CN105603450A - Method for preparing hydrogen and sulfur through photoelectrocatalysis-chemical ring reaction coupling decomposition of hydrogen sulfide - Google Patents
Method for preparing hydrogen and sulfur through photoelectrocatalysis-chemical ring reaction coupling decomposition of hydrogen sulfide Download PDFInfo
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- CN105603450A CN105603450A CN201410640210.7A CN201410640210A CN105603450A CN 105603450 A CN105603450 A CN 105603450A CN 201410640210 A CN201410640210 A CN 201410640210A CN 105603450 A CN105603450 A CN 105603450A
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Abstract
The present invention relates to a method for preparing hydrogen and sulfur through photoelectrocatalysis-chemical ring reaction coupling decomposition of hydrogen sulfide. According to the present invention, the hydrogen sulfide conversion is performed in two steps in two reactors, wherein the first step is performed in a photoelectrocatalysis reaction pool, proton is reduced through photoelectrocatalysis or electrocatalysis to produce hydrogen while the oxidation-reduction pair oxidation state is obtained on the anode, and the oxidation state electrolyte containing the oxidation-reduction pair is pumped to a hydrogen sulfide absorption tower through a pump, and the second step is performed in the hydrogen sulfide absorption tower, the oxidation-reduction pair reacts with the hydrogen sulfide to obtain elemental sulfur, hydrogen ions and the oxidation-reduction pair reduction state, the hydrogen ions and the oxidation-reduction pair reduction state are injected into the photoelectrocatalysis reaction pool so as to participate into the first step process, and the elemental sulfur can be separated and recovered; and the provided approach can be used for production of hydrogen and sulfur through decomposition of hydrogen sulfide.
Description
Technical field
The present invention relates to the method that hydrogen sulfide transforms, be specifically related to a kind of optical, electrical catalysis-chemistry ring reaction coupling pointSeparate the method for hydrogen sulfide hydrogen manufacturing and sulphur.
Background technology
Hydrogen sulfide is a kind of hypertoxic pernicious gas, is present in a large number coal bed gas, in shale gas and natural gas, also simultaneouslyIt is the accessory substance in petroleum refining, natural gas processing and other chemical synthesis process. The Ke Lao of current industrial employingThis (Clauss) technique can generate water and sulphur by hydrogen sulfide partial oxidation, reclaims the sulphur in hydrogen sulfide, and hydrogen is by oxygenChange into water. This process has excessively discharged the chemical energy being stored in hydrogen sulfide, cannot accomplish the efficient utilization of hydrogen sulfideAnd Atom economy.
Summary of the invention
The present invention is the high-valued problem of the resource in order to solve hydrogen sulfide, and a kind of optical, electrical catalysis-chemistry is providedRing reacts the method for coupling decomposing hydrogen sulfide hydrogen manufacturing and sulphur, has both solved the processing problem of hydrogen sulfide, makes again it obtain heightValue utilizes, i.e. a kind of technology turning waste into wealth.
The method of the reaction coupling decomposing hydrogen sulfide hydrogen manufacturing of a kind of optical, electrical catalysis of the present invention-chemistry ring and sulphur in two stepsCarry out, the first step, in photoelectrocatalysis reaction tank, is produced hydrogen by photoelectrocatalysis or electrical catalyze reduction proton, simultaneously at sunExtremely, obtain the oxidation state of oxidation-reduction pair, the electrolyte that contains the right oxidation state of electricity is pumped delivers to hydrogen sulfide suctionReceive tower, second step reacted with hydrogen sulfide by oxidation-reduction pair at hydrogen sulfide absorption tower obtain elementary sulfur, hydrogen ion andThe reduction-state of oxidation-reduction pair, the reduction-state of hydrogen ion and oxidation-reduction pair is injected in photoelectrocatalysis reaction tankParticipate in first step process, the separable recovery of elementary sulfur.
Technical scheme of the present invention is:
In a device being made up of two reactors, react, two reactors are respectively photoelectrocatalysis reaction tankWith hydrogen sulfide absorption tower, between two reactors, be provided with transmission electrolyte pump;
Photoelectrocatalysis reaction tank is a reactor of being separated by barrier film, barrier film by reactor be separated into left and right two mutually notThe chamber being communicated with;
Hydrogen sulfide absorption tower is a reactor of being separated by sieve plate, with the sieve plate of through hole, reactor is separated into up and downTwo chambers, or it also can use industrial mature hydrogen sulfide absorption tower;
The electrolyte of photoelectrocatalysis reaction tank is pumped to hydrogen sulfide absorption tower bottom by pump, the electricity in hydrogen sulfide absorption towerSeparate after liquid reacts with hydrogen sulfide and be transmitted back in photoelectrocatalysis reaction tank by hydrogen sulfide absorption tower top.
