CN106334587A - Method for preparing supported metal catalyst through cold plasma-alcohol synergetic reduction under atmospheric pressure - Google Patents
Method for preparing supported metal catalyst through cold plasma-alcohol synergetic reduction under atmospheric pressure Download PDFInfo
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- 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
- B01J37/02—Impregnation, coating or precipitation
- B01J37/0201—Impregnation
- B01J37/0205—Impregnation in several steps
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- 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
- B01J23/44—Palladium
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- B01J23/00—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
- B01J23/70—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper
- B01J23/72—Copper
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- B01J37/00—Processes, in general, for preparing catalysts; Processes, in general, for activation of catalysts
- B01J37/16—Reducing
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- 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
- B01J37/349—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 flames, plasmas or lasers
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Abstract
The invention provides a method for preparing a supported metal catalyst through cold plasma-alcohol synergetic reduction under an atmospheric pressure. The method comprises the steps that an atmospheric pressure cold plasma is adopted, inert gas is used as working gas and carries alcohol steam, and a metal precursor obtained by adopting an impregnation method and supported on a carrier is reduced to prepare the supported metal catalyst. A plasma preparation method belongs to a dry preparation method, and the shortcoming that later-period drying of a wet-method process exists and metal nanoparticles can become large can be effectively avoided. In addition, the method does not need dangerous hydrogen, metal ion reduction is performed by utilizing the synergistic effect of the atmospheric pressure cold plasma and alcohol low in price and easy to obtain, and the method is a novel simple, rapid, safe and environmentally friendly supported metal catalyst preparation process. The preparation process can effectively solve the problem that the metal ion reduction cannot be achieved when inert gas discharge cold plasma electron energy is lower under the atmospheric pressure.
Description
Technical field
The invention belongs to load type metal catalyst preparation field is and in particular to a kind of air of load type metal catalyst
Pressure cold plasma preparation method.
Background technology
Load type metal catalyst has a wide range of applications in chemical and field of Environment Protection.Its preparation method mainly includes
The methods such as dipping-thermal reduction, electronation and photo-reduction.Dipping-thermal reduction method operating process simple it is adaptable to scale metaplasia
Produce, be widely used to the preparation of load type metal catalyst.But it typically requires and reduces for a long time in hydrogen, and this is easy
Metal particle diameter is caused to become big, dispersiveness is deteriorated, thus causing its activity not high.Chemical reduction method typically requires using excessive boron
The poisonous and hazardous chemical reagent such as sodium hydride, formaldehyde and hydrazine although can obtain that particle diameter is little, good dispersion metal nanoparticle,
Obtain high performance load type metal catalyst.But its environment is unfriendly, is therefore restricted in actual applications.Photoreduction met hod
It is a kind of gentle high-performance supported metal method for preparing catalyst, but it needs high intensity, long illumination, energy consumption is relatively
High.Additionally, electronation and photoreduction met hod, carry out all in liquid environment, later stage drying and other steps easily cause metallic nanoparticle
Seed footpath becomes big, and activity is deteriorated.
4th state of plasma, also referred to as material, is generally produced by gas discharge, is to reach certain degree of ionization, by electricity
The approximately equalised electronics of lotus (sometimes also including the ion of electronegativity) and cation, and the ground state of neutrality and excited atom and
Molecular composition.Cold plasma is a kind of important plasma, and it has high electron energy and low gas temperature, cold etc.
Ion method is a kind of effective ways preparing load type metal catalyst.Patent application cn200410093820.6 adopts low temperature etc.
Gas ions, with inert gas, air or oxygen as working gas, using electron reduction characteristic, prepare load type metal catalyst.
Inventor points out that this process can be carried out between 50pa～0.1mpa, and reducible metal active constituent is " h2ptcl6、
pdcl2、ni(no3)2、au(no3)2、cu(no3)2、ag(no3)2、fe(no3)3、co(no3)2、zn(no3)3、k2cro3Or ammonium molybdate
One or more ".Using atmosphere cold plasma, with inert gas as working gas, using high energy electron reducing metal
Ion, truly feasible in principle.But because under atmospheric pressure, gas density is big, collision increases, and electron energy is relatively low, therefore not yet
Adopt atmosphere cold plasma, with inert gas as working gas, prepare load type metal catalyst using electron reduction
Report.This patent Example is also under low pressure, cold plasma reduction preparation pt/tio2.Additionally, liu et al.
