CN113044832A - Three-dimensional graphene-based hydrogel material, and preparation method and application thereof - Google Patents
Three-dimensional graphene-based hydrogel material, and preparation method and application thereof Download PDFInfo
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Abstract
The invention discloses a three-dimensional graphene-based hydrogel material, and a preparation method and application thereof, and relates to the technical field of graphene materials. The preparation method of the three-dimensional graphene-based hydrogel material comprises the following steps: graphene oxide, a reducing agent and a gas dissolving auxiliary agent are reacted in an aqueous solution system, wherein the aqueous solution system is subjected to defoaming treatment. The inventor creatively adds the gas dissolving auxiliary agent, and carries out degassing treatment on the raw materials before the reaction, thereby effectively avoiding the occurrence of holes in the graphene hydrogel, ensuring the prepared graphene-based hydrogel material to have a compact structure, avoiding the phenomenon of collapse of the internal structure, effectively improving the mechanical property of the graphene-based hydrogel, and widening the application field of the graphene-based hydrogel. The preparation method is simple in preparation process, safe, green, high in yield and easy to realize industrial application.
Description
Technical Field
The invention relates to the technical field of graphene materials, in particular to a three-dimensional graphene-based hydrogel material, and a preparation method and application thereof.
Background
The graphene is a two-dimensional carbon material with a huge specific surface area, and has excellent electrical, thermal and mechanical properties. The macroscopic three-dimensional graphene-based material is assembled by two-dimensional graphite sheets, and can be divided into the following parts according to the form difference: the graphene-based hydrogel, the graphene-based aerogel and the graphene-based xerogel are three materials.
The three-dimensional graphene-based material is a novel material in the field of graphene chemistry in recent years, and can effectively regulate and control the characteristics of graphene, such as electricity, machinery, adsorption, catalysis and the like, by controlling a graphene lamellar unit and a tissue structure. The three-dimensional graphene-based material has the characteristics of large specific surface area, high mechanical strength, excellent electronic and ionic conductivity and the like, and has great application value in various fields such as super capacitors, lithium batteries, catalysis, sensors, adsorption materials and the like.
At present, the method for preparing the macroscopic three-dimensional graphene material comprises the following steps: three main paths of chemical reduction self-assembly, hydrothermal reduction assembly and a template method. The above three methods mainly have the following problems: (1) the prepared three-dimensional graphene-based hydrogel material has bubbles and holes; (2) the reaction conditions are harsh or toxic and polluted reagents are adopted as raw materials, so that the requirements of green and environmental protection are not met.
In view of this, the invention is particularly proposed.
Disclosure of Invention
The invention aims to provide a preparation method of a three-dimensional graphene-based hydrogel material, and aims to prepare a graphene hydrogel which is free of holes inside and compact in structure.
The invention also aims to provide a three-dimensional graphene-based hydrogel material which is compact in structure, free of pores in the interior and good in mechanical property.
The third purpose of the present invention is to provide an application of the three-dimensional graphene-based hydrogel material in preparation of a three-dimensional graphene-based aerogel material and a three-dimensional graphene-based xerogel material.
The invention is realized by the following steps:
the invention provides a preparation method of a three-dimensional graphene-based hydrogel material, which comprises the following steps:
graphene oxide, a reducing agent and a gas dissolving auxiliary agent are reacted in an aqueous solution system, wherein the aqueous solution system is subjected to defoaming treatment.
The invention also provides a three-dimensional graphene-based hydrogel material prepared by the preparation method.
The invention also provides application of the three-dimensional graphene-based hydrogel material in preparation of the three-dimensional graphene-based aerogel material.
The invention also provides an application of the three-dimensional graphene-based hydrogel material in preparation of the three-dimensional graphene-based xerogel material.
The invention has the following beneficial effects: the inventor creatively adds the gas dissolving auxiliary agent, and carries out degassing treatment on the raw materials before the reaction, thereby effectively avoiding the occurrence of holes in the graphene hydrogel, ensuring the prepared graphene-based hydrogel material to have a compact structure, avoiding the phenomenon of collapse of the internal structure, effectively improving the mechanical property of the graphene-based hydrogel, and widening the application field of the graphene-based hydrogel.
Drawings
In order to more clearly illustrate the technical solutions of the embodiments of the present invention, the drawings needed to be used in the embodiments will be briefly described below, it should be understood that the following drawings only illustrate some embodiments of the present invention and therefore should not be considered as limiting the scope, and for those skilled in the art, other related drawings can be obtained according to the drawings without inventive efforts.
