CN107486198B - Bi based on peach blossom biomass carbon modification2WO6Preparation method and application of composite photocatalyst - Google Patents
Bi based on peach blossom biomass carbon modification2WO6Preparation method and application of composite photocatalyst Download PDFInfo
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- CN107486198B CN107486198B CN201710649717.2A CN201710649717A CN107486198B CN 107486198 B CN107486198 B CN 107486198B CN 201710649717 A CN201710649717 A CN 201710649717A CN 107486198 B CN107486198 B CN 107486198B
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- 235000006040 Prunus persica var persica Nutrition 0.000 title claims abstract description 41
- 239000002028 Biomass Substances 0.000 title claims abstract description 34
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 30
- 229910052799 carbon Inorganic materials 0.000 title claims abstract description 30
- 239000011941 photocatalyst Substances 0.000 title claims abstract description 28
- 239000002131 composite material Substances 0.000 title claims abstract description 23
- 238000000034 method Methods 0.000 title description 15
- 240000006413 Prunus persica var. persica Species 0.000 title 1
- 244000144730 Amygdalus persica Species 0.000 claims abstract description 40
- 238000002360 preparation method Methods 0.000 claims abstract description 23
- 239000002243 precursor Substances 0.000 claims abstract description 4
- 239000000243 solution Substances 0.000 claims description 40
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 39
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- 238000003756 stirring Methods 0.000 claims description 22
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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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- IKHGUXGNUITLKF-UHFFFAOYSA-N Acetaldehyde Chemical compound CC=O IKHGUXGNUITLKF-UHFFFAOYSA-N 0.000 description 2
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- PYKYMHQGRFAEBM-UHFFFAOYSA-N anthraquinone Natural products CCC(=O)c1c(O)c2C(=O)C3C(C=CC=C3O)C(=O)c2cc1CC(=O)OC PYKYMHQGRFAEBM-UHFFFAOYSA-N 0.000 description 2
- 150000004056 anthraquinones Chemical class 0.000 description 2
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 2
- 229910052797 bismuth Inorganic materials 0.000 description 2
- JCXGWMGPZLAOME-UHFFFAOYSA-N bismuth atom Chemical compound [Bi] JCXGWMGPZLAOME-UHFFFAOYSA-N 0.000 description 2
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- 241000196324 Embryophyta Species 0.000 description 1
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- AAAQKTZKLRYKHR-UHFFFAOYSA-N triphenylmethane Chemical compound C1=CC=CC=C1C(C=1C=CC=CC=1)C1=CC=CC=C1 AAAQKTZKLRYKHR-UHFFFAOYSA-N 0.000 description 1
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J23/00—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
- B01J23/16—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of arsenic, antimony, bismuth, vanadium, niobium, tantalum, polonium, chromium, molybdenum, tungsten, manganese, technetium or rhenium
- B01J23/24—Chromium, molybdenum or tungsten
- B01J23/31—Chromium, molybdenum or tungsten combined with bismuth
-
- B01J35/39—
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J37/00—Processes, in general, for preparing catalysts; Processes, in general, for activation of catalysts
- B01J37/08—Heat treatment
- B01J37/082—Decomposition and pyrolysis
- B01J37/084—Decomposition of carbon-containing compounds into carbon
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J37/00—Processes, in general, for preparing catalysts; Processes, in general, for activation of catalysts
- B01J37/08—Heat treatment
- B01J37/10—Heat treatment in the presence of water, e.g. steam
-
- 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
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2101/00—Nature of the contaminant
- C02F2101/30—Organic compounds
- C02F2101/308—Dyes; Colorants; Fluorescent agents
Abstract
The invention belongs to the technical field of preparation of environmental materials, and provides a peach blossom biomass carbon modified Bi2WO6A preparation method and application of the composite photocatalyst. The preparation method comprises the following steps: step 1, treating a peach blossom precursor; step 2, preparing biomass carbon; step 3, Bi2WO6Preparing; step 4, Bi2WO6Preparation of/C. Carbon has good conductivity, introduction of carbon material and Bi2WO6The synergistic effect of the two-component composite photocatalyst Bi improves the photocatalytic effect, so that the two-component composite photocatalyst Bi prepared by the invention2WO6the/C has good photocatalytic activity.
Description
Technical Field
The invention belongs to the technical field of preparation of environmental materials, and particularly relates to a peach blossom biomass carbon-modified Bi2WO6A preparation method and application of the composite photocatalyst.
