CN112044430A - Novel lignin carbon/bismuth tungstate composite material for photocatalytic degradation of methylene blue and preparation method thereof - Google Patents
Novel lignin carbon/bismuth tungstate composite material for photocatalytic degradation of methylene blue and preparation method thereof Download PDFInfo
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- 229920005610 lignin Polymers 0.000 title claims abstract description 41
- 239000002131 composite material Substances 0.000 title claims abstract description 36
- 238000002360 preparation method Methods 0.000 title claims abstract description 18
- RBTBFTRPCNLSDE-UHFFFAOYSA-N 3,7-bis(dimethylamino)phenothiazin-5-ium Chemical compound C1=CC(N(C)C)=CC2=[S+]C3=CC(N(C)C)=CC=C3N=C21 RBTBFTRPCNLSDE-UHFFFAOYSA-N 0.000 title claims abstract description 16
- 229960000907 methylthioninium chloride Drugs 0.000 title claims abstract description 16
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 13
- 229910052799 carbon Inorganic materials 0.000 title claims abstract description 13
- 229910052797 bismuth Inorganic materials 0.000 title claims abstract description 12
- JCXGWMGPZLAOME-UHFFFAOYSA-N bismuth atom Chemical compound [Bi] JCXGWMGPZLAOME-UHFFFAOYSA-N 0.000 title claims abstract description 12
- PBYZMCDFOULPGH-UHFFFAOYSA-N tungstate Chemical compound [O-][W]([O-])(=O)=O PBYZMCDFOULPGH-UHFFFAOYSA-N 0.000 title claims abstract description 12
- 238000013033 photocatalytic degradation reaction Methods 0.000 title abstract description 7
- 230000001699 photocatalysis Effects 0.000 claims abstract description 10
- 238000007146 photocatalysis Methods 0.000 claims abstract description 6
- 230000000593 degrading effect Effects 0.000 claims abstract description 5
- 239000003513 alkali Substances 0.000 claims description 29
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 21
- 238000006243 chemical reaction Methods 0.000 claims description 19
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 17
- 238000003756 stirring Methods 0.000 claims description 15
- 238000001354 calcination Methods 0.000 claims description 14
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 13
- 239000000243 solution Substances 0.000 claims description 13
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 claims description 12
- 239000008367 deionised water Substances 0.000 claims description 11
- 229910021641 deionized water Inorganic materials 0.000 claims description 11
- 239000000843 powder Substances 0.000 claims description 11
- 239000002243 precursor Substances 0.000 claims description 10
- 238000001035 drying Methods 0.000 claims description 9
- 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 8
- 238000000034 method Methods 0.000 claims description 8
- XMVONEAAOPAGAO-UHFFFAOYSA-N sodium tungstate Chemical compound [Na+].[Na+].[O-][W]([O-])(=O)=O XMVONEAAOPAGAO-UHFFFAOYSA-N 0.000 claims description 8
- MPNXSZJPSVBLHP-UHFFFAOYSA-N 2-chloro-n-phenylpyridine-3-carboxamide Chemical compound ClC1=NC=CC=C1C(=O)NC1=CC=CC=C1 MPNXSZJPSVBLHP-UHFFFAOYSA-N 0.000 claims description 7
- 238000010438 heat treatment Methods 0.000 claims description 7
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Abstract
A novel lignin carbon/bismuth tungstate composite material for degrading methylene blue by photocatalysis and a preparation method thereof relate to a novel lignin carbon/bismuth tungstate composite material for degrading methylene blue by photocatalysis and a preparation method thereof. The invention discloses a preparation method of a novel lignin carbon/bismuth tungstate composite material, and aims to find a novel composite material and provide a preparation method of the novel lignin carbon/bismuth tungstate composite material. And the photocatalytic performance of the composite material is researched. Research shows that the photocatalytic degradation efficiency of the composite material to methylene blue can reach 99.1% after 2.5 hours, and is 1.1 times of that of single bismuth tungstate.
Description
Technical Field
The invention relates to a novel lignin carbon/bismuth tungstate composite material for degrading methylene blue by photocatalysis and a preparation method thereof.
Background
In the long-term development of human society, environmental pollution not only threatens public health, but also is a main problem facing water quality safety in China. In the production activities of people, such as leather making, spinning, printing and dyeing, plastic processing and other industries, a large amount of industrial wastewater with organic dyes (such as methylene blue) can be generated, so that water pollution is caused, and animal and plant genes in water are mutated; in human beings, even at very low concentrations, the health and safety of human beings are greatly threatened, such as human body distortion, gene mutation, cancer and the like. Therefore, many techniques for removing contaminants from water have been discovered to treat environmental pollution problems, such as chemical precipitation, ion exchange, biological treatment, adsorption, and photocatalytic degradation. Among them, for photocatalytic degradation, a high-efficiency photocatalyst is effective for removing organic pollutants in water, and has been widely noticed due to its low cost and high efficiency. Therefore, the development of efficient visible light-driven photocatalytic degradation catalyst is a unique driving force in the field of photocatalytic degradation.