(changjun liu,minyue li,jiaqi wang,xintong zhou,qiuting guo,jinmao yan,
Yingzhi li.chinese journal ofcatalysis 37 (2016) 340-348.) point out that electronics can only reduce and has
The metal ion of positive electrode potential, and for having the metal ion of negative electrode potential, such as ni2+/ni(eθ=-0.257v), fe3 +/fe(eθ=-0.037v), co2+/co(eθ=-0.28v), zn2+/zn(eθ=-0.7618v), then cannot reduce.
In order to solve the problems, such as under atmospheric pressure electron energy relatively low it is impossible to reducing metal ion, researchers have done in a large number
Correlative study.Patent application cn200910304664.6 adopts low temperature plasma, with hydrogen as working gas, under atmospheric pressure
Reducing metal ion, prepares catalyst carrier and metal active constituent simultaneously, obtains load type metal catalyst.This invention is implemented
The bright the method for illustration is reducible to prepare support type ni catalyst.Additionally, other relevant reports also confirm that using cold containing hydrogen
Plasma is reducible to prepare loaded noble metal catalyst, and the non-precious metal catalyst such as support type ni and co.These grind
Study carefully and show, hydrogeneous cold plasma is strictly a kind of effective ways of reducing metal ion under atmospheric pressure, can obtain high performance
Load type metal catalyst.But these processes are required for using hydrogen although hydrogen is a kind of clear energy sources, but it is inflammable easily
Quick-fried, there is potential safety hazard.
The present invention adopts atmosphere cold plasma, with inert gas as working gas, and carries alcohol steam using it,
Under atmosphere cold plasma -ol synergy, the multiple hydrogeneous active specy that produced in cold plasma using alcohol, to leaching
Stain method obtains the metal precursor being carried on carrier and is reduced, and prepares load type metal catalyst.The method can simply, soon
Speed, safety, environmentally friendly prepare load type metal catalyst.
Content of the invention
For overcoming existing atmosphere cold plasma, it is used hydrogen dangerous as working gas, and with inert gas is
Working gas, electron energy relatively low it is impossible to the shortcoming of reducing metal ion with not enough, the primary and foremost purpose of the present invention is to provide one
Plant the load type metal catalyst preparation method simple, quick, security context is friendly.
The technical solution adopted in the present invention is as follows: adopts atmosphere cold plasma, with inert gas as working gas
And carry alcohol steam, under atmosphere cold plasma -ol synergy, produce multiple hydrogeneous active species, infusion process is obtained
The metal precursor must being carried on carrier is reduced, and obtains load type metal catalyst.
The concretely comprising the following steps of the method:
(1) weigh appropriate metal precursor in beaker, add a certain amount of deionized water, be configured to certain density metal
Precursor salt solution；
(2) adopt infusion process, a certain amount of carrier is put into metal precursor salting liquid, standing, it is dried, obtain and be carried on load
Metal precursor on body；
(3) metal precursor being carried on carrier is put in plasma reactor, with inert gas as work gas
Body, carries alcohol steam and enters plasma reactor.Produce cold plasma under atmospheric pressure, work in coordination with plasma -ol and make
With under, the metal precursor being carried on carrier is reduced, obtain load type metal catalyst.
Wherein, described metal precursor is monometallic component, bimetallic component or many metal components；
In described alcohol steam, alcohol is one or more of methyl alcohol, ethanol, propyl alcohol and ethylene glycol；
Described working gas is one of argon gas, nitrogen, helium or its mixed gas；
Described cold plasma discharge gas temperature is less than 90 DEG C, no extra heating.
Further, described carrier is titanium dioxide, silica, aluminum oxide, molecular sieve, metallic organic framework material
One of material, Graphene, activated carbon, NACF, iron oxide or cerium oxide.
Further, described atmosphere cold plasma is atmospheric dielectric barrier discharge cold plasma, atmospheric pressure
One of radio-frequency glow discharge plasmas, Atomospheric pressure glow discharge cold plasma, atmospheric pressure direct-current discharge cold plasma.
Further, described atmosphere cold plasma electron energy is not enough to be reduced directly the metal ion of load.
Further, described metal precursor salt is palladium bichloride, palladium nitrate, chloroplatinic acid, gold chloride, silver nitrate, nitric acid
One or more of copper, copper chloride, nickel nitrate or cobalt nitrate.Preferably palladium nitrate and copper nitrate.
Further, described cold plasma discharge voltage is 0.1kv～40kv.
Further, described cold plasma process time is 2-30 minute.
Further, the mass fraction of the metal precursor being carried on carrier is 0.01%-60%.