Background
The dye is widely applied to industries of food, medicine, printing and dyeing, cosmetics and the like, statistics shows that the commercial application of the dye is more than 100000, the annual output of the dye in the world is about 80-90 ten thousand tons, the annual output of the dye in China is about 15 ten thousand tons, and the dye in the world is in the top. With the wide use of various dyes, 10 to 15 percent of the dyes are released into the environment in the production and use processes, most of the dyes are extremely stable and difficult to naturally degrade after entering an environmental water area, so that the chromaticity of the polluted water area is increased, the incident ray quantity is influenced, the normal life activities of aquatic animals and plants are further influenced, the ecological balance of the water body is damaged, more seriously, the dyes are mostly toxic substances and have carcinogenic and teratogenic effects, and the dyes are discharged into the environment to form great threat to the health of human beings and other organisms.
The dye wastewater has high Chemical Oxygen Demand (COD), high organic matter content and poor biodegradability. The raw materials for producing the dye mainly comprise aromatic, anthraquinone, aniline, nitrobenzene, phenols and the like, so that the dye wastewater contains a large amount of the substances, the loss dye or dye intermediate ensures that the COD and organic matter content in the wastewater is high, and the biodegradability of the substances is extremely poor, so that the treatment difficulty is increased. The dye wastewater also has the characteristic of high chromaticity, and contains various dyes, so that the chromaticity is very high, and even if the concentration of the dyes is very low, the wastewater can generate obvious color, and the decoloration of the dye wastewater is widely concerned. The components are also very complex, and the water quality fluctuation such as pH value is large. During the production and application of the dye, a large amount of acid or alkali can be used, so that the pH value of the waste water is greatly changed. Meanwhile, the process from raw materials to finished dyes is often complex in operation, more in side reactions and serious in loss, so that the components in the waste water are complex and the biodegradability is poor. In addition, the dye has various types, complex structure and intermittent production process, so that the wastewater quality fluctuation is large and the wastewater is difficult to treat. The toxicity is also high, and the environmental pollution is serious. Most dyes and dye intermediates have carcinogenic, teratogenic and mutagenic effects and high biotoxicity, and some dye varieties are listed as the priority chemical substances for carcinogenic tests. Meanwhile, because the dye has wide application, the dye and the dye intermediate released into the environment cause serious pollution to the environment, and the treatment difficulty is very large. Most dyes have stable chemical properties and complex structures, have carcinogenic, teratogenic and mutagenic effects on human beings and other organisms, have high biological toxicity, are all found to have the triprotic effects and have high biological toxicity no matter azo dyes or anthraquinone and triphenylmethane dyes, and have frequent prohibition on use due to low production and use cost and no suitable substitute, so that the dyes have great influence on ecological environment and human health.
The dye wastewater has complex components, high chromaticity, high COD and biological oxygen demand, more suspended matters, large water quality and water quantity change and more difficultly-degraded substances, so the treatment difficulty of the dye wastewater is increased, the dye wastewater becomes one of the industrial wastewater which is difficult to treat at home and abroad, and the treatment technology of the dye wastewater is fully valued and widely researched by domestic and foreign water treatment workers. At present, the treatment method of dye wastewater internationally mainly comprises a physical method, a chemical method, a biological method and the like.
The photocatalysis technology is a new high-efficiency energy-saving modern sewage treatment technology, and TiO is published in Fujishima equal to 19722After the research paper of hydrogen production by single crystal electrolysis of water, the photocatalytic reaction attracts attention of many scholars in the fields of chemistry, physics, materials, environmental protection and the like. From the research results and the current situation, the effect of the method on the treatment of single dye and actual printing and dyeing wastewater is well recognized. This is mainly due to the strong oxidizing power of the photocatalytic oxidation process, which ultimately results in the complete oxidative decomposition of organic contaminants. The photocatalysis method has the advantages of simple structure, easy control of operation conditions, strong oxidation capability, no secondary pollution and the like.
