CN104724789A - Application of coacervate system in selective photocatalytic degradation of environmental pollutants - Google Patents

Application of coacervate system in selective photocatalytic degradation of environmental pollutants Download PDF

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CN104724789A
CN104724789A CN201510147918.3A CN201510147918A CN104724789A CN 104724789 A CN104724789 A CN 104724789A CN 201510147918 A CN201510147918 A CN 201510147918A CN 104724789 A CN104724789 A CN 104724789A
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coacervate
photocatalytic degradation
phase
solution
rhb
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CN104724789B (en
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吕康乐
伍晓锋
李玫
李覃
邓克俭
朱君江
黄涛
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South Central Minzu University
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South Central University for Nationalities
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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
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
    • G01N21/17—Systems in which incident light is modified in accordance with the properties of the material investigated
    • G01N21/25—Colour; Spectral properties, i.e. comparison of effect of material on the light at two or more different wavelengths or wavelength bands
    • G01N21/31—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry
    • 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
    • C02F2101/10—Inorganic compounds
    • C—CHEMISTRY; METALLURGY
    • C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F2301/00—General aspects of water treatment
    • C—CHEMISTRY; METALLURGY
    • C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F2303/00—Specific treatment goals

Abstract

The invention belongs to technical field of pollution control, and particularly relates to a selective photocatalytic degradation behavior of a model pollutant in a coacervate (PDDA/ATP) system. The method is implemented by using a characteristic that a photocatalyst titanium dioxide easily enters a coacervate phase, but because the distribution coefficients of different pollutants between the coacervate phase and a water phase are different, pollutants easily entering the coacervate phase are in contact with the photocatalyst titanium dioxide and then are degraded preferentially, and pollutants not easily entering the coacervate phase are difficult to decompose because of being difficult to contact with the photocatalyst in the coacervate, so that a situation that some pollutants are preferentially decomposed (subjected to selective photocatalytic degradation) in the coacervate system is caused finally. Coacervate system based selective photocatalytic degradation has a broad application prospect in the field of environmental pollution control.

