CN110127604A - The method of plasma reactor and decomposing hydrogen sulfide - Google Patents

The method of plasma reactor and decomposing hydrogen sulfide Download PDF

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Publication number
CN110127604A
CN110127604A CN201810136792.3A CN201810136792A CN110127604A CN 110127604 A CN110127604 A CN 110127604A CN 201810136792 A CN201810136792 A CN 201810136792A CN 110127604 A CN110127604 A CN 110127604A
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China
Prior art keywords
inner cylinder
plasma reactor
grounding electrode
hydrogen sulfide
block media
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CN201810136792.3A
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Chinese (zh)
Inventor
孙万付
张婧
张铁
任君朋
李亚辉
石宁
朱云峰
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China Petroleum and Chemical Corp
Sinopec Qingdao Safety Engineering Institute
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China Petroleum and Chemical Corp
Sinopec Qingdao Safety Engineering Institute
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Application filed by China Petroleum and Chemical Corp, Sinopec Qingdao Safety Engineering Institute filed Critical China Petroleum and Chemical Corp
Priority to CN201810136792.3A priority Critical patent/CN110127604A/en
Priority to RU2020127670A priority patent/RU2753275C1/en
Priority to US16/968,785 priority patent/US11691119B2/en
Priority to CN201980004595.9A priority patent/CN111278766B/en
Priority to PCT/CN2019/074087 priority patent/WO2019154245A1/en
Publication of CN110127604A publication Critical patent/CN110127604A/en
Pending legal-status Critical Current

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    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D53/00—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols
    • B01D53/32—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols by electrical effects other than those provided for in group B01D61/00
    • B01D53/323—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols by electrical effects other than those provided for in group B01D61/00 by electrostatic effects or by high-voltage electric fields
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B17/00—Sulfur; Compounds thereof
    • C01B17/02—Preparation of sulfur; Purification
    • C01B17/04—Preparation of sulfur; Purification from gaseous sulfur compounds including gaseous sulfides
    • C01B17/0495—Preparation of sulfur; Purification from gaseous sulfur compounds including gaseous sulfides by dissociation of hydrogen sulfide into the elements
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B3/00—Hydrogen; Gaseous mixtures containing hydrogen; Separation of hydrogen from mixtures containing it; Purification of hydrogen
    • C01B3/02—Production of hydrogen or of gaseous mixtures containing a substantial proportion of hydrogen
    • C01B3/04—Production of hydrogen or of gaseous mixtures containing a substantial proportion of hydrogen by decomposition of inorganic compounds, e.g. ammonia
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D2257/00—Components to be removed
    • B01D2257/30—Sulfur compounds
    • B01D2257/304—Hydrogen sulfide
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B2203/00—Integrated processes for the production of hydrogen or synthesis gas
    • C01B2203/02—Processes for making hydrogen or synthesis gas
    • C01B2203/0266—Processes for making hydrogen or synthesis gas containing a decomposition step
    • C01B2203/0277—Processes for making hydrogen or synthesis gas containing a decomposition step containing a catalytic decomposition step
    • 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

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Engineering & Computer Science (AREA)
  • Inorganic Chemistry (AREA)
  • Analytical Chemistry (AREA)
  • General Chemical & Material Sciences (AREA)
  • Oil, Petroleum & Natural Gas (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Health & Medical Sciences (AREA)
  • General Health & Medical Sciences (AREA)
  • Combustion & Propulsion (AREA)
  • Physical Or Chemical Processes And Apparatus (AREA)

Abstract

The present invention relates to plasma chemistry fields, disclose the method for a kind of plasma reactor and decomposing hydrogen sulfide, which includes: inner cylinder (1)；Outer cylinder (2), the outer cylinder (2) are nested in the outside of the inner cylinder (1)；Central electrode (3), the central electrode (3) are arranged in the inner cylinder (1)；The grounding electrode (4) formed by solid conductive material, grounding electrode forms at least partly side wall of inner cylinder or grounding electrode is circumferentially positioned on the inner sidewall of inner cylinder；Block media (6), the block media (6) are arranged on at least partly outer surface of the central electrode (3).Plasma reactor provided by the invention can realize the lasting of hydrogen sulfide decomposable process and be stablized under significantly higher hydrogen sulfide conversion ratio and be carried out, and device can be realized long-term operation.

Description

The method of plasma reactor and decomposing hydrogen sulfide
Technical field
The present invention relates to plasma chemistry fields, and in particular to a kind of plasma reactor and a kind of decomposing hydrogen sulfide Method.
Background technique
Hydrogen sulfide (H2S it is) a kind of hypertoxic, stench sour gas, can not only causes the corrosion of the materials such as metal, but also It can be detrimental to health, pollute environment.The large and medium-sized oil plant in China is all made of traditional Claus method (Claus) processing and contains at present H2The tail gas of S, and Recovered sulphur.This method has only recycled the sulphur in hydrogen sulfide, but converts water for valuable hydrogen.From resource It comprehensively utilizes angle and considers that in traditional hydrogen sulfide recovery process, hydrogen resource is not effectively utilized.Therefore, will Hydrogen sulfide is decomposed into sulphur and hydrogen has been increasingly becoming the technical field that domestic and international researcher is paid close attention to.