According to the band theory, a semiconductor band is composed of a Valence Band (VB) filled with electrons and having low energy and an empty Conduction Band (CB) having high energy, and a region between the conduction band and the valence band is called a forbidden band, and the size of the forbidden band is an important factor affecting the photocatalytic properties of a semiconductor material. Since the energy band of a semiconductor is discontinuous, when it is excited by energy equal to or greater than the forbidden band width (Eg), the lower energy electron absorption energy in the valence band is excited to jumpAnd migrate to the conduction band to form negatively charged electrons. At the same time, a positively charged hole is left in the valence band, generating an electron-hole pair. Photoproduction of electron-hole with H on the surface of semiconductor under certain conditions2O，O2The action of the like produces OH, O with strong activity2 -A free radical. These active radicals, through interaction with the contaminant molecules, can break them down into harmless, non-toxic small molecule compounds and even completely mineralize.
Tungstate materials have good application prospects in the aspects of scintillation materials, optical fibers, photoluminescence materials, microwave applications, humidity sensors, magnetic devices, catalysts, corrosion inhibitors and the like, and become hot spots of research in recent years. Bismuth tungstate (Bi) was first reported by Kudo et al 19992WO6) After having photocatalytic activity under visible radiation with a wavelength of more than 420nm, Bi2WO6Due to its narrow forbidden band width (about 2.7eV), it can be excited by visible light and has high catalytic activity under visible light, thus attracting more and more attention as a new type of photocatalytic material, as discovered by recent research that Bi responds to visible light2WO6Can effectively degrade harmful substances such as chloroform, acetaldehyde and the like, and can effectively degrade dye wastewater. Thus, Bi2WO6The research of the photocatalytic material opens up a new way for removing and degrading organic pollutants by photocatalysis, and has very important practical value in the aspects of environmental purification and new energy development.
In recent years, biomass has attracted a wide range of attention worldwide in terms of its low cost, abundance of raw materials, and renewability. The biomass is a renewable carbon carrier which can be recycled from the nature and developed. The biomass carbon material is prepared by taking biomass as a raw material, so that the cost can be saved, and the problem of environmental pollution caused by burning a large amount of waste biomass can be relieved. The carbon material is an important structural material and a functional material, various carbon materials are prepared by utilizing a biomass raw material, the production cost of the carbon material can be reduced, the sustainable development of the carbon material is realized, and researches show that the carbon-based photocatalyst plays a great role in improving the photocatalytic activity. The carbon material is an environment-friendly and cheap raw material, has good conductivity, and can effectively promote the separation of photogenerated electron-hole pairs.
At present, a photocatalytic material compounded by bismuth tungstate and biomass carbon is rarely reported.
Disclosure of Invention
The invention takes peach blossom as raw material to prepare biomass carbon, and synthesizes a novel composite photocatalyst Bi by a high-temperature calcination method and a hydrothermal method2WO6the/C has the characteristics of wide sources, low cost and the like, is applied to degrading rhodamine B, has stable performance, and greatly improves the photocatalytic effect.
The technical scheme of the invention is as follows:
bi based on peach blossom biomass carbon modification2WO6The preparation method of the composite photocatalyst comprises the following steps:
step 1, peach blossom precursor treatment:
picking up withered peach blossom, washing with water to remove dirt and dust on the surface, washing with deionized water, drying, pulverizing in a pulverizer, and sieving to obtain peach blossom powder for later use;
adding the peach blossom powder obtained in the step 1 into deionized water, sealing and magnetically stirring until the peach blossom powder is uniformly dispersed, standing after ultrasonic treatment, adding a certain amount of NaOH solution, heating in water bath, magnetically stirring, and then adding diluted H2SO4Adjusting the pH value of the solution to be neutral, drying the solution in vacuum to obtain a solid product, and grinding the solid product; placing the ground solid product in a porcelain boat and placing the porcelain boat in a tube furnace N2Calcining in the atmosphere, taking out the porcelain boat after the temperature of the tubular furnace is cooled to the room temperature, grinding the solid sample in the porcelain boat into powder, drying in vacuum, and cooling to the room temperature to obtain biomass carbon;
step 3, Bi2WO6The preparation of (1):
a certain amount of Bi (NO)3)3·5H2Dissolving O in acetic acid, and magnetically stirring until the O is completely dissolved, wherein the solution is called solution A;
adding a certain amount of Na2WO4·2H2O dissolves in the deionizationWater, designated as solution B;
dropwise adding the solution B into the solution A, magnetically stirring, transferring the mixed solution into a stainless steel reaction kettle, heating the reaction kettle under certain conditions, naturally cooling to room temperature, washing the product with deionized water and ethanol, centrifugally separating the precipitate, drying the precipitate in a vacuum oven for later use, and marking the precipitate as Bi2WO6；
Step 4, Bi2WO6Preparation of/C:
the biomass carbon in the step 2 and the Bi in the step 3 are mixed2WO6Dissolving a certain amount of Bi in ethanol, carrying out ultrasonic treatment on the obtained suspension, magnetically stirring, then carrying out vacuum drying, and grinding the product Bi2WO6/C。
In the step 1, the drying temperature is 60-80 ℃.
