CN104549385A - Graphene oxide composite FePO4 heterogeneous visible light Fenton catalyst and preparation method thereof - Google Patents

Graphene oxide composite FePO4 heterogeneous visible light Fenton catalyst and preparation method thereof Download PDF

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CN104549385A
CN104549385A CN201410853655.3A CN201410853655A CN104549385A CN 104549385 A CN104549385 A CN 104549385A CN 201410853655 A CN201410853655 A CN 201410853655A CN 104549385 A CN104549385 A CN 104549385A
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graphene oxide
catalyzer
fepo
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张高科
郭盛
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Wuhan University of Technology WUT
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Abstract

The invention belongs to the technical field of a catalyst novel material technology and environmental purification and relates to a graphene oxide composite FePO4 heterogeneous visible light Fenton catalyst and a preparation method thereof. The preparation method particularly comprises the following steps: (1) adding graphene oxide into water and after carrying out ultrasonic dispersion, obtaining graphene oxide dispersion liquid; (2) heating to a temperature of 70 DEG C, sequentially and slowly adding NH4H2PO4 and Fe(NO3)3.9H2O and regulating the pH value to be 1.5; (3) after stirring for 1h at the temperature of 70 DEG C, taking precipitates, washing the precipitates to be neutral, and drying the precipitates at the temperature of 60-80 DEG C, so as to obtain the graphene oxide composite FePO4 heterogeneous visible light Fenton catalyst. The catalyst prepared by the method can effectively solve the problems of narrow pH range, high post-processing cost and the like, can degrade organisms difficult to degrade in water within a wider pH range (pH is 2.18 to 10.40) and has high catalysis stability.