Currently, hydrogen sulfide decomposition method specifically includes that high-temperature decomposition, electrochemical process, photocatalytic method and low-temperature plasma Body method etc..In aforementioned a variety of methods, high temperature thermal decomposition method relative maturity in industrial technology, but hydrogen sulfide thermal decomposition is consumingly Limited dependent on reaction temperature, and by thermodynamical equilibrium, though reaction temperature at 1000 DEG C or more, the conversion ratio of hydrogen sulfide Only 20%.In addition, hot conditions are to the more demanding of reactor material, this also will increase operating cost.Further, since vulcanization Hydrogen thermal decomposition conversion ratio is low, needs to separate a large amount of hydrogen sulfide gas from tail gas and recycle in systems, therefore also reduce Unit efficiency and energy consumption is increased, these bring difficulty to its large industrialized application.Although using membrane technology can be with Product is efficiently separated to break balance limitation, improves hydrogen sulfide conversion ratio, but thermal decomposition temperature tends to exceed the pole of film Heat resisting temperature is limited, membrane material structure is destroyed.Electrochemistry rule there are operating procedures more, equipment seriously corroded, reaction are steady The disadvantages of qualitative difference and low efficiency.Photocatalytic method decomposing hydrogen sulfide mainly uses for reference the research of photochemical catalyzing, research emphasis collection In in terms of developing high efficiency semiconductor.Using solar energy come decomposing hydrogen sulfide, with low energy consumption, reaction condition temperature It is relatively inexpensive method with simple operation and other advantages.But that there are treating capacities is small for this method, catalytic efficiency is low and is catalyzed Agent is easy the problems such as inactivation.
Compared with other decomposition methods, low-temperature plasma body method has easy to operate, and device volume is small, and energy efficiency is high The advantages that, and the reaction being directed to has the controllability of height, and it can be when small treating capacity, being difficult to focus on flexibly It is applied on ground.Further, since it has the characteristics that high-energy density and can shorten the reaction time, can be realized at a lower temperature Hydrogen sulfide is effectively decomposed, the changeable occasion of different scales, scattered distribution, working condition is suitable for.Moreover, recycling While sulphur, hydrogen resource reclaim can be realized the utilization of hydrogen sulfide recycling by low-temperature plasma body method.
Currently, researchers at home and abroad conduct extensive research low temperature plasma decomposing hydrogen sulfide technology, use Discharge type mainly include glow discharge, corona discharge, sliding arc discharge, microwave plasma, radio frequency plasma and Dielectric barrier discharge etc..
Document " International journal of hydrogen energy ", 2012,37:1335-1347. use The method decomposing hydrogen sulfide for shrinking normal glow discharge, is vulcanized under the conditions of pressure 0.02Mpa, 2000~4000K of temperature The minimum decomposition energy consumption of hydrogen is 2.35eV/H2S.But this reaction temperature is high, pressure is low, and condition harshness is not easy to realize.
Document " International journal of hydrogen energy ", 2012,37:10010-10019 adopt With microwave plasma decomposition hydrogen sulfide, hydrogen sulfide can be decomposed completely under the conditions of atmospheric pressure, temperature 2400K, but after decomposition Hydrogen and sulphur can at high temperature rapidly it is compound regenerate hydrogen sulfide, there has been no corresponding quenching measures at present.
Document " Chemical Engineering Science ", 2009,64 (23): 4826-4834. uses impulse electric corona Electric discharge has carried out H2S decomposes the research of hydrogen making and sulphur, and reactor uses line tubular structure, in constant power 100W condition Under investigated pulse electric capacity, discharge voltage and pulse frequency to H2S conversion ratio and the influence for decomposing efficiency.As a result table Bright, under conditions of power is certain, low pulse electric capacity, low discharge voltage and high pulse frequencies help to obtain high H2S Decompose efficiency；In addition, with Ar and N2It is compared as Balance Air, with Ar-N2It is available higher when gaseous mixture is as Balance Air H2S conversion ratio, in Ar/N2/H2When S volume fraction is 46%/46%/8%, discharge power 60W, pulse electric capacity 720pF, The H of acquisition2The minimum decomposition energy consumption of S is 4.9eV/H2S, but H at this time2S conversion ratio is only 30% or so.In addition, this reaction system Flow is only 1.18 × 10-4SCMs-1, this low discharge, low concentration, low-conversion reaction effect do not have in the industrial production Practical significance.
Document " Journal of applied physics ", 1998,84 (3): 1215-1221 uses sliding arc discharge To H2S decomposition reaction is studied, and method is by H2S Dilution air to concentration is 0~100ppm, in gas overall flow rate To have investigated flow rate of gas, reaction cavity size and frequency under the conditions of 0~100L/min to H2The influence of S decomposition reaction. The experimental results showed that low gas flow rate, shallow bid spacing and low frequency help to obtain higher H2S conversion ratio, in the electric discharge of optimization Under the conditions of obtained H2S conversion ratio is up to 75~80%, but H2S decomposes energy consumption and is up to 500eV/H2S, this concentration is low, energy consumption is high Reaction effect is also without prospects for commercial application.
Dielectric barrier discharge can usually generate under atmospheric pressure, and discharge temp is lower.Further, since the presence of medium The growth of discharge current is limited, punctures completely so as to avoid gas and forms spark or electric arc, this is conducive to large volume, stabilization The generation of plasma has preferable prospects for commercial application.
Document " Plasma chemistry and plasma processing ", 1992,12 (3): 275-285 use changes Into ozone generator investigated H2Flash-over characteristic of the S within the scope of 130~560 DEG C, and have studied reaction temperature, H2S charging is dense Degree, injecting power and addition H2、Ar、N2Deng to H2The influence of S conversion ratio and energy efficiency, experiment discovery addition Ar can promote Into H2The decomposition of S, in 50~100mL/min of total flow, H2S concentration obtained under the conditions of being 20~100% conversion ratio be 0.5~ 12%, most low yield Hydrogen Energy consumption is about 0.75mol/kWh (50eV/H2), however, this process still remains, conversion ratio is low and energy consumption is high The shortcomings that.
CN102408095A cooperates with decomposing hydrogen sulfide using dielectric barrier discharge and photochemical catalyst, and method is that will have light The solid catalyst of catalytic activity is filled in plasma slab, however this method is decomposed the sulphur generated there are hydrogen sulfide and can be deposited The shortcomings that below catalyst bed.
