CN1754615A - Photoelectricity catalytic reactor for degrading organic contaminant and degradation method - Google Patents
Photoelectricity catalytic reactor for degrading organic contaminant and degradation method Download PDFInfo
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Abstract
This invention discloses one photoelectric reactor to degrade organic pollute and one method to remove the pollute assistant with catalyze reactor, wherein, the reactor is located with conductive multi-hole materials load compound semi-conductor photo catalyze positive and negative electrodes; the optimized catalyze can be used as light source; it uses conductive solid electrolyte applied to degrade pollute with gas and liquid and to separate metal ions.
Description
Technical field
The present invention relates to a kind of photoelectric-synergetic catalytic reactor, be specifically related to be used for the photo electrocatalysis reactor and the biodegrading process of degradable organic pollutant.
Background technology
In household, public place of entertainment (as the dance hall etc.), the automobile etc. indoor have that ornament materials etc. discharges as harmful volatile organic matters such as formaldehyde, also have volatility stink with perspiration and detrimental microorganisms bacterium and the virus of organism.These pernicious gases not only damage people's physiological function, have also increased pathophorous chance, and it is particularly important to people's health therefore to solve the room air pollution problem.
The fragrance type air purifier that uses has just been covered organic unhappy smell at present, can not eliminate its harmfulness.
Another method is absorption, as with the organic molecule in the activated carbon granule adsorbed gas, but that this process just becomes vapor phase contaminants is solid-state, can not degradable organic pollutant, also caused the diffusion of solid pollution, and it also is subjected to the restriction of adsorption capacity.
As the method for removing organic pollution in the gas, except that conductor photocatalysis, a kind of method of utilizing electrion and electrostatic precipitation is arranged, this method is mainly used in fixedness organic pollution and the floating dust in the gas, in reducing air, aspect the bulky grain pollutant good result is arranged, but it can not decompose strong adsorb volatile organic pollution.The ozone that the electrion process produces plays bactericidal action when concentration is lower than 0.12ppm, but when surpassing this concentration, human respiratory tract and eyes mucous membrane is had infringement.And be accompanied by the generation of nitrogen oxide in the discharge generation ozone process.Also human body is worked the mischief.Therefore this method is operated in confined space, can increase the risk of human health.
Electrochemical process is handled organic and inorganic pollution can only carry out at the aqueous solution at present, the heavy metal ion that its energy anodic oxidation and cathodic reduction are inorganic etc., make it to produce precipitation or appraise at the current rate and reduce toxicity, handling organic matter can only the oxidation or the organic particular functional group that reduces, but general thorough degradation of organic substances.
According to Semiconductive Theory, semiconductor has band structure, constitute by valence band of filling up electronics and empty conduction band, have the forbidden band between valence band and the conduction band, when penetrating semiconductor with energy more than or equal to the illumination of energy gap, the electronics on the valence band is excited and transits to conduction band and produce the hole, photohole has very strong oxidability, light induced electron has very strong reducing power, if there is the suitable electronics electron donor that advocated peace near electronics and hole, then oxidation and reduction reaction can take place.The adsorbent of positive electricity hole oxidation on it, for example volatile organic compound is as the electron donor, organic compound is remaining hole in their the electronation valence band, thereby oxidized decomposition, like this, organic pollution finally is oxidized to carbon dioxide and water.And the free electron of conduction band carries out reduction reaction, and airborne oxygen is converted to active oxygen, and active oxygen also has strong oxidisability, and energy and organic compound reaction finally generate carbon dioxide and water.(Fujishima，A?and?Honda，K，Nature，1972，vol.37，：pp328)
Light-catalyzed reaction mechanism can be referring to accompanying drawing 1.
Photohole on the photoactivation semiconductor valence band, photocatalytic oxidation is because the strong oxidizing property of photohole, as titanium dioxide, its current potential reaches 3.2v, 2.07v than ozone is much higher, and thoroughly degradable organic pollutant makes it permineralization and generates carbon dioxide and water, and agent almost do not have selectivity, so can make many pollutant mineralisings (inorganicization) that are difficult to degrade.Degradation process can be carried out at normal temperatures and pressures, does not need to add chemical reagent, and non-secondary pollution is easy and simple to handle, raw material and low power consumption and other advantages and receive publicity.But lose activity because photohole is very easily compound, quantum efficiency is low, has limited its application.Simultaneously, the valence band of titanium dioxide and the energy level difference between conduction band have determined it to absorb light and have been in the black light district.
