CN104437553A - Microwave catalyst, preparation method and application thereof - Google Patents
Microwave catalyst, preparation method and application thereof Download PDFInfo
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- CN104437553A CN104437553A CN201410834862.4A CN201410834862A CN104437553A CN 104437553 A CN104437553 A CN 104437553A CN 201410834862 A CN201410834862 A CN 201410834862A CN 104437553 A CN104437553 A CN 104437553A
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/30—Hydrogen technology
- Y02E60/36—Hydrogen production from non-carbon containing sources, e.g. by water electrolysis
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Abstract
The invention provides a microwave catalyst which is a composite catalyst comprising an active component and an auxiliary catalytic component; the active component is nickel sulfide and/or cobalt sulfide; the auxiliary catalytic component is a perovskite type catalyst component; the microwave catalyst optionally contains carriers: the carriers contain one or more of Gamma-Al2O3, active carbon, ZSM-5 molecular sieve and ZSM-11 molecular sieve; the content of the active component in the composite catalyst is 10-60wt%, the content of the carriers is 0-60 wt% and the content of the catalytic component is 20-90 wt%. The invention further provides a preparation method and application of the microwave catalyst. The microwave catalyst provided by the invention is low in cost and simple in preparation method. The reaction condition of decomposing hydrogen sulfide to generate hydrogen and sulfur is mild and the decomposition efficiency is higher.
Description
Technical field
The present invention relates to the catalyst field of exhaust-gas treatment, be specifically related to a kind of microwave catalyst and its preparation method and application.
Background technology
Hydrogen sulfide is a kind of stench, severe toxicity and mordant sour gas, its generation not only can cause corrosion to oil, vapour conveyance conduit and other equipment, and being discharged into the pollution that also can cause environment in air, serious threat is to the health of human body and living space.
At present, mode mainly Crouse (Claus) technique of industrial process hydrogen sulfide, generates sulfur dioxide by hydrogen sulfide imperfect combustion, then the sulfur dioxide of generation and hydrogen sulfide is reacted generate sulphur and water.Sulphur in this process in hydrogen sulfide becomes sulphur and obtains recovery, but hydrogen wherein has then been oxidized to water, causes the serious waste of Hydrogen Energy.Therefore, the hydrogen energy source made full use of in the hydrogen sulfide produced in industrial production has great realistic meaning, such as, use hydrogen sulfide decomposing hydrogen-production method just can reach this object, but the research of its catalyst and catalysis process becomes the bottleneck that this area needs to break through.
The existing catalyst in order to decomposing hydrogen sulfide hydrogen manufacturing mainly exists that reaction condition is harsh, decomposition efficiency is low and the easy shortcoming such as poisoning and deactivation.Such as: Ma Guijun (catalysis journal, 2008,29 (4): 313-315) with the visible ray of characteristic wavelength λ > 420nm for light source, molar fraction of adulterating in ZnS is the Cu of 0.5%
2+time, the hydrogen-producing speed that its hydrogen sulfide decomposes is only up to 17 μm of ol/h.This reaction hydrogen sulfide decomposing hydrogen-production consuming time oversize, decomposition efficiency is not high, and the easy poisoning and deactivation of its photochemical catalyst used, not easily to reclaim again.Again such as, Zhang Yihua (East China University of Science's journal, 1995,21 (6): 738-742) utilizes FeS catalyst 300 DEG C to 600 DEG C decomposing hydrogen sulfide hydrogen manufacturing, the most high yield H of this reaction
2rate is only 10%.Although use the method reaction condition comparatively gentle, its catalytic activity is not high, and is subject to the impact of reactive chemistry balance, and therefore its decomposition efficiency is very low.Some researchers adopt membrane reactor to break the chemical balance in Catalytic Thermal Decomposition reaction, but the prerequisite of its application to develop more efficient catalyst and membrane material that is high temperature resistant, low cost.Some researchers use noble metal such as Ir etc. to support on common transient metal sulfide or oxide catalyst, the hydrogen-producing speed of reaction is significantly improved, but supporting noble metal makes the preparation cost of catalyst greatly improve on the one hand, another side also makes the preparation process of catalyst become complicated and loaded down with trivial details.
Therefore, this area also needs the catalyst for the hydrogen manufacturing of catalytic decomposition hydrogen sulfide developing a kind of catalytic effect excellence.
Summary of the invention
The object of the invention is to overcome the deficiencies in the prior art, the microwave catalyst that a kind of reaction condition is gentleer, decomposition efficiency is higher and with low cost is provided, for catalysed curing hydrogen decomposing hydrogen-production and sulphur.