Document " International Journal of Energy Research ", 2013,37 (11): 1280-1286. By Al2O3, MoOx/Al2O3, CoOx/Al2O3And NiO/Al2O3Catalyst is filled in region of discharge, using dielectric barrier discharge and urges Agent has carried out H2S decomposes research.Reaction result shows MoOx/Al2O3And CoOx/Al2O3Catalyst has better effects；Wherein As filling MoOx/Al2O3Catalyst, in H2S/Ar total flow 150mL/min, H2S concentration is 5 volume %, injection ratio energy SIE is When 0.92kJ/L, catalyst filling length are bed 10%, obtained H2S maximum conversion is about 48%.But this reaction process Concentration of hydrogen sulfide is lower, decomposes the sulfur deposition of generation in inside reactor, with the extension of time, catalyst activity reduction, Discharge stability reduces, and the conversion ratio of hydrogen sulfide is caused to gradually decrease.
The characteristics of CN103204466A discloses a kind of controlling temp type hydrogen sulfide decomposer and method, the device is middle electrocardio Extremely metal, the circulating liquid that grounding electrode is temperature-controllable, are controlled by the temperature of liquid grounding electrode, so that hydrogen sulfide point Solution preocess is capable of the progress of continuous-stable.In addition, CN103204467A, which discloses a kind of hydrogen sulfide, continually and steadily decomposes preparing hydrogen The characteristics of device and method of gas, the prior art is the circulation fluid using central electrode as metal, grounding electrode for temperature-controllable Body carries out temperature control by liquid grounding electrode, and raw material airintake direction is for circumferential air inlet and in a spiral mode along axial reverse By region of discharge, so that the sulphur generated is come out by timely centrifuge separation.However, CN103204466A and CN103204467A is public In order to guarantee that hydrogen sulfide is fully decomposed as far as possible in the method opened, the flow velocity for needing to control hydrogen sulfide makes it in reactor Residence time in inner cylinder is longer and the size electric energy that the gas of unit volume in inner cylinder is obtained of control inner cylinder is more, Also, since the current prior art can not provide more powerful power supply so that using CN103204466A and Method disclosed in CN103204467A even control hydrogen sulfide residence time it is longer and control inner cylinder size so that The electric energy that the gas of unit volume obtains in inner cylinder is more also merely capable of so that the maximum conversion of hydrogen sulfide reaches 20% left side The right side, also, when the maximum conversion of hydrogen sulfide reaches 20% or so, the energy consumption for vulcanizing hydroperoxide decomposition reaction is quite high, and uncomfortable Together in large scale industry application.Further, there is also available liquid in method disclosed in CN103204466A and CN103204467A The few defect of the type of body grounding electrode, disclosed in salting liquid etc. to be generally only capable of maintaining the temperature of reactor be 100 DEG C Hereinafter, and be easy to causeing the blocking of reactor hereinafter, elemental sulfur is generally solid-state at 100 DEG C.
Summary of the invention
The purpose of the invention is to the plasma reactors for overcoming the prior art to provide in the decomposition for hydrogen sulfide When existing hydrogen sulfide conversion ratio it is low and decompose the high defect of energy consumption, provide it is a kind of it is new can be improved hydrogen sulfide conversion ratio with And the method for reducing the plasma reactor for decomposing energy consumption and application the reactor decomposing hydrogen sulfide.
To achieve the goals above, in a first aspect, the present invention provides a kind of plasma reactor, which has same Axle clamp telescoping structure, and the reactor includes:
Inner cylinder is respectively arranged with reactor inlet and product exit on the inner cylinder；
Outer cylinder, the outer cylinder is nested in the outside of the inner cylinder, and heat-conducting medium entrance is respectively arranged on the outer cylinder It is exported with heat-conducting medium；
Central electrode, the central electrode are arranged in the inner cylinder；
Grounding electrode, the material for forming the grounding electrode is solid conductive material, and the grounding electrode forms inner cylinder At least partly side wall or the grounding electrode is circumferentially positioned on the inner sidewall of the inner cylinder；And
Block media, the block media are arranged on at least partly outer surface of the central electrode, so that at least portion Divide the setting that the block media and the block media are enclosed on the outer surface of the central electrode protruded into the inner cylinder Position makes the region of discharge between the central electrode and the grounding electrode by the block media interval；
Wherein, the distance between inner sidewall of the lateral wall of the block media and grounding electrode L1With the blocking The thickness D of medium1Proportionate relationship are as follows: L1: D1=(0.05~100): 1.
Second aspect, the present invention provide a kind of method of decomposing hydrogen sulfide, and this method is described in the first aspect present invention Implement in plasma reactor, this method comprises: under the conditions of dielectric barrier discharge, by the unstripped gas containing hydrogen sulfide from anti- Device entrance is answered to be introduced to the decomposition reaction for carrying out hydrogen sulfide in the inner cylinder of the plasma reactor, the logistics obtained after decomposition It is drawn by the product exit, also, by continuing to be drawn from heat-conducting medium entrance into the outer cylinder of the plasma reactor Temperature needed for entering heat-conducting medium and maintaining the plasma reactor as the heat-conducting medium outlet extraction heat-conducting medium Degree；The dielectric barrier discharge is formed by grounding electrode, block media and central electrode.
The plasma that aforementioned plasma reactor provided by the invention can be used in hydrogen sulfide decomposes, the reactor energy Uniform, efficient dielectric barrier discharge is enough generated, generates hydrogen and sulphur so that hydrogen sulfide directly be decomposed.
Aforementioned plasma reactor provided by the invention is the jacket type dielectric barrier discharge reaction with coaxial configuration Device, basic structure mainly include central electrode, solid grounding electrode and block media etc., which enables to lead Thermal medium carries out circulating-heating or cooling to discharge reactor, controls to realize the flexible temperature of region of discharge.Particularly, The present invention is by controlling the distance between the lateral wall of the block media and the inner sidewall of the grounding electrode L1With the resistance Keep off the thickness D of medium1Proportionate relationship are as follows: L1: D1=(0.05~100): it when 1, can improve compared with the existing technology significantly Energy consumption is decomposed in the conversion ratio of hydrogen sulfide and reduction.
