CN103204467A - Device and method for continuously and steadily decomposing and making up hydrogen with hydrogen sulfide - Google Patents
Device and method for continuously and steadily decomposing and making up hydrogen with hydrogen sulfide Download PDFInfo
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- CN103204467A CN103204467A CN2013101441384A CN201310144138A CN103204467A CN 103204467 A CN103204467 A CN 103204467A CN 2013101441384 A CN2013101441384 A CN 2013101441384A CN 201310144138 A CN201310144138 A CN 201310144138A CN 103204467 A CN103204467 A CN 103204467A
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Abstract
The invention provides a device and a method for continuously and steadily decomposing and making up hydrogen with hydrogen sulfide, belonging to the technical field of hydrogen production and gas purification technologies. Hydrogen sulfide or hydrogen sulfide-containing gas is subjected to axially reverse rotary flow through a dielectric barrier discharge area by adopting a spiral mode, the hydrogen sulfide can be decomposed by high-energy electrons in the discharge area, and the sulfur generated from decomposition can be centrifugally separated in time, and leave away from the discharge area through controlling the temperature of the discharge area. The device and method have the advantages that under the atmospheric and non-catalytic conditions, the high-energy-efficiency decomposition of the hydrogen sulfide can be realized only through dielectric barrier discharge, the hydrogen and sulfur produced from decomposition can leave away from the discharge area in time, the reaction can be performed sustainably and stably, and the decomposition rate and the energy utilization rate of the hydrogen sulfide are high; the method is applicable to producing hydrogen through decomposing hydrogen sulfide-containing gas in natural gas, petroleum and coal chemical industry; and the method has no special requirements or limit on the source and composition of the gas, thereby having general applicability to producing hydrogen and elemental sulfur through decomposing the hydrogen sulfide.
Description
Technical field
The invention belongs to hydrogen manufacturing and gas purification technology field, relate to a kind of hydrogen sulfide that can make and under normal pressure and on-catalytic condition, be decomposed into hydrogen and elemental sulfur apparatus and method continually and steadily.
Technical background
H
2S extensively exists in the waste gas of industries such as oil and natural gas exploitation, petrochemical complex, Coal Chemical Industry, is the sour gas of a kind of severe toxicity, stench, need be with H from the requirement of environmental protection and corrosion aspect
2S carries out nuisanceless processing.Main employing Crouse (Claus) method is elemental sulfur and water with its partial oxidation at present, but Crouse (Claus) method has only reclaimed H
2Sulphur among the S, hydrogen have then generated water in oxidising process, cause the waste of hydrogen resource.
In common nonmetal hydride (water, methyl alcohol and hydrogen sulfide), the ionic dissociation energy of hydrogen sulfide is minimum, and therefore theoretically, it is the easiest that hydrogen is produced in the hydrogen sulfide thermolysis.But the hydrogen sulfide decomposition reaction is strong endothermic reaction, is subjected to the restriction of thermodynamic(al)equilibrium, and considerable transformation efficiency is only at high temperature just arranged.Such as, the transformation efficiency the when rate of decomposition of hydrogen sulfide only is 20%, 1200 ℃ in the time of 1000 ℃ is 38%(Slimane R.B., GasTIPS, and 2004,30-34).Electrochemistry and photocatalysis method also can be realized H
2Hydrogen and sulphur are produced in the S decomposition, but have the many or low shortcoming of reaction efficiency of operation steps.In order to break the chemical reaction equilibrium restriction, the investigator has adopted film reaction technology and nonequilibrium plasma technology etc., but the development and application of the mould material of high temperature resistant and anti-sulphur becomes the key that realizes utilizing the technological breakthrough of film reaction decomposing hydrogen sulfide.Utilize non-equilibrium plasma technology decomposing H
2S can and shrink in normal glow discharge, microwave discharge, corona discharge pulse and the dielectric barrier discharge etc. and realize in arc discharge, rotation glow discharge.H
2Energy consumption (the 3.7eV/H that required energy loss-rate methane steam reforming generates hydrogen is decomposed in the S arc discharge
2) high (J Appl Phys, 1998,84:1215 – 1221).H
2Required energy consumption also generates hydrogen than methane steam reforming energy consumption height (Plasma Chem Plasma Process, 1993,13:77 – 91) is decomposed in S rotation glow discharge.
Open source literature International journal of hydrogen energy, 2012,37:1335-1347. has reported a kind of H
2S shrinks the method that normal glow discharge is decomposed.Its technical characterictic is: when system pressure is 0.197 normal atmosphere, experimental temperature is between 2000-4000K the time, under optimal conditions, and H
2The energy consumption that S shrinks normal glow discharge is 2.35eV/H
2S, this system temperature height, pressure is low, severe reaction conditions.
