CN104773884A - Co-used iron-carbon micro-electrolysis and photo degradation two-section perfluoro octanoic acid degradation method - Google Patents
Co-used iron-carbon micro-electrolysis and photo degradation two-section perfluoro octanoic acid degradation method Download PDFInfo
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- CN104773884A CN104773884A CN201510106537.0A CN201510106537A CN104773884A CN 104773884 A CN104773884 A CN 104773884A CN 201510106537 A CN201510106537 A CN 201510106537A CN 104773884 A CN104773884 A CN 104773884A
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Abstract
The invention discloses a co-used iron-carbon micro-electrolysis and photo degradation two-section perfluoro octanoic acid degradation method. The method comprises the following steps: (a) active carbon pretreatment: soaking active carbon in a perfluoro octanoic acid solution to be processed for 24 hours, washing the active carbon by ultrapure water, and drying the active carbon for later use; (b) adding the perfluoro octanoic acid water solution to be processed in to an iron-carbon micro-electrolysis reactor, adding iron powder and processed active carbon simultaneously, controlling the primary pH value of the reactions at a range of 2 to 4, carrying out reactions at a room temperature under stirring for one hour, and discharging the effluent; (c) subjecting the effluent to suction filtering, then introducing the effluent into a photo degradation reactor, adding H2O2 as the oxidant at the same time, controlling the pH value in a range of 2 to 4, installing an ultraviolet lamp; carrying out reactions at a constant temperature under stirring for 3 to 5 hours, and finally discharging the effluent. The provided method is simple, the two-section cooperative system fully utilizes the functions of the electrolysis and photo degradation, and the fluorine is effectively removed from PFOA.
Description
Technical field
The invention belongs to environmental engineering water-treatment technology field, be the treatment process about perfluorochemicals such as persistence organic pollutant Perfluorocaprylic Acids (PFOA) in water body, be specially a kind of method based on Perfluorocaprylic Acid (PFOA) in iron-carbon micro-electrolysis-VUV/Fenton system degradation water.
Background technology
Perfluorochemical (PFCs) is widely used in the industries such as chemical industry, mechanical industry, textile industry, paper industry.And perfluorinated sulfonic acid and Perfluorocaprylic Acid (PFOA) are current most widely used perfluor organism, it is also multiple PFCs final converted product in the environment.It is produced in a large number and uses in the world's ecosystems, has caused serious environment Cumulate Sum persistence pollution.
PFOA chemical property is very stable, not yet finds the evidence that they are degraded in vivo and relevant report so far, does not also find the research of its any natural degradation.The high-level oxidation technology of some routines is (as O
3, O
3/ UV, O
3/ H
2o
2and H
2o
2/ Fe
2+) it all can not be made effectively to degrade.Although many investigators have carried out with the research of the means removals such as biological degradation, redox, high temperature incineration with recovery technology method for different perfluorinated compound at present, the drawbacks such as degradation efficiency is low, speed is slow, energy consumption is high, the rate of recovery is low, secondary pollution that they exist all to some extent.Therefore, the repairing research at present about PFCs is also in developmental stage, and degradation technique is also mainly experimental study, applies less.Therefore the effective degraded how realizing PFOA is one of problem needing solution badly.
Summary of the invention
The object of the present invention is to provide a kind of apparatus and method of working in coordination with Perfluorocaprylic Acid defluorinate in promotion water based on iron-carbon micro-electrolysis-VUV/Fenton two-stage method, this system can realize the good defluorination of PFOA.
Object of the present invention is achieved through the following technical solutions:
Based on a device for iron-carbon micro-electrolysis-VUV/Fenton two-stage method Synergistic degradation Perfluorocaprylic Acid, this device is made up of iron-carbon micro-electrolysis reaction unit and photodegradation reaction unit two portions.
Described iron-carbon micro-electrolysis reaction unit, comprises for splendid attire containing the iron-carbon micro-electrolysis reactor of the aqueous solution of PFOA, gac and carbon dust and the stirring rake that is provided with.This reactor is obtained by inertia material.
Described photodegradation reaction unit, the cell comprising airtight shading and the constant temperature blender with magnetic force arranged in cell, and the reactor be placed in for the water outlet of splendid attire iron-carbon micro-electrolysis device on agitator, be provided with vacuum UV lamp in described reactor, this reactor is obtained by inertia material.
One end that described vacuum UV lamp connects power supply is fixed on above reactor, and the other end stretches in reactor.