Description

The application of coacervate system in the degraded of environmental pollutant selective photocatalysis
Technical field
The present invention relates to environmental pollution control technique field, be specifically related to the application of coacervate system in the degraded of environmental pollutant selective photocatalysis.
Background technology
Along with socioeconomic development, environmental pollution is increasingly serious.Semi-conductor optically catalytic TiO 2, because the oxygen that can utilize in sun power and air, makes the toxic organic pollutant in water that thoroughly degraded occur, and obtains extensive concern.But titanium dioxide, to the photocatalysis Decomposition of environmental toxic organic pollutant, lacks selectivity (J.Am.Chem.Soc., 2010,132,11914-11916 and Chem.Commun., 2007,1163 – 1165).
In order to realize the selectivity preferential degradation of some toxic pollutant in environment, scientists have employed various strategy, carries out molecular imprinting etc. as (1) titanium dioxide carries out finishing with (2) at titanium dioxide surface.As the discovery such as Liu Shengwei and Yu Jiaguo of Wuhan University of Technology, the surperficial fluorine of high-energy surface titanium dioxide is modified with the photocatalysis Decomposition being beneficial to MO in methyl orange (MO) and methylene blue (MB) mixing colouring agent.But once carry out alkali cleaning to catalyzer to remove fluorine, then be conducive to preferential decomposition (the Tunable Photocatalytic Selectivityof Hollow TiO2 Microspheres Composed of Anatase Polyhedra with Exposed{001}Facets.J.Am.Chem.Soc. of MB, 2010,132,11914-11916).But the introducing of fluorion, can cause water pollution.Central China University of Science and Technology Zhu Lihua and Tang and clear teach problem group, at the polymer macromolecule by there being pollutent template at the coated one deck trace of titanium dioxide surface, successfully realize highly selective photocatalysis Decomposition (the Synthesis of molec μ Lar imprinted polymer coated photocatalystswith high selectivity.Chem.Commun. of phenols target contaminant molecule, 2007,1163 – 1165).But there is the problems such as catalyst preparation process is loaded down with trivial details, program is complicated in these molecular imprintings.
Summary of the invention
Cohesion (coacervation) refers to Ionomer polymer, pedesis is caused to remove with the ion generation electrical counteract with opposite charges in solution, the colloidal particle of formation are flocked together near contact, finally become dense colloidal sol (sol), the phenomenon separated from water-soluble as the small droplets under microscope or macroscopic " phase "." phase " that be separated or system are called coacervate (coacervate), and water layer is called balance liquid (equilibrium).Dispersion and cohesion are opposition, and the impact of electric repulsion, dispersion agent and solvated layer facilitates system stably dispersing, and magnetism and the various motion collision of molecule facilitate cohesion again.The principal element of impact cohesion has electrolytical effect, the interaction of colloidal dispersion, the concentration of colloid and temperature etc.Of many uses in biological and chemical of coacervate.Recently, Mann etc. have carried out systematic study to the coacervate system that the biomolecules such as peptide-nucleosides (peptide-nucleotide) build, and find that nanoparticle is (as Au, Fe 3o 4and Co 2o 3deng) and biological enzyme etc., high power can be concentrated to coacervate liquid (Peptide – nucleotide microdroplets as a step towards a membrane-freeprotocell model.Nature Chem., 2011,3,720-724).But, coacervate is used as light-catalyzed reaction system, also there is no bibliographical information.
For the deficiency existed in existing optically catalytic TiO 2 technology, the object of the present invention is to provide a kind of system and way realizing the degraded of organic pollutant selective photocatalysis.We find, can utilize the difference of model pollutant partition ratio in PDDA/ATP coacervate phase, realize selective photocatalysis degraded.
Diallyl dimethyl ammoniumchloride, is called for short PDDA; Triphosaden, is called for short ATP.
The molecular structural formula of PDDA and ATP is shown in Fig. 1.
Realizing the technical scheme that the object of the invention takes is:
First, a kind of foundation realizing the system of organic pollutant selective photocatalysis, its step is as follows:
(1) in glass reaction bottle (photo catalysis reactor), be weighed into titanium dioxide optical catalyst, then add PDDA solution, the ultrasonic catalyzer that makes fully disperses.
(2) under magnetic stirring, add two kinds of different dyestuffs (model pollutant) and ATP solution successively, make abundant mixing.
(3) open light source, under Keep agitation, carry out the photocatalytic degradation of model pollutant.
(4) sample in illumination different time points, sample sodium chloride solution decomposed P DDA/ATP coacervate phase, centrifugation titanium dioxide optical catalyst, gets supernatant liquor and carries out Visible imaging simulation test, and analytical model pollutent is in the degraded situation of coacervate system.
This research have selected four kinds of model pollutant molecule methylene blues (MB), rhodamine B (RhB), reactive brilliant red X-3B (X3B) and tropeolin-D (MO).
The partition ratio measuring method of titanium dioxide involved by application method of the present invention in coacervate phase:
(1) have in the glass reaction bottle of 4mg titanium dioxide optical catalyst at title, move into the PDDA solution that 6ml concentration is 50mM, ultrasonic 5 minutes, photocatalyst is fully disperseed in the solution.Under magnetic stirring, the ATP solution of 2ml 50mM is added.Conveniently observe, get 1 milliliter of mixing solutions in the plastic centrifuge tube of 2ml, leave standstill 10 hours, find that the titanium dioxide of white has all been enriched in the coacervate phase (Fig. 2) of lower floor.
(2) in order to determine the partition ratio of titanium dioxide between coacervate and aqueous phase, with ultraviolet visible spectrometry, the titanium dioxide concentration be distributed in this two-phase is analyzed.After upper strata aqueous phase solution dilutes 1000 times, measure the light absorption value (A1) of solution at 400nm place, after lower floor's coacervate phase gets 10 μ L, after adding the NaCl solution decomposition coacervate phase of 1mL 5M, dilute 1000 times and measure the light absorption values (A2) of solution at 400nm place equally.
