CN108855043A - A kind of preparation method of alumina fibre-bismuth oxide composite catalyst - Google Patents
A kind of preparation method of alumina fibre-bismuth oxide composite catalyst Download PDFInfo
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- CN108855043A CN108855043A CN201810799505.7A CN201810799505A CN108855043A CN 108855043 A CN108855043 A CN 108855043A CN 201810799505 A CN201810799505 A CN 201810799505A CN 108855043 A CN108855043 A CN 108855043A
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- Prior art keywords
- alumina fibre
- composite catalyst
- oxide composite
- bismuth oxide
- bismuth
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- 229910000416 bismuth oxide Inorganic materials 0.000 title claims abstract description 33
- 239000003054 catalyst Substances 0.000 title claims abstract description 32
- 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 27
- 239000002131 composite material Substances 0.000 title claims abstract description 27
- 238000002360 preparation method Methods 0.000 title claims abstract description 16
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 claims abstract description 35
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 14
- 229960000935 dehydrated alcohol Drugs 0.000 claims abstract description 14
- 238000003756 stirring Methods 0.000 claims abstract description 14
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Chemical compound NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 claims abstract description 13
- 239000004202 carbamide Substances 0.000 claims abstract description 13
- 150000001621 bismuth Chemical class 0.000 claims abstract description 12
- 238000010041 electrostatic spinning Methods 0.000 claims abstract description 12
- 239000000463 material Substances 0.000 claims abstract description 12
- 238000010438 heat treatment Methods 0.000 claims abstract description 11
- 229910000329 aluminium sulfate Inorganic materials 0.000 claims abstract description 10
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 8
- 239000004372 Polyvinyl alcohol Substances 0.000 claims abstract description 7
- 159000000013 aluminium salts Chemical class 0.000 claims abstract description 7
- 239000007864 aqueous solution Substances 0.000 claims abstract description 7
- 239000008367 deionised water Substances 0.000 claims abstract description 7
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 7
- 238000001035 drying Methods 0.000 claims abstract description 7
- 229920002451 polyvinyl alcohol Polymers 0.000 claims abstract description 7
- 238000009987 spinning Methods 0.000 claims abstract description 7
- 238000001816 cooling Methods 0.000 claims abstract description 5
- 238000010792 warming Methods 0.000 claims abstract description 5
- 239000000126 substance Substances 0.000 claims description 12
- 229910052797 bismuth Inorganic materials 0.000 claims description 7
- JCXGWMGPZLAOME-UHFFFAOYSA-N bismuth atom Chemical compound [Bi] JCXGWMGPZLAOME-UHFFFAOYSA-N 0.000 claims description 7
- VSCWAEJMTAWNJL-UHFFFAOYSA-K aluminium trichloride Chemical compound Cl[Al](Cl)Cl VSCWAEJMTAWNJL-UHFFFAOYSA-K 0.000 claims description 6
- TYIXMATWDRGMPF-UHFFFAOYSA-N dibismuth;oxygen(2-) Chemical compound [O-2].[O-2].[O-2].[Bi+3].[Bi+3] TYIXMATWDRGMPF-UHFFFAOYSA-N 0.000 claims description 4
- BNGXYYYYKUGPPF-UHFFFAOYSA-M (3-methylphenyl)methyl-triphenylphosphanium;chloride Chemical compound [Cl-].CC1=CC=CC(C[P+](C=2C=CC=CC=2)(C=2C=CC=CC=2)C=2C=CC=CC=2)=C1 BNGXYYYYKUGPPF-UHFFFAOYSA-M 0.000 claims description 3
- 229910002651 NO3 Inorganic materials 0.000 claims description 3
- NHNBFGGVMKEFGY-UHFFFAOYSA-N Nitrate Chemical compound [O-][N+]([O-])=O NHNBFGGVMKEFGY-UHFFFAOYSA-N 0.000 claims description 3
- IOVCWXUNBOPUCH-UHFFFAOYSA-M Nitrite anion Chemical compound [O-]N=O IOVCWXUNBOPUCH-UHFFFAOYSA-M 0.000 claims description 3
- SMZOGRDCAXLAAR-UHFFFAOYSA-N aluminium isopropoxide Chemical compound [Al+3].CC(C)[O-].CC(C)[O-].CC(C)[O-] SMZOGRDCAXLAAR-UHFFFAOYSA-N 0.000 claims description 3
- DIZPMCHEQGEION-UHFFFAOYSA-H aluminium sulfate (anhydrous) Chemical compound [Al+3].[Al+3].[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O DIZPMCHEQGEION-UHFFFAOYSA-H 0.000 claims description 3
- 150000003839 salts Chemical class 0.000 claims 1
- 230000003197 catalytic effect Effects 0.000 abstract description 3
