CN102826506B - Method and device for preparing hydrogen based on photoelectric degradation organic pollutant driven by visible light - Google Patents
Method and device for preparing hydrogen based on photoelectric degradation organic pollutant driven by visible light Download PDFInfo
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- CN102826506B CN102826506B CN201210344015.0A CN201210344015A CN102826506B CN 102826506 B CN102826506 B CN 102826506B CN 201210344015 A CN201210344015 A CN 201210344015A CN 102826506 B CN102826506 B CN 102826506B
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- hydrogen production
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Abstract
The invention discloses a method and a device for preparing hydrogen based on a photoelectric degradation organic pollutant driven by visible light; the device comprises a reactor, a hydrogen collection device and a light source; the bottom of the reactor is provided with a magnetic stirrer; the inside of the reactor is divided into a photocatalysis primary cell and a photocatalysis hydrogen pool which are independent from each other; a plurality of first photocatalysis electrode pairs are arranged in the photocatalysis primary cell; a plurality of second photocatalysis electrode pairs are arranged in the photocatalysis hydrogen pool; the first photocatalysis electrode pairs and the second photocatalysis electrode pairs are mutually connected serially to form a loop; and magnetons are arranged in the photocatalysis primary cell and the photocatalysis hydrogen pool. According to the method and the device for preparing hydrogen based on the photoelectric degradation organic pollutant driven by visible light, two clean technologies of preparing hydrogen by water electrolysis and preparing hydrogen by degrading the pollutant through solar photocatalysis are coupled, no external power supply is needed, meanwhile the degradation of the organic pollutant and the hydrogen preparation are realized, the hydrogen preparation efficiency is high, and the cost is low.
Description
Technical field
The present invention relates to new energy technology and water-treatment technology field, be specifically related to a kind of method and apparatus of the two n-type semiconductor optoelectronic degradable organic pollutant hydrogen manufacturing driving based on visible ray.
Background technology
Energy shortage, environmental pollution are two hang-ups of facing mankind, and the clean alternative energy source of finding sustainable supply has been the instant major issue in the whole world.Hydrogen is as a kind of secondary energy sources, and energy density is high, burning is clean, is acknowledged as the most desirable alternative energy source of fossil fuel.The method of producing at present hydrogen mainly contains two kinds: a kind of is to take fossil energy as raw material reacts and makes water-gas with steam, then through operations such as conversion, purifications, makes; Another kind is applied more extensively and more ripe method is water electrolysis hydrogen production.Fossil fuel hydrogen manufacturing will consume a large amount of mineral resources, and the pollutant producing in process of production damages earth environment, does not have sustainable developability.
Water electrolysis hydrogen production does not produce CO2 emission, is clean hydrogen producing technology, and current plant-scale apparatus for electrolyzing current efficiency can reach 56-73%, yet the cost of water electrolysis hydrogen production improves constantly along with the raising of electricity price.
Solar photolysis water hydrogen is one of optimal path of solar energy chemical conversion and storage, it utilizes the energy of sunlight, under catalyst action, decomposition water produces hydrogen, convert solar energy into Hydrogen Energy, the form that hydrogen is got back to again water after using as the energy, reaches sustainable exploitation and use completely.But because directly photochemical catalyzing hydrogen generation efficiency is low, limited its practical application, improve hydrogen generation efficiency, must add electron donor and as sacrifice agent, suppress compound and hydrogen and the compound back reaction of oxygen in light induced electron and hole, thereby obtain, produced hydrogen.Adding of electron donor can also promote the Stability Analysis of Structures of catalyst and be difficult for inactivation.
Many organic substances are all good electron donors, can significantly improve the efficiency of photocatalysis Decomposition aquatic products hydrogen, especially utilize the organic pollution in waste water to carry out photocatalytic hydrogen production by water decomposition as electron donor, in the time of the oxidized degraded of debirs, water is reduced generation hydrogen, both improve hydrogen production efficiency, removed again environmental contaminants.
