CN107803208A - A kind of microwave catalyst, its preparation method and the method that hydrogen sulfide is catalytically decomposed - Google Patents

A kind of microwave catalyst, its preparation method and the method that hydrogen sulfide is catalytically decomposed Download PDF

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Publication number
CN107803208A
CN107803208A CN201711122029.7A CN201711122029A CN107803208A CN 107803208 A CN107803208 A CN 107803208A CN 201711122029 A CN201711122029 A CN 201711122029A CN 107803208 A CN107803208 A CN 107803208A
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catalyst
sulfide
hydrogen sulfide
microwave
cnt
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周继承
罗米得
徐文涛
陈佳楠
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Xiangtan University
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Xiangtan University
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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
    • B01J27/00—Catalysts comprising the elements or compounds of halogens, sulfur, selenium, tellurium, phosphorus or nitrogen; Catalysts comprising carbon compounds
    • B01J27/02—Sulfur, selenium or tellurium; Compounds thereof
    • B01J27/04—Sulfides
    • B01J27/043—Sulfides with iron group metals or platinum group metals
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J35/00—Catalysts, in general, characterised by their form or physical properties
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B17/00—Sulfur; Compounds thereof
    • C01B17/02—Preparation of sulfur; Purification
    • C01B17/04—Preparation of sulfur; Purification from gaseous sulfur compounds including gaseous sulfides
    • C01B17/0495—Preparation of sulfur; Purification from gaseous sulfur compounds including gaseous sulfides by dissociation of hydrogen sulfide into the elements
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B3/00—Hydrogen; Gaseous mixtures containing hydrogen; Separation of hydrogen from mixtures containing it; Purification of hydrogen
    • C01B3/02—Production of hydrogen or of gaseous mixtures containing a substantial proportion of hydrogen
    • C01B3/04—Production of hydrogen or of gaseous mixtures containing a substantial proportion of hydrogen by decomposition of inorganic compounds, e.g. ammonia
    • 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

Abstract

The present invention discloses the microwave catalyst that a kind of preparation process is simple and catalytic activity is higher, the catalyst is the loaded catalyst prepared by hydrothermal synthesis method, it includes active component and carrier, and the active component is at least one of transient metal sulfide, and the carrier is CNT.Invention additionally discloses a kind of preparation method of above-mentioned microwave catalyst, step is simplified, and technological parameter is controllable, is easy to large-scale industrial production；Compared with existing grinding shaping mechanical preparation method, the loaded catalyst that is prepared using hydrothermal synthesis method, can retentive activity component activity, and can ensures that active component is most effective is supported on carrier, greatly improves the catalytic decomposition efficiency of hydrogen sulfide.Invention additionally discloses a kind of method that hydrogen sulfide is catalytically decomposed, hydrogen sulfide decomposition efficiency is higher under the conditions of relatively mild, is easy to industrial applications.

