CN109833887B - Preparation method of visible light degradation organic dye composite catalyst - Google Patents
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Abstract
The invention belongs to the technical field of photocatalysis, and particularly relates to a photocatalystVisible light degradation organic dye composite catalyst Bi2Fe4O9The preparation method of the/BiOCl comprises the following steps: (1) weighing bismuth nitrate, adding the bismuth nitrate into a sodium hydroxide aqueous solution, uniformly dispersing, adding ferric nitrate, continuously and uniformly dispersing, transferring the mixture into a reaction kettle, carrying out hydrothermal reaction, cooling, carrying out solid-liquid separation, washing the obtained solid-state separated substance, and carrying out vacuum drying to obtain an intermediate product A. (2) Weighing bismuth nitrate and potassium chloride in water, adding the intermediate product A into the water, uniformly dispersing the mixture, transferring the mixture into a reaction kettle, carrying out hydrothermal reaction, cooling after the reaction is finished, carrying out solid-liquid separation, washing the obtained solid-state separated substance, and carrying out vacuum drying to obtain the composite catalyst. The production raw materials are cheap and easy to obtain, the production process is simple, and the yield is high; the composite material has good stability, acid and alkali resistance and high degradation efficiency on organic dye, and can effectively utilize visible light to degrade the organic dye.
Description
Technical Field
The invention belongs to the technical field of photocatalysis, and particularly relates to a visible light degradation organic dye composite catalyst Bi2Fe4O9A preparation method of BiOCl.
Background
With the improvement of living standard and the development of economic technology, environmental pollution is becoming one of the most concerned and urgent problems for people. Organic pollutants occupy a large proportion of the aspects of environmental pollution, most of the organic pollutants have certain toxicity, and some of the organic pollutants are also 'triple-cause' substances (mutagenic, teratogenic and carcinogenic), so that how to effectively treat the organic pollutants becomes the focus of research of people. The existing methods for treating organic pollutants comprise a physical adsorption method, a biological degradation method, a chemical oxidation method, a photocatalytic method and the like.
Compared with other traditional degradation technologies, the photocatalytic degradation technology is novel, has the characteristics of high degradation efficiency, strong degradation stability, small secondary pollution and the like, and is very simple in synthesis process, cheap and easily available in raw materials and expected to be applied in industrial production and large range, so that the photocatalytic degradation catalyst has great prospect and long-term application value.
The nanometer semiconductor material has good photosensitive performance and is a preferred material for photocatalysis, but the band gap width of some semiconductors limits the light utilization efficiency, and ultraviolet light induction is often needed for overlarge band gap, and the ultraviolet proportion in sunlight is less, so that the factor greatly reduces the degradation application of the nanometer semiconductor material in the aspect of visible light.
Disclosure of Invention
In view of the above problems, the present invention aims to provide a composite catalyst Bi for degrading organic dyes such as rhodamine by visible light2Fe4O9The preparation method of the/BiOCl improves the capability of the catalyst for degrading organic dye under the condition of visible light.
In order to solve the technical problems, the invention is realized by the following technical scheme:
a preparation method of a visible light degradation organic dye composite catalyst is designed, and comprises the following steps:
(1) weighing a certain amount of bismuth nitrate (pentahydrate), adding the bismuth nitrate (pentahydrate) into a proper amount of sodium hydroxide aqueous solution (8-12 mol/L), uniformly dispersing, adding a certain amount of ferric nitrate (nonahydrate), continuously uniformly dispersing, transferring to a reaction kettle, carrying out hydrothermal reaction (at least 6 h) at the temperature of 210 ℃ of 180-; the molar ratio of bismuth nitrate to ferric nitrate used was 1: (0.8-1.2).
