CN1235803C - Method for preparing alumina in fire resistant and high specific surface - Google Patents
Method for preparing alumina in fire resistant and high specific surface Download PDFInfo
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- CN1235803C CN1235803C CN 200410017267 CN200410017267A CN1235803C CN 1235803 C CN1235803 C CN 1235803C CN 200410017267 CN200410017267 CN 200410017267 CN 200410017267 A CN200410017267 A CN 200410017267A CN 1235803 C CN1235803 C CN 1235803C
- Authority
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- China
- Prior art keywords
- specific surface
- gel
- aluminum oxide
- alumina
- high temperature
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- Expired - Fee Related
Links
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 title claims abstract description 26
- 238000000034 method Methods 0.000 title claims abstract description 7
- 230000009970 fire resistant effect Effects 0.000 title 1
- 239000000499 gel Substances 0.000 claims abstract description 19
- 239000011240 wet gel Substances 0.000 claims abstract description 14
- 229910052708 sodium Inorganic materials 0.000 claims abstract description 12
- 239000011734 sodium Substances 0.000 claims abstract description 12
- 235000019353 potassium silicate Nutrition 0.000 claims abstract description 10
- NTHWMYGWWRZVTN-UHFFFAOYSA-N sodium silicate Chemical compound [Na+].[Na+].[O-][Si]([O-])=O NTHWMYGWWRZVTN-UHFFFAOYSA-N 0.000 claims abstract description 10
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 claims abstract description 8
- 238000001035 drying Methods 0.000 claims abstract description 8
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims abstract description 5
- 239000012530 fluid Substances 0.000 claims abstract description 5
- 239000002994 raw material Substances 0.000 claims abstract description 5
- 238000003980 solgel method Methods 0.000 claims abstract description 4
- 229910052814 silicon oxide Inorganic materials 0.000 claims abstract description 3
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 claims description 32
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims description 24
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 13
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical group CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 11
- 238000002360 preparation method Methods 0.000 claims description 11
- 229910052782 aluminium Inorganic materials 0.000 claims description 10
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 claims description 10
- 239000004411 aluminium Substances 0.000 claims description 9
- 238000003756 stirring Methods 0.000 claims description 9
- 229910004298 SiO 2 Inorganic materials 0.000 claims description 7
- 229960000935 dehydrated alcohol Drugs 0.000 claims description 5
- INOXWHFCQLMHDY-UHFFFAOYSA-N ethanol nitric acid Chemical compound [N+](=O)(O)[O-].[N+](=O)(O)[O-].[N+](=O)(O)[O-].C(C)O INOXWHFCQLMHDY-UHFFFAOYSA-N 0.000 claims description 5
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims description 4
- 239000012153 distilled water Substances 0.000 claims description 4
- 229910017604 nitric acid Inorganic materials 0.000 claims description 4
- 238000012545 processing Methods 0.000 claims description 4
- 229960004756 ethanol Drugs 0.000 claims description 3
- 238000001914 filtration Methods 0.000 claims description 3
- 230000008569 process Effects 0.000 claims description 3
- 238000005406 washing Methods 0.000 claims description 3
- 238000004519 manufacturing process Methods 0.000 abstract description 3
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 description 6
- 239000003054 catalyst Substances 0.000 description 5
- 239000007789 gas Substances 0.000 description 5
- 239000000463 material Substances 0.000 description 4
- 230000032683 aging Effects 0.000 description 3
- 230000000694 effects Effects 0.000 description 3
- 239000003345 natural gas Substances 0.000 description 3
- 229910052761 rare earth metal Inorganic materials 0.000 description 3
- 238000005245 sintering Methods 0.000 description 3
- 229910052784 alkaline earth metal Inorganic materials 0.000 description 2
- 150000001342 alkaline earth metals Chemical class 0.000 description 2
- 230000008901 benefit Effects 0.000 description 2
- 238000007084 catalytic combustion reaction Methods 0.000 description 2
- 230000003197 catalytic effect Effects 0.000 description 2
- 230000008859 change Effects 0.000 description 2
- 238000004140 cleaning Methods 0.000 description 2
- 239000002904 solvent Substances 0.000 description 2
- 239000004480 active ingredient Substances 0.000 description 1
- 239000000654 additive Substances 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 238000002485 combustion reaction Methods 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- FAHBNUUHRFUEAI-UHFFFAOYSA-M hydroxidooxidoaluminium Chemical class O[Al]=O FAHBNUUHRFUEAI-UHFFFAOYSA-M 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 238000005554 pickling Methods 0.000 description 1
- 230000002265 prevention Effects 0.000 description 1
- -1 rare earth ion Chemical class 0.000 description 1
- 150000002910 rare earth metals Chemical class 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 239000000377 silicon dioxide Substances 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 239000011343 solid material Substances 0.000 description 1
- 230000006641 stabilisation Effects 0.000 description 1
- 238000011105 stabilization Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000000967 suction filtration Methods 0.000 description 1
- 230000009466 transformation Effects 0.000 description 1
Landscapes
- Compounds Of Alkaline-Earth Elements, Aluminum Or Rare-Earth Metals (AREA)
- Catalysts (AREA)
Abstract
The present invention relates to a method for preparing alumina with high temperature resistance and high specific surface. Sodium metaaluminate and water glass are used as raw materials; the technology that a sol-gel method is used for preparing alumina wet gel, and a supercritical fluid drying method is used for preparing alumina dry gel is adopted to prepare alumina with high temperature resistance and high specific surface; the silicon oxide content in the alumina is from 0.1 to 10 wt%; the alumina dry gel is processed for 4h in air atmosphere with a temperature of 500 DEG C, and the specific surface area is larger than 365m<2>/g; in air atmosphere with a temperature of 1100 DEG C, the alumina dry gel is processed for 4h and the specific surface area is larger than 165m<2>/g. The present invention has the characteristics of simple technology, low production cost, large specific surface area of alumina, and good heat resistant stability.
