CN113058542A - Preparation method and application of copper oxide @ hydrotalcite hybrid material - Google Patents
Preparation method and application of copper oxide @ hydrotalcite hybrid material Download PDFInfo
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- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/02—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
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- B01J20/08—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising oxides or hydroxides of metals not provided for in group B01J20/04 comprising aluminium oxide or hydroxide; comprising bauxite
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/28—Treatment of water, waste water, or sewage by sorption
- C02F1/288—Treatment of water, waste water, or sewage by sorption using composite sorbents, e.g. coated, impregnated, multi-layered
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- 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
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
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- C02F2101/00—Nature of the contaminant
- C02F2101/30—Organic compounds
- C02F2101/34—Organic compounds containing oxygen
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- C02F2101/00—Nature of the contaminant
- C02F2101/30—Organic compounds
- C02F2101/38—Organic compounds containing nitrogen
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2101/00—Nature of the contaminant
- C02F2101/30—Organic compounds
- C02F2101/40—Organic compounds containing sulfur
Abstract
The invention discloses a preparation method and application of a copper oxide @ hydrotalcite hybrid material, wherein the preparation method comprises the following steps: firstly, preparing a copper oxide template with a microsphere appearance in advance, then ultrasonically dispersing the copper oxide template in water, co-precipitating a metal salt solution and an alkali liquor in a copper oxide dispersion system, and carrying out crystallization growth at a high temperature to obtain a hybridized copper oxide @ hydrotalcite material; the material is applied to adsorbing Congo red dye. According to the copper oxide @ hydrotalcite material prepared by the invention, on one hand, the modified hybrid material has a microsphere shape, and the specific surface area is obviously increased compared with that of the hybrid material before being unmodified; on the other hand, the modified hybrid material has more excellent Congo red adsorption performance, and the removal rate of the dye in the water body is improved.
Description
Technical Field
The invention belongs to the field of water adsorption treatment technology and environmental management, and particularly relates to a preparation method and application of a copper oxide @ hydrotalcite hybrid material.
Background
Hydrotalcite (LDH) based materials are two-dimensional inorganic materials with a unique layer structure, the chemical components of the layer are mainly metal ions with positive charges, and negative ion groups with negative charges are arranged between layers. Because the typical structural advantage of the hydrotalcite endows the hydrotalcite with electrostatic effect, ion exchange effect and the like on the pollutants of the dye, the hydrotalcite has more research and application in the aspect of adsorbing and removing the pollutants in the water body.
When the pure hydrotalcite is used as an adsorbent, the defects of low adsorption efficiency, limited adsorption capacity and the like exist, and the metal positive charge density, interlayer spacing and growth morphology on the surface of the hydrotalcite can influence the performance of the hydrotalcite to a certain extent, so that the existing adsorption material based on the hydrotalcite needs to be modified and designed, and the use value of the adsorption material as the adsorbent is improved.
In recent years, a research direction for regulating and controlling the functionality of hydrotalcite by introducing a modification method of a template to control the growth morphology of the hydrotalcite appears, for example, the hydrotalcite is grown outside the nanofiber by adopting a hydrothermal method by adopting a nanowire as the template, so that a nanofiber-hydrotalcite composite material is obtained, and the hydrotalcite-based composite material has better efficiency when being used for adsorbing heavy metal ions in a water body; in addition, the research is that the specific surface area and pore volume of the prepared material are larger by introducing one-step hybridization of graphene oxide and hydrotalcite, and the adsorption application is more facilitated. However, the current research on the adsorbent material has several defects: (1) the preparation process of the material is complicated, and the reaction conditions required by the experiment are not suitable for large-scale production; (2) the preparation process uses more organic solvents, and is easy to cause pollution and the like. Therefore, designing an adsorbent material with simple manufacturing process, low production cost and no self-pollution is a direction of important consideration in subsequent research.
