CN105056981A - Preparation and application of composite photocatalyst g-C3N4-BiFeO3 for efficiently removing persistent organic pollutants - Google Patents

Preparation and application of composite photocatalyst g-C3N4-BiFeO3 for efficiently removing persistent organic pollutants Download PDF

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CN105056981A
CN105056981A CN201510417786.1A CN201510417786A CN105056981A CN 105056981 A CN105056981 A CN 105056981A CN 201510417786 A CN201510417786 A CN 201510417786A CN 105056981 A CN105056981 A CN 105056981A
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preparation
catalyst
persistent organic
organic pollutants
bismuth
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CN105056981B (en
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涂新满
周仁韬
罗胜联
代威力
罗旭彪
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Nanchang Hangkong University
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Abstract

The invention discloses preparation and an application of a composite photocatalyst g-C3N4-BiFeO3 for efficiently removing persistent organic pollutants. The method adopts a sol-gel method for synthesis, and the g-C3N4-BiFeO3 composite photocatalyst is synthesized by one step with the sol-gel method. A xenon lamp is taken as a light source, BPA which is the persistent organic pollutant in the environment is taken as a photodegradation model, and a composite material and a BPA solution are mixed sufficiently for photocatalytic degradation and simulation of the BPA persistent organic pollutant in the water environment. The invention provides a method for efficiently removing the BPA in the water environment, more than 90% of the BPA in the water environment is removed within 2 hours with the method, the concentration is 10 mg/L, the performance is stable, the g-C3N4-BiFeO3 composite photocatalyst is synthesized successfully by one step for the first time, and the preparation and the application has great significance and development prospects in sewage treatment.