Open source literature International journal o f hydrogen energy, 2012,37:10010-10019. has reported a kind of H
2The method that S decomposes.Its technical characterictic is: utilize the microwave plasma body technique at 2400K, and under the atmospheric pressure, H
2S almost can decompose fully, but the hydrogen after decomposing and sulphur at high temperature can be rapidly compound and generation H
2S, and still do not have corresponding quenching device so far.
Open source literature Chem Eng Sci, 2007,62:2216 – 2227. have reported a kind of corona discharge pulse decomposing H of utilizing
2The method of S.Its technical characterictic is: H
2The mixed gas of S and argon gas is 1.322 normal atmosphere at pressure, and under the room temperature, flow velocity is 1.18 * 10
-4SCMs
-1, H
2The S percentage composition is 16% o'clock, H under the corona discharge pulse
2The rate of decomposition of S is about 28%, and minimum decomposition energy consumption is 17eV/H
2S.
Open source literature Chem Eng Sci, 2009,64:4826 – 4834. have reported and have utilized the corona discharge pulse decomposing H
2The method of S.Its technical characterictic is: be 1.322 normal atmosphere at pressure, under the room temperature, flow velocity is 1.18 * 10
-4SCMs
-1, work as H
2The S percentage composition is 8%, and the mixed gas of argon gas and nitrogen is as filling under the gas H
2The transformation efficiency of S is about 33%, and energy consumption has dropped to 4.9eV/H
2S.But so low gas velocity, lower concentration and low-conversion are meaningless in industrial production.
Dielectric barrier discharge have can under atmospheric pressure work, large space discharge, can prevent from forming characteristics such as local spark or arc discharge in the discharge space, thereby have good industrial applications prospect.
Patent documentation CN102408095A(2012) reported a kind of dielectric barrier discharge H that utilizes
2The method that S decomposes.Its technical characterictic is: add photocatalyst in stainless steel wire and kaolin are respectively the line cartridge type dielectric impedance reactor of high voltage electrode and ground-electrode, realize H
2S decomposes preparation hydrogen and elemental sulfur, decomposes the sulphur deposition of generation in the beds downstream.
Open source literature International journal of hydrogen energy, 2012,37:1335-1347. has reported and has utilized the dielectric barrier discharge decomposing H
2The method of S.Its technical characterictic is: under 0.246 normal atmosphere and room temperature, and H
2When the S gas flow rate is 0.09l/min, realized H
2The rate of decomposition of S is 18.5%, and energy consumption is 12eV/H
2S decomposes the sulphur deposition of generation at inside reactor.
Open source literature Plasma Chemistry and Plasma Processing, 1992,12:275-285. has reported and has utilized the dielectric barrier discharge decomposing H
2The method of S.Its technical characterictic is: under atmospheric pressure, utilize dielectric barrier discharge in ozonizer with H
2S decomposes generation hydrogen and sulphur, and experimental temperature is from 443.16-833.16K, and total gas flow rate is 50-100cm
3/ min, H
2The S percentage composition is 20-100%, studies show that Ar can cut down the consumption of energy and voltage breakdown, but its energy consumption is still very high after adding Ar, decomposes energy consumption between 37-106eV/H
2S.
Open source literature International journal of hydrogen energy, 2012,37:2204-2209. has reported and has utilized the dielectric barrier discharge decomposing H
2The method of S.Its technical characterictic is: H
2The rate of decomposition of S gas and energy expenditure depend on service temperature, the residence time, discharge frequency and H
2The initial content of S gas studies show that H
2The rate of decomposition of S under low temperature is higher.
Open source literature Applied Energy, 2012,95:87 – 92. have reported and have utilized the dielectric barrier discharge decomposing H
2The method of S.Its technical characterictic is: at normal temperatures and pressures, utilize dielectric barrier discharge, and under The optimum reaction conditions, H in the unstripped gas
2The content of S be 25%(all the other be argon gas), when flow is 150mL/min, can realize H
2The rate of decomposition of S is 16%, and energy consumption is 1.6eV/H
2S studies show that H under low concentration
2S can obtain higher conversion, and transformation efficiency improves with concentration and reduces, and the sulphur deposition that reaction generates can not in time be removed at inside reactor.