In addition, plasma reactor provided by the invention can realize vulcanization under significantly higher hydrogen sulfide conversion ratio Hydrogen decomposable process continues and stablizes to carry out, and device can be realized long-term operation.And plasma provided by the invention Reactor according can also be used to big flow, the hydrogen sulfide treatment process of high concentration.
Detailed description of the invention
Fig. 1 is a kind of structural schematic diagram of preferred embodiment of plasma reactor provided by the invention.
Description of symbols
1, inner cylinder 2, outer cylinder
11, reactor inlet 21, heat-conducting medium entrance
12, product gas outlet 22, heat-conducting medium outlet
13, liquid product outlet
3, central electrode
4, grounding electrode
5, it is grounded
6, block media
Specific embodiment
The endpoint of disclosed range and any value are not limited to the accurate range or value herein, these ranges or Value should be understood as comprising the value close to these ranges or value.For numberical range, between the endpoint value of each range, respectively It can be combined with each other between the endpoint value of a range and individual point value, and individually between point value and obtain one or more New numberical range, these numberical ranges should be considered as specific open herein.
As previously mentioned, the first aspect of the present invention provides a kind of plasma reactor, which has coaxial folder Telescoping structure, and the reactor includes:
Inner cylinder is respectively arranged with reactor inlet and product exit on the inner cylinder；
Outer cylinder, the outer cylinder is nested in the outside of the inner cylinder, and heat-conducting medium entrance is respectively arranged on the outer cylinder It is exported with heat-conducting medium；
Central electrode, the central electrode are arranged in the inner cylinder；
Grounding electrode, the material for forming the grounding electrode is solid conductive material, and the grounding electrode forms inner cylinder At least partly side wall or the grounding electrode is circumferentially positioned on the inner sidewall of the inner cylinder；And
Block media, the block media are arranged on at least partly outer surface of the central electrode, so that at least portion Divide the setting that the block media and the block media are enclosed on the outer surface of the central electrode protruded into the inner cylinder Position makes the region of discharge between the central electrode and the grounding electrode by the block media interval；
Wherein, the distance between inner sidewall of the lateral wall of the block media and grounding electrode L1With the blocking The thickness D of medium1Proportionate relationship are as follows: L1: D1=(0.05~100): 1.
Difference between " side wall " and " inner sidewall " of the invention are as follows: the inner surface of " inner sidewall " expression " side wall ".
Under preferable case, L1: D1=(0.1~30): 1.
The jacket structured design of the invention, enables to heat-conducting medium to circulate in shell, is guaranteeing that electric discharge is strong Entire reactor can be made to maintain in certain temperature range while spending, make the sulphur generated outflow reactor in liquid form, It can effectively avoid hydrogen sulfide from decomposing the sulphur solidification generated, this decomposable process can be made to hold while reaching higher conversion ratio Continuous, stable realization long-term operation.
The grounding electrode of the invention can be coated on the inner sidewall of the inner cylinder in the form of coating.Or this hair At least partly tube structure of the bright inner cylinder forms the grounding electrode namely the grounding electrode both serves as electrode structure It is formed simultaneously the side wall construction of inner cylinder again.
The block media of the invention is arranged on at least partly outer surface of the central electrode, the block media It can be fixed in a manner of any be capable of fixing on the outer surface of the central electrode, alternatively, the block media can also be with On outer surface in the form of coating coated on the central electrode.
Preferably, the material for forming the block media is electrically insulating material, and forms the material choosing of the block media From at least one of glass, ceramics, enamel, polytetrafluoroethylene (PTFE) and mica.The glass can be quartz glass or hard glass Glass；The material for forming the block media can also be other metals and nonmetallic composite with high voltage electrical isolation design Deng.The ceramics can be aluminium oxide ceramics.
Preferably, which further includes ground line, and the ground line is arranged on the lateral wall of the outer cylinder, and one end It is connect with the grounding electrode.
Preferably, the top of the inner cylinder is arranged in the reactor inlet, and the product exit is arranged in the inner cylinder Lower part and/or bottom.
According to a kind of preferred embodiment, the product exit includes that product gas outlet and product liquid go out Mouthful, and the lower part of the inner cylinder is arranged in for the product gas outlet and the liquid product outlet is arranged in the inner cylinder Bottom.
Under preferable case, the setting direction of the reactor inlet makes the gas entered by the reactor inlet along institute The tangential direction for stating inner cylinder enters in the inner cylinder；And under preferable case, the setting direction of the product gas outlet makes Tangential direction of the gas by the product gas outlet along the inner cylinder in inner cylinder draws the inner cylinder.Of the invention is preferred anti- Answering the setting direction of device entrance and product gas outlet to be conducive to unstripped gas, helically formula direction moves in the inner cylinder, thus It is able to extend mean residence time of the gas in inner cylinder.
The internal diameter of the inner cylinder of the invention and the ratio between the aperture of the product exit can be (0.1~100): 1.
The aperture of the reactor inlet of the invention and the ratio between the aperture of the product exit can be (0.1~120): 1。
Ratio between the length of the inner cylinder of the invention and the internal diameter of the inner cylinder can be (0.5~500): 1.
Preferably, the product gas outlet is arranged in the lower section of the region of discharge, and the product gas outlet Height H of the position relative to the inner cylinder bottom is set1With the length L of the region of discharge2Between proportionate relationship are as follows: H1: L2 =1:(0.05~25000)；Preferably H1: L2=1:(0.1~10000)；More preferably H1: L2=1:(0.5~1000).
Preferably, the heat-conducting medium entrance and heat-conducting medium outlet are separately positioned on the lower part of the outer cylinder and upper Portion.
In the present invention, to the internal diameter ratio between the inner barrel and outer barrel, there is no particular limitation, main in the inner cylinder For occurring to vulcanize hydroperoxide decomposition reaction, and the outer cylinder is mainly used for providing required temperature for the decomposition reaction in inner cylinder, therefore, Those skilled in the art can adjust according to the purposes and select the internal diameter ratio between suitable inner barrel and outer barrel.
