CN104192978B - A kind of apparatus and method of optoacoustic Synergistic degradation perfluoro octane sulfonate - Google Patents
A kind of apparatus and method of optoacoustic Synergistic degradation perfluoro octane sulfonate Download PDFInfo
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Abstract
The invention discloses a kind of apparatus and method of optoacoustic Synergistic degradation perfluoro octane sulfonate, this device includes supersonic generator and is placed on supersonic generator for keeping the tank of reaction temperature, it is provided with for containing the reactor containing potassium perfluoroctane sulfonate waste water in tank, it is provided with uviol lamp, this reactor is obtained by inertia material above described reactor.Method comprises the steps：A) the pending waste water containing potassium perfluoroctane sulfonate is added in reactor, add heteropoly acid as catalyst, add H2O2, control ph is between 2～4；B) uviol lamp and supersonic generator are opened, setting ultrasonic power is 100W, reacts 3～5 hours, you can water outlet.Apparatus of the present invention structure is simple, UV US/H3PW12O40Optoacoustic concerted catalysis oxidation system has given full play to the photocatalysiss under 254nm ultraviolet irradiation of the ultrasonic strong decomposition of 358kHz and heteropoly acid it is achieved that effective degraded of PFOS and defluorinate.
Description
Technical field
The invention belongs to environmental project water-treatment technology field, it is with regard to persistence organic pollutant PFO in water body
The processing meanss of perfluorochemical and the methods such as sulfonate (PFOS), specially one kind are based on UV-US/H3PW12O40System is worked in coordination with
The apparatus and method of potassium perfluoroctane sulfonate (PFOS) in catalyzing oxidizing degrading water.
Background technology
Perfluorochemical (PFCs) is widely used in weaving, papermaking, packaging, pesticide, carpet, leather, polishing floor, washes
The industry such as hair-care shampoo and fire foam and civil area.PFCs present in environment mainly have perfluori piated carboxylic acids, perfluorinated sulfonic acid class,
Perfluor amide-type and perfluor telomeric alcohol etc., and perfluoro caprylic acid (PFOA) is most widely used at present with perfluoro octane sulfonate (PFOS)
General perfluor Organic substance, PFOS is big compared with PFOA degraded difficulty.It produces in a large number and uses and causes in the world's ecosystems
Very serious environment accumulation and persistent pollution.
The C-F key that PFOS has leads to its chemical property sufficiently stable, not yet finds that they are degraded in vivo so far
Any evidence and relevant report, do not find the research of its any natural degradation yet.Conventional high-level oxidation technology is (as O3、
O3/UV、O3/H2O2And H2O2/Fe2+) it all can not be made effectively to degrade.Although many researcheres are directed to different perfluor class chemical combination at present
Thing has been carried out with the research of the removal of the means such as biodegradation, oxidoreduction, high temperature incineration and recovery technology method, but they are all not
There is the drawbacks such as low, slow, the low, secondary pollution of high energy consumption, complex operation, the response rate of speed of degradation efficiency with degree.Therefore, mesh
The front degraded repairing research with regard to PFCs is carried out also in starting stage, the only research of minority, such as subcritical system, light
Catalyst system and catalyzing degradation effect is preferable, but condition requirement is higher, and energy consumption is big；Photochemical catalytic oxidation system reaction condition is relatively mild, but
Defluorinate process is slow and inefficient；Photooxidation system is then because a large amount of oxidants lead to secondary pollution and too high expense using meeting
Problem, all difficult process for actual waste water.The effective defluorinating and degrading complete therefore how realizing PFOS is to be badly in need of asking of solution
One of topic.
Content of the invention
It is an object of the invention to provide a kind of be based on UV-US/H3PW12O40Perfluorooctane sulfonates in system catalysed promoted water
Potassium degraded and the apparatus and method of defluorinate, this system can achieve the efficient degradation of PFOS, improves defluorinate rate, shortens the response time.
