CN101590410B - Catalyst for decomposing hydrogen sulfide by photocatalysis and preparation method of hydrogen and liquid sulfur by employing same - Google Patents

Catalyst for decomposing hydrogen sulfide by photocatalysis and preparation method of hydrogen and liquid sulfur by employing same Download PDF

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CN101590410B
CN101590410B CN2008101130346A CN200810113034A CN101590410B CN 101590410 B CN101590410 B CN 101590410B CN 2008101130346 A CN2008101130346 A CN 2008101130346A CN 200810113034 A CN200810113034 A CN 200810113034A CN 101590410 B CN101590410 B CN 101590410B
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catalyst
hydrogen sulfide
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percentage composition
hydrogen
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CN101590410A (en
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王宏伟
闻学兵
蒲延芳
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Beijing Haixin Energy Technology Co ltd
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Beijing SJ Environmental Protection and New Material Co Ltd
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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
    • 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
    • Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
    • Y02P20/00—Technologies relating to chemical industry
    • Y02P20/50—Improvements relating to the production of bulk chemicals
    • Y02P20/584—Recycling of catalysts

Abstract

The invention relates to a catalyst for decomposing hydrogen sulfide by photocatalysis and a preparation method of hydrogen and liquid sulfur by employing same. The catalyst comprises a carrier, active component and assistant and has the characteristics that the carrier is one or more selected from vanadate, niobate and tantalate, the active component is one or more selected from alkali metal hydroxide, alkaline earth metal hydroxide, alkali metal nonmetal oxysalt, alkali metal nonoxysalt, alkaline earth metal nonmetal oxysalt and alkaline earth metal nonoxysalt and the assistant is lanthanide oxide or VIII group oxide. The catalyst of the invention can be used for preparing hydrogen and liquid sulfur so that the produced sulfur is easy to be separated from the catalyst, the catalyst can be recycled and the sulfur contained in hydrogen sulfide can be fully recycled, thus realizing the comprehensive utilization of hydrogen sulfide.

