CN114307960A - Preparation method and application of cation pi-effect synergistic mesoporous carbon material - Google Patents
Preparation method and application of cation pi-effect synergistic mesoporous carbon material Download PDFInfo
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Abstract
The invention belongs to the technical field of mesoporous carbon materials, and particularly relates to a preparation method and application of a cation pi-effect synergistic mesoporous carbon material. The preparation method of the cation pi-effect synergistic mesoporous carbon material comprises the following steps of S1: respectively weighing Pluronic F127 and potassium chloride with certain mass, dissolving in hydrochloric acid solution, adding 1,3, 5-trimethylbenzene and ethanol after complete dissolution, stirring uniformly, adding formaldehyde solution and 3-aminophenol, and reacting at a certain temperature; s2: and after the reaction in the step S1 is completed, transferring the solution obtained by the reaction into a high-pressure reaction kettle, carrying out hydrothermal treatment, cooling to room temperature, and carrying out centrifugal drying on the solution to obtain the aminophenol formaldehyde resin (APF) polymer. S3: and drying the APF obtained in the step S2, grinding the dried APF, then placing the APF in a tubular furnace, and annealing under the protection of nitrogen to obtain the mesoporous carbon material with developed pores.
Description
Technical Field
The invention belongs to the technical field of mesoporous carbon materials, and particularly relates to a preparation method and application of a cation pi-effect synergistic mesoporous carbon material.
Background
With the development of modern science and technology and industry, industries with high precision requirements such as semiconductors, nano materials, fine ceramics, electronic industry, pharmacy and the like are more and more, the industries have higher requirements on the quality of water for cleaning, manufacturing, medicine dilution and the like in the working procedures, and the high-purity water plays a key role in the manufacturing of materials and devices due to the good quality of the high-purity water, and becomes one of essential basic materials in the modern science and technology development and industrial production. The preparation process of the high-purity water mainly comprises pretreatment, desalination and post-treatment. Wherein, the desalting comprises pre-desalting and deep desalting, and the pre-desalting can remove most ions which are easy to remove in water, thereby reducing the treatment load of subsequent deep desalting; deep desalination needs to remove all impurity ions remained in water, so that the effluent water meets the water quality requirement of high-purity water.
The carbon nano tube has the ultra-fast water permeability confirmed by experiments and the extremely high desalting capability predicted by theory, so the carbon nano tube is considered to be a desalting material with excellent performance for a long time. The carbon nanotube is a hollow tubular structure formed by curling graphite sheets, the diameter of the carbon nanotube is several nanometers, and the longest length of the carbon nanotube can reach several micrometers. In recent years, a plurality of theories and experiments show that the carbon nano tube has good permeability to pure water, and the efficiency of the carbon nano tube far exceeds that of a commercial reverse osmosis desalination membrane. Meanwhile, several developments of Science and Nature have envisioned that the filter membrane made of the carbon nanotubes can be applied to seawater desalination, and the required energy consumption can be greatly reduced. However, the experimental development of the carbon nanotube with a salt removal rate sufficient as a salt removal material is not ideal, and experimental studies have shown that the six-membered cyclic structure composed of carbon atoms on the carbon nanotube is an aromatic ring structure, which is rich in delocalized pi electrons. In the process of seawater desalination, strong interaction exists between cations such as sodium ions and potassium ions and aromatic rings rich in pi electrons on a carbon-based material, namely cation-pi action, so that a large amount of ions can be rapidly adsorbed at the pipe orifice of the carbon nano tube to block the carbon nano tube. The water flow in the carbon nano tube is blocked, thereby greatly reducing the application value of the carbon nano tube as a high-efficiency seawater filtering material. However, the deep desalination treatment in the high-purity water preparation technology is different from the seawater desalination, and the low concentration of salt ions causes low adsorption power of the adsorption material, thereby limiting the application of the adsorption material in the high-purity water technology. Although the cation pi action between the carbon nanotube and the cation can cause the carbon nanotube to lose the application value in the seawater desalination process, in the deep desalination treatment process, the action can enhance the adsorption power of the carbon nanotube to salt, so that the enrichment of the salt of the carbon nanotube in a low-salt environment is realized, and the purposes of efficiently desalting and improving the water quality are achieved.
Disclosure of Invention
In view of the problems raised by the above background art, the present invention is directed to: is intended to provide.
