CN103204466A - Device and method for preparing hydrogen through temperature controlled continuous decomposition of hydrogen sulfide - Google Patents
Device and method for preparing hydrogen through temperature controlled continuous decomposition of hydrogen sulfide Download PDFInfo
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Abstract
The invention discloses a device and a method for preparing hydrogen through temperature controlled continuous decomposition of hydrogen sulfide, belongs to the technical field of hydrogen preparation and gas purification, and relates to a dielectric barrier discharge temperature controllable plasma generating device and a method for preparing hydrogen through continuous and stable ionizing decomposition of a hydrogen sulfide gas or a gas containing hydrogen sulfide by using the device. The device is characterized in that a reactor has a coaxial sleeve type structure, a cylinder of the reactor is made of an insulating medium, a central electrode is formed by a metal, a grounding electrode is formed by a temperature controllable circulating liquid, and decomposed sulfur is separated through temperature control, so that continuous and stable operation of preparing the hydrogen through the decomposition of the hydrogen sulfide is ensured. The invention has the advantages that the method is suitable for preparing the hydrogen and elemental sulfur by dissociating the gases containing the hydrogen sulfide in chemical industries of natural gas, petroleum and coal; and the method does not have special requirement or limitation for the source and the composition of the gases, so the method has universal applicability for preparing the hydrogen and the elemental sulfur through the decomposition of the hydrogen sulfide.
Description
Technical field
The invention belongs to hydrogen manufacturing and gas purification technology field, relate to a kind of apparatus and method of utilizing dielectric barrier discharge hydrogen sulfide to be decomposed into hydrogen and elemental sulfur.
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 only at high temperature it just has considerable transformation efficiency.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 the method for utilizing dielectric barrier discharge decomposing H 2S.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 is when 298K is higher than 430K.
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, when 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 10 minutes the time H
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 problem and stability problem that S decomposes.
Summary of the invention
The purpose of this invention is to provide a kind of controlling temp type hydrogen sulfide and decompose the apparatus and method of producing hydrogen continuously, utilize dielectric barrier discharge that hydrogen sulfide is decomposed and produce hydrogen and elemental sulfur, the circulating liquid of Controllable Temperature is as the ground-electrode of dielectric barrier discharge reactor, make discharge more even, power loss reduces, and by temperature control, makes the sulphur that decomposes generation leave region of discharge, guarantee that the continous-stable that the hydrogen sulfide discharge is decomposed carries out, and improves the efficiency that hydrogen sulfide decomposes.
The present invention is achieved through the following technical solutions.
The present invention relates to controlling temp type hydrogen sulfide and decompose the device of producing hydrogen continuously, this device comprises central electrode, electrical discharge zone, circulating liquid ground-electrode for the coaxial sleeve tube reactor; Central electrode is metal, zone between inner core and the central electrode is electrical discharge zone, inner core and urceolus 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 in the chuck that inner core and urceolus form as ground-electrode, and electrical discharge zone and barrel are carried out temperature control; Fix a metal electric current in the bottom of urceolus and inner core 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; Sidewall is provided with raw material gas inlet in the inner core upper end, is provided with relief outlet in the lower end of inner core, when the temperature of circulating liquid ground-electrode reaches between 119 ℃-444 ℃, decomposes the sulphur fusing that produces and becomes liquid state along under tube wall or the catalyst stream, leaves region of discharge.
Controlling temp type hydrogen sulfide provided by the invention decomposes the apparatus and method of producing hydrogen continuously, has the following advantages:
(1) these apparatus and method improve the homogeneity of hydrogen sulfide discharge;
(2) these apparatus and method can make the elemental sulfur that decomposes generation leave electrical discharge zone, discharge sustain is stablized carried out, and are beneficial to industrialization promotion;
(3) these apparatus and method reduce capacitive current, reduce energy waste, improve capacity usage ratio, improve hydrogen sulfide and decompose the efficiency of producing hydrogen.
Description of drawings
Fig. 1 is coaxial sleeve tube structure of reactor synoptic diagram of the present invention;
Fig. 2 is the coaxial sleeve tube structure of reactor synoptic diagram that is filled with catalyzer of the present invention;
Wherein 1-central electrode, 2-insulation end socket 3-raw material gas inlet, the outlet of 4-circulating liquid, 5-urceolus, 6-inner core, 7-chuck, 8-grounding wire, the import of 9-circulating liquid, 10-relief outlet, 11-catalyzer.
