CN102701247B - Preparation method of mesoporous spherical aluminum oxide - Google Patents
Preparation method of mesoporous spherical aluminum oxide Download PDFInfo
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- CN102701247B CN102701247B CN201210139705.2A CN201210139705A CN102701247B CN 102701247 B CN102701247 B CN 102701247B CN 201210139705 A CN201210139705 A CN 201210139705A CN 102701247 B CN102701247 B CN 102701247B
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Abstract
The invention discloses a preparation method of mesoporous spherical aluminum oxide. The mesoporous spherical aluminum oxide with low price is combined by utilizing industrial aluminum sol as an aluminum source, P123 as a surfactant and ammonium bicarbonate or urea as a neutralizer. A BET test method tests that the BET of the mesoporous spherical aluminum oxide obtained in the method is 186.7-270m<2>/g, and the bore diameter is 5.6nm. Compared with the prior art, the preparation method for combining the aluminum oxide with high BET remarkably reduces cost, is production-environment-friendly and is beneficial for improvement and protection of environment.
Description
Technical field
The present invention relates to a kind of preparation of aluminium sesquioxide, relate in particular to a kind of preparation method of mesoporous sphere aluminium sesquioxide.
Background technology
The aluminum oxide of high-ratio surface is a kind of important support of the catalyst, sorbent material, and its preparation method enjoys attention, and the alumina product of the various high-specific surface areas of large-scale commercial production is widely applied.Chinese patent 01126878.6 once utilized tensio-active agent P123 and isobutanol aluminum in organic solvent, had synthesized spherical porous shape alumina globule under the hydrochloric acid catalysis effect.Comparatively speaking, the isobutanol aluminum price is higher, and this invents organic solvent used and also cry expensively, and toxicity is higher, therefore select more cheap aluminium source and eco-friendly solvent, the high-specific surface area aluminium sesquioxide that synthetic cost is lower will be one of direction promoted this material industry application.
Summary of the invention
For the deficiencies in the prior art, the problem to be solved in the present invention is to provide a kind of preparation method of mesoporous sphere aluminium sesquioxide.
The preparation method of mesoporous sphere aluminium sesquioxide of the present invention, step is:
1) tensio-active agent P123 is dissolved in dehydrated alcohol, then (molecular formula of aluminium colloidal sol is Al (OH) to add 20wt% butt aluminium colloidal sol
2.4cl
0.6), fully mix;
2) above-mentioned mixed solution is put into to watch-glass, volatilization ethanol, become thick solid naturally;
3) will with above-mentioned thick solid abrasive, mix over bicarbonate of ammonia or the urea of neutralization reaction amount 50wt%;
4) above-mentioned grinding mixture is placed into to 500 ± 80 ℃ of roasting 2～5h in retort furnace, obtains the white solid powder, be the mesoporous sphere aluminium sesquioxide.
In the preparation method of above-mentioned mesoporous sphere aluminium sesquioxide, the ratio of mixture of described tensio-active agent P123 and dehydrated alcohol is 1～4 gram: 50ml preferably.
In the preparation method of above-mentioned mesoporous sphere aluminium sesquioxide, the weight ratio of described tensio-active agent P123 and butt aluminium colloidal sol is 1～4:1 preferably.
In the preparation method of above-mentioned mesoporous sphere aluminium sesquioxide, the volume ratio of described dehydrated alcohol and 20wt% butt aluminium colloidal sol is 9～12:1, preferably 10:1.
In the preparation method of above-mentioned mesoporous sphere aluminium sesquioxide, the butt purity (%) >=99.9 of butt aluminium colloidal sol, the solvent of aluminium colloidal sol is water.
In the preparation method of above-mentioned mesoporous sphere aluminium sesquioxide, preferably 500 ℃ of the maturing temperatures in described retort furnace, the preferred 2h of roasting time.
The present invention utilizes industrial aluminum colloidal sol for the aluminium source, and P123 is tensio-active agent, and bicarbonate of ammonia or urea are neutralizing agent, has synthesized more cheap mesoporous sphere aluminium sesquioxide; The mesoporous sphere aluminium sesquioxide specific surface area that BET specific surface area method of testing test the inventive method obtains is 186.7-270m
2/ g, about 5.6nm left and right, aperture.Method than prior art synthesizing high specific surface area aluminium sesquioxide has obviously reduced cost, and production environment is more friendly, is more conducive to environmental improvement and protection.
The accompanying drawing explanation
Fig. 1: 1g tensio-active agent P123 obtains aluminium sesquioxide sample well structure iron
Wherein: surface-area (Surface Area)=186.7m
2/ g, volume of voids (Pore Volume)=0.23cc/g, aperture (Pore Diameter Dv (d))=6.0nm.
Fig. 2: 2g tensio-active agent P123 obtains aluminium sesquioxide sample well structure iron
Wherein: surface-area (Surface Area)=203.3m
2/ g, volume of voids (Pore Volume)=0.40cc/g, aperture (Pore Diameter Dv (d))=5.6nm.
Fig. 3: 4g tensio-active agent P123 obtains aluminium sesquioxide sample well structure iron
Wherein: surface-area (Surface Area)=269.5m
2/ g, volume of voids (Pore Volume)=0.31cc/g, aperture (Pore Diameter Dv (d))=5.6nm.
Fig. 4: 2g tensio-active agent P123 obtains aluminium sesquioxide sample high-resolution electron microscopy photo (60nm).