Description

A kind of microwave catalyst, its preparation method and the method that hydrogen sulfide is catalytically decomposed
Technical field
The present invention relates to Catalytic Technique of Microwave field, more particularly to a kind of microwave catalyst, its preparation method and catalysis The method of decomposing hydrogen sulfide.
Background technology
Hydrogen sulfide (H2S it is) a kind of severe toxicity, the sour gas of stench, can not only causes the corrosion of the materials such as metal, change It is also easy to cause catalyst poisoning to inactivate in work production；In addition, H2S can also be detrimental to health, and cause environmental pollution.Therefore, To caused a large amount of H in the industrial circles such as oil, natural gas, coal and mineral products processing2S gases carry out innoxious process for treating, Through as focus of concern.
And although traditional Crouse's processing method can obtain hydrogen sulfide partial oxidation in Sulfur and water, but it have lost A large amount of hydrogen resources.With increasing for China's high sulfur bauxite amount, oil refining hydrofinishing unit by-product contains H2S acid tail gas amounts Increase year by year, the amounts of hydrogen needed for hydrofinishing is consequently increased；In addition, hydrogen as oil hydrogenation cracking, higher alcohols synthesis, The primary raw material of the chemical engineering processes such as ammonia is synthesized, its demand is also considerable.Therefore, by H2It is an orderliness that S, which is directly decomposed, The H thought2S application technology as the second resource routes, it can both make its innoxious, hydrogen and elemental sulfur can be produced again, not only can be real Existing hydrogen resource recycling in petroleum refining process, can also reduce the great amount of carbon dioxide that conventional hydrocarbon-based reformation hydrogen production is brought Discharge, has very big realistic meaning.
The hydrogen sulfide that is related to reported at present decomposes the catalyst of hydrogen making and sulphur and is primarily present catalyst preparation The shortcomings of process is cumbersome and catalytic activity is not high, easy poisoning and deactivation, severe reaction conditions, catabolite are difficult to separation.
Therefore, develop it is a kind of in a mild condition can efficient-decomposition hydrogen sulfide hydrogen making and sulphur catalyst and catalysis Method is significant.
The content of the invention
The present invention provides the microwave catalyst that a kind of preparation process is simple and catalytic activity is higher, to oil, natural gas, coal With mineral products processing etc. in production process caused hydrogen sulfide waste gas handled, while clean energy resource (hydrogen) can also be obtained Using.Concrete technical scheme is as follows：
A kind of microwave catalyst, the catalyst are the loaded catalyst prepared by hydrothermal synthesis method, and it includes activity Component and carrier, the active component are at least one of transient metal sulfide, and the carrier is CNT；
In the catalyst：The total load mass content of active component is 1%-50%, and the mass content of carrier is 50%- 99%.
Preferable in above technical scheme, the CNT is the modified carbon nano-tube after alkali process.
Preferable in above technical scheme, the detailed process that the CNT carries out alkali process is：By CNT and Aqueous slkali is put into the three-necked flask of stirring in water bath, and treatment temperature is 30 DEG C -90 DEG C, processing time 0.5-8h；The alkali soluble Liquid is at least one of lithium hydroxide solution, sodium hydroxide solution and potassium hydroxide solution, hydroxide in the aqueous slkali The molar concentration of thing is 0.2-6mol/L.
It is preferable in above technical scheme, the transient metal sulfide be iron sulfide, cobalt sulfide, nickel sulfide, manganese sulfide, At least one of tungsten sulfide.
Preferable in above technical scheme, the transient metal sulfide is in cobalt sulfide, nickel sulfide and manganese sulfide It is at least one；In the catalyst：The total load mass content of active component is 2%-45%, and the mass content of carrier is 55%- 98%.
