CN114832842A - Bismuth oxybromide-lignin-based activated carbon composite photocatalyst and preparation method and application thereof - Google Patents
Bismuth oxybromide-lignin-based activated carbon composite photocatalyst and preparation method and application thereof Download PDFInfo
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- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 84
- 229920005610 lignin Polymers 0.000 title claims abstract description 74
- 229910052797 bismuth Inorganic materials 0.000 title claims abstract description 46
- JCXGWMGPZLAOME-UHFFFAOYSA-N bismuth atom Chemical compound [Bi] JCXGWMGPZLAOME-UHFFFAOYSA-N 0.000 title claims abstract description 44
- 239000002131 composite material Substances 0.000 title claims abstract description 43
- 239000011941 photocatalyst Substances 0.000 title claims abstract description 40
- 238000002360 preparation method Methods 0.000 title claims abstract description 24
- OZKCXDPUSFUPRJ-UHFFFAOYSA-N oxobismuth;hydrobromide Chemical compound Br.[Bi]=O OZKCXDPUSFUPRJ-UHFFFAOYSA-N 0.000 claims abstract description 34
- 150000001875 compounds Chemical class 0.000 claims abstract description 19
- 239000006185 dispersion Substances 0.000 claims abstract description 18
- 239000007788 liquid Substances 0.000 claims abstract description 17
- 239000012295 chemical reaction liquid Substances 0.000 claims abstract description 16
- 238000010438 heat treatment Methods 0.000 claims abstract description 15
- 238000001027 hydrothermal synthesis Methods 0.000 claims abstract description 14
- 150000001621 bismuth Chemical class 0.000 claims abstract description 13
- 239000002351 wastewater Substances 0.000 claims abstract description 12
- 238000004537 pulping Methods 0.000 claims abstract description 11
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 10
- 238000001354 calcination Methods 0.000 claims abstract description 9
- WKBOTKDWSSQWDR-UHFFFAOYSA-N Bromine atom Chemical class [Br] WKBOTKDWSSQWDR-UHFFFAOYSA-N 0.000 claims abstract description 7
- 239000003153 chemical reaction reagent Substances 0.000 claims abstract description 6
- 239000012266 salt solution Substances 0.000 claims abstract description 6
- 239000003610 charcoal Substances 0.000 claims abstract description 5
- 239000002270 dispersing agent Substances 0.000 claims abstract description 5
- 238000002156 mixing Methods 0.000 claims abstract description 3
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 16
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 16
- IOLCXVTUBQKXJR-UHFFFAOYSA-M potassium bromide Chemical compound [K+].[Br-] IOLCXVTUBQKXJR-UHFFFAOYSA-M 0.000 claims description 14
- 238000001035 drying Methods 0.000 claims description 11
- 238000006243 chemical reaction Methods 0.000 claims description 10
- JHJLBTNAGRQEKS-UHFFFAOYSA-M sodium bromide Chemical compound [Na+].[Br-] JHJLBTNAGRQEKS-UHFFFAOYSA-M 0.000 claims description 10
- 238000005406 washing Methods 0.000 claims description 8
- 238000001816 cooling Methods 0.000 claims description 7
- 229910052757 nitrogen Inorganic materials 0.000 claims description 7
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 claims description 6
- 239000007789 gas Substances 0.000 claims description 6
- 229920001732 Lignosulfonate Polymers 0.000 claims description 5
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 claims description 4
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims description 4
- 239000003513 alkali Substances 0.000 claims description 4
- 238000004043 dyeing Methods 0.000 claims description 4
- 235000019441 ethanol Nutrition 0.000 claims description 4
- 238000007639 printing Methods 0.000 claims description 4
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims description 3
- 229910017604 nitric acid Inorganic materials 0.000 claims description 3
- QYIGOGBGVKONDY-UHFFFAOYSA-N 1-(2-bromo-5-chlorophenyl)-3-methylpyrazole Chemical compound N1=C(C)C=CN1C1=CC(Cl)=CC=C1Br QYIGOGBGVKONDY-UHFFFAOYSA-N 0.000 claims description 2
- JHXKRIRFYBPWGE-UHFFFAOYSA-K bismuth chloride Chemical compound Cl[Bi](Cl)Cl JHXKRIRFYBPWGE-UHFFFAOYSA-K 0.000 claims description 2
- 229910000380 bismuth sulfate Inorganic materials 0.000 claims description 2
