CN107413161B - Copper oxide/graphene composite material and preparation method and application thereof - Google Patents
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Abstract
The invention discloses a copper oxide/graphene composite material and a preparation method and application thereof, and belongs to the technical field of composite materials and air purification. According to the preparation method provided by the invention, graphene oxide obtained by a modified Hummers method is used as a carrier, copper oxide is slowly precipitated onto the graphene oxide from a prepared cuprammonium solution and is combined with an oxygen-containing group on the graphene oxide to form a stable copper oxide/graphene oxide composite material, the graphene oxide is reduced into graphene through hydrothermal reaction, and the graphene oxide/graphene oxide composite material is prepared through filtering, washing, freeze drying and calcining. The preparation method has the advantages of low price of raw materials, simple preparation process, reusability of products and the like, and has good application prospect. The copper oxide/graphene composite material can be applied to removing formaldehyde and can be recycled after simple heat treatment at the temperature of 100-150 ℃.
Description
Technical Field
The patent relates to the technical field of composite materials and air purification, in particular to a copper oxide/graphene composite material and a preparation method and application thereof.
Background
Volatile Organic Compounds (VOC) are an important factor for indoor air pollution, and among them, formaldehyde is one of the most important indoor volatile organic pollutants, which not only stimulates the respiratory system of people, but also is a carcinogenic substance, and the long-term exposure of formaldehyde seriously affects the health of human beings, especially children. Activated carbon is widely used for removing formaldehyde in air by physical adsorption, but the adsorption capacity of the activated carbon for formaldehyde is limited, and when the adsorption reaches a saturated state, the formaldehyde on the surface of the activated carbon can be diffused into the air again, so that secondary pollution is caused. Therefore, the correct way to remove formaldehyde should be to chemisorb the formaldehyde.
CN 105118682 a discloses a preparation method and application of composite particles composed of activated carbon and graphene hybrid, which fully utilizes the excellent adsorption characteristics of carbon nanomaterials and can adsorb gas or liquid hydrocarbons, however, the method still stays at the level of physical adsorption and is difficult to effectively remove adsorbed pollutants. CN 103691251B discloses a method for adsorbing and decomposing organic waste gas by graphene, which uses multi-layer graphene or modified graphene as an adsorbing material to adsorb and catalytically combust the organic waste gas, but this method needs to pretreat the organic waste gas by ultraviolet light, plasma, etc., and is complex in method and expensive in equipment price.
Disclosure of Invention
In view of the problems in the prior art, the first objective of the present invention is to provide a method for preparing a copper oxide/graphene composite material. The preparation method of the invention is a modified Hummers method (Nina i.kovtyukhova,Chem. Mater.1999,11771-778) as a carrier, slowly precipitating copper oxide onto the graphene oxide from a pre-prepared cuprammonium solution, combining with oxygen-containing groups on the graphene oxide to form a stable copper oxide/graphene oxide composite material, reducing the graphene oxide into graphene through hydrothermal reaction, filtering, washing, freeze-drying, and calcining to prepare the copper oxide/graphene composite material.
The other purpose of the invention is to provide the copper oxide/graphene composite material obtained by the preparation method, wherein the special structure, stability and high specific surface of the graphene oxide nano sheet are beneficial to improving the dispersion degree of the copper oxide, and the copper oxide is prevented from being aggregated in the precipitation process.
The invention further aims to provide application of the copper oxide/graphene composite material obtained by the preparation method. The application is mainly embodied in that the aim of removing formaldehyde is achieved by utilizing the action mechanism that formaldehyde can form formate substances on the surface of copper oxide in a chemical adsorption mode at room temperature. When the formaldehyde adsorption reaches saturation, the copper oxide/graphene composite material is only required to be added at 100-150-oAnd C, the absorbed formate substances can be decomposed into carbon dioxide and water by simple heat treatment, so that the absorbed formaldehyde is thoroughly removed.
