CN104944455A - Sol-gel method for preparing aluminum oxide - Google Patents
Sol-gel method for preparing aluminum oxide Download PDFInfo
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- CN104944455A CN104944455A CN201510355777.4A CN201510355777A CN104944455A CN 104944455 A CN104944455 A CN 104944455A CN 201510355777 A CN201510355777 A CN 201510355777A CN 104944455 A CN104944455 A CN 104944455A
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- aluminum oxide
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Abstract
The invention discloses a sol-gel method for preparing aluminum oxide. Carbohydrate macromolecular gelatin is added to serve as a crosslinking agent, PEG-1000 serves as a dispersing agent, wherein the molar concentration of aluminum isopropoxide is 0.5-1.5 mol/L, the concentration of gelatin is 0.1-0.5 g/ml, the addition amount of the dispersing agent PEG-1000 is 1% the mass of aluminum isopropoxide; obtained sol stands for 4-6 h in a fuming hood to become gel, the gel undergoes freeze drying so that a solvent is removed and a loose aluminum oxide precursor is formed; and in the air atmosphere, the precursor having undergone freeze drying undergoes high temperature calcination to form high-purity nanometer aluminum oxide powder. The sol-gel method has the advantages that the sol-gel method is simple to operate, short in needed cycle and good in repeatability and facilitates industrialization, and gelatin is non-toxic and environmentally friendly.
Description
Technical field
The present invention relates to chemical material technical field, particularly a kind of sol-gel method prepares aluminum oxide.
Background technology
Aluminum oxide is one of maximum, the output value is the highest, purposes is the widest functional materials of 21 century output.Excellent characteristic that high-purity ultra-fine alumina has high rigidity, high strength, resistance to wears, corrosion-resistant, high temperature resistant, anti-oxidant, good insulating, surface-area are large, thermal expansivity is little, thermal shock resistance is good, dielectric loss is low etc., is widely used in the most advanced and sophisticated industry of the high-tech such as insulating material, electronic product, abrasion-proof corrosion-proof corrosion material and aerospace material.Commercial alumina is by bauxitic clay (Al
2o
33H
2o) and diasporite prepare, for the Al that purity requirement is high
2o
3, generally chemically prepare.Wherein sol-gel method prepares ultra-fine powder technology is more and more subject to people concern due to the advantage of its uniqueness.It is simple that sol-gel method has technique, and step, product composition and the advantage such as granularity is controlled are the important method preparing ultrafine particle.
The people such as F.Mirjalili (Ceramics International.2010,36,1253-1257) are with Al (OC
3h
7)
3, Al (NO
3)
3, Na (AOT), SDBS be raw material, adopts sol-gel method to obtain alumina precursor, obtained nanometer α-Al after high-temperature calcination
2o
3but, this method step is complicated, raw materials used more, and cost is large, be difficult to industrialization promotion, and dispersiveness is not fine.
The people such as D.M.Ibrahim (Materials Chemistry and Physics.2008,111,326-330) with urea, formaldehyde solution (37%), toluene, ethylene glycol and stearic acid aluminium soap for raw material, adopt sol-gel polymerization route borolon presoma, obtained nanometer α-Al after high-temperature calcination
2o
3, this method needs first to synthesize urea-formaldehyde resin, and formaldehyde used has special pungent odour, poisonous, has comparatively major injury to human body.
Summary of the invention
The present invention aims to provide a kind of environment-protecting asepsis, easy sol-gel method and prepares ultra-fine alumina.
Technical scheme of the present invention is: a kind of sol-gel method prepares aluminum oxide, comprises the steps:
1. prepare aluminum isopropylate solution, be uniformly mixed;
2. prepare gelatin solution, be uniformly mixed;
3. above-mentioned two solution are mixed while stirring, and add PEG-1000, stir at the temperature of 55-65 DEG C;
4. obtain gel after being left standstill by gained colloidal sol, then by gel refrigeration drying, form loose presoma;
5. presoma is calcined thermal treatment in atmosphere, cool to room temperature with the furnace after calcining thermal treatment completes, after grinding, obtain Al
2o
3powder.