Disclosure of Invention
In view of the above, the invention aims to provide a preparation method and an adsorption application of a copper oxide @ hydrotalcite hybrid material, and when the hydrotalcite-based modified material prepared by the method is used as an adsorbent, the hydrotalcite-based modified material has the advantages of high adsorption efficiency, good stability, low production cost and easiness in operation, and is relatively suitable for treatment of printing and dyeing wastewater in industry due to a simple preparation process; and the method can obtain the copper oxide @ hydrotalcite hybrid material with the best relative adsorption performance by changing the proportion of the copper oxide.
The preparation method of the copper oxide @ hydrotalcite hybrid material comprises the following steps:
step 1: and (3) preparing a copper oxide template with a microsphere shape in advance.
Weighing copper sulfate pentahydrate in a flask, adding deionized water, stirring for dissolving, dissolving ammonium oxalate in the deionized water to prepare a solution, quickly transferring the ammonium oxalate solution into the flask, heating to 70 ℃, magnetically stirring for 3 hours, and then performing suction filtration, washing and drying to obtain a copper oxalate precursor; and finally, putting the copper oxalate precursor obtained by the reaction into a muffle furnace, and calcining for 2 hours at 500 ℃ to obtain a copper oxide template sample.
Step 2: preparing the copper oxide @ hydrotalcite material.
Dispersing the prepared copper oxide sample in deionized water, adding the obtained product into a four-neck flask after ultrasonic dispersion, preparing a sodium nitrate solution, adding the obtained product into the flask, preparing a mixed metal salt solution of magnesium nitrate hexahydrate and aluminum nitrate nonahydrate, quickly adding the mixed metal salt solution of magnesium and aluminum into the flask, stirring, preparing a sodium hydroxide alkali liquor with a certain concentration, titrating the metal salt solution of magnesium and aluminum and the alkali liquor into the flask simultaneously under the protection of nitrogen atmosphere, quickly stirring in the titration process, controlling the titration rate of the alkali liquor so that the pH value of a reaction system in the titration process is 10, stirring for 1 hour after the titration is finished, heating to 75 ℃, standing and aging for 24 hours, performing suction filtration, washing and drying to obtain a hybrid sample precursor; and finally, placing the hybrid sample precursor prepared by the reaction in a muffle furnace at 500 ℃ to calcine for 4 hours to obtain the copper oxide @ hydrotalcite hybrid material.
Preferably, the mole ratio of the copper sulfate pentahydrate to the ammonium oxalate added in the step 1 is 1; the molar concentrations of copper ions and oxalate anions in deionized water are both 0.1 mol/L.
Preferably, the reaction in step 1 is carried out after the temperature is raised to 70 ℃ in advance; the stirring rate was kept constant during the reaction.
Preferably, the specific gravity of the copper oxide sample in the step 2 is 3-20 wt%; the ultrasonic dispersion time is 0.5-3 hours; the concentration of the sodium nitrate solution is 2 mol/L; the molar ratio of magnesium ions to aluminum ions in the solution is 3: 1; the concentration of the sodium hydroxide solution is 2 mol/L; and keeping the pH value of 9.8-10.2 in the reaction process.
Preferably, the deionized water used in the experimental reaction in step 2 needs to be boiled to remove CO2Processing; at the same time, the reaction system is strictly controlled at the strict N2The method is carried out under the protection of atmosphere.
The copper oxide @ hydrotalcite hybrid material prepared by the preparation method disclosed by the invention is applied to adsorption of Congo red dye.
The method for adsorbing Congo red dye by using the copper oxide @ hydrotalcite hybrid material disclosed by the invention uses the hybrid material; carrying out an adsorption test in a water bath constant temperature oscillator which is protected from light; the oscillation rate was 150 rpm; the shaking time is 360 minutes; the shaking temperature was room temperature.
The mechanism of the method is as follows: synthesizing and preparing CuO in a controllable microsphere shape through inorganic chemical reaction; then carrying out hybrid growth of hydrotalcite and copper oxide together by using CuO as a template through a coprecipitation method; and finally, calcining in a muffle furnace to obtain the modified copper oxide @ hydrotalcite hybrid material.
