CN109628272A - A kind of device can be used for producing hydrogen peroxide and its application - Google Patents

A kind of device can be used for producing hydrogen peroxide and its application Download PDF

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CN109628272A
CN109628272A CN201811569324.1A CN201811569324A CN109628272A CN 109628272 A CN109628272 A CN 109628272A CN 201811569324 A CN201811569324 A CN 201811569324A CN 109628272 A CN109628272 A CN 109628272A
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hydrogen peroxide
cathode
anode
water
micro
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CN109628272B (en
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任月萍
王悦
李秀芬
王新华
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Jiangnan University
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Abstract

The invention discloses a kind of device that can be used for producing hydrogen peroxide and its applications, belong to oxidant technical field.The device of the invention can provide O using microalgae photosynthesis for cathode reaction2, it realizes the production of hydrogen peroxide, without external aeration, saves energy consumption, meanwhile, microalgae grease production may be implemented in this device；Hydrogen peroxide manufacture 8d is carried out using the device of the invention, the lipid-producing of microalgae in micro algae growth room can be made to be up to 656mg/Ld, H in cathode chamber2O2Accumulated concentrations be 180mg/L, excellent, application prospect is extremely wide.

Description

A kind of device can be used for producing hydrogen peroxide and its application
Technical field
The present invention relates to a kind of device that can be used for producing hydrogen peroxide and its applications, belong to oxidant technical field.
Background technique
Hydrogen peroxide (H2O2) there is strong oxidizing property, oxygen and water are only generated after decomposition, it is without secondary pollution, it is a kind of ideal Green Oxidant, in the fields such as weaving, printing and dyeing, paper pulp bleaching, food sterilization and chemical industry synthesis using increasingly extensive.Only 2017, China H2O2The yield of (based on 27.5%) is as high as to 830,000 tons, increases by 5.48% on a year-on-year basis.
Currently, H2O2Production method mainly include that isopropanol autoxidation method, O_2 cathodic reduction method, hydrogen-oxygen directly synthesize Method and anthraquinone etc., wherein anthraquinone is domestic and international industrial production H2O2Main technique.
But first alpha-alkyl anthraquinone need to be dissolved in organic solvent due to anthraquinone, under the action of catalyst, it is passed through hydrogen Alkyl-anthraquinone is reduced to alkyl hydrogen anthraquinone, oxygen is then passed through again by alkyl hydrogen anthraquinone and is converted into alkyl-anthraquinone, generate simultaneously H2O2, finally, with H in water extractant2O2And by purification and distillation processing, H is obtained2O2Aqueous solution has production stage numerous The more and higher defect of energy consumption.
Therefore, in recent years succinctly, efficiently, the H of low energy consumption2O2The exploitation of production technology is receive more and more attention.
Microorganism electrocatalytic method is the novel H of one kind developed in recent years2O2Production method, simple with step, The advantage that energy consumption is small, environmentally protective etc., is a kind of H with development potential2O2Production technology.The method relate generally to it is a kind of by The microorganism electrochemical system of anode, cathode, separation membrane and constant voltage source composition, wherein anode surface is enriched with electroactive micro- life Object, degradation substrate generate electronics, and electronics reaches cathode surface and O in the external circuit that acts through of external voltage22 electronics way occurs The reduction reaction of diameter generates H2O2(formula (1) or (2)),
O2+2H2O+2e-→H2O2+2OH-(1),
O2+H2O+2e-→HO2 -+OH- (2)。
And utilize this system production H2O2When, cathode O2Acquisition there are mainly two types of method: one is using gas diffusion yin Pole utilizes O in air2As cathode electronics receptor, the shortcomings that this method is O in air2Divide small, O2It is opposite to cathode three It answers the diffusion at interface slow, seriously limits H2O2Generation；Another kind is to carry out continuing aeration in cathode chamber, and this method is general Need biggish O2Or air mass flow guarantees enough dissolved oxygens (DO) concentration, needs additional high energy consumption, and then increased (cost of aeration is generally 15 yuan/m to the production cost of hydrogen oxide3·d)。
Therefore, microorganism electrocatalytic method is in H2O2There is larger obstructions for the application of production aspect.
Summary of the invention
[technical problem]
The technical problem to be solved in the present invention is to provide a kind of low cost and with the hydrogen peroxide of high added value by-product Production method.
[technical solution]
Microalgae is the high autotroph of widely distributed and photosynthetic availability, can generate oxygen by photosynthesis, make system DO reach saturated concentration.Therefore, to solve the above problems, including micro algae growth room the present invention provides one kind, being provided with yin The cathode chamber of pole, the anode chamber for being internally provided with anode, for providing the light source of luminous energy to microalgae, and for jointed anode and The device that can be used for producing hydrogen peroxide of the power supply of cathode；This device can be provided using microalgae photosynthesis for cathode reaction O2, it realizes the production of hydrogen peroxide, without external aeration, saves energy consumption, meanwhile, it is raw that microalgae grease may be implemented in this device It produces；Hydrogen peroxide manufacture 8d is carried out using this device, the lipid-producing of microalgae in micro algae growth room can be made to be up to 656mg/Ld, H in cathode chamber2O2Accumulated concentrations be 180mg/L, excellent, application prospect is extremely wide.