The internal diameter of the invention indicates diameter.
Preferably, the material for forming the grounding electrode is selected from graphite-pipe, metal tube, metal foil or metal mesh.The present invention Solid grounding electrode, cooperate the structure of plasma reactor of the invention, generated under conditions of injecting power is certain Micro discharge electric current is bigger, is more advantageous to the scission of link decomposition reaction of hydrogen sulfide.Form the metal tube in the material of the grounding electrode It may include elemental metals pipe, elemental metals foil, alloying metal pipe, alloying metal foil with metal foil.The present inventor's hair It is existing, when being circumferentially positioned on the inner sidewall of the inner cylinder using solid conductive material as grounding electrode, enable to using this When the plasma reactor that invention provides carries out vulcanization hydroperoxide decomposition reaction, the conversion ratio of hydrogen sulfide improves more significantly.
The material for forming the central electrode is conductive material, it is preferable that the material for forming the central electrode is selected from stone At least one of Mo Guan, graphite powder, metal bar, metal tube, metal powder and graphite rod.The metal bar, metal tube can wrap Elemental metals stick, alloying metal stick, elemental metals pipe, alloying metal pipe are included, metal powder may include elemental metals powder, alloy gold Belong to the mechanical impurity of powder or elemental metals powder and/or alloying metal powder.The material of the formation central electrode of the invention has It can be the rodlike and tubular material of other conductive energy.
The present invention can be introduced thermally conductive by the region between the lateral wall of the inner cylinder and the inner sidewall of the outer cylinder Medium and the temperature for the reactor for having jacket structured is maintained between such as 119~444.6 DEG C, to guarantee hydrogen sulfide point The sulphur that solution generates flows out region of discharge in liquid form.
Can also be filled in the plasma reactor of the invention can catalysed curing hydrogen resolve into elemental sulfur and The catalyst of hydrogen, the catalyst are preferably seated in the reactor inner cylinder.Filling body of the present invention to the catalyst Product and filling type do not require particularly, about the type of catalyst, for example, can for CN102408095A, In catalyst disclosed in CN101590410A and CN103495427A any one or it is a variety of.
As previously mentioned, the second aspect of the present invention provides a kind of method of decomposing hydrogen sulfide, this method is aforementioned first Implement in plasma reactor described in aspect, this method comprises: hydrogen sulfide will be contained under the conditions of dielectric barrier discharge Unstripped gas carries out the decomposition reaction of hydrogen sulfide from the inner cylinder that reactor inlet is introduced to the plasma reactor, after decomposition The logistics of acquisition is drawn by the product exit, also, by continuing from heat-conducting medium entrance to the plasma reactor Outer cylinder in introduce heat-conducting medium and the heat-conducting medium drawn by heat-conducting medium outlet and maintains the plasma reaction Temperature needed for device, the dielectric barrier discharge are formed by grounding electrode, block media and central electrode.
The plasma reactor provided by the invention does not have the condition of decomposition reaction involved in decomposing hydrogen sulfide Special limitation can come for various conditions involved in the plasma decomposing hydrogen sulfide method in the art routinely used It is decomposed, lists to the embodiment of the present invention exemplary partial the condition of decomposing hydrogen sulfide, those skilled in the art do not answer It is interpreted as limitation of the present invention.
In the present invention, to the material of the formation outer cylinder, there is no particular limitation, as long as forming the material of the outer cylinder It is able to bear the set temperature of heat-conducting medium.
The plasma reactor provided by the invention does not have the concentration of the hydrogen sulfide in the gas at reactor inlet There is special restriction, such as the concentration of hydrogen sulfide can be 0.01~100 volume % in gas.This hair is provided below in conjunction with Fig. 1 A kind of structure of preferred embodiment of bright plasma reactor, specifically:
The reactor has coaxial collet core structure, and the reactor includes:
Inner cylinder 1 is respectively arranged with reactor inlet 11 and product exit on the inner cylinder 1；
Outer cylinder 2, the outer cylinder 2 is nested in the outside of the inner cylinder 1, and is respectively arranged with heat-conducting medium on the outer cylinder 2 Entrance 21 and heat-conducting medium outlet 22；
Central electrode 3, the central electrode 3 are arranged in the inner cylinder 1；
Grounding electrode 4, the material for forming the grounding electrode 4 is solid conductive material, and the grounding electrode 4 forms inner cylinder 1 at least partly side wall or the grounding electrode 4 is circumferentially positioned on the inner sidewall of the inner cylinder 1；And
Block media 6, the block media 6 is arranged on at least partly outer surface of the central electrode 3, so that at least It partially protrudes into and is enclosed with the block media 6 and the block media on the outer surface of the central electrode 3 in the inner cylinder 1 Setting position make the region of discharge between the central electrode and the grounding electrode by the block media interval；
Wherein, the distance between inner sidewall of the lateral wall of the block media 6 and the grounding electrode 4 L1With the resistance Keep off the thickness D of medium1Proportionate relationship are as follows: L1: D1=(0.05~100): 1；It is preferred that L1: D1=(0.1~30): 1.
It is preferred that the reactor further includes ground line 5, the ground line 5 is arranged on the lateral wall of the outer cylinder 2, and one end It is connect with the grounding electrode 4.
It is preferred that the top of the inner cylinder 1 is arranged in the reactor inlet 11, the product exit is arranged in the inner cylinder 1 Lower part and/or bottom.
Under preferable case, the product exit includes product gas outlet 12 and liquid product outlet 13, and the gas The lower part of the inner cylinder 1 is arranged in product exit 12 and the bottom of the inner cylinder 1 is arranged in the liquid product outlet 13.
