CN102701247A - Preparation method of mesoporous spherical aluminum oxide - Google Patents
Preparation method of mesoporous spherical aluminum oxide Download PDFInfo
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- CN102701247A CN102701247A CN2012101397052A CN201210139705A CN102701247A CN 102701247 A CN102701247 A CN 102701247A CN 2012101397052 A CN2012101397052 A CN 2012101397052A CN 201210139705 A CN201210139705 A CN 201210139705A CN 102701247 A CN102701247 A CN 102701247A
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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 catalyst carrier, sorbent material, and its preparation method enjoys attention, and the alumina product of the various high-specific surface areas of large-scale commercial prodn has obtained widespread use.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 should also be costliness by the used organic solvent of invention, and toxicity is higher; Therefore select cheap aluminium source and eco-friendly solvent, the high-specific surface area aluminium sesquioxide that synthetic cost is lower will be to promote one of direction that this material industry is used.
Summary of the invention
To the deficiency of prior art, the problem that the present invention will solve provides a kind of preparation method of mesoporous sphere aluminium sesquioxide.
The preparation method of mesoporous sphere aluminium sesquioxide according to the invention, step is:
1) tensio-active agent P123 is dissolved in the absolute ethyl alcohol, (molecular formula of aluminium colloidal sol is Al (OH) to add 20wt% butt aluminium colloidal sol again
2.4Cl
0.6), thorough mixing;
2) above-mentioned mixed solution is put into watch-glass, volatilization ethanol becomes thick solid naturally;
3) will mix with above-mentioned thick solid abrasive above bicarbonate of ammonia or the urea of neutralization reaction amount 50wt%;
4) above-mentioned grinding mixture is placed into 500 ± 80 ℃ of roasting 2～5h in the retort furnace, obtains the white solid powder, be the mesoporous sphere aluminium sesquioxide.
Among the preparation method of above-mentioned mesoporous sphere aluminium sesquioxide, the ratio of mixture of said tensio-active agent P123 and absolute ethyl alcohol is 1～4 gram: 50ml preferably.
Among the preparation method of above-mentioned mesoporous sphere aluminium sesquioxide, the weight ratio of said tensio-active agent P123 and butt aluminium colloidal sol is 1～4:1 preferably.
Among the preparation method of above-mentioned mesoporous sphere aluminium sesquioxide, the volume ratio of said absolute ethyl alcohol and 20wt% butt aluminium colloidal sol is 9～12:1, preferably 10:1.
Among 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 a water.
Among the preparation method of above-mentioned mesoporous sphere aluminium sesquioxide, preferred 500 ℃ of the maturing temperature in the said retort furnace, the preferred 2h of roasting time.
The present invention utilizes industrial aluminum colloidal sol to be the aluminium source, and P123 is a tensio-active agent, and bicarbonate of ammonia or urea are neutralizing agent, has synthesized 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 is about the about 5.6nm in aperture.Method than prior art synthesizing high specific surface area aluminium sesquioxide has obviously reduced cost, and production environment is friendly more, is more conducive to environmental improvement and protection.
Description of drawings
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 the 50ml absolute ethyl alcohol, adds 1g butt aluminium colloidal sol (5ml weight ratio 20% aluminium sol solution).
2, mixed solution is put into watch-glass, volatilization ethanol becomes thick solid naturally.
3, the urea that adds above neutralization reaction 50wt% mixes with above-mentioned solid abrasive.
4, mixture is placed into 500 ° of C roastings of retort furnace 2h, obtains the white solid powder, be the mesoporous sphere aluminium sesquioxide.(see figure 1)
Embodiment 2
1) 2 gram tensio-active agent P123 is dissolved in the 50ml absolute ethyl alcohol, adds 1 gram 20wt% butt aluminium colloidal sol again, thorough mixing;
2) above-mentioned mixed solution is put into watch-glass, volatilization ethanol becomes thick solid naturally;
3) will mix with above-mentioned thick solid abrasive above the urea of neutralization reaction amount 50wt%;
4) above-mentioned grinding mixture is placed into 500 ℃ of roasting 2h in the 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 is dissolved in the 50ml absolute ethyl alcohol, adds 1 gram 20wt% butt aluminium colloidal sol again, thorough mixing;
2) above-mentioned mixed solution is put into watch-glass, volatilization ethanol becomes thick solid naturally;
3) will mix with above-mentioned thick solid abrasive above the urea of neutralization reaction amount 50wt%;
4) above-mentioned grinding mixture is placed into 500 ℃ of roasting 2h in the 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 is dissolved in the 50ml absolute ethyl alcohol, adds 1 gram 20wt% butt aluminium colloidal sol again, thorough mixing;
2) above-mentioned mixed solution is put into watch-glass, volatilization ethanol becomes thick solid naturally;
3) will mix with above-mentioned thick solid abrasive above the bicarbonate of ammonia of neutralization reaction amount 50wt%;
4) above-mentioned grinding mixture is placed into 500 ℃ of roasting 2h in the retort furnace, obtains the white solid powder, be the mesoporous sphere aluminium sesquioxide.