In one embodiment of the invention, the micro algae growth room is inoculated with microalgae；The cathode is gas diffusion Cathode；Electro-chemical activity microorganism is attached on the anode；The micro algae growth room and cathode chamber are spaced by cathode；Institute It states cathode chamber and anode chamber is spaced by separation membrane；The first water inlet, the first water outlet are provided on the micro algae growth room And algae solution outlet；The second water inlet and the second water outlet are provided on the cathode chamber；It is provided in the anode chamber Third water inlet and third water outlet.The electro-chemical activity microorganism (EAM) is that the one of electron exchange can occur with electrode The functions such as substance conversion, energy conversion may be implemented in quasi-microorganism, the interaction of they and electrode.
In one embodiment of the invention, the microalgae includes chlorella vulgaris (Chlorellavulgaris), three Angle brown algae (Phaeodactylumtricornutum), micro- quasi- ball algae (Nannochloropsissp.), scenedesmus obliquus One of (Scenedesmus obliquus) or salt algae (Dunaliellasalina) or a variety of.
In one embodiment of the invention, the electro-chemical activity microorganism includes that sulphur restores ground bacillus, Xi Washi Bacterium, iron vat red educate one of bacterium, pseudomonas aeruginosa, butyric acid carboxylic bacterium or a variety of.
In one embodiment of the invention, the micro algae growth room is column, contains the first top surface, the first bottom surface And first side；First water inlet, algae solution outlet are located at lower section or the micro algae growth of micro algae growth room first side First bottom surface of room；First water outlet is located at the top of micro algae growth room first side or the first top of micro algae growth room Face.
In one embodiment of the invention, the cathode chamber be column, containing the second top surface, the second bottom surface and Second side；Second water inlet is located at the lower section of cathode chamber second side or the second bottom surface of cathode chamber；Described second goes out The mouth of a river is located at the top of cathode chamber second side or the second top surface of cathode chamber.
In one embodiment of the invention, the anode chamber be column, containing third top surface, third bottom surface and Third side；The third water inlet is located at the lower section of anode chamber third side or the third bottom surface of anode chamber；The third goes out The mouth of a river is located at the top of anode chamber third side or the third top surface of anode chamber.
In one embodiment of the invention, the gas diffusion cathode includes gas diffusion layers, collector and urges Change layer；The gas diffusion layers include porous carbon black-polytetrafluoroethylene (PTFE) (PTFE) layer, porous graphene layer, nylon leaching film or warp Cross one of stainless (steel) wire of hydrophobic treatment or a variety of；The collector includes one of stainless (steel) wire, titanium net or nickel screen Or it is a variety of；The Catalytic Layer includes carbon black-PTFE layers, one of carbon black-- PTFE layers of graphite or-PTFE layers of graphene or more Kind.
In one embodiment of the invention, the anode is in carbon brush, carbon cloth, carbon paper, graphite felt or graphite plate It is one or more.
In one embodiment of the invention, the separation membrane includes cation-exchange membrane or proton exchange membrane.
In one embodiment of the invention, the light source includes fluorescent lamp and/or LED light.
In one embodiment of the invention, the power supply is that the voltage range that constant voltage source and the power supply apply is 0.1V~0.8V.
The present invention also provides a kind of method for producing hydrogen peroxide, the method is that can be used for producing peroxide using above-mentioned Change the device of hydrogen.
In one embodiment of the invention, the method is that will contain the phosphate-buffered of sodium acetate and/or glucose Liquid need to handle waste water A and is passed through in anode chamber by third water inlet, by Na2SO4Solution is passed through cathode chamber by the second water inlet In, it by micro-algae culture medium or waste water B need to be handled is passed through in micro algae growth room by the first water inlet, obtain hydrogen peroxide reactant System；In micro-algae culture medium or need to handle and be inoculated with microalgae in waste water B, open light source and carry out illumination, microalgae is made to produce oxygen, obtain oxygen and Algae solution；Phosphate buffer is seeded to using the anaerobic sludge containing electro-chemical activity microorganism as inoculum or need to handle waste water A In, outer connecting resistance and output voltage until power supply is powered on not less than after 100mV, with constant voltage source in yin at the power supply Apply voltage between anode, obtains hydrogen peroxide；
After the micro algae growth in micro algae growth room enters stationary phase, algae solution can be discharged by algae solution outlet and carry out grease Extraction, while by another batch of micro-algae culture medium or waste water B need to be handled micro algae growth room is passed through by the first water inlet；
The waste water A that need to handle is comprising sanitary sewage, kitchen waste water, food processing wastewater or containing hardly degraded organic substance Waste water；
The waste water B that need to handle is nitrogenous and/or phosphorus waste water.The hardly degraded organic substance refers to microorganism at any The organic matter that cannot be degraded under part with sufficiently fast speed.The anaerobic sludge belongs to activated sludge；The activated sludge is micro- The general name of biocenose and organic substance and inorganic substances that they are depended on, can be divided into aerobic sludge and anaerobic sludge.
In one embodiment of the invention, the waste water containing hardly degraded organic substance includes dyeing waste water.
In one embodiment of the invention, adhesion amount of the electro-chemical activity microorganism on anode is 0.1 μ g/ cm2~10 μ g/cm2。
In one embodiment of the invention, the microalgae in micro-algae culture medium or need to handle inoculum concentration in waste water B It is 1 × 105~5 × 106cell/mL。
In one embodiment of the invention, the Light To Dark Ratio of the illumination is (0h~for 24 hours): (for 24 hours~0h).
In one embodiment of the invention, the Light To Dark Ratio of the illumination is 12h:12h.
In one embodiment of the invention, the waste water B that need to handle adds comprising breeding wastewater, kitchen waste water, food One of work waste water, milk product waste or fermentation waste water are a variety of.