Preferably, the lower section of the region of discharge containing block media, and the gas is arranged in the product gas outlet 12 Height H of the setting position of body product exit 12 relative to 1 bottom of inner cylinder1With the region of discharge containing block media Length L2Between proportionate relationship are as follows: H1: L2=1:(0.05~25000)；Preferably H1: L2=1:(0.1~10000)；More Preferably H1: L2=1:(0.5~1000).
It is preferred that the heat-conducting medium entrance 21 and the heat-conducting medium outlet 22 be separately positioned on the outer cylinder 2 lower part and Top.
The preferred specific reality of another application present invention presented below plasma reactor decomposing hydrogen sulfide above-mentioned Apply mode:
It is passed through nitrogen into the inner cylinder of plasma reactor from reactor inlet, to remove the air in region of discharge, And gas is drawn from product exit.Meanwhile heat-conducting medium, the heat-conducting medium of introducing are introduced into outer cylinder from heat-conducting medium entrance It exports and draws from heat-conducting medium.The temperature of heat-conducting medium remains the temperature of system response needs.Then from reactor inlet to It is passed through the unstripped gas containing hydrogen sulfide in the inner cylinder of plasma reactor, steadily connects high voltage power supply later to flow of feed gas, Make to form plasma discharge field between central electrode and grounding electrode by adjusting voltage and frequency.Hydrogen sulfide gas is discharging Region ionizes, and is decomposed into hydrogen and elemental sulfur, and the elemental sulfur for generation of discharging slowly is flowed down along inner tube wall, and from product exit Outflow.
Plasma reactor provided by the invention also has the advantages that following specific:
(1) reactor uses conductive solids material as grounding electrode, compared with liquid grounding electrode, such ground connection electricity The micro discharge electric current that electric discharge generates when pole cooperates structure of the invention is bigger, and the electric discharge for being more advantageous to hydrogen sulfide molecule is decomposed instead It answers.
(2) setting is jacket structured on the outside of reactor grounding electrode, can by heat-conducting medium temperature in control collet come pair Reactor carries out temperature control, and hydrogen sulfide electric discharge can be made to decompose the sulphur generated and smoothly flow out region of discharge, avoid sulphur solidification stifled Reactor is filled in, continual and steady progress of discharging is made.
(3) reactor by control between the lateral wall of the central electrode and the inner sidewall of the grounding electrode away from From L1With the thickness D of the block media1Proportionate relationship are as follows: L1: D1=(0.05~100): 1, preferably L1: D1=(0.1~ 30): 1, cooperate remaining structure of reactor of the invention, enables to the conversion ratio of hydrogen sulfide to significantly improve and decompose energy consumption drop It is low.
The present invention will be described in detail by way of examples below.In following embodiment, in the feelings being not particularly illustrated Under condition, the various raw materials used are all from commercially available.
The thickness of block media in following embodiment and comparative example is all the same.
The conversion ratio of hydrogen sulfide is calculated according to the following formula in following instance:
Molal quantity/premature cure hydrogen molal quantity × 100% of the hydrogen sulfide of the conversion ratio %=conversion of hydrogen sulfide
The energy consumption of decomposing hydrogen sulfide is detected by oscillograph and is calculated using Lissajou's figure and obtained in following instance.
Embodiment 1
Vulcanization hydroperoxide decomposition reaction, the specific knot of plasma reactor are carried out using plasma reactor shown in FIG. 1 Structure and structural parameters are as follows:
Reactor includes:
Inner cylinder is respectively arranged with reactor inlet, product gas outlet and liquid product outlet on the inner cylinder；
Outer cylinder, the outer cylinder is nested in the outside of the inner cylinder, and heat-conducting medium entrance is respectively arranged on the outer cylinder It is exported with heat-conducting medium；
The axial centerline of the inner cylinder is arranged in central electrode, the central electrode, forms the central electrode Material is stainless steel metal stick；
Grounding electrode, the grounding electrode are arranged on the inner sidewall of the inner cylinder, form the material of the grounding electrode For stainless steel metal foil, and the lower edge of the central electrode in the present embodiment is lower than the lower edge of the grounding electrode；
The appearance for the part that the central electrode stretches in the inner cylinder is arranged in block media, the block media On face, and the upper edge of block media is higher than the upper edge of grounding electrode, and the material for forming the block media is hard glass.
The distance between the inner sidewall of the lateral wall of the block media and grounding electrode L1With the thickness of block media Spend D1Ratio be 8:1；
H1With the length L of the region of discharge containing block media2Between proportionate relationship are as follows: H1: L2=1:40；
The volume of the reactor inner cylinder of the present embodiment is 0.2L.
Gaseous mixture enters in reactor inner cylinder from the top of reactor inner cylinder in the present embodiment, and from positioned at reactor inner cylinder The product gas outlet of lower part draws gaseous product, and elemental sulfur is drawn from the liquid product outlet for being located at reactor bottom；And The heat-conducting medium of the present embodiment is introduced from the lower part of the outer cylinder of reactor, and is drawn from the top of the outer cylinder of reactor.
The operating procedure of plasma reactor:
It is passed through nitrogen into the inner cylinder of plasma reactor from reactor inlet, to remove the air in region of discharge, And gas is drawn from product gas outlet and liquid product outlet.Meanwhile it being introduced from heat-conducting medium entrance into outer cylinder thermally conductive Medium (specially dimethicone), the heat-conducting medium of introducing is exported from heat-conducting medium draws, and the temperature of heat-conducting medium remains 145℃。
Then H is passed through into the inner cylinder of plasma reactor from reactor inlet2S/Ar gaseous mixture, wherein H2S volume point Number be 20%, control gaseous mixture flow velocity make gas region of discharge mean residence time be 9.2s.H2S/Ar gaseous mixture is passed through After reactor 30min, ac high voltage source is connected, makes to be formed between central electrode and grounding electrode by adjusting voltage and frequency Plasma discharge field.Wherein discharging condition are as follows: voltage 18.5kV, frequency 1.5kHz, electric current 1.05A.Stink damp Body is ionized in region of discharge, is decomposed into hydrogen and elemental sulfur, and the elemental sulfur for generation of discharging slowly is flowed down along inner tube wall, and from Liquid product outlet outflow.Gas is flowed out from product gas outlet after reaction.