Compared with the prior art, the invention has the beneficial effects that:
compared with the existing research on the aspect that hydrotalcite hybridization modification is used for adsorbing Congo red dye, the method combines the characteristic that the spherical morphology has the maximum specific surface area, and takes copper oxide microspheres as a template to directionally regulate the hybridization growth of hydrotalcite to form the microsphere morphology, so that the obtained hybridization modified material has the relatively maximum specific surface area, and the maximized adsorption performance of the material is realized. By adjusting the relative content of the copper oxide template, the optimal hybridization proportion for high-efficiency adsorption is explored, and the preparation method and experimental parameters of the hybrid material with the optimal adsorption performance are obtained.
Drawings
FIG. 1 is an X-ray diffraction pattern of the prepared CuO template, calcined hydrotalcite derived oxide and hybrid modified copper oxide @ hydrotalcite.
FIG. 2 is an FTIR plot of prepared CuO template, hydrotalcite calcined derivative oxide and hybrid modified copper oxide @ hydrotalcite.
Fig. 3 is an SEM photograph of the prepared hybrid modified copper oxide @ hydrotalcite.
Fig. 4 is a TEM photograph of the prepared hybrid modified copper oxide @ hydrotalcite.
FIG. 5 shows Congo red adsorption performance of the prepared CuO template, calcined hydrotalcite derived oxide and hybrid modified copper oxide @ hydrotalcite.
Detailed Description
The present invention will be described in further detail with reference to the accompanying drawings and specific embodiments.
Example 1
A. 2.5g of copper sulfate pentahydrate (CuSO) are weighed out4·5H2O) reagent was dissolved in 100mL of water, and 1.42g of ammonium oxalate ((NH)4)2C2O4·H2O) is dissolved in 100mL of water, then the ammonium oxalate solution is rapidly added into the copper sulfate solution, stirred for 3 hours at 70 ℃, filtered, washed and dried to obtain CuC2O4·H2An O precursor; the obtained CuC2O4·H2And calcining the O precursor in a muffle furnace at 500 ℃ for 2 hours to obtain a CuO sample with a microsphere morphology.
B. Dispersing 0.06g of the CuO sample obtained in the step A in 20mL of deionized water, performing ultrasonic dispersion for 0.5 hour, adding the mixture into a four-neck flask, weighing 4.25g of sodium nitrate, dissolving the sodium nitrate in 30mL of deionized water, then respectively dissolving 9.62g of magnesium nitrate hexahydrate and 4.69g of aluminum nitrate nonahydrate in 50mL of deionized water, then rapidly adding the sodium nitrate solution into the flask, stirring, preparing 2mol/L of sodium hydroxide alkaline solution, titrating the magnesium and aluminum metal salt solution and the alkaline solution into the flask simultaneously under the protection of nitrogen atmosphere, rapidly stirring in the titration process, controlling the titration rate of the alkaline solution to ensure that the pH value of a reaction system in the titration process is 9.8-10.2, stirring for 1 hour after the titration is completed, then heating to 75 ℃, standing for 24 hours, performing suction filtration, water washing and drying to obtain a hybrid sample precursor; and finally, placing the hybrid sample precursor prepared by the reaction in a muffle furnace at 500 ℃ to calcine for 4 hours to obtain a copper oxide @ hydrotalcite sample.
And B, putting 50mg of the copper oxide @ hydrotalcite hybrid material prepared in the step B into a 250mL reagent bottle with a small opening, adding a Congo red solution with the initial concentration of 50mg/L into the bottle, oscillating at the constant temperature of 150rpm for 360 minutes at room temperature, sampling at regular intervals to determine the residual concentration of the Congo red, and calculating to obtain the maximum adsorption capacity of 327 mg/g.
Example 2
A. 2.5g of copper sulfate pentahydrate (CuSO) are weighed out4·5H2O) reagent was dissolved in 100mL of water, and 1.42g of ammonium oxalate ((NH)4)2C2O4·H2O) is dissolved in 100mL of water, then the ammonium oxalate solution is rapidly added into the copper sulfate solution, stirred for 3 hours at 70 ℃, filtered, washed and dried to obtain CuC2O4·H2An O precursor; the obtained CuC2O4·H2And calcining the O precursor in a muffle furnace at 500 ℃ for 2 hours to obtain a copper oxide sample with a microsphere morphology.