Description

A kind of graphene oxide compound FePO 4heterogeneous visible ray Fenton Catalysts and its preparation method
Technical field
The invention belongs to catalyzer new material technology and technical field of environmental purification, be specifically related to a kind of graphene oxide compound FePO 4the preparation method of heterogeneous visible ray Fenton catalyzer.
Background technology
Water is Source of life, but along with the development of industry, water pollution problems is more and more serious, how effectively to administer water pollutions, has become one of major issue that the urgent need that generally faces in world wide solves.In recent years, the very big concern of numerous researchers is caused based on the high-level oxidation technology producing oxidative free radical.Wherein, the OH free radical Standard Electrode Potentials that produces of Fenton system is only lower than F 2there is extremely strong oxidation capacity, have good treatment effect to the organic waste water that difficult for biological degradation or general chemical oxidizing agent are difficult to prove effective, and use range is wide, reaction conditions is gentle, is considered to process poisonous and harmful and one of most technology with application prospect of difficult for biological degradation organic waste water.But, for difficult degradation and poisonous and hazardous organic waste water as waste water from dyestuff, phenols wastewater etc., traditional Fenton system still also exists a lot of deficiency in actual applications, as reaction optimal ph be confined to 2-4; Need in reaction by methods such as precipitations, the iron ion in solution to be separated, add processing cost; Great majority need, under UV-irradiation, katalysis occurs, and H 2o 2utilization ratio is not high.
In order to overcome the deficiency of traditional homogeneous phase Fenton system, a lot of scholar is studied heterogeneous Fenton-like photocatalyst material.So-called heterogeneous fenton-type reagent system, refers to the ferrous salt and the H that use heterogeneous iron system solid catalyst to replace homogeneous phase 2o 2or O 2reaction, its advantage is to make solid catalyst easy Separation and Recovery while guarantee catalytic activity also can reuse, and effectively avoids secondary pollution.Although these prior art researchs have been done a large amount of work and have been achieved certain achievement in the problems such as solution iron ion loss, but, wherein a lot of catalytic oxidation still exists affects by pH value, less stable, to deficiencies such as Adsorption of Organic accumulation ability are poor, thus limit application and the popularization of this technology.Therefore, the research direction that new heterogeneous light/Fenton catalyzer remains this field how is designed.
Summary of the invention
The object of the present invention is to provide a kind of graphene oxide compound FePO 4heterogeneous visible ray Fenton Catalysts and its preparation method, this preparation method is simple and convenient, catalyzer synthesis temperature is low, prepared catalyzer can in wider pH scope (pH2.18-10.40) hardly degraded organic substance and there is good catalytic stability in degradation water.
For achieving the above object, the technical solution used in the present invention is:
A kind of graphene oxide compound FePO 4heterogeneous visible ray Fenton catalyzer, is characterized in that, described catalyzer is by graphene oxide, NH 4h 2pO 4with Fe (NO 3) 39H 2o adopts the method for co-precipitation to prepare.
A kind of graphene oxide compound FePO 4the preparation method of heterogeneous visible ray Fenton catalyzer, is characterized in that it comprises the steps:
(1) graphite oxide is added to the water, after ultrasonic disperse, obtains graphene oxide dispersion;
(2) be warming up to 70 DEG C, in graphene oxide dispersion, slowly add NH successively 4h 2pO 4with Fe (NO 3) 39H 2o, the pH=1.5 of regulator solution;
(3) 70 DEG C are stirred after 1h, and taking precipitate is also washed to neutrality, throw out is placed in 60 ~ 80 DEG C of dryings, and the catalyzer obtained for heterogeneous visible ray/Fenton system (or claims graphene oxide compound FePO 4heterogeneous visible ray Fenton catalyzer).
By such scheme, the solid-to-liquid ratio of described graphene oxide dispersion is: be dispersed with graphene oxide 0.05g ~ 0.2g in every 100ml water.
By such scheme, described graphene oxide: NH 4h 2pO 4: Fe (NO 3) 39H 2o=0.05 ~ 0.2:2.29:5.36.
The preparation method of heterogeneous visible ray of the present invention/Fenton system solid catalyst, prepares graphene oxide compound FePO except being applied to 4outward, can also for the preparation of the carbon material Fenton catalyzer of other visible light activity, as FePO 4/ gac, FePO 4/ Graphene visible ray Fenton catalyzer etc.
Prepared graphene oxide compound FePO 4the photocatalytic of heterogeneous visible ray Fenton catalyzer characterizes by visible light photocatalytic degradation organic dye rhodamine B (RhB).Experimentation is as follows: with 300W dysprosium lamp simulated visible light light source, ensures the irradiation (λ >400nm) of visible ray with the spectral filter of 400nm; The RhB solution 100mL measuring 10mg/L during experiment is placed in beaker, adds graphene oxide compound FePO under unglazed whipped state 4catalyzer 0.1g, Keep agitation 20min, make catalyzer be uniformly dispersed in the solution; Then beaker to be transferred to through preheating and in the reactor of stabilized intensity, and in beaker, to add rapidly the H of 3% 2o 2solution 1mL, starts timing, every certain hour sampling, measures the absorbancy of solution at 554nm place.After the completion of reaction, directly can carry out Separation and Recovery by simple leaving standstill, the catalyzer after recovery can continue to recycle this catalyzer.