Using the microwave catalyst of the present invention, effect is：The catalyst passes through transient metal sulfide and CNT Combination, can be the support type microwave catalyst or binary composite transition metal of unitary composite transition metal sulfide The support type microwave catalyst of sulfide, the catalytic performance of active component are maximally utilized；Load is used as by CNT Body, the performance of microwave is absorbed beneficial to catalyst is improved, and be beneficial to the decomposition for promoting hydrogen sulfide.CNT can also be used at alkali Reason, it is easy to clean the surface of CNT and eliminates the influence in acid site, be advantageous to H2S absorption, further improve catalysis point Solve efficiency.
Invention additionally discloses a kind of preparation method of above-mentioned catalyst, preparation process is simplified, and the catalyst obtained has Greater activity, it is specifically：
The preparation method comprises the following steps：
The first step, CNT, ethylene glycol and water after transition metal nitrate, thiocarbamide, alkali process are weighed by proportioning；
Second step, the CNT after transition metal nitrate, thiocarbamide and alkali process is added to water and ethylene glycol mixing Stirred in solution, obtain the first mixed liquor；
3rd step, the first mixed liquor obtained by second step is inserted hydrothermal synthesis reaction is carried out in high-pressure hydrothermal reaction kettle, obtained To the second mixed liquor；
4th step, the second mixed liquor obtained by the 3rd step post-processed, produce microwave catalyst.
It is preferable in above technical scheme, in the second step：The mol ratio of transition metal nitrate and thiocarbamide is 2： 1-1：4；
Water and water in ethylene glycol mixed solution and ethylene glycol volume ratio are 2：8-7：3；Stirring is specifically：First use water-bath Magnetic agitation, then using ultrasonic vibration；The temperature of water-bath magnetic agitation is 30 DEG C -80 DEG C, mixing time 0.2-4h；Ultrasound shake The time for swinging middle supersound process is 0.5-3h.
It is preferable in above technical scheme, in the 3rd step：The temperature of hydrothermal synthesis reaction is 140 DEG C -220 DEG C, instead It is 6-48h between seasonable；Post processing in 4th step specifically includes suction filtration processing, vacuum drying treatment and sieving processing, In vacuum drying treatment：Drying temperature is 40 DEG C -100 DEG C, drying time 4-24h；The sieving processing filters out 20-80 mesh Particle.
Using the preparation method of the microwave catalyst of the present invention, step is simplified, and technological parameter is controllable, is easy to extensive chemical industry Industry produces；With it is existing grinding shaping mechanical preparation method compared with, using hydrothermal synthesis method prepare loaded catalyst, both The activity of energy retentive activity component, and can ensures that active component is most effective and is supported on carrier, greatly improves the catalysis of hydrogen sulfide Decomposition efficiency.
Invention additionally discloses a kind of method that hydrogen sulfide is catalytically decomposed, it is specifically：Quartz reaction in microwave reactor Above-mentioned microwave catalyst is filled in pipe and forms beds, hydrogen sulfide containing mixed gas is then passed through the catalyst bed Layer enters promoting the circulation of qi-solid catalysis reaction, realizes the decomposition of hydrogen sulfide.
It is preferable in above technical scheme, the beds center insertion temperature thermocouple, beds both ends Filling silica wool is fixed, and the temperature of beds is 400 DEG C -800 DEG C；Sulphur in the hydrogen sulfide containing mixed gas It is 10-30% to change hydrogen volume content, and the flow velocity of hydrogen sulfide containing mixed gas is 40-120ml/min.
Using the method for catalytic decomposition hydrogen sulfide disclosed in this invention, hydrogen sulfide decomposition condition is gentle, and microwave catalysis Resolution breaks the balance that existing hydrogen sulfide decomposes, and realizes that high efficiency is decomposed, is easy to industrial applications.
Embodiment
Embodiments of the invention are described in detail with reference to embodiment, so that advantages and features of the invention can be more It is easy to be readily appreciated by one skilled in the art, apparent is clearly defined so as to be made to protection scope of the present invention.
Embodiment 1：
A kind of microwave catalyst, the catalyst are the loaded catalyst prepared by hydrothermal synthesis method, and it includes activity Component and carrier, the total load mass content of active component is 1%-50%, and the mass content of carrier is 50%-99%.