(3) partition ratio method of calculation D=A2/A1.
The partition ratio measuring method of dyestuff involved by application method of the present invention in coacervate phase:
(1) in the plastic centrifuge tube of 2mL, PDDA solution and 10 μ L dye solution (5gL that 600 μ L concentration are 50mM is moved into -1), shake up; Adding 200 μ L concentration is that the ATP solution of 50mM shakes up and leaves standstill 10 hours afterwards, finds upper strata aqueous phase and lower floor's coacervate phase layering interfaces obviously (Fig. 2).
(2) in order to determine the partition ratio of each dyestuff between coacervate and aqueous phase, with ultraviolet visible spectrometry, the dye strength be distributed in this two-phase is analyzed.Upper strata aqueous phase can measure by direct ultraviolet, after lower floor's coacervate phase gets 10 μ L, after adding the NaCl solution decomposition coacervate phase of 1mL 5M, carries out ultraviolet spectroscopy.
(3) according to the light absorption value of dyestuff in maximum absorption wave strong point, calculate the ratio of the concentration of dyestuff in coacervate and aqueous phase, obtain the partition ratio D (table 1) of dyestuff in this coacervate.
The partition ratio of table 1. four kinds of dyestuffs in coacervate
Dyestuff MB RhB X3B MO
Characteristic absorption wavelength (nm) 668 554 530 470
Partition ratio D (coacervate/water) 28 0.55 234 35
Dyestuff involved by application method of the present invention is degraded optionally quantivative approach in coacervate phase:
(1) have in 15 milliliters of glass reaction bottles of 4mg titanium dioxide optical catalyst at title, move into the PDDA solution that 6ml concentration is 50mM, ultrasonic 5 minutes, photocatalyst is fully disperseed in the solution.
(2) under the stirring action of magnetic stir bar, add 2 kinds of mixing colouring agents, make abundant mixing, finally add the ATP solution of 2ml 50mM.
(3) open LED light source (predominant wavelength 365nm), under Keep agitation, carry out photocatalytic degradation reaction (Fig. 3 is shown in by experimental installation) of model pollutant.
(4) sample 800 μ L in 2mL plastic centrifuge tube in illumination different time points, add the sodium chloride solution decomposition coacervate that 10 μ L concentration are 5M, shake up, centrifugation catalyzer, get supernatant liquor and carry out Visible imaging simulation analysis.According to the light absorption value at maximum absorption cutting edge of a knife or a sword place, the dye strength in solution is carried out quantitatively.
(5) dye degrades reaction is pseudo first order reaction, and its kinetics equation can be expressed as: ln (C/C 0)=-Kt, K are observed rate constant, and t is the light-catalyzed reaction time, C 0with the concentration that C is in the initial and reaction process of dyestuff in reaction system (coacervate system) respectively.
(6) with the ratio of the observed rate constant of two kinds of dye degrades, reflect that the selectivity (β=K1/K2) of photocatalytic degradation occurs in coacervate system for they.
Compared with prior art, advantage of the present invention and beneficial effect as follows:
Application art of the present invention is simple, easy handling, for the selective photocatalysis of environmental pollutant is degraded, provides novel method, has more wide application prospect.
Accompanying drawing explanation
Fig. 1 is the molecular structural formula of PDDA and ATP;
Fig. 2 is different dyes, photocatalyst TiO 2distribution condition digital photograph in coacervate;
Fig. 3 is light-catalyzed reaction experimental installation;
Fig. 4 is that degraded spectrogram (A) and corresponding first order kinetics curve (B) occur RhB-MB mixing colouring agent in coacervate system;
Fig. 5 is that degraded spectrogram (A) and corresponding first order kinetics curve (B) occur RhB-MB mixing colouring agent in aqueous;
Fig. 6 is the first order kinetics matched curve of X3B-MB mixing colouring agent photocatalytic degradation in coacervate system;
Fig. 7 is the first order kinetics matched curve of X3B-MB mixing colouring agent photocatalytic degradation in aqueous;
Fig. 8 is the first order kinetics matched curve of MO-RhB mixing colouring agent photocatalytic degradation in coacervate system;
Fig. 9 is the first order kinetics matched curve of MO-RhB mixing colouring agent photocatalytic degradation in aqueous.
Embodiment
Applicant will be described in detail application of the present invention in conjunction with specific embodiments below, further understand, but following examples be interpreted as limiting the scope of the invention never in any form so that those skilled in the art has the present invention.
Main agents: diallyl dimethyl ammoniumchloride (PDDA, molecular-weight average 100 – 200kDa) and Triphosaden (ATP) purchased from sigma-aldrich company, dyestuff (RhB, MB, MO and X3B) and photocatalyst TiO 2(Degussa P25) is purchased from traditional Chinese medicines group.
Embodiment 1:
Decompose to investigate the selective photocatalysis of environmental pollutant in coacervate phase, experiment employing two kinds of dyestuff RhB and MB are that model pollutant carries out mixed degradation experiment.Have in 15 milliliters of glass reaction bottles of 4mg optically catalytic TiO 2 at title, move into the PDDA solution that 6ml concentration is 50mM, ultrasonic 5 minutes, catalyzer is fully disperseed in the solution.Under magnetic force stirs, add 100 μ L RhB solution (5gL -1) and 100 μ L MB solution (5gL -1), make abundant mixing, finally add the ATP solution that 2mL concentration is 50mM.Open light source, under Keep agitation, carry out the photocatalytic degradation of model pollutant.Sample 800 μ L in the plastic centrifuge tube of 2mL in illumination different time points, the sodium chloride solution adding 10 μ L 5M decomposes coacervate, shakes up and obtains homogeneous phase solution, centrifugation catalyzer, get supernatant liquor and carry out Visible imaging simulation analysis.
Fig. 4 A shows the spectrum change situation of solution in Photocatalytic Degradation Process.Spectrum peak 554nm is the charateristic avsorption band of dyestuff RhB, and 668nm is the charateristic avsorption band of dyestuff MB.From the changing conditions at spectrum peak, the light absorption value of 554nm is very little with light application time change, and the absorption value at 668nm place declines very fast, illustrates that MB there occurs preferential degradation.
