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 PDF

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Publication number
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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CN201810803363.7A
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Chinese (zh)
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赵云龙
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Zhangjiagang Dong Wei New Material Technology Development Co Ltd
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Zhangjiagang Dong Wei New Material Technology Development Co Ltd
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    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J23/00Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
    • B01J23/38Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of noble metals
    • B01J23/40Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of noble metals of the platinum group metals
    • B01J23/42Platinum
    • B01J35/39
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J37/00Processes, in general, for preparing catalysts; Processes, in general, for activation of catalysts
    • B01J37/34Irradiation by, or application of, electric, magnetic or wave energy, e.g. ultrasonic waves ; Ionic sputtering; Flame or plasma spraying; Particle radiation
    • B01J37/341Irradiation 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
    • B01J37/343Irradiation 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

A kind of preparation method of silicon dioxide carried platinum composite catalyzing material
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%.
CN201810803363.7A 2018-07-20 2018-07-20 A kind of preparation method of silicon dioxide carried platinum composite catalyzing material Withdrawn CN108940267A (en)

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Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
KR100636424B1 (en) * 2004-06-14 2006-10-19 한국화학연구원 The preparation method of an adsorbent and the purification method of gases using the same
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
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

Patent Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
KR100636424B1 (en) * 2004-06-14 2006-10-19 한국화학연구원 The preparation method of an adsorbent and the purification method of gases using the same
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
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
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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