CN102408095B - Method of decomposing hydrogen sulfide for preparation of hydrogen and elemental sulfur - Google Patents

Method of decomposing hydrogen sulfide for preparation of hydrogen and elemental sulfur Download PDF

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CN102408095B
CN102408095B CN2011102405121A CN201110240512A CN102408095B CN 102408095 B CN102408095 B CN 102408095B CN 2011102405121 A CN2011102405121 A CN 2011102405121A CN 201110240512 A CN201110240512 A CN 201110240512A CN 102408095 B CN102408095 B CN 102408095B
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oxide
sulfide
hydrogen
hydrogen sulfide
elemental sulfur
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王安杰
赵璐
金亮
王瑶
李翔
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Dalian University of Technology
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Abstract

The invention discloses a method of decomposing hydrogen sulfide for preparation of hydrogen and elemental sulfur, which belongs to the technical field of hydrogen production and gas purification. The invention is characterized in that: hydrogen sulfide or gas containing hydrogen sulfide is subjected to ionization through blockage of discharge by using a medium so as to form uniformly distributed non-equilibrium plasma, and hydrogen sulfide spontaneously decomposes into hydrogen and elemental sulfur in the plasma; when there is a photocatalyst in the plasma, energy in the photons of the photocatalyst can be utilized to promote decomposition of hydrogen sulfide, and complete conversion can be realized under proper conditions. All the frequently used solid photocatalysts can be used in the above mentioned process, e.g., titanium oxide, cerium oxide, zirconia, zinc oxide, cadmium oxide, copper oxide, molybdena, tungsten oxide, zinc sulfide, cadmium sulfide, copper sulfide, molybdenum sulfide, tungsten sulfide and a mixture composed of two or more selected from the above-mentioned photocatalysts; the photocatalysts can also be loaded on a porous material to prepare load type catalysts. The method provided in the invention is especially applicable to treatment of gas containing hydrogen sulfide in the industries of natural gas, petroleum and coal chemistry and is also applicable to preparation of hydrogen and elemental sulfur through dissociation of gas containing hydrogen sulfide in the fields of metallurgy, sea and the like. The method has no special requirements for or restriction on the source and composition of gas; thus, the method has universality to preparation of hydrogen through decomposition of hydrogen sulfide.