The purpose of the invention is realized by the following technical scheme: a preparation method of a copper oxide/graphene composite material comprises the following steps:
(1) adding 1-10 parts by weight of graphene oxide into 100-1000 parts by weight of deionized water, and performing ultrasonic dispersion to obtain a graphene oxide dispersion liquid;
(2) adding 25-125 parts by weight of copper nitrate trihydrate into 100 parts by weight of deionized water, and slowly dropwise adding concentrated ammonia water while stirring to adjust the pH value to form a stable copper ammonia solution;
(3) adding the copper ammonia solution obtained in the step (2) into the graphene oxide dispersion liquid obtained in the step (1), stirring at room temperature for 30-60 min, and then continuously heating at 50-80 ℃ for 1-4 h; then transferring the reactant to a high-pressure reaction kettle, and carrying out hydrothermal reduction reaction for 2-10h at the temperature of 120-;
(4) and (4) after the reaction solution in the step (3) is cooled to room temperature, removing the supernatant, washing the solid with deionized water, performing suction filtration, naturally drying at room temperature, performing freeze drying, and calcining for 1-4 hours under the protection of argon to obtain the copper oxide/graphene composite material.
As a preferred embodiment, the graphene oxide in step (1) is obtained by a modified Hummers method.
As a preferred embodiment, the conditions of the ultrasonic treatment in the step (1) are: the ultrasonic time is 20-60min, and the ultrasonic power is 100-150W.
In a preferred embodiment, the concentration of the concentrated ammonia water in the step (2) is 12 mol/L.
In a preferred embodiment, the pH of the stabilized cuprammonium solution in step (2) is 8 to 11.
In a preferred embodiment, the stable cuprammonium solution in step (2) is [ Cu (NH)3)4(H2O)2]2+Status.
In a preferred embodiment, the autoclave in step (3) is a tetrafluoroethylene-lined autoclave.
As a preferred embodiment, the temperature range of the calcination in the step (4) is 200-550 ℃.
A preparation method of a copper oxide/graphene composite material is obtained by the preparation method.
The copper oxide/graphene composite material obtained by the preparation method can be applied to the aspect of adsorbing toxic gas molecules such as formaldehyde, and the action mechanism of formaldehyde adsorption on the surface of the copper oxide/graphene composite material is shown in figure 1. Compared with the prior art, the invention has the following advantages and effects:
the special structure, stability and high specific surface of the graphene oxide nano sheet used in the invention are beneficial to improving the dispersion degree of copper oxide and preventing the copper oxide from gathering in the precipitation process; in addition, the aim of removing formaldehyde is achieved by utilizing the action mechanism that formaldehyde can form formate substances on the surface of copper oxide in a chemical adsorption mode at room temperature, and when the formaldehyde adsorption reaches saturation, the copper oxide/graphene composite material only needs to be subjected to the treatment of 100-oAnd C, performing simple heat treatment to decompose the adsorbed formate substances into carbon dioxide and water, thereby thoroughly removing the adsorbed formaldehyde. The preparation method has the advantages of low price of raw materials, simple preparation process, reusability of products and the like, and has good application prospect.
Drawings
Fig. 1 shows an action mechanism of formaldehyde adsorbed on the surface of the copper oxide/graphene composite material.
Fig. 2 is an online formaldehyde adsorption device using a copper oxide/graphene composite material.
FIG. 3 is a graph showing the results of changes in formaldehyde adsorption rate (removal rate) with time.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the present invention will be described in further detail below with reference to the accompanying drawings and examples. It should be understood that the specific embodiments described herein are merely illustrative of the invention and are not intended to limit the invention.
Example 1:
(1) adding 2g of graphene oxide into 200mL of deionized water, and performing ultrasonic dispersion, wherein the ultrasonic treatment time is 60min, and the ultrasonic power is 150W, so as to obtain a graphene oxide dispersion liquid;
(2) adding 25g of copper nitrate trihydrate into 100mL of deionized water, slowly dropwise adding 12mol/L concentrated ammonia water while stirring to adjust the pH value to 9 to form a stable copper ammonia solution [ Cu (NH)3)4(H2O)2]2+；
(3) Adding the cuprammonium solution in the step (2) into the graphene oxide dispersion liquid in the step (1), stirring for 30min at room temperature, and then stirring at 60 DEGoHeating for 2 hours under the condition C; the reaction was then transferred to a tetrafluoroethylene lined autoclave at 180 deg.foCCarrying out hydrothermal reduction reaction for 5 h;
(4) after the reaction solution in the step (3) is cooled to room temperature, removing the supernatant, washing the solid with deionized water, performing suction filtration, naturally drying at room temperature, performing freeze drying, and then performing 350 ℃ in the presence of argonoAnd C, calcining for 2h to obtain the copper oxide/graphene composite material 1 (sample 1 in figure 3).
