CN108855037A - A kind of preparation method of alumina-silica zinc composite catalyzing material - Google Patents
A kind of preparation method of alumina-silica zinc composite catalyzing material Download PDFInfo
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- CN108855037A CN108855037A CN201810799502.3A CN201810799502A CN108855037A CN 108855037 A CN108855037 A CN 108855037A CN 201810799502 A CN201810799502 A CN 201810799502A CN 108855037 A CN108855037 A CN 108855037A
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- Prior art keywords
- zinc
- hydroxide
- alumina
- preparation
- catalyzing material
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- 239000000463 material Substances 0.000 title claims abstract description 29
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 title claims abstract description 28
- 229910052725 zinc Inorganic materials 0.000 title claims abstract description 28
- 239000011701 zinc Substances 0.000 title claims abstract description 28
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 title claims abstract description 23
- 239000000377 silicon dioxide Substances 0.000 title claims abstract description 23
- 239000002131 composite material Substances 0.000 title claims abstract description 22
- 238000002360 preparation method Methods 0.000 title claims abstract description 21
- POOYUIHPXFHOCL-UHFFFAOYSA-L [OH-].[Zn+2].[OH-].[Al+3] Chemical compound [OH-].[Zn+2].[OH-].[Al+3] POOYUIHPXFHOCL-UHFFFAOYSA-L 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 18
- 239000007788 liquid Substances 0.000 claims abstract description 13
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 13
- 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 abstract description 12
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Chemical compound NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 claims abstract description 12
- 239000004202 carbamide Substances 0.000 claims abstract description 12
- 238000002156 mixing Methods 0.000 claims abstract description 7
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 5
- 229960000935 dehydrated alcohol Drugs 0.000 claims abstract description 5
- 238000003756 stirring Methods 0.000 claims abstract description 4
- 239000000126 substance Substances 0.000 claims description 17
- 229910021502 aluminium hydroxide Inorganic materials 0.000 claims description 8
- UGZADUVQMDAIAO-UHFFFAOYSA-L zinc hydroxide Chemical compound [OH-].[OH-].[Zn+2] UGZADUVQMDAIAO-UHFFFAOYSA-L 0.000 claims description 8
- 229910021511 zinc hydroxide Inorganic materials 0.000 claims description 8
- 229940007718 zinc hydroxide Drugs 0.000 claims description 8
- XIOUDVJTOYVRTB-UHFFFAOYSA-N 1-(1-adamantyl)-3-aminothiourea Chemical group C1C(C2)CC3CC2CC1(NC(=S)NN)C3 XIOUDVJTOYVRTB-UHFFFAOYSA-N 0.000 claims description 4
- 150000003751 zinc Chemical class 0.000 claims description 3
- 239000003292 glue Substances 0.000 claims description 2
- 150000002500 ions Chemical group 0.000 claims 1
- 238000005406 washing Methods 0.000 claims 1
- 239000008367 deionised water Substances 0.000 abstract description 4
- 229910021641 deionized water Inorganic materials 0.000 abstract description 4
- 230000001681 protective effect Effects 0.000 abstract description 3
- 238000000034 method Methods 0.000 description 9
- XLOMVQKBTHCTTD-UHFFFAOYSA-N Zinc monoxide Chemical compound [Zn]=O XLOMVQKBTHCTTD-UHFFFAOYSA-N 0.000 description 6
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 6
- 239000011787 zinc oxide Substances 0.000 description 3
- 239000003054 catalyst Substances 0.000 description 2
- 150000001875 compounds Chemical class 0.000 description 2
- 230000007812 deficiency Effects 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 230000007613 environmental effect Effects 0.000 description 2
- 230000001699 photocatalysis Effects 0.000 description 2
- 238000007146 photocatalysis Methods 0.000 description 2
- 239000004065 semiconductor Substances 0.000 description 2
- 229910010413 TiO 2 Inorganic materials 0.000 description 1
- 239000004411 aluminium Substances 0.000 description 1
- 229910052782 aluminium Inorganic materials 0.000 description 1
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 1
- 230000015556 catabolic process Effects 0.000 description 1
- 230000003197 catalytic effect Effects 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 239000000356 contaminant Substances 0.000 description 1
- 238000006731 degradation reaction Methods 0.000 description 1
- 238000010894 electron beam technology Methods 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 239000002105 nanoparticle Substances 0.000 description 1
- 229910052759 nickel Inorganic materials 0.000 description 1
- PXHVJJICTQNCMI-UHFFFAOYSA-N nickel Substances [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 description 1
- -1 nickel aluminate Chemical class 0.000 description 1
- 239000011941 photocatalyst Substances 0.000 description 1