- BEQZMQXCOWIHRY-UHFFFAOYSA-H dibismuth;trisulfate Chemical compound [Bi+3].[Bi+3].[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O BEQZMQXCOWIHRY-UHFFFAOYSA-H 0.000 claims description 2
- RXPAJWPEYBDXOG-UHFFFAOYSA-N hydron;methyl 4-methoxypyridine-2-carboxylate;chloride Chemical compound Cl.COC(=O)C1=CC(OC)=CC=N1 RXPAJWPEYBDXOG-UHFFFAOYSA-N 0.000 claims description 2
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- PYWVYCXTNDRMGF-UHFFFAOYSA-N rhodamine B Chemical compound [Cl-].C=12C=CC(=[N+](CC)CC)C=C2OC2=CC(N(CC)CC)=CC=C2C=1C1=CC=CC=C1C(O)=O PYWVYCXTNDRMGF-UHFFFAOYSA-N 0.000 description 13
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- 229910052760 oxygen Inorganic materials 0.000 description 5
- 231100000719 pollutant Toxicity 0.000 description 5
- -1 polytetrafluoroethylene Polymers 0.000 description 5
- 229920001343 polytetrafluoroethylene Polymers 0.000 description 5
- 239000004810 polytetrafluoroethylene Substances 0.000 description 5
- 238000009210 therapy by ultrasound Methods 0.000 description 5
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- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 2
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 description 2
- 238000000026 X-ray photoelectron spectrum Methods 0.000 description 2
- 229910052794 bromium Inorganic materials 0.000 description 2
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- RSWGJHLUYNHPMX-UHFFFAOYSA-N 1,4a-dimethyl-7-propan-2-yl-2,3,4,4b,5,6,10,10a-octahydrophenanthrene-1-carboxylic acid Chemical compound C12CCC(C(C)C)=CC2=CCC2C1(C)CCCC2(C)C(O)=O RSWGJHLUYNHPMX-UHFFFAOYSA-N 0.000 description 1
- TUSDEZXZIZRFGC-UHFFFAOYSA-N 1-O-galloyl-3,6-(R)-HHDP-beta-D-glucose Natural products OC1C(O2)COC(=O)C3=CC(O)=C(O)C(O)=C3C3=C(O)C(O)=C(O)C=C3C(=O)OC1C(O)C2OC(=O)C1=CC(O)=C(O)C(O)=C1 TUSDEZXZIZRFGC-UHFFFAOYSA-N 0.000 description 1
- 239000001263 FEMA 3042 Substances 0.000 description 1
- LRBQNJMCXXYXIU-PPKXGCFTSA-N Penta-digallate-beta-D-glucose Natural products OC1=C(O)C(O)=CC(C(=O)OC=2C(=C(O)C=C(C=2)C(=O)OC[C@@H]2[C@H]([C@H](OC(=O)C=3C=C(OC(=O)C=4C=C(O)C(O)=C(O)C=4)C(O)=C(O)C=3)[C@@H](OC(=O)C=3C=C(OC(=O)C=4C=C(O)C(O)=C(O)C=4)C(O)=C(O)C=3)[C@H](OC(=O)C=3C=C(OC(=O)C=4C=C(O)C(O)=C(O)C=4)C(O)=C(O)C=3)O2)OC(=O)C=2C=C(OC(=O)C=3C=C(O)C(O)=C(O)C=3)C(O)=C(O)C=2)O)=C1 LRBQNJMCXXYXIU-PPKXGCFTSA-N 0.000 description 1
- 230000032900 absorption of visible light Effects 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 229910052786 argon Inorganic materials 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 238000010009 beating Methods 0.000 description 1
- 238000004061 bleaching Methods 0.000 description 1
- 239000001569 carbon dioxide Substances 0.000 description 1
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- 150000001805 chlorine compounds Chemical class 0.000 description 1
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- 239000001307 helium Substances 0.000 description 1
- 229910052734 helium Inorganic materials 0.000 description 1
- SWQJXJOGLNCZEY-UHFFFAOYSA-N helium atom Chemical compound [He] SWQJXJOGLNCZEY-UHFFFAOYSA-N 0.000 description 1
- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
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- 239000000463 material Substances 0.000 description 1
- VUZPPFZMUPKLLV-UHFFFAOYSA-N methane;hydrate Chemical compound C.O VUZPPFZMUPKLLV-UHFFFAOYSA-N 0.000 description 1
- QJGQUHMNIGDVPM-UHFFFAOYSA-N nitrogen group Chemical group [N] QJGQUHMNIGDVPM-UHFFFAOYSA-N 0.000 description 1
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- 150000002989 phenols Chemical class 0.000 description 1
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- 229920002258 tannic acid Polymers 0.000 description 1
- LRBQNJMCXXYXIU-NRMVVENXSA-N tannic acid Chemical compound OC1=C(O)C(O)=CC(C(=O)OC=2C(=C(O)C=C(C=2)C(=O)OC[C@@H]2[C@H]([C@H](OC(=O)C=3C=C(OC(=O)C=4C=C(O)C(O)=C(O)C=4)C(O)=C(O)C=3)[C@@H](OC(=O)C=3C=C(OC(=O)C=4C=C(O)C(O)=C(O)C=4)C(O)=C(O)C=3)[C@@H](OC(=O)C=3C=C(OC(=O)C=4C=C(O)C(O)=C(O)C=4)C(O)=C(O)C=3)O2)OC(=O)C=2C=C(OC(=O)C=3C=C(O)C(O)=C(O)C=3)C(O)=C(O)C=2)O)=C1 LRBQNJMCXXYXIU-NRMVVENXSA-N 0.000 description 1
- 229940033123 tannic acid Drugs 0.000 description 1