Description
Technical field
The present invention relates to preparation inorganic and that solid material is chemical, particularly a kind of preparation method of high temperature resistant high specific surface aluminium.
Background technology
Concerning a lot of catalyzer, aluminum oxide is a kind of very good economic again support of the catalyst, the aluminum oxide of a lot of crystalline state all has bigger specific surface area, but critical defect is arranged as the support of the catalyst of aspects such as catalytic cleaning of car tail gas, natural gas catalytic combustion, be that temperature will be transformed into the α phase in the time of 1000～1200 ℃, cause specific surface acutely to reduce, cause that the active ingredient of area load is assembled, thereby catalyst activity is obviously descended.Therefore stablize the structure of aluminum oxide, make it at high temperature keep big specific surface, prevent to be converted into little surface-area and the active alpha-type aluminum oxide that reduces, this is for the thermostability that improves catalyzer, and it is significant to be convenient to industrial application.
In recent years, the heat-resistant stability of aluminium oxide structure is studied extremely people's concern.People are mainly by introducing the component that can play stabilization in the material that maybe can generate aluminum oxide at aluminum oxide, as introduce additives such as rare earth or alkaline-earth metal by pickling process, the high temperature sintering and the α phase transformation of aluminum oxide can be stoped effectively, thereby its high high-temp stability can be improved greatly.Introduce rare-earth elements La
3+, Ce
4+, Pr
3+, Sn
3+On can both stablize aluminum oxide structure, La
3+Modified effect the best is as 5%La/Al
2O
3After 1000 ℃ of roastings, its specific surface still can reach 60～70m
2/ g.Research is thought that the rare earth ion radius is big and valence state is high and can be reduced the ionic movability, thereby at high temperature can be fixed on the sintering of the surface of aluminum oxide with the prevention aluminum oxide.Alkaline-earth metal Ba
2+, Sr
2+, Ca
2+Be found the structure that to stablize aluminum oxide equally Deng oxide compound, be considered to because the introducing of BaO has changed Al as the high-temperature stable effect of BaO
2O
3Structure, formed the aluminic acid salt face and stoped Al
3+Body spread mutually, and BaO also eliminated and caused the removable species AlOH of agglomerating, reduced sintering kinetics speed.But the alumina material of above-mentioned this modification will be as the solid support material of high performance cleaning catalyst for tail gases of automobiles or natural gas catalytic combustion catalyzer, because catalyzer is in the hot environment more than 1000 ℃ for a long time, its heat-resistant stability still is difficult to satisfy its requirement.
Summary of the invention
The technology of preparing that the purpose of this invention is to provide a kind of high temperature resistant high specific surface aluminium of economy.
The invention provides the method for the high temperature resistant high specific surface aluminium of preparation, be that sodium metaaluminate and water glass with cheapness is raw material, adopt sol-gel method to prepare the aluminum oxide wet gel, in the aluminum oxide wet gel process for preparation, earlier sodium metaaluminate is dissolved in the water, adds the water glass of aequum then, it is 8.5～9.5 that the back rare nitric acid of dropping that stirs transfers to the pH value, after continuing to stir 0.5～2h, leave standstill aging 5～24h.Supercritical fluid drying prepares the alumina dry gel, and distilled water filtering and washing 5～8 times of aluminum oxide wet gel with the water in the dehydrated alcohol exchange gel, place in the autoclave more then.Add supercritical medium.Under super critical condition, keep 1～4h, under constant temperature, slowly emit gas then, get the silica/alumina xerogel.In air atmosphere,, make the aluminum oxide of high temperature resistant high-ratio surface through 300～600 ℃ of processing.The content of silicon oxide is 0.1～10wt%.