Therefore, the invention provides a kind of microwave catalyst, described microwave catalyst is the composite catalyst comprising active component and co catalysis component, and described active component is nickel sulfide and/or cobalt sulfide, and described co catalysis component is perovskite type catalyst component; Also selectively comprise carrier in described microwave catalyst, described carrier is for being selected from γ-Al
2o
3, active carbon, ZSM-5 molecular sieve, one or more in ZSM-11 molecular sieve; And the content of active component is 10 ~ 60wt% in described composite catalyst, the content of carrier is 0 ~ 60wt%, and the content of co catalysis component is 20 ~ 90wt%.
Microwave catalyst provided by the invention is with low cost, and preparation method is simple.The while of using the reaction condition of its catalysed curing hydrogen decomposing hydrogen-production and sulphur gentleer, decomposition efficiency is higher.
In a kind of concrete embodiment, described perovskite type catalyst component is BaMn
0.2cu
0.8o
3.
Preferably, in described composite catalyst, the content of active component is 10 ~ 50wt%, and the content of carrier is 5 ~ 60wt%, and the content of co catalysis component is 30 ~ 70wt%.More preferably in described composite catalyst, the content of active component is 20 ~ 30wt%, and the content of carrier is 10 ~ 30wt%, and the content of co catalysis component is 40 ~ 60wt%.In addition, a certain amount of γ-Al is contained in preferred composite catalyst of the present invention
2o
3carrier.
The present invention is the corresponding preparation method providing a kind of catalyst described above also, comprises by active component, available carrier and co catalysis component through ground and mixed aftershaping, then filters out 20 ~ 80 object particles and prepare described composite catalyst.And the hydrogen sulfide decomposition hydrogen making of a kind of catalyst described above in the hydrogen sulfide containing gas of catalysis and the application in sulphur are provided.
The present invention is the corresponding a kind of method providing microwave catalysis decomposing hydrogen sulfide hydrogen and sulphur also, be included in filled composite catalyst in the reaction tube in microwave reactor and form catalytic bed, hydrogen sulfide containing gas by described catalytic bed generation gas-solid-phase catalytic reaction, thus realizes the decomposition of hydrogen sulfide; Described composite catalyst comprises active component, available carrier and co catalysis component, and described active component is nickel sulfide and/or cobalt sulfide, and described carrier is for being selected from γ-Al
2o
3, active carbon, ZSM-5 molecular sieve, one or more in ZSM-11 molecular sieve, described co catalysis component is perovskite type catalyst component; And the content of active component is 10 ~ 60wt% in described composite catalyst, the content of carrier is 0 ~ 60wt%, and the content of co catalysis component is 20 ~ 90wt%.
The present inventor finds, comparatively strong and its stable in properties in decomposition reaction of the present invention of the microwave absorption capacity of cocatalyst component perovskite type catalyst component.By adding a certain amount of perovskite type catalyst component in the composite catalyst that the present invention uses, make composite catalyst catalyst reaction bed while stable in properties stably can remain on a higher temperature levels.In a kind of concrete embodiment, described reaction tube is crystal reaction tube.In the present invention, in described hydrogen sulfide containing gas, the content of hydrogen sulfide is 2 ~ 50vol%, is preferably 10 ~ 20vol%.In a kind of concrete embodiment, the flow velocity of described hydrogen sulfide containing gas is 40 ~ 100ml/min.
In a kind of concrete embodiment, active component, available carrier and co catalysis component through ground and mixed aftershaping, then filter out 20 ~ 80 object particles and prepare described composite catalyst.Described composite catalyst is inserted in reaction tube and is formed microwave catalysis reaction bed, and be inserted with temperature thermocouple in the middle of bed, bed two ends are filled with silica wool and are fixed.In the present invention, the temperature that in described catalytic bed, hydrogen sulfide decomposes is 400 ~ 800 DEG C, preferably 450 ~ 750 DEG C.In the present invention, the pressure of hydrogen sulfide decomposition reaction is that normal pressure or pressure are micro-higher than normal pressure.The air speed of preferred hydrogen sulfide containing gas of the present invention is 900 ~ 3000ml/ (g cat.h).
Detailed description of the invention
Below in conjunction with embodiment, the invention will be further described.
The method of the invention is included in catalyst filling bed in crystal reaction tube, passes into nitrogen and purges removing air (such as nitrogen purge 20min), more in addition microwave irradiation.In reaction tube, pass into hydrogen sulfide containing mist (in the present invention, use the H of 15vol%
2the N of S and 85vol%
2gaseous mixture test), controlled the flow of hydrogen sulfide containing mist by spinner flowmeter, hydrogen sulfide generates hydrogen and sulphur by decomposing during beds.Sulphur Yin Wendu is now higher and be sublimed into gaseous state, by after beds through being condensed into solid sulfur.The a small amount of unreacted of the treated removing of tail gas, completely after hydrogen sulfide, can obtain the mist of nitrogen and hydrogen, with the hydrogen produced after gas chromatographic analysis detection reaction, calculate the conversion ratio of hydrogen sulfide according to the concentration of hydrogen.