In order to achieve the technical purpose, the technical scheme adopted by the invention is as follows:
a method for preparing a cation pi-effect synergistic mesoporous carbon material comprises the following steps,
s1: respectively weighing Pluronic F127 and potassium chloride with certain mass, dissolving in hydrochloric acid solution, adding 1,3, 5-trimethylbenzene and ethanol after complete dissolution, stirring uniformly, adding formaldehyde solution and 3-aminophenol, and reacting at a certain temperature;
s2: and after the reaction in the step S1 is completed, transferring the solution obtained by the reaction into a high-pressure reaction kettle, carrying out hydrothermal treatment, cooling to room temperature, and carrying out centrifugal drying on the solution to obtain the aminophenol formaldehyde resin (APF) polymer.
S3: and drying the APF obtained in the step S2, grinding the dried APF, then placing the APF in a tubular furnace, and annealing under the protection of nitrogen to obtain the mesoporous carbon material with developed pores.
In a preferable embodiment of the invention, the weight of Pluronic F127, potassium chloride, 1,3, 5-trimethylbenzene and 3-aminophenol is as follows;
Pluronic F127 4～6g；
4-6 g of potassium chloride;
4-6 g of 1,3, 5-trimethylbenzene;
2-4 g of 3-aminophenol.
In a preferable scheme of the invention, the concentration of the hydrochloric acid solution is 2Mmol/L, and the formaldehyde solution contains 5-15% by mass of methanol and 37% by mass of formaldehyde;
the volumes of the hydrochloric acid solution, the formaldehyde solution and the ethanol are as follows:
300ml of hydrochloric acid solution;
2-4 ml of formaldehyde solution;
100-300 ml of ethanol.
In a preferable embodiment of the invention, the weight of Pluronic F127, potassium chloride, 1,3, 5-trimethylbenzene and 3-aminophenol is as follows;
pluronic F1275 g; 5g of potassium chloride; 5g of 1,3, 5-trimethylbenzene; 3g of 3-aminophenol;
the volumes of the hydrochloric acid solution, the formaldehyde solution and the ethanol are as follows: 300ml of hydrochloric acid solution; 3ml of formaldehyde solution; 200ml of ethanol.
In a preferred embodiment of the present invention, the reaction temperature in S1 is 20 to 40 ℃, and the reaction time is 40 to 60 min.
As a preferable scheme of the invention, the hydrothermal temperature in S2 is 80-120 ℃, and the hydrothermal time is 12-36 h.
In a preferable embodiment of the present invention, the nitrogen flow rate is 100 to 300ml/min, and the annealing temperature is 400 to 500 ℃.
An application of a mesoporous carbon material, wherein the mesoporous carbon material is applied to deep desalination water quality treatment.
The invention has the beneficial effects that:
the invention controls the growth of the material by regulating the molecular polymerization process so as to achieve the aim of regulating mesoporous carbon materials with different pore canal diameters and lengths; the mesoporous carbon material capable of enhancing the ion-pi effect of the carbon-based functional material is screened, the adsorption kinetics of the mesoporous carbon material for removing trace salt is improved, and the bottleneck problems of low reaction kinetics of an adsorbent and poor desalting efficiency in the deep desalting process are solved. The invention provides a method for regulating a mesoporous carbon pore structure to enhance the cation-pi action of a carbon-based material, and the cation-pi action used by the method obviously improves the adsorption kinetics for removing trace salt. The technology does not need to add chemical reagents, and has the advantages of small occupied area, low operating cost, easy maintenance, high efficiency, safety and stability. In the field of electronic-grade and nuclear-grade ultrapure water, the bottom layer key technology of the top adsorption separation material is broken through by independent intellectual property rights, the long-term monopolized industrial pattern of foreign products is broken through, import substitution is realized, the industrial technical safety of China is guaranteed, and the method has military significance, industrial significance and scientific significance.
Drawings
The invention is further illustrated by the non-limiting examples given in the accompanying drawings;
FIG. 1 is a schematic view of a mesoporous carbon material obtained in example 1 of the present invention at 100 nm;
FIG. 2 is a schematic view of a mesoporous carbon material obtained in example 1 of the present invention at 100 nm;
FIG. 3 is a schematic view of a mesoporous carbon material obtained in example 1 of the present invention at 100 nm;
Detailed Description
In order that those skilled in the art can better understand the present invention, the following technical solutions are further described with reference to the accompanying drawings and examples.