The active component is in transient metal sulfide (iron sulfide, cobalt sulfide, nickel sulfide, manganese sulfide and tungsten sulfide) At least one.
The carrier is the CNT (i.e. CNT) after alkali process, and the detailed process of alkali process is：By CNT and alkali Solution is put into the three-necked flask of stirring in water bath, and treatment temperature is 30 DEG C -90 DEG C, processing time 0.5-8h；The aqueous slkali For at least one of lithium hydroxide solution, sodium hydroxide solution and potassium hydroxide solution, hydroxide in the aqueous slkali Molar concentration be 0.2-6mol/L.
The preparation method of above-mentioned catalyst specifically includes following steps：
The first step, CNT, ethylene glycol and water after transition metal nitrate, thiocarbamide, alkali process are weighed by proportioning；
Second step, the CNT after transition metal nitrate, thiocarbamide and alkali process is added to water and ethylene glycol mixing Stirred in solution, obtain the first mixed liquor；The mol ratio of transition metal nitrate and thiocarbamide is 2：1-1：4；Water and second Water and ethylene glycol volume ratio in two mixed alkoxide solutions are 2：8-7：3, preferably transition metal nitrate in solvent (by water and second two Alcohol formed mixed liquor) in mol ratio be 0.03mol/L-0.5mol/L；Stirring is specifically：First stirred using water-bath magnetic force Mix, then using ultrasonic vibration；The temperature of water-bath magnetic agitation is 30 DEG C -80 DEG C, mixing time 0.2-4h；Surpass in ultrasonic vibration The time of sonication is 0.5-3h；
3rd step, the first mixed liquor obtained by second step inserted into high-pressure hydrothermal reaction kettle (preferably polytetrafluoroethylene reactor) Middle carry out hydrothermal synthesis reaction, obtains the second mixed liquor；The temperature of hydrothermal synthesis reaction is 140 DEG C -220 DEG C, and the reaction time is 6-48h；
4th step, the second mixed liquor obtained by the 3rd step post-processed, produce microwave catalyst, herein：Post processing tool Body includes suction filtration processing, vacuum drying treatment and sieving and handled, in vacuum drying treatment：Drying temperature is 40 DEG C -100 DEG C, Drying time is 4-24h；The sieving processing filters out the particle of 20-80 mesh.
Embodiment 2：
Catalysed curing hydrogen will be used for according to the gained microwave catalyst of embodiment 1, and be specifically：Quartz in microwave reactor Microwave catalyst is filled in reaction tube and forms beds, hydrogen sulfide containing mixed gas is then passed through the beds Enter promoting the circulation of qi-solid catalysis reaction, realize the decomposition of hydrogen sulfide.The beds center insertion temperature thermocouple, catalyst Filling silica wool is fixed at bed both ends.Details as Follows：
(1), the quality of catalyst is 2g, and reaction bed temperature is 650 DEG C, reaction gas flow 60ml/min, instead It is normal pressure to answer pressure, and using 10-30wt% support type microwave catalyst CoS/NiS/CNT, it is different to investigate identical active component Load capacity decomposes the influence of hydrogen making and sulfur reaction to hydrogen sulfide, and details are shown in Table 1：
The influence that table 1 is decomposed using 10-30wt% support type microwave catalyst CoS/NiS/CNT to hydrogen sulfide
Catalyst Reaction bed temperature (DEG C) Conversion ratio (%)
5%CoS5%NiS/CNT 650 39.41
10%CoS10%NiS/CNT 650 43.15
15%CoS15%NiS/CNT 650 33.63
As it can be seen from table 1 under conditions of microwave irradiation, binary composite transition metal sulfide catalyst carries out microwave Decomposing hydrogen sulfide reacts, and wherein mass fraction 10%CoS10%NiS/CNT catalyst effects are optimal, and the conversion ratio of hydrogen sulfide is 43.15%, this is probably that activity component load quantity is too low, causes active catalyst sites few, and opposing activity component load capacity is too high, Active component is caused to be reunited, catalytic reaction activity is not just high.Only appropriate load constituent content can just obtain preferable decomposition Effect, therefore the gross activity component loading content of the catalyst is 20wt%.
(2), the quality of catalyst is 2g, and reaction bed temperature is 700 DEG C, reaction gas flow 60ml/min, instead It is normal pressure to answer pressure, using 20wt% support type microwave catalyst CoS/ or NiS/CNT, investigates the load of different activities component Type catalyst decomposes the influence of hydrogen making and sulfur reaction to hydrogen sulfide, and details are shown in Table 2：