Embodiment 5
1) 4 gram tensio-active agent P123 is dissolved in the 50ml absolute ethyl alcohol, adds 1 gram 20wt% butt aluminium colloidal sol again, thorough mixing;
2) above-mentioned mixed solution is put into watch-glass, volatilization ethanol becomes thick solid naturally;
3) will mix with above-mentioned thick solid abrasive above the bicarbonate of ammonia of neutralization reaction amount 50wt%;
4) above-mentioned grinding mixture is placed into 550 ℃ of roasting 3h in the retort furnace, obtains the white solid powder, be the mesoporous sphere aluminium sesquioxide.
Embodiment 6
1) 3 gram tensio-active agent P123 is dissolved in the 50ml absolute ethyl alcohol, adds 1 gram 20wt% butt aluminium colloidal sol again, thorough mixing;
2) above-mentioned mixed solution is put into watch-glass, volatilization ethanol becomes thick solid naturally;
3) will mix with above-mentioned thick solid abrasive above the bicarbonate of ammonia of neutralization reaction amount 50wt%;
4) above-mentioned grinding mixture is placed into 450 ℃ of roasting 5h in the retort furnace, obtains the white solid powder, be the mesoporous sphere aluminium sesquioxide.
Claims (6)
1. the preparation method of a mesoporous sphere aluminium sesquioxide, step is:
1) tensio-active agent P123 is dissolved in the absolute ethyl alcohol, adds 20wt% butt aluminium colloidal sol again, thorough mixing;
2) above-mentioned mixed solution is put into watch-glass, volatilization ethanol becomes thick solid naturally;
3) will mix with above-mentioned thick solid abrasive above bicarbonate of ammonia or the urea of neutralization reaction amount 50wt%;
4) above-mentioned grinding mixture is placed into 500 ± 80 ℃ of roasting 2～5h in the retort furnace, obtains the white solid powder, be the mesoporous sphere aluminium sesquioxide.
2. the preparation method of mesoporous sphere aluminium sesquioxide according to claim 1, it is characterized in that: the ratio of mixture of said tensio-active agent P123 and absolute ethyl alcohol is 1～4 gram: 50ml.
3. the preparation method of mesoporous sphere aluminium sesquioxide according to claim 1, it is characterized in that: the weight ratio of said tensio-active agent P123 and butt aluminium colloidal sol is 1～4:1.
4. the preparation method of mesoporous sphere aluminium sesquioxide according to claim 1, it is characterized in that: the volume ratio of said absolute ethyl alcohol and 20wt% butt aluminium colloidal sol is 9～12:1.
5. the preparation method of mesoporous sphere aluminium sesquioxide according to claim 1, it is characterized in that: the volume ratio of said absolute ethyl alcohol and 20wt% butt aluminium colloidal sol is 10:1.
6. the preparation method of mesoporous sphere aluminium sesquioxide according to claim 1, it is characterized in that: the maturing temperature in the said retort furnace is 500 ℃, and roasting time is 2h.
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| CN201210139705.2A CN102701247B (en) | 2012-05-08 | 2012-05-08 | Preparation method of mesoporous spherical aluminum oxide |
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Citations (3)
| 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 |
| CN101863499A (en) * | 2010-05-31 | 2010-10-20 | 中南大学 | Preparation method of macroporous-mesoporous alumina |
| CN102219242A (en) * | 2010-04-15 | 2011-10-19 | 中国石油化工股份有限公司 | Method for preparing mesoporous aluminum oxide |
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2012
- 2012-05-08 CN CN201210139705.2A patent/CN102701247B/en not_active Expired - Fee Related
Patent Citations (3)
| 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 |
| CN102219242A (en) * | 2010-04-15 | 2011-10-19 | 中国石油化工股份有限公司 | Method for preparing mesoporous aluminum oxide |
| CN101863499A (en) * | 2010-05-31 | 2010-10-20 | 中南大学 | Preparation method of macroporous-mesoporous alumina |
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Granted publication date: 20140101 Termination date: 20140508 |