The degradation kinetics curve of dyestuff RhB and MB in coacervate, can obtain good matching (Fig. 4 B) with first order kinetics curve.By first order kinetics matching, obtaining the degradation rate constant of RhB and MB in coacervate is 4.46 × 10 respectively -4min -1and 0.019min -1.Therefore, MB is to the relative selectivity β of RhB mB/RhB=0.019/ (4.46 × 10 -4)=42.6>>1, demonstrates the preferential photocatalytic degradation of MB at coacervate phase.
Embodiment 2:
In order to prove the preferential photocatalytic degradation of MB at coacervate phase, being caused by the existence of coacervate, We conducted their photocatalytic degradations in aqueous and contrasting.Have in 15 milliliters of glass reaction bottles of 4mg optically catalytic TiO 2 at title, move into 8 ml distilled waters, within ultrasonic 5 minutes, make abundant dispersion.Under magnetic force stirs, add 100 μ L RhB solution (5gL -1) and 100 μ L MB solution (5gL -1), make abundant mixing.Open light source, carry out the photocatalytic degradation of model pollutant.Sample 800 μ L in the plastic centrifuge tube of 2mL in illumination different time points, centrifugation catalyzer, get supernatant liquor and carry out Visible imaging simulation analysis.Mixing colouring agent degraded spectrogram is in aqueous shown in Fig. 5 A.Can find out, there is remarkable decline in the charateristic avsorption band of RhB and MB in time, shows that these two kinds of dyestuffs all there occurs obvious degraded in aqueous.Their degraded first order kinetics matched curve, is shown in Fig. 5 B.The degradation rate constant of RhB and MB in aqueous phase is respectively 0.28min -1and 0.30min -1, the selectivity β that in the aqueous solution, MB degrades to RhB mB/RhB=0.30/0.28=1.07.
Comparative example 1 and embodiment 2 can be found out, relative to traditional water solution system, the degraded selectivity of MB in coacervate system is greatly improved.Selectivity is increased to 42.6 in coacervate system from 1.07 aqueous phase, adds 39.8 times.
Embodiment 3 (comparative example):
In order to the selective photocatalysis degraded of research model pollutent in coacervate phase, mixing colouring agent MB and X3B is selected to be model pollutant.Except replacing RhB with X3B, other conditions are with embodiment 1.Mixing colouring agent, in the first order kinetics matched curve of coacervate solution generation photocatalytic degradation, is shown in Fig. 6.The degradation rate constant of X3B and MB in coacervate phase is respectively 0.015min -1and 0.010min -1, X3B is to the selectivity β of MB photocatalytic degradation in coacervate system x3B/MB=0.015/0.010=1.5, illustrate that X3B and MB degrades in coacervate system, selectivity is not obvious, and this may be because these two kinds of dyestuffs all easily enter coacervate relevant (table 1).
Embodiment 4 (comparative example):
In order to prove that MB-X3B mixing colouring agent lacks selectivity at the photocatalytic degradation of coacervate, because these two kinds of dyestuffs are all easy to enter caused by coacervate, We conducted this mixing colouring agent photocatalytic degradation in aqueous and contrasting.Except changing into except X3B dyestuff by RhB dyestuff, other operation is identical with embodiment 2.Mixing colouring agent, in the first order kinetics matched curve of aqueous solution generation photocatalytic degradation, is shown in Fig. 7.The degradation rate constant of X3B and MB in aqueous phase is respectively 0.093min -1and 0.13min -1, the selectivity β that in the aqueous solution, X3B degrades to MB x3B/MB=0.093/0.13=0.72.This result illustrates, similar with coacervate system, in the aqueous solution, the degraded of mixing colouring agent MB-X3B lacks selectivity equally.
Comparative example 3 and embodiment 4 can be found out, when two kinds of dyestuffs are all easy to enter coacervate phase, the existence of coacervate in reaction system, significantly can not increase the selectivity of certain dye degrades.
Embodiment 5:
In order to the selective photocatalysis degraded of research model pollutent in coacervate phase, mixing colouring agent RhB and MO is selected to be model pollutant.Except replacing MB with MO, other conditions are with embodiment 1.Mixing colouring agent, in the first order kinetics matched curve of coacervate solution generation photocatalytic degradation, is shown in Fig. 8.The degradation rate constant of RhB and MO in coacervate phase is respectively 5.15 × 10 -4min -1and 0.020min -1, MO is to the selectivity β of RhB photocatalytic degradation in coacervate system mO/RhB=0.020/ (5.15 × 10 -4)=38.8>>1, demonstrates the preferential photocatalytic degradation of MO in coacervate system.
Embodiment 6:
In order to prove in MO-RhB mixing colouring agent, the selective photocatalysis degraded of MO, caused by coacervate, We conducted this mixing colouring agent photocatalytic degradation in aqueous and contrasts.Except changing into except MB dyestuff by MO dyestuff, other operation is identical with embodiment 2.Mixing colouring agent, in the first order kinetics matched curve of aqueous solution generation photocatalytic degradation, is shown in Fig. 9.The degradation rate constant of MO and RhB in aqueous phase is respectively 0.137min -1and 0.162min -1, the selectivity β that in the aqueous solution, MO degrades to RhB mO/RhB=0.137/0.162=0.85.This result illustrates: different from coacervate phase, and in the aqueous solution, the degraded of mixing colouring agent MO-RhB lacks selectivity.
Comparative example 5 and embodiment 6 can be found out, relative to traditional water solution system, the degraded selectivity of MO in coacervate system is greatly improved.Selectivity is increased to 38.8 in coacervate system from 0.85 aqueous phase, adds 45.6 times.
Based on above embodiment, the invention provides a kind of coacervate system and mixing colouring agent is being carried out to the application in selective photocatalysis degraded, described coacervate system is the PDDA/ATP coacervate system that diallyl dimethyl ammoniumchloride solution and Triphosaden solution are mixed to form, and described photocatalytic degradation used catalyst is titanium dioxide;
Described mixing colouring agent is RhB and MB mixture, or described mixing colouring agent is RhB and MO mixture.