- 238000005215 recombination Methods 0.000 description 1
- 230000006798 recombination Effects 0.000 description 1
- 230000006641 stabilisation Effects 0.000 description 1
- 238000011105 stabilization Methods 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
- B01J23/06—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of zinc, cadmium or mercury
-
- 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)
Abstract
The invention discloses a kind of preparation methods of alumina-silica zinc composite catalyzing material, including：(1) aluminum nitrate solution is mixed with excessive urea liquid, quickly stirs 5~10h under 50~60 DEG C of water bath conditions, wherein mixing speed is 1200~1600r/min, obtains aluminum hydroxide sol；(2) a certain amount of zinc solution is added into above-mentioned aluminum hydroxide sol, is uniformly mixed, 1.5~3h is kept the temperature under 70~80 DEG C of water bath conditions, increases bath temperature to 85~95 DEG C, keeps the temperature 4~5h, obtain aluminium hydroxide-zinc hydroxide mixed sols；(3) above-mentioned aluminium hydroxide-zinc hydroxide mixed sols is cooled to room temperature, is filtered by vacuum, is washed 3~5 times with dehydrated alcohol and deionized water respectively, it is dry, 2~3h is calcined under the conditions of 380~450 DEG C, obtains alumina-silica zinc composite catalyzing material.Alumina-silica zinc composite catalyzing material in the present invention has preferable stability, and preparation method is simple, environmentally protective.
Description
Technical field
The present invention relates to field of material technology, more particularly to a kind of preparation of alumina-silica zinc composite catalyzing material
Method.
Background technique
The preparation process of alumina support is simple, and specific surface area is high, and mechanical strength is good, and aperture is suitable for being current using most
One of extensive catalyst carrier, but the co-acting force of the active metal and carrier on pure alumina surface is larger, is easily formed
Inactive species, such as nickel aluminate are not easy to form the II type activity phase of high activity.Therefore the preparation in relation to alumina support
And modified preparation containing aluminium composite oxide is always the direction of scientific worker's research.
Nano zine oxide is a kind of self-activating semiconductor material, and forbidden bandwidth at room temperature is 3.27eV, swashs electron beam
The ability of tiing up is 60meV.This allows for nano zine oxide can stablize the ability of transmitting from ultraviolet light to visible light.Photocatalysis width
It is higher than optically catalytic TiO 2 width, in addition, zinc oxide has very high conductive, heating conduction and very high chemical stabilization again
Property, these have broad application prospects nano zine oxide in fields such as photocatalysis, photoelectric conversions.It is existing nano oxidized
Research of the zinc photochemical catalyst for environmental contaminants degradation has got more and more people's extensive concerning, and in some basic research and application
Research aspect obtains many significant achievements.But for photocatalyst of zinc oxide there is also deficiency, being mainly manifested in it is a kind of broadband
Gap semiconductor material, and Carrier recombination rate is high, quantum efficiency is low, and it is unstable under some extreme conditions, vulnerable to environmental factor
And cause efficiency lower.
For this reason, it is necessary in view of the above-mentioned problems, propose a kind of preparation method of alumina-silica zinc composite catalyzing material,
It 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 preparation methods of alumina-silica zinc composite catalyzing material, existing to overcome
There is the deficiency in technology.
To achieve the above object, the present invention provides the following technical solutions：
A kind of preparation method of alumina-silica zinc composite catalyzing material, including：
(1) aluminum nitrate solution is mixed with excessive urea liquid, quickly stir 5 under 50~60 DEG C of water bath conditions~
10h, wherein mixing speed is 1200~1600r/min, obtains aluminum hydroxide sol；
(2) a certain amount of zinc solution is added into above-mentioned aluminum hydroxide sol, is uniformly mixed, in 70~80 DEG C of water
1.5~3h is kept the temperature under the conditions of bath, is increased bath temperature to 85~95 DEG C, is kept the temperature 4~5h, it is mixed to obtain aluminium hydroxide-zinc hydroxide
Close colloidal sol；
(3) above-mentioned aluminium hydroxide-zinc hydroxide mixed sols is cooled to room temperature, is filtered by vacuum, uses dehydrated alcohol respectively
It is washed 3~5 times with deionized water, it is dry, 2~3h is calcined under the conditions of 380~450 DEG C, obtains that alumina-silica zinc is compound to urge
Change material.