A method for iron-carbon micro-electrolysis and photodegradation two-stage method Synergistic degradation Perfluorocaprylic Acid, comprises the steps:
A) pre-treatment of gac: utilize Perfluorocaprylic Acid solution soaking gac to be dealt with 24 hours, clean with ultrapure water, dry stand-by;
B) the pending Perfluorocaprylic Acid aqueous solution (not soaking the PFOA solution of gac) is added iron-carbon micro-electrolysis reactor, add iron powder and pretreated gac simultaneously, control reaction initial pH value between 2 ~ 4, react 1 hour under the condition of room temperature, stirring, water outlet;
C) water outlet of iron-carbon micro-electrolysis reactor enters light DeR device after suction filtration, adds H simultaneously
2o
2as oxygenant, control ph, between 2 ~ 4, inserts vacuum UV lamp; React 3 ~ 5 hours under the condition of constant temperature, stirring, get final product water outlet.
Described gac dosage is 7.5 ~ 17.5g/L, and iron powder dosage is 2.5 ~ 12.5g/L.
Described gac dosage is 12.5g/L, and iron powder dosage is 7.5g/L, and when in iron-carbon micro-electrolysis reactor and photodegradation reactor, pH is 3, PFOA defluorination effect is best, can determine real reaction condition according to water quality situation, economy etc.。
Described H
2o
2concentration be 0.45 ~ 2.25g/L.
The power of described vacuum UV lamp is 8W, and can launch the UV-light of 185nm and 254nm simultaneously.
Described iron-carbon micro-electrolysis reactor and photodegradation reactor are obtained by tetrafluoroethylene, which is provided with stopple coupon.
Described stir speed (S.S.) is 200r/min.
The present invention does not need to carry out pre-treatment to the polluted water body containing PFOA.The cell that ultraviolet lamp needs outside closed reactor when using, prevents UV-light from damaging around operator.Add oxygenant H
2o
2play a driving role to system, this promoter action improves oxygen concn in the regeneration rate of photocatalyst and increase system by oxygenant and realizes.
Compared with prior art, tool has the following advantages in the present invention:
1) the inventive method technique is simple, photodegradation reaction process given full play to iron-carbon micro-electrolysis effect, photodegradation reaction in direct photolysis effect (VUV) and photocatalytic Degradation (UV/Fenton), achieve effective degraded and the defluorinate of PFOA.
2) reaction conditions is simple: this system ultraviolet lamp power is 8W; System is without the need to out-source gas, and general photochemical catalysis system needs out-source gas to continue air feed, and system of the present invention no requirement (NR) on reaction atmosphere; This system is to temperature-insensitive, and reacting solution pH value can realize effective defluorinate in 2 ~ 4 scopes, and reaction conditions is simpler.
3) additional Fe is not needed
3+: the Fe that the photodegradation stage directly utilizes iron-carbon micro-electrolysis to produce
2+, existing Fenton oxidation Degradation, reaches direct photolysis and photocatalytic Degradation again simultaneously.
4) reduce toxicity: body series can shorten the carbon chain lengths of perfluorochemical, reduces its toxicity, reduce residue, its toxic intermediates comparatively photochemical catalysis system greatly reduces, and is conducive to the environment repairing PFOA pollution.
Accompanying drawing explanation
Fig. 1 is the structural representation of iron-carbon micro-electrolysis reaction unit of the present invention.
Fig. 2 is the structural representation of photodegradation reaction unit of the present invention.
Embodiment
Below in conjunction with embodiment and accompanying drawing, the present invention is described in further detail, but embodiments of the present invention are not limited thereto.
Embodiment 1
A kind of method (iron-carbon micro-electrolysis) of Perfluorocaprylic Acid in iron-carbon micro-electrolysis-VUV/Fenton two-stage method Synergistic degradation water, the method is reacted two portions by iron-carbon micro-electrolysis reaction and photodegradation and is formed.Iron-carbon micro-electrolysis reaction unit, comprise stirring rake 1 and the splendid attire reactor 3 containing the Perfluorocaprylic Acid aqueous solution, stirring rake 1 is placed in the middle of reactor 3.Described reactor 3 is the cylindrical vessel obtained by tetrafluoroethylene, which is provided with stopple coupon 2, and in reactor 3, the aqueous solution 4 is made up of the Perfluorocaprylic Acid aqueous solution, gac and iron powder.Photodegradation reaction unit, comprises time constant-temperature magnetic stirring apparatus 10 and photodegradation reactor 9, and described photodegradation reactor 9 is placed on time constant-temperature magnetic stirring apparatus 10.Place ultraviolet lamp 7 in photodegradation reactor 9, described ultraviolet lamp 7 is perpendicular is placed in photodegradation reactor 9 inside.Described reactor 9 is the cylindrical vessel obtained by tetrafluoroethylene, which is provided with stopple coupon 5.