Compared with prior art, the method have the advantages that:
The present invention provides a kind of simple, quick, safety, eco-friendly load type metal catalyst novel preparation method.Should
Method effectively overcome noble gas discharge cold plasma electron energy under atmospheric pressure in existing method relatively low it is impossible to reduction gold
Belong to shortcoming and the deficiency of ion, the invention belongs to dry-forming method, the drying of wet processing later stage can be prevented effectively from, so that metal is received
The problems such as rice corpuscles becomes big.The present invention, under atmosphere cold plasma -ol synergy, is produced in cold plasma using alcohol
Raw multiple hydrogeneous active specy, obtains, to infusion process, the metal precursor being carried on carrier and reduces, and without using
There is the hydrogen of potential safety hazard, you can prepare load type metal catalyst.
Brief description
The loaded catalyst pd/tio that Fig. 1 is prepared for distinct methods2Photo；Wherein (a) is before processing 2wt%pd/tio2
Sample；B () is to adopt atmosphere cold plasma, with argon gas as working gas, do not carry alcohol vapour preparation 2wt%pd/
tio2Sample；C () is to adopt atmosphere cold plasma, with argon gas as working gas, carry alcohol vapour, prepare 2wt%pd/
tio2Sample；D () is not adopt cold plasma, directly carry alcohol vapour with argon gas, processes 9min and obtain at 80 DEG C
2wt%pd/tio2The photo of sample.
The 2wt%pd/tio that Fig. 2 is prepared for distinct methods2Sample xrd spectrogram；Wherein, (a) adopts atmosphere cold plasma
Body, with argon gas as working gas, does not carry alcohol vapour (b) and carries alcohol vapour, prepare 2wt%pd/tio respectively2Sample
Xrd spectrogram, (c) carries alcohol vapour using argon gas, processes 9min and obtain 2wt%pd/tio at 80 DEG C2The xrd spectrum of sample
Figure.
The loaded catalyst cu/tio that Fig. 3 is prepared for distinct methods2Photo；Wherein, (a) 2wt%cu/tio2At sample
Before reason, and adopt atmosphere cold plasma, with argon gas as working gas, (b) does not carry alcohol vapour or (c) carries ethanol
Steam, prepares 2wt%cu/tio respectively2The photo of sample.
Fig. 4 is to adopt atmosphere cold plasma, with argon gas as working gas, does not carry alcohol vapour or carries ethanol steaming
Vapour, prepares 2wt%cu/tio respectively2The xrd spectrogram of sample.
Specific embodiment
With reference to specific embodiment, technical scheme is further described, but the present invention is not with any shape
Formula is limited to embodiment content.Test method described in embodiment if no special instructions, is conventional method；As no special theory
Bright, described reagent and biomaterial, all commercially obtain.
Embodiment 1
With palladium nitrate as presoma, 2wt%pd/tio is prepared using infusion process2Presoma, standing, be dried.
Put into above-mentioned presoma 0.3g in dielectric barrier discharge reactor, be passed through argon gas (100ml
min-1), regulation discharge frequency is 15khz, and simple alternating current discharge voltage peak-to-peak value is 10kv, and discharging gap is 2mm, in air
Under the conditions of pressure, to 2wt%pd/tio2Presoma processed, each process time be 3min, middle interval 8min, coexistence
Reason 3 times, obtains 2wt%pd/tio2Sample.Cold plasma discharge gas temperature is less than 80 DEG C, no extra heating.
Fig. 1 and Fig. 2 be shown in respectively by the photo of embodiment 1 sample and x-ray diffraction collection of illustrative plates.
The photo of embodiment illustrated in fig. 11 sample shows: produces plasma with argon gas for working gas, does not carry alcohol and steam
In the case of vapour, to 2wt%pd/tio2Presoma processed, color sample is not changed in, and this tentatively illustrates that pd ion does not have
It is reduced；
The X-ray diffraction pattern spectrum of embodiment illustrated in fig. 21 sample shows: produces plasma with argon gas for working gas, no
In the case of carrying alcohol steam, to 2wt%pd/tio2Presoma processed, do not have pd metal simple-substance produce.
Embodiment 2
Substantially the same manner as Example 1, argon gas carries the ethanol being placed under normal temperature in the way of bubbling, to 2wt%pd/tio2
Presoma processed, each process time be 3min, middle interval 8min, coprocessing 3 times, obtain 2wt%pd/tio2Sample
Product.Cold plasma discharge gas temperature is less than 80 DEG C, no extra heating.
Fig. 1 and Fig. 2 be shown in respectively by the photo of embodiment 2 sample and x-ray diffraction collection of illustrative plates.