Example 2:
(1) adding 1g of graphene oxide into 200mL of deionized water, and performing ultrasonic dispersion for 30min at an ultrasonic power of 150W to obtain a graphene oxide dispersion liquid;
(2) adding 17g of copper nitrate trihydrate into 100mL of deionized water, slowly dropwise adding 12mol/L concentrated ammonia water while stirring to adjust the pH value to 9.5 to form a stable copper ammonia solution [ Cu (NH)3)4(H2O)2]2+；
(3) Adding the cuprammonium solution in the step (2) into the graphene oxide dispersion liquid in the step (1), stirring for 50min at room temperature, and then stirring at 70 DEGoHeating for 2 hours under the condition C; the reaction was then transferred to a tetrafluoroethylene lined autoclave at 150 foCCarrying out hydrothermal reduction reaction for 8 h;
(4) after the reaction solution in the step (3) is cooled to room temperature, removing the supernatant, washing the solid by deionized water, filtering, and performing room temperature self-purificationThen after drying, freeze-drying was performed, followed by 250 deg.f under argon protectionoAnd C, calcining for 2h to obtain the copper oxide/graphene composite material 2 (sample 2 in figure 3).
Example 3:
(1) adding 1g of graphene oxide into 200mL of deionized water, and performing ultrasonic dispersion, wherein the ultrasonic treatment time is 60min, and the ultrasonic power is 150W, so as to obtain a graphene oxide dispersion liquid;
(2) adding 10g of copper nitrate trihydrate into 100mL of deionized water, slowly dropwise adding 12mol/L concentrated ammonia water while stirring to adjust the pH value to 9.2 to form a stable copper ammonia solution [ Cu (NH)3)4(H2O)2]2+；
(3) Adding the cuprammonium solution in the step (2) into the graphene oxide dispersion liquid in the step (1), stirring at room temperature for 60min, and then stirring at 80 DEG CoHeating for 2 hours under the condition C; the reaction was then transferred to a tetrafluoroethylene lined autoclave at 180 deg.foCCarrying out hydrothermal reduction reaction for 8 h;
(4) after the reaction solution in the step (3) is cooled to room temperature, removing the supernatant, washing the solid with deionized water, performing suction filtration, naturally drying at room temperature, performing freeze drying, and then under the protection of argon gas, 450oAnd C, calcining for 2h to obtain the copper oxide/graphene composite material 3 (sample 3 in figure 3).
Comparison of the effects of examples and comparative samples
To test the formaldehyde adsorption performance of the copper oxide/graphene composite, a formaldehyde adsorption test was performed by the apparatus of fig. 2 (fixed bed catalytic reactor): 0.2g of the adsorbent was fixed in a stainless steel tube having a diameter of 8mm and a length of 40cm by means of quartz wool, and a mixed gas (volume ratio: formaldehyde/oxygen/helium =300ppm/20%/80%, for convenience of product analysis, helium was substituted for nitrogen in the air) having a concentration of 300ppm was passed through the adsorbent in the reaction tube at room temperature and a gas flow rate of 200cm3Collecting the tail gas at the outlet of the reactor every 30min by using a gas bag, detecting the gas sample by using an Agilent 7890A gas chromatograph equipped with a Thermal Conductivity Detector (TCD), wherein the carrier gas is helium, and the column is CPA Sil 5CB capillary chromatography column (inner diameter 0.53mm, length 25m, film thickness 2 μm). The change with time of the obtained formaldehyde adsorption rate (removal rate) is shown in FIG. 3. As can be seen from fig. 3, the formaldehyde adsorption rates (removal rates) of the three adsorbed samples were almost all 100% at the first 100min of formaldehyde introduction, and the formaldehyde conversion rates (adsorption rates) of the three samples were drastically decreased as the adsorption time was prolonged. When the adsorption time is 450min, the adsorption of formaldehyde gradually reaches saturation. As can be seen from fig. 3, the adsorption performance of the materials 2 and 3 is close, while the formaldehyde adsorption performance of the material 1 is lower than that of the materials 2 and 3. Stopping introducing formaldehyde after formaldehyde is adsorbed and saturated, blowing the formaldehyde by using air, and then heating the reaction tube to 100-oAnd C, collecting the tail gas by using a gas bag, analyzing the tail gas on a gas chromatograph by using a TDX-01 chromatographic column, and detecting the peak of the carbon dioxide by using a Thermal Conductivity Detector (TCD). It can thus be concluded that, at 100-oCNext, formaldehyde adsorbed by the material is converted to carbon dioxide.