The power of described ultraviolet lamp is 8W, and can launch the UV-light of 254nm and 185nm simultaneously.
Process is containing the ultrapure water of PFOA, and the original pH of water sample is 4.6, PFOA concentration is 10mg/L, F
-concentration is about 0 (not detecting), does not need pre-treatment, can directly degrade.
Utilize the method for PFOA in this device degradation water, in the present embodiment, do not open ultraviolet lamp, namely use iron-carbon micro-electrolysis degraded PFOA, comprise the steps:
A) pre-treatment is carried out to gac, take quantitative gac, soak 24 hours in PFOA solution to be dealt with, clean with ultrapure water, dry for standby;
B) pending PFOA solution (not soaking the PFOA solution of gac) is joined in reactor, add pretreated gac 12.5g/L and iron powder 7.5g/L, NaOH and HCl of reaction soln pH 0.1mol/L is adjusted to 3.0 simultaneously;
C) open stirring rake, react 1 hour;
D) close stirring rake, reaction terminates, water outlet, adopts fluoride ion selective electrode to detect F
-concentration, determines defluorinate rate.
After testing, the defluorinate rate of iron-carbon micro-electrolysis water outlet is only 4.66%, illustrates that the defluorinate rate of iron-carbon micro-electrolysis to PFOA is not high.
Embodiment 2
The difference of the present embodiment and embodiment 1 is:
The present embodiment does not carry out iron-carbon micro-electrolysis reaction, comprises the steps:
A) pending PFOA solution is joined in photodegradation reactor, opens magnetic stirring apparatus, close cell 11, open ultraviolet lamp 7 (outside is provided with ultraviolet lamp lampshade 8), react 6 hours:
B) close ultraviolet lamp power supply 6, reaction terminates, water outlet, adopts fluoride ion selective electrode to measure F
-concentration, determines defluorinate rate.
After testing, be used alone ultraviolet lamp, it is 39.89% to the defluorinate rate of PFOA, illustrates that ultraviolet lamp has certain photolysis to PFOA.
Embodiment 3
The difference of the present embodiment and embodiment 1 is:
Utilize the method for PFOA in this device degradation water, comprise the steps:
A) pre-treatment is carried out to gac, take quantitative gac, in solution to be dealt with, invade bubble 24 hours, clean with ultrapure water, dry for standby;
B) join in reactor by pending PFOA solution, add pretreated gac 12.5g/L and iron powder 7.5g/L simultaneously, NaOH and HCl of reaction soln pH 0.1mol/L is adjusted to 3.0; Open stirring rake, react 1 hour;
C) close stirring rake, iron-carbon micro-electrolysis reaction terminates, and filters water outlet, is injected in photodegradation reactor, regulates pH to be 3.0, open UV-light power supply, react 6 hours with NaOH and HCl of 0.1mol/L;
D) close UV-light power supply, reaction terminates, water outlet, adopts fluoride ion selective electrode to detect F in water
-concentration, determines defluorinate rate.
After testing, be used alone VUV, defluorinate rate is 39.89%, and adds iron-carbon micro-electrolysis in front end, and its defluorinate rate is 21.02%, illustrates that after iron-carbon micro-electrolysis, only introduce UV-light does not have the defluorination of raising system to PFOA.
Embodiment 4
The difference of the present embodiment and embodiment 1 is:
Utilize the method for PFOA in this device degradation water, comprise the steps:
A) pre-treatment is carried out to gac, take quantitative gac, in solution to be dealt with, invade bubble 24 hours, clean with ultrapure water, dry for standby;
B) add in reactor 3 by the PFOA aqueous solution, add pretreated gac and iron powder simultaneously, gac dosage is 12.5g/L, and iron powder dosage is that 7.5g/L, solution ph 0.1mol/L NaOH and HCl is adjusted to 3.0, reacts 1 hour;
C) water outlet in filtration reactor 3, in photodegradation reactor 9 in injection device schematic diagram 2, pH value 0.1mol/L NaOH and HCl is adjusted to 3.0, adds hydrogen peroxide simultaneously, and hydrogen peroxide dosage is 0.45g/L, open UV-light power supply 6, close cell 11, whole reaction unit is placed on time constant-temperature magnetic stirring apparatus 10, reacts in atmosphere under normal pressure, without out-source gas, reaction carries out 6 hours;
D) close UV-light power supply 6, reaction terminates, water outlet, adopts fluoride ion selective electrode to detect F in water
-concentration, determines defluorinate rate.
