学物理研究所 | Process for preparing mesopored alumina |
Family Cites Families (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS58156531A (en) * | 1982-03-10 | 1983-09-17 | Nippon Light Metal Co Ltd | Preparation of aluminum hydroxide with low adhesive moisture |
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Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1803618A (en) * | 2005-01-11 | 2006-07-19 | 中国科学院大连化学物理研究所 | Process for preparing mesopored alumina |
Non-Patent Citations (2)
| Title |
|---|
| JP昭58-156531A 1983.09.17 * |
| 纳米纤维状γ-Al2O3粉体的制备与表征;张立岩等;《石油化工》;20041231;第33卷(第3期);全文 * |
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