CN106430515A - Phenol wastewater treatment technology using photoinduced catalytic oxidation energy-efficient method - Google Patents
Phenol wastewater treatment technology using photoinduced catalytic oxidation energy-efficient method Download PDFInfo
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- CN106430515A CN106430515A CN201610511984.9A CN201610511984A CN106430515A CN 106430515 A CN106430515 A CN 106430515A CN 201610511984 A CN201610511984 A CN 201610511984A CN 106430515 A CN106430515 A CN 106430515A
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/72—Treatment of water, waste water, or sewage by oxidation
- C02F1/725—Treatment of water, waste water, or sewage by oxidation by catalytic oxidation
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/30—Treatment of water, waste water, or sewage by irradiation
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/72—Treatment of water, waste water, or sewage by oxidation
- C02F1/722—Oxidation by peroxides
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2101/00—Nature of the contaminant
- C02F2101/30—Organic compounds
- C02F2101/34—Organic compounds containing oxygen
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2305/00—Use of specific compounds during water treatment
- C02F2305/02—Specific form of oxidant
- C02F2305/026—Fenton's reagent
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- Chemical & Material Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Hydrology & Water Resources (AREA)
- Engineering & Computer Science (AREA)
- Environmental & Geological Engineering (AREA)
- Water Supply & Treatment (AREA)
- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Health & Medical Sciences (AREA)
- Toxicology (AREA)
- Treatment Of Water By Oxidation Or Reduction (AREA)
Abstract
The invention discloses a phenol wastewater treatment technology using a photoinduced catalytic oxidation energy-efficient method, belonging to the technical field of environmental pollutant control. The phenol wastewater treatment technology using the photoinduced catalytic oxidation energy-efficient method can remarkably improve the degradation effect of phenol pollutants; under the conditions of visible light irradiation, H2O2 initial concentration of 50mM, pH of 3.0 and 3.0g/L Fe-montmorillonite, the removal rate of phenol can reach 100% within 120 minutes, and the removal rate of TOC can reach 80% in 180 minutes; and meanwhile, electric power resources can be saved by about 66.7%, and the treatment cost of the technology is greatly reduced.
Description
Technical field
The present invention relates to environmental contaminants control technology field, more particularly, to a kind of Photocatalysis energy-efficient side of oxidation
Method processes phenolic waste water technique.
Background technology
Phenol is a kind of important raw material of industry, and it can be used to synthetic plastic, fiber, medicine, agricultural chemicals, dyestuff, explosive
Deng product.It is estimated that domestic phenol annual production in 2015, more than 1,200,000 tons, also produces substantial amounts of phenol industrial wastewater simultaneously.
Phenolic waste water toxicity is big, and microorganism is difficult to it is degraded, and the therefore harm to organism is very big, needs it is effectively located
Reason.Traditional bioremediation concentration for the treatment of is low, and cycle length, it is difficult to reach wastewater discharge standard, has obvious deficiency；Physics
Method, such as active carbon adsorption advantages of good adsorption effect, but there is high cost, sorbing material is difficult to reclaim, and there is secondary pollution etc.
Problem.In recent years, phenol complete oxidation can be CO by chemical oxidation treatment phenolic waste water technology, particularly high-level oxidation technology2、
H2O and other small organic molecules, it is fast to have an oxidation rate, the problems such as non-secondary pollution, therefore obtains numerous researchers extensive
Research and concern.Traditional homogeneous Fenton oxidation method has been widely applied in industrial treatment waster water process, but homogeneously
Exist in Fenton processing procedure：Waste water needs to be acidified, and can produce a large amount of iron cements, H2O2Utilization rate is relatively low, and catalyst is difficult to separate
Deng deficiency, this virtually all can increase the operating cost of technique.For overcoming the photocatalysis that these shortcomings grow up heterogeneous
Fenton oxidation method, has efficient quick, simple operation and other advantages, and illumination is introduced catalysis system by this technology, is greatly facilitated
The catalytic effect of system, improves the degradation efficiency of phenol.
But, still there are many restraining factors in photocatalysis heterogeneous Fenton oxidative treatment phenol, as non-in some equal
Phase catalyst exist catalytic effect is poor, stability is bad and the shortcomings of not reproducible utilization, adds in system simultaneously
Ultraviolet light or visible ray can consume electric energy in a large number, all can increase process operation cost to a certain extent.Research shows, iron is modified to be covered
De- stone (Fe-Mt) has good catalytic effect to multiple hardly degraded organic substances, and catalyst stability is higher, repeats and utilizes
Property is preferable.But, in process treatment process, it is excessive still to there is power consumption, the problems such as high cost.Accordingly, it would be desirable to it is sharp
With develop a kind of energy-efficient technical method, further optimize technique processing procedure, heterogeneous to substantially reduce photocatalysis
Fenton oxidation method processes the processing cost of phenol.