Table 2 investigates the influence that 20wt% different loads type microwave catalyst decomposes to hydrogen sulfide
Catalyst Reaction bed temperature (DEG C) Conversion ratio (%)
20%NiS/CNT 700 38.63
5%CoS15%NiS/CNT 700 41.15
10%CoS10%NiS/CNT 700 49.50
15%CoS5%NiS/CNT 700 40.00
20%CoS/CNT 700 39.30
From table 2 it can be seen that under conditions of microwave irradiation, the catalyst ratio of binary composite transition metal sulfide is loaded Unitary transition metal sulfide catalyst is notable to the discomposing effect of hydrogen sulfide, because having association between two active components Same-action.Wherein mass fraction is that 10%CoS10%NiS/CNT catalyst effects are optimal, and the resolution ratio of hydrogen sulfide is 49.50%.
(3), the quality of catalyst is 2g, and using 10%CoS/10%NiS/CNT catalyst, reaction gas flow is 60ml/min, reaction pressure are normal pressure, investigate different microwave input powers (be respectively set as 500W, 550W, 600W, 650W, 700w) influence decomposed to hydrogen sulfide, details are shown in Table 3：
The influence that same microwave catalyst decomposes to hydrogen sulfide under the conditions of the different microwave of table 3
Microwave input power (W) Reaction bed temperature (DEG C) Conversion ratio (%)
500 514 31.32
550 578 37.16
600 647 42.95
650 686 47.64
700 739 56.89
From table 3 it can be seen that with the increase of microwave input power, the conversion ratio of hydrogen sulfide significantly improves.It follows that Microwave input power decomposes hydrogen making on hydrogen sulfide and sulfur reaction influence is more notable.Hydrogen sulfide converts as can be known from Table 3 The raising of rate gradually tends to be slow with the increase of microwave input power, and therefore, microwave input power is unsuitable too high, and too high is micro- Ripple input power causes reaction bed temperature too high, so as to influence the performance of catalyst to a certain extent.
(4), the quality of catalyst is 2g, and using 10%CoS/10%NiS/CNT catalyst, reaction gas flow is 60ml/min, reaction pressure are normal pressure, investigate reaction bed temperature (be respectively set as 550 DEG C, 600 DEG C, 650 DEG C, 700 DEG C, 750 DEG C) to hydrogen sulfide decompose influence, details such as table 4：
The influence that the different catalysts bed temperature of table 4 decomposes to hydrogen sulfide
Reaction bed temperature (DEG C) Conversion ratio (%)
550 38.72
600 41.46
650 43.15
700 49.50
750 58.15
As can be found from Table 4, with the rise of reaction bed temperature, the conversion ratio of hydrogen sulfide, which has, significantly to be increased. As can be seen here, reaction bed temperature decomposes hydrogen making on hydrogen sulfide and sulfur reaction influence is more notable.
(5), the quality of catalyst is 2g, using 10%CoS/10%NiS/CNT catalyst, reaction bed temperature setting For 700 DEG C, reaction pressure is normal pressure, investigates different air speed (1200mlg-1·h-1、1800ml·g-1·h-1、2400ml· g-1·h-1、3000ml·g-1·h-1、3600ml·g-1·h-1, air speed realized by changing reaction gas flow) influence, It is shown in Table 5：
The influence that different air speeds are decomposed to hydrogen sulfide in the reaction of the microwave catalysis of table 5
Air speed (mlg-1·h-1) Reaction bed temperature (DEG C) Conversion ratio (%)
1200 700 73.38
1800 700 49.50
2400 700 41.45
3000 700 35.21
3600 700 26.65
As known from Table 5, with the increase of air speed, the trend being decreased obviously is presented in the conversion ratio of hydrogen sulfide.As can be seen here, it is empty Speed decomposes the influence of hydrogen making and sulfur reaction also highly significant to hydrogen sulfide.
In summary, support type microwave catalyst of the invention decomposes hydrogen making and sulfur reaction effect for hydrogen sulfide Preferably.Microwave catalyst its preparation method in the present invention is simple, and catalytic activity is good, available for oil, natural gas and coalman The processing of hydrogen sulfide waste gas in industry, and hydrogen and sulphur can be reclaimed.
Embodiments of the invention are the foregoing is only, are not intended to limit the scope of the invention, it is every to utilize this hair The equivalent structure or equivalent flow conversion that bright description is made, or directly or indirectly it is used in other related technology necks Domain, it is included within the scope of the present invention.

