CN104437643A - Solid super-molecular photocatalyst integrating Fenton effect and photocatalysis as well as preparation method and application thereof - Google Patents
Solid super-molecular photocatalyst integrating Fenton effect and photocatalysis as well as preparation method and application thereof Download PDFInfo
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Abstract
The invention discloses a solid super-molecular photocatalyst integrating Fenton effect and photocatalysis as well as preparation methods and application thereof. A first type of the photocatalyst is a compound of an iron complex and g-C3N4, and is prepared by the following steps: dissolving a water-soluble iron salt into ultrapure water to obtain an iron salt solution; adjusting the pH value of the iron salt solution to be not more than 1, and adding a ligand precursor into the iron salt solution to obtain an iron complex; and adding g-C3N4 into the iron complex, stirring, and drying to obtain the solid super-molecular photocatalyst. A second type of the photocatalyst is a compound of ferrocene and g-C3N4 and is prepared by the following steps: dissolving ferrocene into hot water, adding g-C3N4 powder when the mixture is hot, stirring fully, and drying to obtain a ferrocene/g-C3N4 compound photocatalyst. A third type of the photocatalyst is a compound of chlorhematin and g-C3N4, and the preparation method is similar to that of ferrocene/g-C3N4. The solid super-molecular photocatalyst has the following beneficial effects: the iron source is stable, the photocatalysis condition is not influenced by pH, and the solid super-molecular photocatalyst responds to visible light and is high in reaction speed.
Description
Technical field
The present invention relates to a kind of integrated Fenton effect and light-catalysed solid-state supermolecule photochemical catalyst and its preparation method and application, belong to photocatalysis technology field.
Background technology
Along with the development of the mankind, the energy, environment progressively become the two principal themes that the world today faces.The consumption that fossil energy is excessive, both adds the worry of people to future source of energy, has the pressure adding and pollute in a large number environment.Therefore new forms of energy how can be utilized to solve environmental problem and to become a following mankind great existence problem urgently to be resolved hurrily in road for development.Have existed since ancient times to solar energy for people, utilize today clean, without harm, solar energy that energy is huge solves the new energy crisis of people and environment difficulties, the only selection seemed into all researchers.In numerous environmental pollutions, control and our life of water pollutions are closely bound up, and it will directly have influence on our life and health.Just because of these water prevention and cure of pollution have also become the important step of curbing environmental pollution.Photocatalysis technology is applied to water prevention and cure of pollution be also more and more subject to people's attention, and has started actual improvement to a certain degree, and achieve certain effect but still exist a lot of bottleneck need solve.
Photocatalysis technology refers to that application luminous energy provides energy to make pollutant in catalyst surface generation redox reaction, and makes it degrade and technology that self does not change.Its course of reaction can be divided into two stages, i.e. absorption phase and photocatalysis stage.Absorption refers to that the process that Adsorption of Organic contacts to its surface with reaction site by the adsorption function that catalyst possesses, photocatalysis stage are the electronics of the energy generation provided by light by reaction site and hole and then with organic pollution generation redox reaction and the process of being degraded.Along with people are to the continuous research of photocatalysis technology, traditional single one dimension photochemical catalyst (TiO
2, CdS etc.) needs of people's production practices can not be met gradually, the substitute is the photocatalysis of two-dimensional semiconductor nano material namely by the composite photocatalyst semiconductor substrate of photoresponse being supported to reaction site.Be mapped in earth surface sunshine, ultraviolet composition only accounts for 4%, and the content of visible ray then accounts for more than 40%, the main focus therefore more utilizing visible ray to carry out light-catalyzed reaction also to have become photocatalysis to study.
Summary of the invention
The object of the invention is to overcome Fenton react iron ion and to run off the shortcoming that can not reuse, provide a kind of integrated Fenton effect and light-catalysed solid-state supermolecule photochemical catalyst and its preparation method and application to solve the problem.
To achieve these goals, technical scheme of the present invention is as follows:
A kind of integrated Fenton effect and light-catalysed solid-state supermolecule photochemical catalyst are iron complex and g-C
3n
4compound, wherein, the part of described iron complex is organic multicomponent acid, organic polyhydric alcohol, organic multicomponent amine, heteropoly acid or phosphotungstic acid, and described organic multicomponent acid is oxalic acid, citric acid, malonic acid, tartaric acid or malic acid; Described organic polyhydric alcohol is triethanolamine; Described organic multicomponent amine is EDTA.
