CN102849762A - Preparation method for nanoscale alumina powder - Google Patents
Preparation method for nanoscale alumina powder Download PDFInfo
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- CN102849762A CN102849762A CN2011101772104A CN201110177210A CN102849762A CN 102849762 A CN102849762 A CN 102849762A CN 2011101772104 A CN2011101772104 A CN 2011101772104A CN 201110177210 A CN201110177210 A CN 201110177210A CN 102849762 A CN102849762 A CN 102849762A
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Abstract
The invention relates to a preparation method for nanoscale alumina powder. The method includes allowing the reaction between aluminum powder and solvent n-hexanol to prepare an aluminum alkoxide compound, hydrolyzing, distilling, separating, and roasting to prepare nanoscale alumina powder product. The invention has no need for catalyst removal, has no need for large amount of water to wash away the impurities in the material, reduces the discharge of wastewater, reduces pollution and saves the production cost; in the production process, the used alcohol can be recycled (with recovery rate at 90%), to greatly reduce the production cost; and the product has low impurity content, large pore volume, large specific surface, and reasonable pore size distribution, and can be used as an industrial catalyst carrier.
Description
Technical field
The invention belongs to the preparation method of oxide compound, specifically relate to the preparation method of nano-alumina powder.
Background technology
Along with the development of nanotechnology, will day by day improve the ultra-fine property of novel nano-material and inhomogeneity requirement.Nano aluminium oxide not only has the characteristic that common aluminum oxide fusing point is high, refractoriness is high, mechanical behavior under high temperature good, electric insulating quality is good, the acid and alkali-resistance erosion performance is strong and hardness is high, have larger and more cheap and easy to get than other material specific surface, also have the distinctive character of many nano materials such as quantum size effect, small-size effect, surface effects and macro quanta tunnel effect, therefore, nano aluminium oxide many fields that are widely used.
Along with the development of science and technology, the requirement of aluminum oxide purity and granularity is raise day by day, the application of high-purity ultra-fine alumina is more and more paid attention to by people, therefore be badly in need of finding cost low, be easy to industrialized high-purity ultra-fine alumina production method.The nano aluminium oxide preparation method trends towards diversification, and the powder characteristics that present domestic vapor phase process commonly used is prepared is good, but cost is too high; Alkoxide hydrolysis is a kind of comparatively desirable method, and this method prepares nano aluminium oxide, mild condition, and product purity is high, and epigranular can be easy to generate the aluminum oxide that purity is higher, granularity is less.And, the production technique that has new factory of many families to build up both at home and abroad and produce high-purity ultra-fine alumina take metallic aluminium as raw material with alkoxide hydrolysis.
Numerous results of study show, the aluminum isopropylate of preparing by fine aluminium control different reaction conditionss when hydrolysis produces aluminum oxide, and its granularity of aluminum oxide product that then obtains, shape and size distribution also have very large difference.According to different hydrolysising conditions, can obtain alumina powder jointed from several nanometers to tens nanometers of particle diameter.According to the similarity of alcohol, can replace Virahol to prepare n-hexyl alcohol aluminium with n-hexyl alcohol and be hydrolyzed again the generation aluminum oxide.Therefore, by changing starting material, reduce cost, and the amount etc. of how controlling the kind of n-hexyl alcohol aluminium hydrolysis process condition such as pure water mol ratio, temperature of reaction, additive and adding crystal seed is the key problem in technology of aluminum oxide manufacturers, decisive meaning is arranged in market competition.For this reason, this patent is mainly studied take aluminium powder as raw material and is prepared n-hexyl alcohol aluminium and hydrolysis reaction process process on the impact of alumina precursor granularity and form, for satisfying the market provides essential processing parameter to alumina powder jointed technical feature.
In the standby process of n-hexyl alcohol aluminum, aluminium and alcohol are in the presence of catalyzer, and reaction generates aluminium alcoholates, and releasing hydrogen gas:
Aluminum content is more than 99% in the aluminium powder, but low more than the cost of aluminium alcoholates.The n-hexyl alcohol aluminium of preparation can be prepared nano-alumina powder equally after removal of impurities take aluminium powder as raw material.