- 238000000034 method Methods 0.000 description 10
- BDJYZEWQEALFKK-UHFFFAOYSA-N bismuth;hydrate Chemical class O.[Bi] BDJYZEWQEALFKK-UHFFFAOYSA-N 0.000 description 3
- 238000005516 engineering process Methods 0.000 description 3
- 239000000835 fiber Substances 0.000 description 3
- 229910017604 nitric acid Inorganic materials 0.000 description 3
- -1 nitric acid aluminium salt Chemical class 0.000 description 3
- 230000001699 photocatalysis Effects 0.000 description 3
- 238000007789 sealing Methods 0.000 description 3
- WMWLMWRWZQELOS-UHFFFAOYSA-N bismuth(III) oxide Inorganic materials O=[Bi]O[Bi]=O WMWLMWRWZQELOS-UHFFFAOYSA-N 0.000 description 2
- 239000003795 chemical substances by application Substances 0.000 description 2
- 150000001875 compounds Chemical class 0.000 description 2
- 239000004065 semiconductor Substances 0.000 description 2
- 229920000049 Carbon (fiber) Polymers 0.000 description 1
- 230000032900 absorption of visible light Effects 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 239000004917 carbon fiber Substances 0.000 description 1
- 230000015556 catabolic process Effects 0.000 description 1
- 238000006555 catalytic reaction Methods 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 238000006731 degradation reaction Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 239000003344 environmental pollutant Substances 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 238000006864 oxidative decomposition reaction Methods 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 239000002957 persistent organic pollutant Substances 0.000 description 1
- 238000007146 photocatalysis Methods 0.000 description 1
- 231100000719 pollutant Toxicity 0.000 description 1
- HBMJWWWQQXIZIP-UHFFFAOYSA-N silicon carbide Chemical compound [Si+]#[C-] HBMJWWWQQXIZIP-UHFFFAOYSA-N 0.000 description 1
- 229910010271 silicon carbide Inorganic materials 0.000 description 1
- 150000003384 small molecules Chemical class 0.000 description 1
- 239000000243 solution Substances 0.000 description 1
- 230000004083 survival effect Effects 0.000 description 1
Classifications
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J23/00—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
- B01J23/16—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of arsenic, antimony, bismuth, vanadium, niobium, tantalum, polonium, chromium, molybdenum, tungsten, manganese, technetium or rhenium
- B01J23/18—Arsenic, antimony or bismuth
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J35/00—Catalysts, in general, characterised by their form or physical properties
- B01J35/30—Catalysts, in general, characterised by their form or physical properties characterised by their physical properties
- B01J35/39—Photocatalytic properties
Landscapes
- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Catalysts (AREA)
- Inorganic Fibers (AREA)
Abstract
The invention discloses a kind of alumina fibre-bismuth oxide composite catalyst preparation methods, including:(1) the ratio between volume is added in aluminium salt is 1:In 1~3 polyvinyl alcohol and the mixed liquor of dehydrated alcohol, stir 1~2h, it is then injected into electrostatic spinning apparatus, electrostatic spinning is carried out under conditions of voltage is 15~25kV, reception distance is 5~15cm, receiving time is 2~5h, obtained spinning material is placed in heat drying in Muffle furnace, 400~500 DEG C are warming up to by 5~10 DEG C of heating rate, 5~8h of constant temperature obtains alumina fibre;(2) water-soluble bismuth salt is added in the aqueous solution containing urea, 3~8h is stirred under the conditions of 90~105 DEG C, add above-mentioned alumina fibre, continue 15~25min of stirring, seal, is placed in 8~12h of heating in 150~200 DEG C of baking oven, it is cooling, deionized water is respectively adopted and dehydrated alcohol washs 2~5 times, it is dry, obtain alumina fibre-bismuth oxide composite catalyst.Alumina fibre produced by the present invention-bismuth oxide composite catalyst has the characteristics that specific surface area is high, thermal stability is good and catalytic performance is excellent.
Description
Technical field
The present invention relates to field of material technology, more particularly to a kind of alumina fibre-bismuth oxide composite catalyst system
Preparation Method.