(2) Weighing a certain amount of bismuth nitrate (pentahydrate) and potassium chloride in water, adding a certain amount of intermediate product A into the water, uniformly dispersing, transferring the mixture into a reaction kettle, carrying out hydrothermal reaction at the temperature of 120-160 ℃ (at least 10 h), cooling to room temperature after the reaction is finished, carrying out solid-liquid separation, washing the obtained solid-state separated substance (with absolute ethyl alcohol and deionized water for multiple times), and carrying out vacuum drying (drying at the temperature of 70-85 ℃ for at least 4 h) to obtain the composite catalyst. The mass ratio of the bismuth nitrate to the potassium chloride to the intermediate product A is 1: 0.1-0.2: (0.025-0.080).
The invention has the following positive and beneficial effects:
the preparation method has the advantages of cheap and easily obtained production raw materials, simple production process and high yield; the composite material has good stability, acid and alkali resistance and high degradation efficiency on organic dye, and can effectively utilize visible light to degrade the organic dye.
The composite catalyst prepared by the invention forms a heterostructure, can improve the absorption of a semiconductor in a visible light region and the degradation performance of the semiconductor in the visible light region, and needs to introduce another semiconductor with a narrower band gap to improve the degradation performance of the whole semiconductor under visible light.
Drawings
FIG. 1 is an XRD pattern of materials prepared in comparative examples 1-2 and examples 1-3 according to the present invention.
Among them, examples 1 to 3 succeeded in composing a two-phase composite from the comparison of the peak positions of diffraction peaks, and the peak pattern of intermediate A was also slowly increased as the supported amount was increased.
FIG. 2 is a UV-VIS diffuse reflectance spectrum of materials prepared in comparative examples 1-2 and examples 1-3 according to the present invention.
Figure 3 is a graph of the forbidden bandwidth of a single material prepared in comparative examples 1-2.
As can be seen from fig. 2 and 3, the forbidden band width of comparative example 1 is 3.25 eV, and the response is only under ultraviolet light, and the forbidden band width of comparative example 2 is 1.75 eV, and the response is under visible light, and the photocatalytic response under visible light is obviously improved after the two are compounded.
FIG. 4 is an ultraviolet-visible spectrum of the composite catalyst obtained in example 2 for degrading rhodamine B.
In the figure, after visible light is irradiated for one hour, all absorption peaks of rhodamine B basically disappear, and the rhodamine B is basically and completely degraded.
FIG. 5 is a diagram showing the effect of degrading rhodamine B by the materials prepared in comparative examples 1-2 and examples 1-3.
As can be seen from the figure, the catalytic degradation effect of the example 2 is the best, and the visible light photocatalytic performance is obvious.
FIG. 6 is a schematic view showing the cyclic degradation of the composite catalyst obtained in example 2.
In the figure, the catalytic efficiency is not obviously changed after the cyclic degradation is carried out for three times, and the high degradation efficiency can still be maintained, which indicates that the composite catalyst has good stability and catalytic efficiency.
Detailed Description
The invention is described in further detail below with reference to the drawings and specific examples, which are provided for illustration only and are not intended to limit the scope of the invention. The test methods used in the following examples are all conventional methods unless otherwise specified; the materials, reagents and the like used are, unless otherwise specified, commercially available reagents and materials.
Comparative example 1
Bi2Fe4O9Preparation of the catalyst: weighing 5mmol of bismuth nitrate pentahydrate in 20mL of NaOH (10 mol/L) aqueous solution, uniformly stirring, adding 5mmol of ferric nitrate nonahydrate, continuously stirring for half an hour, transferring to a reaction kettle, carrying out hydrothermal reaction at 200 ℃ for 8 hours, cooling to room temperature after the reaction is finished, filtering, washing obtained filter residue for multiple times by using absolute ethyl alcohol and deionized water, carrying out vacuum drying (drying at 80 ℃ for 6 hours) to obtain a product, wherein the XRD (X-ray diffraction) spectrum is shown in figure 1, the ultraviolet-visible diffuse reflection spectrum is shown in figure 2, and the forbidden band width is shown in figure 3.