N-hexyl alcohol aluminium hydrolytic process is a nonpolar very strong Fast Process, prepare in the hydrolysis reaction of aluminium colloidal sol using it as precursor, n-hexyl alcohol aluminium at first exists with tripolymer and tetramer form, simultaneously, exists the balance that coordination structure changes at intramolecule.
Hydrolytic process is the OH group in the water molecules, by the alcohol radical in the nucleophilic process substituted alcohols compound.Between hydrolysate, can spontaneously produce polymerization by oxygen connection process between hydrolysate and the raw material, form oligopolymer and superpolymer.Will prepare colloidal sol take n-hexyl alcohol aluminium as precursor, its precursor must at first be dissolved in the n-hexyl alcohol, and n-hexyl alcohol aluminium easily lumps, not soluble in water, should be first with its grinding before preparation colloidal sol, stirring and dissolving in n-hexyl alcohol again, the more thin more facile hydrolysis of shattering process, the colloid that obtains at last is more even.Hydrolytic process or polymerization process all are subject to the impact of the aspects such as solvent, the water yield, hydrolysis temperature and digestion time simultaneously.Wherein amount of water and hydrolysis temperature can have influence on balance, particle size and the size distribution of speed, colloidal sol and the gel of hydrolysis and polyreaction.Simultaneously, the mixing velocity of precursor and solvent and stirring velocity also can affect hydrolysis degree and the particle size of colloidal sol.
Therefore, rely on the R﹠D force of enterprise, the alkoxide hydrolysis production technique is further optimized, inquire into simultaneously its product in high problems of foreign matter content such as the biggest problem-iron that exports and domestic application is run into, silicon, magnesium.
Summary of the invention
The object of the invention is to overcome the deficiencies in the prior art part, and a kind of product purity that neither affects is provided, do not have again the preparation method of the nano-alumina powder that other impurity sneaks into, the replace imported nano alumina powder fills the domestic gaps; And with the alkoxide recycling, both reduced production cost, can reach again the purpose of environmental protection.
The present invention is achieved by following technical solution:
Reaction formula of the present invention:
(1) pure reactive aluminum prepares pure aluminum compound
The alcohol reactive aluminum activates aluminium powder with titanium salt, and the aluminium alcoholates of circulation is as initiator.Reaction formula:
2AL+6C
6H
11OH=2AL（C
6H
11O）
3+3H
2 
(2) aluminium alcoholates compound hydrolysis reaction preparation nano-alumina powder reaction formula:
AL（C
6H
11O）
3+3H
2O=3C
6H
11OH+AL（OH）
3
The preparation method of nano-alumina powder is characterized in that adopting aluminium powder directly and the n-hexyl alcohol reaction, makes first pure aluminum compound, then pure aluminum compound is through hydrolysis, distillation, separation, get hydrated aluminum oxide, roasting hydrated aluminum oxide, preparation nano-alumina powder product.
Described pure aluminum compound reaction process condition: catalyzer/aluminium powder mass ratio=0-0.10; Aluminium powder/n-hexyl alcohol mol ratio=1:2-1:6; Temperature of reaction: 150～230 ℃; Working pressure: 0-1.0MPa; Reaction times 1-5 hour.
Described pure aluminum compound reaction process optimum condition: catalyzer/aluminium powder mass ratio=0.03-0.06; Aluminium powder/n-hexyl alcohol mol ratio=1:3-1:5; Temperature of reaction 150-180 ℃; Working pressure 0-0.2MPa; Reaction times 1-3 hour.
Described aluminium alcoholates compound hydrolysis reaction process condition: the mol ratio of n-hexyl alcohol aluminium and water is 1:2-1:5; Temperature of reaction: 60～100 ℃; Working pressure: 0-1.0MPa; PH value: 7～10; Reaction times: 1-5 hour.