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- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J27/00—Catalysts comprising the elements or compounds of halogens, sulfur, selenium, tellurium, phosphorus or nitrogen; Catalysts comprising carbon compounds
- B01J27/06—Halogens; Compounds thereof
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- B01J35/00—Catalysts, in general, characterised by their form or physical properties
- B01J35/30—Catalysts, in general, characterised by their form or physical properties characterised by their physical properties
- B01J35/39—Photocatalytic properties
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- B01J37/00—Processes, in general, for preparing catalysts; Processes, in general, for activation of catalysts
- B01J37/08—Heat treatment
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
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- B01J37/08—Heat treatment
- B01J37/10—Heat treatment in the presence of water, e.g. steam
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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
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
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- C02F2103/00—Nature of the water, waste water, sewage or sludge to be treated
- C02F2103/26—Nature of the water, waste water, sewage or sludge to be treated from the processing of plants or parts thereof
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- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
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Abstract
The invention discloses a bismuth oxybromide-lignin-based activated carbon composite photocatalyst as well as a preparation method and application thereof, wherein the composite photocatalyst comprises lignin-based activated carbon and bismuth oxybromide loaded on the lignin-based activated carbon, and the preparation method comprises the following steps: dispersing bromine salt and lignin in a dispersing agent to obtain a dispersion liquid, and dissolving bismuth salt in an alcohol reagent to obtain a bismuth salt solution; adding the bismuth salt solution into the dispersion liquid and uniformly mixing to obtain a reaction liquid; pouring the reaction liquid into a hydrothermal kettle, and heating the hydrothermal kettle to perform hydrothermal reaction on the reaction liquid to obtain a bismuth oxybromide-charcoal compound; and calcining the bismuth oxybromide-charcoal compound to obtain the bismuth oxybromide-lignin-based activated carbon composite photocatalyst. The composite photocatalyst has good photocatalytic reaction performance, effectively utilizes byproduct lignin in the pulping and papermaking industry to treat wastewater in the pulping and papermaking industry, and realizes sustainable utilization of resources.
Description
Technical Field
The invention relates to the field of environmental materials, in particular to a bismuth oxybromide-lignin-based activated carbon composite photocatalyst, and a preparation method and application thereof, aiming at industrial wastewater of printing, dyeing, pulping, papermaking and the like.
Background
The rapid growth of the population and the development of industrialization have led to a wide distribution of organic and inorganic pollutants in aquatic ecosystems, particularly in the pulp and paper industry. During the pulping and papermaking process, the physicochemical properties and toxicity of the wastewater are affected by the process flow (e.g., beating, bleaching, etc. of the raw materials). The global pulping and papermaking market value in 2019 is about $ 5188.3 billion, and is growing at a rate of 3.45% per year. In the actual production process, although a large amount of water (5-100 cubic meters per ton of paper) and various lignocellulosic biomasses are consumed, 85% of the consumed water is returned to the environment without further treatment, causing serious environmental impact. These discharged wastewaters generally have the following characteristics: chemical Oxygen Demand (COD) (500-115000mg/L), lignin (11000-25000mg/L), tannic acid (2730mg/L), resin acid (3.2-550mg/L), phenols (17-800mg/L) and chlorides (13.9-38.5 mg/L).