Comparative example 2
Preparation of a BiOCl catalyst: weighing 5mmol of bismuth nitrate pentahydrate and potassium chloride in 20mL of deionized water, stirring for half an hour, transferring to a reaction kettle, carrying out hydrothermal reaction for 12 hours at 140 ℃, cooling to room temperature after the reaction is finished, filtering, washing the obtained filter residue for multiple times by using absolute ethyl alcohol and deionized water, carrying out vacuum drying (drying for 6 hours at 80 ℃) to obtain a product, and measuring an XRD (X-ray diffraction) spectrum as shown in figure 1, an ultraviolet-visible diffuse reflection spectrum as shown in figure 2 and a forbidden bandwidth as shown in figure 3.
Example 1
Visible light degradation rhodamine organic dye composite catalyst Bi2Fe4O9The preparation method of the/BiOCl comprises the following steps:
(1) weighing 5mmol of bismuth nitrate pentahydrate (2.43 g) in 20mL of NaOH (10 mol/L) aqueous solution, uniformly stirring, adding 5mmol of ferric nitrate nonahydrate (2.02 g), continuously stirring for half an hour, transferring to a reaction kettle, carrying out hydrothermal reaction at 200 ℃ for 8h, cooling to room temperature after the reaction is finished, filtering, washing the obtained filter residue with absolute ethyl alcohol and deionized water for multiple times, and carrying out vacuum drying (drying at 80 ℃ for 6 h) to obtain 1.87 g of an intermediate product A.
(2) Weighing 2mmol of bismuth nitrate pentahydrate (0.97 g) and potassium chloride (0.15 g) in 20mL of deionized water, adding 0.026g of intermediate product A, stirring for 20 minutes, transferring to a reaction kettle, carrying out hydrothermal reaction for 12 hours at 140 ℃, cooling to room temperature after the reaction is finished, filtering, washing the obtained filter residue with absolute ethyl alcohol and deionized water for multiple times, drying in vacuum (drying for 6 hours at 80 ℃) to obtain the composite catalyst, and measuring an XRD (X-ray diffraction) spectrum as shown in figure 1 and an ultraviolet-visible diffuse reflection spectrum as shown in figure 2.
Example 2
Visible light degradation rhodamine organic dye composite catalyst Bi2Fe4O9The preparation method of the/BiOCl comprises the following steps:
(1) weighing 5mmol of bismuth nitrate pentahydrate (2.43 g) in 20mL of NaOH (10 mol/L) aqueous solution, uniformly stirring, adding 5mmol of ferric nitrate nonahydrate (2.02 g), continuously stirring for half an hour, transferring to a reaction kettle, carrying out hydrothermal reaction at 200 ℃ for 8h, cooling to room temperature after the reaction is finished, filtering, washing the obtained filter residue with absolute ethyl alcohol and deionized water for multiple times, and carrying out vacuum drying (drying at 80 ℃ for 6 h) to obtain 1.89g of an intermediate product A.
(2) Weighing 2mmol of bismuth nitrate pentahydrate (0.97 g) and potassium chloride (0.15 g) in 20mL of deionized water, adding 0.052g of intermediate product A, stirring for 20 minutes, transferring to a reaction kettle, carrying out hydrothermal reaction for 12 hours at 140 ℃, cooling to room temperature after the reaction is finished, filtering, washing the obtained filter residue with absolute ethyl alcohol and deionized water for multiple times, carrying out vacuum drying (drying for 6 hours at 80 ℃) to obtain the composite catalyst, and measuring an XRD (X-ray diffraction) spectrum of the composite catalyst as shown in figure 1 and an ultraviolet-visible diffuse reflection spectrum as shown in figure 2.