Photoelectrocatalysis reaction tank comprises two reaction chambers;
One of them is equipped with the anode chamber of anode for its inside, and second is equipped with the cathode cavity of negative electrode for its insideChamber;
Cathode chamber is separated mutually by barrier film and anode chamber;
In two each and every one reaction chambers, be all added with electrolyte, anode and negative electrode be all or part of electrolyte that is placed in allIn; Anode and negative electrode are electrically connected by wire through dc source;
The sieve plate of hydrogen sulfide absorption tower is used for isolating elementary sulfur, is added with the electrolyte identical with anode chamber in it,And pass into hydrogen sulfide gas in bottom;
Described negative electrode is photocathode or conventional cathode, and the first step is in photoelectrocatalysis reaction tank, by photoelectrocatalysis or electricityCatalytic reduction proton produces hydrogen, obtains the oxidation state of oxidation-reduction pair simultaneously on anode, contains the right oxidation state of electricityElectrolyte be pumped and deliver to hydrogen sulfide absorption tower;
Second step is reacted with hydrogen sulfide and is obtained elementary sulfur, hydrogen ion and oxygen by oxidation-reduction pair at hydrogen sulfide absorption towerChange the right reduction-state of reduction electricity, the reduction-state of hydrogen ion and oxidation-reduction pair is injected into photoelectrocatalysis reaction tank internal referenceWith first step process, the separable recovery of elementary sulfur.
Time, is area load MoS very2P-type semiconductor, the semi-conductive material of P-type is Si, CdSe, CdTe,CuInxGa1-xSe2Or CuInxGa1-xS2；
Conventional cathode is area load MoS2Base metal, carbon electrode or electro-conductive glass.
Anode is carbon electrode, electro-conductive glass or base metal electrode.
Metal is Ti, Cu or Fe, and carbon electrode is carbon paper or graphite, and electro-conductive glass is FTO or ITO.
The voltage that dc source applies between anode and negative electrode is 0-10 volt, the energy providing can be sunshine orArtificial light sources or electric energy.
When the voltage that dc source applies between anode and negative electrode is 0 volt, its negative electrode adopting is photocathode, providesEnergy can be sunshine or artificial light sources.
Electrolyte is the aqueous solution or methanol solution, wherein contains Na+、K+、Li+And H+In one or moreHold cation, in electrolyte, support that cation molar concentration scope is 1 × 10-3-10mol/L; Wherein also containCO3 2-、Cl-、SO4 2-、PO4 3-、NO3 -And OH-In one or more support anion, in electrolyte, supportAnion molar concentration scope is 1 × 10-3-10mol/L; Wherein only contain H+During as support cation, supportAnion can not be CO3 2-Or only contain OH-; Wherein only contain OH-During as support anion, support cation notCan be only H+；
In electrolyte component in anode chamber and hydrogen sulfide absorption tower, also contain Fe (CN)6 3-/Fe(CN)6 4-，Fe3+/Fe2+，I3 -/I-，(SCN)2/SCN-，Ce4+/Ce3+，Co(bpy)3 3+/Co(bpy)3 2+，(SeCN)2/SeCN-InOne or more oxidation-reduction pairs, the molar concentration of oxidation-reduction pair is 1 × 10-5-10mol/L；
Preferred oxidation-reduction pair is Fe (CN)6 3-/Fe(CN)6 4-，Fe3+/Fe2+，I3 -/I-，(SCN)2/SCN-；
Pass into hydrogen sulfide gas in hydrogen sulfide absorption tower.
Photoelectrocatalysis reaction tank inner septum is nafion barrier film or quartz sand sieve plate, and hole is 0.01-500 micron;
In hydrogen sulfide absorption tower, sieve plate is quartz sand sieve plate, and hole is 10-500 micron.
Photocathode of the present invention is mainly load MoS2P-type semiconductor, as Si, CdSe, CdTe, CuInxGa1-xSe2Or CuInxGa1-xS2. Negative electrode of the present invention is load MoS2Metal, carbon electrode or electro-conductive glass, as Ti, Cu,Fe, carbon paper, graphite, FTO, ITO, anode of the present invention is base metal, as Ti, Cu, Fe. The present inventionOxidation-reduction pair be Fe (CN)6 3-/Fe(CN)6 4-，Fe3+/Fe2+，I3 -/I-，(SCN)2/SCN-，Ce4+/Ce3+，Co(bpy)3 3+/Co(bpy)3 2+，(SeCN)2/SeCN-, in one or more oxidation-reduction pairs.