Fig. 1 is a cross-sectional view of the interior of the graphene hydrogel prepared in example 1;
FIG. 2 is a cross-sectional view of the interior of the graphene hydrogel prepared in example 2;
FIG. 3 is a cross-sectional view of the interior of the graphene hydrogel prepared in example 3;
FIG. 4 is a cross-sectional view of the interior of the graphene hydrogel prepared in example 4;
FIG. 5 is a cross-sectional view of the interior of the graphene hydrogel prepared in example 5;
fig. 6 is an internal cross-sectional morphology of the graphene hydrogel prepared in comparative example 1;
fig. 7 is an internal cross-sectional morphology of the graphene hydrogel prepared in comparative example 2;
fig. 8 is an internal cross-sectional morphology of the graphene hydrogel prepared in comparative example 3.
Detailed Description
In order to make the objects, technical solutions and advantages of the embodiments of the present invention clearer, the technical solutions in the embodiments of the present invention will be clearly and completely described below. The examples, in which specific conditions are not specified, were conducted under conventional conditions or conditions recommended by the manufacturer. The reagents or instruments used are not indicated by the manufacturer, and are all conventional products available commercially.
The embodiment of the invention provides a preparation method of a three-dimensional graphene-based hydrogel material, which comprises the following steps: and reacting the defoamed graphene oxide, a reducing agent and a gas dissolving auxiliary agent.
The inventor creatively dissolves the auxiliary agent in the reaction raw materials, dissolves the gas generated in the aqueous phase reaction, avoids the gas from gathering into bubbles and being retained in the gel, and is matched with the raw materials to carry out bubble removal treatment before the reaction, thereby effectively avoiding the occurrence of holes in the graphene-based hydrogel, leading the prepared graphene-based hydrogel material to have compact structure, avoiding the occurrence of the phenomenon of collapse of the internal structure, and effectively improving the mechanical property of the graphene-based hydrogel.
The method provided by the embodiment of the invention has the characteristics of uniform gel structure, large size, safety, low cost and easiness in large-scale amplification, and the raw materials are green and pollution-free, so that the method is suitable for industrial application.
The method specifically comprises the following steps:
s1 preparation of raw materials
And a graphene oxide solution, a reducing agent solution and a gas dissolving auxiliary agent solution are respectively prepared, so that the raw materials can be defoamed conveniently. In some embodiments, the graphene oxide solution, the reducing agent solution, and the gas dissolution aid solution are all aqueous solutions, with water as the single solvent to form the solutions.
The preparation process of the graphene oxide solution comprises the following steps: after mixing the graphene oxide and water, the pH value is adjusted to 8-14 to control the pH value of the reaction system, and specifically, the pH value may be 8, 9, 10, 11, 12, 13, 14, and the like.
Specifically, the alkali solution used in the process of adjusting the pH is at least one selected from potassium hydroxide, potassium carbonate, potassium bicarbonate, sodium carbonate, sodium bicarbonate and sodium hydroxide, and the pH can be adjusted by using an aqueous solution of at least one of the above raw materials.
Further, the reducing agent is at least one selected from sodium sulfite, sodium ascorbate, vitamin C and sodium citrate, and may be one or more. The gas dissolving auxiliary agent is at least one selected from ethylene carbonate, dimethyl carbonate, diethyl carbonate, sodium stearate, ethyl methyl carbonate and propylene carbonate, preferably at least one selected from dimethyl carbonate, sodium stearate and propylene carbonate, and specifically may be one or more. The selection of the reducing agent and the gas dissolving auxiliary agent is further controlled, so that the reduction assembly can be carried out at a lower temperature, and meanwhile, the gas generated in the water phase reaction is dissolved by the gas dissolving auxiliary agent, so that the gas is prevented from being converged into bubbles and retained in the gel, and the three-dimensional graphene-based hydrogel material with uniform phase is obtained.
In order to further improve the performance of the obtained three-dimensional graphene-based hydrogel material and avoid pores, the concentration and the dosage of the three raw material solutions are further optimized by the inventor. The concentration of the graphene oxide solution is 1-20mg/mL, the concentration of the reducing agent solution is 0.01-0.5g/mL, the volume fraction of the gas dissolving aid solution is 10-50%, and the mass ratio of the graphene oxide solution to the reducing agent solution to the gas dissolving aid solution is 40-60:10-30: 15-30.