In one embodiment of the invention, the concentration of the phosphate buffer is 50mmol/L.
In one embodiment of the invention, content of the sodium acetate in phosphate buffer is 1g/L；It is described Content of the glucose in phosphate buffer is 1g/L.
In one embodiment of the invention, the Na2SO4The concentration of solution is 50mmol/L.
The present invention also provides the methods of the device of above-mentioned production hydrogen peroxide or above-mentioned production hydrogen peroxide to produce Application in terms of hydrogen oxide.
[beneficial effect]
(1) the device of the invention can provide O using microalgae photosynthesis for cathode reaction2, realize the production of hydrogen peroxide, It is aerated without outside, saves energy consumption, so that the cost of oxygen supply is reduced to 9.6 yuan/m3D, only external aeration cost 64%；
(2) the device of the invention can realize that microalgae grease produces, and carry out hydrogen peroxide manufacture 8d using the device of the invention, The lipid-producing of microalgae in micro algae growth room can be made to be up to 656mg/Ld；
(3) sewage treatment may be implemented in the device of the invention, and sewage can be passed through in apparatus of the present invention, using sewage as sun Pole liquid and micro algae culturing liquid carry out H2O2Preparation, water outlet COD, NH of sewage in micro algae growth room can be made4 +- N, TN and TP difference 60%, 80%, 89% and 94.2% is reduced compared with water inlet.
Detailed description of the invention
Fig. 1: the present invention produces the overall schematic of the device of hydrogen peroxide；
Wherein, 1 micro algae growth room, 2 cathodes, 3 cathode chambers, 4 anodes, 5 anode chambers, 6 light sources, 7 power supplys, 8 separation membranes, 9 One water inlet, 10 first water outlets, 11 algae solution outlets, 12 second water inlets, 13 second water outlets, 14 third water inlets, 15 Third water outlet, 16 first top surfaces, 17 first bottom surfaces, 18 first sides, 19 second top surfaces, 20 second bottom surfaces, 21 second sides, 22 third top surfaces, 23 third bottom surfaces and 24 third sides.
Specific embodiment
The present invention will be further elaborated with reference to the accompanying drawing:
Such as Fig. 1, water treatment facilities of the invention includes micro algae growth room 1, the cathode chamber 3 for being provided with cathode 2, internal setting There is the anode chamber 5 of anode 4, for providing the light source 6 of luminous energy, and the power supply 7 for jointed anode 4 and cathode 2 to microalgae；Institute It states micro algae growth room 1 and is inoculated with microalgae；The cathode 2 is gas diffusion cathode；It is micro- that electro-chemical activity is attached on the anode 4 Biology；The micro algae growth room 1 and cathode chamber 3 are spaced by cathode 2；The cathode chamber 3 and anode chamber 5 pass through separation membrane 8 It is spaced；The first water inlet 9, the first water outlet 10 and algae solution outlet 11 are provided on the micro algae growth room 1；The yin The second water inlet 12 and the second water outlet 13 are provided in pole room 3；Be provided in the anode chamber 5 third water inlet 14 and Third water outlet 15.
As a further preference, the microalgae refers to comprising chlorella vulgaris (Chlorella vulgaris), phaeodactylum tricornutum Algae (Phaeodactylum tricornutum), micro- quasi- ball algae (Nannochloropsis sp.), scenedesmus obliquus One of (Scenedesmus obliquus) or salt algae (Dunaliella salina) or a variety of.
As a further preference, the electro-chemical activity microorganism includes sulphur reduction ground bacillus, Shewanella, iron reduction It is red to educate one of bacterium, pseudomonas aeruginosa, butyric acid carboxylic bacterium or a variety of.
As a further preference, the micro algae growth room 1 be column, containing the first top surface 16, the first bottom surface 17 with And first side 18；First water inlet 9, algae solution outlet 11 are located at the lower section or micro- of 1 first side 18 of micro algae growth room First bottom surface 17 of algae growth room 1；First water outlet 10 is located at top or the microalgae life of 1 first side 18 of micro algae growth room First top surface 16 of long room 1.
As a further preference, the cathode chamber 3 is column, contains the second top surface 19, the second bottom surface 20 and the Two side faces 21；Second water inlet 12 is located at the lower section of 3 second side 21 of cathode chamber or the second bottom surface 20 of cathode chamber 3；Institute It states the second water outlet 13 and is located at the top of 3 second side 21 of cathode chamber or the second top surface 19 of cathode chamber 3.
As a further preference, the anode chamber 5 is column, contains third top surface 22, third bottom surface 23 and the Three sides 24；The third water inlet 14 is located at the lower section of 5 third side 24 of anode chamber or the third bottom surface 23 of anode chamber 5；Institute It states third water outlet 15 and is located at the top of 5 third side 24 of anode chamber or the third top surface 22 of anode chamber 5.
As a further preference, the gas diffusion cathode includes gas diffusion layers, collector and Catalytic Layer；It is described Gas diffusion layers include porous carbon black-polytetrafluoroethylene (PTFE) (PTFE) layer, porous graphene layer, nylon leaching film or pass through hydrophobic treatment One of stainless (steel) wire or a variety of；The collector includes one of stainless (steel) wire, titanium net or nickel screen or a variety of；It is described Catalytic Layer includes carbon black-PTFE layers, one of carbon black-- PTFE layers of graphite or-PTFE layers of graphene or a variety of.