Claims (10)

  1. A kind of 1. microwave catalyst, it is characterised in that：The catalyst is the loaded catalyst prepared by hydrothermal synthesis method, its Including active component and carrier, the active component is at least one of transient metal sulfide, and the carrier is carbon nanometer Pipe；
    In the catalyst：The total load mass content of active component is 1%-50%, and the mass content of carrier is 50%-99%.
  2. 2. microwave catalyst according to claim 1, it is characterised in that the CNT is changing after alkali process Property CNT.
  3. 3. microwave catalyst according to claim 2, it is characterised in that the CNT carries out the specific mistake of alkali process Cheng Shi：CNT and aqueous slkali are put into the three-necked flask of stirring in water bath, treatment temperature is 30 DEG C -90 DEG C, processing time For 0.5-8h；The aqueous slkali is at least one of lithium hydroxide solution, sodium hydroxide solution and potassium hydroxide solution, institute The molar concentration for stating hydroxide in aqueous slkali is 0.2-6mol/L.
  4. 4. microwave catalyst according to claim 3, it is characterised in that the transient metal sulfide is iron sulfide, sulphur Change at least one of cobalt, nickel sulfide, manganese sulfide, tungsten sulfide.
  5. 5. microwave catalyst according to claim 4, it is characterised in that the transient metal sulfide is cobalt sulfide, sulphur Change at least one of nickel and manganese sulfide；
    In the catalyst：The total load mass content of active component is 2%-45%, and the mass content of carrier is 55%-98%.
  6. 6. a kind of preparation method of the microwave catalyst as described in claim 2-5 any one, it is characterised in that including following step Suddenly：
    The first step, CNT, ethylene glycol and water after transition metal nitrate, thiocarbamide, alkali process are weighed by proportioning；
    Second step, the CNT after transition metal nitrate, thiocarbamide and alkali process is added to water and ethylene glycol mixed solution In stir, obtain the first mixed liquor；
    3rd step, the first mixed liquor obtained by second step is inserted hydrothermal synthesis reaction is carried out in high-pressure hydrothermal reaction kettle, obtain the Two mixed liquors；
    4th step, the second mixed liquor obtained by the 3rd step post-processed, produce microwave catalyst.
  7. 7. the preparation method of microwave catalyst according to claim 6, it is characterised in that in the second step：
    The mol ratio of transition metal nitrate and thiocarbamide is 2：1-1：4；
    Water and water in ethylene glycol mixed solution and ethylene glycol volume ratio are 2：8-7：3；
    Stirring is specifically：Water-bath magnetic agitation is first used, then using ultrasonic vibration；The temperature of water-bath magnetic agitation is 30 DEG C -80 DEG C, mixing time 0.2-4h；The time being ultrasonically treated in ultrasonic vibration is 0.5-3h.
  8. 8. the preparation method of microwave catalyst according to claim 6, it is characterised in that in the 3rd step：Hydro-thermal is closed Temperature into reaction is 140 DEG C -220 DEG C, reaction time 6-48h；
    Post processing in 4th step specifically includes suction filtration processing, vacuum drying treatment and sieving and handled, at vacuum drying In reason：Drying temperature is 40 DEG C -100 DEG C, drying time 4-24h；The sieving processing filters out the particle of 20-80 mesh.
  9. A kind of 9. method that hydrogen sulfide is catalytically decomposed, it is characterised in that：Filled such as in crystal reaction tube in microwave reactor Microwave catalyst described in claim 1-5 any one forms beds, then leads to hydrogen sulfide containing mixed gas Enter the beds and carry out gas-solid-phase catalytic reaction, realize the decomposition of hydrogen sulfide.
  10. 10. the method for catalytic decomposition hydrogen sulfide according to claim 9, it is characterised in that：The beds center Temperature thermocouple is inserted, beds both ends filling silica wool is fixed, and the temperature of beds is 400 DEG C -800 ℃；Hydrogen sulfide volume content in the hydrogen sulfide containing mixed gas is 10-30%, the flow velocity of hydrogen sulfide containing mixed gas For 40-120ml/min.
CN201711122029.7A 2017-11-14 2017-11-14 A kind of microwave catalyst, its preparation method and the method that hydrogen sulfide is catalytically decomposed Pending CN107803208A (en)