B. Dispersing 0.1g of the CuO sample obtained in the step A in 20mL of deionized water, adding the mixture into a four-neck flask after ultrasonic dispersion is carried out for 1 hour, weighing 4.25g of sodium nitrate to dissolve in 30mL of deionized water, then respectively dissolving 9.62g of magnesium nitrate hexahydrate and 4.69g of aluminum nitrate nonahydrate in 50mL of deionized water, then quickly adding the sodium nitrate solution into the flask for stirring, additionally preparing 2mol/L of sodium hydroxide alkaline solution, titrating the metal salt solution of magnesium and aluminum and the alkaline solution into the flask simultaneously under the protection of nitrogen atmosphere, quickly stirring in the titration process, controlling the titration rate of the alkaline solution to ensure that the pH value of a reaction system in the titration process is 9.8-10.2, stirring for 1 hour after the titration is finished, then heating to 75 ℃, standing and aging for 24 hours, carrying out suction filtration, water washing and drying to obtain a hybrid sample precursor; and finally, placing the hybrid sample precursor prepared by the reaction in a muffle furnace at 500 ℃ to calcine for 4 hours to obtain the copper oxide @ hydrotalcite hybrid material.
And B, putting 50mg of the copper oxide @ hydrotalcite hybrid material prepared in the step B into a 250mL reagent bottle with a small opening, adding a Congo red solution with the initial concentration of 50mg/L into the bottle, oscillating at the constant temperature of 150rpm for 360 minutes at room temperature, sampling at regular intervals to determine the residual concentration of the Congo red, and calculating to obtain the maximum adsorption capacity of 490 mg/g.
Example 3
A. 2.5g of copper sulfate pentahydrate (CuSO) are weighed out4·5H2O) reagent was dissolved in 100mL of water, and 1.42g of ammonium oxalate ((NH)4)2C2O4·H2O) is dissolved in 100mL of water, then the ammonium oxalate solution is rapidly added into the copper sulfate solution, stirred for 3 hours at 70 ℃, filtered, washed and dried to obtain CuC2O4·H2An O precursor; the obtained CuC2O4·H2And calcining the O precursor in a muffle furnace at 500 ℃ for 2 hours to obtain a CuO sample with a microsphere morphology.
B. Dispersing 0.2g of the CuO sample obtained in the step A in 20mL of deionized water, adding the mixture into a four-neck flask after ultrasonic dispersion is carried out for 2 hours, weighing 4.25g of sodium nitrate to dissolve in 30mL of deionized water, then respectively dissolving 9.62g of magnesium nitrate hexahydrate and 4.69g of aluminum nitrate nonahydrate in 50mL of deionized water, then quickly adding the sodium nitrate solution into the flask for stirring, additionally preparing 2mol/L of sodium hydroxide alkaline solution, titrating the metal salt solution of magnesium and aluminum and the alkaline solution into the flask simultaneously under the protection of nitrogen atmosphere, quickly stirring in the titration process, controlling the titration rate of the alkaline solution to enable the pH of the reaction system in the titration process to be 9.8-10, stirring for 1 hour after the titration is finished, then heating to 75 ℃, standing and aging for 24 hours, carrying out suction filtration, water washing and drying to obtain a hybrid sample precursor; and finally, placing the hybrid sample precursor prepared by the reaction in a muffle furnace at 500 ℃ to calcine for 4 hours to obtain the copper oxide @ hydrotalcite hybrid material.
And B, putting 50mg of the copper oxide @ hydrotalcite hybrid material prepared in the step B into a 250mL reagent bottle with a small opening, adding a Congo red solution with the initial concentration of 50mg/L into the bottle, oscillating at the constant temperature of 150rpm for 360 minutes at room temperature, sampling at regular intervals to determine the residual concentration of the Congo red, and calculating to obtain the maximum adsorption capacity of 540 mg/g.
