CN102303882A - Method for preparing alpha-Al2O3 powder from microemulsion - Google Patents
Method for preparing alpha-Al2O3 powder from microemulsion Download PDFInfo
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- CN102303882A CN102303882A CN201110236817A CN201110236817A CN102303882A CN 102303882 A CN102303882 A CN 102303882A CN 201110236817 A CN201110236817 A CN 201110236817A CN 201110236817 A CN201110236817 A CN 201110236817A CN 102303882 A CN102303882 A CN 102303882A
- Authority
- CN
- China
- Prior art keywords
- oil
- microemulsion
- phase solution
- water
- cosurfactant
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Granted
Links
- 239000004530 micro-emulsion Substances 0.000 title claims abstract description 16
- 239000000843 powder Substances 0.000 title claims abstract description 16
- 238000000034 method Methods 0.000 title abstract description 11
- 229910052594 sapphire Inorganic materials 0.000 title abstract 4
- SMZOGRDCAXLAAR-UHFFFAOYSA-N aluminium isopropoxide Chemical compound [Al+3].CC(C)[O-].CC(C)[O-].CC(C)[O-] SMZOGRDCAXLAAR-UHFFFAOYSA-N 0.000 claims abstract description 18
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 17
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 13
- 239000004064 cosurfactant Substances 0.000 claims abstract description 10
- 239000008367 deionised water Substances 0.000 claims abstract description 9
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 9
- 238000003756 stirring Methods 0.000 claims abstract description 9
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims abstract description 6
- 238000001354 calcination Methods 0.000 claims abstract description 5
- 235000012538 ammonium bicarbonate Nutrition 0.000 claims abstract description 4
- 235000011114 ammonium hydroxide Nutrition 0.000 claims abstract description 4
- 238000005406 washing Methods 0.000 claims abstract description 3
- 239000012071 phase Substances 0.000 claims description 23
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 claims description 12
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 claims description 12
- BDERNNFJNOPAEC-UHFFFAOYSA-N propan-1-ol Chemical compound CCCO BDERNNFJNOPAEC-UHFFFAOYSA-N 0.000 claims description 10
- 239000013543 active substance Substances 0.000 claims description 9
- 239000008346 aqueous phase Substances 0.000 claims description 8
- -1 polyoxy ethene Polymers 0.000 claims description 7
- 239000002994 raw material Substances 0.000 claims description 7
- UHOVQNZJYSORNB-UHFFFAOYSA-N Benzene Chemical compound C1=CC=CC=C1 UHOVQNZJYSORNB-UHFFFAOYSA-N 0.000 claims description 6
- 229960004756 ethanol Drugs 0.000 claims description 5
- 235000010482 polyoxyethylene sorbitan monooleate Nutrition 0.000 claims description 5
- 229920000053 polysorbate 80 Polymers 0.000 claims description 5
- GPRLSGONYQIRFK-MNYXATJNSA-N triton Chemical compound [3H+] GPRLSGONYQIRFK-MNYXATJNSA-N 0.000 claims description 5
- XDTMQSROBMDMFD-UHFFFAOYSA-N Cyclohexane Chemical compound C1CCCCC1 XDTMQSROBMDMFD-UHFFFAOYSA-N 0.000 claims description 4
- 238000000967 suction filtration Methods 0.000 claims description 4
- DUIOKRXOKLLURE-UHFFFAOYSA-N 2-octylphenol Chemical compound CCCCCCCCC1=CC=CC=C1O DUIOKRXOKLLURE-UHFFFAOYSA-N 0.000 claims description 2
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 claims description 2
- 229920001732 Lignosulfonate Polymers 0.000 claims description 2
- LRHPLDYGYMQRHN-UHFFFAOYSA-N N-Butanol Chemical compound CCCCO LRHPLDYGYMQRHN-UHFFFAOYSA-N 0.000 claims description 2
- CTQNGGLPUBDAKN-UHFFFAOYSA-N O-Xylene Chemical compound CC1=CC=CC=C1C CTQNGGLPUBDAKN-UHFFFAOYSA-N 0.000 claims description 2
- 229960000935 dehydrated alcohol Drugs 0.000 claims description 2
- 235000019357 lignosulphonate Nutrition 0.000 claims description 2
- VLKZOEOYAKHREP-UHFFFAOYSA-N n-Hexane Chemical compound CCCCCC VLKZOEOYAKHREP-UHFFFAOYSA-N 0.000 claims description 2