The purpose of the present invention is achieved through the following technical solutions：
A kind of optoacoustic works in coordination with the device promoting potassium perfluoroctane sulfonate degraded and defluorinate in water, and this device includes ultrasound wave and sends out
Give birth to device (high frequency) and be placed on supersonic generator for keeping the tank of reaction temperature, be provided with tank and contain perfluor for containing
The reactor of perfluoroetane sulfonic acid potassium waste water, is provided with uviol lamp above described reactor, and this reactor is obtained by inertia material.
Described uviol lamp is horizontally placed on reactor, and is 3～5cm with the distance of liquid level in reactor.
The power of described uviol lamp is 11W, and launches the ultraviolet light of 254nm.
Described supersonic generator tranmitting frequency is 358kHz, and rated power is 100W.
Described reactor is the cylindrical vessel being obtained by politef, which is provided with probe tube, for sampling analyses；
Described tank is provided with condensate pipe.
Using the method for potassium perfluoroctane sulfonate in said apparatus degradation water, comprise the steps：
A) the pending waste water containing potassium perfluoroctane sulfonate is added in reactor, add heteropoly acid (H3PW12O40) make
For catalyst, add H2O2As oxidant, control ph is between 2～4；
B) uviol lamp and supersonic generator are opened, setting ultrasonic power is 100W, reacts 3～5 hours, you can water outlet.
Described potassium perfluoroctane sulfonate is 1 with the mass ratio of heteropoly acid:50～1:150, the concentration of heteropoly acid is 0.5～
1.5g/L.
Described heteropoly acid is phosphotungstic acid (H7[P(W2O7)6]·XH2O), analysis is pure, is purchased from the limited public affairs of Tianjin all generations chemical industry
Department.
Described reaction is carried out under conditions of 30～40 DEG C of constant temperature.
Described potassium perfluoroctane sulfonate is 1 with the mass ratio of oxidant:5～1:20.
Wherein, pH is best results when 2, can determine actual pH according to water quality situation, economy etc..
Pretreatment is carried out to the polluted water body containing PFOS, the higher water body of turbidity need to be filtered, reduce outstanding in water
The attenuation to ultraviolet for the float.Preferably, in pending polluted water body the concentration range of PFOS in 5～30mg/L,
The dosage of oxidant is 50～200mg/L.
Uviol lamp of the present invention needs the cell outside closed reactor when using, prevent ultraviolet light from operator around are caused hinder
Evil.Add oxidant H2O2System is played a driving role, this facilitation by oxidant improve photocatalyst regeneration rate and
Increased oxygen concentration in system to realize.
The present invention compared with prior art, has the advantage that：
1) structure of apparatus of the present invention is simple, and ultrasound wave, ultraviolet light constitute UV-US/ with the heteropolyacid catalyst adding
H3PW12O40Optoacoustic concerted catalysis oxidation system, has given full play to ultrasonic strong decomposition with heteropoly acid in 254nm ultraviolet irradiation
Under photocatalysiss it is achieved that effective degraded of PFOS and defluorinate.
2) reaction condition is simple：This system uviol lamp power is 11w；System without out-source gas, general photocatalytic system
Out-source gas are needed persistently to supply, and system of the present invention no requirement (NR) on reaction atmosphere；This system is to temperature-insensitive, reaction solution
PH value can achieve efficient degradation in the range of 2～4, and reaction condition is simpler.
3) defluorination effect is good：Under the conditions of same treatment, this UV-US/H3PW12O4The degraded defluorination effect of system is substantially good
In independent ultrasound system and photocatalytic system, defluorinate rate can be promoted to more than 75% compared with traditional method highest, and defluorinate speed is accelerated.
4) reduce toxicity：Ultrasound wave can shorten the carbon chain lengths of perfluorochemical, reduces its toxicity, reduces residue,
Its toxic intermediates is greatly reduced compared with photocatalytic system, is conducive to repairing the environment of PFOS pollution.
Brief description
Fig. 1 is the structural representation of apparatus of the present invention.
Specific embodiment
With reference to embodiment and accompanying drawing, the present invention is described in further detail, but embodiments of the present invention do not limit
In this.
