CN102009993A - Method for preparing submicron aluminium oxide by two-stage roasting method - Google Patents
Method for preparing submicron aluminium oxide by two-stage roasting method Download PDFInfo
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- CN102009993A CN102009993A CN 201010587681 CN201010587681A CN102009993A CN 102009993 A CN102009993 A CN 102009993A CN 201010587681 CN201010587681 CN 201010587681 CN 201010587681 A CN201010587681 A CN 201010587681A CN 102009993 A CN102009993 A CN 102009993A
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- Prior art keywords
- alumina
- submicron order
- prepares
- aluminium oxide
- order method
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Links
- PNEYBMLMFCGWSK-UHFFFAOYSA-N Alumina Chemical compound [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 title claims abstract description 69
- 238000000034 method Methods 0.000 title claims abstract description 37
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims abstract description 22
- 238000001035 drying Methods 0.000 claims abstract description 19
- 238000001914 filtration Methods 0.000 claims abstract description 19
- 239000000843 powder Substances 0.000 claims abstract description 19
- 239000000654 additive Substances 0.000 claims abstract description 18
- 230000000996 additive effect Effects 0.000 claims abstract description 18
- WNROFYMDJYEPJX-UHFFFAOYSA-K aluminium hydroxide Chemical compound [OH-].[OH-].[OH-].[Al+3] WNROFYMDJYEPJX-UHFFFAOYSA-K 0.000 claims abstract description 17
- 229910021502 aluminium hydroxide Inorganic materials 0.000 claims abstract description 17
- 239000002245 particle Substances 0.000 claims abstract description 14
- 229910052757 nitrogen Inorganic materials 0.000 claims abstract description 11
- 239000002994 raw material Substances 0.000 claims abstract description 9
- 239000006185 dispersion Substances 0.000 claims abstract description 7
- 238000005554 pickling Methods 0.000 claims abstract description 6
- 238000005243 fluidization Methods 0.000 claims abstract description 4
- MUBZPKHOEPUJKR-UHFFFAOYSA-N Oxalic acid Chemical compound OC(=O)C(O)=O MUBZPKHOEPUJKR-UHFFFAOYSA-N 0.000 claims description 15
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 claims description 9
- KRKNYBCHXYNGOX-UHFFFAOYSA-N citric acid Chemical compound OC(=O)CC(O)(C(O)=O)CC(O)=O KRKNYBCHXYNGOX-UHFFFAOYSA-N 0.000 claims description 9
- 238000002156 mixing Methods 0.000 claims description 8
- 238000005245 sintering Methods 0.000 claims description 8
- KGBXLFKZBHKPEV-UHFFFAOYSA-N boric acid Chemical compound OB(O)O KGBXLFKZBHKPEV-UHFFFAOYSA-N 0.000 claims description 7
- 239000004327 boric acid Substances 0.000 claims description 7
- 239000003795 chemical substances by application Substances 0.000 claims description 6
- 239000002131 composite material Substances 0.000 claims description 6
- 239000002270 dispersing agent Substances 0.000 claims description 6
- GCLGEJMYGQKIIW-UHFFFAOYSA-H sodium hexametaphosphate Chemical compound [Na]OP1(=O)OP(=O)(O[Na])OP(=O)(O[Na])OP(=O)(O[Na])OP(=O)(O[Na])OP(=O)(O[Na])O1 GCLGEJMYGQKIIW-UHFFFAOYSA-H 0.000 claims description 6
- 235000019982 sodium hexametaphosphate Nutrition 0.000 claims description 6
- 239000001577 tetrasodium phosphonato phosphate Substances 0.000 claims description 6
- 235000006408 oxalic acid Nutrition 0.000 claims description 5
- 239000012467 final product Substances 0.000 claims description 4
- 229920001495 poly(sodium acrylate) polymer Polymers 0.000 claims description 4
- 235000010482 polyoxyethylene sorbitan monooleate Nutrition 0.000 claims description 4
- 229920000053 polysorbate 80 Polymers 0.000 claims description 4
- NNMHYFLPFNGQFZ-UHFFFAOYSA-M sodium polyacrylate Chemical compound [Na+].[O-]C(=O)C=C NNMHYFLPFNGQFZ-UHFFFAOYSA-M 0.000 claims description 4
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 4
- 229910052782 aluminium Inorganic materials 0.000 claims description 3
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 claims description 3
- 239000004411 aluminium Substances 0.000 claims description 3
- 239000004372 Polyvinyl alcohol Substances 0.000 claims description 2
- 238000001354 calcination Methods 0.000 claims description 2
- 229920002521 macromolecule Polymers 0.000 claims description 2
- 150000007524 organic acids Chemical class 0.000 claims description 2
- 230000003647 oxidation Effects 0.000 claims description 2
- 238000007254 oxidation reaction Methods 0.000 claims description 2
- 229920002451 polyvinyl alcohol Polymers 0.000 claims description 2
- 230000001681 protective effect Effects 0.000 claims description 2
- 238000002360 preparation method Methods 0.000 abstract description 5
- 230000005611 electricity Effects 0.000 abstract description 2
- 239000000463 material Substances 0.000 abstract description 2
- 239000013078 crystal Substances 0.000 abstract 3
- 238000009413 insulation Methods 0.000 description 5