Titanium dioxide has good chemistry and biologically inert, can guarantee safe and cheap and easy to get.Therefore, adopt titanium dioxide semiconductor electrode and platinum electrode to form electrochemical system from Fujishima report in 1972 and make water decomposition hydrogen and oxygen, cause the great attention of Chinese scholars.Nineteen eighty-three Davidollis clearly proposes to adopt the conductor photocatalysis degradation of organic substances as method for treating water, indicates that light-catalysed development enters second stage.Over more than 20 year.The researcher of various countries has carried out extensive and deep research in this field, has obtained many achievements.But having got long long way to go aspect raising visible light activity and the catalytic efficiency.The research of most photocatalysis aspect is to carry out in the suspension system, suspension liquid ties up to and exists catalyst to be difficult to separate and the problem that reclaims difficulty in the use, has become titanium dioxide etc. in fact and has been difficult to one of business-like reason for the photocatalytic method of matrix.
The efficient that improves optically catalytic TiO 2 is paid close attention in a large amount of research.And that the subject matter of this process is quantum efficiency is too low, has only usually on the order of magnitude of a few percent.Light induced electron on the photoactivation semiconductor conduction band and the photohole on the valence band, except that respectively with the catalyst surface adsorption site on the organic matter of ADSORPTION STATE carry out the chemical reaction, simple composite always takes place, reaction and compound competition, determined the quantum efficiency of process, the fundamental way that as seen improves quantum efficiency is to stop light induced electron and hole that simple composite takes place.Highly purified titanium dioxide can reduce the density at the simple composite center that is formed by impurity center, and ultra-fine particle diameter has dimensional effect, and the two all helps improving quantum efficiency.U.S. Pat discloses a kind of method No. 5126111, carries out light-catalyzed reaction in ozone or the environment through the oxygen of ozone treatment and hydrogen peroxide, to suppress the compound of electronics and hole.
If as optoelectronic pole, light induced electron can more effectively be separated with hole (carrier) in the semiconductor under the effect of extra electric field the conductor of surface coverage titanium deoxid film, this electric field enhancement effect has reduced simple composite significantly.When photochemical catalyst is applied voltage, the electric field of formed Schottky potential barrier, light induced electron and hole are moved in the opposite direction in electromigratory mode, realize separating, wherein a part can arrive at semiconductor surface and carries out chemical reaction before simple composite.
The research report of at present relevant photoelectrocatalysis is mainly used in the degraded of organic pollution in the aqueous solution, does not see the organic pollution that is useful in the degraded gas phase.
Chinese patent CN1438913A (application number: 01810959.4) proposed a photoelectro catalytic system and removed the device of air pollutants, but this device does not comprise electrolyte, therefore the voltage that need apply the 3000-20000 volt must contain the device that voltage promotes to discharge electrode.Still belong to the high-pressure electrostatic treating apparatus.
Under the above-mentioned situation, the inventor considers the problem that existing charcoal absorption, electrion system, photocatalytic system, electric catalyticing system, high pressure photoelectro catalytic system exist, electrode and solid electrolyte that photochemical catalyst is arranged by application load, develop a kind of new photoelectric-synergetic catalytic reaction system, it is mainly used in degradation of organic substances, the inorganic matter of also can degrading mainly is applicable to gaseous fluid, also is applicable to liquid fluid.
Summary of the invention
The purpose of this invention is to provide a kind of new photoelectric-synergetic catalyst reaction device, it is equipped with the porous anode and the negative electrode of load composite semiconductor light-catalyst on the conductive porous material, the catalyst of optimizing can use visible light as light source, and the solid electrolyte that uses conduction solid polymer electrolyte especially, the organic pollution especially organic pollution and the separation and Extraction metal ion of gas of gas and liquid can be applicable to degrade, reactor provides the novel internal geometrical construction, disposes the organic matter content detection device in case of necessity.