Application number is that 200910138275.0 Chinese patent application discloses hybrid battery and the application thereof that a kind of optical drive degrading waste water produces hydrogen and mainly comprises: light anode has dye molecule and as the semi-conducting material of the metal nanoparticle of catalyst for absorption; Cathode material is to have catalysis to produce the material of hydrogen effect to hydrogen, and industrial wastes is fuel, and employing salts substances is electrolyte, and semi-conducting material is the material with photocatalysis property; Dye molecule is to mate and sunlight is had to absorption efficiency with the energy level of semi-conducting material, and material that can stable existence in waste liquid.This invention is incorporated into the concept of DSSC and fuel cell in same battery device, although can utilize dyestuff to absorb solar energy, be converted into electric energy, organic substance in the industrial production of simultaneously degrading waste liquid produces Hydrogen Energy, but the organic substance that this hybrid battery should be degraded in industrial production waste liquid in same reaction tank, electrogenesis again, also to produce hydrogen, the electron-hole pair of photocatalysis anode does not only have additional actuating force to impel its separation, after the reaction of hole, remaining electronics also can be subject to the obstruction of external resistor R in producing hydrogen cathodic migration process, cause the efficiency can be very not high.
Summary of the invention
The invention provides a kind of method and apparatus of the photoelectrochemical degradation organic pollution hydrogen manufacturing driving based on visible ray, separate photocatalysis primary cell and photocatalysis hydrogen production pond will be divided in reactor, photocatalysis primary cell changes into electric energy by solar energy, the electron-hole pair that provides certain bias voltage to drive photocatalysis anode in photocatalysis hydrogen production pond is efficiently separated, hole is for oxidative degradation organic pollution, electronics is for generation of hydrogen, thereby contaminant removal efficiency and hydrogen generation efficiency are all improved greatly.
A device for the photoelectrochemical degradation organic pollution hydrogen manufacturing driving based on visible ray, comprises reactor, collection hydrogen production device and light source, and described reactor bottom is with magnetic stirring apparatus; In described reactor, be divided into separate photocatalysis primary cell and photocatalysis hydrogen production pond, in described photocatalysis primary cell, be provided with some to the first photochemical catalyst electrode pair, in described photocatalysis hydrogen production pond, be provided with somely to the second photochemical catalyst electrode pair, described the first photochemical catalyst electrode is to forming loop with the second photochemical catalyst electrode to mutual series connection; In described photocatalysis primary cell and photocatalysis hydrogen production pond, be equipped with magneton.
Described the first photochemical catalyst electrode is to referring to that to mutual series connection every right anode negative electrode right with corresponding a pair of the second photochemical catalyst electrode of a pair of the first photochemical catalyst electrode is connected by wire with the second photochemical catalyst electrode, and every right negative electrode anode right with the second corresponding photochemical catalyst electrode of a pair of the first photochemical catalyst electrode is connected by wire; Reactor is made by the good quartz of light transmission, glass or polymethyl methacrylate; Described photocatalysis primary cell contains oxidation-reduction pair mixed liquor, is preferably reversible redox electricity right, for example I
-/ IO
3 -, Fe
2+/ Fe
3+, S
2-/ S
2 -deng, under the irradiation of visible ray, light energy conversion can be become to electric energy, produce enough voltage and make semiconductor light-catalyst in photoelectrocatalysis hydrogen manufacturing pond (as BiVO
4, BiVWO
4, Fe
2o
3deng) be that the electron-hole pair of anode is separated, separated hole can efficient degradation pollutant, and the electronics after separation drives and is moved to negative electrode and produces hydrogen at photocatalysis primary cell voltage.Photoelectrocatalysis hydrogen manufacturing is equipped with organic pollutant wastewater in pond, and two reaction tanks, are realized efficient degradation organic substance and produce hydrogen from coupling matching by perfect.
