CN105129959B - Using the method for trivalent arsenic in small molecule diketone photooxidation treatment water - Google Patents
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Abstract
The invention discloses the method for trivalent arsenic in a kind of utilization small molecule diketone photooxidation treatment water：By in small molecule diketone water of the addition containing trivalent arsenic, the concentration of rear water small molecular diketone is added for 0.05 1 mM, adjustment pH is 39, then water is placed under ultraviolet source and irradiates 10 60 min, you can the trivalent arsenic in water is oxidized to pentavalent arsenic；The UV/ small molecule diketone systems set up by the present invention, under ultraviolet source irradiation, the trivalent arsenic in water can be promptly oxidized to the pentavalent arsenic for being more easy to be removed by Physical, and its first order reaction kinetic constant is up to 0.15 min‑1, when As (III) concentration is in 0 10 mg/L, oxidation time is substantially within 10 min.The method is easy to operate, and compared to traditional UV/H2O2、UV/TiO2Etc. method, applicable pH value of solution scope is wider, between 39.Can be widely applied to containing As (III) underground water and high concentration containing in the oxidation processes of As (III) in As (III) waste water.
Description
Technical field
The present invention relates to water treatment field, the side of trivalent arsenic in particularly a kind of utilization small molecule diketone photooxidation treatment water
Method.
Background technology
Arsenic (As) is the element being widely present in a kind of underground water, and the water of arsenic content overproof is drunk for a long time, may cause skin
Skin pigment deposition, skin keratin, cutaneum carcinoma, carcinoma of urinary bladder, hypertension, cardiovascular and cerebrovascular diseases, DPN, diabetes etc. are a series of
Health problem, has very big harm to health.By natural Geological Reasons（Geological activity cause containing the molten of arsenic ore
Solution）With the activity of the mankind（The discharge of arsenic-containing waste water in industry）The arsenic pollution for causing has become worldwide environment and asks
Topic.
The maximum allowable content of World Health Organization's regulation Arsenic in Drinking Water is 10 μ g/L, Environmental Protection Agency（US-
EPA）Propose that the maximum level of Arsenic in Drinking Water is not to be exceeded 5 μ g/L, what China used at present《Standards for drinking water quality》
(GB5749-2006) require that the Cmax of Arsenic in Drinking Water have to be lower than 10 μ g/L.Worldwide, arsenic pollution is at least
The water safety problem of more than 5,000 ten thousand people is threaten, and in China, about 15,000,000 populations are exposed to the poisonous harm area of arsenic.
According to《Urban wastewater treatment firm pollutant emission standard》The relevant regulations of GB 18918-2002, arsenic content is not in industrial water drainage
Can be higher than 0.5 mg/L, effluent of municipal sewage plant arsenic content is not above 0.1 mg/L.However, with work, agricultural production
The increase of intensity, the exploitation and smelting of non-ferrous metal, the production containing arsenic agricultural chemicals and uses, and increasing arsenic pollution thing enters water
In, serious harm health realizes that the reparation of arsenic-containing water is extremely urgent.
In common water, there are trivalent arsenic As (III）With two kinds of pentavalent arsenic As (V), wherein As (III) has very big harm
Property, toxicity is more than 60 times of As (V).As (III) is in pH<With non-ionic H when 93AsO3Form is present, and As (V) is then with ionic state
H2AsO4 -And HAsO4 2-Form is present.As (V) can remove (Environ. by methods such as absorption, coagulation/precipitations
Pollut. 2010, 158, 1105−1118).Relative to As (III) the then more difficult removals that As (V), molecular state are present.Therefore,
As (III) is carried out into oxidation transformation for toxicity is smaller, be easier the As (V) of removal, the final removal tool for As in water (III)
It is significant.
Mainly there are air oxidation, chlorine oxidation, iron and manganese oxides oxidation and sweet smell currently for the method for oxidation of As (III)
Reagent oxidation of pausing etc., these methods there is a problem that different：The oxidation rate of oxygen is slower, and chlorine has generation harmful by-products
Risk, and iron and manganese oxides oxidation and Fenton reagent oxidation then need regulation solution to suitable acid-base property, to reacting bar
Part requirement is harsh.