Embodiment 1
A kind of optoacoustic works in coordination with the device (UV/H promoting potassium perfluoroctane sulfonate degraded and defluorinate in water3PW12O40System), should
Device includes supersonic generator 1 and is placed on supersonic generator 1 for keeping the tank 3 of reaction temperature, is provided with tank 3
For containing the reactor 5 containing potassium perfluoroctane sulfonate waste water, above described reactor 5, it is provided with low pressure ultraviolet lamp 4, described ultraviolet
Lamp 4 is horizontally placed on reactor 5, and is 3cm with the distance of liquid level in reactor 5.Described reactor 5 is by politef system
The cylindrical vessel obtaining, which is provided with probe tube 6.Tank 3 is provided with condensate pipe 2.
The power of described uviol lamp 4 is 11W, and launches the ultraviolet light of 254nm.
Process the ultra-pure water containing PFOS, the original pH of water sample is 6.91, PFOS concentration is 10mg/L, F-Concentration is about 0 (not
Detection), it is not required to pretreatment, can directly be degraded.
Using the method for PFOS in this device degradation water, only apply uviol lamp in the present embodiment, be not turned on high frequency ultrasound
Generating meanss, that is, be used alone UV/H3PW12O40System degraded PFOS, comprises the steps：
A) pending waste water containing PFOS is added in reactor 5, be simultaneously introduced heteropoly acid, concentration is 1g/L, PFOS/
H3PW12O40(mass concentration ratio) is 1：100, one of which reactor adds 200mg/LH2O2Solution, another group of matched group is not added with
H2O2Solution, two groups of test reacting liquid pH values are adjusted to 2 with 0.1mol/LNaOH and HCl；
B) open ultraviolet light power supply 7, in course of reaction, the water in tank 3 relies on condensate pipe 2 to realize continuously flowing,
React under in the air normal pressure, no out-source gas, reaction temperature is held at 30 DEG C by tank 3-dimensional, and system reacts 4 under conditions of constant temperature
Hour；
C) close ultraviolet light power supply 7, close supersonic generator 1, reaction terminates, water outlet, water is detected using chromatography of ions
Middle F-Concentration, determines defluorinate rate.
After testing, without H2O2When, UV/H3PW12O40The defluorinate rate only 9.47% of system, and add H2O2, PFOS's is de-
Fluorine rate reaches 33.33%, illustrates that the addition of oxidant can promote the photocatalysis defluorination effect of PFOS.
Embodiment 2
A kind of optoacoustic works in coordination with device (the low frequency US-UV/H promoting potassium perfluoroctane sulfonate degraded and defluorinate in water3PW12O40
System), this device includes supersonic generator 1 and is placed on supersonic generator 1 for keeping the tank 3 of reaction temperature, water
It is provided with groove 3 for containing the reactor 5 containing potassium perfluoroctane sulfonate waste water, above described reactor 5, be provided with low pressure ultraviolet lamp
4, described uviol lamp 4 is horizontally placed on reactor 5, and is 3cm with the distance of liquid level in reactor 5.Described reactor 5 is by gathering
The cylindrical vessel that tetrafluoroethene is obtained, which is provided with probe tube 6.Tank 3 is provided with condensate pipe 2.
The power of described uviol lamp 4 is 11W, and launches the ultraviolet light of 254nm.Described supersonic generator 1 surpasses for low frequency
Acoustic transmitter, tranmitting frequency is 40kHz, and rated power is 120W.
Process the ultra-pure water containing PFOS, the original pH of water sample is 6.96, PFOS concentration is 10mg/L, F-Concentration is about 0 (not
Detection), it is not required to pretreatment, can directly be degraded.
Using the method for PFOS in this device degradation water, that is, adopt independent low frequency ultrasound and low frequency US-UV/H3PW12O40Body
System contrast degraded PFOS, comprises the steps：
A) pending waste water containing PFOS is added in reactor 5, be simultaneously introduced heteropoly acid, concentration is 1g/L, PFOS/
H3PW12O40(mass concentration ratio) is 1：100, add 200mg/L H2O2Solution, pH value is adjusted with 0.1mol/L NaOH and HCl
For 2；
B) open the power supply of ultrasound wave 1, set reaction power as 100W, open ultraviolet light power supply 7 simultaneously, and matched group examination
Test and be not turned on uviol lamp, in course of reaction, the water in tank 3 relies on condensate pipe 2 to realize continuously flowing, in atmosphere under normal pressure
Reaction, no out-source gas, reaction temperature is held at 30 DEG C by tank 3-dimensional, and system is reacted 4 hours under conditions of constant temperature；
C) close ultraviolet light power supply 7, close supersonic generator 1, reaction terminates, water outlet, water is detected using chromatography of ions
Middle F-Concentration, determines defluorinate rate.