Description

A kind of catalyst of photocatalysis Decomposition hydrogen sulfide and utilize the method for this Preparation of Catalyst hydrogen and liquid sulfur
Technical field
The present invention relates to a kind of catalyst of photocatalysis Decomposition hydrogen sulfide and utilize this catalyst decomposes hydrogen sulfide to prepare the method for hydrogen and liquid sulfur, belong to catalysis technical field.
Background technology
Hydrogen sulfide directly discharges not only contaminated environment as the accessory substance in the petroleum refining process with it, and has caused the waste of available resources, so the processing of hydrogen sulfide people's attention extremely always.At present, for the improvement of hydrogen sulfide, what the big-and-middle-sized oil plant of China adopted usually is traditional Crouse (Claus) method, and to reclaim the sulphur in the hydrogen sulfide, hydrogen has then generated water in oxidizing process.Consider that from the comprehensive utilization aspect of resource it is the waste to the hydrogen resource that traditional hydrogen sulfide reclaims technology.On the one hand, hydrogen can provide the energy to the mankind as a kind of fuel of cleanliness without any pollution; On the other hand, if can above-mentioned hydrogen be collected, it then can fully be applied in the hydroprocessing technique of petroleum refining, thereby has realized the comprehensive utilization of hydrogen sulfide.
This shows, simple, economical, be converted into hydrogen to hydrogen in the hydrogen sulfide and sulphur with elemental sulfur and separate and collect and just seem extremely important effectively.At present, technological means commonly used comprises high temperature direct heat decomposition method, catalysis thermal decomposition method, photocatalysis Decomposition method, electrochemical process and super-thermal insulating burning technology etc. in the prior art.Wherein, the photocatalysis Decomposition method is to utilize abundant and cheap solar energy as energy source on the one hand, than other method its more can energy savings (for example electric energy etc.), environmentally friendly pollution-free; On the other hand, photochemical catalyst can catalytic decomposition hydrogen sulfide under the initiation of light, and reaction condition relaxes, and does not need high-temperature high-pressure apparatus, and the technology cost is low, has therefore received those skilled in the art's concern.
But the method for present photocatalysis Decomposition hydrogen sulfide of the prior art is only paid attention to for Preparation of Hydrogen and collection, and does not give enough attention to sulphur contained in the hydrogen sulfide, it is not recycled fully.Thereby disclose a kind of method of using the hydrogen sulfide that is dissolved in the radiation of visible light akaline liquid medium to prepare hydrogen such as Chinese patent document CN1005102B, do not mentioned recycling in this method institute's sulfur-bearing in the hydrogen sulfide.Though paid attention to recovery and utilization to elemental sulfur in the other document, the technology more complicated is separated relatively difficulty, and for example, it is light source that U.S. Pat 6248218 adopts the visible light of 450-500nm, with Pt-CdS, ZnS, ZnFe 2O 4, In 2S 3Be catalyst, utilize polysulfide to be circulation fluid, under alkali condition, absorb H through regulating the pH value 2S is through photocatalysis Decomposition H 2S generates hydrogen and solid-state elemental sulfur, isolates elemental sulfur through the method for filtering then.
Summary of the invention
Technical problem to be solved by this invention is sulphur contained in the hydrogen sulfide not to be recycled fully in the process of photocatalysis Decomposition hydrogen sulfide in the prior art; The technology more complicated of recovery sulphur, separation be the defective of difficulty relatively, and then a kind of catalyst of photocatalysis Decomposition hydrogen sulfide is provided and utilizes this catalyst decomposes hydrogen sulfide to prepare the method for the hydrogen and the liquid sulfur of easy and catalyst separation.
For solving the problems of the technologies described above, the method that the invention provides a kind of catalyst of photocatalysis Decomposition hydrogen sulfide and utilize this Preparation of Catalyst hydrogen and liquid sulfur, it comprises as follows:
A kind of catalyst of photocatalysis Decomposition hydrogen sulfide; Said catalyst is made up of carrier, active component and auxiliary agent; Said carrier is one or more in vanadate, niobates and the tantalates; Said active component is one or more in the non-oxysalt of nonmetal oxyacid hydrochlorate and alkaline-earth metal of alkali metal hydroxide, alkaline earth metal hydroxide, alkali-metal nonmetal oxyacid hydrochlorate, alkali-metal non-oxysalt, alkaline-earth metal, and said auxiliary agent is the metal oxide of group of the lanthanides or VIII family.
The quality percentage composition of said carrier is 50-85%; The quality percentage composition of said active component is 10-45%; The quality percentage composition of said auxiliary agent is 5-20%.
Said active component is hydroxide, nonmetal oxyacid hydrochlorate or the non-oxysalt of lithium, sodium, potassium, rubidium, beryllium, magnesium, calcium or strontium, and the quality percentage composition is 15-40%.
Said carrier quality percentage composition is 60-70%.
Said auxiliary agent is the metal oxide of lanthanum, cerium, praseodymium, samarium, terbium, erbium, iron, cobalt, nickel, ruthenium, osmium or rhodium, and the quality percentage composition is 10-15%.
The quality percentage composition of said active component is 25-35%.
A kind ofly utilize described catalyst decomposes hydrogen sulfide to prepare the method for hydrogen and liquid sulfur, it comprises the steps:
(a) with hydrogen sulfide gas through being mounted with the said reactor that is used for the catalyst of photocatalysis Decomposition hydrogen sulfide;
(b) utilize wavelength to penetrate the catalyst of said photocatalysis Decomposition hydrogen sulfide for the illumination of 400-600nm, reaction temperature is 120-270 ℃, and the gaseous state air speed is 15-550h -1
Said reaction temperature is 170-220 ℃, and the gaseous state air speed is 150-260h -1
Collect the liquid sulfur that generates from the bottom of reactor, collect the hydrogen that generates from the top of reactor.
Technique scheme of the present invention is compared prior art and is had the following advantages:
(1) catalyst of photocatalysis Decomposition hydrogen sulfide of the present invention absorbs photon under the effect of the light of 400-600nm; It is right to form electronics-hole; Then separation of charge and transfer to the surface reactivity point on, carry out chemical reaction on the surface, thereby separate out hydrogen and elemental sulfur; Therefore decomposing hydrogen sulfide gas obtains hydrogen and elemental sulfur effectively, and the hydrogen of generation can be used as fuel or is applied in the hydrogenation technique, and the sulphur of generation can be recycled, thereby has realized the comprehensive utilization of hydrogen sulfide; Preferred carrier is a tantalates, and preferred active ingredient is hydroxide, nonmetal oxyacid hydrochlorate and the non-oxysalt of sodium and magnesium, makes that like this activity of such catalysts is higher; Add auxiliary agent and can prevent that light induced electron-hole from combining taking place again; Reduce photoelectron-hole to arriving the distance of catalyst surface active point; Thereby the raising activity of such catalysts, preferred auxiliary agent is oxide and the La series metal oxide of Ni, makes activity of such catalysts higher.
(2) using the liquid sulfur that catalyst decomposes hydrogen sulfide of the present invention obtains can effectively separate with catalyst, and its recycling rate is very high, has fully realized the comprehensive utilization to hydrogen sulfide; And do not need to be provided with separately separating technology; Automatic and the catalyst separation of liquid sulfur; Avoid decomposing hydrogen sulfide in the prior art to generate that solid-state sulphur can't effectively separate with catalyst and problem that the catalyst that causes can't recycle, improved the utilization rate of catalyst.
(3) the photocatalysis Decomposition hydrogen sulfide of the present invention method reaction condition for preparing hydrogen and liquid sulfur is easy to realize that it is less demanding to reaction temperature, and reaction control easily, energy savings.
(4) through test shows, it is higher to the conversion ratio of hydrogen sulfide that photocatalysis Decomposition hydrogen sulfide of the present invention prepares the method for hydrogen and liquid sulfur, can be up to 99.90%.
The specific embodiment
Preparation of catalysts
Embodiment 1
With 140g Na 2Ta 2O 7With 44g Ba (OH) 2Mix at normal temperatures and stir, mixing time 6h, oven dry 6h is subsequent use in 110 ℃ of baking ovens afterwards; With NiO quality percentage composition in the finished catalyst is 7.5% calculating, gets 0.2027mol Ni (NO 3) 2Be mixed with solution, with above-mentioned biased sample dipping, 6h is dried in the dipping back in 110 ℃ of baking ovens, obtain reacting required catalyst behind 650 ℃ of roasting 4h.Catalyst is ground to 40 order particles uses catalyst as reaction.The quality percentage composition of carrier is 70.3% described in the final gained catalyst, and the quality percentage composition of active component is 22.1%, and the quality percentage composition of auxiliary agent is 7.5%.
Embodiment 2
With 50g NH 4VO 3Mix stirring at normal temperatures with 45g LiOH, mixing time 6h, oven dry 6h is subsequent use in 110 ℃ of baking ovens afterwards; With Fe in the finished catalyst 2O 3The quality percentage composition is 5% calculating, gets 0.0625mol Fe (OH) 3Be mixed with solution, with above-mentioned biased sample dipping, 6h is dried in the dipping back in 110 ℃ of baking ovens, obtain reacting required catalyst behind 650 ℃ of roasting 4h.Catalyst is ground to 80 order particles uses catalyst as reaction.The quality percentage composition of carrier is 50% described in the final gained catalyst, and the quality percentage composition of active component is 45%, and the quality percentage composition of auxiliary agent is 5%.
Embodiment 3
With 85g NaNbO 3And 10gNa 2CO 3Mix at normal temperatures and stir, mixing time 6h, oven dry 6h is subsequent use in 110 ℃ of baking ovens afterwards; With Co in the finished catalyst 3O 4The quality percentage is 5% calculating, gets 0.0622mol Co (NO 3) 2Be mixed with solution, with above-mentioned biased sample dipping, 6h is dried in the dipping back in 110 ℃ of baking ovens, obtain reacting required catalyst behind 650 ℃ of roasting 4h.Catalyst is ground to 60 order particles uses catalyst as reaction.The quality percentage composition of carrier is 85% described in the final gained catalyst, and the quality percentage composition of active component is 10%, and the quality percentage composition of auxiliary agent is 5%.
Embodiment 4
With 65g K 3TaO 4Mix stirring at normal temperatures with 15gKCl, mixing time 6h, oven dry 6h is subsequent use in 110 ℃ of baking ovens afterwards; With NiO quality percentage in the finished catalyst is 20% calculating, gets 0.2667mol Ni (NO 3) 2Be mixed with solution, with above-mentioned biased sample dipping, 6h is dried in the dipping back in 110 ℃ of baking ovens, obtain reacting required catalyst behind 650 ℃ of roasting 4h.Catalyst is ground to 50 order particles uses catalyst as reaction.The quality percentage composition of carrier is 65% described in the final gained catalyst, and the quality percentage composition of active component is 15%, and the quality percentage composition of auxiliary agent is 20%.