- 229920002401 polyacrylamide Polymers 0.000 description 5
- 230000000694 effects Effects 0.000 description 4
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 description 2
- 239000000047 product Substances 0.000 description 2
- 108010022579 ATP dependent 26S protease Proteins 0.000 description 1
- 230000004913 activation Effects 0.000 description 1
- 238000005054 agglomeration Methods 0.000 description 1
- 230000002776 aggregation Effects 0.000 description 1
- 239000013590 bulk material Substances 0.000 description 1
- 229910010293 ceramic material Inorganic materials 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 230000007062 hydrolysis Effects 0.000 description 1
- 238000006460 hydrolysis reaction Methods 0.000 description 1
- 238000005185 salting out Methods 0.000 description 1
Abstract
The invention provides a method for preparing submicron aluminium oxide by a two-stage roasting method, relating to a method for preparing important structural and functional material submicron aluminium oxide used in the fields of electricity, medical treatment, information and the like. The method is characterized in that fluidization primary roasting is carried out on industrial aluminium hydroxide taken as a raw material at the temperature of 400-900 DEG C under the protection of nitrogen, thus obtaining activated aluminium oxide; then organic pickling is carried out, filtering and drying are carried out, and additive is added, so that particle dispersion is uniform, aluminium oxide crystal grains are inhibited from growing at high temperature, and the crystal grains purified; and the crystal grains are evenly mixed, and secondary roasting is carried out at the temperature of 1100-1400 DEG C, thus obtaining the submicron aluminium oxide powder. The submicron aluminium oxide powder prepared by the method has uniform particles, the average grain size is less than or equal to 0.9mu m, the purity is high, and the dispersibility is good. The preparation method is simple, and is low in cost and good in repeatability, thus being easy to realize industrialization.
Description
Technical field
A kind of two-section roasting prepares the submicron order method of alumina, relate to a kind ofly be used for, the important 26S Proteasome Structure and Function material submicron order method of alumina in fields such as electricity, medical treatment and information.
Background technology
Alumina powder jointed because the purity height of submicron order, particle is tiny and be evenly distributed, bigger variation takes place in its surface electronic structure and crystalline structure, thereby have properties such as small-size effect, surface effects, quantum effect and macro quanta tunnel effect, with bulk material diverse characteristic is arranged, thereby make it have more excellent characteristic and application prospects.
Patent CN92104368.6 has reported the preparation method of a kind of controllable nanon size, submicron order aluminum oxide powder, and this method is utilized fine aluminium sheet activation hydrolysis, carries out high-temperature heat treatment then and obtains alumina powder jointed.Patent CN101704680 has reported a kind of submicron order alumina ceramic material and preparation method thereof.Patent CN1565975A has reported that a kind of improvement salting-out process prepares submicron order alumina technology method.
At present still there is great number of issues in the alumina powder jointed technology of preparing of submicron order with using, and mainly is: the pattern of submicron order aluminum oxide is difficult to control, the agglomeration traits of product is difficult to solve, size distribution broad, complex process, condition harshness, cost height and the preparation process poor repeatability of product.
Summary of the invention
Purpose of the present invention mainly is the deficiency that exists at above-mentioned prior art, provides that a kind of method is simple, with low cost, uniform particles, purity height, and the two-section roasting with good dispersing property prepares the submicron order method of alumina.
The objective of the invention is to be achieved through the following technical solutions.
A kind of two-section roasting prepares the submicron order method of alumina, it is characterized in that with the industrial aluminium hydroxide being raw material, under nitrogen protection, under 400 ℃ of-900 ℃ of temperature, carry out one section roasting of fluidization, obtain activated alumina, carry out organic pickling then, add additive behind the filtering drying, make its particles dispersed evenly, the inhibited oxidation aluminium grain at high temperature grows, and makes its purifying; After mixing, under 1100 ℃ of-1400 ℃ of temperature, carry out two-section calcining, finally obtain the alumina powder jointed of submicron order size.