Description

The composite photo-catalyst g-C of efficient removal persistent organic pollutants 3n 4the preparation of-bismuth ferrite and application thereof
Technical field
The invention belongs to field of Environment Protection, be specifically related to the composite photo-catalyst g-C efficiently removing persistent organic pollutants 3n 4the preparation of-bismuth ferrite and application thereof.
Background technology
In recent years, environmental pollution badly influences daily life, therefore how effectively to eliminate the organic pollution to human hazard, has become the focus that scientific circles pay close attention to.Traditional administering method not only poor effect, and not environmentally, easily secondary pollution is caused to environment.Photocatalysis technology, in solution problem of environmental pollution, shows great application potential.And, because Photocatalitic Technique of Semiconductor self has plurality of advantages, as: cheap, nontoxic, energy consumption is low.Therefore, this technology obtains extensive research.
Bismuth ferrite, as a kind of novel conductor photocatalysis material, can be used for degradable organic pollutant.BFO energy gap, at 2.1eV-2.9eV, has good response in visible-range, with TiO 2compare, more effectively can utilize visible ray, but its photocatalytic activity is lower, this just hinders it as the application in photochemical catalyst realization.The factor affecting material light catalysis activity mainly contains three aspects: the specific area of (1) catalysis material; (2) photochemical catalyst produces the ability of electron-hole pair; (3) electronics and the hole separation rate on material.The photocatalytic activity that bismuth ferrite is lower is also mainly subject to the restriction of these factors.For this reason, improve the photocatalytic activity of bismuth ferrite, improve its light absorpting ability, the method for improvement has multiple, that relatively commonly uses at present has following three kinds: (1) improves the specific area of material by the bismuth ferrite preparing different-shape and structure, thus improves its photocatalytic activity; (2) by carrying out metal or doped metallic oxide, as Zn, Mn, La etc. to bismuth ferrite material.Thus effectively strengthen absorbing properties, and then improve the catalytic performance of material in photocatalytic applications; (3) the secret band structure of ferrous acid can be improved by ion doping, increase carrier concentration, reduce electron-hole pair recombination rate, the photocatalysis performance that ferrous acid is secret can not only be improved, its magnetic can also be strengthened.But its photo-quantum efficiency is still to be strengthened, and bismuth ferrite exists photoetch.Although can be improved the cycle performance of material by the modification of material, its visible light catalysis activity still has much room for improvement.
G-C 3n 4be considered to a kind of sustainable, non-metal semiconductive photochemical catalyst that can utilize Visible Light Induced Photocatalytic pollutant, good stability, nontoxic, can photolysis water hydrogen, its band gap width is about 2.7eV, and energy absorbing wavelength is less than the light of 460nm, in photocatalysis and degraded, have potential application.But single g-C 3n 4itself can only absorb the visible ray of small part, thus independent g-C 3n 4photocatalytic activity not high, which has limited its practice.
Therefore, in conjunction with g-C 3n 4with the respective advantage of bismuth ferrite material, sol-gal process one step is adopted to prepare g-C 3n 4-bismuth ferrite composite photocatalyst material, by this composite light degradation persistent organic pollutants bisphenol-A, has good photocatalysis effect, and can repeatedly recycle, and has important practical guided significance to degraded persistent organic pollutants aspect.
Summary of the invention
The photo-generated carrier recombination rate that the object of the invention is to solve photochemical catalyst in current photocatalysis field is high, the low and g-C of a kind of efficiency light response of exploitation of quantum efficiency 3n 4-bismuth ferrite composite photo-catalyst and preparation method thereof, the method adopts sol-gal process synthesis.By sol-gal process one-step synthesis g-C 3n 4-bismuth ferrite composite photo-catalyst.And by this catalyst application in photocatalysis treatment persistent organic pollutants.
The present invention is achieved like this, a kind of composite photo-catalyst g-C of efficient removal persistent organic pollutants 3n 4the preparation method of-bismuth ferrite, is characterized in that method step is as follows;
(1) with bismuth source and source of iron for raw material, the two dissolved respectively in organic solvent, normal temperature lower magnetic force stirs until dissolve completely, mixing and stirring;
(2) add a certain amount of melamine, until be uniformly dissolved, heating obtains sol solution, and continue to stir certain hour, dry 24-48 hour at 80-100 DEG C of temperature, obtains xerogel;
(3) xerogel grinding is transferred in Muffle furnace and calcines 3-5 hour, be cooled to room temperature, after grinding sample.
Further, described bismuth source is bismuth nitrate and hydrate thereof, and source of iron is ferric nitrate and hydrate thereof.
Further, described organic solvent is EGME.
Further, described certain hour is 0.5-1 hour.
Further, in Muffle furnace, calcining heat is 500-550 DEG C.
G-C of the present invention 3n 4the application of-bismuth ferrite composite photo-catalyst is: employing xenon lamp is light source, in environment, persistent organic pollutants bisphenol-A is as light degradation model, composite and bisphenol-A solution are fully mixed with the bisphenol-A organic pollution in photocatalytic degradation Simulated Water environment, bisphenol-A in efficient removal water environment, the bisphenol-A removed in 2 hours in water environment reaches more than 90% (concentration is 10mg/L), photocatalytic activity is good, and stable performance, is successful one-step synthesis method g-C first 3n 4-bismuth ferrite composite photo-catalyst, reacted catalyst can recycled for multiple times, has great importance and good development prospect in waste water control.
G-C provided by the invention 3n 4the preparation method of-bismuth ferrite composite photo-catalyst and its original had advantage as follows:
1. by sol-gal process one-step synthesis method g-C 3n 4-bismuth ferrite composite photo-catalyst;
2.g-C 3n 4introducing be conducive to the right separation of photo-generate electron-hole, and the specific area of material can be improved thus can fully contact with organic pollution;
3. take xenon lamp as light source, without the need to oxidant applying and auxiliary agent, the persistent organic pollutants in water can be removed efficiently;
4. the preparation of catalyst has good repeatability, and catalytic activity is high, and abundant raw material is easy to get, and facilitates industrialization promotion.
Accompanying drawing explanation
Fig. 1 is g-C 3n 4the XRD figure of-bismuth ferrite composite photo-catalyst, has as can be seen from the figure successfully synthesized g-C 3n 4-bismuth ferrite composite photo-catalyst.
Fig. 2 is g-C 3n 4the infrared spectrum of-bismuth ferrite composite photo-catalyst, can confirm g-C in composite further from spectrogram 3n 4existence.
Fig. 3 is g-C 3n 4the uv drs figure of-bismuth ferrite composite photo-catalyst, as can be seen from the figure composite there occurs obvious red shift, and explanation better can utilize visible ray.
Fig. 4 is g-C 3n 4the design sketch of the light degradation bisphenol-A of-bismuth ferrite composite photo-catalyst, as can be seen from the figure composite reached 90% to bisphenol-A degradation effect in 2 hours, compared single bismuth ferrite and g-C 3n 4be significantly improved.
Detailed description of the invention
Realizing key technology of the present invention is prepare g-C 3n 4-bismuth ferrite composite photo-catalyst, for achieving the above object, the invention provides following technical scheme:
G-C 3n 4the preparation method of-bismuth ferrite composite photo-catalyst, the method comprises:
(1) make bismuth salt and molysite dissolve in organic solvent respectively, form the organic solution of bismuth-containing salt and the organic solution containing molysite;
(2) fully mix by the organic solution of the bismuth-containing salt of same ratio in (1) with containing the organic solution of molysite, the magnetic agitation regular hour, form bismuth-containing salt and the mixed organic solvents containing molysite;
(3) a certain amount of melamine is added by the mixed solution of (2);
(4) mixed organic solvents in (3) is carried out evaporate to dryness, obtain xerogel;
(5) the xerogel grind into powder in (4) be transferred in Muffle furnace calcine, be cooled to room temperature, grind to obtain sample:
Bismuth salt described in step (1) is bismuth nitrate and hydrate thereof, and described molysite is ferric nitrate and hydrate thereof, and described organic solution is EGME;
The magnetic agitation regular hour described in step (2) is 0.5-1 hour;
A certain amount of melamine that adds described in step (3) is 30-50%;
The temperature of organic solution being carried out evaporate to dryness described in step (4) is 80-100 DEG C, and the evaporate to dryness time is 24-48 hour;
Described in step (5) powder is carried out calcination processing time temperature be 500-550 DEG C, the time is 3-5 hour;
The g-C that said method is prepared 3n 4-bismuth ferrite composite photo-catalyst is for the treatment of the persistent organic pollutants in environment.
Embodiment one
First Bi (the NO of 0.005mol is taken 3) 35H 2o and 0.005molFe (NO 3) 39H 2o sample is dissolved in the EGME solution of 30ml respectively, is uniformly dissolved at normal temperatures under magnetic agitation, will containing Bi (NO 3) 3eGME solution and 0.005molFe (NO 3) 3eGME solution mixing, normal temperature lower magnetic force stirs 30 minutes, add the melamine of 0.01mol, after being uniformly dissolved, heating is stirred to colloidal sol shape, the sample of colloidal sol shape is transferred to baking oven 90 DEG C of dryings 24 hours, obtain gel, by being transferred in Muffle furnace 550 DEG C of calcinings 4 hours after gel abrasive powdered, be cooled to room temperature, after grinding sample.Take the above-mentioned catalyst of 0.100g, joining 100mL initial concentration is in the bisphenol-A organic pollution of 10mg/L, dark reaction carried out light degradation after 40 minutes, light source power is 300W, from liquid level 15cm, sampling in every 20 minutes, by the absorbance of spectrophotometer measurement sample, light-catalyzed reaction, after 120 minutes, reaches 90% to the clearance of persistent organic pollutants bisphenol-A.