Beneficial effect of the present invention:
(1) preparation method is simple and convenient, catalyzer synthesis temperature low (60-80 DEG C), can difficult degradation in degradation water in wider pH scope (pH 2.18 ~ 10.40) organism and there is good catalytic stability, effectively overcome the deficiency that traditional homogeneous phase Fenton system pH scope is narrower;
(2) by FePO 4with the graphene oxide compound with high absorption property, add photoresponse scope and the absorption property of catalyzer, thus effectively improve the speed of catalytic degradation reaction, for process poisonous and harmful organic wastewater with difficult degradation thereby provides wide prospect.
Accompanying drawing explanation
Fig. 1 is graphene oxide and the FePO of different content 4the XRD figure of the catalyzer of compound.
Fig. 2 is graphene oxide and the FePO of different content 4the UV-vis DRS collection of illustrative plates of the catalyzer of compound, wherein a is FePO 4, b is 2.5GO-FePO 4, c is 5GO-FePO 4, d is 10GO-FePO 4.
Fig. 3 is graphene oxide and the FePO of different content 4the catalyzer of compound is to the visible ray Fenton catalytic degradation effect figure of RhB.
Fig. 4 is graphene oxide compound FePO 4catalyzer recycles number of times effect contrast figure to photocatalytic degradation RhB in visible light/Fenton system.
Fig. 5 is graphene oxide compound FePO under different solution initial pH value 4catalyzer in visible light/Fenton system to the percent of decolourization of RhB.
Embodiment
In order to understand the present invention better, illustrate content of the present invention further below in conjunction with embodiment, but content of the present invention is not only confined to the following examples.
Embodiment 1
A kind of graphene oxide compound FePO 4heterogeneous visible ray Fenton catalyzer, its preparation method comprises the steps:
(1) taking 0.05g, 0.1g, 0.2g graphite oxide joins in 3 parts of 100mL water respectively, and respective ultrasonic disperse 1h, obtains 3 parts of graphene oxide dispersion;
(2) be warming up to 70 DEG C, slowly add 2.29g NH successively respectively 4h 2pO 4with 5.36g Fe (NO 3) 39H 2o, regulates pH=1.5;
After (3) 70 DEG C of stirring 1h, taking precipitate is washed to neutrality, and throw out, in 80 DEG C of dryings, obtains the catalyzer (2.5GO-FePO for heterogeneous visible ray/Fenton system 4, 5GO-FePO 4, 10GO-FePO 4).
The graphene oxide compound FePO of different content 4heterogeneous Fenton catalyzer (5GO-FePO 4, 10GO-FePO 4) XRD figure spectrum as shown in Figure 1.Graphite oxide (001) diffraction peak appears at 2 θ=10.67 °, and corresponding spacing of lattice is fePO 4in the composite to exist, by simple FePO without pattern form 4sample 800 DEG C of roastings after 4 hours, FePO 4be crystal form (JCPDS:84-876) from amorphous state.As can be seen from the figure, graphene oxide-loaded amount is the mixture (10GO-FePO of 0.2g 4) XRD figure spectrum in there is a weak graphite oxide diffraction peak (001), show graphene oxide and FePO 4success compound, and charge capacity is 0.05g (2.5GO-FePO 4) and charge capacity be 0.1g (5GO-FePO 4) mixture in because there is the characteristic peak of graphite oxide very little and not in graphite oxide content.
The graphene oxide compound FePO of different content 4heterogeneous Fenton catalyzer (2.5GO-FePO 4, 5GO-FePO 4, 10GO-FePO 4) UV-vis DRS collection of illustrative plates as shown in Figure 2.Along with graphene oxide content in the composite increases, the Absorption edge Red Shift Phenomena of mixture is more obvious, illustrates that the absorbing properties of graphene oxide to mixture has very large promoter action.
This catalyzer is in the experiment of degraded RhB, and dosage is 1.0g/L, RhB starting point concentration is 10mg/L, H 2o 2concentration is 10mmol/L, irradiates the wavelength X >400nm of light, the graphene oxide compound FePO of 120min different content 4to the degradation effect of RhB as shown in Figure 3, along with the increase of graphene oxide content in the composite, mixture strengthens the absorption of RhB and degradation property catalyzer all gradually.For the consideration of degradation efficiency and cost, follow-uply all adopt 5GO-FePO 4sample is tested as optimum sample.
Catalyzer (the 5GO-FePO that Fig. 4 obtains for embodiment 1 4) the circulation experiment degradation effect comparison diagram of catalyzed degradation RhB, result shows that this catalyzer has good catalytic stability in visible light/Fenton system, can realize recycling by simple precipitate and separate, successfully solve iron ion losing issue.
In order to inquire into solution initial pH value (pH 2.18-10.40) impact on the catalytic performance of catalyzer, the HCl solution of the initial pH value 0.1mol/L of RhB solution or the NaOH solution of 0.1mol/L regulate, catalyst amounts is 1.0g/L, RhB starting point concentration is 10mg/L, H 2o 2concentration is 10mmol/L, and irradiate the wavelength X >400nm of light, the degradation rate of the RhB of the initial pH of the solution that 120min is different all more than 90% (as Fig. 5).