Example 3
Visible light degradation rhodamine organic dye composite catalyst Bi2Fe4O9The preparation method of the/BiOCl comprises the following steps:
(1) weighing 5mmol of bismuth nitrate pentahydrate (2.43 g) in 20mL of NaOH (10 mol/L) aqueous solution, uniformly stirring, adding 5mmol of ferric nitrate nonahydrate (2.02 g), continuously stirring for half an hour, transferring to a reaction kettle, carrying out hydrothermal reaction at 200 ℃ for 8h, cooling to room temperature after the reaction is finished, filtering, washing the obtained filter residue with absolute ethyl alcohol and deionized water for multiple times, and carrying out vacuum drying (drying at 80 ℃ for 6 h) to obtain 1.83 g of an intermediate product A.
(2) Weighing 2mmol of bismuth nitrate pentahydrate (0.97 g) and potassium chloride (0.15 g) in 20mL of deionized water, adding 0.078g of intermediate product A, stirring for 20 minutes, transferring to a reaction kettle, carrying out hydrothermal reaction for 12 hours at 140 ℃, cooling to room temperature after the reaction is finished, filtering, washing the obtained filter residue with absolute ethyl alcohol and deionized water for multiple times, drying in vacuum (drying for 6 hours at 80 ℃) to obtain the composite catalyst, and measuring an XRD (X-ray diffraction) spectrum of the composite catalyst as shown in figure 1 and an ultraviolet-visible diffuse reflection spectrum as shown in figure 2.
The catalyst obtained in the embodiment is subjected to property characterization and performance test, wherein the specific operation steps for degrading the organic dye rhodamine B are as follows: preparing 10 mg/L rhodamine B solution, putting 100 mL into a degradation tank, weighing 500mg of catalyst, adding into the tank, ultrasonically dispersing for 2 min, placing in a dark environment, stirring for 30 min to ensure that the absorption and desorption balance of the dye on the surface of the catalyst is achieved, absorbing 2.5 mL of suspension solution, filtering by using a filter membrane, then irradiating by using a 500W xenon lamp light source (the light filter is Cut 400 nm), taking the solution once at the interval of 15 min of illumination, filtering by using the same operation method, and then measuring the absorbance by using an ultraviolet-visible spectrophotometer, wherein the result is shown in figures 4-6.
Example 4
Visible light degradation rhodamine organic dye composite catalyst Bi2Fe4O9The preparation method of the/BiOCl comprises the following steps:
(1) weighing 5mmol of bismuth nitrate pentahydrate in 20mL of NaOH (8 mol/L) aqueous solution, uniformly stirring, adding 4mmol of ferric nitrate nonahydrate, continuously stirring for half an hour, transferring to a reaction kettle, carrying out hydrothermal reaction at 180 ℃ for 6 hours, cooling to room temperature after the reaction is finished, filtering, washing obtained filter residue with absolute ethyl alcohol and deionized water for multiple times, and carrying out vacuum drying (drying at 80 ℃ for 6 hours) to obtain an intermediate product A.
(2) Weighing 1g of bismuth nitrate pentahydrate and 0.1g of potassium chloride, putting into 20mL of deionized water, adding 0.025g of intermediate product A, stirring for 20 minutes, transferring into a reaction kettle, carrying out hydrothermal reaction for 10 hours at 140 ℃, cooling to room temperature after the reaction is finished, filtering, washing the obtained filter residue with absolute ethyl alcohol and deionized water for multiple times, and carrying out vacuum drying (drying at 80 ℃ for 6 hours) to obtain the composite catalyst.
Example 5
Visible light degradation rhodamine organic dye composite catalyst Bi2Fe4O9The preparation method of the/BiOCl comprises the following steps:
(1) weighing 5mmol of bismuth nitrate pentahydrate in 20mL of NaOH (12 mol/L) aqueous solution, uniformly stirring, adding 6mmol of ferric nitrate nonahydrate, continuously stirring for half an hour, transferring to a reaction kettle, carrying out hydrothermal reaction at 200 ℃ for 8 hours, cooling to room temperature after the reaction is finished, filtering, washing the obtained filter residue with absolute ethyl alcohol and deionized water for multiple times, and carrying out vacuum drying (drying at 80 ℃ for 6 hours) to obtain an intermediate product A.