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Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
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
CN109772422A (en) * 2019-03-22 2019-05-21 湘潭大学 A kind of preparation method and catalyst of hetero-junctions catalyst
CN109865526A (en) * 2019-03-22 2019-06-11 湘潭大学 A kind of method that hetero-junctions catalyst is used to that hydrogen sulfide to be catalytically decomposed

Citations (17)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1345694A (en) * 2000-09-22 2002-04-24 株式会社日进纳米技术 Method for synthesizing carbon nano tube and equipment thereof
CN1429767A (en) * 2001-10-04 2003-07-16 佳能株式会社 Method for preparing nanometer carbon material
CN1814349A (en) * 2006-03-08 2006-08-09 清华大学 Method for preparing fuel cell catalyst using sulfide precipitation process
CN101327429A (en) * 2008-07-18 2008-12-24 清华大学 Catalyst for catalytic decomposition of hydrogen iodide and preparation method thereof
CN101801526A (en) * 2007-09-14 2010-08-11 丰田自动车株式会社 Fine-particle composite, process for producing the fine-particle composite, catalyst for solid polymer electrolyte fuel cell, and solid polymer electrolyte fuel cell
CN102408095A (en) * 2011-08-20 2012-04-11 大连理工大学 Method of decomposing hydrogen sulfide for preparation of hydrogen and elemental sulfur
CN102407071A (en) * 2011-12-30 2012-04-11 湘潭大学 Denitration method utilizing microwave catalytic selective reduction reaction
CN104437553A (en) * 2014-12-29 2015-03-25 湘潭大学 Microwave catalyst, preparation method and application thereof
CN104524934A (en) * 2014-12-29 2015-04-22 湘潭大学 Method for producing hydrogen and sulfur by using microwave catalytic decomposition of hydrogen sulfide
CN105013512A (en) * 2015-06-08 2015-11-04 中国科学院长春应用化学研究所 Self-supporting transitional metal sulfide catalyst and preparation methods and applications thereof
CN105280900A (en) * 2015-09-22 2016-01-27 复旦大学 Tungsten disulfide/graphene nanobelt composite material and preparation method thereof
CN105271175A (en) * 2015-11-16 2016-01-27 中南大学 Dispersion method of carbon nano tube
CN106179421A (en) * 2016-07-19 2016-12-07 天津大学 The preparation of sulfide catalyst and the application in lignin conversion thereof
CN106299262A (en) * 2015-06-04 2017-01-04 北京化工大学 The preparation method of the CNT of a kind of filler metal sulfide and the application in lithium ion battery
CN106311254A (en) * 2016-11-16 2017-01-11 东北石油大学 Residual oil hydrogenation catalyst, preparation method and hydrogenation method
CN106669739A (en) * 2016-12-30 2017-05-17 温州大学 Transition metal sulfide/carbon nanotube composite material as well as preparation method and application thereof
CN106944098A (en) * 2017-03-27 2017-07-14 中国科学院福建物质结构研究所 Carbon material supported copper cobalt dual-metal sulfide composite and its preparation method and application in the treatment of waste water

