CN108940267A - A kind of preparation method of silicon dioxide carried platinum composite catalyzing material - Google Patents
A kind of preparation method of silicon dioxide carried platinum composite catalyzing material Download PDFInfo
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- CN108940267A CN108940267A CN201810803363.7A CN201810803363A CN108940267A CN 108940267 A CN108940267 A CN 108940267A CN 201810803363 A CN201810803363 A CN 201810803363A CN 108940267 A CN108940267 A CN 108940267A
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- Prior art keywords
- silicon dioxide
- composite catalyzing
- catalyzing material
- dioxide carried
- silica suspension
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- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 title claims abstract description 148
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 title claims abstract description 104
- 239000000377 silicon dioxide Substances 0.000 title claims abstract description 74
- 229910052697 platinum Inorganic materials 0.000 title claims abstract description 51
- 239000000463 material Substances 0.000 title claims abstract description 36
- 239000002131 composite material Substances 0.000 title claims abstract description 34
- 235000012239 silicon dioxide Nutrition 0.000 title claims abstract description 33
- 238000002360 preparation method Methods 0.000 title claims abstract description 18
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 claims abstract description 72
- 239000000725 suspension Substances 0.000 claims abstract description 37
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 23
- 229960000935 dehydrated alcohol Drugs 0.000 claims abstract description 22
- 238000003756 stirring Methods 0.000 claims abstract description 21
- BOTDANWDWHJENH-UHFFFAOYSA-N Tetraethyl orthosilicate Chemical compound CCO[Si](OCC)(OCC)OCC BOTDANWDWHJENH-UHFFFAOYSA-N 0.000 claims abstract description 16
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 claims abstract description 14
- 239000000908 ammonium hydroxide Substances 0.000 claims abstract description 14
- 239000000047 product Substances 0.000 claims abstract description 9
- NGNBDVOYPDDBFK-UHFFFAOYSA-N 2-[2,4-di(pentan-2-yl)phenoxy]acetyl chloride Chemical compound CCCC(C)C1=CC=C(OCC(Cl)=O)C(C(C)CCC)=C1 NGNBDVOYPDDBFK-UHFFFAOYSA-N 0.000 claims abstract description 7
- 239000002994 raw material Substances 0.000 claims abstract description 7
- 239000012265 solid product Substances 0.000 claims abstract description 7
- 238000001291 vacuum drying Methods 0.000 claims abstract description 7
- 238000005406 washing Methods 0.000 claims abstract description 7
- 238000000034 method Methods 0.000 claims description 14
- 238000002242 deionisation method Methods 0.000 claims description 4
- 239000007788 liquid Substances 0.000 claims description 4
- 239000012298 atmosphere Substances 0.000 claims description 3
- 239000012299 nitrogen atmosphere Substances 0.000 claims description 3
- QBUKAFSEUHGMMX-MTJSOVHGSA-N (5z)-5-[[3-(1-hydroxyethyl)thiophen-2-yl]methylidene]-10-methoxy-2,2,4-trimethyl-1h-chromeno[3,4-f]quinolin-9-ol Chemical class C1=CC=2NC(C)(C)C=C(C)C=2C2=C1C=1C(OC)=C(O)C=CC=1O\C2=C/C=1SC=CC=1C(C)O QBUKAFSEUHGMMX-MTJSOVHGSA-N 0.000 claims 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 abstract description 5
- 239000002245 particle Substances 0.000 abstract description 4
- 239000008367 deionised water Substances 0.000 abstract description 3
- 229910021641 deionized water Inorganic materials 0.000 abstract description 3
- 230000001699 photocatalysis Effects 0.000 abstract description 2
- VQTUBCCKSQIDNK-UHFFFAOYSA-N Isobutene Chemical compound CC(C)=C VQTUBCCKSQIDNK-UHFFFAOYSA-N 0.000 description 18
- NNPPMTNAJDCUHE-UHFFFAOYSA-N isobutane Chemical compound CC(C)C NNPPMTNAJDCUHE-UHFFFAOYSA-N 0.000 description 8
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 6
- 230000003197 catalytic effect Effects 0.000 description 5
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 description 4
- 239000001282 iso-butane Substances 0.000 description 4
- 235000013847 iso-butane Nutrition 0.000 description 4
- 238000006356 dehydrogenation reaction Methods 0.000 description 3
- 238000004519 manufacturing process Methods 0.000 description 3
- 229910052757 nitrogen Inorganic materials 0.000 description 3