In the step 2, the dosage ratio of the peach blossom powder, the deionized water and the NaOH solution is 1-5 g: 15-75 mL: 5mL of the above NaOH and H2SO4All the concentrations of (A) and (B) are 1 mol. L-1。
In the step 2, the calcining temperature is 450-550 ℃, and the calcining temperature is kept for 4 hours at the constant temperature, wherein the heating rate is 1.0-10 ℃ per minute-1。
In the step 2, the temperature of the vacuum drying is 60-80 ℃.
In step 3, Bi (NO) is used3)3·5H2The dosage ratio of the O to the acetic acid is 0.5-5 g: 15-150 mL; na used2WO4·2H2The dosage ratio of O to deionized water is 0.1-1 g: 20-200 mL;
when the solution B is dripped into the solution A, Bi (NO)3)3·5H2O and Na2WO4·2H2The mass ratio of O is 0.5-5 g: 0.1 to 1 g.
In the step 3, the heating temperature is 180 ℃ and the heating time is 20 h.
In step 4, Bi is2WO6The mass ratio of C to C is 1-8: 1.
in the step 4, the ultrasonic time is 1-5 h, the magnetic stirring reaction time is 2-5h, and the vacuum drying temperature is 60-80 ℃.
The method prepares Bi2WO6the/C composite photocatalyst is used for photocatalytic degradation of rhodamine B.
The invention has the beneficial effects that:
(1) the peach blossom is used as the raw material to prepare the biomass carbon, the source is wide, the cost is low, and the waste of resources is avoided.
(2) Bi prepared by the method of the invention2WO6the/C composite photocatalyst has better photocatalytic activity and stability.
Drawings
FIG. 1 is an XRD pattern of a sample prepared in example 1; are respectively C, Bi2WO6，Bi2WO6XRD profile of/C;
FIG. 2 is an SEM photograph of a sample prepared in example 1; wherein, a is SEM picture of C; b is as the drawing Bi2WO6SEM picture of (1); c, d are Bi2WO6/C；
FIG. 3 is a graph of UV-vis DRS of samples prepared in example 1; wherein a is Bi2WO6B is Bi2WO6UV-vis DRS curve for/C.
Detailed Description
The invention is further described below with reference to specific examples:
evaluation of photocatalytic activity: the method is carried out in a D1 type photochemical reaction instrument (purchased from teaching instrument factories of Yangzhou university), 100mL of 20mg/L rhodamine B simulation wastewater is added into a reaction bottle, magnetons and 0.05g of photocatalyst are added, a visible light power supply and an aeration device are opened for dynamic adsorption, and an external super constant temperature water bath is started to control the temperature of a reaction system to be 30 ℃. Performing illumination reaction after reaching adsorption equilibrium, sampling every 15min, centrifuging, measuring the concentration of rhodamine B in the supernatant, and passing through C/C0The degradation effect of rhodamine B is judged. Wherein, C0The concentration of rhodamine B after adsorption equilibrium is shown, and C is the concentration of rhodamine B in the reaction time T.