Description

The method of a kind of preparing hydrogen gas by decomposing hydrogen sulfide and elemental sulfur
Technical field
The invention belongs to hydrogen manufacturing and gas purification technology field, relate to and a kind of harmful hydrogen sulfide is decomposed into the method that nontoxic elemental sulfur obtains hydrogen simultaneously.
Technical background
Hydrogen sulfide is the colourless gas of a kind of severe toxicity, stench, not only is detrimental to health, and can causes the corrosion of the materials such as metal, therefore need to carry out on the spot harmless treatment.Sweet natural gas, oil, coal and mineral products processing industry produce a large amount of H 2 S-containing gas, and main at present is elemental sulfur and water by Crouse (Claus) method with its partial oxidation:
H 2S+3/2O 2→SO 2+H 2O
2H 2S+SO 2→3/xS x+2H 2O
Although claus process can realize that hydrogen sulfide is innoxious, make to have more that the hydrogen resource conversion of high added value is water, wasted valuable resource.Obviously, if hydrogen sulfide can be decomposed, then not only can make hydrogen sulfide innoxious, and can obtain the hydrogen of high added value and nontoxic elemental sulfur.Theoretically, in common Nonmetal hydride (water, ammonia and hydrogen sulfide), the dissociation energy of hydrogen sulfide is minimum, thereby hydrogen sulfide thermolysis hydrogen manufacturing is the easiest.Yet the decomposition reaction of hydrogen sulfide is subjected to thermodynamics equilibrium limit, only have at low temperatures very low equilibrium conversion (Qian Xinping, Ling Zhongqian, Zhou Wu, Cen Kefa, the chemistry of fuel journal, 2005,33 (6), 722-725).Such as, in the time of 1000 ℃ the transformation efficiency of hydrogen sulfide only be 20%, 1200 ℃ transformation efficiency be 38% (Slimane R.B., GasTIPS, 2004,30-34).In order to produce localized hyperthermia, have many investigators to adopt superinsulation method decomposing hydrogen sulfide, but its energy consumption is still very high.In order to break the chemical reaction equilibrium restriction, have many investigators to adopt film reaction technology, but the development and application of the mould material of high temperature resistant and anti-sulphur become the key that realizes technological breakthrough.The reaction of hydrogen sulfide decomposing hydrogen-production and sulphur can also realize by methods such as electrochemistry and photochemical catalysis, but have the many or low shortcoming of reaction efficiency of operation steps.
When hydrogen sulfide was used for hydrogen manufacturing as a kind of hydrogen source, the residual meeting of trace hydrogen sulfide brought many serious problems when using.Hydrogen is mainly used in the reductive agent of fuel cell and chemical industry, makes catalyzer owing to all use precious metal in these two kinds of occasions, and hydrogen sulfide very easily makes the precious metal poisoning and loses activity.In the method for existing hydrogen sulfide pyrolysis hydrogen manufacturing, owing to be subjected to the restriction of thermodynamic(al)equilibrium can not realize transforming fully, must relate to separating of product hydrogen and reactant hydrogen sulfide, and the lock out operation of H 2 S-containing gas is very harsh, and is difficult to realize separating fully.Therefore, the complete decomposition technique of hydrogen sulfide is only a kind of desirable hydrogen producing technology.
Summary of the invention
The invention provides the method for a kind of preparing hydrogen gas by decomposing hydrogen sulfide and elemental sulfur, under dielectric barrier discharge and photocatalysis synergy, hydrogen sulfide is efficiently decomposed, hydrogen sulfide can 100% be converted into hydrogen and elemental sulfur under optimum conditions.
The technical scheme that technical solution problem of the present invention adopts is as follows:
Plasma body is the 4th attitude of material, is rich in the as lively as a cricket high reactivity species such as atom, molecule and free radical of ion, electronics, excited state, is a kind of gas with electroconductibility.The present invention adopts the plasma body of the dielectric barrier discharge of atmospheric operation to be combined with catalyzer, utilizes plasma body to the fully decomposition that the promotion of reaction is realized hydrogen sulfide with catalyzer that excites of hydrogen sulfide.The energy of the high energy particle in the plasma body is generally several to tens electron-volts (eV), and the activation energy that provides chemical reaction required is provided.In addition, plasma body is nonequilibrium situations, thereby can break the thermodynamics equilibrium limit of hydrogen sulfide decomposition reaction.Moreover, contain the mutually equally distributed a large amount of photons of body in the plasma body, not only can effectively utilize this part energy by photochemical catalysis, and can improve the transformation efficiency of reaction, thereby realize less energy-consumption, high-level efficiency decomposing hydrogen sulfide production high-purity hydrogen and elemental sulfur.
The fully decomposition of hydrogen sulfide is worked in coordination with by dielectric barrier discharge and photochemical catalysis and realized particularly: dielectric barrier discharge makes hydrogen sulfide or hydrogen sulfide containing ionization of gas, form equally distributed nonequilibrium plasma, hydrogen sulfide Auto-decomposition in plasma body is hydrogen and elemental sulfur; When in the plasma body photocatalyst being arranged, the transformation efficiency of hydrogen sulfide can significantly improve, and can realize under the suitable condition transforming fully.Dielectric barrier discharge both can use AC power, also can use direct supply.The photocatalyst of plasma body zone filling is solid particulate and powder, and the solid photocatalyst with photocatalytic activity all is suitable for the present invention.Such as, titanium oxide, cerium oxide, zirconium white, zinc oxide, Cadmium oxide, cupric oxide, molybdenum oxide, Tungsten oxide 99.999, zinc sulphide, Cadmium Sulfide, cupric sulfide, moly-sulfide, tungsten sulfide, and two kinds or two or more mixtures being formed by them.Photocatalyst can be used metal and non-metallic element modification and modification, to improve catalytic perfomance.