Specifically, the concentration of the graphene oxide solution may be 1mg/mL, 5mg/mL, 10mg/mL, 15mg/mL, 20mg/mL, or the like, or may be any value between the two concentration values adjacent thereto. The concentration of the reducing agent solution may be 0.01g/mL, 0.1g/mL, 0.2g/mL, 0.3g/mL, 0.4g/mL, 0.5g/mL, or the like, or may be any value between the two concentration values adjacent thereto. The volume fraction of the gas dissolution aid solution may be 10%, 20%, 30%, 40%, 50%, or the like, or may be any value between the two concentration values adjacent to each other.
S2 degassing bubble
And (3) defoaming the graphene oxide solution, the reducing agent solution and the gas dissolving aid solution respectively to avoid introducing gas into the raw materials.
In other embodiments, the three solutions may be mixed and then deaerated.
Further, the operation mode of the defoaming treatment is at least one selected from vacuum pumping treatment and high-speed defoaming treatment, and the above two defoaming modes can well remove bubbles in the raw material solution.
Specifically, the treatment time of the vacuumizing treatment is 1-20 min; preferably 5-10min, and can effectively remove gas through short-time vacuum treatment, wherein the vacuum degree in the vacuum treatment process is approximately controlled to be 0-30 bar. The time for vacuumizing can be 1min, 5min, 10min, 15min, 20min and the like, and can also be any value between the adjacent time values.
Specifically, the high-speed defoaming machine is used for treating for 1-30min under the condition of rotating speed of 1000-3000 rpm; preferably 5-15 min. Under high-speed stirring, the bubbles can be effectively removed through short-time treatment. The rotating speed of the high-speed defoaming machine can be 1000rpm, 1500rpm, 2000rpm, 2500rpm, 3000rpm and the like; the treatment time can be 1min, 5min, 10min, 15min, 20min, 25min, 30min, etc.
S3, mixing reaction
Mixing the three solutions after the defoaming, reacting in a two-stage low-temperature heating treatment mode, and carrying out reduction assembly at a lower temperature.
Further, the two-stage low-temperature heating treatment comprises the steps of reacting for 1-10 hours at the temperature of 20-50 ℃ and then reacting for 1-10 hours at the temperature of 50-100 ℃. The reaction is carried out in two stages to obtain a uniform three-dimensional graphene-based hydrogel material.
Specifically, the temperature of the first stage reaction can be 20 ℃, 30 ℃, 40 ℃ and 50 ℃, and the reaction time can be 1h, 3h, 5h, 8h and 10 h; the temperature of the second stage reaction can be 50 ℃, 60 ℃, 70 ℃, 80 ℃, 90 ℃ and 100 ℃, and the reaction time can be 1h, 3h, 5h, 8h and 10 h.
In a preferred embodiment, after the graphene oxide solution, the reducing agent solution and the gas dissolution aid solution are mixed, ultrasonic treatment is performed first, and then two-stage low-temperature heating treatment is performed. The three raw materials are uniformly mixed through ultrasonic treatment, so that the uniformity of the prepared three-dimensional graphene-based hydrogel material is improved.
Specifically, the ultrasonic treatment is carried out for 1-30min under the condition that the power is 20-100 KHz. The power of ultrasonic treatment can be controlled to be 20KHz, 50KHz, 70KHz, 90KHz, 100KHz and the like, and can also be any value between the adjacent power values; the ultrasonic time can be 1min, 5min, 10min, 15min, 20min, 25min, 30min, or any value between the above adjacent time values.
The embodiment of the invention also provides a three-dimensional graphene-based hydrogel material which is prepared by the preparation method, and the hydrogel has the characteristics of smooth surface, uniform appearance, compact interior and no holes and has better mechanical property.
The embodiment of the invention also provides application of the three-dimensional graphene-based hydrogel material in preparation of a three-dimensional graphene-based aerogel material, and the three-dimensional graphene-based aerogel material with uniform pore size and no bubbles can be further obtained by taking the three-dimensional graphene-based hydrogel as a raw material and freeze-drying the three-dimensional graphene-based hydrogel material.
The embodiment of the invention also provides application of the three-dimensional graphene-based hydrogel material in preparation of the three-dimensional graphene-based xerogel material, and the three-dimensional graphene-based xerogel material with a uniform structure can be obtained by taking the three-dimensional graphene-based hydrogel as a raw material and drying and dehydrating the three-dimensional graphene-based hydrogel material by heating.