Major experimental instrument in following examples and raw material: microwave catalysis reactor is the microwave catalysis reaction unit such as shown in CN 102133516A, in microwave reactor of the present invention, the power 0-1000W continuously adjustabe of microwave field, frequency is 2400-2500MHz.The external diameter of crystal reaction tube is 20mm, internal diameter 10mm, length 540mm.The detection of hydrogen adopts the GC-7890A gas chromatographic detection of Agilent company of U.S. production.Hydrogen sulfide gas is provided by Dalian great Te gas Co., Ltd, and nitrogen is provided by Xiangtan City special gas Co., Ltd.The γ of carrier described in the present invention-Al
2o
3, active component nickel sulfide and cobalt sulfide and co catalysis component perovskite type catalyst component all can be purchased in acquisition or laboratory and prepare voluntarily, all do not affect enforcement of the present invention.
Embodiment 1
The preparation of catalyst: take appropriate commercially available γ-Al
2o
3carrier (specific area 200m
2/ g) nickel sulfide prepared with laboratory fully grinds a period of time, then add the perovskite type catalyst component prepared in laboratory and continue fully grinding, after three's consistent mechanical is mixed, shaping under stress, then sieve out the composite catalyst NiS/ γ-Al that namely 20-80 order particle obtains in the present invention
2o
3/ BaMn
0.2cu
0.8o
3.In kind can obtain composite catalyst CoS/ γ-Al
2o
3/ BaMn
0.2cu
0.8o
3.
Embodiment 2
The present embodiment investigates the 30%NiS/30% γ-Al prepared with method in embodiment 1
2o
3/ 40%BaMn
0.2cu
0.8o
3catalyst and 30%CoS/10% γ-Al
2o
3/ 60%BaMn
0.2cu
0.8o
3catalyst (the percentage sign data in catalyst represent each component in catalyst and account for the mass percentage of composite catalyst) two kinds of composite catalysts decomposition efficiency of hydrogen sulfide in the hydrogen sulfide containing mist of catalysis under different microwave powers.The composite catalyst quality used in the present embodiment is 2g, and entrance mixed gas flow is 60ml/min, and reaction pressure is normal pressure, and microwave input power controls as 400W, 600W, 800W.Be deposited on the faint yellow sulphur product in beds downstream after collecting condensation, analyze known through X-ray powder diffraction, the sulphur produced is mainly α phase sulphur.
Table 1
As seen from Table 1, concerning same catalyst, along with the increase of microwave input power, the conversion ratio of hydrogen sulfide increases gradually; And microwave input power on the conversion ratio impact of hydrogen sulfide significantly.
Embodiment 3
The present embodiment investigates two kinds of composite catalysts in the same manner as in Example 2 decomposition efficiency of hydrogen sulfide in the hydrogen sulfide containing mist of catalysis under different reaction bed temperatures.The composite catalyst quality used in the present embodiment is 2g, and entrance mixed gas flow is 60ml/min, and reaction pressure is normal pressure.For the special catalyst of filling in beds, the temperature controlling beds by changing microwave input power reaches and is stabilized in object temperature.
Table 2
As seen from Table 2, concerning same catalyst, along with the increase of reaction temperature, the conversion ratio of hydrogen sulfide increases gradually; And reaction temperature on the conversion ratio impact of hydrogen sulfide significantly.
Embodiment 4
The present embodiment investigates the different composite catalyst (in table 3, the mass ratio of each component refers to the mass ratio of active component in catalyst, carrier and co catalysis component) for preparing with method in embodiment 1 decomposition efficiency of hydrogen sulfide in the hydrogen sulfide containing mist of catalysis under different reaction bed temperatures.The composite catalyst quality used in the present embodiment is 2g, and entrance mixed gas flow is 60ml/min, and reaction pressure is normal pressure.
Table 3
As can be seen from result of Table 3, the consumption of each component in composite catalyst of the present invention is all to final H
2s conversion ratio makes a significant impact.
Embodiment 5
The present embodiment investigates the 30%NiS/30% γ-Al prepared with method in embodiment 1
2o
3/ 40%BaMn
0.2cu
0.8o
3composite catalyst decomposition efficiency of hydrogen sulfide in the hydrogen sulfide containing mist of catalysis under different air speeds.In the present embodiment, reaction pressure is normal pressure, and adjustment microwave input power makes catalyst bed reaction temperature be 600 DEG C.Add by what regulate catalyst the air speed that quality and the flow of mist that passes into change reaction in reaction.
