CN115228503A - Preparation method of carbon nitride-based copper material for ozone catalytic oxidation water treatment - Google Patents
Preparation method of carbon nitride-based copper material for ozone catalytic oxidation water treatment Download PDFInfo
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- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
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- C02F1/725—Treatment of water, waste water, or sewage by oxidation by catalytic oxidation
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
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- C02F1/00—Treatment of water, waste water, or sewage
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Abstract
The invention discloses a preparation method of a carbon nitride-based copper material for ozone catalytic oxidation water treatment, which comprises the following steps: the carbon nitride micro powder with relatively stable C-N bonds is further synthesized by sputtering a graphite phase carbon nitride precursor and assisting microwave nitrogen plasma, the prepared carbon nitride micro powder is mixed with copper salt to prepare a copper-based solution, and then the copper-based solution is dried, calcined and subjected to post-treatment to obtain the carbon nitride-based copper material.
Description
Technical Field
The invention relates to the technical field of catalytic materials, in particular to a preparation method of a carbon nitride-based copper material for ozone catalytic oxidation water treatment.
Background
The catalytic ozonation technology is an advanced ozonation technology based on ozone, combines strong oxidizing property of ozone and active oxygen free radicals with adsorption and catalysis characteristics of a catalyst, and can effectively solve the problem of incomplete degradation of organic matters; for the ozone catalytic oxidation technology, the selection of the solid catalyst is the key to whether the technology has high-efficiency oxidation efficiency; however, the existing catalyst generally has the defects of low efficiency and poor stability.
The traditional ozone oxidation technology mainly adopts direct oxidation, has the problems of poor mass transfer effect, selectivity of oxidation, low utilization rate, high investment and operation cost and the like, and is not suitable for large-scale application.
The copper-based catalyst is a common ozone catalytic material and has the advantages of high catalytic activity and low price. However, the general copper-based catalytic material is a catalytic material formed by loading copper on a specific carrier, is limited by a regulation means, and has a problem of poor stability. In order to solve the problem of the conventional sewage treatment of the existing copper-based catalyst, the invention provides a preparation method of a carbon nitride-based copper material with stronger stability for an ozone catalytic oxidation water treatment technology.
Disclosure of Invention
The purpose of the invention is as follows: based on the problem of low efficiency of the ozone catalytic oxidation technology in the prior art, the preparation method of the carbon nitride-based copper material with high stability for the ozone catalytic oxidation water treatment technology is provided.
The technical scheme of the invention is as follows: a preparation method of carbon nitride-based copper material for ozone catalytic oxidation water treatment comprises the following steps:
s1, preparation of carbon nitride micro powder
Placing the graphite-phase carbon nitride precursor as a target material over a placing plate 10-15cm below microwave nitrogen plasma equipment, adjusting the distance between the placing plate and the plasma, starting the microwave nitrogen plasma equipment for reaction, and obtaining carbon nitride micro powder after the reaction is finished;
s2, preparing copper-based blending liquid
S2-1, preparing 2-5 g of carbon nitride micro powder into a carbon nitride precursor solution;
s2-2, and mixing the components in a mass ratio of 1:1 to 1.5, weighing 1.0 to 2.5g of mixed powder of copper acetate and copper chloride, adding the mixed powder into a carbon nitride precursor solution, stirring for 20 to 30min, and standing for 5 to 10min to obtain a copper-based mixed solution;
s3, drying
Putting the copper-based blend liquid into an electric heating constant-temperature air drying oven, keeping the temperature in the drying oven at 70-90 ℃, and drying for 10-15h to obtain a dry mixture;
s4, calcining
The dried mixture is calcined: raising the temperature to 400-500 ℃ at the heating rate of 5-10 ℃/min under the protection atmosphere of nitrogen, keeping the temperature for 1.5-3 h, and then cooling to room temperature to obtain the preposed carbon nitride-based copper;
s5, post-processing
And carrying out post-treatment on the preposed carbon nitride-based copper to obtain the carbon nitride-based copper material.