Described aluminium alcoholates compound hydrolysis reaction process optimum condition: the mol ratio of n-hexyl alcohol aluminium and water is 1:3-1:4; Temperature of reaction: 70-90 ℃; Working pressure: 0-0.2MPa; PH value: 7-9; Reaction times: 2～4 hours.
Described hydrated aluminum oxide roasting, maturing temperature are 500-1000 ℃, and soaking time is 2-5h, and method of cooling is naturally cooling under the room temperature.
Described catalyzer is selected Al salt or Ti salt, preferred AlCl3 or TiCl3; Select tensio-active agent to be: a kind of in the Macrogol 200,400,600 or 800.
The present invention compared with prior art has following advantage:
A. need not catalyst removal, catalyzer can directly be removed in the roasting drying process;
B. do not need large water gaging to come impurity in the flush away material, reduce the discharging of waste water, reduce and pollute, saved production cost;
C. in the production process, hexanol can recycle (rate of recovery is 90%), can greatly reduce production costs;
D. the product foreign matter content is few, pore volume is large, specific surface is large, pore size distribution is reasonable, can reach the index of import SB powder.
Description of drawings
Fig. 1 is the process flow sheet of nano-alumina powder of the present invention.
Embodiment
The below enumerates 2 embodiment, and by reference to the accompanying drawings the present invention is further specified, but the present invention is not only limited to these embodiment.
Embodiment 1
Experimental raw
The selection of raw material (such as kind, purity, granularity etc.) is directly determining the powder feature of glue effect and nano-powder.The alcohol reactive aluminum prepares pure aluminum compound processing condition: 80-100 order aluminium powder 54g, catalyzer/aluminium powder mass ratio=0.05, aluminium powder/n-hexyl alcohol mol ratio=1:4, temperature of reaction: 160 ℃, working pressure :≤0.1Mpa, reaction times: 2 hours, react and obtain intermediate product n-hexyl alcohol aluminium 616g.
Aluminium alcoholates compound hydrolysis reaction preparation nano-alumina powder processing condition: the mol ratio of 616g n-hexyl alcohol aluminium and deionized water is 1:3,1% the poly-second ニ alcohol 400 of tensio-active agent that adds n-hexyl alcohol aluminium weight, temperature of reaction: 70 ℃, working pressure :≤0.1Mpa, pH value: 7.5, reaction times: 3 hours, through hydrolysis, distillation, separation, obtain hydrated aluminum oxide 148g.
In the retort furnace roasting, temperature is 800 ℃ with the 148g hydrated aluminum oxide, 2-3 hour, in stove, progressively cool off room temperature, and obtain γ-aluminium sesquioxide 95g.
Embodiment 2
The alcohol reactive aluminum prepares pure aluminum compound processing condition: 100-200 order aluminium powder 54g, catalyzer/aluminium powder mass ratio=0.03, aluminium powder/n-hexyl alcohol mol ratio=1:5, temperature of reaction: 160 ℃, working pressure :≤0.15Mpa, reaction times: 3 hours, react and obtain intermediate product n-hexyl alcohol aluminium 640g.
Aluminium alcoholates compound hydrolysis reaction preparation nano-alumina powder processing condition: the mol ratio of 640g n-hexyl alcohol aluminium and deionized water is 1:3, the poly-second ニ alcohol 600 of 0.5% tensio-active agent that adds n-hexyl alcohol aluminium weight, temperature of reaction: 80 ℃, working pressure :≤0.1Mpa, pH value: 7, reaction times: 4 hours, through distillation, separation, hydrolysis, obtain hydrated aluminum oxide 156g.
In the retort furnace roasting, temperature is 800 ℃ with the 100g hydrated aluminum oxide, 2-3 hour, in stove, progressively cool off room temperature, and obtain γ-aluminium sesquioxide 65g.
In the retort furnace roasting, temperature is 1300 ℃ with the 56g hydrated aluminum oxide, 2-3 hour, in stove, progressively cool off room temperature, and obtain α-aluminium sesquioxide 35g.
The nano-alumina powder product that the inventive method is produced, purity is more than 99.99%, granularity is specially adapted to the carrier of catalyzer less than 100nm.