Fig. 5: 2g tensio-active agent P123 obtains aluminium sesquioxide sample high-resolution electron microscopy photo (100nm).
Embodiment
Embodiment 1
1,1 gram P123 is dissolved in to the 50ml dehydrated alcohol, adds 1g butt aluminium colloidal sol (5ml weight ratio 20% aluminium sol solution).
2, mixed solution is put into to watch-glass, volatilization ethanol, become thick solid naturally.
3, the urea added over neutralization reaction 50wt% mixes with above-mentioned solid abrasive.
4, mixture is placed into to 500 ° of C roasting 2h of retort furnace, obtains the white solid powder, be the mesoporous sphere aluminium sesquioxide.(see figure 1)
Embodiment 2
1) 2 gram tensio-active agent P123 are dissolved in the 50ml dehydrated alcohol, then add 1 gram 20wt% butt aluminium colloidal sol, fully mix;
2) above-mentioned mixed solution is put into to watch-glass, volatilization ethanol, become thick solid naturally;
3) will with above-mentioned thick solid abrasive, mix over the urea of neutralization reaction amount 50wt%;
4) above-mentioned grinding mixture is placed into to 500 ℃ of roasting 2h in retort furnace, obtains the white solid powder, be the mesoporous sphere aluminium sesquioxide.(seeing Fig. 2,4,5)
Embodiment 3
1) 4 gram tensio-active agent P123 are dissolved in the 50ml dehydrated alcohol, then add 1 gram 20wt% butt aluminium colloidal sol, fully mix;
2) above-mentioned mixed solution is put into to watch-glass, volatilization ethanol, become thick solid naturally;
3) will with above-mentioned thick solid abrasive, mix over the urea of neutralization reaction amount 50wt%;
4) above-mentioned grinding mixture is placed into to 500 ℃ of roasting 2h in retort furnace, obtains the white solid powder, be the mesoporous sphere aluminium sesquioxide.(see figure 3)
Embodiment 4
1) 2 gram tensio-active agent P123 are dissolved in the 50ml dehydrated alcohol, then add 1 gram 20wt% butt aluminium colloidal sol, fully mix;
2) above-mentioned mixed solution is put into to watch-glass, volatilization ethanol, become thick solid naturally;
3) will with above-mentioned thick solid abrasive, mix over the bicarbonate of ammonia of neutralization reaction amount 50wt%;
4) above-mentioned grinding mixture is placed into to 500 ℃ of roasting 2h in retort furnace, obtains the white solid powder, be the mesoporous sphere aluminium sesquioxide.
Embodiment 5
1) 4 gram tensio-active agent P123 are dissolved in the 50ml dehydrated alcohol, then add 1 gram 20wt% butt aluminium colloidal sol, fully mix;
2) above-mentioned mixed solution is put into to watch-glass, volatilization ethanol, become thick solid naturally;
3) will with above-mentioned thick solid abrasive, mix over the bicarbonate of ammonia of neutralization reaction amount 50wt%;
4) above-mentioned grinding mixture is placed into to 550 ℃ of roasting 3h in retort furnace, obtains the white solid powder, be the mesoporous sphere aluminium sesquioxide.
Embodiment 6
1) 3 gram tensio-active agent P123 are dissolved in the 50ml dehydrated alcohol, then add 1 gram 20wt% butt aluminium colloidal sol, fully mix;
2) above-mentioned mixed solution is put into to watch-glass, volatilization ethanol, become thick solid naturally;
3) will with above-mentioned thick solid abrasive, mix over the bicarbonate of ammonia of neutralization reaction amount 50wt%;
4) above-mentioned grinding mixture is placed into to 450 ℃ of roasting 5h in retort furnace, obtains the white solid powder, be the mesoporous sphere aluminium sesquioxide.
Claims (1)
1. the preparation method of a mesoporous sphere aluminium sesquioxide, step is:
1) tensio-active agent P123 is dissolved in dehydrated alcohol, the ratio of mixture that makes tensio-active agent P123 and dehydrated alcohol is 1～4 gram: 50mL, add again 20 wt % butt aluminium colloidal sols, making the weight ratio of tensio-active agent P123 and butt aluminium colloidal sol is 1～4:1, the volume ratio of dehydrated alcohol and 20 wt % butt aluminium colloidal sols is 10:1, fully mixes;
2) above-mentioned mixed solution is put into to watch-glass, volatilization ethanol, become thick solid naturally;
3) will with above-mentioned thick solid abrasive, mix over bicarbonate of ammonia or the urea of neutralization reaction amount 50wt%;
4) above-mentioned grinding mixture is placed into to 500 ℃ of roasting 2h in retort furnace, obtains the white solid powder, be the mesoporous sphere aluminium sesquioxide.
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| CN102701247A CN102701247A (en) | 2012-10-03 |
| CN102701247B true CN102701247B (en) | 2014-01-01 |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH05105425A (en) * | 1991-10-16 | 1993-04-27 | Matsushita Electric Works Ltd | Production of aluminum oxide powder |
| CN102219242B (en) * | 2010-04-15 | 2013-01-09 | 中国石油化工股份有限公司 | Method for preparing mesoporous aluminum oxide |
| CN101863499B (en) * | 2010-05-31 | 2012-10-24 | 中南大学 | Preparation method of macroporous-mesoporous alumina |
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Granted publication date: 20140101 Termination date: 20140508 |