It is some right that electrode pair in described photocatalysis primary cell and photocatalysis hydrogen production pond can be set to as required, every a pair of all corresponding series connection in two reaction tanks, electrode pair in photocatalysis primary cell is accepted visible ray, produce voltage, for the electrode pair in photocatalysis hydrogen production pond provides voltage, the organic substance decomposing in photocatalysis hydrogen production pond produces hydrogen.
Preferably, described the first photochemical catalyst electrode is to being all set to 1～3 pair with the right quantity of the second photochemical catalyst electrode, every right anode negative electrode right with the second corresponding photochemical catalyst electrode of a pair of the first photochemical catalyst electrode is connected by wire, and every right negative electrode anode right with the second corresponding photochemical catalyst electrode of a pair of the first photochemical catalyst electrode is connected by wire.
Preferably, described the first photochemical catalyst electrode is to being visible-light response type optoelectronic pole with the right anode of the second photochemical catalyst electrode; Described the first photochemical catalyst electrode is to being product hydrogen electrode with the right negative electrode of the second photochemical catalyst electrode.More preferably, described anode is visible-light response type nano pipe optoelectronic pole.
Visible-light response type nano pipe optoelectronic pole can adopt the novel visible response type nano pipe optoelectronic pole of the transient metal doped modification of having developed in prior art, for example, can be visible light type BiVO
4, BiVWO
4, modification TiO
2, Fe
2o
3deng material, make; Negative electrode preferably adopts platinum electrode, nickel sheet, stainless (steel) wire etc.
In photocatalysis primary cell and photocatalysis hydrogen production pond, be respectively provided with 1～3 pair of photochemical catalyst electrode pair, each is to the certain distance in interval between the negative electrode and positive electrode of electrode pair, preferably, distance between the right negative electrode and positive electrode of described the first photochemical catalyst electrode is 1～10cm, 2～5cm more preferably, distance between the right negative electrode and positive electrode of described the second photochemical catalyst electrode is 1～10cm, more preferably 2～5cm.
Distance between the right negative electrode and positive electrode of the first photochemical catalyst electrode is that 1～10cm refers to that the distance between the right negative electrode and positive electrode of every a pair of the first photochemical catalyst electrode is wherein 1～10cm; Distance between the right negative electrode and positive electrode of the second photochemical catalyst electrode is that 1～10cm refers to that the distance between the right negative electrode and positive electrode of every a pair of the second photochemical catalyst electrode is wherein 1～10cm.
Spacing is too little, and between two electrodes, easily short circuit, also has certain inhibition to visible ray; Spacing is too large, and two resistance between electrode increase, and the distance that reactant is diffused into electrode surface is too large, and mass transfer rate is affected.
Preferably, the described hydrogen production device that integrates is as vacuum collection hydrogen production device, and this collection hydrogen production device can also be other any hydrogen gathering-devices that can meet requirement of the present invention.
In course of reaction, need the solution that contains organic pollution that takes out from photocatalysis hydrogen production pond regularly to detect, detect the resolution ratio of organic pollution and the indexs such as COD of waste water in photocatalysis hydrogen production pond, but in course of reaction, photocatalysis hydrogen production pond must keep closed state, prevent the escape of hydrogen, therefore, preferably, described photocatalysis hydrogen production pond is provided with sample tap, by this sample tap, sample, while not needing to sample, seal this sample tap, convenient and swift.
For convenient, timely the hydrogen of collecting is detected to analysis, preferably, on described hydrogen gathering-device, be connected with gas chromatograph.
The present invention also provides a kind of technique of the photoelectrochemical degradation organic pollution hydrogen manufacturing driving based on visible ray, comprising:
Solution containing oxidation-reduction pair is introduced in photocatalysis primary cell, containing the waste water of organic pollution, introduce in photocatalysis hydrogen production pond, anode in photocatalysis primary cell and photocatalysis hydrogen production pond is visible-light response type optoelectronic pole, negative electrode is product hydrogen electrode, anode in described photocatalysis primary cell is connected with the negative electrode in photocatalysis hydrogen production pond, and the negative electrode in described photocatalysis primary cell is connected with the anode in photocatalysis hydrogen production pond;
Visible ray irradiates the anode in photocatalysis primary cell and photocatalysis hydrogen production pond simultaneously, stirs the solution of photocatalysis primary cell and the waste water in photocatalysis hydrogen production pond, collects the hydrogen producing in photocatalysis hydrogen production pond.