Advanced Oxidation Processes (AOPs) have attracted considerable attention as an effective means of degrading various recalcitrant and toxic organic pollutants. AOPs can be exposed to external energy (e.g., electricity, Ultraviolet (UV) light and sound waves) or chemical oxidizing agents (O) 3 And H 2 O 2 ) In the presence of (2) induces the generation of Reactive Oxygen Species (ROS) (in particular hydroxyl (. OH) radicals, the oxidation potential of which is + 2.80V). But is clean and reproducible in useThe solar photocatalysis technology is one of effective ways for solving environmental problems such as water pollution and the like. BiOBr is a typical ternary p-type semiconductor, the minimum value of a Conduction Band (CBM) and the maximum value of a Valence Band (VBM) of the semiconductor are located at different positions, the forbidden band width is 2.7-2.9eV, the BiOBr is a narrow forbidden band semiconductor, the visible light response is good, and the photo-generated electron-hole separation efficiency is high. However, BiOBr has some disadvantages of poor adsorption performance, low quantum efficiency, rapid recombination of electron-hole pairs, and small specific surface area, which impair the performance of catalytic degradation. The method has the advantages that the method is an effective way for improving the separation efficiency of the photo-induced electron-hole pairs of the photocatalyst, the problem of the separation efficiency of the BiOBr photo-induced electron-hole pairs can be solved by doping the active carbon, the concentration of pollutants around the photocatalyst can be improved, and the reaction speed is increased. The lignin is used as a byproduct in the pulp and paper industry, is low in price, easy to degrade and low in toxicity, and can be used for producing activated carbon. At present, no relevant report for preparing the bismuth oxybromide-lignin-based activated carbon composite photocatalyst by combining BiOBr and lignin-based activated carbon exists.
Disclosure of Invention
Aiming at the problems in the prior art, the invention aims to provide a bismuth oxybromide-lignin-based activated carbon composite photocatalyst, and a preparation method and application thereof, so as to enhance the photocatalytic effect of bismuth oxybromide (BiOBr), recover byproducts of pulping and papermaking, realize the effective utilization of resources, and apply the bismuth oxybromide-lignin-based activated carbon composite photocatalyst to the actual wastewater treatment.
In order to achieve the purpose, the invention adopts the technical scheme that:
the first purpose of the invention is to provide a preparation method of the bismuth oxybromide-lignin-based activated carbon composite photocatalyst, which comprises the following steps:
dispersing bromine salt and lignin in a dispersing agent to obtain a dispersion liquid, and dissolving bismuth salt in an alcohol reagent to obtain a bismuth salt solution; adding the bismuth salt solution into the dispersion liquid and uniformly mixing to obtain a reaction liquid; pouring the reaction liquid into a hydrothermal kettle, heating the hydrothermal kettle to perform hydrothermal reaction, cooling to room temperature after the reaction is finished, separating, washing and heating the obtained product at 50-60 DEG CVacuum drying at the temperature to obtain a bismuth oxybromide-charcoal compound; the main chemical reactions involved in the hydrothermal reaction process are as follows: bi and O in the reaction solution are linked by a covalent bond to form [ Bi 2 O 2 ]And forming a BiOBr laminated structure with the double Br layer, wherein the lignin is changed into biochar (biochar) through a hydrothermal reaction, and the BiOBr grows on the biochar to obtain the bismuth oxybromide-biochar compound.
And (3) placing the bismuth oxybromide-biochar compound in a tubular furnace, introducing nitrogen gas for calcination treatment, and further carbonizing the biochar to obtain Activated Carbon (AC), thereby obtaining the bismuth oxybromide-Lignin-based activated carbon (BiOBr/Lignin-AC) composite photocatalyst. The nitrogen gas may be replaced by an inert gas such as helium gas or argon gas, and these gases have the same function as nitrogen gas and all cause carbonization of the reactant in an oxygen-free atmosphere.
Preferably, the molar ratio of the bismuth salt to the bromine salt is 1: 1-1: 2.
Preferably, the dispersant is water, nitric acid or sulfuric acid; the alcohol reagent is absolute ethyl alcohol, ethylene glycol or isopropanol.
Preferably, the temperature of the hydrothermal reaction is 130-230 ℃, and the time is 24-48 h.
Preferably, the gas environment for the calcination treatment is nitrogen, the temperature is 400-700 ℃, and the time is 1-5 h.
Preferably, the lignin is at least one of alkali lignin and lignosulfonate; the bismuth salt is any one of bismuth nitrate, bismuth sulfate, bismuth chloride or bismuth acetate; the bromine salt is any one of potassium bromide and sodium bromide.
Preferably, the mass of lignin in the bismuth oxybromide-biochar composite is 1 wt% -10 wt% of the mass of the bismuth oxybromide.
The invention has the second aim of providing the bismuth oxybromide-lignin-based activated carbon composite photocatalyst, which is prepared by the preparation method in the first aim.
The third purpose of the invention is to provide the application of the bismuth oxybromide-lignin-based activated carbon composite photocatalyst as in the second purpose in treating wastewater under visible light. Further preferably, the wastewater is printing and dyeing wastewater or pulping and papermaking wastewater.
Compared with the prior art, the invention has the following advantages:
(1) the BiOBr/Lignin-AC composite photocatalyst prepared by the invention effectively utilizes byproduct Lignin in the pulping and papermaking industry to treat wastewater in the pulping and papermaking industry, and realizes sustainable utilization of resources.