Component with photocatalytic activity also can load on makes loaded catalyst on the porous material, employed carrier does not have particular restriction, it can be gac, carbonaceous molecular sieve, carbon nanotube, carbon fiber, Graphene, soccerballene, silicon oxide, aluminum oxide, silico-aluminate, phosphoric acid salt, carbonate, magnesium oxide, titanium oxide, calcium oxide, zirconium white, cerium oxide, zeolite molecular sieve, mesopore molecular sieve, mesoporous-microporous composite material, the high-specific surface area large pore material, in high molecular polymer and the porous metal one or both and two or more mixtures, preferable shape are spherical, bar shaped, the trifolium shape, the Herba Galii Bungei shape, sheet, tooth is spherical.The preparation method can adopt traditional pickling process, coprecipitation method, sedimentation and sputtering method etc.
Effect of the present invention and benefit are that the method not only can be carried out harmless treatment to hydrogen sulfide, and can prepare from hydrogen sulfide the hydrogen of high added value.The method does not have particular requirement or restriction to source and the composition of gas, thereby has universality for the decomposing hydrogen-production of various concentration of H 2 S.
Description of drawings
Fig. 1 is CdS/Al during decomposing hydrogen sulfide in the dielectric barrier discharge plasma 2O 3The activity of photocatalyst is with the variation in reaction times.
Embodiment
Be described in detail specific embodiments of the invention below in conjunction with technical scheme.
Embodiment 1
The preparation of catalyzer: commercially available titanium dioxide, silicon-dioxide and aluminum oxide pressed powder at forming under the pressure, are then sieved out 20~40 order particles.
Embodiment 2
Taking by weighing 1.50 gram particle degree is 20~40 purpose γ-Al 2O 3Carrier (specific surface area 270m 2/ g), get the Cd (NO of 0.40 gram 3) 24H 2O is dissolved in 1.5 ml deionized water, this solution is slowly splashed into carrier and stir, at room temperature flooded 8 hours, then in 120 ℃ baking oven dry 12 hours, the gained solid in retort furnace under 450 ℃ of air atmosphere roasting be down to room temperature after 5 hours, the gained catalyzer is labeled as CdO/Al 2O 3Adopt that use the same method can making ZnO/Al 2O 3
Embodiment 3
With the CdO/Al that obtains among the embodiment 3 2O 3Sulfuration pack into passing into vulcanizing agent (10%H with 30mL/min in the silica tube 2S/Ar), rise to 400 ℃ and kept 100 minutes in 20 minutes.Obtain the catalyzer that contains 10% (massfraction) Cadmium Sulfide of alumina load, be denoted as CdS/Al 2O 3ZnS/Al 2O 3The preparation of employing same procedure.
Embodiment 4
The dielectric barrier discharge structure of reactor: discharge electrode adopts the line barrel structure, and high-pressure stage is positioned on the axis of tubular reactor, and earthing pole is looped around the outer wall of quartz glass tube.High voltage electrode is the stainless steel wire of 2.5 millimeters of diameters, and ground connection is kaolin very.The external diameter of silica tube is 10 millimeters.
Beaded catalyst is placed in the cavity between quartz glass tube and high voltage electrode, pass into nitrogen 5 minutes to remove the oxygen in the reactor.By mass flowmeter control, make the argon gas gas mixture that contains 10% hydrogen sulfide pass through beds with certain flow.Connect the plasma electrical source that connects high-pressure stage and earthing pole, regulating voltage, electric current and frequency can change power input.After reacted gas process aqueous sodium hydroxide solution and two sections absorptions of copper sulfate solution, hydrogen content chromatographic instrument on-line analysis in the tail gas.Calculate the transformation efficiency of hydrogen sulfide according to the concentration of hydrogen.Under 100% conversion condition, further verify with Lead acetate paper.
Table 1 has compared the transformation efficiency that different catalysts hydrogen sulfide under identical power input condition is decomposed into hydrogen and elemental sulfur.Reaction conditions is as follows: catalyst volume 1mL, and inlet gas flow: 10mL/min, reaction pressure is normal pressure, power input is 24 watts of (55V * 0.43A).Can find out that under the synergy of plasma body and titanium dioxide, hydrogen sulfide can be converted into hydrogen and elemental sulfur fully.The faint yellow sulphur product that is deposited on the beds downstream is mainly α phase sulphur through the analysis of x-ray powder diffraction.Using three kinds of catalyzer to be showed no transformation efficiency in 10 hours in reaction descends.
Table 1 under identical power input hydrogen sulfide at TiO 2, SiO 2And Al 2O 3On be decomposed into the transformation efficiency of hydrogen and elemental sulfur
Catalyzer TiO 2 SiO 2 Al 2O 3
The hydrogen sulfide transformation efficiency, % 100 85 90
Embodiment 5
Adopt reaction unit and reactions steps among the embodiment 4 to carry out the decomposition reaction of hydrogen sulfide in plasma body under solid photocatalyst existence condition.The plasma discharge frequency is 10kHz, and loaded catalyst is 1.5mL, reaction gas (10%H 2The gas mixture of S and 90%Ar) flow velocity is 60mL/min.Reaction result such as following table:
The reactivity worth of the collaborative decomposing hydrogen sulfide of plasma body and solid photocatalyst and product Hydrogen Energy consumption under table 2 different input power
Figure BDA0000084858260000051
Figure BDA0000084858260000061
Embodiment 6
Adopt reaction unit and reactions steps among the embodiment 4 to investigate CdS/Al 2O 3The activity stability of photocatalyst in the hydrogen sulfide decomposition reaction.The plasma discharge frequency is 10kHz, and loaded catalyst is 1.5mL, reaction gas (10%H 2The gas mixture of S and 90%Ar) flow velocity is 60mL/min.Reaction result as shown in Figure 1.As seen, CdS/Al 2O 3Has good activity stability.
Above-mentioned test-results shows that the collaborative thermodynamics equilibrium limit of not only can breaking of dielectric barrier discharge and photocatalyst realizes transforming fully, and energy utilization rate is high, is the effective ways of a kind of direct decomposing hydrogen sulfide hydrogen making and sulphur.
Above-described embodiment has illustrated dielectric barrier discharge plasma and the collaborative efficient decomposition method of hydrogen sulfide, the employed Catalysts and its preparation method realized of photochemical catalysis with the example that is decomposed into of hydrogen sulfide in the argon gas.Can carry out some modifications and improvement to the present invention, for example, reactor and electrode structure are improved, with metal or nonmetal and its esters carrier surface is carried out modification, perhaps add some metals or nonmetal Primary Catalysts of the present invention is carried out certain modification etc.