(2) Weighing 1g of bismuth nitrate pentahydrate and 0.2g of potassium chloride, putting the bismuth nitrate pentahydrate and the potassium chloride into 20mL of deionized water, adding 0.08g of the intermediate product A, stirring for 20 minutes, transferring the mixture into a reaction kettle, carrying out hydrothermal reaction for 14 hours at 160 ℃, cooling to room temperature after the reaction is finished, filtering, washing the obtained filter residue with absolute ethyl alcohol and deionized water for multiple times, and carrying out vacuum drying (drying for 6 hours at 80 ℃) to obtain the composite catalyst.
Example 6
Visible light degradation rhodamine organic dye composite catalyst Bi2Fe4O9The preparation method of the/BiOCl comprises the following steps:
(1) weighing 5mmol of bismuth nitrate pentahydrate in 20mL of NaOH (10 mol/L) aqueous solution, uniformly stirring, adding 5mmol of ferric nitrate nonahydrate, continuously stirring for half an hour, transferring to a reaction kettle, carrying out hydrothermal reaction at 210 ℃ for 8 hours, cooling to room temperature after the reaction is finished, filtering, washing obtained filter residue with absolute ethyl alcohol and deionized water for multiple times, and carrying out vacuum drying (drying at 80 ℃ for 6 hours) to obtain an intermediate product A.
(2) Weighing 1g of pentahydrate bismuth nitrate and 0.15g of potassium chloride in 20mL of deionized water, adding 0.05g of intermediate product A into the deionized water, stirring the mixture for 20 minutes, transferring the mixture into a reaction kettle, carrying out hydrothermal reaction for 10 hours at 120 ℃, cooling the mixture to room temperature after the reaction is finished, filtering the mixture, washing the obtained filter residue with absolute ethyl alcohol and deionized water for multiple times, and drying the filter residue in vacuum (drying the filter residue for 6 hours at 80 ℃) to obtain the composite catalyst.
Claims (5)
1. A preparation method of a visible light degradation organic dye composite catalyst is characterized by comprising the following steps:
(1) weighing a certain amount of bismuth nitrate, adding the bismuth nitrate into a proper amount of sodium hydroxide aqueous solution, uniformly dispersing, adding a certain amount of ferric nitrate, continuously uniformly dispersing, transferring the mixture into a reaction kettle, carrying out hydrothermal reaction, cooling after the reaction is finished, carrying out solid-liquid separation, washing the obtained solid-state separated substance, and carrying out vacuum drying to obtain an intermediate product A;
(2) weighing a certain amount of bismuth nitrate and potassium chloride in water, adding a certain amount of intermediate product A into the water, uniformly dispersing the intermediate product A, transferring the intermediate product A into a reaction kettle, carrying out hydrothermal reaction, cooling the reaction product after the reaction is finished, carrying out solid-liquid separation, washing the obtained solid-state separated substance, and carrying out vacuum drying to obtain the composite catalyst;
the molar ratio of bismuth nitrate to ferric nitrate used in the step (1) is 1: (0.8-1.2);
the mass ratio of the bismuth nitrate and the potassium chloride to the intermediate product A in the step (2) is 1: (0.1-0.2): (0.025-0.080);
the hydrothermal reaction in the step (1) is carried out for at least 6h at the temperature of 210 ℃ of 180-;
the hydrothermal reaction in the step (2) is carried out for at least 10h at the temperature of 120-160 ℃.
2. The method of claim 1, wherein: the bismuth nitrate is pentahydrate, and the ferric nitrate is nonahydrate.
3. The method of claim 1, wherein: the concentration of the sodium hydroxide aqueous solution is 8-12 mol/L.
4. The method of claim 1, wherein: the washing is carried out for multiple times by using absolute ethyl alcohol and deionized water.
5. The method of claim 1, wherein: the vacuum drying is drying at 70-85 ℃ for at least 4 h.
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