After testing, after reaction, the defluorinate rate of PFOA reaches 46.81%, and under the same reaction conditions, the defluorinate rate of independent VUV to PFOA is 39.89%, its defluorinate rate of iron-carbon micro-electrolysis is only used to be only 4.66%, utilize iron-carbon micro-electrolysis-VUV defluorinate rate to be also only 21.02% (see embodiment 2), illustrate that the introducing of oxidant hydrogen peroxide can promote photocatalysis.
Above-described embodiment is the present invention's preferably embodiment; but embodiments of the present invention are not restricted to the described embodiments; change, the modification done under other any does not deviate from spirit of the present invention and principle, substitute, combine, simplify; all should be the substitute mode of equivalence, be included within protection scope of the present invention.
Claims (7)
1. a method for iron-carbon micro-electrolysis and photodegradation two-stage method Synergistic degradation Perfluorocaprylic Acid, is characterized in that, comprise the steps:
A) pre-treatment of gac: utilize Perfluorocaprylic Acid solution soaking gac to be dealt with 24 hours, clean with ultrapure water, dry stand-by;
B) the pending Perfluorocaprylic Acid aqueous solution is added iron-carbon micro-electrolysis reactor, add iron powder and pretreated gac simultaneously, control reaction initial pH value between 2 ~ 4, react 1 hour under the condition of room temperature, stirring, water outlet;
C) water outlet of iron-carbon micro-electrolysis reactor enters light DeR device after suction filtration, adds H simultaneously
2o
2as oxygenant, control ph, between 2 ~ 4, inserts vacuum UV lamp; React 3 ~ 5 hours under the condition of constant temperature, stirring, get final product water outlet.
2. method according to claim 1, is characterized in that, described gac dosage is 7.5 ~ 17.5g/L, and iron powder dosage is 2.5 ~ 12.5g/L.
3. method according to claim 2, is characterized in that, described gac dosage is 12.5g/L, and iron powder dosage is 7.5g/L, and in iron-carbon micro-electrolysis reactor and photodegradation reactor, pH is 3.
4. the method according to claim 1 or 2 or 3, is characterized in that, described H
2o
2concentration be 0.45 ~ 2.25g/L.
5. method according to claim 4, is characterized in that, the power of described vacuum UV lamp is 8W, and can launch the UV-light of 185nm and 254nm simultaneously.
6. method according to claim 5, is characterized in that, described iron-carbon micro-electrolysis reactor and photodegradation reactor are obtained by tetrafluoroethylene.
7. the method according to claim 1 or 2 or 3, it is characterized in that, described stir speed (S.S.) is 200r/min.
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN102849893A (en) * | 2012-08-06 | 2013-01-02 | 南京凯盛国际工程有限公司 | Treatment method of high-concentration nondegradable organic wastewater |
| CN103183397A (en) * | 2013-03-05 | 2013-07-03 | 华南理工大学 | Device and method for carrying out catalytic degradation on perfluorooctanoic acid in water |
| CN103613229A (en) * | 2013-08-07 | 2014-03-05 | 煤科集团杭州环保研究院有限公司 | Reinforced electrochemical coupling catalytic oxidation device and technology |
| CN104192978A (en) * | 2014-08-26 | 2014-12-10 | 华南理工大学 | Optoacoustic synergic perfluorooctane sulfonate (PFOS) degradation device and method |
-
2015
- 2015-03-11 CN CN201510106537.0A patent/CN104773884A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102849893A (en) * | 2012-08-06 | 2013-01-02 | 南京凯盛国际工程有限公司 | Treatment method of high-concentration nondegradable organic wastewater |
| CN103183397A (en) * | 2013-03-05 | 2013-07-03 | 华南理工大学 | Device and method for carrying out catalytic degradation on perfluorooctanoic acid in water |
| CN103613229A (en) * | 2013-08-07 | 2014-03-05 | 煤科集团杭州环保研究院有限公司 | Reinforced electrochemical coupling catalytic oxidation device and technology |
| CN104192978A (en) * | 2014-08-26 | 2014-12-10 | 华南理工大学 | Optoacoustic synergic perfluorooctane sulfonate (PFOS) degradation device and method |
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Application publication date: 20150715 |
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