The photo of embodiment illustrated in fig. 12 sample shows: produces plasma with argon gas for working gas, carries ethanol and steam
In the case of vapour, to 2wt%pd/tio2Presoma processed, color sample occur significant change, this tentatively illustrate pd from
Son is reduced；
The X-ray diffraction pattern spectrum of embodiment illustrated in fig. 22 sample shows: produces plasma with argon gas for working gas, takes
In the case of taking alcohol steam, to 2wt%pd/tio2Presoma processed, have obvious pd metal simple-substance to produce.This says
Bright atmosphere cold plasma -ol synergy, can effectively overcome existing atmosphere cold plasma, with inert gas for work
Gas, electron energy relatively low it is impossible to the shortcoming of reducing metal ion.
Embodiment 3
It is, do not apply cold plasma, argon gas carries the second being placed under normal temperature in the way of bubbling with embodiment 2 difference
Alcohol steam, under the conditions of 80 DEG C, to 2wt%pd/tio2Presoma processed, coprocessing time 9min, obtain 2wt%
pd/tio2Sample.
Fig. 1 and Fig. 2 be shown in respectively by the photo of embodiment 3 sample and x-ray diffraction collection of illustrative plates.
The photo of embodiment illustrated in fig. 13 sample shows: carries alcohol vapour with argon gas, under the conditions of 80 DEG C, to 2wt%
pd/tio2Presoma processed, color sample is unchanged, and this preliminary explanation only can not reduce pd ion using alcohol steam；
The X-ray diffraction pattern spectrum of embodiment illustrated in fig. 23 sample shows: carries alcohol vapour with argon gas, in 80 DEG C of conditions
Under, to 2wt%pd/tio2Presoma processed, do not have metal pd simple substance produce.
Embodiment 4
With copper nitrate as presoma, 2wt%cu/tio is prepared using infusion process2Presoma, standing, be dried.
Put into above-mentioned presoma 0.3g in dielectric barrier discharge reactor, be passed through argon gas (100ml
min-1), regulation discharge frequency is 15khz, and simple alternating current discharge voltage peak-to-peak value is 10kv, and discharging gap is 2mm, in air
Under the conditions of pressure, to 2wt%pd/tio2Presoma processed, each process time be 3min, middle interval 8min, coexistence
Reason 3 times, obtains 2wt%pd/tio2Sample.Cold plasma discharge gas temperature is less than 80 DEG C, no extra heating.
Fig. 3 and Fig. 4 be shown in respectively by the photo of embodiment 4 sample and x-ray diffraction collection of illustrative plates.
The photo of embodiment illustrated in fig. 44 sample shows: produces plasma with argon gas for working gas, does not carry alcohol and steam
In the case of vapour, to 2wt%cu/tio2Presoma processed, color sample is not changed in, and this tentatively illustrates that cu ion does not have
It is reduced；
The X-ray diffraction pattern spectrum of embodiment illustrated in fig. 44 sample shows: produces plasma with argon gas for working gas, no
In the case of carrying alcohol steam, to 2wt%cu/tio2Presoma processed, do not have cu metal simple-substance produce.
Embodiment 5
Substantially the same manner as Example 4, argon gas carries the ethanol being placed under normal temperature in the way of bubbling, to 2wt%cu/tio2
Presoma processed, each process time be 3min, middle interval 8min, coprocessing 3 times, obtain 2wt%cu/tio2Sample
Product.Cold plasma discharge gas temperature is less than 80 DEG C, no extra heating.
Fig. 3 and Fig. 4 be shown in respectively by the photo of embodiment 5 sample and x-ray diffraction collection of illustrative plates.
The photo of embodiment illustrated in fig. 35 sample shows: produces plasma with argon gas for working gas, carries ethanol and steam
In the case of vapour, to 2wt%cu/tio2Presoma processed, color sample occur significant change, this tentatively illustrate cu from
Son is reduced；
The X-ray diffraction pattern spectrum of embodiment illustrated in fig. 45 sample shows: produces plasma with argon gas for working gas, takes
In the case of taking alcohol steam, to 2wt%cu/tio2Presoma processed, have obvious cu metal simple-substance to produce.This enters
One step explanation atmosphere cold plasma -ol synergy, can effectively overcome existing atmosphere cold plasma, with inert gas
For working gas, electron energy relatively low it is impossible to the shortcoming of reducing metal ion.
Claims (9)
1. under a kind of atmospheric pressure cold plasma -ol collaborative SCM prepare load type metal catalyst method it is characterised in that
Using atmosphere cold plasma, with inert gas as working gas and carry alcohol steam, infusion process is obtained and is carried on carrier
On metal precursor carry out reduction and prepare load type metal catalyst.