The method comprises the following steps:
bi based on peach blossom biomass carbon modification2WO6The preparation method of the composite photocatalyst comprises the following steps:
step 1, peach blossom precursor treatment:
picking up withered peach blossom, washing with water to remove dirt and dust on the surface, washing with deionized water, drying at 60-80 ℃, putting into a crusher for crushing, and sieving to obtain peach blossom powder for later use;
adding the peach blossom powder obtained in the step 1 into deionized water, sealing and magnetically stirring until the peach blossom powder is uniformly dispersed, standing after ultrasonic treatment, adding a certain amount of NaOH solution, heating in water bath, magnetically stirring, and then adding diluted H2SO4Adjusting the pH value of the solution to be neutral, drying the solution in vacuum to obtain a solid product, and grinding the solid product; placing the ground solid product in a porcelain boat and placing the porcelain boat in a tube furnace N2Calcining in the atmosphere, taking out the porcelain boat after the temperature of the tubular furnace is cooled to the room temperature, grinding the solid sample in the porcelain boat into powder, drying in vacuum, and cooling to the room temperature to obtain biomass carbon;
step 3, Bi2WO6The preparation of (1):
a certain amount of Bi (NO)3)3·5H2Dissolving O in acetic acid, and magnetically stirring until the O is completely dissolved, wherein the solution is called solution A;
adding a certain amount of Na2WO4·2H2Dissolving O in deionized water to obtain solution B;
dropwise adding the solution B into the solution A, magnetically stirring, transferring the mixed solution into a stainless steel reaction kettle, heating the reaction kettle under certain conditions, naturally cooling to room temperature, washing the product with deionized water and ethanol, centrifugally separating the precipitate, drying the precipitate in a vacuum oven for later use, and marking the precipitate as Bi2WO6；
Step 4, Bi2WO6Preparation of/C:
the biomass carbon in the step 2 and the step3 of Bi2WO6Dissolving a certain amount of Bi in ethanol, carrying out ultrasonic treatment on the obtained suspension, magnetically stirring, then carrying out vacuum drying, and grinding the product Bi2WO6/C。
Example 1:
in the step 1, the mass of the picked peach blossom is 200 g.
In the step 2, the used amount of the peach blossom powder is 2g, the used amount of deionized water is 30mL, and the amount of NaOH solution is 5 mL; the NaOH and H2SO4All the concentrations of (A) and (B) are 1 mol. L-1. The calcination temperature is 500 ℃, and the calcination temperature is kept for 4 hours at the constant temperature, wherein the heating rates are both 2.3 ℃ and min-1(ii) a The temperature of the vacuum drying was 60 ℃.
In step 3, Bi (NO) is used3)3·5H2The dosage of O is 1.0g, and the dosage of acetic acid used is 30 mL; na used2WO4·2H2The dosage of O is 0.3g, and the dosage of deionized water is 50 mL; the heating temperature is 180 ℃, and the heating time is 20 h.
In step 4, Bi is2WO6The mass ratio of C to C is 4: 1; the ultrasonic time is 2 hours, the stirring reaction time at constant temperature is 3 hours, and the constant temperature is 70 ℃.
0.05g of Bi obtained in step 4 are taken2WO6adding/C to 100mL of a solution containing 20mg of L-1Stirring the rhodamine B solution in a reactor at 30 ℃ in a dark place to achieve adsorption balance; turning on xenon lamp and aerating, sampling once every certain time, taking 5mL each time, centrifuging, taking clear liquid, and measuring absorbance value at 554nm by using ultraviolet spectrometer.
Example 2:
in the step 1, the mass of the picked peach blossom is 200 g.
In the step 2, the used amount of the peach blossom powder is 1g, the used amount of deionized water is 15mL, and the amount of NaOH solution is 5 mL; the NaOH and H2SO4All the concentrations of (A) and (B) are 1 mol. L-1. The calcination temperature is 450 ℃ and is maintained at this constant temperature for 4 hours, wherein the temperature is raisedThe speed is 1.0 ℃ min-1. The temperature of the vacuum drying was 70 ℃.
In step 3, Bi (NO) is used3)3·5H2The dosage of O is 0.5g, and the dosage of acetic acid used is 15 mL; na used2WO4·2H2The dosage of O is 20mL of 0.1g of deionized water; the heating temperature is 180 ℃, and the heating time is 20 h.
In step 4, Bi is2WO6The mass ratio of C to C is 1: 1; the ultrasonic time is 1h, the stirring reaction time at the constant temperature is 2h, and the constant temperature is 60 ℃.
0.05g of Bi obtained in step 4 are taken2WO6adding/C to 100mL of a solution containing 20mg of L-1Stirring the rhodamine B solution in a reactor at 30 ℃ in a dark place to achieve adsorption balance; turning on xenon lamp and aerating, sampling once every certain time, taking 5mL each time, centrifuging, taking clear liquid, and measuring absorbance value at 554nm by using ultraviolet spectrometer.
Example 3:
in the step 1, the mass of the picked peach blossom is 200 g.
In the step 2, the used amount of the peach blossom powder is 5g, the used amount of deionized water is 75mL, and the amount of NaOH solution is 5 mL; the NaOH and H2SO4All the concentrations of (A) and (B) are 1 mol. L-1. The calcination temperature is 550 ℃, and the calcination temperature is kept for 4 hours at the constant temperature, wherein the heating rates are both 10 ℃ and min-1. The temperature of the vacuum drying was 80 ℃.