A preparation method for solid-state supermolecule photochemical catalyst described above, it comprises the steps:
Water-soluble molysite is dissolved in ultra-pure water, obtains the iron salt solutions of 1 ~ 50mM;
After regulating the pH of described iron salt solutions to be not more than 1, stoichiometrically add part precursor wherein, obtain iron complex;
G-C is added in described iron complex
3n
4, after stirring 8 ~ 16h, dry at 70 ~ 90 DEG C, obtain described solid-state supermolecule photochemical catalyst;
Wherein, described part precursor is sodium oxalate, trisodium citrate, heteropoly acid, the sodium salt of heteropoly acid or the ammonium salt of heteropoly acid, and described heteropoly acid is the one in phosphotungstic acid, phosphomolybdic acid and silico-tungstic acid.
Preferably, described molysite is ferric nitrate, ferric sulfate or iron chloride.
Preferably, described iron complex and g-C
3n
4proportioning be the g-C of every 0.1g
3n
4corresponding 1 × 10
-4~ 1 × 10
-3the iron complex of mol, preferably 2 × 10
-4mol.
A kind of integrated Fenton effect and light-catalysed solid-state supermolecule photochemical catalyst are ferrocene and g-C
3n
4compound.
A preparation method for solid-state supermolecule photochemical catalyst described above, is characterized in that, comprise the steps:
Ferrocene is dissolved in hot water, adds g-C while hot
3n
4powder, fully stirs 8 ~ 16h, heating, drying under 70 ~ 90 DEG C of conditions, obtains ferrocene/g-C
3n
4composite photo-catalyst, wherein, described ferrocene and g-C
3n
4proportioning be the g-C of every 0.1g
3n
4corresponding 1 × 10
-4~ 1 × 10
-3the ferrocene of mol, preferably 2 × 10
-4mol.
A kind of integrated Fenton effect and light-catalysed solid-state supermolecule photochemical catalyst are hemin and g-C
3n
4compound.
A preparation method for solid-state supermolecule photochemical catalyst as above-mentioned in power, it comprises the steps:
Hemin is dissolved in acid-heated water's acetone, adds g-C while hot
3n
4powder, fully stirs 8 ~ 16h, heating, drying under 70 ~ 90 DEG C of conditions, obtains hemin/g-C
3n
4composite photo-catalyst, wherein, described hemin and g-C
3n
4proportioning be the g-C of every 0.1g
3n
4with 1 × 10
-4~ 1 × 10
-3the hemin of mol is corresponding, and preferably 2 × 10
-4.
Aforementioned three kinds of solid-state supermolecule photochemical catalysts all may be used for the photocatalytic degradation of organic dyestuff.
Graphite phase carbon nitride (g-C
3n
4) because the graphite-like lamellar structure of its uniqueness and nitrogen substitute doping become a kind of porous material both with strong adsorption capacity, possess again the New Two Dimensional nano semiconductor material that good electric conductivity can also respond visible ray simultaneously.Meanwhile, because it can be prepared by urea, therefore its preparation cost is very cheap, is suitable for large-scale actual production practice.
Traditional homogeneous phase Fenton reaction is by Fe
2+with H
2o
2effect produces the process of OH, and OH has very high oxidizing potential, and its oxidability is only second to simple substance fluoride, can carry out the oxidation of non-selectivity to organic pollution, therefore Fenton reagent is regarded as the reaction site of very good two-dimentional composite photo-catalyst.But homogeneous phase Fenton reaction has a lot of bottleneck and needs to solve, must by continuous adjust ph (Optimal pH=3.5) as reacted, reaction needs constantly in system, to supplement Fe
2+and H
2o
2, have a large amount of iron mud after having reacted and generate and bring secondary pollution etc.Therefore, improve existing Fenton system, solve the above problem found, thus build new, efficient two-dimentional photocatalysis reflection system, for we specify the direction of future studies.