Background technique
The seriousness of environmental pollution at present, it has also become one directly threatens human survival, the focal issue of urgent need to resolve.Light
Catalysis technique be gradually grow up the seventies from twentieth century have the green of important application prospect in the energy and environmental area
Color technology.The technology can make the organic pollutant in environment that oxidative decomposition occur, and finally be degraded to CO2, water and it is inorganic from
The small-molecule substances such as son, therefore without secondary pollution, high palliating degradation degree is considered as current most promising pollution treatment method.
Bismuth based semiconductor photochemical catalyst can have good photocatalytic activity by excited by visible light, and can effectively degrade has
Machine pollutant has good development prospect.Their common feature and significant advantage is exactly to have absorption in visible-range,
With good photocatalysis performance.However, bismuth based semiconductor photochemical catalyst especially Bi2O3There are light induced electron-skies for photochemical catalyst
Cave be easy in conjunction with, it is fairly limited to the absorption of visible light the problems such as, significantly limit its large-scale application.Therefore, must
Certain measure must be taken to improve light induced electron transport efficiency, it is effective limit electron-hole in conjunction with.
Fiber-loaded type catalyst is a kind of new catalytic material.Alumina fibre is a kind of novel ultra-light matter high-temperature flame-proof
Material, compared with the non-oxidized substances fiber such as carbon fiber, silicon carbide fibre, alumina fibre not only has high intensity, high-modulus, good
The excellent performances such as good chemical resistance of concrete ability, and there are also good high-temperature oxidation resistance, corrosion resistance and electrical insulating properties.Such as
What is by alumina fibre and Bi2O3In conjunction with to prepare high performance catalyst, become current research hotspot.
For this reason, it is necessary in view of the above-mentioned problems, propose a kind of preparation side of alumina fibre-bismuth oxide composite catalyst
Method is able to solve problems of the prior art.
Summary of the invention
The purpose of the present invention is to provide a kind of alumina fibre-bismuth oxide composite catalyst preparation methods, to overcome
Deficiency in the prior art.
To achieve the above object, the present invention provides the following technical solutions:
A kind of preparation method of alumina fibre-bismuth oxide composite catalyst, including:
(1) the ratio between volume is added in aluminium salt is 1:In 1~3 polyvinyl alcohol and the mixed liquor of dehydrated alcohol, stirring 1~
2h is then injected into electrostatic spinning apparatus, voltage be 15~25kV, receive distance be 5~15cm, receiving time is 2~5h
Under conditions of carry out electrostatic spinning, obtained spinning material is placed in heat drying in Muffle furnace, by 5~10 DEG C of heating rate liter
For temperature to 400~500 DEG C, 5~8h of constant temperature obtains alumina fibre;
(2) water-soluble bismuth salt is added in the aqueous solution containing urea, 3~8h of stirring under the conditions of 90~105 DEG C, then plus
Enter above-mentioned alumina fibre, continue 15~25min of stirring, seal, is placed in 8~12h of heating in 150~200 DEG C of baking oven, it is cold
But, deionized water is respectively adopted and dehydrated alcohol washs 2~5 times, it is dry, obtain alumina fibre-bismuth oxide composite catalyst.
Preferably, in step (1), the diameter of the alumina fibre is 150~200nm.
Preferably, in step (1), the aluminium salt is selected from one of aluminum nitrate, aluminum sulfate, aluminium chloride, aluminium isopropoxide.
Preferably, in step (2), the bismuth salt is the nitrate or nitrite of bismuth.
Preferably, in step (2), the ratio between amount of substance of bismuth salt and urea is 1:50~150.
Preferably, the ratio between bismuth salt and the amount of substance of urea are 1:100.
Preferably, in the alumina fibre-bismuth oxide composite catalyst, aluminium oxide accounts for 50~80wt%, and bismuth oxide accounts for
20~50%.
Compared with the prior art, the advantages of the present invention are as follows:Alumina fibre produced by the present invention-bismuth oxide composite catalyzing
In agent, bismuth oxide can be evenly dispersed in alumina fibre surface, have specific surface area height, thermal stability good and catalytic performance
Excellent feature.
Specific embodiment
The present invention is described further by the following example:According to following embodiments, the present invention may be better understood.
However, as it will be easily appreciated by one skilled in the art that specific material ratio, process conditions and its result described in embodiment are only used
In illustrating the present invention, without the present invention described in detail in claims should will not be limited.