Further, the graphite-phase carbon nitride precursor is any one of dicyandiamide, melamine and urea;
description of the drawings: dicyanodiamine, melamine and urea are used as nitrogen-rich organic matters with low cost, and the materials are used as graphite phase carbon nitride precursors, so that the preparation process can be simplified, and the preparation cost can be reduced.
Further, in step S1, the reaction parameters are: the air pressure is 4.0 to 4.5kPa, and the nitrogen flow rate is 40 to 50cm 3 Min, microwave power of 450 to 500W and reaction time of 10 to 30min;
description of the invention: the carbon nitride micro powder with high nitrogen content is prepared by using the microwave nitrogen plasma, and the C-N bond contained in the carbon nitride micro powder is relatively stable, so that the subsequent preparation of the carbon nitride-based copper material is more facilitated.
Further, in the step S2-1, the method for preparing the carbon nitride precursor solution by using the carbon nitride micro powder includes: adding 2-5 g of carbon nitride micro powder into a flask filled with 70-100ml of ethanol solution, heating to 80-90 ℃, fully stirring for 20-30min, and standing for 5-10min to obtain a carbon nitride precursor solution.
Description of the invention: the ethanol solution can better disperse the graphite-phase carbon nitride micro powder, and further improve the utilization rate of the carbon nitride micro powder.
Further, in step S5, the post-processing method includes: heating the preposed carbon nitride-based copper to 550-600 ℃ at a heating rate of 15-20 ℃ in a nitrogen protective atmosphere, carrying out secondary calcination treatment for 0.5-1h, and cooling to room temperature to obtain the carbon nitride-based copper catalytic material.
Description of the invention: the primary calcined copper ions can be completely coordinated through secondary calcination to form the carbon nitride-based copper catalytic material with a copper-nitrogen coordination structure.
Further, in the step S2-1, the method for preparing the carbon nitride precursor solution by using the carbon nitride micro powder includes: according to the mass ratio of 5: placing the template agent and the aqueous solution in a flask according to the proportion of 1-10, heating to 80-90 ℃, fully stirring for 20-30min, standing for 5-10min, then adding 2-5g of carbon nitride micropowder, and fully stirring for 20min to obtain a carbon nitride precursor solution.
Description of the drawings: the small holes on the mesoporous carbon nitride can increase the specific surface area of the material, and the mesoporous carbon nitride has higher specific surface area and pore area, and the higher specific surface area can bring more catalytic reaction surface active points and more excellent adsorption capacity, and can play a better catalytic effect in ozone catalytic water treatment.
Further, the template agent is specifically selected from any one of nano silica spheres, silica sol and SBA-15 mesoporous molecular sieves.
Further, in step S5, the post-processing method includes:
s5-1, template removal
Placing the preposed carbon nitride-based copper in a triangular flask filled with sodium hydroxide or hydrofluoric acid according to the mass ratio of 1-2-30-70, adding 200-300ml of deionized water, keeping the temperature in the triangular flask at 80-90 ℃, and stirring for 15-20h to obtain the preposed carbon nitride-based copper with the template removed;
s5-2, washing for later use
According to the mass ratio of 1:50 to 70, washing the front copper nitride with the template removed in a three-neck bottle filled with deionized water for 10 to 20min, then washing in a three-neck bottle filled with absolute ethyl alcohol for 10 to 20min, and drying the washed front copper nitride in an electric heating constant-temperature air-blast drying box for 20 to 30min to obtain a copper nitride-based material; wherein the temperature of the electric heating constant temperature air drying box is 100 to 130 ℃.
Description of the drawings: in order to avoid introducing new impurities to generate other influences on the catalytic effect and destroy the structure of carbon nitride due to unclean template removal, the template is removed by adopting sodium hydroxide or hydrofluoric acid.
Furthermore, the concentration of the sodium hydroxide is 2.1 to 3.0mol/L, and the concentration of the hydrofluoric acid is 1.5 to 2.5mol/L.
Description of the drawings: the sodium hydroxide and the hydrofluoric acid can react with the template agent on the premise of not influencing the structure of the carbon nitride material to fully remove the template agent, so that the catalytic performance of the catalytic material is improved.