The features and properties of the present invention are described in further detail below with reference to examples.
Example 1
The embodiment provides a preparation method of a three-dimensional graphene-based hydrogel material, which comprises the following steps:
(1) dispersing 0.5g of graphene oxide into 50mL of water, and slowly adding a sodium hydroxide solution under the stirring condition to adjust the pH value to 11;
(2) dissolving 2g of vitamin C into 20mL of water to obtain a vitamin C solution;
(3) dissolving 6mL of dimethyl carbonate into 30mL of water to obtain a dimethyl carbonate solution;
(4) carrying out defoaming treatment on the alkaline graphene solution, the vitamin C solution and the dimethyl carbonate solution for 10min by using a high-speed defoaming machine, and controlling the rotating speed to be 2000 rpm;
(5) mixing an alkaline graphene solution, a vitamin C solution and a dimethyl carbonate solution according to a mass ratio of 5:2:3 under a stirring condition, carrying out ultrasonic treatment for 5min under the condition of 50KHz power, placing the mixed solution at a water bath temperature of 55 ℃ for heating for 4h, then heating the water bath kettle to 65 ℃ for 3h, and recovering the room temperature to obtain the graphene hydrogel.
Example 2
The embodiment provides a preparation method of a three-dimensional graphene-based hydrogel material, which comprises the following steps:
(1) dispersing 0.5g of graphene oxide into 50mL of water, and slowly adding a sodium hydroxide solution under the stirring condition to adjust the pH value to 11;
(2) dissolving 2g of sodium ascorbate into 20mL of water to obtain a sodium ascorbate solution;
(3) dissolving 6mL of dimethyl carbonate into 30mL of water to obtain a dimethyl carbonate solution;
(4) defoaming the alkaline graphene solution, the sodium ascorbate solution and the dimethyl carbonate solution by using a high-speed defoaming machine for 10min, and controlling the rotating speed to be 2000 rpm;
(5) mixing an alkaline graphene solution, a sodium ascorbate solution and a dimethyl carbonate solution according to a mass ratio of 5:2:3 under a stirring condition, carrying out ultrasonic treatment for 5min under a condition of 50KHz power, placing the mixed solution at a water bath temperature of 55 ℃ for heating for 4h, then heating the water bath temperature to 65 ℃ for 3h, and recovering to room temperature to obtain the graphene hydrogel.
Example 3
The embodiment provides a preparation method of a three-dimensional graphene-based hydrogel material, which comprises the following steps:
(1) dispersing 0.5g of graphene oxide into 50mL of water, and slowly adding a sodium hydroxide solution under the stirring condition to adjust the pH value to 11;
(2) dissolving 2g of sodium ascorbate into 20mL of water to obtain a sodium ascorbate solution;
(3) dissolving 6mL of propylene carbonate into 30mL of water to obtain a propylene carbonate solution;
(4) defoaming the alkaline graphene solution, the sodium ascorbate solution and the propylene carbonate solution by using a high-speed defoaming machine for 10min, and controlling the rotating speed to be 2000 rpm;
(5) mixing an alkaline graphene solution, a sodium ascorbate solution and a propylene carbonate solution according to a mass ratio of 5:2:3 under a stirring condition, carrying out ultrasonic treatment for 5min under a condition of 50KHz power, placing the mixed solution at a water bath temperature of 55 ℃ for heating for 4h, then heating the water bath to 65 ℃ for 3h, and recovering to room temperature to obtain the graphene hydrogel.
Example 4
The embodiment provides a preparation method of a three-dimensional graphene-based hydrogel material, which comprises the following steps:
(1) dispersing 0.05g of graphene oxide into 50mL of water, and slowly adding a sodium hydroxide solution under the stirring condition to adjust the pH value to 8;
(2) dissolving 0.2g of vitamin C into 20mL of water to obtain a vitamin C solution;
(3) dissolving 3mL of dimethyl carbonate into 30mL of water to obtain a dimethyl carbonate solution;
(4) defoaming the alkaline graphene solution, the vitamin C solution and the dimethyl carbonate solution for 30min by using a high-speed defoaming machine, and controlling the rotating speed to be 1000 rpm;
(5) mixing an alkaline graphene solution, a vitamin C solution and a dimethyl carbonate solution according to a mass ratio of 40:10:15 under a stirring condition, carrying out ultrasonic treatment for 30min under the condition of 20KHz power, placing the mixed solution at a water bath temperature of 20 ℃ for heating for 10h, then heating the water bath kettle to 50 ℃ for 10h, and recovering the room temperature to obtain the graphene hydrogel.