Step 1. in, the volumetric molar concentration of aluminum isopropylate solution is 0.5-1.5mol/L, and its solvent is dehydrated alcohol.
Step 2. in, the concentration of gelatin solution is 0.1-0.5g/ml, and wherein solvent is deionized water.
Step 3. in, the add-on of PEG-1000 is 1% of aluminum isopropylate quality, and churning time is 4-6h.
Step 4. in, time of repose is 4-6h.
Step 5. in, the heat treated time is 2-4h, and thermal treatment temp is 850-1200 DEG C, and temperature rise rate is 5 DEG C/min.
Present method, compared with other method preparing aluminum oxide, has following beneficial effect:
1. the present invention adopts carbohydrate macromole gelatin to be that linking agent carrys out borolon first, has nontoxic, eco-friendly feature;
2. the present invention is simple to operate, and the described cycle is short, and repeatability is high, is convenient to realize suitability for industrialized production;
3. the diameter of particle prepared is little, is less than 50nm, good dispersity;
4. do not introduce other inorganic impurities in preparation process, obtained powder purity is high.
Accompanying drawing explanation
Fig. 1 is α-Al in the embodiment of the present invention 1
2o
3the X-ray diffractogram of powder.
Fig. 2 is α-Al in the embodiment of the present invention 1
2o
3the scanning electron microscope diagram sheet of powder.
Fig. 3 is α-Al in the embodiment of the present invention 1
2o
3the transmission electron micrograph of powder.
Fig. 4 is α-Al in the embodiment of the present invention 2
2o
3the X-ray diffractogram of powder.
Fig. 5 is α-Al in the embodiment of the present invention 2
2o
3the scanning electron microscope diagram sheet of powder.
Fig. 6 is α-Al in the embodiment of the present invention 2
2o
3the transmission electron micrograph of powder.
Fig. 7 is α-Al in the embodiment of the present invention 3
2o
3the X-ray diffractogram of powder.
Embodiment
Embodiment 1: γ-Al
2o
3the preparation of powder
The PEG-1000 taking 5g aluminum isopropylate, the gelatin of 5g and 0.05g is for subsequent use, is joined by aluminum isopropylate in the dehydrated alcohol of 50ml, stirs and treats that aluminum isopropylate dissolves completely, form solution A at 55-65 DEG C of temperature.Gelatin is joined in 20ml deionized water, beaker is placed in the water-bath of 30 DEG C, be ceaselessly stirred to gelatin and dissolve completely, form solution B.Solution B is joined inside solution A slowly, after stirring reaction 10min, adds PEG-1000, continue to stir 4h.Gained colloidal sol is placed in stink cupboard, leaves standstill 4-6h, then by gel refrigeration drying, except desolventizing, form loose alumina precursor.By lyophilize completely alumina precursor be put in corundum crucible and by corundum crucible and be put in KSL-1400X-A4 type retort furnace, temperature rise rate is set as 5 DEG C/min.Be warming up to 850 DEG C, be incubated 2h at such a temperature, retort furnace starts cooling subsequently, and in the temperature range of 850 DEG C to 500 DEG C, it is 10 DEG C/min that rate of temperature fall controls.When temperature is reduced to below 500 DEG C, rate of temperature fall is about 5 DEG C/min.When temperature reduces to room temperature, close retort furnace, take out product.The result of X-ray diffraction analysis (Fig. 1) shows, the diffraction peak of obtained sample and γ-Al
2o
3standard card fits like a glove, without other assorted peak.Scanning electronic microscope (Fig. 2) and transmission electron microscope (Fig. 3) show the made γ-Al obtained
2o
3diameter of particle is less, <20nm, and better dispersed, and hard aggregation is not obvious.