In recent years, with UV/TiO2、UV/H2O2For the photochemical oxidation technology for representing receives extensive concern, however, TiO2
Photochemical catalyst is difficult to be reclaimed, be also easy to produce sludge, and H2O2Property is unstable, and efficiency of light absorption is relatively low, limits it in As (III) oxygen
Application in change.The A of patent CN 103936136 disclose a kind of using As (III) in ultraviolet excitation oxalic acid and then oxidation water
Method, but the method is needed to adjust water pH to 2-6, and 30-120 min are generally the time required to oxidation, speed is slow.
Therefore, a kind of fast and efficiently As (III) oxidation technology is found significant.
The B of patent CN 102491450 disclose a kind of photooxidation treatment dyestuff based on acetylacetone,2,4-pentanedione (2,4- pentanedione)
The method of waste water, its decolorizing efficiency is much better than UV/H202And UV/Ti02Etc. method；The B of patent CN 102642890 disclose utilization
Two kinds of small molecule diketones（2,3- diacetyl or 2,5- acetyl butyryls）The method for making optical active matter oxidation processes waste water from dyestuff；Thus may be used
Know, small molecule diketone, including acetylacetone,2,4-pentanedione (AA), 2,3- diacetyl (BD), 2,5- acetyl butyryls (HD) have photochemical activity, energy
Enough efficient decolorizing dye solutions.
Small molecule diketone (AA, BD, HD), mainly by absorbing photon, forms dyestuff-diketone light and swashs multiple to the decolouring of dyestuff
Compound, carries out electron and energy transfer, so that the chromophore destroyed in dyestuff；And arsenious acid is a kind of inorganic acid, its structure and
Can chemical property be completely different with dyestuff type organic, and the absorption efficiency to light is very low, form light with small molecule diketone and swash multiple
Compound is on the knees of the gods.At present, there are no the method report using As (III) in UV/ small molecule diketone method oxidation processes water.
The content of the invention
Regarding to the issue above, the invention provides the side of trivalent arsenic in a kind of utilization small molecule diketone photooxidation treatment water
Method, fast and efficiently can be oxidized to pentavalent arsenic by the trivalent arsenic in water, what the present invention was realized in：
A kind of method of trivalent arsenic in utilization small molecule diketone photooxidation treatment water, it is comprised the following steps that：By small molecule
In diketone water of the input containing trivalent arsenic, the concentration of rear water small molecular diketone is added for 0.05-1 mM, adjustment pH is 3-9, so
Water is placed under ultraviolet source afterwards irradiates 10-60 min, the trivalent arsenic in water body is to be oxidized to pentavalent arsenic.
Further, in the present invention, the small molecule diketone is in acetylacetone,2,4-pentanedione, 2,3- diacetyl or 2,5- acetyl butyryl
Kind.
Further, in the present invention, the ultraviolet source is 300 W or 500 W mercury lamps.
Further, in the present invention, trivalent arsenic concentration is 1-50 mg/L in the water containing trivalent arsenic.
The beneficial effects of the present invention are the UV/ small molecule diketone systems set up using the present invention, in the photograph of ultraviolet source
Penetrate down, you can rapid that trivalent arsenic in water is oxidized to the pentavalent arsenic for being more easy to removal, so as to further flocculation sediment, its oxygenation efficiency
It is most fast reachable 0.15 min-1, the reaction time, the reaction time was short substantially within 10 min（Existing UV/TiO2、UV/H2O2Deng
Photo chemistry technology, generally requires 50 min or so, and could effectively aoxidize trivalent arsenic between pH is 3-6）, speed is fast, fits
It is wider with pH value of solution scope, can be widely applied to containing As (III) underground water and high concentration containing As in As (III) waste water
(III) in oxidation processes.