- 239000002253 acid Substances 0.000 description 2
- 229910021529 ammonia Inorganic materials 0.000 description 2
- 230000008901 benefit Effects 0.000 description 2
- 239000003054 catalyst Substances 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- XOLBLPGZBRYERU-UHFFFAOYSA-N tin dioxide Chemical compound O=[Sn]=O XOLBLPGZBRYERU-UHFFFAOYSA-N 0.000 description 2
- WJQOZHYUIDYNHM-UHFFFAOYSA-N 2-tert-Butylphenol Chemical compound CC(C)(C)C1=CC=CC=C1O WJQOZHYUIDYNHM-UHFFFAOYSA-N 0.000 description 1
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 1
- 241000790917 Dioxys <bee> Species 0.000 description 1
- GYCMBHHDWRMZGG-UHFFFAOYSA-N Methylacrylonitrile Chemical compound CC(=C)C#N GYCMBHHDWRMZGG-UHFFFAOYSA-N 0.000 description 1
- 229920002367 Polyisobutene Polymers 0.000 description 1
- 229910003978 SiClx Inorganic materials 0.000 description 1
- 150000001335 aliphatic alkanes Chemical class 0.000 description 1
- 239000003963 antioxidant agent Substances 0.000 description 1
- 230000003078 antioxidant effect Effects 0.000 description 1
- 229920005549 butyl rubber Polymers 0.000 description 1
- 239000006227 byproduct Substances 0.000 description 1
- 238000006555 catalytic reaction Methods 0.000 description 1
- 229910052802 copper Inorganic materials 0.000 description 1
- 239000010949 copper Substances 0.000 description 1
- 238000005336 cracking Methods 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- AQEFLFZSWDEAIP-UHFFFAOYSA-N di-tert-butyl ether Chemical compound CC(C)(C)OC(C)(C)C AQEFLFZSWDEAIP-UHFFFAOYSA-N 0.000 description 1
- 239000012530 fluid Substances 0.000 description 1
- 239000000446 fuel Substances 0.000 description 1
- 239000003317 industrial substance Substances 0.000 description 1
- 125000000959 isobutyl group Chemical group [H]C([H])([H])C([H])(C([H])([H])[H])C([H])([H])* 0.000 description 1
- 239000002086 nanomaterial Substances 0.000 description 1
- 239000002105 nanoparticle Substances 0.000 description 1
- 238000004230 steam cracking Methods 0.000 description 1
- 239000002699 waste material Substances 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
- B01J23/38—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of noble metals
- B01J23/40—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of noble metals of the platinum group metals
- B01J23/42—Platinum
-
- B01J35/39—
-
- 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
- B01J37/00—Processes, in general, for preparing catalysts; Processes, in general, for activation of catalysts
- B01J37/34—Irradiation by, or application of, electric, magnetic or wave energy, e.g. ultrasonic waves ; Ionic sputtering; Flame or plasma spraying; Particle radiation
- B01J37/341—Irradiation by, or application of, electric, magnetic or wave energy, e.g. ultrasonic waves ; Ionic sputtering; Flame or plasma spraying; Particle radiation making use of electric or magnetic fields, wave energy or particle radiation
- B01J37/343—Irradiation by, or application of, electric, magnetic or wave energy, e.g. ultrasonic waves ; Ionic sputtering; Flame or plasma spraying; Particle radiation making use of electric or magnetic fields, wave energy or particle radiation of ultrasonic wave energy
Abstract
The invention discloses a kind of preparation methods of silicon dioxide carried platinum composite catalyzing material, it include: that (1) prepares silica suspension: using ethyl orthosilicate as raw material, dehydrated alcohol is added, stir 20~40min, add ammonium hydroxide, continue 1~2h of stirring, obtains silica suspension;(2) ethylene glycol is added into above-mentioned silica suspension, it stirs evenly, add 1.5~2g/L platinum acid chloride solution, 2~3h of ultrasonic disperse, 3~5h is condensed back under 120 DEG C of inert atmospheres, wherein, the ratio of the silica suspension and the ethylene glycol are as follows: contain 0.5~1.5mg silica suspension in every 1mL ethylene glycol;(3) products therefrom in step (2) is filtered by vacuum, dehydrated alcohol and deionized water washing is respectively adopted in solid product, in 80 DEG C of 10~15h of vacuum drying, obtains silicon dioxide carried platinum composite catalyzing material.In silicon dioxide carried platinum composite catalyzing material in the present invention, platinum particles can be loaded relatively evenly on silica, therefore have stronger photocatalytic activity.