Open source literature Int.J.Energy Res, 2012:2924-2930. have reported and have utilized the dielectric barrier discharge decomposing H
2The method of S.Its technical characterictic is: be filled with MoOx/Al
2O
3In the dielectric barrier discharge reactor of catalyzer, unstripped gas is H
2The mixed gas of S and Ar, H
2The volume content of S is 5%, and total gas flow rate is 150mL/min, discharges H 10 minutes
2The S transformation efficiency is 48%, and energy consumption is 0.92kJ/l H
2S.Decompose the sulphur of producing and be attached to catalyzer and inside reactor, cause catalyst deactivation and system electric capacity to change, it is very unstable to discharge, with the prolongation of discharge time, H
2The rate of decomposition of S reduces gradually.
Master's thesis " plasma body cooperative ZnS decomposing H
2S hydrogen manufacturing ", 2012. have reported plasma body cooperative ZnS decomposing H
2The situation of rate of decomposition, not mentioned H have been reported in S hydrogen manufacturing
2Efficiency and stability problem that S decomposes.
Summary of the invention
The purpose of this invention is to provide the continual and steady apparatus and method of producing hydrogen of decomposing of a kind of hydrogen sulfide, hydrogen sulfide or hydrogen sulfide containing gas are with helicon mode in the present invention, reverse eddy flow passes through electrical discharge zone vertically, form reverse vortex, utilize the high-energy electron of region of discharge that hydrogen sulfide is decomposed, decomposing the sulphur that produces is come out by centrifugation in time, promote the decomposition reaction forward to carry out, an elemental sulfur part that generates is discharged with the hydrogen of unreacted unstripped gas and generation, a part is attached on middle tube inwall and the inner tank theca, by control region of discharge temperature, make the elemental sulfur fusing, along leaving region of discharge under the wall flow, improve hydrogen sulfide rate of decomposition and capacity usage ratio.
The present invention is achieved through the following technical solutions.
The present invention relates to the continual and steady device of producing hydrogen that decomposes of a kind of hydrogen sulfide, this device comprises central electrode, electrical discharge zone, circulating liquid ground-electrode for the coaxial sleeve tube reactor; Central electrode is the metal of inner core parcel, zone between inner core and the middle tube is electrical discharge zone, urceolus and middle tube form chuck, the outer tube side wall lower end is provided with the circulating liquid import, the outer tube side wall upper end is provided with the circulating liquid outlet, feed circulating liquid as ground-electrode in the chuck that middle tube and urceolus form, and electrical discharge zone and barrel are carried out temperature control; Fix a metal electric current in the bottom of urceolus and middle tube annular space and derive line, the one end gos deep into chuck and contacts with the liquid ground-electrode, and the other end stretches out urceolus and is connected with grounding wire; The sidewall that stretches out urceolus in middle tube lower end is provided with raw material gas inlet, lower end at middle tube is provided with relief outlet, the intake method of unstripped gas is circumferential air inlet, guarantee that air inlet is with helicon mode, reverse eddy flow passes through electrical discharge zone vertically, increase gas in the residence time of electrical discharge zone, and the sulphur of generation is come out by centrifugation in time, promote the decomposition reaction forward to carry out; The sulphur that decompose to produce partly is attached on the barrel, and the temperature by control circulating liquid ground-electrode makes the elemental sulfur fusing between 119 ℃-444 ℃, flow down along tube wall, leaves region of discharge.
Dielectric barrier discharge decomposing hydrogen sulfide provided by the invention produces hydrogen and elemental sulfur has the following advantages:
(1) these apparatus and method have improved the homogeneity of hydrogen sulfide discharge;
(2) these apparatus and method have reduced energy waste, have improved capacity usage ratio, have improved hydrogen sulfide and have decomposed the efficiency of producing hydrogen;
(3) intake method of unstripped gas is circumferential air inlet in these apparatus and method, and air inlet is with helicon mode, and reverse eddy flow passes through electrical discharge zone vertically, gas increased in the residence time of electrical discharge zone, the sulphur that produces is come out by centrifugation in time, promotes the decomposition reaction forward to carry out, and rate of decomposition improves;
(4) these apparatus and method can make the elemental sulfur that decomposes generation in time leave electrical discharge zone, discharge sustain is stablized carried out, and are beneficial to industrialization promotion.
Description of drawings
Fig. 1 is the structural representation of coaxial sleeve tube reactor of the present invention;
Fig. 2 is the vertical view of coaxial sleeve tube reactor of the present invention.
Wherein tube, 5-inner core, 6-chuck, the import of 7-circulating liquid, 8-raw material gas inlet, 9-grounding wire, 10-relief outlet among 1-central electrode, the outlet of 2-circulating liquid, 3-urceolus, the 4-.