After testing, high-frequency ultrasonic directly degrade PFOS defluorinate rate be 10.1%, low frequency US-UV/H3PW12O40System
Defluorinate rate reaches 20.4%, but UV/H3PW12O40The defluorinate rate of system has reached 33.33% (see embodiment 1), and low frequency ultrasound is described
Introducing PFOS has been degraded inhibitory action.
Embodiment 3
A kind of optoacoustic works in coordination with device (the high frequency US-UV/H promoting potassium perfluoroctane sulfonate degraded and defluorinate in water3PW12O40
System), this device includes supersonic generator 1 and is placed on supersonic generator 1 for keeping the tank 3 of reaction temperature, water
It is provided with groove 3 for containing the reactor 5 containing potassium perfluoroctane sulfonate waste water, above described reactor 5, be provided with low pressure ultraviolet lamp
4, described uviol lamp 4 is horizontally placed on reactor 5, and is 3cm with the distance of liquid level in reactor 5.Described reactor 5 is by gathering
The cylindrical vessel that tetrafluoroethene is obtained, which is provided with probe tube 6.Tank 3 is provided with condensate pipe 2.
The power of described uviol lamp 4 is 11W, and launches the ultraviolet light of 254nm.Described supersonic generator 1 surpasses for high frequency
Acoustic generator, tranmitting frequency is 358kHz, and rated power is 100W.
Process the ultra-pure water containing PFOS, the original pH of water sample is 6.86, PFOS concentration is 10mg/L, F-Concentration is about 0 (not
Detection), it is not required to pretreatment, can directly be degraded.
Using the method for PFOS in this device degradation water, that is, adopt independent high frequency ultrasound and high frequency US-UV/H3PW12O40Body
System contrast degraded PFOS, comprises the steps：
A) pending waste water containing PFOS is added in reactor 5, be simultaneously introduced heteropoly acid, concentration is 1g/L, PFOS/
H3PW12O40(mass concentration ratio) is 1：100, add 200mg/L H2O2Solution, pH value is adjusted with 0.1mol/L NaOH and HCl
For 2；
B) open the power supply of ultrasound wave 1, set reaction power as 100W, open ultraviolet light power supply 7 (independent high frequency surpasses simultaneously
Sound system is not turned on ultraviolet source), in course of reaction, the water in tank 3 relies on condensate pipe 2 to realize continuously flowing, in air
React under middle normal pressure, no out-source gas, reaction temperature is held at 30 DEG C by tank 3-dimensional, and it is little that system reacts 4 under conditions of constant temperature
When；
C) close ultraviolet light power supply 7, close supersonic generator 1, reaction terminates, water outlet, water is detected using chromatography of ions
Middle F-Concentration, determines defluorinate rate.
After testing, high frequency US-UV/H3PW12O40In system, the defluorinate rate of PFOS reaches 82.5%, and independent ultrasound system takes off
Fluorine rate is 58.5%, UV/H3PW12O40The defluorinate rate of system is 33.3% (see embodiment 1), illustrates that the introducing of high frequency ultrasound is favourable
In the degraded of PFOS, the UV-US/H of the present invention3PW12O4Optoacoustic collaboration system has good degradation effect for PFOS, can be real
Existing simple condition is issued to higher defluorinate rate.