As a further preference, the gas diffusion cathode 2 is carbon black-polytetrafluoroethylene (PTFE) (PTFE) gas diffusion yin Pole includes carbon black-PTFE layers and collector；Carbon black-polytetrafluoroethylene (PTFE) (PTFE) gas diffusion cathode is by by carbon black- What the tow sides of PTFE layers of roll-in to collector obtained；The collector includes one of stainless (steel) wire, titanium net or nickel screen Or it is a variety of.
As a further preference, the anode 4 is one of carbon brush, carbon cloth, carbon paper, graphite felt or graphite plate or more Kind.
As a further preference, the light source 6 includes fluorescent lamp and/or LED light.
As a further preference, the power supply 7 be the voltage range that constant voltage source and the power supply apply be 0.1V~ 0.8V。
As a further preference, the separation membrane 8 includes cation-exchange membrane or proton exchange membrane.
The present invention will be further elaborated combined with specific embodiments below:
Microalgae involved in following embodiments is purchased from the Chinese Academy of Sciences, aquatic institute's fresh water algae library, Wuhan；In following embodiments The cation-exchange membrane and proton exchange membrane being related to are purchased from Shanghai and gloomy Electrical Appliances Co., Ltd；Detest involved in following embodiments Oxygen sludge is respectively denitrification pond sludge and the Wuxi Hui Lian rubbish steam power plant for deriving from Wuxi Taihu Lake new city sewage treatment plant UASB reactor granules sludge；The cultivation that waste water involved in following embodiments respectively derives from Yixing prosperity pig farm is useless Water and sanitary sewage from Wuxi Taihu Lake new city sewage treatment plant；Culture medium involved in following embodiments is respectively to purchase TAP culture medium from the BG-11 culture medium of the rich biology in Qingdao sea and purchased from upper sea light language Biotechnology Co., Ltd.
Carbon black-PTFE gas diffusion cathode involved in following embodiments is the ultrasound by the way that carbon black to be dissolved into ethyl alcohol Lower dropwise addition PTFE emulsion (60%), then mixture is stirred in water-bath at 80 DEG C, ultimately forms paste mixture, is placed in roll squeezer On, respectively in roll-in to the tow sides of collector, and it is sintered made from 20min at 340 DEG C；The carbon black purchased from Shanghai and Gloomy Electrical Appliances Co., Ltd；The PTFE emulsion is purchased from Guangzhou Xing Shengjie Science and Technology Ltd.；The collector is titanium net or not Become rusty one of steel mesh or a variety of；The titanium net is purchased from Baoji prosperity Tai Ye Co., Ltd；The stainless (steel) wire is purchased from gloomy crown wire Net Products Co., Ltd
Detection method involved in following embodiments is as follows:
The detection method of lipid-producing:
Appropriate algae solution is taken, by natural subsidence or frond precipitating is centrifugally separating to obtain, frond is precipitated by freeze-drying After obtain algae powder；Take 50mg algae powder that 2.5mL chloroform and 5.0mL methanol is added, concussion is extracted at 37 DEG C takes upper layer organic afterwards for 24 hours Phase；Algae-residue according to the method described above extract 2 times again by concussion；After the organic phase extracted three times is merged, 9mL ultrapure water is added, in It is centrifuged 1min under 4000r/min, upper organic phase is taken to set in a round bottom flask, rotary evaporation removes chloroform at 30 DEG C, weighs To total oil quantity；Wherein, the calculation formula of lipid-producing is as follows:
The detection method of DO concentration:
DO concentration uses plum Teller FiveGoTMDO tester is measured.
The detection method of COD concentration:
Specific step is as follows:
(1) oxidation solution, ferroin indicator and 0.1mol/L l ferrous ammonium sulfate solution are configured；
Wherein, the preparation method of oxidation solution is to weigh in 105 DEG C of dry 2 hours pure K2Cr2O74.9g、AgSO4(sulfuric acid Silver) 20g is dissolved in 166mL distilled water, the 834mL concentrated sulfuric acid is added；
Ferroin indicator: 1.485g ferroin is dissolved in a little distilled water, and 0.695gFeSO is added4·7H2O It is diluted to 100mL, is contained in brown bottle；
L ferrous ammonium sulfate solution: by 40.0gFe (NH4)2(SO4)2·6H2O (iron ammonium sulfate) is placed in 1000mL reagent bottle In, it is slowly added to move into after the 20mL concentrated sulfuric acid is cooling while stirring and water is added in 1000mL volumetric flask is diluted to graticule, before use It is demarcated with potassium bichromate titer.
(2) l ferrous ammonium sulfate solution is demarcated
It draws 0.1000mol/L standard solution 20mL to be placed in conical flask, 1:1 sulfuric acid solution 20mL is added, and (sulfuric acid is added In water), it mixes；After cooling, add 3 drop ferroin indicator, be titrated to l ferrous ammonium sulfate solution and reddened brown by bright green, As terminal calculates the concentration of l ferrous ammonium sulfate solution；
Wherein, the calculation formula of l ferrous ammonium sulfate solution concentration is as follows:
In formula, V: the volume (mL) of the l ferrous ammonium sulfate solution consumed when titration.