Claims (6)

1. efficiently remove the composite photo-catalyst g-C of persistent organic pollutants for one kind 3n 4the preparation of-bismuth ferrite, is characterized in that method step is as follows;
(1) with bismuth source and source of iron for raw material, the two dissolved respectively in organic solvent, normal temperature lower magnetic force stirs until dissolve completely, mixing and stirring;
(2) add a certain amount of melamine, until be uniformly dissolved, heating obtains sol solution, and continue to stir certain hour, dry 24-48 hour at 80-100 DEG C of temperature, obtains xerogel;
(3) xerogel grinding is transferred in Muffle furnace and calcines 3-5 hour, be cooled to room temperature, after grinding sample.
2. the composite photo-catalyst g-C of a kind of efficient removal persistent organic pollutants according to claim 1 3n 4the preparation method of-bismuth ferrite, is characterized in that; Described bismuth source is bismuth nitrate and hydrate thereof, and source of iron is ferric nitrate and hydrate thereof.
3. the composite photo-catalyst g-C of a kind of efficient removal persistent organic pollutants according to claim 1 3n 4the preparation method of-bismuth ferrite, is characterized in that; Described organic solvent is EGME.
4. the composite photo-catalyst g-C of a kind of efficient removal persistent organic pollutants according to claim 1 3n 4the preparation method of-bismuth ferrite, is characterized in that; Described certain hour is 0.5-1 hour.
5. the composite photo-catalyst g-C of a kind of efficient removal persistent organic pollutants according to claim 1 3n 4the preparation method of-bismuth ferrite, is characterized in that; In Muffle furnace, calcining heat is 500-550 DEG C.
6. an application according to claim 1, it is characterized in that: employing xenon lamp is light source, in environment, persistent organic pollutants bisphenol-A is as light degradation model, composite and bisphenol-A solution are fully mixed with the bisphenol-A organic pollution in photocatalytic degradation Simulated Water environment, bisphenol-A in efficient removal water environment, the bisphenol-A removed in 2 hours in water environment reaches more than 90%, and photocatalytic activity is good, stable performance.
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CN107055492A (en) * 2016-10-09 2017-08-18 南京睿磐内尔环保复合新材料有限公司 A kind of directly synthesis g C3N4The method of Supporting cerium oxide nano composite material
CN107930664A (en) * 2017-10-08 2018-04-20 南京邮电大学 One kind prepares BiFeO3/g‑C3N4The method of heterojunction photocatalyst
CN108144585A (en) * 2018-02-05 2018-06-12 中南林业科技大学 A kind of ternary magnetic composite for being used for heavy metal and dye wastewater treatment and preparation method thereof
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CN108686697A (en) * 2018-05-14 2018-10-23 福建农林大学 A kind of alginic acid alkali composite nitride carbon photocatalysis aerogel material and the preparation method and application thereof
CN111450865A (en) * 2020-04-28 2020-07-28 中山大学 Preparation method and application of catalyst for oxidative degradation of bisphenol A by sulfate radical
CN112246269A (en) * 2020-10-14 2021-01-22 吉林化工学院 C3N4-Cu2ZnSnS4Composite photocatalyst for photoreduction of Cr6+In (1)
CN113578368A (en) * 2021-08-29 2021-11-02 蚌埠学院 g-C3N4/Ag3PO4/BiFeO3Preparation method and application of composite visible-light-driven photocatalyst
CN114308097A (en) * 2021-12-06 2022-04-12 哈尔滨学院 Preparation method of nitrogen/bismuth ferrite-graphene composite material