Brief description of the drawings
Fig. 1 is As (III) change in concentration schematic diagram in embodiment UV/AA oxidation processes；
Fig. 2 be embodiment UV/AA oxidation processes in difference pH on As (III) concentration influence schematic diagram；
Fig. 3 be embodiment UV/AA oxidation processes in different ions on As (III) concentration influence schematic diagram；
Fig. 4 be embodiment UV/AA oxidation processes in coexisting ion on As (III) concentration influence schematic diagram；
Fig. 5 is embodiment UV/AA and UV/H2O2As (III) concentrations versus' schematic diagram in oxidation processes；
Fig. 6 is As (III) concentrations versus' schematic diagram of the mg/L of embodiment UV/AA oxidation processes 5；
Fig. 7 is As (III) change in concentration schematic diagram of the mg/L of embodiment UV/AA oxidation processes 20；
Fig. 8 is embodiment UV/AA UV/H2O2As (III) change in concentration schematic diagram of the mg/L of oxidation processes 50；
Fig. 9 is As (III) change in concentration schematic diagram in the oxidation of embodiment UV/BD, UV/HD.
Specific embodiment
（1）Embodiment is related to reagent
Acetylacetone,2,4-pentanedione used in embodiment（Hereinafter referred to as AA）, 2,3- diacetyl（Hereinafter referred to as BD）, 2,5- oneself two
Ketone（Hereinafter referred to as HD）, hydrogen peroxide（H2O2）The pure level of analysis is, is provided by Nanjing chemical reagent Co., Ltd., Factory；
Na3AsO3There is provided by Sigma-Aldrich companies, the Na of 1000 mg/L is configured in embodiment3AsO3Storing solution；
（2）Reaction unit
Apparatus for photoreaction by Nanjing Si Dongke electrical equipments company provide, its structure with（Environ Sci Technol
Letters. 2014,1（2）, 167-171）One text discloses identical；Light source used by the device has 300 W, the mercury of two kinds of 500 W
Lamp, mercury lamp is placed in a condensate tank(trap), there is provided light source, and the cylindrical light reaction tube of 25 ml is used for holding reaction solution, should
Tube inner diameter is 3 cm, and light reaction pipe is 5 cm with the distance of mercury lamp, and light reaction pipe revolves around mercury lamp during the course of the reaction
Turn；Unless otherwise specified, light source used in the present embodiment is the mercury lamp of 300 W.
（3）As (III) detection method of content
As (III) content passes through document in solution（Environ Sci Technol,2013,47(16),6064-74）In
The atomic fluorescence spectrometry of description is measured, the citric acid-sodium citrate solution by the use of pH=4 as current-carrying, with hydroboration
Potassium solution（1% KOH、10% KBH4）Used as reducing agent, all of sample is the pure level of analysis, and sample analysis is within 24 h
Complete.
Embodiment 1
（1）UV/AA oxidation effectivenesses
To adding Na in the colorimetric cylinder of 25mL3AsO3Storing solution and AA solution, add As (III) storing solution of 1g/L（Unit
With Na3AsO3Plant As (III) meters, 3.468 g Na3AsO3It is dissolved in 1 L water, concentration as described below is in terms of As (III)）Step by step
As (III) concentration is diluted to for 2 mg/L, AA concentration are 0.05 mM；It is subsequently poured into the reaction tube of 25 mL of apparatus for photoreaction
In, carry out photochemical oxidation and react 10 min, sample one-time detection As (III) concentration every 2 min；Set up without AA simultaneously
（As (III) concentration is 2 mg/L）Check experiment (control)；
Fig. 1 is As (III) change in concentration schematic diagram in reaction solution in 10 min, and in figure, abscissa is the time（min）,
Ordinate is real-time As (III) concentration（C）With initial As (III) concentration（C0）Ratio, as seen from Figure 1, As (III) oxidation speed
Rate is higher, and within the time of ten minutes, substantially all to there occurs that oxidation reaction generates As (V), after reaction terminates, As (III) is dense
It is 0.01 mg/L to spend, and is free of the control group of AA, and As (III) concentration does not almost change.