(3) COD concentration mensuration
10mL oxidation solution is accurately drawn with pipette in 250mL triangular pyramidal bottle, is drawn waste water sample 5mL and is added thereto, Upper cover is put into the baking having warmed up to 160 DEG C with 50mL small beaker (first is that preventing floating material from entering, second is that preventing evaporation when heating) In case, timing 30min takes out, 30mL distilled water is added in cooling, bottle, after cooling, the ferrous clever indicator of 3 drops is added, with mark Quasi- l ferrous ammonium sulfate solution drops to bright green and reddens brown as terminal, and the water of blank secondary distilled water or comparable purity replaces water Sample, same dry titrate it with iron ammonium sulfate after 30min；
Wherein, the calculation formula of COD concentration is as follows:
In formula, V0: iron ammonium sulfate ml is consumed when blank titration；
V1: iron ammonium sulfate ml is consumed when water sample titrates；
C: l ferrous ammonium sulfate solution molar concentration mol/L；
8:(1/4) O2Scaled value of the molal weight as unit of mg/L；
V: ml of waste water.
NH4 +The detection method of-N concentration:
NH4 +- N concentration is measured using Berthelot method, the specific steps are as follows:
(1) color developing agent is configured
Color developing agentPhenol 10g adds sodium nitroprusside 0.02g to be settled to 1L, sets dark-brown bottle in saving in refrigerator, Validity period 1 month；
Color developing agentSodium hydroxide 6g adds liquor natrii hypochloritis (Active Chlorine is greater than 5.2%) 6mL to be settled to 1L, validity period 1 A month.
(2)NH4 +The measurement of standard curve
5.35g ammonium chloride is dissolved in ultrapure water and is settled to 1L, is made into the NH of 0.1mol/L4 +Solution, and with this solution For mother liquor, it is configured to the NH of 0.5,1.0,1.5,2.0,2.5mmol/L4 +Standard solution (makees graticule with 0,7,14,21,28,35).
(3)NH4 +The measurement of-N concentration
0.2mL is taken to wait for that in test tube, 2.5mL color developing agent is first added in test sampleIt mixes well, adds 2.5mL color developing agent It mixes well, after keeping the temperature 20min at 37 DEG C, OD value is measured under 550nm.
The test method of TN concentration:
The measurement of TN uses potassium persulfate oxidation method, the specific steps are as follows:
(1) configuration of reagent
The configuration of NaOH (20%) solution: it weighs 20gNaOH and is dissolved in 100mL ultrapure water；
The configuration of alkaline chitinase solution: weighing 40g potassium peroxydisulfate, and 15gNaOH is dissolved in 1000mL ultrapure water；
Potassium nitrate standard solution: it weighs 0.7218g potassium nitrate and is dissolved in 1000mL ultrapure water.
(2) drafting of standard curve
Respectively draw 0,0.5,1.0,2.0,3.0,5.0,7.0,8.0mL potassium nitrate standard solution in 25mL colorimetric cylinder, Ultrapure water is added and is diluted to 10mL；5mL alkaline chitinase solution is added, stoppers grinding port plug, wraps pipe close with gauze and yarn rope, It is placed in autoclave and heats 0.5h；Take out colorimetric cylinder cooled to room temperature；1mLHCl (5molL is added-1), it is dilute with ultrapure water Release 25mL；Make reference with ultrapure water, is respectively that 220nm and 275nm measures absorbance in wavelength, takes reading, and calculate Correct absorbance A；
Wherein, A=A220- 2A275。
(3) water sample TN concentration mensuration
10mL water sample is taken, tests its absorbance at 220nm and 275nm respectively, according to correction absorbance and standard curve Calculate TN concentration.
The test method of TP concentration:
The measurement of TP concentration uses ammonium molybdate spectrophotometric method, the specific steps are as follows:
(1) configuration of reagent
Sulfuric acid (1molL-1): the 27mL concentrated sulfuric acid is added in 973mL water, stirs evenly and is placed in reagent bottle；
NaOH solution (1molL-1): it weighs 40gNaOH and is dissolved in 1L water；
NaOH solution (6molL-1): it weighs 240gNaOH and is dissolved in 1L water；
Potassium persulfate solution (50gL-1): it weighs 5g potassium peroxydisulfate and is dissolved in the water of 100mL；
Ascorbic acid solution (100gL-1): 10g dissolution of ascorbic acid is weighed in 100mL water；
Ammonium molybdate solution: it weighs 13g ammonium molybdate and is dissolved in 100mL water；0.35g potassium antimony tartrate is dissolved in 100mL In water；300mL sulfuric acid (1molL is added in above-mentioned ammonium molybdate solution and antimony tartrate potassium solution under constant stirring-1) in, it mixes It closes uniformly, is stored in brown reagent bottle；
Turbidity-chromatic compensation liquid: by sulfuric acid (1molL-1) and ascorbic acid solution (100gL-1) according to volume ratio be 2:1 mixing；
Phosphorus standard stock solution: the di(2-ethylhexyl)phosphate that 0.2197 ± 0.001g is let cool in drier in 110 DEG C of dry 2h is weighed Hydrogen potassium is transferred in 1000mL volumetric flask after being dissolved with water, adds 5mL sulfuric acid (1molL-1), it is diluted with water to graticule and mixes； Finally, this standard solution of 1.00mL contains 50.0 μ g phosphorus；
Phosphorus standard uses solution: the above-mentioned phosphorus standard stock solution of 10.0mL is transferred in 250mL volumetric flask, it is dilute with water It releases to graticule and mixes；Finally, this standard solution of 1.00mL contains 2.0 μ g phosphorus；
Phenolphthalein solution (10gL-1): it weighs 0.5g phenolphthalein and is dissolved in 50mL95% ethyl alcohol.
