CN102701247B - A kind of preparation method of mesoporous spherical aluminum oxide - Google Patents

Abstract

The invention discloses a method for preparing mesoporous spherical alumina, which uses industrial aluminum sol as aluminum source, P123 as surfactant, ammonium bicarbonate or urea as neutralizing agent, and synthesizes relatively cheap mesoporous spherical aluminum oxide. Aluminum oxide. The mesoporous spherical aluminum oxide obtained by the method of the present invention has a specific surface area of 186.7-270 m ² /g and a pore diameter of about 5.6 nm. Compared with the method of synthesizing aluminum oxide with high specific surface area in the prior art, the method of the present invention obviously reduces the cost, the production environment is more friendly, and it is more conducive to the improvement and protection of the environment.

Description

A kind of preparation method of mesoporous spherical aluminum oxide

technical field

The invention relates to a preparation of aluminum oxide, in particular to a preparation method of mesoporous spherical aluminum oxide. the

Background technique

Alumina with high specific surface area is an important catalyst carrier and adsorbent. Its preparation method has attracted much attention, and various alumina products with high specific surface area produced in large-scale industrial production have been widely used. Chinese patent 01126878.6 used surfactant P123 and aluminum isobutoxide in an organic solvent to synthesize spherical porous alumina pellets under the catalysis of hydrochloric acid. Relatively speaking, the price of aluminum isobutoxide is higher, and the organic solvent used in the invention is also expensive and has higher toxicity. Therefore, a cheaper aluminum source and an environmentally friendly solvent are selected to synthesize the low-cost high specific surface area dioxide. Aluminum will be one of the directions to promote the industrial application of this material. the

Contents of the invention

Aiming at the deficiencies of the prior art, the problem to be solved by the present invention is to provide a preparation method of mesoporous spherical alumina. the

The preparation method of mesoporous spherical aluminum oxide of the present invention, the steps are:

1) Dissolve surfactant P123 in absolute ethanol, then add 20wt% dry basis aluminum sol (the molecular formula of aluminum sol is Al(OH) _2.4 Cl _0.6 ), and mix thoroughly;

2) Put the above mixture into a watch glass, and naturally volatilize the ethanol to form a viscous solid;

3) Grinding and mixing ammonium bicarbonate or urea exceeding 50wt% of the neutralization reaction amount with the above viscous solid;

4) Put the above grinding mixture in a muffle furnace and roast at 500±80°C for 2-5 hours to obtain a white solid powder, which is mesoporous spherical alumina. the

In the preparation method of the above-mentioned mesoporous spherical alumina, the mixing ratio of the surfactant P123 and absolute ethanol is preferably 1-4 grams: 50ml. the

In the above method for preparing mesoporous spherical alumina, the weight ratio of the surfactant P123 to the dry aluminum sol is preferably 1˜4:1. the

In the above method for preparing mesoporous spherical alumina, the volume ratio of the absolute ethanol to 20wt% dry basis aluminum sol is 9-12:1, preferably 10:1. the

In the preparation method of the above-mentioned mesoporous spherical alumina, the dry basis purity (%) of the dry basis aluminum sol is ≥ 99.9, and the solvent of the aluminum sol is water. the

In the above method for preparing mesoporous spherical alumina, the calcination temperature in the muffle furnace is preferably 500° C., and the calcination time is preferably 2 hours. the

The present invention utilizes industrial aluminum sol as an aluminum source, P123 as a surfactant, and ammonium bicarbonate or urea as a neutralizing agent to synthesize relatively cheap mesoporous spherical alumina; the BET specific surface area test method tests the obtained method of the present invention The specific surface area of mesoporous spherical alumina is 186.7-270m ² /g, and the pore diameter is about 5.6nm. Compared with the method of synthesizing aluminum oxide with high specific surface area in the prior art, the cost is obviously reduced, the production environment is more friendly, and it is more conducive to environmental improvement and protection.

Description of drawings

Figure 1: 1g surfactant P123 obtains the pore structure diagram of Al2O3 sample

Among them: Surface Area=186.7m ² /g, Pore Volume=0.23cc/g, Pore Diameter Dv(d)=6.0nm.

Figure 2: 2g surfactant P123 obtains the sample pore structure of aluminum oxide

Among them: Surface Area=203.3m ² /g, Pore Volume=0.40cc/g, Pore Diameter Dv(d)=5.6nm.

Figure 3: 4g surfactant P123 obtains the pore structure diagram of Al2O3 sample

Among them: Surface Area=269.5m ² /g, Pore Volume=0.31cc/g, Pore Diameter Dv(d)=5.6nm.

