CN102491390A - Method for preparing gamma-Al2O3 powder with combustion method - Google Patents
Method for preparing gamma-Al2O3 powder with combustion method Download PDFInfo
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- CN102491390A CN102491390A CN2011103908522A CN201110390852A CN102491390A CN 102491390 A CN102491390 A CN 102491390A CN 2011103908522 A CN2011103908522 A CN 2011103908522A CN 201110390852 A CN201110390852 A CN 201110390852A CN 102491390 A CN102491390 A CN 102491390A
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- powder
- combustion
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- heating
- al2o3 powder
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Abstract
The invention relates to a method for preparing gamma-Al2O3 powder with a combustion method. According to the invention, the gamma-Al2O3 powder material prepared by using the method is short in reaction time; and the puffy gamma-Al2O3 powder product can be prepared by controlling raw material proportion and solution pH value and combining with calcining temperature and constant-temperature calcining time after self-spreading combustion. The raw materials of the gamma-Al2O3 powder comprise Al(NO3)3.9H2O3 and C2H5NO2. The method comprises the following steps of: mixing Al(NO3)3.9H2O3 with C2H5NO2 in a molar ratio of 1: (1-4) in a ceramic crucible, and then adding a proper amount of distilled water; heating a mixed solution with a magnetic stirring apparatus with a heating function to 70 DEG C and evenly stirring; dropwise adding ammonia water and regulating the pH value of the mixed solution to be between 1 and 3; drying for 2 hours in an oven at the temperature of 110 DEG C so as to obtain sol; and heating the sol in a muffle furnace until self-spreading combustion happens, and calcining for 1-4 hours at the temperature of 700-850 DEG C, so as to obtain the puffy powder product, namely, the gamma-Al2O3 powder.
Description
Technical field
The present invention relates to a kind ofly prepare γ-Al with combustion method
2O
3The method of powder belongs to γ-Al
2O
3The preparing technical field of powder body material.
Background technology
Aluminum oxide (Al
2O
3) be a kind of high performance material that is widely used, have multiple crystal formation, γ-Al
2O
3Be wherein a kind of.γ-Al
2O
3Be a kind of porous solid material, belong to the tightly packed configuration of cube center of area, be similar to the structure of spinel.Because its specific surface area is big, the surface possesses characteristic such as acidity and is called as " activated alumina ", and extensive application in support of the catalyst is like the carrier of hydrogen cracking, hydrogenating desulfurization and the dehydrogenation catalyst in refining of petroleum field; Purifying vehicle exhaust, the support of the catalyst of Polymer Synthesizing etc.
Prepare γ-Al at present
2O
3Method mainly contain: chemical precipitation method, sol-gel method, hydrothermal method, microemulsion method etc., these methods, the complex technical process that has is prone to sneak into impurity; The synthetic product that has exists particle size big, and the serious and specific surface area of particle aggregation is generally lower etc.Combustion method is a kind of emerging method, comes into one's own day by day in the world in recent years, and develops rapidly.Combustion synthesis method is to utilize oxidation-reduction reaction between fuel (reductive agent) and the oxygenant to promote the carrying out that reacts; Institute's liberated heat impels the form automatic spreading of reaction with combustion wave; Along with the passing of combustion wave, the chemical reaction of accelerated reaction thing generates title product.Compare other method, combustion method prepare powder to have technology simple, and experimental period is short, and distribution of reaction products is even, and purity is high, and therefore characteristics such as its lytic activity height are obtaining using widely aspect the preparation oxide powder.
The present invention is with aluminum nitrate (Al (NO
3)
39H
2O
3) be oxygenant, glycocoll (C
2H
5NO
2) as incendiary material, adopt combustion method to prepare γ-Al
2O
3Powder has been confirmed preparation γ-Al
2O
3The optimum process condition of powder.
Summary of the invention
The purpose of this invention is to provide and a kind ofly prepare γ-Al with combustion method
2O
3The method of powder, γ-Al that this method of using makes
2O
3Powder body material; Because the reaction times is short, the severe impact of combustion gas flowing, helps the refinement of particle, has reduced interparticle reunion degree; Through control proportioning raw materials, pH value of solution value, combine γ-Al that calcining temperature and calcining at constant temperature time behind the setting self-propagating combustion can prepare puffy
2O
3The powder product.
For realizing above-mentioned purpose, the present invention adopts following technical scheme: raw material is Al (NO
3)
39H
2O
3, C
2H
5NO
2With mol ratio is 1: the Al (NO of (1～4)
3)
39H
2O
3With C
2H
5NO
2Be mixed in the ceramic crucible, add an amount of zero(ppm) water, mixing solutions with the magnetic stirring apparatus of band heating be heated to 70 ℃ and stir after; Pass through dropping ammonia; The pH value of regulating mixing solutions is between 1～3, and dry 2h obtains colloidal sol under 110 ℃ in baking oven, is placed on to be heated in the retort furnace self-propagating combustion to take place and calcine 1～4h at 700～850 ℃; Obtain bulk powdery product, i.e. γ-Al
2O
3Powder.