(2) TP concentration mensuration
500mL water sample is taken, 1mL sulfuric acid (1molL is added-1) by pH value be transferred to 1 hereinafter, pipette 25mL to tool fill in graded tube In, after shaking up, be added plus 4mL potassium persulfate solution, will tool plug graded tube lid stopper after, with a napkin and line by glass stopper It tightens, is placed on to be placed in high pressure steam boiler in large beaker and heat, reach 1.1kg/cm to pressure2, relevant temperature is 120 DEG C When, stop heating after keeping 30min；After pressure gauge reading is down to zero, taking-up is let cool；Then it is diluted with water to graticule；
7 50mL tool plug test tubes are taken to be separately added into 0.00,0.50,1.00,2.50,5.00,10.00,15.00mL phosphate Standard solution is diluted with water 50mL；2mL molybdate solution is added, shakes up, 1mL ascorbic acid solution is added, is diluted with water Absorbance of the test sample at 700nm after 50mL, 15min obtains standard working curve；It is added respectively into each digestion solution 2mL molybdate solution, shakes up, and 1mL ascorbic acid solution is added, is diluted with water 50mL, test sample is in 700nm after 15min Sample TP concentration is calculated according to working curve in the absorbance at place.
Embodiment 1
Specific step is as follows:
It is point with cation-exchange membrane (20cm × 50cm) with carbon brush (long 45cm, diameter 15cm) for anode according to Fig. 1 Diaphragm, using carbon black-polytetrafluoroethylene (PTFE) (PTFE) gas diffusion cathode as cathode (20cm × 50cm), anode chamber and cathode chamber body Product is 20L (20cm × 20cm × 50cm), and micro algae growth building volume is 30L (20cm × 30cm × 50cm), anode and cathode spacing For 10cm；
PBS buffer solution (50mM) containing 1g/L sodium acetate is passed through in anode chamber by third water inlet, by Na2SO4It is molten Liquid (50mM) is passed through in cathode chamber by the second water inlet, by Wastewater from Pig Farm (COD2257mg/L, NH4 +-N789mg/L、 TN910mg/L, TP85mg/L) it is passed through in micro algae growth room by the first water inlet, obtain hydrogen peroxide reaction system；It is raising pigs It is inoculated with chlorella vulgaris (Chlorellavulgaris) in the waste water of field, inoculation initial concentration is 5 × 106Cell/mL opens light Source (being made of 2 38W fluorescent tubes) carries out illumination (Light To Dark Ratio 12h:12h), and microalgae is made to produce oxygen, after 2d, micro algae growth room 10.2mg/L and 8.5mg/L or so are maintained essentially in DO in cathode chamber, microalgae reaches growth stationary phase after 10d, stop water inlet, The algae solution of 80% volume is discharged by the discharge outlet of micro algae growth room lower part, re-starts into water, continues to cultivate；With sewage treatment plant Cotton-shaped denitrification pond sludge is that inoculum is that inoculum is seeded in PBS buffer solution, external 1000 Ω resistance and is connect at power supply Energization source until the output voltage of power supply is not less than after 100mV, with constant voltage source to apply between anode and cathode 0.8V voltage with Prepare hydrogen peroxide.
When 10d, the algae solution of taking-up is subjected to grease extraction, discovery lipid-producing reaches 656mg/Ld, detects cathode chamber Middle H2O2Concentration, find H2O2Accumulated concentrations be 220mg/L, meanwhile, by micro algae growth room water outlet detect, find out Water COD, NH4 +- N, TN and TP are reduced to 902.8mg/L, 157.8mg/L, 100.1mg/L, 4.9mg/L, removal rate difference It is 60%, 80%, 89% and 94.2%.
In this embodiment, maintain essentially in DO in micro algae growth room (30L) and cathode chamber (20L) using the present invention Cost needed for 10.2mg/L and 8.5mg/L or so includes the 9.6 yuan/m of the electricity charge of micro algae growth light source3·d；And made using aeration The aeration pump power that DO maintains essentially in 10.2mg/L and 8.5mg/L or so needs in micro algae growth room and cathode chamber is 25W, is pressed It is calculated according to daily aeration 12h, cost is about 15 yuan/m3D, therefore, the cost needed for being supplied oxygen using water treatment facilities of the present invention The 64% of only external aeration cost.
Embodiment 2
Specific step is as follows:
It is to separate with cation-exchange membrane (20cm × 50cm) with graphite felt (20cm × 50cm) for anode according to Fig. 1 Film, using carbon black-polytetrafluoroethylene (PTFE) (PTFE) gas diffusion cathode as cathode (20cm × 50cm), anode chamber and cathode building volume It is 20L (20cm × 20cm × 50cm), micro algae growth building volume is 30L (20cm × 30cm × 50cm), and anode and cathode spacing is 10cm；
PBS buffer solution (50mM) containing 1g/L glucose is passed through in anode chamber by third water inlet, by Na2SO4It is molten Liquid (50mM) is passed through in cathode chamber by the second water inlet, and micro-algae culture medium is passed through micro algae growth room by the first water inlet In, obtain hydrogen peroxide reaction system；It is inoculated with scenedesmus obliquus (Scenedesmusobliquus) in micro algae culturing liquid, inoculation Initial concentration is 5 × 106Cell/mL, unlatching light source (being made of 2 8WLED fluorescent tubes) progress illumination (Light To Dark Ratio 12h: 12h), microalgae is made to produce oxygen, after 2d, DO maintains essentially in 9.9mg/L and 7.8mg/L or so, 8d in micro algae growth room and cathode chamber Microalgae reaches growth stationary phase afterwards, stops water inlet, the algae solution of 80% volume is discharged by the discharge outlet of micro algae growth room lower part, again It intakes, continues to cultivate；It is that inoculum is seeded in PBS buffer solution by inoculum of UASB reactor granules sludge, in electricity At source external 1000 Ω resistance and output voltage until power supply is powered on not less than after 100mV, with constant voltage source in yin Apply 0.3V voltage between anode to prepare hydrogen peroxide.