The photo electrocatalysis reactor that is used for degradable organic pollutant of the present invention comprises:
Anode with anodal feature;
Negative electrode with negative pole feature;
The solid electrolyte of separating anode and negative electrode;
Above-mentioned plate-load photochemical catalyst;
Above-mentioned cathode load composite catalyst;
Be installed in the ultraviolet or the visible light source on electrode opposite;
Be used for providing the power supply of Dc bias for electrode.
Above-mentioned anode carrier is made of porous conductive material, and porous material comprises porous carbon cloth, porous graphite plate, copper, the stainless (steel) wire that nickel foam, acetylene black and graphite powder add polytetrafluoroethylene (PTFE) and cohere.
Above-mentioned anode porous conductive material surface and internal load have catalyst.
The photochemical catalyst of above-mentioned plate-load is composited by light-sensitive coloring agent and semiconductor, and above-mentioned semiconductor is transition metal Ti, W, Fe, Cr, Ni, Cu, Cd, Mn, Sn, V, rare-earth metal La, Eu, Ce, Er, precious metals pt, Au, Pd, the metal oxide or the sulfide of a kind of oxide of Ag or sulfide, the composite gained of multiple slaine.
Above-mentioned negative electrode is made up of conductive layer, watertight composition, Catalytic Layer; Conductive layer comprises carbon cloth, graphite, nickel, copper, stainless (steel) wire; Watertight composition graphitiferous powder, acetylene black, polytetrafluoroethylene (PTFE) binder; Load has pair hydrogen reduction to become hydrogen peroxide that catalytic activity is arranged and has that the catalyst of photocatalytic activity is composite to have constituted cathode catalysis layer, and wherein oxygen reduction catalyst is made up of the transition metal macrocyclic complex.
Above-mentioned electrolyte is an especially solid polymer electrolyte of solid electrolyte.
The chamber wall that inside reactor has illumination to arrive, photochemical catalyst in the load is to increase degradation efficiency.
Reactor can be applicable to gaseous fluid, installs to the following side is an air inlet, and top is the gas outlet, utilizes the different generation of cold and hot density convection current to finish exchange gas, also circulation fan can be installed, and air inlet and gas outlet are installed dust and filtered collecting net.
The biodegrading process that is used for the photo electrocatalysis reactor of degradable organic pollutant of the present invention may further comprise the steps:
(1) contains the photochemical catalyst of fluid by on anode carrier, being coated with of organic pollution, photochemical catalyst is penetrated in illumination and is produced photohole and light induced electron down, under electric field action, effectively separated, photohole on the anode and organic matter effect with high oxidation activity, organic matter is oxidized, and final catabolite is carbon dioxide and water;
(2) light induced electron moves to negative electrode under electric field action, contain organic fluid by the negative electrode composite catalytic layer, oxygen at negative electrode by electrical catalyze reduction, generate hydrogen peroxide, penetrate down in illumination, hydrogen peroxide and photochemical catalyst effect generate the OH free radical with high oxidation activity, organic matter and the oxidized degraded of free radical effect, final catabolite is carbon dioxide and water;
(3) solid polymer electrolyte places the both sides of negative electrode and anode, with the hydraulic press compacting in flakes;
(4) anode and cathode side only can enter fluid from the import of reactor with sealings such as transparent material such as quartz glass, carry out photoelectric catalysis degrading through negative electrode and anode successively, leave from outlet then, to increase fluid photoelectrocatalysis time in reactor.
Photo electrocatalysis reactor of the present invention: have the anode of the anodal characteristic of oxidation, load has composite semiconductor light-catalyst on the porous conductive material; Negative electrode with negative pole characteristic of reduction, load have pair light to become hydrogen peroxide that the catalyst of catalytic activity is arranged with hydrogen reduction; Separate with solid electrolyte between anode, the negative electrode; Be used for providing the power supply of Dc bias (0--10V) for electrode; Be installed in ultraviolet or the visible light source and the line related of electrode right opposite.Dust filters gatherer, the device that impels fluid to flow.
The present invention has also comprised the agent of preparation photoelectrocatalysis and catalyst cupport has been arrived porous conductive material, adopts methods such as electrophoresis, sol-gel, electrochemical oxidation that the catalyst of requirement is fixed on the porous conductive material.The present invention also provides to increase when impelling fluid by photo electrocatalysis reactor and has contacted to react fully with catalyst.