The present invention compares with existing preparation technology and has the following advantages:
1, it is simple to have technology, and preparation cycle is short, and equipment requirements is low, and productive rate is high, the uniform characteristics of distribution of reaction products, easy realization of industrial production.
2, the present invention is through control proportioning raw materials, pH value of solution value, combines to set γ-Al that after climing combustion calcining temperature and calcining at constant temperature time can prepare puffy
2O
3The powder product because the reaction times is short, the severe impact of combustion gas flowing, helps the refinement of particle, has reduced interparticle reunion degree, the control process easy handling.
Description of drawings
A among the figure, b and c are the γ-Al of corresponding embodiment 1,3 and 6
2O
3The X-ray diffraction spectrogram (XRD) of powder product.
Embodiment
Embodiment 1
A certain amount of Al (NO of difference weighing
3)
39H
2O
3And C
2H
5NO
2, make Al (NO
3)
39H
2O
3With C
2H
5NO
2Mol ratio be 1: 1, be mixed in the ceramic crucible, add an amount of zero(ppm) water; Mixing solutions with the magnetic stirring apparatus of band heating be heated to 70 ℃ and stir after, to said solution dropping ammonia, the pH=2 of regulator solution; Dry 2h obtains colloidal sol under 110 ℃ in baking oven; Be placed on and be heated to self-propagating combustion in the retort furnace, and continue to be heated to 800 ℃ of following calcination 3h, the XRD spectra analytical results shows that product is γ-Al
2O
3
Embodiment 2
A certain amount of Al (NO of difference weighing
3)
39H
2O
3And C
2H
5NO
2, make Al (NO
3)
39H
2O
3With C
2H
5NO
2Mol ratio be 1: 1, be mixed in the ceramic crucible, add an amount of zero(ppm) water; Mixing solutions with the magnetic stirring apparatus of band heating be heated to 70 ℃ and stir after, to said solution dropping ammonia, the pH=1 of regulator solution; Dry 2h obtains colloidal sol under 110 ℃ in baking oven; Be placed on and be heated to self-propagating combustion in the retort furnace, and continue to be heated to 750 ℃ of following calcination 4h, the XRD spectra analytical results shows that product is γ-Al
2O
3
Embodiment 3
A certain amount of Al (NO of difference weighing
3)
39H
2O
3And C
2H
5NO
2, make Al (NO
3)
39H
2O
3With C
2H
5NO
2Mol ratio be 1: 2, be mixed in the ceramic crucible, add an amount of zero(ppm) water; Mixing solutions with the magnetic stirring apparatus of band heating be heated to 70 ℃ and stir after, to said solution dropping ammonia, the pH=2 of regulator solution; Dry 2h obtains colloidal sol under 110 ℃ in baking oven; Be placed on and be heated to self-propagating combustion in the retort furnace, and continue to be heated to 800 ℃ of following calcination 2h, the XRD spectra analytical results shows that product is γ-Al
2O
3
Embodiment 4
A certain amount of Al (NO of difference weighing
3)
39H
2O
3And C
2H
5NO
2, make Al (NO
3)
39H
2O
3With C
2H
5NO
2Mol ratio be 1: 1, be mixed in the ceramic crucible, add an amount of zero(ppm) water; Mixing solutions with the magnetic stirring apparatus of band heating be heated to 70 ℃ and stir after, to said solution dropping ammonia, the pH=3 of regulator solution; Dry 2h obtains colloidal sol under 110 ℃ in baking oven; Be placed on and be heated to self-propagating combustion in the retort furnace, and continue to be heated to 750 ℃ of following calcination 3h, the XRD spectra analytical results shows that product is γ-Al
2O
3
Embodiment 5
A certain amount of Al (NO of difference weighing
3)
39H
2O
3And C
2H
5NO
2, make Al (NO
3)
39H
2O
3With C
2H
5NO
2Mol ratio be 1: 3, be mixed in the ceramic crucible, add an amount of zero(ppm) water; Mixing solutions with the magnetic stirring apparatus of band heating be heated to 70 ℃ and stir after, to said solution dropping ammonia, the pH=3 of regulator solution; Dry 2h obtains colloidal sol under 110 ℃ in baking oven; Be placed on and be heated to self-propagating combustion in the retort furnace, and continue to be heated to 850 ℃ of following calcination 1h, the XRD spectra analytical results shows that product is γ-Al