Embodiment 5
With 50g Na 4V 2O 7Mix stirring at normal temperatures with 40gRbCl, mixing time 6h, oven dry 6h is subsequent use in 110 ℃ of baking ovens afterwards; With La in the finished catalyst 2O 3The quality percentage is 10% calculating, gets 0.0613mol La (OH) 3Be mixed with solution, with above-mentioned biased sample dipping, 6h is dried in the dipping back in 110 ℃ of baking ovens, obtain reacting required catalyst behind 650 ℃ of roasting 4h.Catalyst is ground to 70 order particles uses catalyst as reaction.The quality percentage composition of carrier is 50% described in the final gained catalyst, and the quality percentage composition of active component is 40%, and the quality percentage composition of auxiliary agent is 10%.
Embodiment 6
With 70g Na 4V 2O 7And 15gMgSO 4Mix at normal temperatures and stir, mixing time 6h, oven dry 6h is subsequent use in 110 ℃ of baking ovens afterwards; With CeO in the finished catalyst 2The quality percentage is 15% calculating, gets 0.0872mol Ce (NO 3) 3Be mixed with solution, with above-mentioned biased sample dipping, 6h is dried in the dipping back in 110 ℃ of baking ovens, obtain reacting required catalyst behind 650 ℃ of roasting 4h.Catalyst is ground to 70 order particles uses catalyst as reaction.The quality percentage composition of carrier is 70% described in the final gained catalyst, and the quality percentage composition of active component is 15%, and the quality percentage composition of auxiliary agent is 15%.
Embodiment 7
With 75g K 3TaO 4And 18gCaSO 4Mix at normal temperatures and stir, mixing time 6h, oven dry 6h is subsequent use in 110 ℃ of baking ovens afterwards; With Eu in the finished catalyst 2O 3The quality percentage is 17% calculating, gets 0.0966mol Eu (NO 3) 3Be mixed with solution, with above-mentioned biased sample dipping, 6h is dried in the dipping back in 110 ℃ of baking ovens, obtain reacting required catalyst behind 650 ℃ of roasting 4h.Catalyst is ground to 70 order particles uses catalyst as reaction.The quality percentage composition of carrier is 75% described in the final gained catalyst, and the quality percentage composition of active component is 18%, and the quality percentage composition of auxiliary agent is 17%.
Embodiment 8
With 40gNH 4VO 3, 40gNaNbO 3And 12gBeCl 2Mix at normal temperatures and stir, mixing time 6h, oven dry 6h is subsequent use in 110 ℃ of baking ovens afterwards; With Tb in the finished catalyst 4O 7The quality percentage composition is 8% calculating, gets 0.0428mol Tb (NO 3) 3Be mixed with solution, with above-mentioned biased sample dipping, 6h is dried in the dipping back in 110 ℃ of baking ovens, obtain reacting required catalyst behind 650 ℃ of roasting 4h.Catalyst is ground to 70 order particles uses catalyst as reaction.The quality percentage composition of carrier is 80% described in the final gained catalyst, and the quality percentage composition of active component is 12%, and the quality percentage composition of auxiliary agent is 8%.
Embodiment 9
With 20gNa 4V 2O 7, 20gNa 2Ta 2O 7, 20gNaNbO 3, 15gK 2SO 4Mix at normal temperatures and stir, mixing time 6h, oven dry 6h is subsequent use in 110 ℃ of baking ovens afterwards; With Er in the finished catalyst 2O 3The quality percentage composition is 25% calculating, gets 0.1309mol Er (NO 3) 3Be mixed with solution, with above-mentioned biased sample dipping, 6h is dried in the dipping back in 110 ℃ of baking ovens, obtain reacting required catalyst behind 650 ℃ of roasting 4h.Catalyst is ground to 70 order particles uses catalyst as reaction.The quality percentage composition of carrier is 60% described in the final gained catalyst, and the quality percentage composition of active component is 25%, and the quality percentage composition of auxiliary agent is 15%.
The test of preparing hydrogen gas by decomposing hydrogen sulfide and liquid sulfur
Getting the catalyst 20g that the foregoing description 1-embodiment 9 makes respectively is loaded in 9 different fixed bed bioreactors; Feed hydrogen sulfide gas then respectively from the bottom of fixed bed reactors; Penetrate catalyst with the illumination of 400nm～600nm respectively under the normal pressure, reaction temperature, air speed, time, inlet amount and reaction result are as shown in table 1 below.After reaction finished, the hydrogen of generation flowed out from the top of fixed bed reactors, can be used as fuel and perhaps was applied in the hydrogenation technique; The liquid sulfur that generates flows out from the bottom of fixed bed reactors, make sulphur and catalyst separate than be easier to, avoid reaction to generate solid-state sulphur and cause catalyst not recycle, practiced thrift catalyst, also realized the comprehensive utilization of hydrogen sulfide; And the method reaction condition that catalytic decomposition hydrogen sulfide prepares sulphur and hydrogen is realized relatively easily; Reaction temperature is relatively low, makes the course of reaction ratio be easier to control, and conversion ratio is also than higher; Be up to 99.90%, the content of hydrogen sulfide is also relatively low in the reacted gas.
Figure S2008101130346D00071
Obviously, the foregoing description only be for explanation clearly done for example, and be not qualification to embodiment.For the those of ordinary skill in affiliated field, can also make other multi-form variation or change on the basis of the above description.Here need not also can't give exhaustive to all embodiments.And conspicuous variation of being extended out thus or change still are among the protection domain of claim of the present invention.