When 10d, the algae solution of taking-up is subjected to grease extraction, discovery lipid-producing reaches 284mg/Ld, meanwhile, detection yin H in pole room2O2Concentration, find H2O2Accumulated concentrations be 180mg/L.
In this embodiment, maintain essentially in DO in micro algae growth room (30L) and cathode chamber (20L) using the present invention Cost needed for 9.9mg/L and 7.8mg/L or so includes the 9.6 yuan/m of the electricity charge of micro algae growth light source3·d；And made using aeration The aeration pump power that DO maintains essentially in 9.9mg/L and 7.8mg/L or so needs in micro algae growth room and cathode chamber is 25W, is pressed It is calculated according to daily aeration 12h, cost is about 15 yuan/m3D, therefore, the cost needed for being supplied oxygen using water treatment facilities of the present invention The 64% of only external aeration cost.
Embodiment 3
Specific step is as follows:
It is to separate with cation-exchange membrane (20cm × 50cm) with graphite felt (20cm × 50cm) for anode according to Fig. 1 Film, using carbon black-polytetrafluoroethylene (PTFE) (PTFE) gas diffusion cathode as cathode (20cm × 50cm), anode chamber and cathode building volume It is 20L (20cm × 20cm × 50cm), micro algae growth building volume is 30L (20cm × 30cm × 50cm), and anode and cathode spacing is 10cm；
PBS buffer solution (50mM) containing 1g/L sodium acetate is passed through in anode chamber by third water inlet, by Na2SO4It is molten Liquid (50mM) is passed through in cathode chamber by the second water inlet, and micro-algae culture medium BG-11 is passed through microalgae life by the first water inlet In long room, hydrogen peroxide reaction system is obtained；Micro- quasi- ball algae (Nannochloropsissp.), inoculation are inoculated in micro-algae culture medium Initial concentration is 5 × 106Cell/mL opens light source (being made of 2 8WLED fluorescent tubes) and carries out illumination (Light To Dark Ratio 18h:6h), Microalgae is set to produce oxygen, after 2d, DO maintains essentially in 11.3mg/L and 10.1mg/L or so in micro algae growth room and cathode chamber, after 10d Microalgae reach growth stationary phase, stop water inlet, by micro algae growth room lower part discharge outlet be discharged 80% volume algae solution, again into Traveling water continues to cultivate；It is that inoculum is seeded to PBS buffer solution using the cotton-shaped denitrification pond sludge of sewage treatment plant as inoculum In, external 1000 Ω resistance and output voltage until power supply is powered on not less than after 100mV, with constant voltage source at the power supply To between anode and cathode apply 0.5V voltage to prepare hydrogen peroxide.
When 10d, the algae solution of taking-up is subjected to grease extraction, discovery lipid-producing reaches 314mg/Ld；After 8d, detection yin H in pole room2O2Concentration, find H2O2Accumulated concentrations be 150mg/L.
In this embodiment, maintain essentially in DO in micro algae growth room (30L) and cathode chamber (20L) using the present invention Cost needed for 9.9mg/L and 7.8mg/L or so includes the 9.6 yuan/m of the electricity charge of micro algae growth light source3·d；And made using aeration The aeration pump power that DO maintains essentially in 9.9mg/L and 7.8mg/L or so needs in micro algae growth room and cathode chamber is 25W, is pressed It is calculated according to daily aeration 12h, cost is about 15 yuan/m3D, therefore, the cost needed for being supplied oxygen using water treatment facilities of the present invention The 64% of only external aeration cost.
Embodiment 4:
Specific step is as follows:
It is to separate with cation-exchange membrane (20cm × 50cm) with graphite felt (20cm × 50cm) for anode according to Fig. 1 Film, using carbon black-polytetrafluoroethylene (PTFE) (PTFE) gas diffusion cathode as cathode (20cm × 50cm), anode chamber and cathode building volume It is 20L (20cm × 20cm × 50cm), micro algae growth building volume is 30L (20cm × 30cm × 50cm), and anode and cathode spacing is 10cm；
Sanitary sewage is passed through in anode chamber by third water inlet, by Na2SO4Solution (50mM) passes through the second water inlet It is passed through in cathode chamber, micro-algae culture medium is passed through in micro algae growth room by the first water inlet, obtains hydrogen peroxide reaction system； It is inoculated with micro- quasi- ball algae (Nannochloropsissp.) in micro-algae culture medium, inoculation initial concentration is 5 × 106Cell/mL is opened Light source (being made of 2 8WLED fluorescent tubes) carries out illumination (Light To Dark Ratio 12h:12h), and microalgae is made to produce oxygen, after 2d, micro algae growth room Maintain essentially in 11.3mg/L and 10.1mg/L or so with DO in cathode chamber, after 10d microalgae reach growth stationary phase, stop into The algae solution of 80% volume is discharged by the discharge outlet of micro algae growth room lower part, re-starts into water, continues to cultivate for water；At sewage It is that inoculum is seeded in PBS buffer solution that the reason cotton-shaped denitrification pond sludge of factory, which is inoculum, the external 1000 Ω resistance at power supply And power on after the output voltage of power supply is not less than 100mV, it is electric to 0.4V is applied between anode and cathode with constant voltage source Pressure is to prepare hydrogen peroxide.