Claims (1)

1. coacervate system is carrying out the application in selective photocatalysis degraded to mixing colouring agent, described coacervate system is the PDDA/ATP coacervate system that diallyl dimethyl ammoniumchloride solution and Triphosaden solution are mixed to form, and described photocatalytic degradation used catalyst is titanium dioxide;
Described mixing colouring agent is RhB and MB mixture, or described mixing colouring agent is RhB and MO mixture.
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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN108221091A (en) * 2018-03-22 2018-06-29 江南大学 A kind of compound carbon fiber with molecular recognition effect

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Publication number Priority date Publication date Assignee Title
CN101733133A (en) * 2009-12-10 2010-06-16 浙江大学 Titanium dioxide photocatalyst with coating layer coated on surface and preparation method thereof
CN102172540A (en) * 2011-01-27 2011-09-07 东北师范大学 Polyoxometallate-based industrial dye decoloring photocatalyst and preparation method thereof
CN102962089A (en) * 2012-11-26 2013-03-13 杭州电子科技大学 Method for preparing nitrogen-doped rutile TiO2 selective photocatalyst

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101733133A (en) * 2009-12-10 2010-06-16 浙江大学 Titanium dioxide photocatalyst with coating layer coated on surface and preparation method thereof
CN102172540A (en) * 2011-01-27 2011-09-07 东北师范大学 Polyoxometallate-based industrial dye decoloring photocatalyst and preparation method thereof
CN102962089A (en) * 2012-11-26 2013-03-13 杭州电子科技大学 Method for preparing nitrogen-doped rutile TiO2 selective photocatalyst

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN108221091A (en) * 2018-03-22 2018-06-29 江南大学 A kind of compound carbon fiber with molecular recognition effect

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