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Cited By (15)

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CN107055492A (en) * 2016-10-09 2017-08-18 南京睿磐内尔环保复合新材料有限公司 A kind of directly synthesis g C3N4The method of Supporting cerium oxide nano composite material
CN107029773B (en) * 2017-03-14 2019-11-19 沃邦环保有限公司 Boron nitride-bismuth tungstate composite photocatalyst of degradating organic dye and preparation method thereof
CN107029773A (en) * 2017-03-14 2017-08-11 沃邦环保有限公司 Boron nitride bismuth tungstate composite photocatalyst of degradating organic dye and preparation method thereof
CN107930664A (en) * 2017-10-08 2018-04-20 南京邮电大学 One kind prepares BiFeO3/g‑C3N4The method of heterojunction photocatalyst
CN108246334A (en) * 2018-01-30 2018-07-06 中南林业科技大学 A kind of functionalization tri compound catalysis material and preparation method thereof and purposes
CN108246334B (en) * 2018-01-30 2021-04-09 中南林业科技大学 Functionalized ternary composite photocatalytic material and preparation method and application thereof
CN108144585A (en) * 2018-02-05 2018-06-12 中南林业科技大学 A kind of ternary magnetic composite for being used for heavy metal and dye wastewater treatment and preparation method thereof
CN108686697B (en) * 2018-05-14 2020-12-29 福建农林大学 Alginate-based composite carbon nitride photocatalytic aerogel material and preparation method and application thereof
CN108686697A (en) * 2018-05-14 2018-10-23 福建农林大学 A kind of alginic acid alkali composite nitride carbon photocatalysis aerogel material and the preparation method and application thereof
CN111450865A (en) * 2020-04-28 2020-07-28 中山大学 Preparation method and application of catalyst for oxidative degradation of bisphenol A by sulfate radical
CN111450865B (en) * 2020-04-28 2021-06-11 中山大学 Preparation method and application of catalyst for oxidative degradation of bisphenol A by sulfate radical
CN112246269A (en) * 2020-10-14 2021-01-22 吉林化工学院 C3N4-Cu2ZnSnS4Composite photocatalyst for photoreduction of Cr6+In (1)
CN113578368A (en) * 2021-08-29 2021-11-02 蚌埠学院 g-C3N4/Ag3PO4/BiFeO3Preparation method and application of composite visible-light-driven photocatalyst
CN113578368B (en) * 2021-08-29 2023-07-07 蚌埠学院 g-C 3 N 4 /Ag 3 PO 4 /BiFeO 3 Preparation method and application of composite visible light catalyst
CN114308097A (en) * 2021-12-06 2022-04-12 哈尔滨学院 Preparation method of nitrogen/bismuth ferrite-graphene composite material

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