Claims (9)

1. the method for a preparing hydrogen gas by decomposing hydrogen sulfide and elemental sulfur, the fully decomposition of hydrogen sulfide is by dielectric barrier discharge and the collaborative realization of photochemical catalysis, it is characterized in that: make hydrogen sulfide ionization by dielectric barrier discharge, form equally distributed nonequilibrium plasma, hydrogen sulfide Auto-decomposition in plasma body is hydrogen and elemental sulfur; Filling has the solid photocatalyst of photocatalytic activity in the plasma body zone, improves the transformation efficiency of hydrogen sulfide.
2. method according to claim 1 is characterized in that, dielectric barrier discharge had both used AC power, also uses direct supply.
3. method according to claim 1 is further characterized in that, the photocatalyst of plasma body zone filling is solid particulate and powder.
4. method according to claim 1, be further characterized in that the solid photocatalyst comprises a kind of in titanium oxide, cerium oxide, zirconium white, zinc oxide, Cadmium oxide, cupric oxide, molybdenum oxide, Tungsten oxide 99.999, zinc sulphide, Cadmium Sulfide, cupric sulfide, moly-sulfide, the tungsten sulfide and two kinds or two or more mixtures being comprised of them.
5. according to claim 1,3 or 4 described methods, be further characterized in that photocatalyst improves catalytic perfomance with metal and non-metallic element modification and modification.
6. according to claim 1,3 or 4 described methods, be further characterized in that, component with photocatalytic activity loads on and makes loaded catalyst on the porous material, and employed carrier is gac, carbon molecular sieve, carbon nanotube, carbon fiber, Graphene, soccerballene, silicon oxide, aluminum oxide, silico-aluminate, phosphoric acid salt, carbonate, magnesium oxide, titanium oxide, calcium oxide, zirconium white, cerium oxide, zeolite molecular sieve, mesopore molecular sieve, mesoporous-microporous composite material, high molecular polymer, a kind of in the porous metal or and two kinds or two or more mixtures being formed by them.
7. method according to claim 5, be further characterized in that, component with photocatalytic activity loads on and makes loaded catalyst on the porous material, and employed carrier is gac, carbon molecular sieve, carbon nanotube, carbon fiber, Graphene, soccerballene, silicon oxide, aluminum oxide, silico-aluminate, phosphoric acid salt, carbonate, magnesium oxide, titanium oxide, calcium oxide, zirconium white, cerium oxide, zeolite molecular sieve, mesopore molecular sieve, mesoporous-microporous composite material, high molecular polymer, a kind of in the porous metal or and two kinds or two or more mixtures being formed by them.
8. method according to claim 6 is further characterized in that, described carrier is that sphere, bar shaped, trifolium shape, Herba Galii Bungei shape, sheet, tooth are spherical.
9. method according to claim 6 is further characterized in that, the preparation method adopts pickling process, coprecipitation method, sedimentation, sputtering method.
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