Preferably, the speed of described stirring is 400～500r/min.
Beneficial effect of the present invention:
(1) dexterously by photoelectrocatalysis primary cell system, photoelectrocatalysis hydrogen generating system from coupling matching, built novel, the efficient photoelectrochemical degradation pollutant coupled hydrogen making system of solar energy as driving of take, avoid using D.C. regulated power supply, saved energy consumption, solar photoelectric is chemically converted to clean Hydrogen Energy, has realized waste water treatment simultaneously.
(2) adopted the novel visible response type nano pipe photo cathode of transient metal doped modification, having solved traditional photocatalysis technology can only utilize ultraviolet light as the restriction of light source, work in coordination with and utilized the effect of anode catalytic oxidation simultaneously, greatly improved light-catalysed quantum efficiency and rate of contaminant degradation.
(3) be suitable for removing reproducibility organic pollution from liquid, can remove organic pollution, alcohols of aldehyde, aromatic series and so on etc., and prepare clean energy resource hydrogen.
(4) apparatus of the present invention are simple to operate, facility compact, and various parameters are easily controlled, and can regulate at any time as required.
(5) when apparatus of the present invention are moved, utilizing inexhaustible solar energy, produce green energy resource hydrogen, to environment, can not cause secondary pollution, is a kind of method for treating water of green.
The present invention is by water electrolysis hydrogen production and the collaborative coupling of two kinds of clean hydrogen producing technologies of solar energy photocatalytic degradation of contaminant hydrogen manufacturing, do not need additional power source, solve the high difficult problem of the cost of electric energy that water electrolysis hydrogen production technology exists, simultaneously for photocatalysis hydrogen production technology provides certain bias voltage, light induced electron is delivered in time to electrode, thereby effectively suppressed the compound of light induced electron and hole, the degraded of organic pollution and the generation of hydrogen have been promoted, realized highly effective hydrogen yield, remove and pollute, improve the multiple targets such as economy, at alleviating energy crisis, reduce the aspects such as environmental pollution and there is very important scientific value and far-reaching realistic meaning.
Accompanying drawing explanation
Fig. 1 is structural representation of the present invention.
Embodiment
As shown in Figure 1, a kind of device of the photoelectrochemical degradation organic pollution hydrogen manufacturing driving based on visible ray, comprise reactor 1, reactor 1 is by the good quartz of light transmission, glass or polymethyl methacrylate are made, in present embodiment, adopt quartz to make, reactor 1 is closed reactor, the bottom of reactor 1 is with magnetic stirring apparatus 10, in reactor 1, by quartz or glass partition, be divided into two separate reaction tanks, one for photocatalysis primary cell 5, (semiconductor 1, be abbreviated as SCS1), one is that (semiconductor 2 in photoelectrocatalysis hydrogen manufacturing pond 6, be abbreviated as SCS2), above photoelectrocatalysis hydrogen manufacturing pond 6, be provided with thief hatch 12, in photocatalysis primary cell 5 and photoelectrocatalysis hydrogen manufacturing pond 6, be respectively provided with a magneton 4.
Photoelectrocatalysis hydrogen manufacturing pond 6 connects a collection hydrogen production device 9 by breather pipe 8, in present embodiment, integrates hydrogen production device 9 as vacuum collection hydrogen production device, on collection hydrogen production device 9, connects gas chromatograph 11.
Near reactor 1, an adjustable xenon arc lamp of 500W is set is light source at distance reactor 5cm place, and adopting edge filter to obtain can be by light.
In photocatalysis primary cell 5, be provided with three pairs of the first photochemical catalyst electrodes to (3 is anode in figure, and 2 is negative electrode), the spacing between every a pair of negative electrode and positive electrode is 1～10cm.