Preferably, in step (1), the ratio between amount of the aluminum nitrate solution and the urea liquid substance is 1:10~15.
Preferably, the ratio between amount of the aluminum nitrate solution and the urea liquid substance is 1:10~12.
Preferably, in step (2), aluminium hydroxide and zinc hydroxide in the aluminium hydroxide-zinc hydroxide mixed sols
The ratio between the amount of substance be 1:1~10.
Preferably, the amount of the substance of the aluminium hydroxide in the aluminium hydroxide-zinc hydroxide mixed sols and zinc hydroxide
The ratio between be 1:1~5.
Preferably, in step (2), the zinc salt is zinc nitrate hexahydrate.
Compared with the prior art, the advantages of the present invention are as follows：Alumina-silica zinc composite catalyzing material tool in the present invention
There is preferable stability, preparation method is simple, environmentally protective.
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-silica zinc composite catalyzing material, including：
(1) aluminum nitrate solution is mixed with excessive urea liquid, quickly stir 5 under 50~60 DEG C of water bath conditions~
10h, wherein mixing speed is 1200~1600r/min, obtains aluminum hydroxide sol；
(2) a certain amount of zinc solution is added into above-mentioned aluminum hydroxide sol, is uniformly mixed, in 70~80 DEG C of water
1.5~3h is kept the temperature under the conditions of bath, is increased bath temperature to 85~95 DEG C, is kept the temperature 4~5h, it is mixed to obtain aluminium hydroxide-zinc hydroxide
Close colloidal sol；
(3) above-mentioned aluminium hydroxide-zinc hydroxide mixed sols is cooled to room temperature, is filtered by vacuum, uses dehydrated alcohol respectively
It is washed 3~5 times with deionized water, it is dry, 2~3h is calcined under the conditions of 380~450 DEG C, obtains that alumina-silica zinc is compound to urge
Change material.
In step (1), the ratio between amount of the aluminum nitrate solution and the urea liquid substance is 1:10~15, it is preferred that
The ratio between amount of the aluminum nitrate solution and the urea liquid substance is 1:10~12, it is further preferred that the aluminum nitrate is molten
The ratio between amount of liquid and the urea liquid substance is 1:11.
In step (2), the substance of aluminium hydroxide and zinc hydroxide in the aluminium hydroxide-zinc hydroxide mixed sols
The ratio between amount is 1:1~10, it is preferred that aluminium hydroxide and zinc hydroxide in the aluminium hydroxide-zinc hydroxide mixed sols
The ratio between amount of substance is 1:1~5, it is further preferred that aluminium hydroxide in the aluminium hydroxide-zinc hydroxide mixed sols and
The ratio between amount of substance of zinc hydroxide is 1:3；The zinc salt is zinc nitrate hexahydrate.
Following preparation sides that alumina-silica zinc composite catalyzing material in the present invention is illustrated with specifically embodiment
Method.
Embodiment 1
It (1) is 1 by the ratio between amount of substance:11 aluminum nitrate solution is mixed with excessive urea liquid, in 55 DEG C of water-bath items
8h is quickly stirred under part, wherein mixing speed 1500r/min obtains aluminum hydroxide sol；
(2) a certain amount of zinc nitrate hexahydrate solution is added into above-mentioned aluminum hydroxide sol, is uniformly mixed, in 75
2.5h is kept the temperature under DEG C water bath condition, bath temperature is increased to 90 DEG C, keeps the temperature 4.5h, and it is molten to obtain aluminium hydroxide-zinc hydroxide mixing
Glue, wherein the ratio between amount of substance of aluminium hydroxide and zinc hydroxide in the aluminium hydroxide-zinc hydroxide mixed sols is 1:
3；
(3) above-mentioned aluminium hydroxide-zinc hydroxide mixed sols is cooled to room temperature, is filtered by vacuum, uses dehydrated alcohol respectively
It is washed 3~5 times with deionized water, it is dry, 2.5h is calcined under the conditions of 420 DEG C, obtains alumina-silica zinc composite catalyzing material
Material.