Bismuth tungstate (Bi)2WO6) Is a typical n-type semiconductor with a forbidden band width of 2.75 eV. It is prepared from Bi2O2 2+Layer and WO4 2-The perovskite lamellar structure formed by the layers along the c axis in an alternating mode belongs to an orthorhombic system. The layered structure of the material makes the material possess unique physical and chemical properties, and thus has wide application in ferroelectric, piezoelectric, catalytic and other fields. Especially in the aspect of photocatalysis, Bi2WO6As a novel photocatalytic material, the photocatalytic material has the advantages of narrow band gap, high photochemical stability, strong oxidation capacity, low manufacturing cost, easy excitation under the irradiation of visible light, high utilization rate of solar energy, high efficient organic matter degradation capacity, high catalytic activity and the like, so that the photocatalytic material is attracted by researchers.
In addition, industrial lignin is a main byproduct in the paper making and biorefinery industries, the annual output is about 5000 ten thousand tons, and due to the complex chemical structure, the high separation difficulty and the high cost and the very low high-valued utilization rate, most of the lignin is not effectively recycled and is directly discharged into a water body, so that the serious pollution of the water environment is caused. Thus, the high value application of industrial lignin is resource-recyclingThe ring utilization, environmental protection and new material development are of great significance. The invention develops a new material for alkali lignin, synthesizes a novel lignin carbon/bismuth tungstate (LC/Bi)2WO6) The research on the photocatalytic performance of the composite material shows that the photodegradation efficiency of the composite material to methylene blue can reach 99.1 percent after 2.5 hours, and is 1.1 times of that of single bismuth tungstate.
Disclosure of Invention
The invention aims to find an LC/Bi for degrading methylene blue by photocatalysis2WO6A novel composite material and a preparation method thereof, thereby providing an LC/Bi2WO6A method for preparing a novel composite material. The method has simple and effective preparation process, low reagent consumption and high yield.
The invention provides an LC/Bi2WO6The preparation method of the novel composite material is carried out according to the following steps:
(1) activating alkali lignin, using alkali lignin as a carbon source to activate the alkali lignin, dissolving a certain amount of alkali lignin in a sodium hydroxide solution under the condition of stirring, adding a certain amount of trimethyl ammonium chloride, raising the temperature, heating and stirring for a period of time, putting the product into a dialysis bag to dialyze until the product is neutral, drying and grinding to obtain quaternized alkali lignin powder.
The adding amount of the alkali lignin in the step (1) is 10 g;
the mass fraction of the sodium hydroxide solution in the step (1) is 20 percent;
the adding amount of the trimethyl ammonium chloride in the step (1) is 9 g;
the temperature rise temperature in the step (1) is 85 +/-5 ℃.
And (2) heating and stirring for 3-4 h.
(2) Under the condition of stirring, dissolving a certain amount of bismuth nitrate, sodium tungstate and the product obtained in the step (1) in a mixed solution of ethylene glycol and deionized water in sequence;
the adding amount of the bismuth nitrate in the step (2) is 0.73 g;
the adding amount of the sodium tungstate in the step (2) is 0.25 g;
the product obtained in the step (1) in the step (2) is activated alkali lignin powder, and the addition amount is 0g and 0.1 g;
the volume of the ethanol solution in the step (2) is 20ml, and the volume of the deionized water is 15 ml.
(3) Transferring the reaction system obtained in the step (2) into a reaction kettle, placing the reaction kettle into an oven, reacting for a period of time at a certain temperature, naturally cooling to room temperature, washing with deionized water and absolute ethyl alcohol for three times respectively, centrifugally separating, and drying to obtain a product precursor;
the reaction conditions in the step (3) are as follows: the reaction is carried out for 24h at 160 ℃.
(4) And (4) transferring the product precursor obtained in the step (3) into a magnetic boat, placing the magnetic boat in a tube furnace for calcination, and calcining at a certain temperature for a period of time to obtain a product.
The calcining conditions in the step (4) are as follows: calcining at 550 ℃ for 2 h.
The invention has the beneficial effects that:
the invention adopts a solvothermal method, takes alkali lignin, bismuth nitrate and sodium tungstate as raw materials to synthesize a product precursor, and calcines the product precursor to obtain LC/Bi2WO6Novel composite materials. The method has simple and effective preparation process, low reagent consumption and high yield.