Embodiment 2: α-Al
2o
3the preparation of powder
The PEG-1000 taking 5g aluminum isopropylate, the gelatin of 5g and 0.05g is for subsequent use, is joined by aluminum isopropylate in the dehydrated alcohol of 50ml, stirs and treats that aluminum isopropylate dissolves completely, form solution A at 55-65 DEG C of temperature.Gelatin is joined in 20ml deionized water, beaker is placed in the water-bath of 30 DEG C, be ceaselessly stirred to gelatin and dissolve completely, form solution B.Solution B is joined inside solution A slowly, after stirring reaction 10min, adds PEG-1000, continue to stir 4h.Gained colloidal sol is placed in stink cupboard, leaves standstill 4-6h, then by gel refrigeration drying, except desolventizing, form loose alumina precursor.By lyophilize completely alumina precursor be put in corundum crucible and by corundum crucible and be put in KSL-1400X-A4 type retort furnace, temperature rise rate is set as 5 DEG C/min.Be warming up to 1200 DEG C, be incubated 2h at such a temperature, retort furnace starts cooling subsequently, and in the temperature range of 1200 DEG C to 600 DEG C, it is 10 DEG C/min that rate of temperature fall controls.When temperature is reduced to below 600 DEG C, rate of temperature fall is about 5 DEG C/min.When temperature reduces to room temperature, close retort furnace, take out product.The result of X-ray diffraction analysis (Fig. 4) shows, the diffraction peak of obtained sample and α-Al
2o
3standard card fits like a glove, without other assorted peak.Scanning electronic microscope (Fig. 5) and transmission electron microscope (Fig. 6) show the made α-Al obtained
2o
3diameter of particle is less, <50nm, and better dispersed, and hard aggregation is not obvious.
Change the temperature of reaction in embodiment 2, other parameters remain unchanged, and when temperature of reaction is lower than 55 DEG C, aluminum isopropylate dissolves not exclusively, the α-Al prepared
2o
3particle diameter is uneven, when temperature of reaction is higher than 65 DEG C, can cause the evaporation of solvent, and in reaction process, pressed powder is separated out, the α-Al prepared
2o
3particle diameter is comparatively large, and uneven.
Embodiment 3: α-Al
2o
3the preparation of powder
The PEG-1000 taking 10g aluminum isopropylate, the gelatin of 5g and 0.05g is for subsequent use, is joined by aluminum isopropylate in the dehydrated alcohol of 50ml, stirs and treats that aluminum isopropylate dissolves completely, form solution A at 55-65 DEG C of temperature.Gelatin is joined in 20ml deionized water, beaker is placed in the water-bath of 30 DEG C, be ceaselessly stirred to gelatin and dissolve completely, form solution B.Solution B is joined inside solution A slowly, after stirring reaction 10min, adds PEG-1000, continue to stir 4h.Gained colloidal sol is placed in stink cupboard, leaves standstill 4-6h, then by gel refrigeration drying, except desolventizing, form loose alumina precursor.By lyophilize completely alumina precursor be put in corundum crucible and by corundum crucible and be put in KSL-1400X-A4 type retort furnace, temperature rise rate is set as 5 DEG C/min.Be warming up to 1200 DEG C, be incubated 2h at such a temperature, retort furnace starts cooling subsequently, and in the temperature range of 1200 DEG C to 600 DEG C, it is 10 DEG C/min that rate of temperature fall controls.When temperature is reduced to below 600 DEG C, rate of temperature fall is about 5 DEG C/min.When temperature reduces to room temperature, close retort furnace, take out product.The result of X-ray diffraction analysis (Fig. 7) shows, the diffraction peak of obtained sample and α-Al
2o
3standard card fits like a glove, without other assorted peak.
Claims (6)
1. sol-gel method prepares an aluminum oxide, it is characterized in that, comprises the steps:
1. prepare aluminum isopropylate solution, be uniformly mixed;
2. prepare gelatin solution, be uniformly mixed;
3. above-mentioned two solution are mixed while stirring, and add PEG-1000, stir at the temperature of 55-65 DEG C;
4. obtain gel after being left standstill by gained colloidal sol, then by gel refrigeration drying, form loose presoma;
5. presoma is calcined thermal treatment in atmosphere, cool to room temperature with the furnace after calcining thermal treatment completes, after grinding, obtain Al
2o
3powder.