2. under a kind of atmospheric pressure according to claim 1, cold plasma -ol collaborative SCM prepares load type metal catalysis
The method of agent is it is characterised in that the method concretely comprises the following steps:
(1) weigh appropriate metal precursor in beaker, add deionized water, be configured to metal precursor salting liquid；
(2) adopt infusion process, carrier is put into metal precursor salting liquid, standing, it is dried, obtain the metal being carried on carrier
Presoma；
(3) metal precursor being carried on carrier is put in plasma reactor, with inert gas as working gas, take
Band alcohol steam enters plasma reactor, produces cold plasma under atmospheric pressure, under plasma -ol synergy,
The metal precursor being carried on carrier is reduced, obtains load type metal catalyst；
Described metal precursor is monometallic component, bimetallic component or many metal components；
In described alcohol steam, alcohol is one or more of methyl alcohol, ethanol, propyl alcohol and ethylene glycol；
Described working gas is one of argon gas, nitrogen, helium or its mixed gas；
Described cold plasma discharge gas temperature is less than 90 DEG C, no extra heating.
3. under a kind of atmospheric pressure according to claim 1, cold plasma -ol collaborative SCM prepares load type metal catalysis
The method of agent is it is characterised in that described carrier is titanium dioxide, silica, aluminum oxide, molecular sieve, metallic organic framework material
A kind of in material, Graphene, activated carbon, NACF, iron oxide or cerium oxide.
4. under a kind of atmospheric pressure according to claim 1, cold plasma -ol collaborative SCM prepares load type metal catalysis
The method of agent is it is characterised in that described atmosphere cold plasma is atmospheric dielectric barrier discharge cold plasma, atmospheric pressure
One of radio-frequency glow discharge plasmas, Atomospheric pressure glow discharge cold plasma, atmospheric pressure direct-current discharge cold plasma.
5. under a kind of atmospheric pressure according to claim 1, cold plasma -ol collaborative SCM prepares load type metal catalysis
The method of agent it is characterised in that the atmosphere cold plasma electron energy that adopts be not enough to be reduced directly the metal of load from
Son.
6. under a kind of atmospheric pressure according to claim 1, cold plasma -ol collaborative SCM prepares load type metal catalysis
The method of agent is it is characterised in that described metal precursor is palladium bichloride, palladium nitrate, chloroplatinic acid, gold chloride, silver nitrate, nitric acid
One or more of copper, copper chloride, nickel nitrate or cobalt nitrate.
7. under a kind of atmospheric pressure according to claim 1, cold plasma -ol collaborative SCM prepares load type metal catalysis
The method of agent is it is characterised in that described cold plasma discharge voltage is 0.1kv～40kv.
8. under a kind of atmospheric pressure according to claim 1, cold plasma -ol collaborative SCM prepares load type metal catalysis
The method of agent is it is characterised in that described cold plasma process time is 2-30 minute.
9. under a kind of atmospheric pressure according to claim 1, cold plasma -ol collaborative SCM prepares load type metal catalysis
The method of agent is it is characterised in that the mass fraction being carried on the metal precursor on carrier is 0.01%-60%.
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| CN108855166A (en) * | 2018-06-20 | 2018-11-23 | 郑州轻工业学院 | A kind of loaded catalyst and preparation method thereof, application |
| CN109590028A (en) * | 2018-11-28 | 2019-04-09 | 浙江工商大学 | A method of nm-class catalyst is prepared using ultrasonic atomizatio plasma reaction |
| CN112691542A (en) * | 2020-12-31 | 2021-04-23 | 华南理工大学 | Metal composite molecular sieve material for adsorbing-catalytically oxidizing VOCs (volatile organic compounds), and preparation method and application thereof |
| CN113019329A (en) * | 2021-03-09 | 2021-06-25 | 湖南加法检测有限公司 | Method for modifying MOFs material by low-temperature plasma and application |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN108855166A (en) * | 2018-06-20 | 2018-11-23 | 郑州轻工业学院 | A kind of loaded catalyst and preparation method thereof, application |
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| CN109590028A (en) * | 2018-11-28 | 2019-04-09 | 浙江工商大学 | A method of nm-class catalyst is prepared using ultrasonic atomizatio plasma reaction |
| CN112691542A (en) * | 2020-12-31 | 2021-04-23 | 华南理工大学 | Metal composite molecular sieve material for adsorbing-catalytically oxidizing VOCs (volatile organic compounds), and preparation method and application thereof |
| CN113019329A (en) * | 2021-03-09 | 2021-06-25 | 湖南加法检测有限公司 | Method for modifying MOFs material by low-temperature plasma and application |
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