- TVMXDCGIABBOFY-UHFFFAOYSA-N octane Chemical compound CCCCCCCC TVMXDCGIABBOFY-UHFFFAOYSA-N 0.000 claims description 2
- 238000002360 preparation method Methods 0.000 claims description 2
- 230000001105 regulatory effect Effects 0.000 claims description 2
- 239000003643 water by type Substances 0.000 claims description 2
- 239000008096 xylene Substances 0.000 claims description 2
- 239000002245 particle Substances 0.000 abstract description 4
- 230000007062 hydrolysis Effects 0.000 abstract description 2
- 238000006460 hydrolysis reaction Methods 0.000 abstract description 2
- ATRRKUHOCOJYRX-UHFFFAOYSA-N Ammonium bicarbonate Chemical compound [NH4+].OC([O-])=O ATRRKUHOCOJYRX-UHFFFAOYSA-N 0.000 abstract 1
- 229910000013 Ammonium bicarbonate Inorganic materials 0.000 abstract 1
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 abstract 1
- 239000001099 ammonium carbonate Substances 0.000 abstract 1
- 238000001035 drying Methods 0.000 abstract 1
- 238000005265 energy consumption Methods 0.000 abstract 1
- 238000001914 filtration Methods 0.000 abstract 1
- 239000000203 mixture Substances 0.000 abstract 1
- 239000004094 surface-active agent Substances 0.000 abstract 1
- 239000000243 solution Substances 0.000 description 18
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 9
- 239000000463 material Substances 0.000 description 5
- 229910052782 aluminium Inorganic materials 0.000 description 3
- 239000004411 aluminium Substances 0.000 description 3
- 238000003980 solgel method Methods 0.000 description 3
- 229910052799 carbon Inorganic materials 0.000 description 2
- 238000005054 agglomeration Methods 0.000 description 1
- 230000002776 aggregation Effects 0.000 description 1
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 1
- REDXJYDRNCIFBQ-UHFFFAOYSA-N aluminium(3+) Chemical compound [Al+3] REDXJYDRNCIFBQ-UHFFFAOYSA-N 0.000 description 1
- 239000007864 aqueous solution Substances 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 238000000975 co-precipitation Methods 0.000 description 1
- 230000001276 controlling effect Effects 0.000 description 1
- 230000005611 electricity Effects 0.000 description 1
- 238000001027 hydrothermal synthesis Methods 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 239000007791 liquid phase Substances 0.000 description 1
- 125000005447 octyloxy group Chemical group [H]C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])O* 0.000 description 1
- 239000013110 organic ligand Substances 0.000 description 1
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 description 1
- 238000006116 polymerization reaction Methods 0.000 description 1
- 238000005118 spray pyrolysis Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
Landscapes
- Compounds Of Alkaline-Earth Elements, Aluminum Or Rare-Earth Metals (AREA)
- Colloid Chemistry (AREA)
Abstract
The invention discloses a method for preparing high-purity alpha-Al2O3 powder from a microemulsion. The method comprises the following steps: selecting a corresponding oil phase, a surfactant and a cosurfactant according to the property of the microemulsion; preparing an aluminum isopropoxide microemulsion according to the basic property of aluminum isopropoxide, and evenly stirring; adding ammonia water or ammonium bicarbonate to regulate the pH value to 8-10, and carrying out hydrolysis in a water bath for 20-90 minutes at the temperature of 50-100 DEG C; filtering obtained gel in vacuum, washing with a large amount of deionized water, absolute ethyl alcohol or acetone and drying; and calcining at the temperature of 900-1200 DEG C so as to obtain the high-purity alpha-Al2O3 powder. The process disclosed by the invention has the advantages of simple equipment and low energy consumption; and the obtained alpha-Al2O3 powder has adjustable composition, good particle dispersity and high purity, and is easy to produce.