A kind of two-section roasting of the present invention prepares the submicron order method of alumina, it is characterized in that described one section roasting be under the protective atmosphere of inflated with nitrogen under 450 ℃ of-800 ℃ of temperature, carried out fluosolids roasting 1-3 hour, obtain activated alumina.
A kind of two-section roasting of the present invention prepares the submicron order method of alumina, it is characterized in that described organic pickling of carrying out, and used organic acid is oxalic acid, acetic acid or citric acid, and it adds concentration is 0.5-3 g/100g aluminium hydroxide, washs 1-5 time.
A kind of two-section roasting of the present invention prepares the submicron order method of alumina, it is characterized in that adding additive behind the described filtering drying, contain dispersion agent, make its final particles dispersed even, this dispersion agent is that water soluble dispersing agent or water soluble dispersing agent and macromolecule dispersing agent are composite, comprise that sodium polyacrylate, Sodium hexametaphosphate 99, polyvinyl alcohol, tween 80, sodium polyacrylate and Sodium hexametaphosphate 99 are composite by 1:2, Sodium hexametaphosphate 99 and tween 80 be composite by 2:1, selects wherein a kind of getting final product.
A kind of two-section roasting of the present invention prepares the submicron order method of alumina, it is characterized in that adding additive behind the described filtering drying, contains dispersion agent, and its add-on is the 0.1%-5% of aluminium hydroxide.
A kind of two-section roasting of the present invention prepares the submicron order method of alumina, it is characterized in that adding additive behind the described filtering drying, contains to suppress the additive that particle is grown up, and comprises NH
4Cl, MgCl
2, NH
4F, MgF
2, select wherein a kind of getting final product.
A kind of two-section roasting of the present invention prepares the submicron order method of alumina, it is characterized in that adding additive behind the described filtering drying, contains to suppress the additive that particle is grown up, and add-on is the 0.1%-5% of aluminium hydroxide.
A kind of two-section roasting of the present invention prepares the submicron order method of alumina, it is characterized in that adding additive behind the described filtering drying, contains the boric acid that makes its purifying, and add-on is the 0.5-2.0% of aluminium hydroxide.
A kind of two-section roasting of the present invention prepares the submicron order method of alumina, it is characterized in that describedly carrying out second section sintering under 1200 ℃ of-1380 ℃ of temperature, is incubated 2-3 hour, finally obtains the alumina powder jointed of submicron order size.
The submicron order alumina powder uniform particles of method preparation of the present invention, median size≤0.9 μ m, and purity height have good dispersiveness, and method of the present invention is simple, and is with low cost, and good reproducibility is easy to realize industrialization.
Embodiment
A kind of two-section roasting prepares the submicron order method of alumina; with the industrial aluminium hydroxide is raw material, carrying out one section roasting of fluidization under 400 ℃ of-900 ℃ of temperature under the inflated with nitrogen protection, obtains activated alumina; carry out organic pickling then; add additive behind the filtering drying, make its particles dispersed even, suppress; and make its purifying; after mixing, under 1100 ℃ of-1400 ℃ of temperature, carry out second section sintering, finally obtain the alumina powder jointed of submicron order size.
The present invention will be further described below in conjunction with example.
Alumina powder jointed grain graininess utilizes scanning electronic microscope (JSM-6360LV NEC company) to carry out granule-morphology and measures, and ZS-90 zeta potential instrument (Britain Ma Erwen instrument company) carries out the powder diameter test.
Embodiment 1
With the industrial aluminium hydroxide is raw material, and 400 ℃ are carried out one section roasting under the inflated with nitrogen protection, are incubated 3 hr, obtain activated alumina, and the oxalic acid with 3mol/l washs 3 times then, adds 0.5% NH behind the filtering drying
4Cl, 1.0% polyacrylamide, 0.8% boric acid after mixing, carries out double sintering at 1400 ℃, and insulation 2hr finally obtains the alumina powder jointed of 0.7 μ m.
Embodiment 2
With the industrial aluminium hydroxide is raw material, and 900 ℃ are carried out one section roasting under the inflated with nitrogen protection, are incubated 1 hr, obtain activated alumina, and the oxalic acid with 3mol/l washs 3 times then, adds 0.2% NH behind the filtering drying
4Cl, 0.2% polyacrylamide, 0.8% boric acid after mixing, carries out double sintering at 1100 ℃, and insulation 2hr finally obtains the alumina powder jointed of 0.8 μ m.