Beneficial effect of the present invention is mainly reflected in:
1, source of iron is stablized, and obtains by making complex the loss that mode greatly reduces iron, and this feature can be checked by cycle performance test in example;
2, photocatalysis condition does not affect by pH, same because iron ion coordinates;
3, fast to visible light-responded and reaction speed, carrier g-C
3n
4because the ability of its excellent absorption property and conduction electron makes reaction speed greatly accelerate.
Accompanying drawing explanation
Fig. 1 is the transmission electron microscope picture of the solid-state supermolecule photochemical catalyst that the present invention obtains;
Fig. 2 is degradation efficiency and the cycle performance of the solid-state supermolecule photocatalyst for degrading dye, rhodamine B that the present invention obtains.
Detailed description of the invention
Embodiment 1
One, ferric chloride hexahydrate is dissolved in ultra-pure water, obtains the ferric chloride solution of 1mM;
Two, after regulating the pH of ferric chloride solution to be not more than 1, stoichiometrically add sodium oxalate wherein, obtain iron-Oxalate Complexes;
Three, by the g-C of every 0.1g
3n
4add 1 × 10
-4the ratio of the iron-Oxalate Complexes of mol is by g-C
3n
4with iron-Oxalate Complexes mixing, after stirring 12h, dry at 80 DEG C, obtain solid-state supermolecule photochemical catalyst.
Embodiment 2
One, six nitric hydrate iron are dissolved in ultra-pure water, obtain the iron nitrate solution of 10mM;
Two, after regulating the pH of ferric chloride solution to be not more than 1, stoichiometrically add trisodium citrate wherein, obtain iron-citric acid compound;
Three, by the g-C of every 0.1g
3n
4add 2 × 10
-4the ratio of the iron-citric acid compound of mol is by g-C
3n
4with iron-citric acid compound mixing, after stirring 12h, dry at 80 DEG C, obtain solid-state supermolecule photochemical catalyst.
Embodiment 3
One, seven ferric sulfate hydrates are dissolved in ultra-pure water, obtain the ferrum sulfuricum oxydatum solutum of 20mM;
Two, after regulating the pH of ferric chloride solution to be not more than 1, stoichiometrically add phosphotungstic acid wherein, obtain iron-phosphotungstic acid complex;
Three, by the g-C of every 0.1g
3n
4add 1 × 10
-3the ratio of the iron-phosphotungstic acid complex of mol is by g-C
3n
4with iron-phosphotungstic acid complex mixing, after stirring 12h, dry at 80 DEG C, obtain solid-state supermolecule photochemical catalyst.As shown in Figure 1.Lamellar is large-sized is g-C
3n
4, iron-phosphotungstic acid complex adsorption is at g-C
3n
4on the surface, can't see the particle that iron is formed in transmission electron microscope, illustrate that iron exists with the state of complex.
Embodiment 4
One, six nitric hydrate iron are dissolved in ultra-pure water, obtain the iron nitrate solution of 30mM;
Two, after regulating the pH of ferric chloride solution to be not more than 1, stoichiometrically add triethanolamine wherein, obtain iron-Triethanolamine complex;
Three, by the g-C of every 0.1g
3n
4add 2 × 10
-4the ratio of the iron-Triethanolamine complex of mol is by g-C
3n
4with iron-Triethanolamine complex mixing, after stirring 12h, dry at 80 DEG C, obtain solid-state supermolecule photochemical catalyst.
Embodiment 5
One, ferric chloride hexahydrate is dissolved in ultra-pure water, obtains the ferric chloride solution of 50mM;
Two, after regulating the pH of ferric chloride solution to be not more than 1, stoichiometrically add EDTA wherein, obtain the complex of iron-EDTA;
Three, by the g-C of every 0.1g
3n
4add 2 × 10
-4the ratio of the iron-EDTA complex of mol is by g-C
3n
4with the mixing of iron-EDTA complex, after stirring 12h, dry at 80 DEG C, obtain solid-state supermolecule photochemical catalyst.
Embodiment 6
One, ferrocene is added in ultra-pure water, drip nitric acid and water heating is made ferrocene accelerate dissolution, obtaining ferrocene solution;
Two, by the g-C of every 0.1g
3n
4add 2 × 10
-4the ratio of the ferrocene of mol adds g-C while hot
3n
4, after stirring 12h, dry at 80 DEG C, obtain solid-state supermolecule photochemical catalyst.