Catalyzer (the 5GO-FePO that Fig. 5 obtains for embodiment 1 4) under different solutions initial pH value to the degradation rate of RhB, result shows that this catalyzer is in the visible light/Fenton system of heterogeneous catalyst, the initial pH value scope of application can be widened to 2.18-10.40, well solves the drawback that conventional homogeneous lightwave CATV system is suitable for pH value narrow range (pH 2-4).
Embodiment 2
A kind of graphene oxide compound FePO 4heterogeneous visible ray Fenton catalyzer, its preparation method comprises the steps:
(1) take 0.1g graphite oxide ultrasonic disperse 2h in 100mL water, obtain the graphene oxide dispersion that solid-liquid mass ratio is 0.1%;
(2) be warming up to 70 DEG C, slowly add 2.29g NH successively 4h 2pO 4with 5.36g Fe (NO 3) 39H 2o, regulates pH=1.5;
After (3) 70 DEG C of stirring 1h, taking precipitate, is washed to neutrality, and throw out, in 60 DEG C of dryings, obtains graphene oxide compound FePO 4the catalyzer of heterogeneous visible ray/Fenton system.
Catalyzer prepared by this embodiment is in the experiment of degraded RhB, and dosage is 1.0g/L, RhB starting point concentration is 10mg/L, H 2o 2concentration is 10mmol/L, and irradiate the wavelength X >400nm of light, the degradation rate of 120min RhB is 96.8%.Catalyzer prepared by explanation has good visible light catalytic performance to difficult degradation organic dye RhB in heterogeneous visible ray/Fenton system.
Prepared catalyzer (pH 2.18-10.40) under wider pH condition all has good catalytic stability, the circulation degraded experiment effect of the catalyst degraded RhB that the present embodiment obtains and under different solution initial pH value to the result of the degradation rate of RhB with embodiment 1.
Embodiment 3
A kind of graphene oxide compound FePO 4heterogeneous visible ray Fenton catalyzer, its preparation method comprises the steps:
(1) take 0.1g graphite oxide ultrasonic disperse 0.5h in 100mL water, obtain the graphene oxide dispersion that solid-liquid mass ratio is 0.1%;
(2) be warming up to 70 DEG C, slowly add 2.29g NH successively 4h 2pO 4with 5.36g Fe (NO 3) 39H 2o, regulates pH=1.5;
After (3) 70 DEG C of stirring 1h, taking precipitate, is washed to neutrality, and throw out, in 70 DEG C of dryings, obtains graphene oxide compound FePO 4the catalyzer of heterogeneous visible ray/Fenton system.
This catalyzer is in the experiment of degraded RhB, and dosage is 1.0g/L, RhB starting point concentration is 10mg/L, H 2o 2concentration is 10mmol/L, and irradiate the wavelength X >400nm of light, the degradation rate of 120min RhB is 97.2%.Catalyzer prepared by explanation has good visible light catalytic performance to Persistent organic pollutants in heterogeneous visible ray/Fenton system.
Prepared catalyzer all has good catalytic stability under pH environment comparatively widely, the circulation degraded experiment effect of the catalyst degraded RhB that the present embodiment obtains and under different solution initial pH value to the result of the degradation rate of RhB with embodiment 1.
Embodiment 4
A kind of graphene oxide compound FePO 4heterogeneous visible ray Fenton catalyzer, its preparation method comprises the steps:
(1) take 0.05g graphite oxide ultrasonic disperse 1h in 100mL water, obtain the graphene oxide dispersion that solid-liquid mass ratio is 0.05%;
(2) be warming up to 70 DEG C, slowly add 2.29g NH successively 4h 2pO 4with 5.36g Fe (NO 3) 39H 2o, regulates pH=1.5;
After (3) 70 DEG C of stirring 1h, taking precipitate, is washed to neutrality, and throw out, in 80 DEG C of dryings, obtains graphene oxide compound FePO 4the catalyzer of heterogeneous visible ray/Fenton system.
This heterogeneous Fenton catalyzer is in the experiment of degraded RhB, and dosage is 1.0g/L, RhB starting point concentration is 10mg/L, H 2o 2concentration is 10mmol/L, and irradiate the wavelength X >400nm of light, the degradation rate of 120min RhB is 91.2%.Catalyzer prepared by explanation has good visible light catalytic performance to Persistent organic pollutants in heterogeneous visible ray/Fenton system.
Prepared catalyzer all has good catalytic stability under pH environment comparatively widely, the circulation degraded experiment effect of the catalyst degraded RhB that the present embodiment obtains and under different solution initial pH value to the result of the degradation rate of RhB with embodiment 1.
Embodiment 5
A kind of graphene oxide compound FePO 4heterogeneous visible ray Fenton catalyzer, its preparation method comprises the steps:
(1) take 0.2g graphite oxide ultrasonic disperse 1h in 100mL water, obtain the graphene oxide dispersion that solid-liquid mass ratio is 0.2%;
(2) be warming up to 70 DEG C, slowly add 2.29g NH successively 4h 2pO 4with 5.36g Fe (NO 3) 39H 2o, regulates pH=1.5;
After (3) 70 DEG C of stirring 1h, taking precipitate, is washed to neutrality, and throw out, in 80 DEG C of dryings, obtains graphene oxide compound FePO 4the catalyzer of heterogeneous visible ray/Fenton system.
This catalyzer is in the experiment of degraded RhB, and dosage is 1.0g/L, RhB starting point concentration is 10mg/L, H 2o 2concentration is 10mmol/L, and irradiate the wavelength X >400nm of light, the degradation rate of 120min RhB is 97.3%.Catalyzer prepared by explanation has good visible light catalytic performance to Persistent organic pollutants in heterogeneous visible ray/Fenton system.
Prepared catalyzer all has good catalytic stability under pH environment comparatively widely, the circulation degraded experiment effect of the catalyst degraded RhB that the present embodiment obtains and under different solution initial pH value to the result of the degradation rate of RhB with embodiment 1.