(2) The BiOBr/Lignin-AC composite photocatalyst prepared by the method overcomes the defects of poor adsorption performance, low quantum efficiency, rapid recombination of electron-hole pairs, small specific surface area and the like of BiOBr, improves the concentration of pollutants around the catalyst, and enhances the photocatalytic reaction performance of the catalyst.
(3) The activated carbon formed by calcining lignin by a hydrothermal method has large specific surface area, more pores and obvious adsorption effect on pollutants, the pollutants can be quickly enriched around the catalyst, and the composite catalyst formed by calcining has better stability and recoverability.
Drawings
FIG. 1 is an XRD pattern of BiOBr and BiOBr/Lignin-AC;
FIG. 2 is a scanning electron microscope photograph of BiOBr (a), AC (b) and F-BiOBr/1 wt% Lignin (c-d),
FIG. 3 is an X-ray energy spectrum (EDS) of BiOBr/2 wt% Lignin;
FIG. 4 is a high resolution XPS spectrum (a-d) of Br, Bi, O and C elements for F-BiOBr/1 wt% Lignin.
Detailed Description
The present invention will be further described with reference to the following examples so that those skilled in the art can better understand the present invention and can practice the present invention, but the examples are not intended to limit the present invention. The starting materials or reagents used in the following examples are all commercially available products.
Example 1:
putting 1g of alkali lignin into a beaker, and drying the alkali lignin in an oven at 40 ℃ for 30 minutesStandby; 4mmol of Bi (NO) 3 ) 3 ·5H 2 Dissolving O in 30mL of absolute ethyl alcohol, and uniformly stirring by ultrasonic waves to obtain Bi (NO) 3 ) 3 ·5H 2 O solution; respectively adding 4mmol of KBr and 0.0122g of lignin into 20ml of distilled water, and uniformly stirring to obtain a dispersion liquid; then Bi (NO) 3 ) 3 ·5H 2 Adding the O solution into a dispersion liquid containing KBr and lignin, carrying out ultrasonic treatment for 30min, and then carrying out vigorous stirring for 30min to obtain a reaction liquid; pouring the reaction liquid into a 100mL stainless steel water heating kettle with a polytetrafluoroethylene lining, and placing the stainless steel water heating kettle in an oven to be heated for 24 hours at 160 ℃ to carry out hydrothermal reaction; after the reaction is finished, separating, washing and drying the obtained product in sequence to obtain a bismuth oxybromide-biochar compound; putting the bismuth oxybromide-biochar compound into a tubular furnace, heating the tubular furnace at the speed of 5 ℃/min in a nitrogen environment to 550 ℃, keeping the temperature of the bismuth oxybromide-biochar compound at 550 ℃ for 3 hours, and naturally cooling to obtain the F-BiOBr/1 wt% Lignin-AC composite photocatalyst, which is marked as F-BL1, wherein 1 wt% represents the mass percentage of Lignin raw materials used in the preparation of F-BL1 in the BiOBr of a target product (the same below).
Comparative example 1
Compared with example 1, in comparative example 1, the addition amount of lignin in the preparation of the dispersion was 0g, i.e., no lignin was added, and the BiOBr photocatalyst, denoted as F-BiOBr, was obtained without calcination in a tube furnace.
Comparative example 2
Adding 0.0122g of lignin into 20ml of distilled water, and uniformly stirring to obtain a dispersion liquid; carrying out ultrasonic treatment on the dispersion liquid for 30min, then carrying out vigorous stirring for 30min, pouring the dispersion liquid into a 100mL stainless steel hot kettle with a polytetrafluoroethylene lining, and placing the kettle in an oven to heat for 24h at 160 ℃ to carry out hydrothermal reaction; after the reaction is finished, separating, washing and drying the obtained product in sequence to obtain biochar; putting the biochar into a tube furnace, heating the tube furnace to 550 ℃ at the speed of 5 ℃/min in a nitrogen environment, preserving the temperature of the biochar at 550 ℃ for 3 hours, and naturally cooling to obtain the lignin-based Activated Carbon (AC).
Example 2 to example 4
Compared with example 1, examples 2 to 4 are different in the addition amount of lignin, and the other processes are the same as example 1, and the addition amounts of lignin in examples 2 to 4 are respectively as follows: 0.0244g, 0.0488g, 0.0976 g; the products obtained in examples 2 to 4 were identified as F-BiOBr/2 wt% Lignin-AC (F-BL2), F-BiOBr/4 wt% Lignin-AC (F-BL4), F-BiOBr/8 wt% Lignin-AC (F-BL8), respectively.