Embodiment 7
One, ferrocene is added in ultra-pure water, drip nitric acid and water heating is made ferrocene accelerate dissolution, obtaining ferrocene solution;
Two, by the g-C of every 0.1g
3n
4add 1 × 10
-3the ratio of the ferrocene of mol adds g-C while hot
3n
4, after stirring 16h, dry at 80 DEG C, obtain solid-state supermolecule photochemical catalyst.
Embodiment 8
One, ferrocene is added in ultra-pure water, drip nitric acid and water heating is made ferrocene accelerate dissolution, obtaining ferrocene solution;
Two, by the g-C of every 0.1g
3n
4add 1 × 10
-4the ratio of the ferrocene of mol adds g-C while hot
3n
4, after stirring 8h, dry at 80 DEG C, obtain solid-state supermolecule photochemical catalyst.
Embodiment 9
One, hemin is added in ultra-pure water, drip acid acetone and heating make hemin accelerate dissolution, obtain hemin solution;
Two, by the g-C of every 0.1g
3n
4add 2 × 10
-4the ratio of the hemin of mol adds g-C while hot
3n
4, after stirring 12h, dry at 80 DEG C, obtain solid-state supermolecule photochemical catalyst.
Embodiment 10
One, hemin is added in ultra-pure water, drip acid acetone and heating make hemin accelerate dissolution, obtain hemin solution;
Two, by the g-C of every 0.1g
3n
4add 1 × 10
-4the ratio of the hemin of mol adds g-C while hot
3n
4, after stirring 8h, dry at 80 DEG C, obtain solid-state supermolecule photochemical catalyst.
Embodiment 11
One, hemin is added in ultra-pure water, drip acid acetone and heating make hemin accelerate dissolution, obtain hemin solution;
Two, by the g-C of every 0.1g
3n
4add 1 × 10
-3the ratio of the hemin of mol adds g-C while hot
3n
4, after stirring 16h, dry at 80 DEG C, obtain solid-state supermolecule photochemical catalyst.
Embodiment 12
One, hemin is added in ultra-pure water, drip acid acetone and heating make hemin accelerate dissolution, obtain hemin solution;
Two, by the g-C of every 0.1g
3n
4add 2 × 10
-4the ratio of the hemin of mol adds g-C while hot
3n
4, after stirring 12h, dry at 80 DEG C, obtain solid-state supermolecule photochemical catalyst.
For setting forth practical function of the present invention, below by reaction better and have the example of feature to be discussed.This process is used three kinds of organic dyestuff and is simulated three kinds of different organic pollutions, is respectively methylene blue simulation cationic pollutant, rhodamine B simulation anionic pollutant, methyl orange simulation acid contaminant.Note: three kinds of catalyst all can above-mentioned three kinds of simulation dyestuff generation degradation reactions, and respond well.
Application example 1: the methylene blue solution and 10mg oxalic acid-Fe (the III)/g-C that get 100mL 10mg/L
3n
4composite photo-catalyst mixes, and after ultrasonic 10min, adds 0.5mL 30%H in stirring
2o
2, lucifuge absorption 1h, then react under xenon lamp simulating nature optical condition, 35min dye solution becomes colorless, and is disappeared, illustrate degradable by ultraviolet-uisible spectrophotometer test methylene blue specific absorption.After filtering recovering catalyst, make above-mentioned reaction occurs again, circulate after 2 times, catalyst degradation ability is constant.Circulate after 4 times, catalyst degradation ability slightly declines.As shown in Figure 2.
Application example 2: the rhodamine B solution and 10mg citric acid-Fe (the III)/g-C that get 100mL 10mg/L
3n
4composite photo-catalyst mixes, and after ultrasonic 10min, adds 0.5mL 30%H in stirring
2o
2, lucifuge absorption 1h, then react under xenon lamp simulating nature optical condition, 30min dye solution becomes colorless, and is disappeared, illustrate degradable by ultraviolet-uisible spectrophotometer test rhodamine B specific absorption.After filtering recovering catalyst, make above-mentioned reaction occurs again, circulate after 2 times, catalyst degradation ability is constant.Circulate after 4 times, catalyst degradation ability does not still decline.