Embodiment 3
With the industrial aluminium hydroxide is raw material, and 600 ℃ are carried out one section roasting under the inflated with nitrogen protection, are incubated 1.5 hr, obtain activated alumina, and the oxalic acid with 3mol/l washs 3 times then, adds 2.2% NH behind the filtering drying
4Cl, 1.2% polyacrylamide, 0.5% boric acid after mixing, carries out double sintering at 1320 ℃, and insulation 2hr finally obtains the alumina powder jointed of 0.4 μ m.
Embodiment 4
With the industrial aluminium hydroxide is raw material, and 550 ℃ are carried out one section roasting under the inflated with nitrogen protection, are incubated 2 hr, obtain activated alumina, and the citric acid with 2.5mol/l washs 3 times then, adds 0.3% NH behind the filtering drying
4Cl, 0.8% polyacrylamide, 0.2% boric acid after mixing, carries out double sintering at 1240 ℃, and insulation 3hr finally obtains the alumina powder jointed of 0.6 μ m.
Embodiment 5
With the industrial aluminium hydroxide is raw material, and 700 ℃ are carried out one section roasting under the inflated with nitrogen protection, are incubated 1 hr, obtain activated alumina, and the acetic acid with 3mol/l washs 5 times then, adds 0.2% NH behind the filtering drying
4Cl, 1.5% polyacrylamide, 1.0% boric acid after mixing, carries out double sintering at 1400 ℃, and insulation 2hr finally obtains the alumina powder jointed of 0.5 μ m.
Claims (9)
1. a two-section roasting prepares the submicron order method of alumina, it is characterized in that with the industrial aluminium hydroxide being raw material, under nitrogen protection, under 400 ℃ of-900 ℃ of temperature, carry out one section roasting of fluidization, obtain activated alumina, carry out organic pickling then, add additive behind the filtering drying, make its particles dispersed evenly, the inhibited oxidation aluminium grain at high temperature grows, and makes its purifying; After mixing, under 1100 ℃ of-1400 ℃ of temperature, carry out second section calcining, finally obtain the alumina powder jointed of submicron order size.
2. prepare the submicron order method of alumina according to the described a kind of two-section roasting of claim duty; it is characterized in that described one section roasting be under the protective atmosphere of inflated with nitrogen under 450 ℃ of-800 ℃ of temperature; carried out fluosolids roasting 1-3 hour, and obtained activated alumina.
3. a kind of two-section roasting according to claim 1 prepares the submicron order method of alumina, it is characterized in that described organic pickling of carrying out, used organic acid is oxalic acid, acetic acid or citric acid, and it adds concentration is 0.5-3 g/100g aluminium hydroxide, washs 1-5 time.
4. a kind of two-section roasting according to claim 1 prepares the submicron order method of alumina, it is characterized in that adding additive behind the described filtering drying, contain dispersion agent, make its final particles dispersed even, this dispersion agent is that water soluble dispersing agent or water soluble dispersing agent and macromolecule dispersing agent are composite, comprise that sodium polyacrylate, Sodium hexametaphosphate 99, polyvinyl alcohol, tween 80, sodium polyacrylate and Sodium hexametaphosphate 99 are composite by 1:2, Sodium hexametaphosphate 99 and tween 80 be composite by 2:1, selects wherein a kind of getting final product.
5. a kind of two-section roasting according to claim 1 prepares the submicron order method of alumina, it is characterized in that adding additive behind the described filtering drying, contains dispersion agent, and its add-on is the 0.1%-5% of aluminium hydroxide.
6. a kind of two-section roasting according to claim 1 prepares the submicron order method of alumina, it is characterized in that adding additive behind the described filtering drying, contains to suppress the additive that particle is grown up, and comprises NH
4Cl, MgCl
2, NH
4F, MgF
2, select wherein a kind of getting final product.
7. a kind of two-section roasting according to claim 1 prepares the submicron order method of alumina, it is characterized in that adding additive behind the described filtering drying, contains to suppress the additive that particle is grown up, and add-on is the 0.1%-5% of aluminium hydroxide.
8. a kind of two-section roasting according to claim 1 prepares the submicron order method of alumina, it is characterized in that adding additive behind the described filtering drying, contains the boric acid that makes its purifying, and add-on is the 0.5-2.0% of aluminium hydroxide.