Content of the invention
For solving the problems, such as existing phenolic waste water processing method, the invention provides Photocatalysis oxidation is efficiently
Power-economizing method processes phenolic waste water technique.
The present invention adopts the following technical scheme that：
The Photocatalysis of the present invention aoxidize efficient energy-saving method and process comprising the following steps that of phenolic waste water technique：
(1) phenol waste liquid is added in the quartzy light-catalyzed reaction pipe being totally dried, quartzy outer tube layer connects thermostat, adjust
Section pH to 3.0-3.5；
(2) add Fe- montmorillonite catalyst in phenol waste liquid, addition is 0.6-4.0g/L, magnetic agitation makes catalysis
Agent is sufficiently mixed uniformly；
(3) open xenon lamp, adjust power to 450-1000W, be then quantitatively adding the H that mass concentration is 30%2O2, make
H2O2And phenol molar concentration rate is between 35-48；
(4), after reaction starts 40-60 minute, turn off xenon lamp, when reaction continues to 120-180 minute, phenol degrading
Rate can reach 100%.
In step (1), preferably adjust pH to 3.3.
In step (1), adjust the H that pH agents useful for same is 2mol/L2SO4Or NaOH solution.
In step (1), the temperature of thermostat is 25-40 DEG C, preferably >=30 DEG C.
In step (2), the addition of preferably Fe- montmorillonite is 3.0g/L.
In step (2), magnetic agitation 1h.
Above-mentioned photoinduction Fe- montmorillonite catalysis heterogeneous Fenton oxidizing process degradation of phenol technical process both can ensure that height
The phenol degradation efficiency of effect, can save nearly 66.7% electric power resource simultaneously again.Card is tested by 100mg/L phenol degrading
Real, processing procedure can popularization and application in processing phenolic waste water.
Fe- montmorillonite, because having larger interlamellar spacing and specific surface area, therefore has good catalytic performance.Fe-Mt
Catalysis H2O2Generate hydroxyl radical free radical (OH), OH has stronger oxidisability, phenol can aoxidize generation aromatic series further
Intermediate product and short chain organic acid, finally oxidation generates CO2And H2O.When increasing xenon lamp radiation of visible light, can induce and produce virtue
Fragrant race intermediate product o-phenol and to biphenol.And the Fe (III) in Fe- montmorillonite can be reduced by both intermediate products
For Fe (II), thus accelerating the formation speed of OH, significantly lift the degradation rate of phenol.When visible light-inducing o-phenol
With the effect that may act as during to biphenol fast enriching to finite concentration similar to catalyst, even if turning off lamp source, not having can
See the catalyzing cooperation effect of light, still can keep higher phenol degradation efficiency.
Compared with prior art, the present invention has advantages below and beneficial effect：
The Photocatalysis oxidation efficient energy-saving method of the present invention processes phenolic waste water technique and can be obviously improved phenol dirt
The degradation effect of dye thing, in radiation of visible light, 50mM H2O2Initial concentration, under the conditions of pH 3.0, Fe- montmorillonite 3.0g/L, 120
In minute, phenol clearance just can reach 100%, and when 180 minutes, TOC clearance can reach 80%.At the same time it can also save
Nearly 66.7% electric power resource, greatly reduces the processing cost of technique.
Brief description
Fig. 1 is phenol removal efficiency contrast curve chart under different technology conditions.
Fig. 2 is the dynamics matched curve figure of heterogeneous Fenton oxidation of phenol under three kinds of different conditions.
Fig. 3 is two benches first-order kinetics constant k under three kinds of different conditions1And k2The schematic diagram of value.
Fig. 4 is initial H2O2The impact schematic diagram of concentration Pyrogentisinic Acid's transformation power constant.
Fig. 5 is the impact schematic diagram of Fe-Mt initial concentration Pyrogentisinic Acid's transformation power constant.
Fig. 6 is the impact schematic diagram of temperature Pyrogentisinic Acid's transformation power constant.
Fig. 7 is TOC and H2O2Time trend curve map.
Fig. 8 is aromatic intermediate concentration changes with time curve map.
Fig. 9 is that carboxylic acids concentration of intermediate products changes over curve map.