Above-mentioned aluminum oxide wet gel is sodium metaaluminate-water glass-aqueous systems, presses Al
2O
3: SiO
2: H
2O=1: 0.017～0.17: the ratio of 40～80 (mol ratios).
Described water glass contains SiO
220～30wt%, Na
2O 5～10%wt%.
Described supercritical medium is a kind of solvent in ethanol, methyl alcohol, ethanol-methyl alcohol or the ethanol-nitric acid (pH is 3～4).
Described super critical condition is pressure 6.5～10MPa, 1.0～3.5 ℃/min of temperature rise rate, 245～300 ℃ of temperature.
Above-mentioned alumina dry gel is 300～600 ℃ of processing 1～5h in air atmosphere, obtain the aluminum oxide of high temperature resistant high-ratio surface.
The technology of preparation provided by the present invention is high temperature resistant high specific surface aluminium, its advantage is: adopting cheap sodium metaaluminate and water glass is raw material, and production cost is low; Adopting sol-gel method to prepare aluminum oxide wet gel and supercritical fluid drying, to prepare the technology of alumina dry gel simple, and reaction process is controlled easily, realizes industrialized production easily; The alumina material specific surface that makes is big, resistance to elevated temperatures good, handles 4h as the alumina dry gel in 500 ℃ of air atmospheres, and its specific surface area is greater than 365m
2/ g handles 4h in 1100 ℃ of air atmospheres, its specific surface area is greater than 165m
2/ g, high temperature resistant high specific surface aluminum of the present invention will have broad application prospects at aspects such as catalyst for catalytic purifying car tail gas or combustion of natural gas catalyzer.
Method of the present invention has the advantages that cost is low, the specific surface of aluminum oxide is big and resistance to elevated temperatures is good.
Embodiment
Embodiment 1
Ratio Al in the aluminum oxide wet gel
2O
3: SiO
2: H
2O=1: 0.017～0.17: 40～80 (mol ratios),
Sodium metaaluminate is dissolved in the water, under intensive stirs, drips water glass (SiO
220～30wt%, Na
2O5～10%wt%), it is 8.5～9.5 that the back rare nitric acid of dropping that stirs transfers to the pH value, continues to stir after 0.5～2 hour, leaves standstill aging 5～24 hours, promptly obtains the aluminum oxide wet gel.With distilled water filtering and washing 5～8 times of aluminum oxide wet gel, again with the water in the dehydrated alcohol exchange gel, place in the autoclave then, add supercritical medium (as a kind of solvent of ethanol, methyl alcohol, ethanol-methyl alcohol or ethanol-nitric acid (pH is 3～4)), carry out the supercritical methanol technology drying, temperature rise rate 1.5K/min kept 1～4 hour after reaching 280 ℃ of temperature and pressure 8.5MPa, slowly emit gas then under the constant temperature, obtain the alumina dry gel; In air atmosphere,, make the aluminum oxide of high temperature resistant high-ratio surface through 300～600 ℃ of processing.
Embodiment 2
At first, get the 3.5g meta-aluminic acid and receive and be dissolved in the 40g water, under intensive stirs, drip 0.68g water glass (SiO
225.9wt%, Na
2O 8.0%wt%), dripping the rare nitric acid of 0.1M after stirring again is 9 to pH, after half an hour is stirred in continuation, leaves standstill aging ten hours, promptly obtains the aluminum oxide wet gel.With distilled water filter wash six times of this aluminum oxide wet gel, with water 2 times and suction filtration in the 50ml dehydrated alcohol exchange gel, place then in the autoclave again, add 50ml dehydrated alcohol (being supercritical medium), carry out the supercritical methanol technology drying.Temperature rise rate 1.5K/min kept 2 hours after reaching 280 ℃ of temperature and pressure 8.5MPa, slowly emitted gas then under the constant temperature, obtained the alumina dry gel.This alumina dry gel is handled 4h in 500 ℃ of air atmospheres, the specific surface area 436m of aluminum oxide
2/ g handles 4h in 1100 ℃ of air atmospheres, its specific surface area 171m
2/ g.
Embodiment 3
With embodiment 1 identical operations, difference is: change supercritical medium into 50ml methyl alcohol, postcritical temperature and pressure changes 270 ℃ and 10MPa respectively into.Resulting alumina dry gel is handled 4h in 500 ℃ of air atmospheres, the specific surface area 395m of aluminum oxide
2/ g handles 4h in 1100 ℃ of air atmospheres, its specific surface area 168m
2/ g.