Energy level difference between titanium dioxide valence band and conduction band, determined its absorption to be in the black light district, therefore, the light source of normal light catalyst is selected uviol lamp for use, the present invention is by compound with semiconductors such as light-sensitive coloring agent and titanium dioxide, make absorption spectrum move to visible region, therefore can select visible light source for use, also can utilize sunshine.
Catalyst with microcellular structure high surface, the organic matter in the energy preferential adsorption fluid, anode, negative electrode participate in the organic reaction of photoelectric-synergetic catalytic degradation simultaneously, and degradation efficiency is improved greatly.
Aspect anode, owing under effect of electric field, reduced the activation energy that is adsorbed on electrode surface and the reaction of inner organic matter degradation, degradation reaction is carried out, add photocatalytic degradation, the degradation efficiency of anode is improved greatly.
Aspect negative electrode, because the Catalytic Layer load has pair hydrogen reduction to become hydrogen peroxide to have the catalyst of electro catalytic activity, airborne oxygen catalytic reduction under certain electrode potential in the pole catalyze layer, generate hydrogen peroxide with the steam reaction, hydrogen peroxide is a kind of strong oxidizer, and degradation of organic substances effectively is under the effect of light, the peroxidating Hydrogen Energy generates free radicals such as OH, and participates in organic degraded.
, comprise in gas and the liquid and remove organic pollution in from fluid according to reactor adapted of the present invention,, can remove the organic matter of aldehyde, aromatic series and so on, germ etc. for gas.
The beneficial effect of photoelectrocatalysis electrochemical reactor of the present invention can be removed particle and volatile organic matter, the ozoniferous hidden danger that does not have electrion to bring again, device need not the voltage lifting device, reduce cost, increased security, also saved energy consumption.
Can capture from the photochemical catalyst electrons excited according to electrode of the present invention, stop the compound of electronics and hole, thereby keep the activity of photochemical catalyst for a long time.
Therefore photo electrocatalysis reactor of the present invention can be widely used in industry and civilian owing to have excellent catalytic activity and the structure design.
Description of drawings
Fig. 1 is the schematic diagram that organic pollution is removed in photocatalysis.The reaction mechanism of photocatalysis degradation organic contaminant has been described.
Fig. 2 represents the reaction mechanism schematic diagram according to photoelectric-synergetic catalyze and degrade organic pollutants of the present invention.
Fig. 3 represents the organigram of photo electrocatalysis reactor of the present invention.Be used for gaseous fluid.
Fig. 4 is the comparison diagram of toluene degradation efficiency.
1. ultraviolets or visible light source 2. electrodes 3. catalyst 4. negative electrodes 5. anodes among the above-mentioned figure
6. solid electrolyte 7. power supplys 8. conduits 9. imports 10. outlets
11. transparent material 12. circulating pumps or fan 13. funnel-form pipes, 14. plates
15. dotted line has shown the direction that fluid flows
The specific embodiment
Objects and advantages of the present invention can more fully be understood from next contrast the detailed description that accompanying drawing does.
When the illumination of certain intensity of sending as ultraviolet or visible light source 1 is mapped to and loads on electrode 2 catalyst 3, conduction band (Conduct band) is arrived in electron transition in valence band (Valence band), electronics and hole have been produced, have strong oxidizing property and reproducibility respectively, with airborne water vapour and oxygen reaction, generate living radical, as OH group such as OH, H, O
2 -, H etc., they have the strong respond with other material, the bonding of breaking organic pollution makes it degraded, generates carbon dioxide and water at last.
When photo electrocatalysis reactor was used for gaseous fluid, it comprised:
After fluid enters from the import 9 of negative electrode 4, be directed passing through respectively negative electrode 4, conduit 8, anode 5, leave from the outlet 10 of anode 5 then; All sides of negative electrode 4 and anode 5 are with transparent materials 11 sealings, and it can allow light by shining directly on the catalyst 3, but can prevent that fluid from entering negative electrode 4 and anode 5 from the side.Therefore fluid only can enter from the import 9 of reactor and leave from another outlet 10.