In step 3, Bi (NO) is used3)3·5H2The dosage of O is 5g, and the dosage of acetic acid used is 150 mL; na used2WO4·2H2The dosage of O is 1g of deionized water and 200 mL; the heating temperature is 180 ℃, and the heating time is 20 h.
In step 4, Bi is2WO6The mass ratio of C to C is 8: 1; the ultrasonic time is 5 hours, the stirring reaction time at constant temperature is 5 hours, and the constant temperature is 80 ℃.
0.05g of Bi obtained in step 4 is taken2WO6adding/C to 100mL of a solution containing 20mg of L-1Stirring the rhodamine B solution in a reactor at 30 ℃ in a dark place to achieve adsorption balance; turning on xenon lamp and aerating, sampling once every certain time, taking 5mL each time, centrifuging, taking clear liquid, and measuring absorbance value at 554nm by using ultraviolet spectrometer.
Evaluation of photocatalytic activity: irradiating in DW-01 photochemical reactor with visible light lamp, and mixing 100mL of 20mgL-1Adding rhodamine B simulation wastewater into a reactor, measuring an initial value of the wastewater, then adding a photocatalyst, magnetically stirring, starting an aeration device, introducing air to keep the catalyst in a suspended or floating state, sampling after dark adsorption balance, sampling and analyzing at an interval of 20min in the illumination process, taking supernatant after centrifugal separation, measuring absorbance at a position where a spectrophotometer lambda max is 554nm, and determining the absorbance through a formula: DC ═ C0-Ci/C0]× 100 the degradation rate was calculated at 100%, where C0Absorbance of rhodamine B to reach adsorption equilibrium, CiThe absorbance of the rhodamine B solution was determined for the timed sampling.
FIG. 1 shows C, Bi2WO6And Bi2WO6X-ray diffraction pattern of/C composite photocatalyst, from which pure Bi can be seen2WO6 Characteristic diffraction peaks 2 θ correspond to 28.3 °, 32.9 °, 47.3 °, 56.2 °, 58.8 °, 68.7 °, 76.3 ° and 78.5 ° of a standard card. Shows that we successfully prepare Bi2WO6A photocatalytic material; and in the photocatalyst carried by C, Bi2WO6The characteristic peak intensity of (A) is slightly weakened, which sufficiently proves that Bi is successfully synthesized2WO6a/C composite photocatalyst.
FIG. 2 shows C (a), Bi2WO6(b),Bi2WO6SEM image of/C (C, d). As shown in FIG. 2(a), the C nanoparticles have a rod-like structure. FIG. 2(b) shows synthesized Bi2WO6SEM image of the multilevel nanostructured material, from which it can be seen that Bi was synthesized2WO6The microspheres are spherical structures, are uniformly dispersed and have uniform sizes, and can be judged to be in flower-shaped multi-stage structuresThe diameter is about 5 mu m; it is clear that the exterior of the multilevel structure is constituted by flower-like nanosheets. Thus, Bi2WO6The three-dimensional flower-like microsphere structure is formed by mutually overlapping two-dimensional nano sheets. From FIGS. 2(c) and (d), it can be seen that Bi is doped due to carbon2WO6The spherical structure of (a) is gradually destroyed and the external flower-like lamellar structure is gradually reduced. C rod and Bi2WO6Are uniformly doped together.
Shown in FIG. 3 is Bi2WO6(a),Bi2WO6UV-vis DRS spectrogram of/C (b) composite photocatalyst, and Bi can be seen from the graph2WO6And Bi2WO6The light absorption edges of the/C photocatalyst are all around 450nm, however, Bi is introduced along with the introduction of C2WO6The absorption of visible light by/C is significantly enhanced. Therefore, the introduction of the assay C plays a crucial role in the light absorption of the photocatalytic material.