Patent Citations (18)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1345694A (en) * 2000-09-22 2002-04-24 株式会社日进纳米技术 Method for synthesizing carbon nano tube and equipment thereof
CN1429767A (en) * 2001-10-04 2003-07-16 佳能株式会社 Method for preparing nanometer carbon material
CN1814349A (en) * 2006-03-08 2006-08-09 清华大学 Method for preparing fuel cell catalyst using sulfide precipitation process
CN101801526A (en) * 2007-09-14 2010-08-11 丰田自动车株式会社 Fine-particle composite, process for producing the fine-particle composite, catalyst for solid polymer electrolyte fuel cell, and solid polymer electrolyte fuel cell
CN105047954A (en) * 2007-09-14 2015-11-11 丰田自动车株式会社 Fine-particle composite, process for producing fine-particle composite, catalyst for solid polymer electrolyte fuel cell, and solid polymer electrolyte fuel cell
CN101327429A (en) * 2008-07-18 2008-12-24 清华大学 Catalyst for catalytic decomposition of hydrogen iodide and preparation method thereof
CN102408095A (en) * 2011-08-20 2012-04-11 大连理工大学 Method of decomposing hydrogen sulfide for preparation of hydrogen and elemental sulfur
CN102407071A (en) * 2011-12-30 2012-04-11 湘潭大学 Denitration method utilizing microwave catalytic selective reduction reaction
CN104524934A (en) * 2014-12-29 2015-04-22 湘潭大学 Method for producing hydrogen and sulfur by using microwave catalytic decomposition of hydrogen sulfide
CN104437553A (en) * 2014-12-29 2015-03-25 湘潭大学 Microwave catalyst, preparation method and application thereof
CN106299262A (en) * 2015-06-04 2017-01-04 北京化工大学 The preparation method of the CNT of a kind of filler metal sulfide and the application in lithium ion battery
CN105013512A (en) * 2015-06-08 2015-11-04 中国科学院长春应用化学研究所 Self-supporting transitional metal sulfide catalyst and preparation methods and applications thereof
CN105280900A (en) * 2015-09-22 2016-01-27 复旦大学 Tungsten disulfide/graphene nanobelt composite material and preparation method thereof
CN105271175A (en) * 2015-11-16 2016-01-27 中南大学 Dispersion method of carbon nano tube
CN106179421A (en) * 2016-07-19 2016-12-07 天津大学 The preparation of sulfide catalyst and the application in lignin conversion thereof
CN106311254A (en) * 2016-11-16 2017-01-11 东北石油大学 Residual oil hydrogenation catalyst, preparation method and hydrogenation method
CN106669739A (en) * 2016-12-30 2017-05-17 温州大学 Transition metal sulfide/carbon nanotube composite material as well as preparation method and application thereof
CN106944098A (en) * 2017-03-27 2017-07-14 中国科学院福建物质结构研究所 Carbon material supported copper cobalt dual-metal sulfide composite and its preparation method and application in the treatment of waste water

Non-Patent Citations (6)

* Cited by examiner, † Cited by third party
Title
YAN-RU LIU: "Facile one-pot synthesis of CoS2-MoS2/CNTs as efficient electrocatalyst for hydrogen evolution reaction", 《YAN-RU LIU》 *
姜山，等: "《中国科学院科学传播系列丛书 纳米》", 30 September 2013, 科学普及出版社 *
崔虹云，等: "《碳纳米管网络复合结构与纳米膜接触特性的研究》", 31 August 2017, 东北大学出版社 *
田永君，等: "《先进材料导论》", 31 December 2014, 哈尔滨工业大学出版社 *
谢昆，等: "《纳米技术在水污染控制中的应用》", 30 June 2014, 武汉大学出版社 *
贾瑛，等: "《轻质碳材料的应用》", 30 November 2013, 国防工业出版社 *

Cited By (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
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
CN109772422A (en) * 2019-03-22 2019-05-21 湘潭大学 A kind of preparation method and catalyst of hetero-junctions catalyst
CN109865526A (en) * 2019-03-22 2019-06-11 湘潭大学 A kind of method that hetero-junctions 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
CN109865526B (en) * 2019-03-22 2022-01-18 湘潭大学 Method for catalytic decomposition of hydrogen sulfide by using heterojunction catalyst

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