Example 5
The embodiment provides a preparation method of a three-dimensional graphene-based hydrogel material, which comprises the following steps:
(1) dispersing 1.0g of graphene oxide into 50mL of water, and slowly adding a sodium hydroxide solution under the stirring condition to adjust the pH value to 13;
(2) dissolving 10g of sodium ascorbate into 20mL of water to obtain a sodium ascorbate solution;
(3) dissolving 30mL of dimethyl carbonate into 30mL of water to obtain a dimethyl carbonate solution;
(4) defoaming the alkaline graphene solution, the sodium ascorbate solution and the dimethyl carbonate solution by using a high-speed defoaming machine for 1min, and controlling the rotating speed to be 3000 rpm;
(5) mixing an alkaline graphene solution, a sodium ascorbate solution and a dimethyl carbonate solution according to a mass ratio of 60:30:30 under a stirring condition, carrying out ultrasonic treatment for 1min under the condition of 100KHz power, placing the mixed solution at a water bath temperature of 50 ℃ for heating for 1h, then heating the water bath kettle to 90 ℃ for 1h, and recovering the room temperature to obtain the graphene hydrogel.
Comparative example 1
The comparative example provides a preparation method of a three-dimensional graphene-based hydrogel material, which comprises the following steps:
(1) dispersing 0.5g of graphene oxide into 50mL of water, and slowly adding a sodium hydroxide solution under the stirring condition to adjust the pH value to 11;
(2) dissolving 2g of sodium ascorbate into 20mL of water to obtain a sodium ascorbate solution;
(3) dissolving 6mL of propylene carbonate into 30mL of water to obtain a propylene carbonate solution;
(4) mixing an alkaline graphene solution, a sodium ascorbate solution and a propylene carbonate solution according to a mass ratio of 5:2:3 under a stirring condition, carrying out ultrasonic treatment for 5min, heating the mixed solution at a water bath temperature of 55 ℃ for 4h, heating the water bath kettle to 65 ℃ for 3h, and recovering the temperature to room temperature to obtain the graphene hydrogel.
Comparative example 2
The comparative example provides a preparation method of a three-dimensional graphene-based hydrogel material, which comprises the following steps:
(1) dispersing 0.5g of graphene oxide into 50mL of water, and slowly adding a sodium hydroxide solution under the stirring condition to adjust the pH value to 11;
(2) dissolving 2g of sodium ascorbate into 20mL of water to obtain a sodium ascorbate solution;
(3) defoaming the alkaline graphene solution and the sodium ascorbate solution by using a high-speed defoaming machine for 10min, and controlling the rotating speed to be 2000 rpm;
(4) mixing an alkaline graphene solution and a sodium ascorbate solution according to a mass ratio of 5:2 under a stirring condition, carrying out ultrasonic treatment for 5min, placing the mixed solution at a water bath temperature of 55 ℃ for heating for 4h, then heating a water bath kettle to 65 ℃ for heating for 3h, and recovering to room temperature to obtain the graphene hydrogel.
Comparative example 3
The comparative example provides a preparation method of a three-dimensional graphene-based hydrogel material, which comprises the following steps:
(1) dispersing 0.5g of graphene oxide into 50mL of water, and slowly adding a sodium hydroxide solution under the stirring condition to adjust the pH value to 11;
(2) dissolving 2g of sodium ascorbate into 20mL of water to obtain a sodium ascorbate solution;
(3) dissolving 6mL of propylene carbonate into 30mL of water to obtain a propylene carbonate solution;
(4) mixing an alkaline graphene solution, a sodium ascorbate solution and a propylene carbonate solution according to a mass ratio of 5:2:3 under a stirring condition, carrying out ultrasonic treatment for 5min, heating the mixed solution at an oil bath temperature of 80 ℃ for 4h, heating the oil bath pot to 120 ℃ for 3h, and recovering the temperature to room temperature to obtain the graphene hydrogel.
Test example 1
The topography of the three-dimensional graphene-based hydrogel materials prepared in examples 1-5 and comparative examples 1-3 was tested and the results are shown in fig. 1-8.
As can be seen from the figure, the three-dimensional graphene-based hydrogel material prepared in the embodiments 1 to 5 of the present invention has a compact structure and no internal pores. The three-dimensional graphene-based hydrogel materials prepared in comparative examples 1-3 have obvious holes, collapse and poor density.