Specific embodiment
The following examples are that the present invention is described in further detail.
Embodiment 1
The Photocatalysis of the present invention aoxidize efficient energy-saving method and process comprising the following steps that of phenolic waste water technique：
(1) phenol waste liquid is added in the quartzy light-catalyzed reaction pipe being totally dried, quartzy outer tube layer connects thermostat, adjust
Section pH to 3.0；
(2) add Fe- montmorillonite catalyst in phenol waste liquid, addition is 4.0g/L, magnetic agitation makes catalyst fill
Divide and mix；
(3) open xenon lamp, adjust power to 400W, be then quantitatively adding the H that mass concentration is 30%2O2, make H2O2With benzene
Phenol molar concentration rate is 35；
(4), after reaction starts 40 minutes, turn off xenon lamp, when reaction continues to 120 minutes, phenol degrading rate can reach
100%.
In step (1), adjust the H that pH agents useful for same is 2mol/L2SO4Or NaOH solution.
In step (1), the temperature of thermostat is 25 DEG C.
In step (2), magnetic agitation 1h.
Embodiment 2
The Photocatalysis of the present invention aoxidize efficient energy-saving method and process comprising the following steps that of phenolic waste water technique：
(1) phenol waste liquid is added in the quartzy light-catalyzed reaction pipe being totally dried, quartzy outer tube layer connects thermostat, adjust
Section pH to 3.5；
(2) add Fe- montmorillonite catalyst in phenol waste liquid, addition is 0.6g/L, magnetic agitation makes catalyst fill
Divide and mix；
(3) open xenon lamp, adjust power to 600W, be then quantitatively adding the H that mass concentration is 30%2O2, make H2O2With benzene
Phenol molar concentration rate is 48；
(4), after reaction starts 40 minutes, turn off xenon lamp, when reaction continues to 120 minutes, phenol degrading rate can reach
100%.
In step (1), adjust the H that pH agents useful for same is 2mol/L2SO4Or NaOH solution.
In step (1), the temperature of thermostat is 40 DEG C.
In step (2), magnetic agitation 1h.
Embodiment 3
The Photocatalysis of the present invention aoxidize the concrete steps of the method for efficient energy-saving method process phenolic waste water technique such as
Under：
(1) phenol waste liquid is added in the quartzy light-catalyzed reaction pipe being totally dried, quartzy outer tube layer connects thermostat, adjust
Section pH to 3.3；
(2) add Fe- montmorillonite catalyst in phenol waste liquid, addition is 3.0g/L, magnetic agitation makes catalyst fill
Divide and mix；
(3) open xenon lamp, adjust power to 450W, be then quantitatively adding the H that mass concentration is 30%2O2Make H2O2With benzene
Phenol molar concentration rate is 48；
(4), after reaction starts 40 minutes, turn off xenon lamp, when reaction continues to 120 minutes, phenol degrading rate can reach
100%.
In step (1), adjust the H that pH agents useful for same is 2mol/L2SO4Or NaOH solution.
In step (1), the temperature of thermostat is 30 DEG C.
In step (2), magnetic agitation 1h.
Fig. 1 illustrates sample in only visible ray it is seen that light/H2O2, former state montmorillonite (Mt)/visible ray/H2O2, Fe- illiteracy
De- stone (Fe-Mt)/H2O2, Fe-Mt/ visible ray (initial illumination 40min)/H2O2With Fe-Mt/ visible ray/H2O2Five kinds of different works
The Contrast on effect curve of degraded 100mg/L phenol under the conditions of skill.When only visible light conditions irradiate, phenol clearance is 0.5%
Within；In visible ray/H2O2In compound system, phenol clearance is only 7.5%；As Mt and visible ray/H2O2In the presence of common,
Phenol clearance is promoted to 38.0%.When Fe-Mt is catalyzed H under dark condition2O2When, when 180 minutes, phenol clearance is promoted to
88.0%, but degradable not yet.But work as Fe-Mt/H2O2When system adds radiation of visible light, even if only irradiating 40 minutes, phenol
Clearance remains to reach 100% in 120 minutes.If can light irradiation always in the presence of, phenol conversion rate is not significantly yet
Lifting, is also degradable phenol in 120 minutes.This is because in the reaction first stage it is seen that photoinduction produces
As to biphenol, Fe in catalyst (III) can be reduced to Fe (II), promote OH aromatic intermediate by o-phenol
Quickly generate, thus significantly lifted phenol degradation rate.