The device of the reaction coupling decomposing hydrogen sulfide hydrogen manufacturing of a kind of optical, electrical catalysis of the present invention-chemistry ring and sulphur is by photoelectricityCatalytic reaction pond and hydrogen sulfide absorption tower composition. Wherein photoelectrocatalysis reaction tank is by cathode chamber and anode chamber groupBecome.
Brief description of the drawings
The schematic diagram of Fig. 1 photoelectrocatalysis-chemistry ring reaction coupling decomposing hydrogen sulfide; (1. photo electrocatalysis reactor; 2.Hydrogen sulfide absorption tower; 3. pump; 4. negative electrode; 5. anode; 6. barrier film; 7. sieve plate; 8. hydrogen is collected;9. elementary sulfur is collected; 10. hydrogen sulfide passes into; 11. light sources).
Detailed description of the invention
In order to further illustrate the present invention, enumerate following embodiment.
Embodiment mono-:
Be followed successively by from left to right photoelectrocatalysis reaction tank and hydrogen sulfide absorption tower (referring to Fig. 1). Photoelectrocatalysis reactionBetween pond inner cathode chamber and anode chamber, separate with nafion barrier film, in hydrogen sulfide absorption tower, have quartz sand sieve plate.In cathode chamber, add the K of 0.2mol/L2SO4The aqueous solution. In anode chamber and hydrogen sulfide absorption tower, all addEnter containing K4Fe(CN)6And K2SO4Be respectively the aqueous solution of 0.2mol/L and 0.25mol/L. To be of a size of 2cm × 2The load MoS of cm2P-type CdS semiconductor e be placed in cathode chamber, will be of a size of the FTO of 2cm × 2cmBe placed in anode chamber as anode, additional constant pressure source connects negative electrode and anode by wire, and ammeter is connected into electricityLu Zhong. This reacts light source used is 300W xenon lamp, and constant pressure source applies 0.4V DC voltage, and hydrogen sulfide passes intoGas flow rate is 1.0ml/min, and purity is greater than 99.9%. Apply after voltage, reaction system electric current is 0mA.Open after light source reaction system generation current 110mA. On photocathode, produce a large amount of bubbles, utilize drainage to receiveCollection. The color of anodic dissolution is deepened gradually, has faint yellow Precipitation in hydrogen sulfide absorption tower. A whole set of course of reactionHighly stable, reaction is carried out stopping illumination and applied voltage input after 10h, and hydrogen generation speed is 45ml/h,Precipitum in hydrogen sulfide absorption tower is collected, and centrifugation goes out elementary sulfur, and 0.64g weighs after being dried. WholeCourse of reaction passes into hydrogen sulfide 26.8mmol, obtains hydrogen 20.1mmol, elementary sulfur 20mmol, hydrogen sulfideConversion ratio is 75%.
Embodiment bis-: be with embodiment mono-difference:
In anode chamber and hydrogen sulfide absorption tower, all add (the NO containing Fe3)2And K2SO4Be respectively 0.2mol/L andThe aqueous solution of 0.25mol/L. Hydrogen sulfide conversion ratio is 72%.
Embodiment tri-: be with embodiment mono-difference:
In anode chamber and hydrogen sulfide absorption tower, all add containing KI and K2SO4Be respectively 0.2mol/L and 0.25The aqueous solution of mol/L. Hydrogen sulfide conversion ratio is 70%.
Embodiment tetra-: be with embodiment mono-difference:
In anode chamber and hydrogen sulfide absorption tower, all add containing KSCN and K2SO4Be respectively 0.2mol/L and 0.25The aqueous solution of mol/L. Hydrogen sulfide conversion ratio is 65%.
Embodiment five: be with embodiment mono-difference:
In anode chamber and hydrogen sulfide chamber, add (the NO containing Ce3)3And K2SO4Be respectively 0.2mol/L and 0.25The aqueous solution of mol/L. Hydrogen sulfide conversion ratio is 36%.
Embodiment six: be with embodiment mono-difference:
In anode chamber and hydrogen sulfide absorption tower, all add containing Co (bpy)3Cl2And K2SO4Be respectively 0.2mol/LThe aqueous solution with 0.25mol/L. Hydrogen sulfide conversion ratio is 48%.