Figure 4: High-resolution electron micrographs (60nm) of aluminum oxide samples obtained with 2g of surfactant P123. the

Figure 5: High-resolution electron micrographs (100nm) of aluminum oxide samples obtained with 2g of surfactant P123. the

Detailed ways

Example 1

1. Dissolve 1 gram of P123 in 50ml of absolute ethanol, and add 1g of dry-based aluminum sol (5ml of 20% aluminum sol solution by weight). the

2. Put the mixture into a watch glass, and naturally volatilize the ethanol to form a viscous solid. the

3. Add more than 50wt% urea for neutralization reaction and grind and mix with the above-mentioned solid. the

4. The mixture is placed in a muffle furnace and roasted at 500° C. for 2 hours to obtain a white solid powder, which is mesoporous spherical alumina. (see picture 1)

Example 2

1) Dissolve 2 grams of surfactant P123 in 50ml of absolute ethanol, then add 1 gram of 20wt% dry basis aluminum sol, and mix thoroughly;

2) Put the above mixture into a watch glass, and naturally volatilize the ethanol to form a viscous solid;

3) Grinding and mixing urea exceeding 50wt% of the neutralization reaction amount with the above viscous solid;

4) Put the above grinding mixture in a muffle furnace and bake at 500°C for 2 hours to obtain a white solid powder, which is mesoporous spherical alumina. (See Figure 2, 4, 5)

Example 3

1) Dissolve 4 grams of surfactant P123 in 50ml of absolute ethanol, then add 1 gram of 20wt% dry basis aluminum sol, and mix thoroughly;

2) Put the above mixture into a watch glass, and naturally volatilize the ethanol to form a viscous solid;

3) Grinding and mixing urea exceeding 50wt% of the neutralization reaction amount with the above viscous solid;

4) Put the above grinding mixture in a muffle furnace and bake at 500°C for 2 hours to obtain a white solid powder, which is mesoporous spherical alumina. (See Figure 3)

Example 4

1) Dissolve 2 grams of surfactant P123 in 50ml of absolute ethanol, then add 1 gram of 20wt% dry basis aluminum sol, and mix thoroughly;

2) Put the above mixture into a watch glass, and naturally volatilize the ethanol to form a viscous solid;

3) Grinding and mixing ammonium bicarbonate exceeding 50wt% of the neutralization reaction amount with the above viscous solid;

4) Put the above grinding mixture in a muffle furnace and bake at 500°C for 2 hours to obtain a white solid powder, which is mesoporous spherical alumina. the

Example 5

1) Dissolve 4 grams of surfactant P123 in 50ml of absolute ethanol, then add 1 gram of 20wt% dry basis aluminum sol, and mix thoroughly;

2) Put the above mixture into a watch glass, and naturally volatilize the ethanol to form a viscous solid;

3) Grinding and mixing ammonium bicarbonate exceeding 50wt% of the neutralization reaction amount with the above viscous solid;

4) Put the above grinding mixture in a muffle furnace and roast at 550°C for 3 hours to obtain a white solid powder, which is mesoporous spherical alumina. the

Example 6

1) Dissolve 3 grams of surfactant P123 in 50ml of absolute ethanol, then add 1 gram of 20wt% dry basis aluminum sol, and mix thoroughly;

2) Put the above mixture into a watch glass, and naturally volatilize the ethanol to form a viscous solid;

3) Grinding and mixing ammonium bicarbonate exceeding 50wt% of the neutralization reaction amount with the above viscous solid;

4) Put the above grinding mixture in a muffle furnace and bake at 450°C for 5 hours to obtain a white solid powder, which is mesoporous spherical alumina. the

Claims (1)

1. a preparation method of mesoporous spherical aluminum oxide, the steps are: 1) Dissolve surfactant P123 in absolute ethanol so that the mixing ratio of surfactant P123 and absolute ethanol is 1 to 4 grams: 50mL, then add 20 wt % dry base aluminum sol to make surfactant P123 and The weight ratio of dry-based aluminum sol is 1 to 4:1, and the volume ratio of absolute ethanol to 20 wt % dry-based aluminum sol is 10:1, fully mixed; 2) Put the above mixture into a watch glass, and naturally volatilize the ethanol to form a viscous solid; 3) Grinding and mixing ammonium bicarbonate or urea exceeding 50wt% of the neutralization reaction amount with the above viscous solid; 4) Put the above grinding mixture in a muffle furnace and bake at 500°C for 2 hours to obtain a white solid powder, which is mesoporous spherical alumina.

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