The fluid that contains pollutant also can or be fanned 12 and force by porous electrode by circulating pump, funnel-form pipe 13 be placed on circulating pump or fan 12 and import 9 between.Another piece plate 14 is placed on and enters import 9 and export between 10, mixes with the fluid before and after preventing to react.
Dc source offers electrode, and AC power offers the light source and the circulatory system.
Photochemical catalyst is a kind of material that can be converted into luminous energy chemical energy, and it is made up of the composite semiconductor nanocrystal, and semiconductor comprises valence band V, conduction band D and band gap E, and band gap E has determined the wave-length coverage that light source is required.Photochemical catalyst is selected from the oxide of transition metal, rare earth metal, noble metal and sulfide, as TiO
2,, WO
3, SrTiO
3, Fe
2O
3,, SnO
2, ZnO,, Cu
2O,, AgO, CdS, ZnS, MoS
2, and contain solid super-strong acid and heteropoly acid, light-sensitive coloring agent etc.
Compound purpose is to change band gap E, band gap E as titanium dioxide is 3.2eV, wavelength corresponding to 400nm, therefore, if apply the light that wavelength is shorter than 400 nanometers, the electronics in the valence band is excited, when compound some element such as cerium, silver, tungsten, manganese etc., to form solid solution or eutectic mixture etc., and cause energy level splitting, red shift will take place in its absorbing wavelength.Another method is by means of the strong absorption of light-sensitive coloring agent to visible light, semi-conductive spectral response can be widened the visual field, screens the composite form of catalyst by the Structure Calculation of quantum chemistry.
Ultraviolet or visible light source are installed in the right opposite of electrode, and its power and number can be according to the size adjustment of reactor, and AC power and dc source provide electric energy for respectively light source and electrode.
Explained later is used according to photo electrocatalysis reactor degradable organic pollutant of the present invention.After the Electron absorption luminous energy on the composite semiconductor is greater than band gap E, the photochemical catalyst electronics that is filled among the valence band V will transit to conduction band D, this process is called and excites, form excitation electron and hole, the energy of oxidation in hole is greater than the also proper energy of electronics, organic pollution is accepted in the hole, and oxidative degradation, is degraded to carbon dioxide and water at last.
Photo electrocatalysis reactor of the present invention can long-time steady operation.
The effect of photo electrocatalysis reactor degradable organic pollutant in the preferred working example of the following description of the present invention.
Toluene is put into 20 liters of reactors, its volumetric concentration is 2%, contrasted according to photoelectric catalysis degrading reaction of the present invention, do not apply the photocatalytic degradation reaction of voltage, the simple light degradation reaction that does not have photochemical catalyst, what do not have illumination applies the voltage degradation reaction merely, represents to decompose effect with the resolution ratio of toluene.By the reaction of toluene time in the gas chromatographic analysis reactor.Gas chromatographic detector is the FID type, and inlet temperature is 200 ℃, and furnace temp is 50-200 ℃, and detector temperature is 250 ℃, and carrier gas is a helium, and its flow rate is 10ml/min-20ml/min.
The result as shown in Figure 4, aspect decomposition toluene, for the system that does not have photochemical catalyst, the decomposition efficiency of simple photodegradative toluene is very low, be higher than according to photoelectric-synergetic catalytic degradation efficient of the present invention simple light catalytic degradation efficient 60% and electrochemical reaction degradation efficiency 80%, also be higher than the summation of their degradation efficiencies.The additional electrical energy that consumes for increase degradation efficiency 60% is 15% or lower.
Photo electrocatalysis reactor of the present invention serves many purposes, and the organic pollution that not only can be used to degrade household and public place distribute is in the automobile of also can degrading and the organic pollution that distributes of factory.
As mentioned above, use this photoelectric-synergetic catalytic reactor of solid electrolyte to have to remove the especially advantage of organic pollution in the gas of fluid, although described the present invention with reference to some preferred embodiment, those skilled in the art should be realized that, do not departing under the scope prerequisite of spirit of the present invention, those skilled in the art can be to photo electrocatalysis reactor of the present invention, its manufacture method is made various improvement and change, if therefore these improvement and change then present invention includes these improvement and change in claims and equivalent scope.