Embodiment seven: be with embodiment mono-difference:
In anode chamber and hydrogen sulfide absorption tower, all add containing KSeCN and K2SO4Be respectively 0.2mol/L and 0.25The aqueous solution of mol/L. Hydrogen sulfide conversion ratio is 35%.
Embodiment eight: be with embodiment mono-difference:
Use is of a size of the load MoS of 2cm × 2cm2Ti as negative electrode, do not use light source, directly apply voltage1.5V, hydrogen sulfide conversion ratio is 40%.
Embodiment nine: be with embodiment mono-difference:
Use is of a size of the load MoS of 2cm × 2cm2CuGaS2As negative electrode, only adopt 300W xenon lamp to irradiate,Do not apply external voltage, hydrogen sulfide conversion ratio is 22%.
It will be readily appreciated by those skilled in the art that the thought that does not depart from disclosed materials and methods in above-mentioned descriptionUnder condition, can the present invention be combined or be changed, think that this change comprises within the scope of the invention. Therefore,Above, specifically described special embodiment is only illustrative, and does not limit the scope of the invention, by additional powerProfit requires and its any and whole equivalent way provide complete scope of the present invention.
Claims (9)
1. the method for the reaction coupling decomposing hydrogen sulfide hydrogen manufacturing of optical, electrical catalysis-chemistry ring and sulphur, is characterized in that:
In a device being made up of two reactors, react, two reactors are respectively photoelectrocatalysis reaction tankWith hydrogen sulfide absorption tower, between two reactors, be provided with transmission electrolyte pump;
Photoelectrocatalysis reaction tank is a reactor of being separated by barrier film, barrier film by reactor be separated into left and right two mutually notThe chamber being communicated with;
Hydrogen sulfide absorption tower is a reactor of being separated by sieve plate, with the sieve plate of through hole, reactor is separated into up and downTwo chambers, or it also can use industrial mature hydrogen sulfide absorption tower;
The electrolyte of photoelectrocatalysis reaction tank is pumped to hydrogen sulfide absorption tower bottom by pump, the electricity in hydrogen sulfide absorption towerSeparate after liquid reacts with hydrogen sulfide and be transmitted back in photoelectrocatalysis reaction tank by hydrogen sulfide absorption tower top.
2. method according to claim 1, is characterized in that:
Photoelectrocatalysis reaction tank comprises two reaction chambers;
One of them is equipped with the anode chamber of anode for its inside, and second is equipped with the cathode cavity of negative electrode for its insideChamber;
Cathode chamber is separated mutually by barrier film and anode chamber;
In two each and every one reaction chambers, be all added with electrolyte, anode and negative electrode be all or part of electrolyte that is placed in allIn; Anode and negative electrode are electrically connected by wire through dc source;
The sieve plate of hydrogen sulfide absorption tower is used for isolating elementary sulfur, is added with the electrolyte identical with anode chamber in it,And pass into hydrogen sulfide gas in bottom;
Described negative electrode is photocathode or conventional cathode, and the first step is in photoelectrocatalysis reaction tank, by photoelectrocatalysis or electricityCatalytic reduction proton produces hydrogen, obtains the oxidation state of oxidation-reduction pair simultaneously on anode, contains the right oxidation state of electricityElectrolyte be pumped and deliver to hydrogen sulfide absorption tower;
Second step is reacted with hydrogen sulfide and is obtained elementary sulfur, hydrogen ion and oxygen by oxidation-reduction pair at hydrogen sulfide absorption towerChange the right reduction-state of reduction electricity, the reduction-state of hydrogen ion and oxidation-reduction pair is injected into photoelectrocatalysis reaction tank internal referenceWith first step process, the separable recovery of elementary sulfur.
3. method according to claim 2, is characterized in that:
Time, is area load MoS very2P-type semiconductor, the semi-conductive material of P-type is Si, CdSe, CdTe,CuInxGa1-xSe2Or CuInxGa1-xS2；
Conventional cathode is area load MoS2Base metal, carbon electrode or electro-conductive glass.
4. according to the method described in claim 2, it is characterized in that: anode be carbon electrode, electro-conductive glass orBase metal electrode.
5. according to the method described in claim 3 or 4, it is characterized in that:
Metal is Ti, Cu or Fe, and carbon electrode is carbon paper or graphite, and electro-conductive glass is FTO or ITO.
6. according to the method described in claim 2, it is characterized in that:
The voltage that dc source applies between anode and negative electrode is 0-10 volt, the energy providing can be sunshine orArtificial light sources or electric energy.