Description
Technical field
The present invention relates to catalysis material technical fields, more particularly to a kind of silicon dioxide carried platinum composite catalyzing material
Preparation method.
Background technique
Isobutene is very important industrial chemicals, mainly for the preparation of butyl rubber, polyisobutene, methacrylonitrile,
Antioxidant, tertiary butyl phenol, tertbutyl ether etc..It is corresponding as the demand to isobutene downstream product increasingly increases, to isobutene
Demand be consequently increased.However isobutene does not have natural origin, mainly from naphtha steam cracking device and fluid catalytic
The by-product of cracking unit.Original isobutene production method is no longer satisfied chemical industry to the needs of isobutene, accelerates
The production method for studying isobutene is current urgent problem to be solved.
Contain a large amount of iso-butane in C 4 fraction, utilization rate is low, is largely used as domestic fuel burn-up, causes greatly
Waste.Preparing isobutene through dehydrogenation of iso-butane has wide Research Prospects, is the Main way in current research.By by isobutyl
The utilization rate that iso-butane not only can be improved in the chemical products that isobutene is made in alkane dehydrogenation and then production is more worth can also generate warp
Ji benefit.It is in the prior art, although platinum group catalyst excellent catalytic effect used in dehydrogenation of isobutane technique, environmental-friendly,
Platinum is expensive, and catalyst is easily assembled, to influence catalytic effect.
For this reason, it is necessary in view of the above-mentioned problems, propose a kind of preparation method of silicon dioxide carried platinum 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 silicon dioxide carried platinum composite catalyzing material, existing to overcome
There is the deficiency in technology.
To achieve the above object, the invention provides the following technical scheme:
A kind of preparation method of silicon dioxide carried platinum composite catalyzing material, comprising:
(1) it prepares silica suspension: using ethyl orthosilicate as raw material, dehydrated alcohol is added, stirs 20~40min,
Ammonium hydroxide is added, continues 1~2h of stirring, obtains silica suspension;
(2) ethylene glycol is added into above-mentioned silica suspension, stirs evenly, it is molten to add 1.5~2g/L chloroplatinic acid
Liquid, 2~3h of ultrasonic disperse, under 120 DEG C of inert atmospheres be condensed back 3~5h, wherein the silica suspension with it is described
The ratio of ethylene glycol are as follows: contain 0.5~1.5mg silica suspension in every 1mL ethylene glycol;
(3) products therefrom in step (2) is filtered by vacuum, dehydrated alcohol and deionized water is respectively adopted in solid product
Washing, in 80 DEG C of 10~15h of vacuum drying, obtains silicon dioxide carried platinum composite catalyzing material.
Preferably, in step (1), the ethyl orthosilicate, the dehydrated alcohol, the ammonium hydroxide weight ratio be 1:10~
15:10~20.
Preferably, the ethyl orthosilicate, the dehydrated alcohol, the ammonium hydroxide weight ratio be 1:12:15.
Preferably, in step (2), the concentration of the platinum acid chloride solution is 1.8g/L.
Preferably, in step (2), the ratio of the silica suspension and the ethylene glycol are as follows: in every 1mL ethylene glycol
Contain 1mg silica suspension.
Preferably, in step (2), the inert atmosphere is nitrogen atmosphere.
Preferably, in step (2), the power of ultrasonic disperse process is 800~1000W.
Preferably, in obtained silicon dioxide carried platinum composite catalyzing material, the mass fraction of the platinum is 10~
30%.
Compared with the prior art, the advantages of the present invention are as follows: the silicon dioxide carried platinum composite catalyzing material in the present invention
In, platinum particles can be loaded relatively evenly on silica, therefore have stronger photocatalytic activity.
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 silicon dioxide carried platinum composite catalyzing material, comprising:
(1) it prepares silica suspension: using ethyl orthosilicate as raw material, dehydrated alcohol is added, stirs 20~40min,
Ammonium hydroxide is added, continues 1~2h of stirring, obtains silica suspension;
(2) ethylene glycol is added into above-mentioned silica suspension, stirs evenly, it is molten to add 1.5~2g/L chloroplatinic acid
Liquid, 2~3h of ultrasonic disperse, under 120 DEG C of inert atmospheres be condensed back 3~5h, wherein the silica suspension with it is described
The ratio of ethylene glycol are as follows: contain 0.5~1.5mg silica suspension in every 1mL ethylene glycol;
(3) products therefrom in step (2) is filtered by vacuum, dehydrated alcohol and deionized water is respectively adopted in solid product
Washing, in 80 DEG C of 10~15h of vacuum drying, obtains silicon dioxide carried platinum composite catalyzing material.