Compared with the prior art, the preparation method is simple, stable C-N bonds can be obtained by applying the carbon nitride micro powder to the preparation process of the carbon nitride-based copper catalytic material so as to further improve the catalytic stability of the carbon nitride-based copper catalytic material, and on the other hand, the structure of the prepared carbon nitride micro powder synthetic product is adjusted by using the template agent, so that the catalytic material with higher specific surface area and pore area is prepared, and the adsorption capacity of the carbon nitride-based copper on pollutants in sewage is improved.
Detailed Description
The present invention will be described in further detail with reference to specific embodiments thereof, so as to better illustrate the advantages thereof.
Example 1
A preparation method of carbon nitride-based copper material for ozone catalytic oxidation water treatment comprises the following steps:
s1, preparation of carbon nitride micro powder
Placing dicyandiamide as target material 10cm above a placing plate under microwave nitrogen plasma equipment, and controlling the gas pressure at 4.0kPa and the nitrogen flow rate at 40cm 3 Reacting for 30min under the condition that the microwave power is 450W, and obtaining carbon nitride micro powder after the reaction is finished;
s2, preparing copper-based blending liquid
S2-1, adding 2g of carbon nitride micro powder into a flask filled with 70ml of ethanol solution, heating to 80 ℃, fully stirring for 20min, and standing for 10min to obtain a carbon nitride precursor solution;
s2-2, and mixing the components in a mass ratio of 1:1, weighing 1.0g of mixed powder of copper acetate and copper chloride, adding the mixed powder into a carbon nitride precursor solution, stirring for 20min, and standing for 5min to obtain a copper-based blending solution;
s3, drying
Putting the copper-based blend liquid into an electric heating constant-temperature air drying oven, and drying for 10 hours while keeping the temperature in the drying oven at 70 ℃ to obtain a dry mixture;
s4, calcining
The dried mixture is calcined: heating to 400 ℃ at a heating rate of 5 ℃/min under the nitrogen protection atmosphere, keeping for 3h, and then cooling to room temperature to obtain preposed carbon nitride-based copper;
s5, post-processing
Heating the preposed carbon nitride-based copper to 550 ℃ at the heating rate of 15 ℃ in the nitrogen protective atmosphere, carrying out secondary calcination treatment for 0.5h, and cooling to room temperature to obtain the carbon nitride-based copper catalytic material.
Example 2
A preparation method of a carbon nitride-based copper material for ozone catalytic oxidation water treatment comprises the following steps:
s1, preparation of carbon nitride micro powder
Melamine is used as a target material and is placed at a position 12cm above a placing plate under microwave nitrogen plasma equipment, the air pressure is 4.3kPa, and the nitrogen flow rate is 45cm 3 Reacting for 20min under the conditions that the microwave power is 470W and the reaction time is 20min to obtain carbon nitride micro powder after the reaction is finished;
s2, mixing the solution
S2-1, adding 3g of carbon nitride micro powder into a flask filled with 80ml of ethanol solution, heating to 85 ℃, fully stirring for 25min, and standing for 7min to obtain a carbon nitride precursor solution;
s2-2, and mixing the components in a mass ratio of 1:1.3, weighing 2.0g of mixed powder of copper acetate and copper chloride, adding the mixed powder into the carbon nitride precursor solution, stirring for 25min, and standing for 8min to obtain copper-based blending solution;
s3, drying
Putting the copper-based blend liquid into an electric heating constant-temperature air drying oven, keeping the temperature in the drying oven at 80 ℃, and drying for 13 hours to obtain a dry mixture;
s4, calcining
Calcining the dry mixture: heating to 450 ℃ at a heating rate of 8 ℃/min under the protection of nitrogen, keeping for 2h, and then cooling to room temperature to obtain the preposed carbon nitride-based copper;
s5, post-processing
Heating the preposed carbon nitride-based copper to 580 ℃ at the heating rate of 18 ℃ in the nitrogen protective atmosphere, carrying out secondary calcination treatment for 0.7h, and cooling to room temperature to obtain the carbon nitride-based copper catalytic material.