Description
Technical field
What the present invention relates to is that a kind of microemulsion prepares high-purity α-Al
2O
3The method of powder.
Background technology
High-purity superfine alumina powder be purity at the super-fine powder material more than 99.99%, be one of tip materials that output is maximum in the 21st century novel material, the output value is the highest, purposes is the widest.High-purity superfine alumina powder is because of its purity is high, particle diameter is little, narrower size distribution, no serious agglomeration and stable phase are arranged; Demonstrated the light that conventional material did not have, electricity, magnetic, heat and mechanical characteristics, thereby it is widely used in a plurality of fields such as optics, chemical industry and special cermacis as a kind of new function material.
The most frequently used method of preparation high purity alumina powder has sol-gel method, aluminium alcoholates hydrolysis method, liquid-phase coprecipitation.Sol-gel method prepares aluminum oxide and is characterised in that adding organic ligand and metallic aluminium ion formation title complex in the aqueous solution; Conditions such as pH value, temperature of reaction are hydrolyzed through controlling, polymerization; Form a kind of spatial skeleton structure through the sol-gel approach, the roasting of dewatering at last gets the purpose product.In addition, the method for preparing high purity aluminium oxide also has hydrothermal method, spray pyrolysis.
Introduce a kind of employing sol-gel method in the patent (application number US4615875) of applications such as Stephen T.Gonczy, Mt.Prospect, Roy T.Mitsche, Wauconda and prepared high-purity α-Al
2O
3Method.Introduced among the CN1201014A of application such as Dai Longxiu, Duan Qiwei (application number 97104442.2) and in the low-carbon alkoxy aluminium molecule, introduced different octyloxy; Obtain being the low-carbon alkoxy of liquid, different octyloxy aluminium under the room temperature, being hydrolyzed as raw material makes high purity aluminium oxide.But oil-in-water prepared with microemulsion reactor α-Al
2O
3Do not appear in the newspapers.
Summary of the invention
The object of the present invention is to provide a kind of processing unit simple, form adjustable, gained particle good dispersity, microemulsion that purity is high prepares α-Al
2O
3The method of powder.
Concrete steps are:
(1) mass percent of raw material is: water is 10～70%; Oil phase is 5～40%; Cosurfactant and tensio-active agent sum are 10～80%, and the total mass percent sum of raw material is 100%, and wherein cosurfactant is 2: 1～7: 1 with the ratio of tensio-active agent volume.
(2) set by step (1) proportioning mixes tensio-active agent and cosurfactant, is divided into two equal portions, and adding oil phase and water fully stir and be mixed with oil-phase solution and aqueous phase solution in two parts respectively;
(3) aluminum isopropylate fully is dissolved in the oil-phase solution that step (2) makes, aluminum isopropylate and oil-phase solution massfraction are than being 0.15-0.45: 1;
(4) oil-phase solution that step (3) is made mixes with the aqueous phase solution that step (2) makes, and stirs, and makes the aluminum isopropylate microemulsion;
(5) the aluminum isopropylate microemulsion that step (4) is made adds ammoniacal liquor or bicarbonate of ammonia is regulated pH=8～10; Be hydrolyzed at 50～100 ℃ of water-bath 20～90min; The gel that obtains is carried out suction filtration; A large amount of deionized waters, dehydrated alcohol or washing with acetone; Oven dry, calcining obtains high-purity α-Al under 900～1200 ℃
2O
3Powder.
Said water is a deionized water;
Said oil phase is a kind of in hexanaphthene, normal hexane, benzene,toluene,xylene and the octane;
Said tensio-active agent is that OP-10 (alkylphenol-polyethenoxy (10) ether), OPE-2 (octyl phenol polyoxy ethene (2) ether), OPE-10 (polyoxyethylene octylphenol ether), Tween-40, tween-80, triton x-100 and sulfonated lignin HLB value are one or more of 8-18;
Said cosurfactant is a kind of in ethanol, propyl alcohol, propyl carbinol and the Virahol.