9. a kind of two-section roasting according to claim 1 prepares the submicron order method of alumina, it is characterized in that describedly carrying out double sintering under 1200 ℃ of-1380 ℃ of temperature, is incubated 2-3 hour, finally obtains the alumina powder jointed of submicron order size.
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| CN 201010587681 CN102009993A (en) | 2010-12-15 | 2010-12-15 | Method for preparing submicron aluminium oxide by two-stage roasting method |
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|---|---|---|---|
| CN 201010587681 CN102009993A (en) | 2010-12-15 | 2010-12-15 | Method for preparing submicron aluminium oxide by two-stage roasting method |
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| CN 201010587681 Pending CN102009993A (en) | 2010-12-15 | 2010-12-15 | Method for preparing submicron aluminium oxide by two-stage roasting method |
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Cited By (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102910659A (en) * | 2012-10-29 | 2013-02-06 | 上海飞凯光电材料股份有限公司 | Preparation method and application of high-purity aluminum oxide |
| CN104860342A (en) * | 2015-05-07 | 2015-08-26 | 贵州省分析测试研究院 | Method for preparing high-purity ultrafine aluminium oxide |
| CN105664904A (en) * | 2014-11-20 | 2016-06-15 | 中国石油化工股份有限公司 | Potassium retarder preparation method |
| CN109530721A (en) * | 2018-12-11 | 2019-03-29 | 湖南金昊新材料科技股份有限公司 | A kind of sub-micron aluminium powder and acieral powder preparation method |
| CN110625109A (en) * | 2019-09-30 | 2019-12-31 | 中南大学 | Preparation method of submicron aluminum-based alloy powder |
| CN111205070A (en) * | 2020-03-11 | 2020-05-29 | 苏州贝尔德新材料科技有限公司 | Preparation method of easily-sintered high-purity alumina |
| CN111348668A (en) * | 2020-03-16 | 2020-06-30 | 中国铝业股份有限公司 | Preparation method of aluminum oxide for heat-conducting filler |
| CN113830809A (en) * | 2021-10-27 | 2021-12-24 | 中国科学院青海盐湖研究所 | Preparation method of superfine alumina powder and product thereof |
| KR102517803B1 (en) * | 2022-02-03 | 2023-04-05 | 주식회사 씨아이에스케미칼 | High purity alumina, preparation thereof and slurry for coating a separator of a secondary battery comprising the same |
| WO2024029464A1 (en) * | 2022-08-04 | 2024-02-08 | 住友化学株式会社 | Alumina powder, resin composition and method for producing alumina powder |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102910659A (en) * | 2012-10-29 | 2013-02-06 | 上海飞凯光电材料股份有限公司 | Preparation method and application of high-purity aluminum oxide |
| CN105664904A (en) * | 2014-11-20 | 2016-06-15 | 中国石油化工股份有限公司 | Potassium retarder preparation method |
| CN105664904B (en) * | 2014-11-20 | 2018-09-14 | 中国石油化工股份有限公司 | Hinder the preparation method of potassium agent |
| CN104860342A (en) * | 2015-05-07 | 2015-08-26 | 贵州省分析测试研究院 | Method for preparing high-purity ultrafine aluminium oxide |
| CN109530721A (en) * | 2018-12-11 | 2019-03-29 | 湖南金昊新材料科技股份有限公司 | A kind of sub-micron aluminium powder and acieral powder preparation method |
| CN110625109A (en) * | 2019-09-30 | 2019-12-31 | 中南大学 | Preparation method of submicron aluminum-based alloy powder |
| CN111205070A (en) * | 2020-03-11 | 2020-05-29 | 苏州贝尔德新材料科技有限公司 | Preparation method of easily-sintered high-purity alumina |
| CN111348668A (en) * | 2020-03-16 | 2020-06-30 | 中国铝业股份有限公司 | Preparation method of aluminum oxide for heat-conducting filler |
| CN111348668B (en) * | 2020-03-16 | 2022-03-15 | 中国铝业股份有限公司 | Preparation method of aluminum oxide for heat-conducting filler |
| CN113830809A (en) * | 2021-10-27 | 2021-12-24 | 中国科学院青海盐湖研究所 | Preparation method of superfine alumina powder and product thereof |
| KR102517803B1 (en) * | 2022-02-03 | 2023-04-05 | 주식회사 씨아이에스케미칼 | High purity alumina, preparation thereof and slurry for coating a separator of a secondary battery comprising the same |
| WO2024029464A1 (en) * | 2022-08-04 | 2024-02-08 | 住友化学株式会社 | Alumina powder, resin composition and method for producing alumina powder |
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Application publication date: 20110413 |