Example 3
A preparation method of carbon nitride-based copper material for ozone catalytic oxidation water treatment comprises the following steps:
s1, preparation of carbon nitride micro powder
Placing urea as target material 15cm above a placing plate under microwave nitrogen plasma equipment, under the conditions of 4.5kPa of air pressure and 50cm of nitrogen flow rate 3 Reacting for 10min under the conditions of 500W of microwave power and 500W of reaction time to obtain carbon nitride micro powder after the reaction is finished;
s2, mixing liquid
S2-1, adding 5g of carbon nitride micro powder into a flask filled with 100ml of ethanol solution, heating to 90 ℃, fully stirring for 30min, and standing for 5min to obtain a carbon nitride precursor solution;
s2-2, mixing the components in a mass ratio of 1:1.5, weighing 2.5g of mixed powder of copper acetate and copper chloride, adding the mixed powder into a carbon nitride precursor solution, stirring for 30min, and standing for 10min to obtain a copper-based blend solution;
s3, drying
Putting the copper-based blend solution into an electric heating constant-temperature air drying oven, keeping the temperature in the drying oven at 90 ℃, and drying for 15 hours to obtain a dry mixture;
s4, calcining
The dried mixture is calcined: heating to 500 ℃ at a heating rate of 10 ℃/min under the protection of nitrogen, keeping for 1.5h, and then cooling to room temperature to obtain the preposed carbon nitride-based copper;
s5, post-processing
Heating the preposed carbon nitride-based copper to 600 ℃ at the heating rate of 20 ℃ in the nitrogen protective atmosphere, carrying out secondary calcination treatment for 1h, and cooling to room temperature to obtain the carbon nitride-based copper catalytic material.
Example 4
The difference from the embodiment 1 is that:
in the step S2-1, the method for preparing the carbon nitride precursor solution by using the carbon nitride micro powder comprises the following steps:
according to the mass ratio of 5:1, placing the template agent and the aqueous solution into a flask, heating to 80 ℃, fully stirring for 20min, standing for 5min, adding 2g of carbon nitride micro powder, and fully stirring for 20min to obtain a carbon nitride precursor solution; the template agent specifically adopts nano silicon oxide pellets;
in step S5, the post-processing method includes:
s5-1, template removal
Placing the preposed carbon nitride-based copper in a triangular flask filled with sodium hydroxide according to the mass ratio of 1; wherein the concentration of the sodium hydroxide is 2.1mol/L;
s5-2, washing for later use
According to the mass ratio of 1:50, taking the front copper nitride based on template removal, placing the front copper nitride based on template removal in a three-mouth bottle filled with deionized water, washing for 10min, placing the three-mouth bottle filled with absolute ethyl alcohol, washing for 10min, placing the front copper nitride based on template removal in an electric heating constant temperature blast drying oven, and drying for 20min to obtain a copper nitride based on carbon nitride; wherein the temperature of the electric heating constant temperature air blast drying oven is 100 ℃.
Example 5
The difference from the embodiment 2 is that:
in the step S2-1, the method for preparing the carbon nitride precursor solution by using the carbon nitride micro powder comprises the following steps:
according to the mass ratio of 1:1, placing the template agent and the aqueous solution in a flask, heating to 85 ℃, fully stirring for 20min, standing for 8min, adding 3g of carbon nitride micro powder, and fully stirring for 25min to obtain a carbon nitride precursor solution; the template agent is silica sol;
in step S5, the post-processing method includes:
s5-1, template removal
Placing the preposed carbon nitride-based copper in a triangular flask filled with sodium hydroxide according to the mass ratio of 1; wherein the concentration of the sodium hydroxide is 3.0mol/L;
s5-2, washing for later use
According to the mass ratio of 1:60, taking the front copper nitride based on template removal, placing the front copper nitride based on template removal in a three-mouth bottle filled with deionized water, washing for 15min, placing the three-mouth bottle filled with absolute ethyl alcohol, washing for 15min, placing the washed front copper nitride based on carbon nitride in an electric heating constant temperature blast drying oven, and drying for 25min to obtain a copper nitride based on carbon nitride; wherein the temperature of the electric heating constant temperature air blast drying oven is 120 ℃.