Claims (9)
1. Bi based on peach blossom biomass carbon modification2WO6The preparation method of the composite photocatalyst is characterized by comprising the following steps:
step 1, peach blossom precursor treatment:
picking up withered peach blossom, washing with water to remove dirt and dust on the surface, washing with deionized water, drying, pulverizing in a pulverizer, and sieving to obtain peach blossom powder for later use;
step 2, preparing biomass carbon:
adding the peach blossom powder obtained in the step 1 into deionized water, sealing and magnetically stirring until the peach blossom powder is uniformly dispersed, standing after ultrasonic treatment, adding a certain amount of NaOH solution, heating in water bath, magnetically stirring, and then adding diluted H2SO4Adjusting the pH value of the solution to be neutral, drying the solution in vacuum to obtain a solid product, and grinding the solid product; placing the ground solid product in a porcelain boat and placing the porcelain boat in a tube furnace N2Calcining in the atmosphere, taking out the porcelain boat after the temperature of the tubular furnace is cooled to the room temperature, grinding the solid sample in the porcelain boat into powder, drying in vacuum, and cooling to the room temperature to obtain biomass carbon;
step 3, Bi2WO6The preparation of (1):
a certain amount of Bi (NO)3)3·5H2Dissolving O in acetic acid, and magnetically stirring until the O is completely dissolved, wherein the solution is called solution A;
adding a certain amount of Na2WO4·2H2Dissolving O in deionized water to obtain solution B;
dropwise adding the solution B into the solution A, magnetically stirring, transferring the mixed solution into a stainless steel reaction kettle, heating the reaction kettle under certain conditions, naturally cooling to room temperature, washing the product with deionized water and ethanol, centrifugally separating the precipitate, drying the precipitate in a vacuum oven for later use, and marking the precipitate as Bi2WO6；
Step 4, Bi2WO6Preparation of/C:
the biomass carbon in the step 2 and the Bi in the step 3 are mixed2WO6Dissolving a certain amount of Bi in ethanol, carrying out ultrasonic treatment on the obtained suspension, magnetically stirring, then carrying out vacuum drying, and grinding the product Bi2WO6/C。
2. Bi based on peach blossom biomass carbon modification according to claim 12WO6The preparation method of the composite photocatalyst is characterized in that in the step 1, the drying temperature is 60-80 ℃.
3. Bi based on peach blossom biomass carbon modification according to claim 12WO6The preparation method of the composite photocatalyst is characterized in that in the step 2, the dosage ratio of the peach blossom powder, the deionized water and the NaOH solution is 1-5 g: 15-75 mL: 5mL of the above NaOH and H2SO4All the concentrations of (A) and (B) are 1 mol. L-1。
4. Bi based on peach blossom biomass carbon modification according to claim 12WO6The preparation method of the composite photocatalyst is characterized in that in the step 2, the calcination temperature isKeeping the temperature at 450-550 ℃ for 4h, wherein the heating rate is 1.0-10 ℃ per minute-1。
5. Bi based on peach blossom biomass carbon modification according to claim 12WO6The preparation method of the composite photocatalyst is characterized in that in the step 2, the temperature of vacuum drying is 60-80 ℃.
6. Bi based on peach blossom biomass carbon modification according to claim 12WO6The preparation method of the composite photocatalyst is characterized in that in the step 3, Bi (NO) is used3)3·5H2The dosage ratio of the O to the acetic acid is 0.5-5 g: 15-150 mL; na used2WO4·2H2The dosage ratio of O to deionized water is 0.1-1 g: 20-200 mL;
when the solution B is dripped into the solution A, Bi (NO)3)3·5H2O and Na2WO4·2H2The mass ratio of O is 0.5-5 g: 0.1 to 1 g.
7. Bi based on peach blossom biomass carbon modification according to claim 12WO6The preparation method of the composite photocatalyst is characterized in that in the step 3, the heating temperature is 180 ℃ and the heating time is 20 hours.
8. Bi based on peach blossom biomass carbon modification according to claim 12WO6The preparation method of the composite photocatalyst is characterized in that in the step 4, the Bi is2WO6The mass ratio of C to C is 1-8: 1.
9. bi based on peach blossom biomass carbon modification according to claim 12WO6The preparation method of the composite photocatalyst is characterized in that in the step 4, the ultrasonic time is 1-5 hours, the magnetic stirring reaction time is 2-5 hours, and the vacuum drying temperature is 60-80 ℃.
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| CN108479756A (en) * | 2018-03-05 | 2018-09-04 | 江苏大学 | A kind of Bi based on the carbon-based modification of phoenix tree leaf biomass2WO6The Preparation method and use of composite photo-catalyst |
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| CN112108150A (en) * | 2020-09-13 | 2020-12-22 | 通化师范学院 | Based on magnetic Fe3O4Modified corncob biomass carbon dot composite Bi2WO6Preparation method and application of photocatalyst |
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