2. sol-gel method as claimed in claim 1 prepares aluminum oxide, it is characterized in that, step 1. in, the volumetric molar concentration of aluminum isopropylate solution is 0.5-1.5mol/L, and its solvent is dehydrated alcohol.
3. sol-gel method as claimed in claim 1 prepares aluminum oxide, it is characterized in that, step 2. in, the concentration of gelatin solution is 0.1-0.5g/ml, and wherein solvent is deionized water.
4. sol-gel method as claimed in claim 1 prepares aluminum oxide, it is characterized in that, step 3. in, the add-on of PEG-1000 is 1% of aluminum isopropylate quality, and churning time is 4-6h.
5. sol-gel method as claimed in claim 1 prepares aluminum oxide, it is characterized in that, step 4. in, time of repose is 4-6h.
6. sol-gel method as claimed in claim 1 prepares aluminum oxide, it is characterized in that, step 5. in, the heat treated time is 2-4h, and thermal treatment temp is 850-1200 DEG C, and temperature rise rate is 5 DEG C/min.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105524359A (en) * | 2016-01-21 | 2016-04-27 | 苏州市景荣科技有限公司 | Wear-resistant and heat-resistant EPDM (ethylene-propylene-diene monomer) sole material and preparation method thereof |
| CN113289595A (en) * | 2021-05-31 | 2021-08-24 | 淄博开迈新材料科技有限公司 | Spherical aluminum-based catalyst carrier based on composite hydrogel molding and preparation method thereof |
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| CN1565972A (en) * | 2003-06-30 | 2005-01-19 | 王海舟 | Technological process for preparing superfine aluminium oxide using sol gel method |
| CN102826597A (en) * | 2012-08-17 | 2012-12-19 | 南京信息工程大学 | Method for preparing nanometer titanium dioxide |
| CN103508476A (en) * | 2012-06-21 | 2014-01-15 | 中国石油化工股份有限公司 | Mesoporous nanometer alumina, preparation method and application thereof |
| CN103663548A (en) * | 2013-12-27 | 2014-03-26 | 南京信息工程大学 | Preparation method for anatase titanium dioxide nanocrystalline mesoporous microsphere |
-
2015
- 2015-06-24 CN CN201510355777.4A patent/CN104944455A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1565972A (en) * | 2003-06-30 | 2005-01-19 | 王海舟 | Technological process for preparing superfine aluminium oxide using sol gel method |
| CN103508476A (en) * | 2012-06-21 | 2014-01-15 | 中国石油化工股份有限公司 | Mesoporous nanometer alumina, preparation method and application thereof |
| CN102826597A (en) * | 2012-08-17 | 2012-12-19 | 南京信息工程大学 | Method for preparing nanometer titanium dioxide |
| CN103663548A (en) * | 2013-12-27 | 2014-03-26 | 南京信息工程大学 | Preparation method for anatase titanium dioxide nanocrystalline mesoporous microsphere |
Non-Patent Citations (2)
| Title |
|---|
| SHI TAO ET AL.: ""preparation and characterization of nanocrystalline γ-Al2O3 by sol-gel process"", 《稀有金属材料与工程》 * |
| 石涛等: ""络合溶胶–凝胶法制备Al2O3 纳米晶及其表征"", 《硅酸盐学报》 * |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105524359A (en) * | 2016-01-21 | 2016-04-27 | 苏州市景荣科技有限公司 | Wear-resistant and heat-resistant EPDM (ethylene-propylene-diene monomer) sole material and preparation method thereof |
| CN105524359B (en) * | 2016-01-21 | 2018-01-16 | 苏州市景荣科技有限公司 | A kind of EPDM material for sole of shoe of antiwear heat resisting and preparation method thereof |
| CN113289595A (en) * | 2021-05-31 | 2021-08-24 | 淄博开迈新材料科技有限公司 | Spherical aluminum-based catalyst carrier based on composite hydrogel molding and preparation method thereof |
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Application publication date: 20150930 |