Claims (8)
1. the preparation method of nano-alumina powder is characterized in that: adopt aluminium powder directly and the n-hexyl alcohol reaction, make first pure aluminum compound, then pure aluminum compound is through hydrolysis, distillation, separation, get hydrated aluminum oxide, roasting hydrated aluminum oxide, preparation nano-alumina powder product.
2. the preparation method of described nano-alumina powder according to claim 1 is characterized in that: pure aluminum compound reaction process condition: catalyzer/aluminium powder mass ratio=0-0.10; Aluminium powder/n-hexyl alcohol mol ratio=1:2-1:6; Temperature of reaction: 150～230 ℃; Working pressure: 0-1.0MPa; Reaction times 1-5 hour.
3. the preparation method of described nano-alumina powder according to claim 2 is characterized in that: pure aluminum compound reaction process condition: catalyzer/aluminium powder mass ratio=0.03-0.06; Aluminium powder/n-hexyl alcohol mol ratio=1:3-1:5; Temperature of reaction 150-180 ℃; Working pressure 0-0.2MPa; Reaction times 1-3 hour.
4. the preparation method of described nano-alumina powder according to claim 1, it is characterized in that: aluminium alcoholates compound hydrolysis reaction process condition: the mol ratio of n-hexyl alcohol aluminium and water is 1:2-1:5; Temperature of reaction: 60～100 ℃; Working pressure: 0-1.0MPa; PH value: 7～10; Reaction times: 1-5 hour.
5. the preparation method of described nano-alumina powder according to claim 4, it is characterized in that: aluminium alcoholates compound hydrolysis reaction preferred processing condition: the mol ratio of n-hexyl alcohol aluminium and water is 1:3-1:4; Temperature of reaction: 70-90 ℃; Working pressure: 0-0.2MPa; PH value: 7-9; Reaction times: 2～4 hours.
6. the preparation method of described nano-alumina powder according to claim 1, it is characterized in that: hydrated aluminum oxide roasting, maturing temperature are 500-1000 ℃, and soaking time is 2-5h, and method of cooling is naturally cooling under the room temperature.
7. the preparation method of described nano-alumina powder according to claim 1, it is characterized in that: catalyzer is selected Al salt or Ti salt; Select tensio-active agent to be: a kind of in the Macrogol 200,400,600 or 800.
8. the preparation method of described nano-alumina powder according to claim 7, it is characterized in that: catalyzer is selected AlCl3 or TiCl3.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103303950A (en) * | 2013-07-05 | 2013-09-18 | 泰山医学院 | Solvent thermal synthesis method for preparing boehmite powder |
| CN107983297A (en) * | 2017-12-27 | 2018-05-04 | 河北麦森钛白粉有限公司 | A kind of heavy metal absorbent α-Al2O3The preparation method of nano-particle |
| CN115448343A (en) * | 2022-10-25 | 2022-12-09 | 河北铭万精细化工有限公司 | Production process of electronic grade nano alumina |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1374251A (en) * | 2002-04-08 | 2002-10-16 | 常耀辉 | Prepn of superpurity nano level alumina powder |
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2011
- 2011-06-28 CN CN2011101772104A patent/CN102849762A/en active Pending
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1374251A (en) * | 2002-04-08 | 2002-10-16 | 常耀辉 | Prepn of superpurity nano level alumina powder |
Non-Patent Citations (1)
| Title |
|---|
| 赵琰: ""氧化铝（拟薄水铝石）的孔结构研究"", 《工业催化》 * |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103303950A (en) * | 2013-07-05 | 2013-09-18 | 泰山医学院 | Solvent thermal synthesis method for preparing boehmite powder |
| CN107983297A (en) * | 2017-12-27 | 2018-05-04 | 河北麦森钛白粉有限公司 | A kind of heavy metal absorbent α-Al2O3The preparation method of nano-particle |
| CN115448343A (en) * | 2022-10-25 | 2022-12-09 | 河北铭万精细化工有限公司 | Production process of electronic grade nano alumina |
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Application publication date: 20130102 |