Embodiment 4
A kind of optoacoustic works in coordination with device (the high frequency US-UV/H promoting potassium perfluoroctane sulfonate degraded and defluorinate in water3PW12O40
System), this device includes supersonic generator 1 and is placed on supersonic generator 1 for keeping the tank 3 of reaction temperature, water
It is provided with groove 3 for containing the reactor 5 containing potassium perfluoroctane sulfonate waste water, above described reactor 5, be provided with low pressure ultraviolet lamp
4, described uviol lamp 4 is horizontally placed on reactor 5, and is 3cm with the distance of liquid level in reactor 5.Described reactor 5 is by gathering
The cylindrical vessel that tetrafluoroethene is obtained, which is provided with probe tube 6.Tank 3 is provided with condensate pipe 2.
The power of described uviol lamp 4 is 11W, and launches the ultraviolet light of 254nm.Described supersonic generator 1 surpasses for high frequency
Acoustic generator, tranmitting frequency is 358kHz, and rated power is 100W.
Process the ultra-pure water containing PFOS, the original pH of water sample is 6.90, PFOS concentration is 10mg/L, F-Concentration is about 0 (not
Detection), it is not required to pretreatment, can directly be degraded.
Using the method for PFOS in this device degradation water, attempt contrast degraded PFOS at a temperature of differential responses, including such as
Lower step：
A) pending waste water containing PFOS is added in reactor 5, be simultaneously introduced heteropoly acid, concentration is 1g/L, PFOS/
H3PW12O40(mass concentration ratio) is 1：100, add 200mg/L H2O2Solution, pH value is adjusted with 0.1mol/L NaOH and HCl
For 2；
B) open the power supply of ultrasound wave 1, set reaction power as 100W, open ultraviolet light power supply 7, course of reaction simultaneously
In, the water in tank 3 relies on condensate pipe 2 to realize continuously flowing, and reacts in atmosphere, no out-source gas under normal pressure, reaction temperature
Degree is held at 35 DEG C by tank 3-dimensional, and another group of design temperature is 40 DEG C, and system is reacted 4 hours under conditions of constant temperature；
C) close ultraviolet light power supply 7, close supersonic generator 1, reaction terminates, water outlet, water is detected using chromatography of ions
Middle F-Concentration, determines defluorinate rate.
After testing, when reaction temperature is 35 DEG C, high frequency US-UV/H3PW12O40In system, the defluorinate rate of PFOS reaches
84.1%, and reaction temperature is that when 40 DEG C, system defluorinate rate is 81.2%, that is, when reaction temperature is 30～40 DEG C, system defluorinate
Rate is more or less the same, the UV-US/H of the present invention3PW12O4Optoacoustic collaboration system has good degradation effect for PFOS, can be real
Existing simple condition is issued to higher defluorinate rate.
Embodiment 5
High frequency US-UV/H3PW12O40System is degraded in aqueous medium from the beginning
Process the tap water containing PFOS, the original pH of water sample is 7.3, PFOS concentration is 10mg/L, F-Concentration is about 0 (not
Detection), turbidity is relatively low, is not required to pretreatment, can directly be degraded.
Using the method for PFOS in this device degradation water, comprise the steps：
A) pending waste water containing PFOS is added in reactor 5, be simultaneously introduced heteropoly acid, concentration is 1g/L, PFOS/
H3PW12O40(mass concentration ratio) is 1：100, add 200mg/L H2O2Solution, pH value is adjusted with 0.1mol/L NaOH and HCl
For 2；
B) open the power supply of ultrasound wave 1, set reaction power as 100W, open ultraviolet light power supply 7, course of reaction simultaneously
In, the water in tank 3 relies on condensate pipe 2 to realize continuously flowing, and reacts in atmosphere, no out-source gas under normal pressure, reaction temperature
Degree is held at 30 DEG C by tank 3-dimensional, and system is reacted 4 hours under conditions of constant temperature；
C) close ultraviolet light power supply 7, close supersonic generator 1, reaction terminates, water outlet, water is detected using chromatography of ions
Middle F-Concentration, determines defluorinate rate.
After testing, after reaction, the defluorinate rate of PFOS reaches 74.6%, and under the same reaction conditions, UV/H3PW12O40System
Defluorinate rate be 5.65%, independent ultrasound system defluorinate rate be 48.7%, the UV-US/H of the present invention is described3PW12O4Optoacoustic is worked in coordination with
System has good degradation effect for PFOS in tap water medium, and achievable simple condition is issued to higher defluorinate
Rate.