Example 6
The difference from the embodiment 2 is that:
in the step S2-1, the method for preparing the carbon nitride precursor solution by using the carbon nitride micro powder comprises the following steps:
according to the mass ratio of 1:2, placing the template agent and the aqueous solution into a flask, heating to 90 ℃, fully stirring for 30min, standing for 10min, adding 5g of carbon nitride micro powder, and fully stirring for 30min to obtain a carbon nitride precursor solution; the template agent specifically adopts SBA-15 mesoporous molecular sieve;
in step S5, the post-processing method includes:
s5-1, template removal
Taking the preposed carbon nitride-based copper according to the mass ratio of 2; wherein the concentration of hydrofluoric acid is 1.5mol/L;
s5-2, washing for later use
According to the mass ratio of 1:70, washing the preposed carbon nitride-based copper without the template in a three-mouth bottle filled with deionized water for 20min, then washing in a three-mouth bottle filled with absolute ethyl alcohol for 20min, and drying the washed preposed carbon nitride-based copper in an electric heating constant temperature blast drying oven for 30min to obtain a carbon nitride-based copper material; wherein, the temperature of the electric heating constant temperature air blast drying oven is 130 ℃.
Example 7
The difference from example 6 is that the concentration of hydrofluoric acid was 2.5mol/L.
Examples of the experiments
Applying the carbon nitride-based copper material prepared by the methods of examples 1 to 6 to a catalytic treatment test of degrading oxalic acid pollutants by ozone;
preparing 7 groups of pollutants with the initial concentration of oxalic acid of 100mg/L, respectively introducing ozone with the dose of 0.25g/L into the 7 groups of pollutants, respectively adding carbon nitride-based copper materials prepared in the examples 1 to 6 with the dose of 0.16g/L into 6 groups of pollutants in a one-to-one correspondence manner, reacting for 30min, and detecting the concentration of the pollutants; group 7 is set as comparative example: directly reacting for 30min without adding carbon nitride-based copper material;
calculating to obtain the degradation rate shown in the table 1;
table 1: degradation rate of ozone degradation of oxalic acid pollutants of each group
| Carbon nitride based copper material | The degradation rate of ozone% |
| Example 1 preparation | 89.3 |
| Example 2 preparation | 91.7 |
| Example 3 preparation | 88.9 |
| Example 4 preparation | 97.8 |
| Example 5 preparation | 98.6 |
| Example 6 preparation | 97.5 |
| Comparative example 1: ozone alone degradation | 5.3 |
And (4) conclusion: the carbon nitride-based copper materials prepared by the methods of examples 1 to 6 show high ozone catalytic efficiency. The catalytic efficiency of the carbon nitride-based copper material prepared in the embodiments 1, 2 and 3 to pollutants in an ozone system can be stabilized at about 90%, so that the carbon nitride-based copper material prepared by the method has high catalytic stability; while the catalytic efficiency of the carbon nitride-based copper material prepared in the embodiments 4, 5 and 6 to pollutants in an ozone system reaches about 98%, it can be seen that the addition of the template agent can increase the specific surface area and the pore area of the carbon nitride-based copper material, so that the carbon nitride-based copper material has more excellent adsorption performance, and further a more excellent catalytic effect is achieved.
Claims (9)
1. A preparation method of a carbon nitride-based copper material for ozone catalytic oxidation water treatment is characterized by comprising the following steps:
s1, preparation of carbon nitride micro powder
Placing the graphite-phase carbon nitride precursor as a target material over a placing plate 10-15cm below microwave nitrogen plasma equipment, adjusting the distance between the placing plate and the plasma, starting the microwave nitrogen plasma equipment for reaction, and obtaining carbon nitride micro powder after the reaction is finished;
s2, preparing copper-based blending liquid
S2-1, preparing 2-5 g of carbon nitride micro powder into a carbon nitride precursor solution;
s2-2, and mixing the components in a mass ratio of 1:1 to 1.5, weighing 1.0 to 2.5g of mixed powder of copper acetate and copper chloride, adding the mixed powder into a carbon nitride precursor solution, stirring for 20 to 30min, and standing for 5 to 10min to obtain a copper-based mixed solution;
s3, drying
Putting the copper-based blend liquid into an electric heating constant-temperature air drying oven, keeping the temperature in the drying oven at 70-90 ℃, and drying for 10-15h to obtain a dry mixture;
s4, calcining
The dried mixture is calcined: raising the temperature to 400-500 ℃ at a heating rate of 5-10 ℃/min under the nitrogen protection atmosphere, keeping the temperature for 1.5-3 h, and then cooling to room temperature to obtain the preposed carbon nitride-based copper;
s5, post-processing
And carrying out post-treatment on the preposed carbon nitride-based copper to obtain the carbon nitride-based copper material.