As a result: the vulcanization hydroperoxide decomposition reaction of the present embodiment measures H after persistently carrying out 20min2S conversion ratio is 74.2%；And Continuous discharge 100h has not yet to see exception, discharge condition and H2S conversion ratio keeps stable.And the decomposition energy consumption of the present embodiment is 12.5eV/H2S molecule (1 molecule H of every decomposition2The energy that S needs is 12.5eV).
Comparative example 1
This comparative example carries out vulcanization hydroperoxide decomposition reaction using plasma reactor similar to Example 1, different It is:
Grounding electrode in this comparative example is liquid grounding electrode, and be molten condition molar ratio be 1:1 LiCl with AlCl3, which is also heat-conducting medium, and keeping temperature is 145 DEG C, and is placed in reactor outer cylinder.
Control gaseous mixture flow velocity make gas region of discharge mean residence time be 20.1s.
The volume of the reactor inner cylinder of this comparative example is 0.05L.
Remaining is in the same manner as in Example 1.
And this comparative example carries out vulcanization hydroperoxide decomposition reaction using operating method same as Example 1.
As a result: the vulcanization hydroperoxide decomposition reaction of this comparative example measures H after persistently carrying out 20min2S conversion ratio is 16.0%, is held H after continuous electric discharge 1.5h2S conversion ratio is reduced to 6.3%.
The decomposition energy consumption of this comparative example is 105eV/H2S molecule.
Comparative example 2
This comparative example is carried out using plasma reactor similar with comparative example 1, except that:
The distance between the inner sidewall of the lateral wall of block media in this comparative example and grounding electrode L1With block media Thickness D1Ratio be 0.01:1.
Control gaseous mixture flow velocity make gas region of discharge mean residence time be 20.1s.
The volume of the inner cylinder of this comparative example is 0.02L.
Remaining is identical with comparative example 1.
As a result: the vulcanization hydroperoxide decomposition reaction of this comparative example measures H after persistently carrying out 20min2S conversion ratio is 21.8%, is held H after continuous electric discharge 1.5h2S conversion ratio is reduced to 5.8%.
The decomposition energy consumption of this comparative example is 141eV/H2S molecule.
Embodiment 2
The present embodiment carries out the decomposition reaction of hydrogen sulfide using plasma reactor similar to Example 1, different It is, in the present embodiment:
Whole side walls of inner cylinder are formed by grounding electrode, and the material for forming the grounding electrode is stainless steel metal foil；
The distance between the lateral wall of block media and the inner sidewall (being also the inner sidewall of inner cylinder) of the grounding electrode L1With the thickness D of block media1Ratio be 25:1；
H1With the length L of the region of discharge containing block media2Between proportionate relationship are as follows: H1: L2=1:120.
H is passed through into the inner cylinder of plasma reactor from reactor inlet in the present embodiment2S/Ar gaseous mixture, wherein H2S Volume fraction is 30%, control gaseous mixture flow velocity make gas region of discharge mean residence time be 8.5s.H2S/Ar mixing After gas is passed through reactor 30min, connect ac high voltage source, by adjust voltage and frequency make central electrode and grounding electrode it Between formed plasma discharge field.Wherein discharging condition are as follows: voltage 19.5kV, frequency 5.5kHz, electric current 1.45A.
Remaining is in the same manner as in Example 1.
As a result: the vulcanization hydroperoxide decomposition reaction of the present embodiment measures H after persistently carrying out 20min2S conversion ratio is 73.5%；And Continuous discharge 100h has not yet to see exception, discharge condition and H2S conversion ratio keeps stable.And the decomposition energy consumption of the present embodiment is 13.2eV/H2S molecule.
Embodiment 3
The present embodiment carries out the decomposition reaction of hydrogen sulfide using plasma reactor similar to Example 1, different It is, in the present embodiment:
The grounding electrode is arranged on the inner sidewall of the inner cylinder, and the material for forming the grounding electrode is copper foil；
Block media is arranged in the central electrode and stretches on the outer surface of the part in the inner cylinder, and stops to be situated between The upper edge of matter is higher than the upper edge of grounding electrode, forms the material of the block media as ceramics；
The distance between the inner sidewall of the lateral wall of block media and grounding electrode L1With the thickness D of block media1's Ratio is 0.7:1；
H1With the length L of the region of discharge containing block media2Between proportionate relationship are as follows: H1: L2=1:250.
H is passed through into the inner cylinder of plasma reactor from reactor inlet in the present embodiment2S/Ar gaseous mixture, wherein H2S Volume fraction is 25%, control gaseous mixture flow velocity make gas region of discharge mean residence time be 12.5s.H2S/Ar mixing After gas is passed through reactor 30min, connect ac high voltage source, by adjust voltage and frequency make central electrode and grounding electrode it Between formed plasma discharge field.Wherein discharging condition are as follows: voltage 8.5kV, frequency 2.5kHz, electric current 1.08A.
Remaining is in the same manner as in Example 1.
As a result: the vulcanization hydroperoxide decomposition reaction of the present embodiment measures H after persistently carrying out 20min2S conversion ratio is 73.8%；And Continuous discharge 100h has not yet to see exception, discharge condition and H2S conversion ratio keeps stable.And the decomposition energy consumption of the present embodiment is 13.8eV/H2S molecule.
Embodiment 4
The present embodiment carries out the decomposition reaction of hydrogen sulfide using plasma reactor similar to Example 1, different It is, in the present embodiment:
The distance between the inner sidewall of the lateral wall of block media and grounding electrode L1With the thickness D of block media1's Ratio is 35:1.
Remaining is in the same manner as in Example 1.