Photocatalytic Performance test
The photocatalysts prepared in examples 1 to 4 and the comparative example were respectively subjected to a photocatalytic performance test by the following methods: adding 50mg of photocatalyst into 250mL of 30mg/L rhodamine B solution, irradiating by using a 300wXe lamp (a cut-off filter with the wavelength of 420 nanometers is arranged at the outlet of a light source), and testing the degradation rate of the rhodamine B after 1 hour. The results are shown in Table 1 below.
TABLE 1 degradation rate of rhodamine B by the photocatalysts prepared in examples 1-4 and comparative example
From table 1, it can be seen that the catalytic performance of the calcined composite catalyst is improved, and the catalytic effect is first enhanced and then weakened with the increase of the lignin doping amount, wherein the catalytic effect of F-BL1 is strongest.
F-BiOBr/1 wt% Lignin-AC subjected to a catalytic performance test is centrifugally separated from the rhodamine B solution and taken out, after washing and drying, the F-BiOBr/1 wt% Lignin-AC is used for treating 250mL of 30mg/L rhodamine B solution in the same environment repeatedly for three times, a 300wXe lamp (a cut-off filter of 420 nanometers is arranged at the outlet of a light source) is used for irradiating, and the degradation rate of the rhodamine B after 1 hour is shown in the following table 2:
TABLE 2 degradation rate of rhodamine B after repeated three times of use of F-BiOBr/1 wt% Lignin-Biochar
From table 2, it can be seen that the catalytic effect of the catalyst is still significant after three cycles, indicating that the catalyst has good stability and repeatability.
Example 5
And (3) putting 1g of lignosulfonate into a beaker, and drying in a drying oven at 40 ℃ for 30 minutes to obtain the lignin. 4mmol of BiCl 3 Dissolving the mixture in 30mL of absolute ethyl alcohol, and uniformly stirring the mixture by ultrasonic waves to obtain BiCl 3 A solution; adding 4mmol of KBr and 0.122g of lignin into 20ml of distilled water, and uniformly stirring to obtain a dispersion liquid; then adding BiCl 3 Adding the solution into a dispersion liquid containing NaBr and lignin, carrying out ultrasonic treatment for 30min, and then carrying out vigorous stirring for 30min to obtain a reaction liquid; pouring the reaction liquid into a 100mL stainless steel water heating kettle with a polytetrafluoroethylene lining, and placing the stainless steel water heating kettle in an oven to be heated for 48 hours at 230 ℃ to carry out hydrothermal reaction; after the reaction is finished, separating, washing and drying the obtained product in sequence to obtain a bismuth oxybromide-biochar compound; and (2) putting the bismuth oxybromide-biochar compound into a tubular furnace, heating the tubular furnace to 400 ℃ at the speed of 5 ℃/min in a nitrogen environment, keeping the temperature of the bismuth oxybromide-biochar compound at 400 ℃ for 3 hours, and naturally cooling to obtain the F-BiOBr/10 wt% Lignin-AC composite photocatalyst, which is marked as F-BL 10.
Adding 50mg of F-BiOBr/10 wt% Lignin-AC composite photocatalyst into 250mL of 30mg/L rhodamine B solution, and irradiating by using a 300wXe lamp (a cut-off filter with the wavelength of 420 nanometers is arranged at the outlet of a light source), wherein the degradation rate of rhodamine B is 49.13% after 1 h.
Example 6
The lignin was prepared as in example 1. 2mmol of Bi 2 (SO 4 ) 3 Dissolving the Bi in 30mL of absolute ethyl alcohol and uniformly stirring by ultrasonic waves to obtain Bi 2 (SO 4 ) 3 A solution; adding 4mmol of NaBr and 0.0488g g lignin into 20ml of distilled water, and uniformly stirring to obtain a dispersion liquid; then Bi is added 2 (SO 4 ) 3 Adding the solution into a dispersion liquid containing NaBr and lignin, carrying out ultrasonic treatment for 30min, and then carrying out vigorous stirring for 30min to obtain a reaction liquid; pouring the reaction liquid into a 100mL stainless steel water heating kettle with a polytetrafluoroethylene lining, and placing the kettle in an oven to be heated for 48 hours at 160 ℃ to carry out hydrothermal reaction; reaction ofAfter the reaction is finished, sequentially separating, washing and drying the obtained product to obtain a bismuth oxybromide-biochar compound; and (2) putting the bismuth oxybromide-biochar compound into a tubular furnace, heating the tubular furnace to 400 ℃ at the speed of 5 ℃/min in a nitrogen environment, keeping the temperature of the bismuth oxybromide-biochar compound at 400 ℃ for 1 hour, and naturally cooling to obtain the F-BiOBr/4 wt% Lignin-AC composite photocatalyst.