Drawings
FIG. 1 shows LC/Bi2WO6X-ray powder diffraction patterns of the novel composite materials;
FIG. 2 shows LC/Bi2WO6Fourier infrared spectrogram of the novel composite material;
FIG. 3 shows LC/Bi2WO6Light degradation pattern of novel composite material to methylene blue.
Detailed Description
The invention is further illustrated by the following examples, which are merely illustrative of the process of the invention and are not intended to limit the scope of the invention in any way.
Detailed description of the invention: LC/Bi of the present embodiment2WO6The preparation method of the novel composite material is completed according to the following steps:
(1) activating alkali lignin, namely activating the alkali lignin by taking the alkali lignin as a carbon source, dissolving a certain amount of alkali lignin in a sodium hydroxide solution, stirring, adding a certain amount of trimethyl ammonium chloride, raising the temperature, heating and stirring for a period of time, putting the product into a dialysis bag, dialyzing until the product is neutral, drying and grinding to obtain activated alkali lignin powder.
The adding amount of the alkali lignin in the step (1) is 10 g;
the mass fraction of the sodium hydroxide solution in the step (1) is 20 percent;
the adding amount of the trimethyl ammonium chloride in the step (1) is 9 g;
the temperature rise temperature in the step (1) is 85 +/-5 ℃;
and (2) heating and stirring for 3-4 h.
(2) Under the condition of stirring, dissolving a certain amount of bismuth nitrate, sodium tungstate and the alkali lignin powder activated in the step (1) in a mixed solution of ethylene glycol and deionized water in sequence;
the adding amount of the bismuth nitrate in the step (2) is 0.73 g;
the adding amount of the sodium tungstate in the step (2) is 0.25 g;
the adding amount of the activated alkali lignin powder in the step (2) is 0g and 0.1 g;
the volume of the ethanol solution in the step (2) is 20ml, and the volume of the deionized water is 15 ml.
(3) Transferring the reaction system obtained in the step (2) into a reaction kettle, placing the reaction kettle into an oven, reacting for a period of time at a certain temperature, naturally cooling to room temperature, washing with deionized water and absolute ethyl alcohol for three times respectively, performing centrifugal separation, and drying to obtain a product precursor;
the reaction conditions in the step (3) are as follows: the reaction is carried out for 24h at 160 ℃.
(4) And (4) transferring the product precursor obtained in the step (3) into a magnetic boat, placing the magnetic boat in a tube furnace for calcination, and calcining at a certain temperature for a period of time to obtain a product.
The calcining conditions in the step (4) are as follows: calcining at 550 ℃ for 2 h.
The second embodiment is as follows: the first difference between the present embodiment and the specific embodiment is: the addition amount of the activated alkali lignin powder in the step (2) is 0g, and other steps and parameters are the same as those in the first specific embodiment;
the third concrete implementation mode: the present embodiment differs from the first or second embodiment in that: the addition amount of the activated alkali lignin powder in the step (2) is 0.1g, and other steps and parameters are the same as those in the first specific embodiment;
the following examples are given to illustrate the present invention, and the following examples are carried out on the premise of the technical solution of the present invention, and give detailed embodiments and specific procedures, but the scope of the present invention is not limited to the following examples.
Example 1: LC/Bi2WO6The preparation method of the novel composite material is completed according to the following steps:
(1) dissolving 10g of alkali lignin into a sodium hydroxide solution with the mass fraction of 20% under the stirring condition, adding 9g of trimethyl ammonium chloride, raising the temperature to 85 +/-5 ℃, heating and stirring for 3-4 h, putting the product into a dialysis bag, dialyzing until the product is neutral, drying and grinding to obtain activated alkali lignin powder.
(2) And (2) sequentially dissolving 0.73g of bismuth nitrate, 0.25g of sodium tungstate and 0.1g of activated alkali lignin powder obtained in the step (1) into a mixed solution of 20ml of ethylene glycol and 15ml of deionized water under the condition of stirring.
(3) And (3) transferring the reaction system obtained in the step (2) into a reaction kettle, placing the reaction system into an oven, reacting for 24 hours at 160 ℃, naturally cooling to room temperature, washing with deionized water and absolute ethyl alcohol for three times respectively, performing centrifugal separation, and drying to obtain a product precursor.
(4) And (4) transferring the product precursor obtained in the step (3) into a magnetic boat, placing the magnetic boat in a tube furnace for calcination, and calcining at 550 ℃ for 2h to obtain the composite material.