The above is only a preferred embodiment of the present invention, and is not intended to limit the present invention, and various modifications and changes will occur to those skilled in the art. Any modification, equivalent replacement, or improvement made within the spirit and principle of the present invention should be included in the protection scope of the present invention.
Claims (10)
1. A preparation method of a three-dimensional graphene-based hydrogel material is characterized by comprising the following steps:
reacting graphene oxide, a reducing agent and a gas dissolving auxiliary agent in an aqueous solution system, wherein the aqueous solution system is subjected to defoaming treatment.
2. The preparation method according to claim 1, wherein the graphene oxide solution, the reducing agent solution and the gas dissolution aid solution are subjected to defoaming treatment respectively and then mixed for reaction;
wherein the graphene oxide solution, the reducing agent solution and the gas dissolution aid solution are all aqueous solutions.
3. The preparation method according to claim 2, wherein the preparation process of the graphene oxide solution comprises: mixing graphene oxide and water, and adjusting the pH value to 8-14;
preferably, the alkali solution used in the process of adjusting the pH is selected from at least one of potassium hydroxide, potassium carbonate, potassium bicarbonate, sodium carbonate, sodium bicarbonate and sodium hydroxide;
preferably, the reducing agent is selected from at least one of sodium sulfite, sodium ascorbate, vitamin C and sodium citrate;
preferably, the gas dissolution aid is selected from at least one of ethylene carbonate, dimethyl carbonate, diethyl carbonate, sodium stearate, ethyl methyl carbonate and propylene carbonate; more preferably, the gas dissolution aid is selected from at least one of dimethyl carbonate, sodium stearate and propylene carbonate.
4. The preparation method according to claim 3, wherein the concentration of the graphene oxide solution is 1-20mg/mL, the concentration of the reducing agent solution is 0.01-0.5g/mL, and the volume fraction of the gas dissolution aid solution is 10-50%;
preferably, the mass ratio of the graphene oxide solution to the reducing agent solution to the gas dissolution aid solution is 40-60:10-30: 15-30.
5. The production method according to claim 2, wherein the defoaming process is operated in a manner selected from at least one of an evacuation process and a high-speed defoaming machine process;
preferably, the treatment time of the vacuumizing treatment is 1-20 min; more preferably 5-10 min;
preferably, the high-speed defoaming machine is used for treating for 1-30min under the condition of rotating speed of 1000-3000 rpm; more preferably 5-15 min.
6. The method according to claim 2, wherein the reaction is carried out by means of two-stage low-temperature heat treatment;
preferably, the two-stage low-temperature heating treatment comprises the steps of reacting for 1-10h at 20-50 ℃ and then reacting for 1-10h at 50-100 ℃.
7. The preparation method according to claim 6, wherein after the graphene oxide solution, the reducing agent solution and the gas dissolution aid solution are mixed, ultrasonic treatment is performed first, and then the two-stage low-temperature heating treatment is performed;
preferably, the ultrasonic treatment is carried out for 1-30min under the condition that the power is 20-100 KHz.
8. A three-dimensional graphene-based hydrogel material prepared by the preparation method of any one of claims 1 to 7.
9. Use of the three-dimensional graphene-based hydrogel material of claim 8 in the preparation of a three-dimensional graphene-based aerogel material.
10. Use of the three-dimensional graphene-based hydrogel material of claim 8 in the preparation of a three-dimensional graphene-based xerogel material.
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106475132A (en) * | 2016-10-11 | 2017-03-08 | 中国科学院山西煤炭化学研究所 | A kind of Graphene/molecular sieve/metal-oxide composite catalyst and preparation method thereof |
| CN210845430U (en) * | 2019-10-09 | 2020-06-26 | 福建中科宏业化工科技有限公司 | A filter equipment for preparing propylene carbonate |
| CN111392715A (en) * | 2019-11-07 | 2020-07-10 | 杭州电子科技大学 | Preparation method of three-dimensional graphene material |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106475132A (en) * | 2016-10-11 | 2017-03-08 | 中国科学院山西煤炭化学研究所 | A kind of Graphene/molecular sieve/metal-oxide composite catalyst and preparation method thereof |
| CN210845430U (en) * | 2019-10-09 | 2020-06-26 | 福建中科宏业化工科技有限公司 | A filter equipment for preparing propylene carbonate |
| CN111392715A (en) * | 2019-11-07 | 2020-07-10 | 杭州电子科技大学 | Preparation method of three-dimensional graphene material |
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