2. The method for preparing the carbon-based copper nitride material for water treatment by ozone catalytic oxidation according to claim 1, wherein the graphite-phase carbon nitride precursor is any one of dicyanodiamine, melamine and urea.
3. The preparation method of the carbon-based copper nitride material for ozone catalytic oxidation water treatment according to claim 1, wherein in the step S1, reaction parameters are as follows: the air pressure is 4.0 to 4.5kPa, and the nitrogen flow rate is 40 to 50cm 3 Min, microwave power of 450 to 500W and reaction time of 10 to 30min.
4. The method for preparing the carbon nitride-based copper material for ozone catalytic oxidation water treatment according to claim 1, wherein in the step S2-1, the method for preparing the carbon nitride precursor solution from the carbon nitride micro powder comprises the following steps: adding 2-5g of carbon nitride micropowder into a flask filled with 70-100ml of ethanol solution, heating to 80-90 ℃, fully stirring for 20-30min, and standing for 5-10min to obtain a carbon nitride precursor solution.
5. The method for preparing the carbon-based copper nitride material for ozone catalytic oxidation water treatment according to claim 1, wherein in the step S5, the post-treatment method comprises the following steps: heating the preposed carbon nitride-based copper to 550-600 ℃ at a heating rate of 15-20 ℃ in a nitrogen protective atmosphere, carrying out secondary calcination treatment for 0.5-1h, and cooling to room temperature to obtain the carbon nitride-based copper catalytic material.
6. The method for preparing a carbon nitride-based copper material for ozone catalytic oxidation water treatment according to claim 1, wherein in step S2-1, the method for preparing the carbon nitride precursor solution from the carbon nitride micro powder comprises: according to the mass ratio of 5: and (3) putting the template and the aqueous solution into a flask according to the proportion of 1 to 10, heating to 80 to 90 ℃, fully stirring for 20 to 30min, standing for 5 to 10min, then adding 2 to 5g of carbon nitride micropowder, and fully stirring for 20 to 30min to obtain a carbon nitride precursor solution.
7. The method for preparing the carbon-based copper nitride material for water treatment by catalytic oxidation of ozone according to claim 6, wherein the template is selected from one of nano silica spheres, silica sol and SBA-15 mesoporous molecular sieves.
8. The method for preparing the carbon-based copper nitride material for ozone catalytic oxidation water treatment according to claim 6, wherein in the step S5, the post-treatment method comprises the following steps:
s5-1, template removal
Placing the preposed carbon nitride-based copper in a triangular flask filled with sodium hydroxide or hydrofluoric acid according to the mass ratio of 1-2-30-70, adding 200-300ml of deionized water, keeping the temperature in the triangular flask at 80-90 ℃, and stirring for 15-20h to obtain the preposed carbon nitride-based copper with the template removed;
s5-2, washing for later use
According to the mass ratio of 1:50 to 70, washing the preposed carbon nitride copper without the template in a three-neck bottle filled with deionized water for 10 to 20min, then washing in a three-neck bottle filled with absolute ethyl alcohol for 10 to 200 min, and drying the washed preposed carbon nitride in an electric heating constant-temperature air-blast drying box for 20 to 30min to obtain a carbon nitride copper material; wherein the temperature of the electric heating constant temperature air drying box is 100 to 130 ℃.
9. The method for preparing the carbon-based copper nitride material for water treatment by ozone catalytic oxidation according to claim 8, wherein the concentration of the sodium hydroxide is 2.1 to 3.0mol/L, and the concentration of the hydrofluoric acid is 1.5 to 2.5mol/L.
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