Embodiment 4
With embodiment 1 identical operations, difference is: change supercritical medium into 50ml ethanol-nitric acid (pH is 3～4).Resulting alumina dry gel is handled 4h in 500 ℃ of air atmospheres, the specific surface area 378m of aluminum oxide
2/ g handles 4h in 1100 ℃ of air atmospheres, its specific surface area 171m
2/ g.
Claims (4)
1, a kind of preparation method of high temperature resistant high specific surface aluminium, with sodium metaaluminate and water glass is raw material, adopt sol-gel method to prepare the aluminum oxide wet gel, adopt supercritical fluid drying to prepare the alumina dry gel, it is characterized in that described aluminum oxide wet gel process for preparation, earlier sodium metaaluminate is dissolved in the water, presses Al then
2O
3: SiO
2: H
2The mol ratio of O is 1: 0.017～0.17: 40～80 adding water glass, and it is 8.5～9.5 that the back rare nitric acid of dropping that stirs transfers to the pH value, continues to stir after 0.5～2 hour, leaves standstill and wears out 5～24 hours; Described supercritical fluid drying prepares the alumina dry gel, earlier with aluminum oxide wet gel distilled water filtering and washing, again with the water in the dehydrated alcohol exchange gel, place then in the autoclave, the adding supercritical medium is a kind of of ethanol, methyl alcohol, ethanol-methyl alcohol or ethanol-nitric acid, and wherein the pH of ethanol-nitric acid is 3～4, carry out the supercritical methanol technology drying, super critical condition kept 1～4 hour down, slowly emitted gas then under the constant temperature, obtained the alumina dry gel; In air atmosphere,, make the aluminum oxide of high temperature resistant high-ratio surface through 300～600 ℃ of processing.
2, the preparation method of high temperature resistant high specific surface aluminium according to claim 1 is characterized in that: described water glass raw material contains SiO
220～30wt%, Na
2O 5～10wt%.
3, the preparation method of high temperature resistant high specific surface aluminium according to claim 1 is characterized in that: described super critical condition is 245～300 ℃ of pressure 6.5～10MPa, 1.0～3.5 ℃/min of temperature rise rate, temperature.
4, the preparation method of high temperature resistant high specific surface aluminium according to claim 1 is characterized in that: make in the aluminum oxide, the content of silicon oxide is 0.1～10wt%.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 200410017267 CN1235803C (en) | 2004-03-25 | 2004-03-25 | Method for preparing alumina in fire resistant and high specific surface |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 200410017267 CN1235803C (en) | 2004-03-25 | 2004-03-25 | Method for preparing alumina in fire resistant and high specific surface |
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| Publication Number | Publication Date |
|---|---|
| CN1562753A CN1562753A (en) | 2005-01-12 |
| CN1235803C true CN1235803C (en) | 2006-01-11 |
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| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN 200410017267 Expired - Fee Related CN1235803C (en) | 2004-03-25 | 2004-03-25 | Method for preparing alumina in fire resistant and high specific surface |
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| Country | Link |
|---|---|
| CN (1) | CN1235803C (en) |
Families Citing this family (22)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101104523B (en) * | 2006-07-14 | 2010-09-01 | 中国科学院大连化学物理研究所 | Method for preparing high specific surface area high thermal stability aluminum oxide |
| CN101343075B (en) * | 2008-08-22 | 2011-01-26 | 中国铝业股份有限公司 | Control method for b value of sodium aluminate solution |
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| CN105597634A (en) * | 2016-01-29 | 2016-05-25 | 卓达新材料科技集团有限公司 | Supercritical drying method for glass wool/silicon-aluminum aerogel composite heat preservation plate |
| CN105776965A (en) * | 2016-01-29 | 2016-07-20 | 卓达新材料科技集团有限公司 | Preparation method of glass wool-aluminum silicon aerogel composite heat preservation plate |
| CN105664809A (en) * | 2016-01-29 | 2016-06-15 | 卓达新材料科技集团有限公司 | Supercritical drying method of felt/silicon-aluminum aerogel composite insulation board |
| CN105753439A (en) * | 2016-01-29 | 2016-07-13 | 卓达新材料科技集团有限公司 | Fiber punched felt/sliicon-alumininm aerogel composite insulation board |
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| CN114797753A (en) * | 2022-04-29 | 2022-07-29 | 武汉理工大学 | Alumina-based trapping material for efficiently adsorbing carbon dioxide and preparation method and application thereof |
-
2004
- 2004-03-25 CN CN 200410017267 patent/CN1235803C/en not_active Expired - Fee Related
Also Published As
| Publication number | Publication date |
|---|---|
| CN1562753A (en) | 2005-01-12 |
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