Wherein, pH changes are as shown in table 1 in the min of photooxidation reaction 10 in reaction group：
Table 1:PH changes in reaction solution in the min of photooxidation reaction 10
| Light application time (min) | 0 | 2 | 4 | 6 | 8 | 10 |
| pH | 5.69 | 4.80 | 4.55 | 4.44 | 4.36 | 4.32 |
From table 1, during photooxidation reaction, reacting liquid pH value is gradually reduced, because AA is decomposed in reaction
The acid of small molecule is generated, causes pH constantly to decline.
（2）PH influences
To adding Na in 5 25 mL colorimetric cylinders3AsO3Storing solution and AA solution, with As (III) storing solution of 1 g/L step by step
As (III) concentration is diluted to for 2 mg/L, AA concentration are 0.05 mM；Then with the HClO of 0.1 M4Solution and 0.1 mM's
NaOH solution carries out acid-base accommodation respectively, and regulation solution end pH value is followed successively by 3,6,7,9,10, respectively numbering 1-5；By 5 groups of solution
Pour into respectively in the reaction tube of apparatus for photoreaction, carry out photochemical oxidation and react 10 min, every 2 min sampling one-time detections As
(III) concentration；
Fig. 2 is As (III) change in concentration schematic diagram in difference pH solution in 10 min, as can be known from Fig. 2, when pH value of solution=
When 10, the oxidation to As (III) causes obvious inhibitory action, because the pKa=9 of AA, when the ph is increased, can influence it
Property and effect performance, and pH value of solution in the range of 3-9 when, AA shows preferable oxidation, even if being in initial pH
When alkaline, AA can also play effect well, because AA can generate small molecule acid during the course of the reaction, and then reduce solution
pH；Result, it is believed that the pH scopes that UV/AA oxidations trivalent arsenic As (III) is applicable are between 3-9.
（3）Coexisting ion influences
Single ionic impact analysis：SO present in water is detected respectively4 2-、HCO3 -、F-、NO3 -、PO4 3-As is aoxidized to UV/AA
(III) influence of speed, using NaClO4Regulation ionic strength is consistent, under same ion strength condition, relatively more several ions
Influence；The SO being related in the present embodiment4 2-Plasma concentration is foundation《Arsenic from underwater under the influence of Hetao Plain agricultural irrigation
Behaviors of migration and enrichment research China University of Geosciences, 2010》One text determines.
Specific experiment step：As (III) storing solution stepwise dilutions with 1 g/L are dense as 2 mg/L, AA to As (III) concentration
It is 0.05 mM to spend；Then it is poured into respectively in 7 colorimetric cylinders, every group of 25 ml, respectively numbering 1-7；Then take 1 g/L's respectively
Na2SO4、NaHCO3、NaF、NaNO3、Na3PO4In addition 1-5 group colorimetric cylinders, wherein SO in the 1st group4 2-Final concentration of 400 mg/
L, HCO in the 2nd group3 -Final concentration of 600 mg/L, F in the 3rd group-Final concentration of 1 mg/L, NO in the 4th group3Final concentration of 0.5
Mg/L, PO in the 5th group4 3-Final concentration of 0.21 mg/L, calculates ionic strength, using NaClO4By the ion of 1-5 group colorimetric cylinders
Intensity adjustment is consistent（It is 12.5 mM）；NaClO is added in 6th group4, its ionic strength is adjusted for 12.5 mM, the 7th group is not then
Do any treatment；Then 7 groups of each 25 ml of reactant are carried out into photochemical oxidation and reacts 10 min, once examined every 2 min samplings
Survey As (III) concentration；
Fig. 3 is that different ions influence schematic diagram to As in reaction solution (III) change in concentration in 10 min, can be with from figure
Find out, HCO3 -、PO4 3-Presence can suppress the oxidation of As (III), this is mainly and is acted on by pH, the addition of both ions
All so that pH value of solution is under stronger alkalescence condition, AA is set to there occurs dissociation, and then have impact on the oxidation of As (III).