Embodiment 6
High frequency US-UV/H3PW12O40System is degraded in natural aqueous medium
Process the Urban River Water containing PFOS (Zhujiang River university city section), the original pH of water sample is 7.03, PFOS concentration is 10mg/
L, F-Concentration is about 0 (detection), because raw water turbidity is higher, need to be processed after 0.22 μm of membrane filtration again.
Using the method for PFOS in this device degradation water, comprise the steps：
A) pending waste water containing PFOS is added in reactor 5, be simultaneously introduced heteropoly acid, concentration is 1g/L, PFOS/
H3PW12O40(mass concentration ratio) is 1：100, add 200mg/L H2O2Solution, pH value is adjusted with 0.1mol/L NaOH and HCl
For 2；
B) open the power supply of ultrasound wave 1, set reaction power as 100W, open ultraviolet light power supply 7, course of reaction simultaneously
In, the water in tank 3 relies on condensate pipe 2 to realize continuously flowing, and reacts in atmosphere, no out-source gas under normal pressure, reaction temperature
Degree is held at 30 DEG C by tank 3-dimensional, and system is reacted 4 hours under conditions of constant temperature；
C) close ultraviolet light power supply 7, close supersonic generator 1, reaction terminates, water outlet, water is detected using chromatography of ions
Middle F-Concentration, determines defluorinate rate.
After testing, after reaction, the defluorinate rate of PFOS reaches 58.3%, and under the same reaction conditions, UV/H3PW12O40System
Defluorinate rate be 2.14%, independent ultrasound system defluorinate rate be 47.7%, the UV-US/H of the present invention is described3PW12O4Optoacoustic is worked in coordination with
System still has good degradation effect for PFOS in natural aqueous medium, and achievable simple condition is issued to higher defluorinate
Rate.
Above-described embodiment is the present invention preferably embodiment, but embodiments of the present invention are not subject to above-described embodiment
Limit, other any spirit without departing from the present invention and the change made under principle, modification, replacement, combine, simplify,
All should be equivalent substitute mode, be included within protection scope of the present invention.
Claims (4)
1. a kind of method of optoacoustic Synergistic degradation perfluoro octane sulfonate is it is characterised in that adopt following device, including ultrasound wave
Generator and be placed in and be used for keeping the tank of reaction temperature on supersonic generator, is provided with tank and contains PFO for containing
The reactor of potassium sulfonate waste water, is provided with uviol lamp above described reactor, and described uviol lamp is horizontally placed on reactor, and with anti-
The distance answering liquid level in device is 3～5cm, and this reactor is obtained by inertia material；Degradation step is as follows：
A) the pending waste water containing potassium perfluoroctane sulfonate is added in above-mentioned reactor, adds heteropoly acid as catalyst,
Add H2O2As oxidant, control ph is between 2～4；Described heteropoly acid be phosphotungstic acid, described potassium perfluoroctane sulfonate with
The mass ratio of heteropoly acid is 1:50～1:150, the concentration of heteropoly acid is 0.5～1.5g/L；
B) uviol lamp and supersonic generator are opened, the power of uviol lamp is 11W, and launches the ultraviolet light of 254nm；Ultrasound wave is sent out
Raw device tranmitting frequency is 358kHz, and ultrasonic power is 100W, reacts 3～5 hours, you can water outlet.
2. method according to claim 1 is it is characterised in that described reactor is the cylinder being obtained by politef
Vessel, which is provided with probe tube；Described tank is provided with condensate pipe.
3. method according to claim 1 and 2 is it is characterised in that described reaction is entered under conditions of 30～40 DEG C of constant temperature
OK.
4. method according to claim 3 is it is characterised in that described potassium perfluoroctane sulfonate with the mass ratio of oxidant is
1:5～1:20.
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| CN109179569A (en) * | 2018-11-14 | 2019-01-11 | 四川中盛净源环保设备有限公司 | A kind of processing organic wastewater with difficult degradation thereby oxidant cooperative photocatalysis oxidation reaction apparatus and application |
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