50mg of F-BiOBr/4 wt% of Lignin-AC composite catalyst is added into 250mL of 30mg/L rhodamine B solution, a 300wXe lamp (a cut-off filter with the wavelength of 420 nanometers is arranged at the outlet of a light source) is used for irradiation, and the degradation rate of rhodamine B is 64.78% after 1 hour.
Example 7
The lignin was prepared as in example 1. 4mmol of Bi (NO) 3 ) 3 ·5H 2 Dissolving O in 30mL nitric acid, and ultrasonically stirring uniformly to obtain Bi (NO) 3 ) 3 ·5H 2 O solution; adding 4mmol of KBr and 0.0976g of lignin into 20ml of distilled water, and uniformly stirring to obtain a dispersion liquid; then Bi (NO) 3 ) 3 ·5H 2 Adding the O solution into a dispersion liquid containing KBr and lignin, carrying out ultrasonic treatment for 30min, and then carrying out vigorous stirring for 30min to obtain a reaction liquid; pouring the reaction liquid into a 100mL stainless steel water heating kettle with a polytetrafluoroethylene lining, and placing the kettle in an oven to be heated for 12 hours at 160 ℃ to carry out hydrothermal reaction; after the reaction is finished, separating, washing and drying the obtained product in sequence to obtain a bismuth oxybromide-biochar compound; and (2) putting the bismuth oxybromide-biochar compound into a tubular furnace, heating the tubular furnace to 550 ℃ at the speed of 5 ℃/min in a nitrogen environment, keeping the temperature of the bismuth oxybromide-biochar compound at 550 ℃ for 3 hours, and naturally cooling to obtain the F-BiOBr/8 wt% Lignin-AC composite photocatalyst.
50mg of F-BiOBr/8 wt% of Lignin-AC composite catalyst is added into 250mL of 30mg/L rhodamine B solution, a 300wXe lamp (a cut-off filter with the wavelength of 420 nanometers is arranged at the outlet of a light source) is used for irradiation, and the degradation rate of rhodamine B is 56.34% after 1 hour.
Material characterization
As shown in fig. 1, we performed XRD characterization of the catalyst in order to study the crystalline phase and structure of BiOBr and its composites. Fig. 1 shows that all samples showed similar diffraction peaks in the X-ray diffraction pattern, indicating that all samples were highly pure crystals without impurity peaks. All diffraction peaks of the sample obtained by hydrothermal reaction and calcination treatment are matched with quadrilateral crystal JCPDF No. 09-0393. At 10.90 °, 21.93 °, 25.16 °, 31.69 °, 32.22 °, 39.38 °, 44.69 °, 46.21 °, 50.67 °, 53.38 °, 57.12 °, 61.90 °, 67.40 °, 71. At 00 ° and 76.70 °, diffraction peaks correspond to the crystal planes of (001), (002), (101), (102), (110), (112), (004), (200), (104), (211), (212), (105), (220), (214) and (310), respectively. The diffraction peak intensities for all of the composite catalysts prepared in examples 1 through 5 of figure 1 were significantly reduced compared to the pure BiOBr prepared by the comparative example, indicating that the addition of lignin-based activated carbon may cause lattice defects in the BiOBr. The XRD patterns of F-BL10 and F-BL8 showed several new diffraction peaks between 30 ° and 40 °, indicating that lignin was converted to activated carbon with a graphitic structure. While other samples did not have these diffraction peaks, which may be due to the low lignin content in the composite. This also indicates that there is some interaction between the BiOBr crystals and the lignin-based activated carbon structure.
FIG. 2 is a scanning electron microscope photograph of BiOBr (a), AC (b) and F-BiOBr/1 wt% Lignin (c-d). In fig. 2a and 2b, SEM images of pure BiOBr and AC respectively, it can be seen that BiOBr is a layered structure with a smooth surface and a size distribution between 500nm and 1 μm. The lignin-based Activated Carbon (AC) is a block structure with a rough surface. Fig. 2c and 2d are SEM images of F-BiOBr/1 wt% Lignin-AC composite photocatalyst at different magnifications, and it can be seen that BiOBr is uniformly dispersed on Lignin-based activated carbon, grows in all directions, forms a three-dimensional layered structure, and the thickness of each layer of the BiOBr of the composite catalyst is reduced, which allows the BiOBr to expose more active sites, increasing the chance of contact between it and reactant molecules. And simultaneously performing EDS (electron-dispersive spectroscopy) energy spectrum analysis on F-BiOBr/1 wt% Lignin (F-BL1), as shown in figure 3, as can be seen from figure 3, F-BL1 contains Br, Bi, O and C elements, and further proves that BiOBr successfully and uniformly disperses and grows on the surface of the Lignin-based activated carbon.