Anode is visible-light response type nano pipe optoelectronic pole, for example, can be modification TiO
2, Fe
2o
3, visible light type BiVO
4, BiVWO
4deng material, make; Negative electrode can adopt nickel sheet, stainless (steel) wire, platinum electrode etc.
In photoelectrocatalysis hydrogen manufacturing pond 6, be provided with three pairs with the first photochemical catalyst electrode to the second the same photochemical catalyst electrode pair, anode in photocatalysis primary cell 5 is connected by wire 7 with the interior corresponding negative electrode in photoelectrocatalysis hydrogen manufacturing pond 6, and the negative electrode in photocatalysis primary cell 5 is connected by wire 7 with the interior corresponding anode in photoelectrocatalysis hydrogen manufacturing pond 6.
In present embodiment, the light absorption area of every plate electrode is 4cm
2.
Embodiment 1.
Reaction unit is with visible light type BiVO
4material is anode, take platinized platinum as negative electrode, and regulating negative and positive two die openings is 2cm, and apart from reactor 5cm place, placing an adjustable xenon arc lamp of 500W is light source, adopts edge filter to obtain visible ray.In photocatalysis primary cell, contain certain density oxidation-reduction pair mixed solution, reaction equation:
.
By optimizing oxidation-reduction pair concentration, pH, visual intensity etc., make system produce the above bias voltage of 1.2V, the interaction relationship between research visible light catalyst and oxidation-reduction pair.Take hydroquinones as simulating pollution thing, at photoelectrocatalysis, produce hydroquinones and the 0.1M Na that adds 0.01M in H-H reaction pond
2sO
4the aqueous solution, different according to electrode material, photoelectrocatalysis produces H-H reaction pond probably needs 0.8V left and right bias voltage to realize pollution degradation produce hydrogen.Primary cell can provide enough voltage to impel product H-H reaction to carry out like this.
Using argon gas as carrier gas, get rid of air in reactor; Irradiate anode material, after 15min, open magnetic stirring apparatus, control rotating speed at 500r/min.Abstraction reaction device top air detection is analyzed hydrogen content.Organic Pollutants in Wastewater and intermediates change in concentration thereof are by high effective liquid chromatography for measuring.60min analyzes by detection after processing, and hydroquinones degradation rate is 82%, and hydrogen generating quantity is 180 μ mol, 3.0 μ mol/min.
Embodiment 2.
Reaction unit is with visible light type Fe
2o
3material is anode, take platinized platinum as negative electrode, uses hydroquinones simulative organic wastewater, with NaI and NaIO
3mixed solution is as oxidation-reduction pair.Using argon gas as carrier gas, get rid of air in reactor.Apart from reactor 5cm place, placing a 500W xenon arc lamp is light source, adopts edge filter to obtain visible ray.Irradiate anode material, after 15min, open magnetic stirring apparatus, control rotating speed at 500r/min.Abstraction reaction device static headspace gas detects analyzes hydrogen content.Organic Pollutants in Wastewater and intermediates change in concentration thereof are by high effective liquid chromatography for measuring.60min analyzes by detection after processing, and hydroquinones degradation rate is 86%, and hydrogen generating quantity is 220 μ mol, 3.67 μ mol/min.
Claims (5)
1. a device for the photoelectrochemical degradation organic pollution hydrogen manufacturing driving based on visible ray, comprises reactor, collection hydrogen production device and light source, it is characterized in that, described reactor bottom is with magnetic stirring apparatus; In described reactor, be divided into separate photocatalysis primary cell and photocatalysis hydrogen production pond, in described photocatalysis primary cell, be provided with some to the first photochemical catalyst electrode pair, in described photocatalysis hydrogen production pond, be provided with somely to the second photochemical catalyst electrode pair, described the first photochemical catalyst electrode is to forming loop with the second photochemical catalyst electrode to mutual series connection; In described photocatalysis primary cell and photocatalysis hydrogen production pond, be equipped with magneton; Described the first photochemical catalyst electrode is to being all set to 1～3 pair with the right quantity of the second photochemical catalyst electrode; Described the first photochemical catalyst electrode is to being visible-light response type optoelectronic pole with the right anode of the second photochemical catalyst electrode; Described the first photochemical catalyst electrode is to being product hydrogen electrode with the right negative electrode of the second photochemical catalyst electrode; Distance between the right negative electrode and positive electrode of described the first photochemical catalyst electrode is 2～5cm, and the distance between the right negative electrode and positive electrode of described the second photochemical catalyst electrode is 2～5cm.