Fig. 2 illustrates the dynamics matched curve of heterogeneous Fenton oxidation of phenol under three kinds of different conditions.As seen from the figure,
Fe-Mt/H2O2, Fe-Mt/H2O2/ visible ray (initial 40 minutes) and Fe-Mt/H2O2Second order is all met under the conditions of three kinds of/visible ray
The pseudo- first kernel response dynamics of section.Under dark condition, when carrying out to about 50 minutes, side enters second stage for reaction, but when can
In the case of seeing that optical condition exists, reaction time first stage foreshortens to 40 minutes about.Fig. 3 illustrates two under three kinds of different conditions
The different dynamic constant k of stage first order kinetics1And k2.In the presence of radiation of visible light, first stage kinetic constant k1From
0.125×10-2Increase to 0.744 × 10-2min-1, increase to original 5.95 times；But second stage kinetic constant k2From
1.871×10-2Increase to 5.077 × 10-2min-1, it is only increased to original 2.71 times, increase multiple much smaller than the first stage.
Even if radiation of visible light only exists 40 minutes, second stage kinetics constant k2Also from 1.871 × 10-2Increase to 4.481
×10-2min-1, increase to original 2.39 times, 2.71 increasing when irradiating all the time with visible ray times are approximate.This explanation, anti-
When should carry out to 40 minutes, close xenon lamp, do not significantly affect the transformation efficiency of phenol.
Fig. 3 illustrates initial H2O2The impact of concentration Pyrogentisinic Acid's transformation power constant.Work as H2O2Concentration increases to from 20mM
During 50mM, phenol degrading kinetic constant k1And k2All with H2O2Concentration increases and increases, this is because H2O2Concentration increases
When, OH yield is consequently increased, and therefore increased the conversion rate of phenol.But work as H2O2Concentration increases to 100mM from 50mM
When, phenol degrading kinetic constant k1Increase but k2But reduce, this is because the H of excess2O2OH can be captured, so that phenol
Conversion ratio reduces.
Fig. 4 illustrates the impact of Fe-Mt initial concentration Pyrogentisinic Acid's transformation power constant.When Fe-Mt mass concentration from
When 0.6g/L increases to 3.0g/L, the transformation power constant k of phenol1And k2All be gradually increased, but when catalyst concn from
When 3.0g/L increases to 4.0g/L, the transformation power constant k of phenol1And k2All reduce.Reason is as follows:When Fe-Mt mass
When concentration is relatively low, increase with Fe-Mt mass concentration, be catalyzed H2O2Decompose and produce the increase of OH avtive spot, therefore phenol conversion
Kinetic constant increases therewith.But when Fe-Mt concentration exceedes optium concentration, although avtive spot increases, excessive active sites
Point may capture OH thus forming competition, another aspect H with phenol2O2Decompose too fast, O can be directly generated2And H2O.Except this
Outside, when Fe-Mt mass concentration is excessive, solution can become more muddy, and the utilization blocking visible ray absorbs, so that phenol
Degradation kinetics constant reduces.
Fig. 5 illustrates the impact of temperature Pyrogentisinic Acid's transformation power constant.When temperature is when being increased to 40 DEG C for 25 DEG C, phenol
Degradation kinetics constant k1And k2All it is gradually increased, illustrate that rising high-temperature is conducive to H2O2Decompose, and then oxidation of phenol, even if
When temperature is more than 30 DEG C, H2O2It is readily decomposed to CO2And H2O.Meanwhile, rise high-temperature and can shorten reaction induction time.
The determination data of total organic carbon (TOC), usually by an important indicator as mineralization of organic material rate, H simultaneously2O2
Utilization rate be also usually used to evaluate the treatment effeciency of technique and processing cost.Fig. 6 illustrates Fe-Mt/ visible ray/H2O2System
Under, TOC and H2O2Variation tendency over time.As seen from the figure, 180 minutes when, the clearance of TOC is about 80%, and mineralization rate is relatively
High.But H2O2Consume and only account for the 40% of initial concentration, H is described2O2Utilization rate is higher.
Fig. 7 illustrates Fe-Mt/ visible ray/H2O2Under system, aromatic intermediate concentration changes with time curve.Fragrance
Race's intermediate product toxicity is stronger, and the toxicity of particularly benzoquinones is the decades of times of phenol toxicity, therefore understands these intermediate products
Evolution trend is particularly significant to the treatment effect evaluating waste water.As shown in Figure 7,150 minutes when, aromatic intermediate is complete
Oxidation.