Embodiment
The invention will be further described below in conjunction with drawings and Examples.
The continual and steady device of producing hydrogen that decomposes of a kind of hydrogen sulfide, as shown in Figure 1, reactor shell is the coaxial sleeve structure made from insulating material, urceolus 3 all seals with the above and below of middle tube 4, form chuck 6, it is the circulating liquid as temperature control and ground-electrode in the chuck 6, middle tube 4 seals and is fixed on the insulating material with inner core 5, the top open-ended of inner core 5, its top barrel is fixed on the insulating material, be provided with central electrode 1 in the inner core 5, its part of stretching out insulating material is connected with the high voltage end of ac step-up transformer, fix a metal electric current at urceolus 3 with the bottom of middle tube 4 annular spaces and derive line, the one end gos deep into chuck 6 and contacts with the circulating liquid ground-electrode, the other end stretches out urceolus 3 and is connected with grounding wire 9, and the material of central electrode 1 and grounding wire 9 is platinum, rhodium, palladium, gold, copper, tungsten, iron and nickeliferous and stainless steel titanium; Urceolus 3 side wall lower ends are provided with circulating liquid import 7, urceolus 3 sidewall upper are provided with circulating liquid outlet 2, the sidewall that stretches out urceolus 3 in middle tube 4 lower ends is provided with raw material gas inlet 8, lower end at middle tube 4 is provided with relief outlet 10, reactant carries out exoelectrical reaction in the tubular annular space space that middle tube 4 and inner core 5 constitute, in tube 4 be reactor shell with the barrel of inner core 5, be again the block media of discharge, urceolus 3, middle tube 4 and inner core 5 are made by insulating material; Insulating material comprises oxide glass, corundum, pottery and quartzy.
The continual and steady method of producing hydrogen of decomposing of a kind of hydrogen sulfide, its concrete steps are:
(1) feed nitrogen in the device of plasma decomposes hydrogen sulfide, remove the air in the electrical discharge zone, export its discharge as the liquid of ground-electrode and from circulating liquid from the feeding of circulating liquid entrance simultaneously, fluid temperature is room temperature;
(2) in raw material gas inlet hydrogen sulfide or hydrogen sulfide containing gas are circumferentially fed, air inlet is with helicon mode, and reverse eddy flow forms reverse vortex by electrical discharge zone vertically; Connect ac high voltage source, then by voltage regulator and frequency regulator, ac high-voltage progressively is loaded on the electrode of plasma producing apparatus, make and form the plasma discharge field between central electrode and the liquid ground-electrode, and reaching even discharge condition, the interior hydrogen sulfide of electrical discharge zone this moment is subjected to effect of electric field generation ionization;
(3) hydrogen sulfide is decomposed into hydrogen and elemental sulfur in electrical discharge zone generation ionization, and the elemental sulfur part of generation is discharged with the hydrogen of unreacted unstripped gas and generation, and a part is attached on middle tube inwall and the inner tank theca;
(4) when the sulphur that adheres on the wall has a strong impact on discharge, in discharge, make the fluid temperature in the chuck reach 120 ℃, make on the tube inwall and the fusing of the elemental sulfur on the inner tank theca, flow out electrical discharge zone with liquid form, treat again the circulating liquid temperature to be returned to room temperature after sulphur fusing on the wall is left, carry out so repeatedly; 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.
The continual and steady method of producing hydrogen of decomposing of a kind of hydrogen sulfide, its concrete steps are:
(1) feed nitrogen in the device of plasma decomposes hydrogen sulfide, remove the air in the electrical discharge zone, export its discharge as the liquid of ground-electrode and from circulating liquid from the feeding of circulating liquid entrance simultaneously, fluid temperature remains on 120 ℃;
(2) at the unstripped gas inlet mouth hydrogen sulfide or hydrogen sulfide containing gas are circumferentially fed, air inlet is with helicon mode, and reverse eddy flow forms reverse vortex by electrical discharge zone vertically; Connect ac high voltage source, then by voltage regulator and frequency regulator, ac high-voltage progressively is loaded on the electrode of plasma producing apparatus, make and form the plasma discharge field between central electrode and the liquid ground-electrode, and reaching even discharge condition, the interior hydrogen sulfide of electrical discharge zone this moment is subjected to effect of electric field generation ionization;
(3) hydrogen sulfide is decomposed into hydrogen and elemental sulfur in electrical discharge zone generation ionization, and the elemental sulfur part of generation is discharged with the hydrogen of unreacted unstripped gas and generation, and a part is attached on middle tube inwall and the inner tank theca;
(4) 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.