Processing unit of the present invention is simple, be prone to produce, power consumption is low, it is adjustable to form, gained particle good dispersity, purity are high.
Embodiment
Embodiment 1:
(1) mass percent of raw material: deionized water is 30%, and hexanaphthene is 20%, and tensio-active agent tween-80 and cosurfactant ethanol sum are 50%, and wherein ethanol and tween-80 volume ratio are 6: 1;
(2) set by step (1) proportioning mixes tween-80 and ethanol, is divided into two equal portions, and adding hexanaphthene and deionized water fully stir and be mixed with oil-phase solution and aqueous phase solution in two parts respectively;
(3) aluminum isopropylate fully is dissolved in the oil-phase solution that step (2) makes, aluminum isopropylate and oil-phase solution massfraction ratio are 0.35: 1;
(4) oil-phase solution that step (3) is made mixes with the aqueous phase solution that step (2) makes, and stirs, and makes the aluminum isopropylate microemulsion;
(5) the aluminum isopropylate microemulsion that step (4) made adds bicarbonate of ammonia and regulates pH=8.5, be hydrolyzed at 80 ℃ of water-bath 60min, with the gel suction filtration that obtains, a large amount of deionized water wash, oven dry, 900～1200 ℃ down calcining obtain high-purity α-Al
2O
3Powder.
Embodiment 2:
(1) mass percent of raw material: deionized water is 30%, toluene 10%, and triton x-100 and propyl alcohol sum are 60%, propyl alcohol and triton x-100 volume ratio are 4: 1;
(2) set by step (1) proportioning mixes triton x-100 and propyl alcohol, is divided into two equal portions, and adding toluene and deionized water fully stir and be mixed with oil-phase solution and aqueous phase solution in two parts respectively;
(3) aluminum isopropylate fully is dissolved in the oil-phase solution that step (2) makes, aluminum isopropylate and oil-phase solution massfraction ratio are 0.4: 1;
(4) oil-phase solution that step (3) is made mixes with the aqueous phase solution that step (2) makes, and stirs, and makes the aluminum isopropylate microemulsion;
(5) the aluminum isopropylate microemulsion that step (4) made adds ammoniacal liquor and regulates pH=9, be hydrolyzed at 60 ℃ of water-bath 60min, with the gel suction filtration that obtains, a large amount of deionized water wash, oven dry, 900～1200 ℃ down calcining obtain high-purity α-Al
2O
3Powder.
Claims (1)
1. α-Al
2O
3The preparation method of powder is characterized in that concrete steps are:
(1) mass percent of raw material is: water is 10～70%; Oil phase is 5～40%; Cosurfactant and tensio-active agent sum are 10～80%, and the total mass percent sum of raw material is 100%, and wherein cosurfactant is 2: 1～7: 1 with the ratio of tensio-active agent volume;
(2) set by step (1) proportioning mixes tensio-active agent and cosurfactant, is divided into two equal portions, and adding oil phase and water fully stir and be mixed with oil-phase solution and aqueous phase solution in two parts respectively;
(3) aluminum isopropylate fully is dissolved in the oil-phase solution that step (2) makes, aluminum isopropylate and oil-phase solution massfraction are than being 0.15-0.45: 1;
(4) oil-phase solution that step (3) is made mixes with the aqueous phase solution that step (2) makes, and stirs, and makes the aluminum isopropylate microemulsion;
(5) the aluminum isopropylate microemulsion that step (4) is made adds ammoniacal liquor or bicarbonate of ammonia is regulated pH=8～10; Be hydrolyzed at 50～100 ℃ of water-bath 20～90min; The gel that obtains is carried out suction filtration; A large amount of deionized waters, dehydrated alcohol or washing with acetone; Oven dry, calcining obtains high-purity α-Al under 900～1200 ℃