Coexisting ion concentration impact analysis：To adding Na in colorimetric cylinder3AsO3Storing solution and AA solution, with the As of 1 g/L
(III) storing solution stepwise dilution to As (III) concentration is 5 mg/L, and AA concentration is 0.1 mM, and solution then is separately added into 3
In 25 mL colorimetric cylinders, numbering 1-3 respectively：
To the SO that final concentration of 400 mg/L is added in the 1st group of colorimetric cylinder4 2-, 600 mg/L HCO3 -, 1 mg/L F-、
The NO of 0.5 mg/L3 -With the PO of 0.21 mg/L4 3-, adjustment pH is 10.86；
To the SO that final concentration of 400 mg/L is added in the 2nd group of colorimetric cylinder4 2-, 600 mg/L HCO3 -, 1 mg/L F-、
The NO of 0.5 mg/L3 -With the PO of 0.21 mg/L4 3-, adjustment pH is 6；
3rd group is left intact, used as control（control）；
3 groups of each 25 ml of solution are carried out into photochemical oxidation and reacts 10 min, one-time detection As (III) is sampled every 2 min
Concentration；As (III) concentration results are as shown in figure 4, it can be seen that when there is coexisting ion, UV/AA methods are aoxidized
The speed of arsenic still quickly, but the 2nd group（During initial pH=6）Within 4min, you can with by the As of 5 mg/L (III) whole oxygen
Change, as initial pH=10.86（1st group）, oxidation rate reduction, this is mainly due to initial soln meta-alkalescence, but 10 min
Within, it is also possible to by 90% oxidation of initial arsenic, this is primarily due to NO3 -Nitrite anions free radical can be produced under the conditions of ultraviolet,
Play a part of catalysis oxidation（Environ Sci Technol, 2014, 48（7）,4030-4037）, why just this be also
During beginning pH=6, the As (III) of initial 5 mg/L can all be aoxidized in 4 min.
（4）UV/AA and UV/H2O2Contrast on effect
UV/AA groups：To adding Na in 25mL colorimetric cylinders3AsO3Storing solution and AA solution, stepwise dilution to As (III) concentration
It is 1 mg/L, AA concentration is 0.05 mM；
UV/H2O2Group：To adding Na in 25 mL colorimetric cylinders3AsO3Storing solution and H2O2, stepwise dilution to As (III) concentration
It is 1 mg/L, H2O2Concentration is 0.05 mM；
Two groups of solution are poured into the reaction tube of apparatus for photoreaction respectively, photochemical oxidation is carried out and is reacted 10 min, every 2
Min sampling detection As (III) concentration, testing result is as shown in figure 5, as seen from Figure 5, UV/AA methods substantially can within 4 min
By As（III）All oxidation, has monitored less than As after 4 min（III）, and UV/H2O2Method after 10 min, As
(III) concentration of concentration is 0.4 mg/L, and only oxidized 60% As (III), speed is much smaller than UV/AA methods.
Embodiment 2
Using Na3AsO3Storing solution and AA solution, the stepwise dilution in the colorimetric cylinder of 25 mL, As (III) concentration after dilution
It is 5 mg/L, AA concentration is 0.1 mM, then pouring into light reaction pipe solution carries out photochemical oxidation 20 min of reaction, every
10 min sampling detection As (III) concentration, while the Na not contain AA3AsO3Solution（As (III) concentration is 5 mg/L）As
Control（control）.
According to final result, as shown in fig. 6, as seen from Figure 6, compared with control group, after adding AA, As (III) oxidation speed
Rate is very fast, and substantially in 10 min, As (III) all there occurs oxidation reaction, generation As (V).
Embodiment 3
Using Na3AsO3Storing solution and AA solution, the stepwise dilution in the colorimetric cylinder of 25mL, As (III) concentration after dilution
It is 20 mg/L, AA concentration is 0.5 mM, then pouring into light reaction pipe solution carries out photochemical oxidation 60 min of reaction, often
Every 10 min sampling detection As (III) concentration, while the Na not contain AA3AsO3Solution（As (III) concentration is 20 mg/L）
As control（control）.
Testing result is as shown in fig. 7, compared with control group, after adding AA, As (III) is in the mg/L of 60 min internal oxiditions 20
As (III) can be fully oxidized.