Example 4
A. 2.5g of copper sulfate pentahydrate (CuSO) are weighed out4·5H2O) reagent was dissolved in 100mL of water, and 1.42g of ammonium oxalate ((NH)4)2C2O4·H2O) is dissolved in 100mL of water, then the ammonium oxalate solution is rapidly added into the copper sulfate solution, stirred for 3 hours at 70 ℃, filtered, washed and dried to obtain CuC2O4·H2An O precursor; the obtained CuC2O4·H2And calcining the O precursor in a muffle furnace at 500 ℃ for 2 hours to obtain a CuO sample with a microsphere morphology.
B. Dispersing 0.4g of the CuO sample obtained in the step A in 20mL of deionized water, adding the mixture into a four-neck flask after ultrasonic dispersion is carried out for 3 hours, weighing 4.25g of sodium nitrate to dissolve in 30mL of deionized water, then respectively dissolving 9.62g of magnesium nitrate hexahydrate and 4.69g of aluminum nitrate nonahydrate in 50mL of deionized water, then quickly adding the sodium nitrate solution into the flask for stirring, additionally preparing 2mol/L of sodium hydroxide alkaline solution, titrating the metal salt solution of magnesium and aluminum and the alkaline solution into the flask simultaneously under the protection of nitrogen atmosphere, quickly stirring in the titration process, controlling the titration rate of the alkaline solution to ensure that the pH value of a reaction system in the titration process is 9.8-10.1, stirring for 1 hour after the titration is finished, then heating to 75 ℃, standing and aging for 24 hours, carrying out suction filtration, water washing and drying to obtain a hybrid sample precursor; and finally, placing the hybrid sample precursor prepared by the reaction in a muffle furnace at 500 ℃ to calcine for 4 hours to obtain the copper oxide @ hydrotalcite hybrid material.
And B, putting 50mg of the copper oxide @ hydrotalcite hybrid material prepared in the step B into a 250mL reagent bottle with a small opening, adding a Congo red solution with the initial concentration of 50mg/L into the bottle, oscillating at the constant temperature of 150rpm for 360 minutes at room temperature, sampling at regular intervals to determine the residual concentration of the Congo red, and calculating to obtain the maximum adsorption capacity of 378 mg/g.
FIG. 1 is an X-ray diffraction pattern of the prepared CuO template, calcined hydrotalcite derived oxide and hybrid modified copper oxide @ hydrotalcite. As can be seen from the figure, the hybridized copper oxide @ hydrotalcite clearly shows the crystal face diffraction peaks of oxides derived from calcined hydrotalcite and CuO, which indicates that the obtained product is the required material after hybridization modification.
FIG. 2 is an FTIR plot of prepared CuO template, hydrotalcite calcined derivative oxide and hybrid modified copper oxide @ hydrotalcite. As can be seen, 657cm-1At points corresponding to the vibration peaks of the Mg-O metal oxide bond, 538 and 443cm-1Corresponding to the stretching vibration peaks of the Cu-O functional group along the (002) and (111) crystal planes.
Fig. 3 is an SEM photograph of the prepared hybrid modified copper oxide @ hydrotalcite. The appearance of the copper oxide @ hydrotalcite sample is mainly microspherical, the particle size of the microspheres is uniform, small gaps are dispersed on the surface of the microspheres, the size of the microspheres is approximately 1-3 micrometers, the specific surface area of the material is maximized due to the appearance of the microspheres, and the adsorption performance of the material is improved. As can be seen from the TEM photograph of fig. 4, CuO mainly acts as a template to control the morphology inside, and hydrotalcite sheets generated after calcination grow on the surface of the template to form a core-shell structure.
FIG. 5 shows Congo red adsorption performance of the prepared copper oxide @ hydrotalcite hybrid material; therefore, the modified hybrid material can quickly establish adsorption balance, the adsorption balance can be achieved within 20 minutes, the adsorption capacity after the adsorption balance is achieved is higher than that of the material before the modification, and the modified material is proved to have better adsorption performance.
The experiment also proves that: the adsorption performance of the copper oxide @ hydrotalcite hybrid material prepared by the method is better than that of pure hydrotalcite, and the adsorption stability of the copper oxide @ hydrotalcite hybrid material in different acid-base environments is better.
The above description is only for the purpose of illustrating the preferred embodiments of the present invention and is not to be construed as limiting the invention, and any modifications, equivalents, improvements and the like that fall within the spirit and principle of the present invention are intended to be included therein.