Embodiment
The invention will be further described below in conjunction with drawings and Examples.
Embodiment 1
A kind of controlling temp type hydrogen sulfide decomposes the device of producing hydrogen continuously, as shown in Figure 1, it is a kind of temperature controllable formula plasma producing apparatus that belongs to dielectric barrier discharge, its housing is the coaxial sleeve structure made from insulating material, urceolus (5) all seals with the above and below of inner core (6), form chuck (7), it is the circulating liquid as temperature control and ground-electrode in the chuck (7), seal with the insulation end socket on the top of inner core (6), central electrode (1) is inserted in center by this insulation end socket in inner core (6), its part of stretching out insulating material is connected with the high voltage end of ac step-up transformer, fix a metal electric current in urceolus (5) and the bottom of inner core (6) annular space and derive line, the one end gos deep into chuck (7) and contacts with the liquid ground-electrode, the other end stretches out urceolus (5) and is connected with grounding wire (8), and the material of central electrode (1) and grounding wire (8) is platinum, rhodium, palladium, gold, copper, tungsten, iron and nickeliferous and stainless steel titanium.Urceolus (5) side wall lower ends is provided with circulating liquid import (9), urceolus (5) sidewall upper is provided with circulating liquid outlet (4), sidewall is provided with raw material gas inlet (3) in inner core (6) upper end, be provided with relief outlet (10) in the lower end of inner core (6), reactant carries out exoelectrical reaction in the tubular space that inner core (6) and central electrode (1) constitute, the barrel of inner core (6) is reactor shell, be the block media of discharge simultaneously, urceolus (5) and inner core (6) are made by insulating material; Insulating material can be oxide glass, corundum, pottery and quartzy.
A kind of controlling temp type hydrogen sulfide decomposes the method for producing hydrogen continuously, and 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 from circulating liquid entrance feeding liquid and from circulating liquid simultaneously, fluid temperature remains room temperature;
(2) in raw material gas inlet hydrogen sulfide or hydrogen sulfide containing gas are fed, 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 attached to inner tube wall, and a part is discharged with the hydrogen of unreacted unstripped gas and generation;
(4) when the sulphur that adheres on the inner tube wall has a strong impact on discharge, in discharge, make the temperature of chuck internal recycle liquid reach 120 ℃, treat the sulphur fusing on the wall, flow out with liquid form, leave region of discharge, again the circulating liquid temperature is returned to room temperature, 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.
A kind of controlling temp type hydrogen sulfide decomposes the device of producing hydrogen continuously, as shown in Figure 2, it is a kind of temperature controllable formula plasma producing apparatus that belongs to dielectric barrier discharge, its housing is the coaxial sleeve structure made from insulating material, urceolus (5) all seals with the above and below of inner core (6), form chuck (7), it is the circulating liquid ground-electrode as temperature control and ground connection purpose in the chuck (7), seal with the insulation end socket on the top of inner core (6), central electrode (1) is inserted in center by this insulation end socket in inner core (6), its part of stretching out insulating material is connected with the high voltage end of ac step-up transformer, fix a metal electric current in urceolus (5) and the bottom of inner core (6) annular space and derive line, the one end gos deep into chuck (7) and contacts with the liquid ground-electrode, the other end stretches out urceolus (5) and is connected with grounding wire (8), and the material of central electrode (1) and grounding wire (8) is platinum, rhodium, palladium, gold, copper, tungsten, iron and nickeliferous and stainless steel titanium.Urceolus (5) side wall lower ends is provided with circulating liquid import (9), urceolus (5) sidewall upper is provided with circulating liquid outlet (4), sidewall is provided with raw material gas inlet (3) in inner core (6) upper end, be provided with relief outlet (10) in the lower end of inner core (6), reactant carries out exoelectrical reaction in the tubular space that inner core (6) and central electrode (1) constitute, the barrel of inner core (6) is reactor shell, be the block media of discharge simultaneously, urceolus (5) and inner core (6) are made by insulating material, are filled with hydrogen sulfide in the inner core (6) and decompose with catalyzer (11); Insulating material can be oxide glass, corundum, pottery and quartzy.