2O
3Powder;
Said water is a deionized water;
Said oil phase is a kind of in hexanaphthene, normal hexane, benzene,toluene,xylene and the octane;
Said tensio-active agent is that OP-10 is that alkylphenol-polyethenoxy (10) ether, OPE-2 are that octyl phenol polyoxy ethene (2) ether, OPE-10 are that polyoxyethylene octylphenol ether, Tween-40, tween-80, triton x-100 and sulfonated lignin HLB value are one or more of 8-18;
Said cosurfactant is a kind of in ethanol, propyl alcohol, propyl carbinol and the Virahol.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 201110236817 CN102303882B (en) | 2011-08-16 | 2011-08-16 | Method for preparing alpha-Al2O3 powder from microemulsion |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 201110236817 CN102303882B (en) | 2011-08-16 | 2011-08-16 | Method for preparing alpha-Al2O3 powder from microemulsion |
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|---|---|
| CN102303882A true CN102303882A (en) | 2012-01-04 |
| CN102303882B CN102303882B (en) | 2013-04-03 |
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|---|---|---|---|
| CN 201110236817 Active CN102303882B (en) | 2011-08-16 | 2011-08-16 | Method for preparing alpha-Al2O3 powder from microemulsion |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108585017A (en) * | 2018-07-24 | 2018-09-28 | 中铝稀土（江苏）有限公司 | A kind of preparation method of rare earth oxide ceria |
| CN108706618A (en) * | 2018-08-28 | 2018-10-26 | 内江师范学院 | Utilize the method for micro-emulsion method for preparing nano aluminium oxide |
| CN112744863A (en) * | 2021-02-03 | 2021-05-04 | 浙江爱科新材料有限公司 | Preparation method of high-purity superfine zirconia |
| CN112939043A (en) * | 2021-03-19 | 2021-06-11 | 山东大学 | Preparation method and application of alpha-alumina with reduced phase transition temperature |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH08198622A (en) * | 1995-01-18 | 1996-08-06 | Sumitomo Chem Co Ltd | Production of aluminum hydroxide and alumina |
| CN101391786A (en) * | 2008-11-10 | 2009-03-25 | 国家纳米科学中心 | Method for preparing high specific surface area nano alumina material |
| CN101792164A (en) * | 2009-11-19 | 2010-08-04 | 国家纳米科学中心 | Method for preparing nano aluminum oxide through vacuum freeze drying technology |
-
2011
- 2011-08-16 CN CN 201110236817 patent/CN102303882B/en active Active
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH08198622A (en) * | 1995-01-18 | 1996-08-06 | Sumitomo Chem Co Ltd | Production of aluminum hydroxide and alumina |
| CN101391786A (en) * | 2008-11-10 | 2009-03-25 | 国家纳米科学中心 | Method for preparing high specific surface area nano alumina material |
| CN101792164A (en) * | 2009-11-19 | 2010-08-04 | 国家纳米科学中心 | Method for preparing nano aluminum oxide through vacuum freeze drying technology |
Non-Patent Citations (1)
| Title |
|---|
| 朴玲钰等: "反相微乳液法制备纳米氧化铝", 《物理化学学报》 * |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108585017A (en) * | 2018-07-24 | 2018-09-28 | 中铝稀土（江苏）有限公司 | A kind of preparation method of rare earth oxide ceria |
| CN108706618A (en) * | 2018-08-28 | 2018-10-26 | 内江师范学院 | Utilize the method for micro-emulsion method for preparing nano aluminium oxide |
| CN112744863A (en) * | 2021-02-03 | 2021-05-04 | 浙江爱科新材料有限公司 | Preparation method of high-purity superfine zirconia |
| CN112939043A (en) * | 2021-03-19 | 2021-06-11 | 山东大学 | Preparation method and application of alpha-alumina with reduced phase transition temperature |
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| Publication number | Publication date |
|---|---|
| CN102303882B (en) | 2013-04-03 |
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