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 and improvements made within the spirit and principle of the present invention are intended to be included within the scope of the present invention.
Claims (6)
1. The preparation method of the copper oxide/graphene composite material is characterized by comprising the following steps:
(1) adding 1-10 parts by weight of graphene oxide into 100-1000 parts by weight of deionized water, and performing ultrasonic dispersion to obtain a graphene oxide dispersion liquid;
(2) adding 25-125 parts by weight of copper nitrate trihydrate into 100 parts by weight of deionized water, and slowly dropwise adding concentrated ammonia water while stirring to adjust the pH value to form a stable copper ammonia solution, wherein the pH value of the copper ammonia solution is 8-9.5;
(3) adding the copper ammonia solution obtained in the step (2) into the graphene oxide dispersion liquid obtained in the step (1), stirring at room temperature for 30-60 min, and then continuously heating at 50-80 ℃ for 1-4 hours; then transferring the reactant to a high-pressure reaction kettle, and carrying out hydrothermal reduction reaction for 2-10h at the temperature of 120-;
(4) and (4) after the reaction solution in the step (3) is cooled to room temperature, removing the supernatant, washing the solid by deionized water, performing suction filtration, naturally drying at room temperature, performing freeze drying, and calcining for 1-4 hours at the calcining temperature of 250-550 ℃ under the protection of argon gas to obtain the copper oxide/graphene composite material.
2. The application of the copper oxide/graphene composite material in the aspect of absorbing formaldehyde toxic gas molecules according to claim 1 is characterized in that: the graphene oxide in the step (1) is obtained by a modified Hummers method.
3. The application of the copper oxide/graphene composite material in the aspect of absorbing formaldehyde toxic gas molecules according to claim 1 is characterized in that: the ultrasonic treatment conditions in the step (1) are as follows: the ultrasonic time is 20-60min, and the ultrasonic power is 100-150W.
4. The application of the copper oxide/graphene composite material in the aspect of absorbing formaldehyde toxic gas molecules according to claim 1 is characterized in that: the concentration of the strong ammonia water in the step (2) is 12 mol/L.
5. The application of the copper oxide/graphene composite material in the aspect of absorbing formaldehyde toxic gas molecules according to claim 1 is characterized in that: the stable cuprammonium solution in the step (2) is [ Cu (NH ]3)4(H2O)2]2+Status.
6. The application of the copper oxide/graphene composite material in the aspect of absorbing formaldehyde toxic gas molecules according to claim 1 is characterized in that: and (4) in the step (3), the high-pressure reaction kettle is a tetrafluoroethylene-lined high-pressure reaction kettle.
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| CN108187653B (en) * | 2018-01-11 | 2021-01-26 | 绍兴文理学院 | Preparation method of graphene-based photocatalytic material |
| CN108358193B (en) * | 2018-01-31 | 2019-09-27 | 黑龙江大学 | Room temperature volatilization uniform deposition prepares graphene/metal oxide-compound method |
| CN108610282A (en) * | 2018-05-03 | 2018-10-02 | 江苏医药职业学院 | A method of passing through sandmeyer reaction catalyst preparation 2,3- dichloropyridines |
| CN108940282A (en) * | 2018-08-16 | 2018-12-07 | 佛山博发智能科技有限公司 | A kind of room temperature based on Cu-series catalyst is except formaldehyde material and preparation method thereof |
| CN110813293A (en) * | 2019-10-31 | 2020-02-21 | 曲阜师范大学 | Preparation method and application of Cu NPs-rGO electrocatalyst |
| CN112473666A (en) * | 2020-11-17 | 2021-03-12 | 上海应用技术大学 | Catalyst for low-temperature catalytic oxidation of formaldehyde and preparation method and application thereof |
| CN112520780A (en) * | 2021-01-18 | 2021-03-19 | 太原理工大学 | Preparation method of folded rodlike self-assembled walnut-like copper oxide |
| CN113457619A (en) * | 2021-05-10 | 2021-10-01 | 沈阳大学 | Three-dimensional CuxO graphene and preparation method and application thereof |
| CN113731467B (en) * | 2021-09-06 | 2023-04-07 | 湘潭大学 | Nitrogen-modified graphene-loaded copper oxide composite material and preparation method and application thereof |
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