The present invention discloses a kind of preparation method of alumina fibre-bismuth oxide composite catalyst, including:
(1) the ratio between volume is added in aluminium salt is 1:In 1~3 polyvinyl alcohol and the mixed liquor of dehydrated alcohol, stirring 1~
2h is then injected into electrostatic spinning apparatus, voltage be 15~25kV, receive distance be 5~15cm, receiving time is 2~5h
Under conditions of carry out electrostatic spinning, obtained spinning material is placed in heat drying in Muffle furnace, by 5~10 DEG C of heating rate liter
For temperature to 400~500 DEG C, 5~8h of constant temperature obtains alumina fibre;
(2) water-soluble bismuth salt is added in the aqueous solution containing urea, 3~8h of stirring under the conditions of 90~105 DEG C, then plus
Enter above-mentioned alumina fibre, continue 15~25min of stirring, seal, is placed in 8~12h of heating in 150~200 DEG C of baking oven, it is cold
But, deionized water is respectively adopted and dehydrated alcohol washs 2~5 times, it is dry, obtain alumina fibre-bismuth oxide composite catalyst.
In above-mentioned steps (1), the diameter of the alumina fibre is 150~200nm, it is preferred that the alumina fibre
Diameter be 180nm;The aluminium salt is selected from one of aluminum nitrate, aluminum sulfate, aluminium chloride, aluminium isopropoxide.
In above-mentioned steps (2), the bismuth salt is the nitrate or nitrite of bismuth;The ratio between bismuth salt and the amount of substance of urea
It is 1:50~150, it is preferred that the ratio between bismuth salt and the amount of substance of urea are 1:100.
In the alumina fibre according to made from the above method-bismuth oxide composite catalyst, aluminium oxide accounts for 50~80wt%, oxygen
Change bismuth and accounts for 20~50%.
It is following that alumina fibre in the present invention-bismuth oxide composite catalyst preparation side is illustrated with specifically embodiment
Method.
Embodiment 1
(1) the ratio between volume is added in nitric acid aluminium salt is 1:In 1 polyvinyl alcohol and the mixed liquor of dehydrated alcohol, 1h is stirred,
It is then injected into electrostatic spinning apparatus, is carried out under conditions of voltage is 15kV, reception distance is 5cm, receiving time is 2h quiet
Electrospun, obtained spinning material are placed in heat drying in Muffle furnace, are warming up to 400 DEG C by 5~10 DEG C of heating rate, constant temperature
5h obtains alumina fibre;
It (2) is 1 by the ratio between amount of substance:50 five nitric hydrate bismuth salts are mixed with the aqueous solution containing urea, at 90 DEG C
Under the conditions of stir 3h, add above-mentioned alumina fibre, continue stir 15min, sealing, be placed in 150 DEG C of baking oven and heat 8h,
It is cooling, deionized water is respectively adopted and dehydrated alcohol washs 2~5 times, it is dry, obtain alumina fibre-bismuth oxide composite catalyzing
Agent.
Embodiment 2
(1) the ratio between volume is added in nitric acid aluminium salt is 1:In 2 polyvinyl alcohol and the mixed liquor of dehydrated alcohol, stirring
1.5h is then injected into electrostatic spinning apparatus, under conditions of voltage is 20kV, reception distance is 10cm, receiving time is 3h
Electrostatic spinning is carried out, obtained spinning material is placed in heat drying in Muffle furnace, is warming up to 450 by 5~10 DEG C of heating rate
DEG C, constant temperature 6h obtains alumina fibre;
It (2) is 1 by the ratio between amount of substance:100 five nitric hydrate bismuth salts are mixed with the aqueous solution containing urea, 100
5h is stirred under the conditions of DEG C, adds above-mentioned alumina fibre, continues to stir 20min, sealing is placed in 180 DEG C of baking oven and heats
10h, it is cooling, deionized water is respectively adopted and dehydrated alcohol washs 2~5 times, it is dry, it is compound to obtain alumina fibre-bismuth oxide
Catalyst.
Embodiment 3
(1) the ratio between volume is added in nitric acid aluminium salt is 1:In 3 polyvinyl alcohol and the mixed liquor of dehydrated alcohol, 2h is stirred,
It is then injected into electrostatic spinning apparatus, is carried out under conditions of voltage is 25kV, reception distance is 15cm, receiving time is 5h quiet
Electrospun, obtained spinning material are placed in heat drying in Muffle furnace, are warming up to 500 DEG C by 5~10 DEG C of heating rate, constant temperature
8h obtains alumina fibre;
It (2) is 1 by the ratio between amount of substance:150 five nitric hydrate bismuth salts are mixed with the aqueous solution containing urea, 105
8h is stirred under the conditions of DEG C, adds above-mentioned alumina fibre, continues to stir 25min, sealing is placed in 200 DEG C of baking oven and heats
12h, it is cooling, deionized water is respectively adopted and dehydrated alcohol washs 2~5 times, it is dry, it is compound to obtain alumina fibre-bismuth oxide
Catalyst.