When 10d, the algae solution of taking-up is subjected to grease extraction, discovery lipid-producing reaches 305mg/Ld；After 8d, detection yin H in pole room2O2Concentration, find H2O2Accumulated concentrations be 150mg/L.
In this embodiment, maintain essentially in DO in micro algae growth room (30L) and cathode chamber (20L) using the present invention Cost needed for 9.9mg/L and 7.8mg/L or so includes the 9.6 yuan/m of the electricity charge of micro algae growth light source3·d；And made using aeration The aeration pump power that DO maintains essentially in 9.9mg/L and 7.8mg/L or so needs in micro algae growth room and cathode chamber is 25W, is pressed It is calculated according to daily aeration 12h, cost is about 15 yuan/m3D, therefore, the cost needed for being supplied oxygen using water treatment facilities of the present invention The 32% of only external aeration cost.
Although the present invention has been described by way of example and in terms of the preferred embodiments, it is not intended to limit the invention, any to be familiar with this skill The people of art can do various change and modification, therefore protection model of the invention without departing from the spirit and scope of the present invention Enclosing subject to the definition of the claims.

Claims (10)

1. a kind of device that can be used for producing hydrogen peroxide, which is characterized in that described device includes micro algae growth room, is provided with yin The cathode chamber of pole, the anode chamber for being internally provided with anode, for providing the light source of luminous energy to microalgae, and for jointed anode and The power supply of cathode；
The micro algae growth room is inoculated with microalgae；The cathode is gas diffusion cathode；It is living that electrochemistry is attached on the anode Property microorganism；
The micro algae growth room and cathode chamber are spaced by cathode；The cathode chamber and anode chamber are spaced by separation membrane；
The first water inlet, the first water outlet and algae solution outlet are provided on the micro algae growth room；It is set on the cathode chamber It is equipped with the second water inlet and the second water outlet；Third water inlet and third water outlet are provided in the anode chamber.
2. a kind of device that can be used for producing hydrogen peroxide as described in claim 1, which is characterized in that the micro algae growth room For column, contain the first top surface, the first bottom surface and first side；First water inlet, algae solution outlet are located at microalgae The lower section of growth room's first side or the first bottom surface of micro algae growth room；First water outlet is located at the first side of micro algae growth room The top in face or the first top surface of micro algae growth room.
3. a kind of device that can be used for producing hydrogen peroxide as claimed in claim 1 or 2, which is characterized in that the cathode chamber For column, contain the second top surface, the second bottom surface and second side；Second water inlet is located at cathode chamber second side Lower section or the second bottom surface of cathode chamber；Second water outlet is located at the top of cathode chamber second side or the second top of cathode chamber Face.
4. a kind of device that can be used for producing hydrogen peroxide a method according to any one of claims 1-3, which is characterized in that the anode Room is column, contains third top surface, third bottom surface and third side；The third water inlet is located at anode chamber third side Lower section or anode chamber third bottom surface；The third water outlet is located at the top of anode chamber third side or the third of anode chamber Top surface.
5. a kind of device that can be used for producing hydrogen peroxide as described in claim 1-4 is any, which is characterized in that the anode For one of carbon brush, carbon cloth, carbon paper, graphite felt or graphite plate or a variety of.
6. a kind of device that can be used for producing hydrogen peroxide a method as claimed in any one of claims 1 to 5, which is characterized in that the separation Film includes cation-exchange membrane or proton exchange membrane.
7. a kind of device that can be used for producing hydrogen peroxide as described in claim 1-6 is any, which is characterized in that the power supply Voltage range for constant voltage source and power supply application is 0.1V~0.8V.
8. a kind of method for producing hydrogen peroxide, which is characterized in that the method be using it is as claimed in claim 1 to 7 it is described can For producing the device of hydrogen peroxide.
9. a kind of method for producing hydrogen peroxide as claimed in claim 8, which is characterized in that the method is that will contain sodium acetate And/or glucose phosphate buffer or waste water A need to be handled be passed through in anode chamber by third water inlet, by Na2SO4Solution It is passed through in cathode chamber by the second water inlet, by micro-algae culture medium or waste water B need to be handled by the first water inlet to be passed through microalgae raw In long room, hydrogen peroxide reaction system is obtained；In micro-algae culture medium or it need to handle and be inoculated with microalgae in waste water B, open light source and carry out Illumination makes microalgae produce oxygen, obtains oxygen and algae solution；It is seeded to using the anaerobic sludge containing electro-chemical activity microorganism as inoculum Phosphate buffer need to be handled in waste water A, outer connecting resistance and be powered on until the output voltage of power supply is not low at power supply After 100mV, with constant voltage source to voltage is applied between anode and cathode, hydrogen peroxide is obtained；
After the micro algae growth in micro algae growth room enters stationary phase, algae solution can be discharged by algae solution outlet and carry out mentioning for grease It takes, while by another batch of micro-algae culture medium or waste water B need to be handled micro algae growth room is passed through by the first water inlet；
The waste water A that need to handle includes sanitary sewage, kitchen waste water, food processing wastewater or the waste water containing hardly degraded organic substance；
The waste water B that need to handle is nitrogenous and/or phosphorus waste water.
10. production peroxidating described in the device or claim 8 or 9 of production hydrogen peroxide as claimed in claim 1 to 7 Application of the method for hydrogen in terms of producing hydrogen peroxide.
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CN110684645A (en) * 2019-11-25 2020-01-14 中国科学院天津工业生物技术研究所 High-efficiency carbon or nitrogen supply device for microalgae autotrophy
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