In above-mentioned steps (1), the ethyl orthosilicate, the dehydrated alcohol, the ammonium hydroxide weight ratio be 1:10~15:
10~20, it is preferred that the ethyl orthosilicate, the dehydrated alcohol, the ammonium hydroxide weight ratio be 1:12:15.
In above-mentioned steps (2), the inert atmosphere is nitrogen atmosphere;In step (2), the power of ultrasonic disperse process is
800~1000W.
In the silicon dioxide carried platinum composite catalyzing material according to obtained by the above method, the mass fraction of the platinum is 10
~30%, it is preferred that the mass fraction of the platinum is 20%.
The preparation method of silicon dioxide carried platinum composite catalyzing material is illustrated with specific embodiment below.
Embodiment 1
(1) silica suspension is prepared: using ethyl orthosilicate as raw material, addition dehydrated alcohol, stirring 20min, then plus
Enter ammonium hydroxide, continues to stir 1h, obtain silica suspension, wherein the ethyl orthosilicate, the dehydrated alcohol, the ammonia
The weight ratio of water is 1:10:10;
(2) ethylene glycol is added into above-mentioned silica suspension, stirs evenly, add 1.5g/L platinum acid chloride solution,
The ultrasonic disperse 2h under the power of 800W, is condensed back 3h under 120 DEG C of nitrogen atmospheres, wherein the silica suspension
With the ratio of the ethylene glycol are as follows: contain 0.5mg silica suspension in every 1mL ethylene glycol;
(3) products therefrom in step (2) is filtered by vacuum, dehydrated alcohol and deionization washing is respectively adopted in solid product
It washs, in 80 DEG C of vacuum drying 10h, obtains silicon dioxide carried platinum composite catalyzing material.
In the silicon dioxide carried platinum composite catalyzing material according to obtained by the method for above-described embodiment, the quality of the platinum
Score is 10%.
Embodiment 2
(1) silica suspension is prepared: using ethyl orthosilicate as raw material, addition dehydrated alcohol, stirring 30min, then plus
Enter ammonium hydroxide, continue to stir 1.5h, obtain silica suspension, wherein is the ethyl orthosilicate, the dehydrated alcohol, described
The weight ratio of ammonium hydroxide is 1:12:15;
(2) ethylene glycol is added into above-mentioned silica suspension, stirs evenly, add 1.8g/L platinum acid chloride solution,
The ultrasonic disperse 2.5h under the power of 900W, is condensed back 4h under 120 DEG C of nitrogen atmospheres, wherein the silica suspends
The ratio of liquid and the ethylene glycol are as follows: contain 1mg silica suspension in every 1mL ethylene glycol;
(3) products therefrom in step (2) is filtered by vacuum, dehydrated alcohol and deionization washing is respectively adopted in solid product
It washs, in 80 DEG C of vacuum drying 12h, obtains silicon dioxide carried platinum composite catalyzing material.
In the silicon dioxide carried platinum composite catalyzing material according to obtained by the method for above-described embodiment, the quality of the platinum
Score is 20%.
Embodiment 3
(1) silica suspension is prepared: using ethyl orthosilicate as raw material, addition dehydrated alcohol, stirring 40min, then plus
Enter ammonium hydroxide, continues to stir 2h, obtain silica suspension, wherein the ethyl orthosilicate, the dehydrated alcohol, the ammonia
The weight ratio of water is 1:15:20;
(2) ethylene glycol is added into above-mentioned silica suspension, stirs evenly, add 2g/L platinum acid chloride solution,
Ultrasonic disperse 3h under the power of 1000W, is condensed back 5h under 120 DEG C of nitrogen atmospheres, wherein the silica suspension with
The ratio of the ethylene glycol are as follows: contain 1.5mg silica suspension in every 1mL ethylene glycol;
(3) products therefrom in step (2) is filtered by vacuum, dehydrated alcohol and deionization washing is respectively adopted in solid product
It washs, in 80 DEG C of vacuum drying 15h, obtains silicon dioxide carried platinum composite catalyzing material.