Claims (9)
1. photo electrocatalysis reactor that is used for degradable organic pollutant is characterized in that it comprises:
Anode with anodal feature;
Negative electrode with negative pole feature;
The solid electrolyte of separating anode and negative electrode;
Above-mentioned plate-load photochemical catalyst;
Above-mentioned cathode load composite catalyst;
Be installed in the ultraviolet or the visible light source on electrode opposite;
Be used for providing the power supply of Dc bias for electrode.
2. the photo electrocatalysis reactor that is used for degradable organic pollutant according to claim 1, it is characterized in that: above-mentioned anode carrier is made of porous conductive material, and porous material comprises porous carbon cloth, porous graphite plate, copper, the stainless (steel) wire that nickel foam, acetylene black and graphite powder add polytetrafluoroethylene (PTFE) and cohere.
3. the photo electrocatalysis reactor that is used for degradable organic pollutant according to claim 1 is characterized in that: above-mentioned anode porous conductive material surface and internal load have catalyst.
4. the photo electrocatalysis reactor that is used for degradable organic pollutant according to claim 1 is characterized in that: the photochemical catalyst of above-mentioned plate-load is composited by light-sensitive coloring agent and semiconductor, and above-mentioned semiconductor is transition metal Ti, W, Fe, Cr, Ni, Cu, Cd, Mn, Sn, V, rare-earth metal La, Eu, Ce, Er, precious metals pt, Au, Pd, the metal oxide or the sulfide of a kind of oxide of Ag or sulfide, the composite gained of multiple slaine.
5. the photo electrocatalysis reactor that is used for degradable organic pollutant according to claim 1 is characterized in that: above-mentioned negative electrode is made up of conductive layer, watertight composition, Catalytic Layer; Conductive layer comprises carbon cloth, graphite, nickel, copper, stainless (steel) wire; Watertight composition graphitiferous powder, acetylene black, polytetrafluoroethylene (PTFE) binder; Load has pair hydrogen reduction to become hydrogen peroxide that catalytic activity is arranged and has that the catalyst of photocatalytic activity is composite to have constituted cathode catalysis layer, and wherein oxygen reduction catalyst is made up of the transition metal macrocyclic complex.
6. the photo electrocatalysis reactor that is used for degradable organic pollutant according to claim 1 is characterized in that: above-mentioned electrolyte is an especially solid polymer electrolyte of solid electrolyte.
7. the photo electrocatalysis reactor that is used for degradable organic pollutant according to claim 1 is characterized in that: the chamber wall that inside reactor has illumination to arrive, photochemical catalyst in the load is to increase degradation efficiency.
8. the photo electrocatalysis reactor that is used for degradable organic pollutant according to claim 1, it is characterized in that: reactor can be applicable to gaseous fluid, device is an air inlet for the following side, top is the gas outlet, utilize the different generation of cold and hot density convection current to finish exchange gas, also circulation fan can be installed, air inlet and gas outlet are installed dust and are filtered collecting net.
9. biodegrading process that is used for the photo electrocatalysis reactor of degradable organic pollutant may further comprise the steps:
(1) contains the photochemical catalyst of fluid by on anode carrier, being coated with of organic pollution, photochemical catalyst is penetrated in illumination and is produced photohole and light induced electron down, under electric field action, effectively separated, photohole on the anode and organic matter effect with high oxidation activity, organic matter is oxidized, and final catabolite is carbon dioxide and water;
(2) light induced electron moves to negative electrode under electric field action, contain organic fluid by the negative electrode composite catalytic layer, oxygen at negative electrode by electrical catalyze reduction, generate hydrogen peroxide, penetrate down in illumination, hydrogen peroxide and photochemical catalyst effect generate the OH free radical with high oxidation activity, organic matter and the oxidized degraded of free radical effect, final catabolite is carbon dioxide and water;
(3) solid polymer electrolyte places the both sides of negative electrode and anode, with the hydraulic press compacting in flakes;
(4) anode and cathode side only can enter fluid from the import of reactor with sealings such as transparent material such as quartz glass, carry out photoelectric catalysis degrading through negative electrode and anode successively, leave from outlet then, to increase fluid photoelectrocatalysis time in reactor.
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2004
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