Claims (7)
1. The preparation method of the copper oxide @ hydrotalcite hybrid material is characterized by comprising the following steps of:
step 1: preparing a copper oxide template with a microsphere shape in advance:
weighing copper sulfate pentahydrate in a flask, adding deionized water, stirring for dissolving, dissolving ammonium oxalate in the deionized water to prepare a solution, quickly transferring the ammonium oxalate solution into the flask, heating to 70 ℃, magnetically stirring for 3 hours, and then performing suction filtration, washing and drying to obtain a copper oxalate precursor; finally, putting the copper oxalate precursor obtained by the reaction into a muffle furnace, and calcining for 2 hours at 500 ℃ to obtain a copper oxide template sample;
step 2: preparing a copper oxide @ hydrotalcite material;
dispersing the prepared copper oxide sample in deionized water, adding the obtained product into a four-neck flask after ultrasonic dispersion, preparing a sodium nitrate solution, adding the obtained product into the flask, preparing a mixed metal salt solution of magnesium nitrate hexahydrate and aluminum nitrate nonahydrate, quickly adding the mixed metal salt solution of magnesium and aluminum into the flask, stirring, preparing a sodium hydroxide alkali liquor with a certain concentration, titrating the metal salt solution of magnesium and aluminum and the alkali liquor into the flask simultaneously under the protection of nitrogen atmosphere, quickly stirring in the titration process, controlling the titration rate of the alkali liquor so that the pH value of a reaction system in the titration process is 10, stirring for 1 hour after the titration is finished, heating to 75 ℃, standing and aging for 24 hours, performing suction filtration, washing and drying to obtain a hybrid sample precursor; and finally, placing the hybrid sample precursor prepared by the reaction in a muffle furnace at 500 ℃ to calcine for 4 hours to obtain the copper oxide @ hydrotalcite hybrid material.
2. The preparation method of the copper oxide @ hydrotalcite hybrid material according to claim 1, wherein the molar ratio of the copper sulfate pentahydrate to the ammonium oxalate added in the step 1 is 1; the molar concentrations of copper ions and oxalate anions in deionized water are both 0.1 mol/L.
3. The preparation method of the copper oxide @ hydrotalcite hybrid material according to claim 1, wherein the reaction in the step 1 is performed after the temperature is raised to 70 ℃ in advance; the stirring rate was kept constant during the reaction.
4. The preparation method of the copper oxide @ hydrotalcite hybrid material according to claim 1, wherein the copper oxide sample in the step 2 is taken in an amount of 3 wt% to 20 wt%; the ultrasonic dispersion time is 0.5-3 hours; the concentration of the sodium nitrate solution is 2 mol/L; the molar ratio of magnesium ions to aluminum ions in the solution is 3: 1; the concentration of the sodium hydroxide solution is 2 mol/L; and keeping the pH value of 9.8-10.2 in the reaction process.
5. The method for preparing the copper oxide @ hydrotalcite hybrid material according to claim 1, wherein the deionized water used in the experimental reaction in the step 2 needs to be boiled to remove CO2Processing; at the same time, the reaction system is strictly controlled at the strict N2The method is carried out under the protection of atmosphere.
6. The application of the copper oxide @ hydrotalcite hybrid material prepared by the preparation method of any one of claims 1 to 5 in adsorbing Congo red dye.
7. A method for adsorbing Congo red dye by a copper oxide @ hydrotalcite hybrid material is characterized in that an adsorption test is carried out in a water bath constant temperature oscillator which is protected from light; the oscillation rate was 150 rpm; the shaking time is 360 minutes; the shaking temperature was room temperature.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN116082822A (en) * | 2023-01-17 | 2023-05-09 | 盛鼎高新材料有限公司 | Preparation method of high-temperature-resistant halogen-free flame-retardant polyurethane elastomer |
| CN116082822B (en) * | 2023-01-17 | 2023-11-21 | 盛鼎高新材料有限公司 | Preparation method of high-temperature-resistant halogen-free flame-retardant polyurethane elastomer |
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