In the silicon dioxide carried platinum composite catalyzing material according to obtained by the method for above-described embodiment, the quality of the platinum
Score is 30%.
Electron-microscope scanning is carried out to silicon dioxide carried platinum composite catalyzing material obtained in above-described embodiment 1~3 to test
Know, the nano material uniform particle diameter, copper particle can be relatively evenly distributed on stannic oxide;Wherein, when obtained dioxy
The mass fraction of platinum is 20% in SiClx Supported Pt Nanoparticles composite catalyzing material, and catalytic efficiency is maximum, can reach 86.2%, therefore have
There is stronger catalytic 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 (8)
1. a kind of preparation method of silicon dioxide carried platinum composite catalyzing material characterized by comprising
(1) silica suspension is prepared: using ethyl orthosilicate as raw material, addition dehydrated alcohol, 20~40min of stirring, then plus
Enter ammonium hydroxide, continues 1~2h of stirring, obtain silica suspension;
(2) ethylene glycol is added into above-mentioned silica suspension, stirs evenly, add 1.5~2g/L platinum acid chloride solution, surpass
Sound disperses 2~3h, and 3~5h is condensed back under 120 DEG C of inert atmospheres, wherein the silica suspension and the second two
The ratio of alcohol are as follows: contain 0.5~1.5mg silica suspension in every 1mL ethylene glycol;
(3) products therefrom in step (2) is filtered by vacuum, dehydrated alcohol and deionization washing is respectively adopted in solid product
It washs, in 80 DEG C of 10~15h of vacuum drying, obtains silicon dioxide carried platinum composite catalyzing material.
2. the preparation method of silicon dioxide carried platinum composite catalyzing material according to claim 1, which is characterized in that step
(1) in, the ethyl orthosilicate, the dehydrated alcohol, the ammonium hydroxide weight ratio be 1:10~15:10~20.
3. the preparation method of silicon dioxide carried platinum composite catalyzing material according to claim 2, which is characterized in that described
Ethyl orthosilicate, the dehydrated alcohol, the ammonium hydroxide weight ratio be 1:12:15.
4. the preparation method of silicon dioxide carried platinum composite catalyzing material according to claim 1, which is characterized in that step
(2) in, the concentration of the platinum acid chloride solution is 1.8g/L.
5. the preparation method of silicon dioxide carried platinum composite catalyzing material according to claim 1, which is characterized in that step
(2) in, the ratio of the silica suspension and the ethylene glycol are as follows: suspend in every 1mL ethylene glycol containing 1mg silica
Liquid.
6. the preparation method of silicon dioxide carried platinum composite catalyzing material according to claim 1, which is characterized in that step
(2) in, the inert atmosphere is nitrogen atmosphere.
7. the preparation method of silicon dioxide carried platinum composite catalyzing material according to claim 1, which is characterized in that step
(2) in, the power of ultrasonic disperse process is 800~1000W.
8. the preparation method of silicon dioxide carried platinum composite catalyzing material according to claim 1, which is characterized in that made
In the silicon dioxide carried platinum composite catalyzing material obtained, the mass fraction of the platinum is 10~30%.
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CN102380376A (en) * | 2010-08-30 | 2012-03-21 | 中国中化股份有限公司 | Method for loading noble metal on silicon oxide, aluminum oxide or titanium oxide |
CN103350226A (en) * | 2013-07-16 | 2013-10-16 | 合肥工业大学 | SiO2/Ag composite micron sphere and preparation method thereof |
CN106955701A (en) * | 2017-03-01 | 2017-07-18 | 西安交通大学 | One kind SiO containing aluminium2Load high dispersive Pt catalyst and its preparation method and application |
CN108067249A (en) * | 2017-03-29 | 2018-05-25 | 天津大学 | A kind of high dispersive is in platinum based catalyst of carrier silicas and its preparation method and application |
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2018
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Patent Citations (6)
Publication number | Priority date | Publication date | Assignee | Title |
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KR100636424B1 (en) * | 2004-06-14 | 2006-10-19 | 한국화학연구원 | The preparation method of an adsorbent and the purification method of gases using the same |
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CN102019431A (en) * | 2010-09-30 | 2011-04-20 | 大连理工大学 | Metallic nano cluster/silicon dioxide hollow nuclear shell structured nanoparticles and preparation method thereof |
CN103350226A (en) * | 2013-07-16 | 2013-10-16 | 合肥工业大学 | SiO2/Ag composite micron sphere and preparation method thereof |
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