Fig. 8 illustrates Fe-Mt/ visible ray/H2O2Under system, carboxylic acids intermediate product changes over curve.Can by Fig. 8
Know, after phenyl ring open loop, aromatic intermediate is oxidized to short chain small molecular organic acid, and these acids are difficult to be degraded, but malicious
Property be far below phenol and aromatic intermediate.Toxicity be greatly lowered explanation this technique there is huge commercial Application before
Scape.
Although an embodiment of the present invention has been shown and described, for the ordinary skill in the art, permissible
Understand and can carry out multiple changes, modification, replacement to these embodiments without departing from the principles and spirit of the present invention
And modification, the scope of the present invention be defined by the appended.
Claims (6)
1. a kind of Photocatalysis oxidation efficient energy-saving method process phenolic waste water technique it is characterised in that：Comprise the following steps that：
(1) phenol waste liquid is added in the quartzy light-catalyzed reaction pipe being totally dried, quartzy outer tube layer connects thermostat, adjust pH
To 3.0-3.5；
(2) add Fe- montmorillonite catalyst in phenol waste liquid, addition is 0.6-4.0g/L, and magnetic agitation or machinery stir
Mix, so that catalyst is sufficiently mixed uniformly；
(3) open xenon lamp, adjust power to 450-1000W, be then quantitatively adding the H that mass concentration is 30%2O2, make H2O2With benzene
Phenol molar concentration rate is in 35-48；
(4) after reaction starts 40-60 minute, turn off xenon lamp, reaction continues to 120-180 minute, and reaction terminates.
2. Photocatalysis as claimed in claim 1 oxidation efficient energy-saving method process phenolic waste water technique it is characterised in that：
In step (1), adjust pH to 3.3.
3. Photocatalysis as claimed in claim 1 oxidation efficient energy-saving method process phenolic waste water technique it is characterised in that：
In step (1), adjust the H that pH agents useful for same is 2mol/L2SO4Or NaOH solution.
4. Photocatalysis as claimed in claim 1 oxidation efficient energy-saving method process phenolic waste water technique it is characterised in that：
In step (1), the temperature of thermostat is 25-40 DEG C.
5. Photocatalysis as claimed in claim 1 oxidation efficient energy-saving method process phenolic waste water technique it is characterised in that：
In step (2), the addition of Fe- montmorillonite is 3.0g/L.
6. Photocatalysis as claimed in claim 1 oxidation efficient energy-saving method process phenolic waste water technique it is characterised in that：
In step (2), magnetic agitation 1h.
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2006070384A1 (en) * | 2004-12-27 | 2006-07-06 | Council Of Scientific And Industrial Research | Eco-friendly photo-fenton catalyst-immobilized fe(iii) over hy-zeolite |
| CN102407117A (en) * | 2011-11-14 | 2012-04-11 | 江苏星晨环保集团有限公司 | Photocatalysis water-treating material as well as preparation method and application thereof |
| CN103506164A (en) * | 2013-09-25 | 2014-01-15 | 济南大学 | Method for preparing poly(hydroquinone)/graphene/Fe3O4 Fenton catalyst |
| MX2014001241A (en) * | 2014-01-30 | 2015-07-30 | Univ Nac Autónoma De México | Heterogeneous photo fenton solar process using metal slags as photocatalysts for disinfecting and detoxifying water. |
-
2016
- 2016-06-30 CN CN201610511984.9A patent/CN106430515A/en active Pending
Patent Citations (4)
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|---|---|---|---|---|
| WO2006070384A1 (en) * | 2004-12-27 | 2006-07-06 | Council Of Scientific And Industrial Research | Eco-friendly photo-fenton catalyst-immobilized fe(iii) over hy-zeolite |
| CN102407117A (en) * | 2011-11-14 | 2012-04-11 | 江苏星晨环保集团有限公司 | Photocatalysis water-treating material as well as preparation method and application thereof |
| CN103506164A (en) * | 2013-09-25 | 2014-01-15 | 济南大学 | Method for preparing poly(hydroquinone)/graphene/Fe3O4 Fenton catalyst |
| MX2014001241A (en) * | 2014-01-30 | 2015-07-30 | Univ Nac Autónoma De México | Heterogeneous photo fenton solar process using metal slags as photocatalysts for disinfecting and detoxifying water. |
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| Title |
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| 仇雁翎等: "光催化氧化苯酚中间产物的分析与降解途径探讨", 《四川环境》 * |
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Application publication date: 20170222 |