Claims (8)

1. the catalyst of a photocatalysis Decomposition hydrogen sulfide; Said catalyst is made up of carrier, active component and auxiliary agent; It is characterized in that; Said carrier is one or more in vanadate, niobates and the tantalates; Said active component is one or more in the non-oxysalt of nonmetal oxyacid hydrochlorate and alkaline-earth metal of alkali metal hydroxide, alkaline earth metal hydroxide, alkali-metal nonmetal oxyacid hydrochlorate, alkali-metal non-oxysalt, alkaline-earth metal, and said auxiliary agent is the metal oxide of group of the lanthanides or VIII family, and the quality percentage composition of said carrier is 50-85%; The quality percentage composition of said active component is 10-45%; The quality percentage composition of said auxiliary agent is 5-20%.
2. catalyst according to claim 1 is characterized in that, said active component is hydroxide, nonmetal oxyacid hydrochlorate or the non-oxysalt of lithium, sodium, potassium, rubidium, beryllium, magnesium, calcium or strontium, and the quality percentage composition is 15-40%.
3. catalyst according to claim 1 is characterized in that, said carrier quality percentage composition is 60-70%.
4. catalyst according to claim 1 is characterized in that, said auxiliary agent is the metal oxide of lanthanum, cerium, praseodymium, samarium, terbium, erbium, iron, cobalt, nickel, ruthenium, osmium or rhodium, and the quality percentage composition is 10-15%.
5. according to each described catalyst in the claim 1 to 4, it is characterized in that the quality percentage composition of said active component is 25-35%.
6. method of utilizing each described catalyst decomposes hydrogen sulfide in the claim 1 to 4 to prepare hydrogen and liquid sulfur, it comprises the steps:
(a) with hydrogen sulfide gas through being mounted with the said reactor that is used for the catalyst of photocatalysis Decomposition hydrogen sulfide;
(b) utilize wavelength to penetrate the catalyst of said photocatalysis Decomposition hydrogen sulfide for the illumination of 400-600nm, reaction temperature is 120-270 ℃, and the gaseous state air speed is 15-550h -1
7. method according to claim 6 is characterized in that, reaction temperature is 170-220 ℃, and the gaseous state air speed is 150-260h -1
8. according to claim 6 or 7 described methods, it is characterized in that, collect the liquid sulfur that generates, collect the hydrogen that generates from the top of reactor from the bottom of reactor.
CN2008101130346A 2008-05-27 2008-05-27 Catalyst for decomposing hydrogen sulfide by photocatalysis and preparation method of hydrogen and liquid sulfur by employing same Active CN101590410B (en)

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