As a result: the vulcanization hydroperoxide decomposition reaction of the present embodiment measures H after persistently carrying out 20min2S conversion ratio is 71.0%；And Continuous discharge 100h has not yet to see exception, discharge condition and H2S conversion ratio keeps stable.And the decomposition energy consumption of the present embodiment is 23.8eV/H2S molecule.
Using energy when the decomposition of plasma reactor provided by the invention progress hydrogen sulfide it can be seen from the above results Enough conversion ratios for improving hydrogen sulfide compared with the existing technology significantly and reactor provided by the invention can be in low decomposition High hydrogen sulfide conversion ratio is kept to long period under energy consumption.
The preferred embodiment of the present invention has been described above in detail, and still, the present invention is not limited thereto.In skill of the invention In art conception range, can with various simple variants of the technical solution of the present invention are made, including each technical characteristic with it is any its Its suitable method is combined, and it should also be regarded as the disclosure of the present invention for these simple variants and combination, is belonged to Protection scope of the present invention.

Claims (11)

1. a kind of plasma reactor, which has coaxial collet core structure, and the reactor includes:
Inner cylinder (1) is respectively arranged with reactor inlet (11) and product exit on the inner cylinder (1)；
Outer cylinder (2), the outer cylinder (2) are nested in the outside of the inner cylinder (1), and are respectively arranged on the outer cylinder (2) thermally conductive Medium inlet (21) and heat-conducting medium outlet (22)；
Central electrode (3), the central electrode (3) are arranged in the inner cylinder (1)；
Grounding electrode (4), the material for forming the grounding electrode (4) is solid conductive material, in grounding electrode (4) formation At least partly side wall or the grounding electrode (4) of cylinder (1) are circumferentially positioned on the inner sidewall of the inner cylinder (1)；And
Block media (6), the block media (6) is arranged on at least partly outer surface of the central electrode (3), so that extremely The block media (6) and described is enclosed on the outer surface for the central electrode (3) that small part protrudes into the inner cylinder (1) The setting position of block media makes the region of discharge between the central electrode and the grounding electrode by the block media Interval；
Wherein, the distance between the lateral wall of the block media (6) and the inner sidewall of the grounding electrode (4) L1With the resistance Keep off the thickness D of medium1Proportionate relationship are as follows: L1: D1=(0.05~100): 1.
2. plasma reactor according to claim 1, wherein L1: D1=(0.1~30): 1.
3. plasma reactor according to claim 1 or 2, wherein it is exhausted for electricity to form the material of the block media Edge material；Preferably,
Form at least one of the material of the block media in glass, quartz, ceramics, enamel, polytetrafluoroethylene (PTFE) and mica Kind.
4. plasma reactor according to claim 1 or 2, wherein the reactor further includes ground line (5), described Ground line is arranged on the lateral wall of the outer cylinder (2), and one end is connect with the grounding electrode (4).
5. plasma reactor according to claim 1 or 2, wherein the reactor inlet (11) is arranged described The top of inner cylinder (1), the product exit are arranged in the lower part and/or bottom of the inner cylinder (1).
6. plasma reactor according to claim 5, wherein the product exit includes product gas outlet (11) With liquid product outlet (12), and lower part in the inner cylinder (1) and the liquid is arranged in the product gas outlet (11) Product exit (12) is arranged in the bottom of the inner cylinder (1).
7. plasma reactor according to claim 6, wherein product gas outlet (12) setting is put described The lower section in electric region, and height H of the setting position of the product gas outlet (12) relative to the inner cylinder (1) bottom1With The length L of the region of discharge2Between proportionate relationship are as follows: H1: L2=1:(0.05~25000)；Preferably H1: L2=1:(0.1 ~10000)；More preferably H1: L2=1:(0.5~1000).
8. plasma reactor described in any one of -3 according to claim 1, wherein the heat-conducting medium entrance (21) The lower part and top of the outer cylinder (2) are separately positioned on heat-conducting medium outlet (22).
9. plasma reactor according to claim 1, wherein the material for forming the grounding electrode (4) is selected from stone Mo Guan, metal tube, metal foil or metal mesh.
10. plasma reactor according to claim 1, wherein the material for forming the central electrode (3) is selected from stone At least one of Mo Guan, graphite powder, metal bar, metal tube, metal powder and graphite rod.
11. a kind of method of decomposing hydrogen sulfide, plasma reaction of this method described in any one of claim 1-10 Implement in device, this method comprises: introducing the unstripped gas containing hydrogen sulfide from reactor inlet under the conditions of dielectric barrier discharge The decomposition reaction of hydrogen sulfide is carried out into the inner cylinder of the plasma reactor, the logistics obtained after decomposition is gone out by the product Mouthful draw, also, by continue introduced from heat-conducting medium entrance into the outer cylinder of the plasma reactor heat-conducting medium with And the heat-conducting medium is drawn as heat-conducting medium outlet and temperature needed for maintaining the plasma reactor, the medium resistance Gear electric discharge is formed by grounding electrode, block media and central electrode.
CN201810136792.3A 2018-02-09 2018-02-09 The method of plasma reactor and decomposing hydrogen sulfide Pending CN110127604A (en)

Priority Applications (5)

Application Number Priority Date Filing Date Title
CN201810136792.3A CN110127604A (en) 2018-02-09 2018-02-09 The method of plasma reactor and decomposing hydrogen sulfide
RU2020127670A RU2753275C1 (en) 2018-02-09 2019-01-31 Apparatus for executing low-temperature plasma reaction and method for decomposing hydrogen sulphide
US16/968,785 US11691119B2 (en) 2018-02-09 2019-01-31 Low temperature plasma reaction device and hydrogen sulfide decomposition method
CN201980004595.9A CN111278766B (en) 2018-02-09 2019-01-31 Low temperature plasma reaction apparatus and method for decomposing hydrogen sulfide
PCT/CN2019/074087 WO2019154245A1 (en) 2018-02-09 2019-01-31 Low temperature plasma reaction device and hydrogen sulphide decomposition method

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