Claims (4)

1. a graphene oxide compound FePO 4heterogeneous visible ray Fenton catalyzer, is characterized in that, described catalyzer is by graphite oxide, NH 4h 2pO 4with Fe (NO 3) 3.9H 2o adopts the method for co-precipitation to prepare.
2. graphene oxide compound FePO as claimed in claim 1 4the preparation method of heterogeneous visible ray Fenton catalyzer, is characterized in that it comprises the steps:
(1) graphite oxide is added to the water, after ultrasonic disperse, obtains graphene oxide dispersion;
(2) be warming up to 70 DEG C, in graphene oxide dispersion, slowly add NH successively 4h 2pO 4with Fe (NO 3) 3.9H 2o, the pH=1.5 of regulator solution;
After (3) 70 DEG C of stirring 1 h, taking precipitate is also washed to neutrality, throw out is placed in 60 ~ 80 DEG C of dryings, obtains graphene oxide compound FePO 4heterogeneous visible ray Fenton catalyzer.
3. preparation method according to claim 2, the solid-liquid mass ratio of described graphene oxide dispersion is: be dispersed with graphene oxide 0.05g ~ 0.2g in every 100ml water.
4. preparation method according to claim 2, described graphene oxide: NH 4h 2pO 4: Fe (NO 3) 3.9H 2the mass ratio of O is 0.05 ~ 0.2:2.29: 5.36.
CN201410853655.3A 2014-12-31 2014-12-31 Graphene oxide composite FePO4 heterogeneous visible light Fenton catalyst and preparation method thereof Pending CN104549385A (en)

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CN113244937A (en) * 2021-04-25 2021-08-13 中南民族大学 Fenton oxidation water treatment method of coupling sludge biochar-iron phosphate catalyst
CN113244937B (en) * 2021-04-25 2022-05-03 中南民族大学 Fenton oxidation water treatment method of coupling sludge biochar-iron phosphate catalyst

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Application publication date: 20150429