Embodiment 4
（1）：Using Na3AsO3Storing solution and AA solution, the stepwise dilution in the colorimetric cylinder of 25 mL, As (III) after dilution
Concentration is 50 mg/L, and AA concentration is 1 mM, and then pouring into light reaction pipe solution carries out photochemical oxidation 60 min of reaction,
Every 5 min sampling detection As (III) concentration.
（2）：Using Na3AsO3Storing solution and H2O2Solution, the stepwise dilution in the colorimetric cylinder of 25 mL, As after dilution
(III) concentration is 50 mg/L, H2O2Concentration is 1 mM, and then pouring into light reaction pipe solution carries out photochemical oxidation reaction 60
Min, every 5 min sampling detection As (III) concentration.
While not contain AA, H2O2Na3AsO3Solution（As (III) concentration is 50 mg/L）As control
（control）.
Testing result adds the AA of 1mM as shown in figure 8, compared with control group in solution, under conditions of additional light source,
The As (III) of 70% can aoxidized in 60min, and the addition H under its oxidation efficiency equal conditions2O2Solution.
Embodiment 5
UV/BD methods：Using Na3AsO3Storing solution and BD solution, the stepwise dilution in the colorimetric cylinder of 25 mL, As after dilution
(III) concentration is 10 mg/L, and BD concentration is 0.2 mM, and then pouring into solution carries out photochemical oxidation reaction in light reaction pipe
20 min, every 4 min sampling detection As (III) concentration, while the Na not contain AA3AsO3Solution（As (III) concentration is
10 mg/L）As control；
UV/HD methods：Outside divided by HD solution substitution BD solution, remaining test procedure is consistent with UV/BD methods；
Testing result is as shown in figure 9, after to BD, HD is added in arsenic containing solution, As (III) oxidation rate is very fast, 20
In min, As (III) all there occurs oxidation reaction.
Embodiment 6
（1）：Using Na3AsO3Storing solution and AA solution, the stepwise dilution in the colorimetric cylinder of 25 mL, As (III) after dilution
Concentration is 2 mg/L, and AA concentration is 0.05 mM, then solution is poured into light reaction pipe under the conditions of 300W lamp sources carry out it is photochemical
The min of oxidation reaction 10 is learned, every 2 min sampling detections As（III）Concentration.
（2）：Using Na3AsO3Storing solution and H2O2Solution, the stepwise dilution in the colorimetric cylinder of 25 mL, As after dilution
(III) concentration is 2 mg/L, H2O2Concentration is 0.01 mM, then pours into light reaction pipe to enter under the conditions of 500W lamp sources by solution
Row photochemical oxidation reacts 60 min, every 5 min sampling detections As（III）Concentration.
According to experimental result, under the light source of 300 W mercury lamps, the As (III) for having 89% within 10 min is oxidized.Improve
When the power of additional light source is to 500 W, As (III) can be fully oxidized in 10 min.
Embodiment described above only expresses embodiments of the present invention, and its description is more specific and detailed, but can not
Therefore it is interpreted as the limitation to the scope of the claims of the present invention.It should be pointed out that to those skilled in the art, not taking off
On the premise of present inventive concept, some improvement can also be made, these improvement belong to protection scope of the present invention.
Claims (3)
1. a kind of method that utilization small molecule diketone photooxidation processes trivalent arsenic in water, it is characterised in that comprise the following steps that：Will
In small molecule diketone water of the input containing trivalent arsenic, the concentration of rear water small molecular diketone is added for 0.05-1 mM, adjustment pH is
, then be placed in water under ultraviolet source and irradiate 10-60 min by 3-9, and the trivalent arsenic in water body is to be oxidized to pentavalent arsenic；
The small molecule diketone is the one kind in acetylacetone,2,4-pentanedione, 2,3- diacetyl or 2,5- acetyl butyryl.
2. according to claim 1 using the method for trivalent arsenic in small molecule diketone photooxidation treatment water, it is characterised in that institute
Ultraviolet source is stated for 300 W or 500 W mercury lamps.
3. the method that utilization small molecule diketone photooxidation according to claim 1 or claim 2 processes trivalent arsenic in water, its feature exists
In trivalent arsenic concentration is 1-50 mg/L in the water containing trivalent arsenic.
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