Alumina-silica zinc composite catalyzing material made from method in the present invention, zinc oxide nano-particle can be uniform
Ground is dispersed in the surface of aluminium oxide, has preferable stability, and the preparation method is simple, environmentally protective, has and preferably answers
Use prospect.
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 (6)
1. a kind of preparation method of alumina-silica zinc composite catalyzing material, which is characterized in that including：
(1) aluminum nitrate solution is mixed with excessive urea liquid, quickly stirs 5~10h under 50~60 DEG C of water bath conditions,
In, mixing speed is 1200~1600r/min, obtains aluminum hydroxide sol；
(2) a certain amount of zinc solution is added into above-mentioned aluminum hydroxide sol, is uniformly mixed, in 70~80 DEG C of water-bath items
1.5~3h is kept the temperature under part, bath temperature is increased to 85~95 DEG C, keeps the temperature 4~5h, and it is molten to obtain aluminium hydroxide-zinc hydroxide mixing
Glue；
(3) above-mentioned aluminium hydroxide-zinc hydroxide mixed sols is cooled to room temperature, is filtered by vacuum, respectively with dehydrated alcohol and going
It is ion water washing 3~5 times, dry, 2~3h is calcined under the conditions of 380~450 DEG C, obtains alumina-silica zinc composite catalyzing material
Material.
2. the preparation method of alumina-silica zinc composite catalyzing material according to claim 1, which is characterized in that step
(1) in, the ratio between amount of the aluminum nitrate solution and the urea liquid substance is 1:10~15.
3. the preparation method of alumina-silica zinc composite catalyzing material according to claim 2, which is characterized in that described
The ratio between amount of aluminum nitrate solution and the urea liquid substance is 1:10~12.
4. the preparation method of alumina-silica zinc composite catalyzing material according to claim 1, which is characterized in that step
(2) in, the ratio between amount of substance of aluminium hydroxide and zinc hydroxide in the aluminium hydroxide-zinc hydroxide mixed sols is 1:1
~10.
5. the preparation method of alumina-silica zinc composite catalyzing material according to claim 4, which is characterized in that described
The ratio between amount of substance of aluminium hydroxide and zinc hydroxide in aluminium hydroxide-zinc hydroxide mixed sols is 1:1~5.
6. the preparation method of alumina-silica zinc composite catalyzing material according to claim 1, which is characterized in that step
(2) in, the zinc salt is zinc nitrate hexahydrate.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108855043A (en) * | 2018-07-19 | 2018-11-23 | 刘青 | A kind of preparation method of alumina fibre-bismuth oxide composite catalyst |
| CN115467047A (en) * | 2022-09-09 | 2022-12-13 | 南通大学 | Preparation method of efficient antibacterial photocatalytic continuous alumina fiber |
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| CN101927158A (en) * | 2010-07-12 | 2010-12-29 | 中国日用化学工业研究院 | Preparation method of nano ZnO/gamma-Al2O3 composite photocatalyst |
| CN102451768A (en) * | 2010-10-15 | 2012-05-16 | 中国石油化工股份有限公司 | Method for preparing zirconia-alumina composite oxide xerogel |
| CN102616829A (en) * | 2012-04-17 | 2012-08-01 | 吉林大学 | Production method for aluminum-doped zinc oxide nanometer material |
| CN103395826A (en) * | 2013-08-06 | 2013-11-20 | 大连交通大学 | Preparation method of aluminum doped zinc oxide nano powder |
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2018
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| CN101927158A (en) * | 2010-07-12 | 2010-12-29 | 中国日用化学工业研究院 | Preparation method of nano ZnO/gamma-Al2O3 composite photocatalyst |
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| CN102616829A (en) * | 2012-04-17 | 2012-08-01 | 吉林大学 | Production method for aluminum-doped zinc oxide nanometer material |
| CN103395826A (en) * | 2013-08-06 | 2013-11-20 | 大连交通大学 | Preparation method of aluminum doped zinc oxide nano powder |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108855043A (en) * | 2018-07-19 | 2018-11-23 | 刘青 | A kind of preparation method of alumina fibre-bismuth oxide composite catalyst |
| CN115467047A (en) * | 2022-09-09 | 2022-12-13 | 南通大学 | Preparation method of efficient antibacterial photocatalytic continuous alumina fiber |
| CN115467047B (en) * | 2022-09-09 | 2023-10-03 | 南通大学 | Preparation method of high-efficiency antibacterial photocatalytic continuous alumina fiber |
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Application publication date: 20181123 |