A kind of controlling temp type hydrogen sulfide decomposes the method for producing hydrogen continuously, and its concrete steps are:
(1) feed nitrogen continuous the decomposition in the device of producing hydrogen at controlling temp type 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 room temperature;
(2) in raw material gas inlet hydrogen sulfide or hydrogen sulfide containing gas are fed, 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 attached on inner tube wall and the catalyzer, and a part is discharged with the hydrogen of unreacted unstripped gas and generation;
(4) when the sulphur that adheres to has a strong impact on discharge on the inner tube wall and on the catalyzer, in discharge, make the temperature of chuck internal recycle liquid reach 120 ℃, treat on the inner tube wall and catalyzer on the sulphur fusing, flow out with liquid form, leave region of discharge, again the circulating liquid temperature is returned to room temperature, 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.
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 (6)
1. a controlling temp type hydrogen sulfide decomposes the apparatus and method of producing hydrogen continuously, relate to a kind of temperature controllable formula plasma producing apparatus of dielectric barrier discharge, its housing is the coaxial sleeve structure made from insulating material, urceolus (5) all seals with the above and below of inner core (6), form chuck (7), it is the circulating liquid ground-electrode as temperature control and ground-electrode in the chuck (7), seal with the insulation end socket on the top of inner core (6), central electrode (1) is inserted in center by this insulation end socket in inner core (6), its part of stretching out insulating material is connected with the high voltage end of ac step-up transformer, fix a metal electric current in urceolus (5) and the bottom of inner core (6) annular space and derive line, the one end gos deep into chuck (7) and contacts with the circulating liquid ground-electrode, the other end stretches out urceolus (5) and is connected with grounding wire (8), and the material of central electrode (1) and grounding wire (8) is platinum, rhodium, palladium, gold, copper, tungsten, iron and nickeliferous and stainless steel titanium; Urceolus (5) side wall lower ends is provided with circulating liquid import (9), urceolus (5) sidewall upper is provided with circulating liquid outlet (4), sidewall is provided with raw material gas inlet (3) in inner core (6) upper end, be provided with relief outlet (10) in the lower end of inner core (6), reactant carries out exoelectrical reaction in the tubular space that inner core (6) and central electrode (1) constitute, the barrel of inner core (6) is reactor shell, be the block media of discharge simultaneously, urceolus (5) and inner core (6) are made by insulating material; Insulating material is oxide glass, corundum, pottery and quartzy.
2. a kind of controlling temp type hydrogen sulfide according to claim 1 decomposes the apparatus and method of producing hydrogen continuously, it is characterized in that the ratio of the diameter of described central electrode (1) and inner core (6) internal diameter is 1:20-1:1.5.
3. a kind of controlling temp type hydrogen sulfide according to claim 1 decomposes the apparatus and method of producing hydrogen continuously, it is characterized in that, the diameter of the diameter of described grounding wire (8) and central electrode (1) is than being 1:1-5:1.
4. a kind of controlling temp type hydrogen sulfide according to claim 1 decomposes the apparatus and method of producing hydrogen continuously, it is characterized in that, can be by regulating the temperature of the interior liquid of chuck (7), the temperature of control region of discharge and barrel, make the sulphur fusing of generation, leave region of discharge, the assurance discharge sustain is stable carries out.
5. a kind of controlling temp type hydrogen sulfide according to claim 1 decomposes the apparatus and method of producing hydrogen continuously, it is characterized in that the temperature of the interior liquid of chuck (7) can remain in discharge process between 119 ℃-444 ℃ always; Or in discharge starting stage maintenance room temperature, when the sulphur that adheres on inner core (6) inwall or the catalyzer (11) has a strong impact on discharge, again the temperature of liquid is brought up between 119 ℃-444 ℃, treat on the wall and catalyzer (11) on sulphur fusing leave after, again the circulating liquid temperature is returned to room temperature, carry out so repeatedly.
6. a kind of controlling temp type hydrogen sulfide according to claim 1 decomposes the apparatus and method of producing hydrogen continuously, it is characterized in that, the liquid as ground-electrode in the chuck (7) is a kind of of salts solution, alkaline solution and ionic liquid.
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