Table 4
As can be seen from result of Table 4, the air speed of gas is to H
2s conversion ratio also can make a significant impact.
Above embodiment shows, the reaction using microwave catalyst provided by the invention effectively can carry out microwave catalysis hydrogen sulfide to decompose hydrogen making and sulphur, have high compared with reaction decomposes efficiency under temperate condition, reaction is fast, the advantage of non-secondary pollution.The present invention is specially adapted to the process of sulfide hydrogen waste gas in natural gas, oil and coal chemical industry, can by catalytic decomposition hydrogen sulfide wherein thus recover hydrogen and sulphur.
Claims (7)
1. a microwave catalyst, described microwave catalyst is the composite catalyst comprising active component and co catalysis component, and described active component is nickel sulfide and/or cobalt sulfide, and described co catalysis component is perovskite type catalyst component; Also selectively comprise carrier in described microwave catalyst, described carrier is for being selected from γ-Al
2o
3, active carbon, ZSM-5 molecular sieve, one or more in ZSM-11 molecular sieve; And the content of active component is 10 ~ 60wt% in described composite catalyst, the content of carrier is 0 ~ 60wt%, and the content of co catalysis component is 20 ~ 90wt%.
2. catalyst according to claim 1, it is characterized in that, described perovskite type catalyst component is BaMn
0.2cu
0.8o
3.
3. catalyst according to claim 1, it is characterized in that, in described composite catalyst, the content of active component is 10 ~ 50wt%, and the content of carrier is 5 ~ 60wt%, and the content of co catalysis component is 30 ~ 70wt%.
4. catalyst according to claim 3, is characterized in that, in described composite catalyst, the content of active component is 20 ~ 30wt%, and the content of carrier is 10 ~ 30wt%, and the content of co catalysis component is 40 ~ 60wt%.
5. catalyst according to claim 1, it is characterized in that, described carrier is γ-Al
2o
3.
6. as a preparation method for catalyst as described in any one in Claims 1 to 5, comprise by active component, available carrier and co catalysis component through ground and mixed aftershaping, then filter out 20 ~ 80 object particles and prepare described composite catalyst.
7. one kind to be decomposed the application in hydrogen making and sulphur as the hydrogen sulfide of catalyst as described in any one in Claims 1 to 5 in the hydrogen sulfide containing gas of catalysis.
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105498740A (en) * | 2016-01-28 | 2016-04-20 | 中国科学院电子学研究所 | Strong microwave absorption catalyst and preparation method and application thereof |
| CN106673068A (en) * | 2016-11-22 | 2017-05-17 | 中国科学院生态环境研究中心 | Application of perovskite type composite oxide catalytic material to process of selective oxidation of H2S |
| CN107803208A (en) * | 2017-11-14 | 2018-03-16 | 湘潭大学 | A kind of microwave catalyst, its preparation method and the method that hydrogen sulfide is catalytically decomposed |
| CN109174126A (en) * | 2018-09-18 | 2019-01-11 | 张玉英 | A kind of photochemical catalyst and preparation method of Ca-Ti ore type layer structure |
| CN109759106A (en) * | 2019-03-22 | 2019-05-17 | 湘潭大学 | A kind of method that composite catalyst is used to that hydrogen sulfide to be catalytically decomposed |
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105498740A (en) * | 2016-01-28 | 2016-04-20 | 中国科学院电子学研究所 | Strong microwave absorption catalyst and preparation method and application thereof |
| CN106673068A (en) * | 2016-11-22 | 2017-05-17 | 中国科学院生态环境研究中心 | Application of perovskite type composite oxide catalytic material to process of selective oxidation of H2S |
| CN107803208A (en) * | 2017-11-14 | 2018-03-16 | 湘潭大学 | A kind of microwave catalyst, its preparation method and the method that hydrogen sulfide is catalytically decomposed |
| CN109174126A (en) * | 2018-09-18 | 2019-01-11 | 张玉英 | A kind of photochemical catalyst and preparation method of Ca-Ti ore type layer structure |
| CN109759106A (en) * | 2019-03-22 | 2019-05-17 | 湘潭大学 | A kind of method that composite catalyst is used to that hydrogen sulfide to be catalytically decomposed |
| CN109759106B (en) * | 2019-03-22 | 2021-09-24 | 湘潭大学 | Method for catalytic decomposition of hydrogen sulfide by using composite catalyst |
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