Electron-microscope scanning test is carried out to alumina fibre obtained in the present invention-bismuth oxide composite catalyst and learns that this is urged
The average grain diameter for changing the alumina fibre in material is 150~200nm, and bismuth oxide can be evenly dispersed in alumina fibre
Surface, to have preferable photocatalytic activity.
Finally, it is to be noted that, the terms "include", "comprise" or its any other variant be intended to it is non-exclusive
Property include so that include a series of elements process, method, article or equipment not only include those elements, but also
Further include other elements that are not explicitly listed, or further include for this process, method, article or equipment it is intrinsic
Element.
Claims (7)
1. a kind of alumina fibre-bismuth oxide composite catalyst preparation method, which is characterized in that including:
(1) the ratio between volume is added in aluminium salt is 1:In 1~3 polyvinyl alcohol and the mixed liquor of dehydrated alcohol, 1~2h is stirred, so
Afterwards inject electrostatic spinning apparatus in, voltage be 15~25kV, receive distance be 5~15cm, the condition that receiving time is 2~5h
Lower carry out electrostatic spinning, obtained spinning material are placed in heat drying in Muffle furnace, are warming up to by 5~10 DEG C of heating rate
400~500 DEG C, 5~8h of constant temperature obtains alumina fibre;
(2) water-soluble bismuth salt is added in the aqueous solution containing urea, 3~8h is stirred under the conditions of 90~105 DEG C, is added
Alumina fibre is stated, 15~25min of stirring is continued, is sealed, 8~12h of heating in 150~200 DEG C of baking oven is placed in, it is cooling, point
Not Cai Yong deionized water and dehydrated alcohol wash 2~5 times, it is dry, obtain alumina fibre-bismuth oxide composite catalyst.
2. alumina fibre according to claim 1-bismuth oxide composite catalyst preparation method, which is characterized in that step
Suddenly in (1), the diameter of the alumina fibre is 150~200nm.
3. alumina fibre according to claim 1-bismuth oxide composite catalyst preparation method, which is characterized in that step
Suddenly in (1), the aluminium salt is selected from one of aluminum nitrate, aluminum sulfate, aluminium chloride, aluminium isopropoxide.
4. alumina fibre according to claim 1-bismuth oxide composite catalyst preparation method, which is characterized in that step
Suddenly in (2), the bismuth salt is the nitrate or nitrite of bismuth.
5. alumina fibre according to claim 1-bismuth oxide composite catalyst preparation method, which is characterized in that step
Suddenly in (2), the ratio between amount of substance of bismuth salt and urea is 1:50~150.
6. alumina fibre according to claim 5-bismuth oxide composite catalyst preparation method, which is characterized in that bismuth
The ratio between amount of substance of salt and urea is 1:100.
7. alumina fibre according to claim 1-bismuth oxide composite catalyst preparation method, which is characterized in that institute
It states in alumina fibre-bismuth oxide composite catalyst, aluminium oxide accounts for 50~80wt%, and bismuth oxide accounts for 20~50%.
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Cited By (1)
Publication number | Priority date | Publication date | Assignee | Title |
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CN110230106A (en) * | 2019-04-16 | 2019-09-13 | 天津工业大学 | A kind of spinning process of continuous nascent oxidation aluminium nano and micro fiber |
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CN103011778A (en) * | 2012-12-14 | 2013-04-03 | 山东大学 | Porous alumina nano fiber and preparation method thereof |
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CN103011778A (en) * | 2012-12-14 | 2013-04-03 | 山东大学 | Porous alumina nano fiber and preparation method thereof |
CN104801294A (en) * | 2015-05-14 | 2015-07-29 | 北京石油化工学院 | Preparation method of bismuth trioxide nanosphere |
CN108855037A (en) * | 2018-07-19 | 2018-11-23 | 刘青 | A kind of preparation method of alumina-silica zinc composite catalyzing material |
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CN110230106A (en) * | 2019-04-16 | 2019-09-13 | 天津工业大学 | A kind of spinning process of continuous nascent oxidation aluminium nano and micro fiber |
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