Above-described specific embodiment; purpose of the present invention, technical scheme and beneficial effect are had been described in detail; institute is understood that; the above only is specific embodiments of the invention; be not limited to the present invention; within the spirit and principles in the present invention all, any modification of making, be equal to replacement, improvement etc., all should be included among the protection of the present invention.
Claims (9)
1. a hydrogen sulfide decomposes the apparatus and method of producing hydrogen continually and steadily, it is characterized in that, reactor shell is the coaxial sleeve structure made from insulating material, urceolus (3) all seals with the above and below of middle tube (4), form chuck (6), it is the circulating liquid as temperature control and ground-electrode in the chuck (6), middle tube (4) seals and is fixed on the insulating material with inner core (5), the top open-ended of inner core (5), its top barrel is fixed on the insulating material, be provided with central electrode (1) in the inner core (5), its part of stretching out insulating material is connected with the high voltage end of ac step-up transformer, fix a metal electric current at urceolus (3) with the bottom of middle tube (4) annular space and derive line, the one end gos deep into chuck (6) and contacts with the liquid ground-electrode, the other end stretches out urceolus (3) and is connected with grounding wire (9), and the material of central electrode (1) and grounding wire (9) is platinum, rhodium, palladium, gold, copper, tungsten, iron and nickeliferous and stainless steel titanium; Urceolus (3) side wall lower ends is provided with circulating liquid import (7), urceolus (3) sidewall upper is provided with circulating liquid outlet (2), the sidewall that stretches out urceolus (3) in middle tube (4) lower end is provided with raw material gas inlet (8), lower end at middle tube (4) is provided with relief outlet (10), reactant carries out exoelectrical reaction in the tubular annular space space that middle tube (4) and inner core (5) constitute, the inwall of middle tube (4) and the outer wall of inner core (5) are reactor shell, are again the block medias of discharge; Urceolus (3), middle tube (4) and inner core (5) are made by insulating material, and insulating material is oxide glass, corundum, pottery and quartzy.
2. the continual and steady apparatus and method of producing hydrogen of decomposing of a kind of hydrogen sulfide according to claim 1 is characterized in that, the ratio of the diameter of described central electrode (1) and middle tube (4) internal diameter is 1:20-1:1.5.
3. the continual and steady apparatus and method of producing hydrogen of decomposing of a kind of hydrogen sulfide according to claim 1 is characterized in that reactor is line-cartridge type electrode structure or tube-cartridge type electrode structure.
4. the continual and steady apparatus and method of producing hydrogen of decomposing of a kind of hydrogen sulfide according to claim 1 is characterized in that, the diameter of the diameter of described grounding wire (9) and central electrode (1) is than being 1:1-5:1.
5. the continual and steady apparatus and method of producing hydrogen of decomposing of a kind of hydrogen sulfide according to claim 1 is characterized in that described raw material gas inlet (8) is arranged in the side wall lower ends of tube (4), make the gas of electrical discharge zone form reverse vortex.
6. the apparatus and method of hydrogen are produced in the continual and steady decomposition of a kind of hydrogen sulfide according to claim 1, it is characterized in that, the intake method of described raw material gas inlet (8) is circumferential air inlet, guarantee that air inlet is with helicon mode, reverse eddy flow passes through electrical discharge zone vertically, increase gas in the residence time of electrical discharge zone, the sulphur of generation is come out by centrifugation in time, promotes the decomposition reaction forward to carry out.
7. the apparatus and method of hydrogen are produced in the continual and steady decomposition of a kind of hydrogen sulfide according to claim 1, it is characterized in that, can be by regulating the temperature of chuck (6) internal recycle liquid, the temperature of control region of discharge and barrel, make the sulphur fusing of generation, flow down along barrel, leave region of discharge, the assurance discharge sustain is stable carries out.
8. the continual and steady apparatus and method of producing hydrogen of decomposing of a kind of hydrogen sulfide according to claim 1 is characterized in that the temperature of the interior liquid of chuck (6) can remain between 119 ℃-444 ℃ always in discharge process; Or keep room temperature in the discharge starting stage, and when the sulphur that adheres on the wall has a strong impact on discharge, its temperature is brought up between 119 ℃-444 ℃, treat again the circulating liquid temperature to be returned to room temperature after sulphur fusing on the wall is left, carry out so repeatedly.
9. the continual and steady apparatus and method of producing hydrogen of decomposing of a kind of hydrogen sulfide according to claim 1 is characterized in that the liquid as ground-electrode in the chuck (6) is a kind of of salts solution, alkaline solution and ionic liquid.
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| 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 |
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