7. according to the method described in claim 2 or 6, it is characterized in that:
When the voltage that dc source applies between anode and negative electrode is 0 volt, its negative electrode adopting is photocathode, providesEnergy can be sunshine or artificial light sources.
8. according to the method described in claim 2, it is characterized in that:
Electrolyte is the aqueous solution or methanol solution, wherein contains Na+、K+、Li+And H+In one or moreHold cation, in electrolyte, support that cation molar concentration scope is 1 × 10-3-10mol/L; Wherein also containCO3 2-、Cl-、SO4 2-、PO4 3-、NO3 -And OH-In one or more support anion, in electrolyte, supportAnion molar concentration scope is 1 × 10-3-10mol/L; Wherein only contain H+During as support cation, supportAnion can not be CO3 2-Or only contain OH-; Wherein only contain OH-During as support anion, support cation notCan be only H+；
In electrolyte component in anode chamber and hydrogen sulfide absorption tower, also contain Fe (CN)6 3-/Fe(CN)6 4-，Fe3+/Fe2+，I3 -/I-，(SCN)2/SCN-，Ce4+/Ce3+，Co(bpy)3 3+/Co(bpy)3 2+，(SeCN)2/SeCN-InOne or more oxidation-reduction pairs, the molar concentration of oxidation-reduction pair is 1 × 10-5-10mo1/L；
Preferred oxidation-reduction pair is Fe (CN)6 3-/Fe(CN)6 4-，Fe3+/Fe2+，I3 -/I-，(SCN)2/SCN-；
Pass into hydrogen sulfide gas in hydrogen sulfide absorption tower.
9. according to the method described in claim 1, it is characterized in that:
Photoelectrocatalysis reaction tank inner septum is nafion barrier film or quartz sand sieve plate, and hole is 0.01-500 micron;
In hydrogen sulfide absorption tower, sieve plate is quartz sand sieve plate, and hole is 10-500 micron.
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| CN107815698A (en) * | 2016-09-12 | 2018-03-20 | 中国科学院大连化学物理研究所 | A kind of method of the electrochemical decomposition hydrogen sulfide of mediator auxiliary |
| CN108529714A (en) * | 2018-05-08 | 2018-09-14 | 中国科学技术大学苏州研究院 | The method of optical electro-chemistry reaction tank and its Treatment of Hydrogen Sulfide Waste Gas and waste water |
| CN110607531A (en) * | 2018-06-14 | 2019-12-24 | 中国科学院大连化学物理研究所 | Cyclic electrochemical conversion treatment method and device for gas containing hydrogen sulfide and carbon dioxide |
| CN110923736A (en) * | 2019-10-23 | 2020-03-27 | 安徽中研理工仪器设备有限公司 | Photoelectrocatalysis chemical reaction electrolytic cell device |
| CN111232921A (en) * | 2018-11-29 | 2020-06-05 | 中国科学院大连化学物理研究所 | Method and device for preparing hydrogen and sulfur by decomposing hydrogen sulfide assisted by flow battery |
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN107815698A (en) * | 2016-09-12 | 2018-03-20 | 中国科学院大连化学物理研究所 | A kind of method of the electrochemical decomposition hydrogen sulfide of mediator auxiliary |
| CN107815698B (en) * | 2016-09-12 | 2019-11-26 | 中国科学院大连化学物理研究所 | A kind of method of the electrochemical decomposition hydrogen sulfide of mediator auxiliary |
| CN108529714A (en) * | 2018-05-08 | 2018-09-14 | 中国科学技术大学苏州研究院 | The method of optical electro-chemistry reaction tank and its Treatment of Hydrogen Sulfide Waste Gas and waste water |
| CN110607531A (en) * | 2018-06-14 | 2019-12-24 | 中国科学院大连化学物理研究所 | Cyclic electrochemical conversion treatment method and device for gas containing hydrogen sulfide and carbon dioxide |
| CN111232921A (en) * | 2018-11-29 | 2020-06-05 | 中国科学院大连化学物理研究所 | Method and device for preparing hydrogen and sulfur by decomposing hydrogen sulfide assisted by flow battery |
| CN111232921B (en) * | 2018-11-29 | 2023-04-07 | 中国科学院大连化学物理研究所 | Method and device for preparing hydrogen and sulfur by decomposing hydrogen sulfide with assistance of flow battery |
| CN110923736A (en) * | 2019-10-23 | 2020-03-27 | 安徽中研理工仪器设备有限公司 | Photoelectrocatalysis chemical reaction electrolytic cell device |
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Application publication date: 20160525 |