(5) The X-ray powder diffraction pattern of the sample is shown in figure 1, a is Bi2WO6In comparison with a standard XRD card, Bi2WO6The peak position of (A) corresponds to that of (B), thus showing that Bi is successfully synthesized2WO6. b is composite material LC/Bi2WO6The X-ray powder diffraction pattern of (A) shows that the peak at 20 to 25 ℃ is a carbon peak and Bi2WO6Also appears in the X-ray powder diffraction pattern of the composite material, indicating LC/Bi2WO6Composite materials have been successfully synthesized.
(6) The Fourier infrared spectrum of the sample is shown in FIG. 2, b is Bi2WO6The infrared spectrum of (2), 820cm in the spectrum-1The peak is the asymmetric stretching vibration of the O-W-O bond; 736cm-1The position is the superposition of the stretching vibration peak of the W-O-W bond and the Bi-O bond; 571cm-1The peak at (B) is caused by stretching vibration of the W-O bond. and a is an infrared spectrum of LC. c is the infrared spectrum of the composite material, the graph and Bi2WO6Has similar infrared spectrum not only at 736cm-1Is shown by Bi2WO6And a characteristic absorption peak of 1435cm-1Characteristic absorption peaks of LC also appear; description of LC/Bi2WO6Composite materials have been successfully synthesized.
(7) Novel composite material LC/Bi2WO6Has good photodegradation efficiency on methylene blue under the condition of visible light. The reaction solution was pH 10, 50ml of methylene blue solution (30 mg/L), 10mg of LC/Bi2WO6The new composite material is used as a photocatalyst, dark reaction is carried out for 30min, after adsorption-desorption equilibrium is reached, the reactor is placed under a light source for visible light illumination, samples are taken once every 30min and centrifuged, then the light absorption C of supernatant is tested at the position of which the lambda is 665nm, and the relative concentration C/C of methylene blue is calculated0Photocatalytic activity was analyzed. Bi alone, as shown in FIG. 32WO6The photodegradation efficiency of methylene blue reaches only 88.6 percent after 2.5 hours, and the new composite material LC/Bi2WO6Exhibits a higher photodegradation efficiency of 99.1% and is Bi alone2WO61.1 times of that of the compound, which shows that the increase of LC can effectively improve Bi2WO6Photodegradation efficiency for methylene blue.
Claims (5)
1. Lignin carbon/bismuth tungstate (LC/Bi)2WO6) A process for the preparation of a novel composite material, characterized in that it comprises the following steps:
(1) activating alkali lignin, namely activating the alkali lignin by taking the alkali lignin as a carbon source, dissolving a certain amount of alkali lignin in a sodium hydroxide solution, stirring, adding a certain amount of trimethyl ammonium chloride, raising the temperature, heating and stirring for a period of time, putting the product into a dialysis bag, dialyzing until the product is neutral, drying and grinding to obtain activated alkali lignin powder;
(2) under the condition of stirring, dissolving a certain amount of bismuth nitrate, sodium tungstate and the product obtained in the step (1) in a mixed solution of ethylene glycol and deionized water in sequence;
(3) transferring the reaction system obtained in the step (2) into a reaction kettle, placing the reaction kettle into an oven, reacting for a period of time at a certain temperature, naturally cooling to room temperature, washing with deionized water and absolute ethyl alcohol for three times respectively, centrifugally separating, and drying to obtain a product precursor;
(4) and (4) transferring the product precursor obtained in the step (3) into a magnetic boat, placing the magnetic boat in a tube furnace for calcination, and calcining at a certain temperature for a period of time to obtain a product.
2. An LC/Bi according to claim 12WO6The preparation method of the novel composite material is characterized by comprising the following steps: the adding amount of the alkali lignin in the step (1) is 10 g; the mass fraction of the sodium hydroxide solution is 20 percent; the adding amount of trimethyl ammonium chloride is 9 g; the temperature is 85 +/-5 ℃; the heating and stirring time is 3-4 h.
3. The method of claim 1LC/Bi2WO6The preparation method of the novel composite material is characterized by comprising the following steps: the adding amount of the bismuth nitrate in the step (2) is 0.73 g; the addition amount of sodium tungstate is 0.25 g; the addition amount of the activated alkali lignin powder is 0g and 0.1 g; the volume of the ethanol solution is 20 ml; the volume of the deionized water is 15 ml; the reaction temperature is 160 ℃; the reaction time is 24 h; the sample drying temperature was 80 ℃.
4. An LC/Bi according to claim 12WO6The preparation method of the novel composite material is characterized by comprising the following steps: the calcining temperature in the step (4) is 550 ℃; the calcination time was 2 h.
5. An LC/Bi according to claim 12WO6The preparation method of the novel composite material is used for preparing the composite material and degrading methylene blue through photocatalysis.
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