In order to analyze the element composition and the valence state of each element in F-BiOBr/1 wt% Lignin (F-BL1), an X-ray photoelectron energy spectrum is used for characterization, and FIG. 4 is an XPS spectrum of each element of F-BL 1. From the spectrum of Br 3d in FIG. 4a, it can be seen that there are two strong peaks of spin-orbit splitting energy at 68.39eV and 69.41eV, respectively, which are associated with Br 3d 5/ 2 and Br 3d 3/2 It is related. And the Bi 4f spectrum of 4b has two independent symmetrical peaks at 159.37 and 16468eV, which belong to Bi 4f 7/2 And Bi 4f 5/2 . The O1s peak of F-BL1 (FIG. 4c) was split into two peaks at 530.06 and 530.55eV, which are associated with the lattice O atom (Bi-O bond) and the surface-OH, respectively. The peak at 530.85eV may be due to physical absorption of carbon dioxide and water molecules. The binding energy of C1s (fig. 4d) of F-BL1 at 284.84, 286.64, 289.11eV matches the C-C, C-O, C ═ O bond, respectively. While the peak binding energy at 294.64eV may be due to satellite jitter caused by vacuum contamination. The peaks of C1s were very uneven due to the lower amount of lignin doping.
In conclusion, the BiOBr/Lignin-AC photocatalyst prepared by the method can accelerate the separation of photoproduction electrons and holes, improve the absorption of visible light and the concentration of pollutants around the catalyst, enhance the photocatalytic reaction performance, has stable property and high recycling efficiency, and has good effect on treatment of industrial wastewater of printing and dyeing, pulping, papermaking and the like.
Claims (10)
1. A preparation method of a bismuth oxybromide-lignin-based activated carbon composite photocatalyst is characterized by comprising the following steps: dispersing bromine salt and lignin in a dispersing agent to obtain a dispersion liquid, and dissolving bismuth salt in an alcohol reagent to obtain a bismuth salt solution; adding the bismuth salt solution into the dispersion liquid and uniformly mixing to obtain a reaction liquid; pouring the reaction liquid into a hydrothermal kettle, heating the hydrothermal kettle to perform hydrothermal reaction on the reaction liquid, cooling to room temperature after the reaction is finished, and sequentially separating, washing and drying the obtained product to obtain a bismuth oxybromide-biochar compound; and (3) placing the bismuth oxybromide-charcoal compound in protective gas for calcination treatment, namely the bismuth oxybromide-lignin-based activated carbon composite photocatalyst.
2. The preparation method of the bismuth oxybromide-lignin-based activated carbon composite photocatalyst as claimed in claim 1, wherein the preparation method comprises the following steps: the molar ratio of the bismuth salt to the bromine salt is 1: 1-1: 2.
3. The preparation method of the bismuth oxybromide-lignin-based activated carbon composite photocatalyst as claimed in claim 1, wherein the preparation method comprises the following steps: the dispersant is water, nitric acid or sulfuric acid; the alcohol reagent is absolute ethyl alcohol, ethylene glycol or isopropanol.
4. The preparation method of the bismuth oxybromide-lignin-based activated carbon composite photocatalyst as claimed in claim 1, wherein the preparation method comprises the following steps: the temperature of the hydrothermal reaction is 130-230 ℃, and the time is 24-48 h.
5. The preparation method of the bismuth oxybromide-lignin-based activated carbon composite photocatalyst as claimed in claim 1, wherein the preparation method comprises the following steps: the protective gas is nitrogen or inert gas; the temperature of the calcination treatment is 400-700 ℃, and the time is 1-5 h.
6. The preparation method of the bismuth oxybromide-lignin-based activated carbon composite photocatalyst as claimed in claim 1, wherein the preparation method comprises the following steps: the lignin is at least one of alkali lignin and lignosulfonate; the bismuth salt is any one of bismuth nitrate, bismuth sulfate, bismuth chloride or bismuth acetate; the bromine salt is any one of potassium bromide and sodium bromide.
7. The preparation method of the bismuth oxybromide-lignin-based activated carbon composite photocatalyst as claimed in claim 1, wherein the preparation method comprises the following steps: the mass of the lignin in the bismuth oxybromide-charcoal composite is 1 wt% -10% of the mass of the bismuth oxybromide.
8. A bismuth oxybromide-lignin-based activated carbon composite photocatalyst is characterized in that: the bismuth oxybromide-lignin-based activated carbon composite photocatalyst is prepared by the preparation method of any one of claims 1 to 7.
9. The use of a bismuth oxybromide-lignin-based activated carbon composite photocatalyst as claimed in claim 8 for the treatment of wastewater under visible light.
10. Use according to claim 9, characterized in that: the waste water is printing and dyeing waste water or pulping and papermaking waste water.
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