2. device according to claim 1, is characterized in that, the described hydrogen production device that integrates is as vacuum collection hydrogen production device.
3. device according to claim 2, is characterized in that, described photocatalysis hydrogen production pond is provided with sample tap.
4. device according to claim 3, is characterized in that, on described hydrogen gathering-device, is connected with gas chromatograph.
5. a technique for the photoelectrochemical degradation organic pollution hydrogen manufacturing driving based on visible ray, is characterized in that, comprising:
Solution containing oxidation-reduction pair is introduced in photocatalysis primary cell, containing the waste water of organic pollution, introduce in photocatalysis hydrogen production pond, anode in photocatalysis primary cell and photocatalysis hydrogen production pond is visible-light response type optoelectronic pole, negative electrode is product hydrogen electrode, anode in described photocatalysis primary cell is connected with the negative electrode in photocatalysis hydrogen production pond, and the negative electrode in described photocatalysis primary cell is connected with the anode in photocatalysis hydrogen production pond;
Visible ray irradiates the anode in photocatalysis primary cell and photocatalysis hydrogen production pond simultaneously, stirs the solution of photocatalysis primary cell and the waste water in photocatalysis hydrogen production pond, collects the hydrogen producing in photocatalysis hydrogen production pond.
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| CN104630816B (en) * | 2015-02-15 | 2017-02-01 | 浙江工商大学 | Hydrogen production device and technology via photoelectric degradation of organic pollutant based on solar energy and sea water cell collaborative drive |
| CN111101142B (en) * | 2018-10-26 | 2021-05-18 | 中国科学院金属研究所 | Construction method of graphical integrated high-efficiency photocatalytic decomposition water system |
| EP4129931A1 (en) | 2021-08-05 | 2023-02-08 | Universitat Rovira I Virgili (URV) | Photocatalytic panel reactor for the anaerobic photoreforming of waste aqueous effluents and the production of hydrogen as co-product |
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| CN101608316A (en) * | 2009-07-27 | 2009-12-23 | 新奥科技发展有限公司 | A kind of device for producing hydrogen through decomposing water |
| CN101908418A (en) * | 2009-06-04 | 2010-12-08 | 青岛生物能源与过程研究所 | Hybrid battery for degrading waste water to produce hydrogen through photic driving |
| CN101913693A (en) * | 2010-09-21 | 2010-12-15 | 浙江工商大学 | Device and method for activating molecular oxygen by electrocatalysis to treat persistent organic wastewater |
| CN202880862U (en) * | 2012-09-17 | 2013-04-17 | 浙江工商大学 | Device for hydrogen production by photoelectrically degrading organic pollutants on basis of visible light drive |
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Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101908418A (en) * | 2009-06-04 | 2010-12-08 | 青岛生物能源与过程研究所 | Hybrid battery for degrading waste water to produce hydrogen through photic driving |
| CN101608316A (en) * | 2009-07-27 | 2009-12-23 | 新奥科技发展有限公司 | A kind of device for producing hydrogen through decomposing water |
| CN101913693A (en) * | 2010-09-21 | 2010-12-15 | 浙江工商大学 | Device and method for activating molecular oxygen by electrocatalysis to treat persistent organic wastewater |
| CN202880862U (en) * | 2012-09-17 | 2013-04-17 | 浙江工商大学 | Device for hydrogen production by photoelectrically degrading organic pollutants on basis of visible light drive |
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