Application example 3: the methyl orange solution and the 10mg ferrocene/g-C that get 100mL 10mg/L
3n
4composite photo-catalyst mixes, and after ultrasonic 10min, adds 0.5mL 30%H in stirring
2o
2, lucifuge absorption 1h, then react under xenon lamp simulating nature optical condition, 30min dye solution becomes colorless, and is disappeared, illustrate degradable by ultraviolet-uisible spectrophotometer test methyl orange specific absorption.Circulate after 2 times, catalyst ability slightly declines.
In sum, be only preferred embodiment of the present invention, not be used for limiting scope of the invention process, all equalizations of doing according to shape, structure, feature and the spirit described in the claims in the present invention scope change and modify, and all should be included in right of the present invention.
Claims (10)
1. integrated Fenton effect and a light-catalysed solid-state supermolecule photochemical catalyst, is characterized in that, is iron complex and g-C
3n
4compound, wherein, the part of described iron complex is organic multicomponent acid, organic polyhydric alcohol, organic multicomponent amine, heteropoly acid or phosphotungstic acid, and described organic multicomponent acid is oxalic acid, citric acid, malonic acid, tartaric acid or malic acid; Described organic polyhydric alcohol is triethanolamine; Described organic multicomponent amine is EDTA.
2. a preparation method for solid-state supermolecule photochemical catalyst as claimed in claim 1, is characterized in that, comprise the steps:
Water-soluble molysite is dissolved in ultra-pure water, obtains the iron salt solutions of 1 ~ 50mM;
After regulating the pH of described iron salt solutions to be not more than 1, stoichiometrically add part precursor wherein, obtain iron complex;
G-C is added in described iron complex
3n
4, after stirring 8 ~ 16h, dry at 70 ~ 90 DEG C, obtain described solid-state supermolecule photochemical catalyst;
Wherein, described part precursor is sodium oxalate, trisodium citrate, heteropoly acid, the sodium salt of heteropoly acid or the ammonium salt of heteropoly acid, and described heteropoly acid is the one in phosphotungstic acid, phosphomolybdic acid and silico-tungstic acid.
3. the preparation method of solid-state supermolecule photochemical catalyst as claimed in claim 2, is characterized in that, described molysite is ferric nitrate, ferric sulfate or iron chloride.
4. the preparation method of solid-state supermolecule photochemical catalyst as claimed in claim 2, is characterized in that, described iron complex and g-C
3n
4proportioning be the g-C of every 0.1g
3n
4corresponding 1 × 10
-4~ 1 × 10
-3the iron complex of mol.
5. solid-state supermolecule photocatalyst applications as claimed in claim 1 is in the photocatalytic degradation of organic dyestuff.
6. integrated Fenton effect and a light-catalysed solid-state supermolecule photochemical catalyst, is characterized in that, is ferrocene and g-C
3n
4compound.
7. a preparation method for solid-state supermolecule photochemical catalyst as claimed in claim 6, is characterized in that, comprise the steps:
Ferrocene is dissolved in hot water, adds g-C while hot
3n
4powder, fully stirs 8 ~ 16h, heating, drying under 70 ~ 90 DEG C of conditions, obtains ferrocene/g-C
3n
4composite photo-catalyst, wherein, described ferrocene and g-C
3n
4proportioning be the g-C of every 0.1g
3n
4with 1 × 10
-4~ 1 × 10
-3the ferrocene of mol is corresponding.
8. solid-state supermolecular catalysis agent is as claimed in claims 6 or 7 applied to the photocatalytic degradation of organic dyestuff.
9. integrated Fenton effect and a light-catalysed solid-state supermolecule photochemical catalyst, is characterized in that, is hemin and g-C
3n
4compound.
10. a preparation method for solid-state supermolecule photochemical catalyst as claimed in claim 9, is characterized in that, comprise the steps:
Hemin is dissolved in acid-heated water's acetone, adds g-C while hot
3n
4powder, fully stirs 8 ~ 16h, heating, drying under 70 ~ 90 DEG C of conditions, obtains hemin/g-C
3n
4composite photo-catalyst, wherein, described hemin and g-C
3n
4proportioning be the g-C of every 0.1g
3n
4with 1 × 10
-4~ 1 × 10
-3the hemin of mol is corresponding.
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