2O
3
Embodiment 6
A certain amount of Al (NO of difference weighing
3)
39H
2O
3And C
2H
5NO
2, make Al (NO
3)
39H
2O
3With C
2H
5NO
2Mol ratio be 1: 4, be mixed in the ceramic crucible, add an amount of zero(ppm) water; Mixing solutions with the magnetic stirring apparatus of band heating be heated to 70 ℃ and stir after, to said solution dropping ammonia, the pH=2 of regulator solution; Dry 2h obtains colloidal sol under 110 ℃ in baking oven; Be placed on and be heated to self-propagating combustion in the retort furnace, and continue to be heated to 700 ℃ of following calcination 3h, the XRD spectra analytical results shows that product is γ-Al
2O
3
Claims (4)
1. one kind prepares γ-Al with combustion method
2O
3The method of powder is characterized in that, raw material is Al (NO
3)
39H
2O
3, C
2H
5NO
2, with the Al (NO of suitable mol ratio
3)
39H
2O
3With C
2H
5NO
2Be mixed in the ceramic crucible, add an amount of zero(ppm) water, and with after the magnetic stirring apparatus heating of being with heating and stirring; Pass through dropping ammonia; Regulate the pH value of mixing solutions, drying obtains colloidal sol in baking oven, is placed on to be heated to the generation self-propagating combustion in the retort furnace and to calcine in certain temperature; Obtain bulk powdery product, i.e. γ-Al
2O
3Powder.
2. require describedly to prepare γ-Al according to right 1 with combustion method
2O
3The method of powder is characterized in that, Al (NO
3)
39H
2O
3With C
2H
5NO
2Mol ratio be 1: (1～4), add an amount of zero(ppm) water, mixing solutions is heated to 70 ℃ and stir with the magnetic stirring apparatus of band heating.
3. require describedly to prepare γ-Al according to right 1 with combustion method
2O
3The method of powder is characterized in that, through dropping ammonia, the pH value of regulating mixing solutions places baking oven between 1～3, and 110 ℃ of following dry 2h obtain colloidal sol.
4. require describedly to prepare γ-Al according to right 1 with combustion method
2O
3The method of powder body material is characterized in that, said calcining temperature is between 700～850 ℃, calcination time 1～4h.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111747434A (en) * | 2020-08-03 | 2020-10-09 | 辽宁石油化工大学 | Method for preparing modified gamma-Al 2O3 powder by microwave-assisted combustion method |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1843919A (en) * | 2006-05-17 | 2006-10-11 | 北京嘉益亨元科技发展有限公司 | Method for preparing superfine powder of alumina by gas atomization method |
| CN101518734A (en) * | 2009-03-27 | 2009-09-02 | 华中科技大学 | La, Mn modified Pd/gamma-Al2O3 catalyst and preparation method thereof |
| US20110204293A1 (en) * | 2010-02-24 | 2011-08-25 | William Peter Addiego | Gold catalysts for co oxidation and water gas shift reactions |
-
2011
- 2011-12-01 CN CN2011103908522A patent/CN102491390A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1843919A (en) * | 2006-05-17 | 2006-10-11 | 北京嘉益亨元科技发展有限公司 | Method for preparing superfine powder of alumina by gas atomization method |
| CN101518734A (en) * | 2009-03-27 | 2009-09-02 | 华中科技大学 | La, Mn modified Pd/gamma-Al2O3 catalyst and preparation method thereof |
| US20110204293A1 (en) * | 2010-02-24 | 2011-08-25 | William Peter Addiego | Gold catalysts for co oxidation and water gas shift reactions |
Non-Patent Citations (4)
| Title |
|---|
| 《无机材料学报》 20050531 储刚等 燃烧法合成的纳米alpha-Al2O3晶格热膨胀系数研究 第756页第1段至第2段 1-4 第20卷, 第3期 * |
| 《物理化学学报》 20090731 尹晓光等 alpha-Al2O3纳米片的自燃烧法控制合成及其抛光性能 摘要及第1444页右栏第2段 1-4 第25卷, 第7期 * |
| 储刚等: "燃烧法合成的纳米α-Al2O3晶格热膨胀系数研究", 《无机材料学报》, vol. 20, no. 3, 31 May 2005 (2005-05-31) * |
| 尹晓光等: "α-Al2O3纳米片的自燃烧法控制合成及其抛光性能", 《物理化学学报》, vol. 25, no. 7, 31 July 2009 (2009-07-31), pages 1444 - 2 * |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111747434A (en) * | 2020-08-03 | 2020-10-09 | 辽宁石油化工大学 | Method for preparing modified gamma-Al 2O3 powder by microwave-assisted combustion method |
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Application publication date: 20120613 |