Example 1
A method for preparing a cation pi-effect synergistic mesoporous carbon material comprises the following steps,
s1: respectively weighing 4g of Pluronic F127 and 6g of potassium chloride, dissolving the Pluronic F127 and the potassium chloride in 300ml of hydrochloric acid solution with the concentration of 2Mmol/L, adding 5g of 1,3, 5-trimethylbenzene and 100ml of ethanol after the Pluronic F127 and the potassium chloride are completely dissolved, uniformly stirring, adding 2ml of formaldehyde solution containing 5-15% of mass fraction and 37% of mass fraction and 0.2g of 3-aminophenol, and reacting for 40min at the temperature of 20-25 ℃;
s2: and after the reaction in the step S1 is completed, transferring the solution obtained by the reaction into a high-pressure reaction kettle, carrying out hydrothermal treatment for 12 hours at the hydrothermal temperature of 80-90 ℃, cooling to room temperature, and carrying out centrifugal drying on the solution to obtain the aminophenol formaldehyde resin (APF) polymer.
S3: and drying the APF obtained in the step S2, grinding the dried APF, then placing the APF in a tubular furnace, and annealing under the protection of nitrogen, with the nitrogen flow of 100-150 ml/min and the annealing temperature of 400-450 ℃ to obtain the mesoporous carbon material with developed pores.
Example 2
A method for preparing a cation pi-effect synergistic mesoporous carbon material comprises the following steps,
s1: respectively weighing 6g of Pluronic F127 and 4g of potassium chloride, dissolving the Pluronic F127 and the potassium chloride in 300ml of hydrochloric acid solution with the concentration of 2Mmol/L, adding 6g of 1,3, 5-trimethylbenzene and 300ml of ethanol after the Pluronic F127 and the potassium chloride are completely dissolved, uniformly stirring, adding 2ml of formaldehyde solution containing 5-15% of methanol and 37% of ethanol and 0.4g of 3-aminophenol, and reacting for 6min at the temperature of 35-40 ℃;
s2: and after the reaction in the step S1 is completed, transferring the solution obtained by the reaction into a high-pressure reaction kettle, performing hydrothermal treatment for 36 hours at the hydrothermal temperature of 110-120 ℃, cooling to room temperature, and performing centrifugal drying on the solution to obtain the aminophenol formaldehyde resin (APF) polymer.
S3: and drying the APF obtained in the step S2, grinding the dried APF, then placing the APF in a tubular furnace, and annealing under the protection of nitrogen, with the nitrogen flow of 100-150 ml/min and the annealing temperature of 400-450 ℃ to obtain the mesoporous carbon material with developed pores.
Example 3
A method for preparing a cation pi-effect synergistic mesoporous carbon material comprises the following steps,
s1: respectively weighing 5g of Pluronic F127 and 5g of potassium chloride, dissolving the Pluronic F127 and the potassium chloride in 300ml of hydrochloric acid solution with the concentration of 2Mmol/L, adding 5g of 1,3, 5-trimethylbenzene and 200ml of ethanol after the Pluronic F127 and the potassium chloride are completely dissolved, uniformly stirring, adding 3ml of formaldehyde solution containing 5-15% of mass fraction and 37% of mass fraction and 0.3g of 3-aminophenol, and reacting for 50min at the temperature of 30-35 ℃;
s2: and after the reaction in the step S1 is completed, transferring the solution obtained by the reaction into a high-pressure reaction kettle, performing hydrothermal treatment for 30 hours at the hydrothermal temperature of 100-110 ℃, cooling to room temperature, and performing centrifugal drying on the solution to obtain the aminophenol formaldehyde resin (APF) polymer.
S3: and drying the APF obtained in the step S2, grinding the dried APF, then placing the APF in a tube furnace, and annealing under the protection of nitrogen, with the nitrogen flow of 200-250 ml/min and the annealing temperature of 450-480 ℃ to obtain the mesoporous carbon material with developed pores.
The mesoporous carbon materials obtained in examples 1 to 3 were applied to deep desalination water quality treatment.
As shown in fig. 1 to 3, the mesoporous carbon materials obtained in examples 1 to 3 have developed pores, and thus have excellent effects in deep desalination water treatment applications.
The foregoing embodiments are merely illustrative of the principles of the present invention and its efficacy, and are not to be construed as limiting the invention. Any person skilled in the art can modify or change the above-mentioned embodiments without departing from the spirit and scope of the present invention. Accordingly, it is intended that all equivalent modifications or changes which can be made by those skilled in the art without departing from the spirit and technical spirit of the present invention be covered by the claims of the present invention.
Claims (8)
1. A preparation method of a cation pi-effect synergistic mesoporous carbon material is characterized by comprising the following steps: comprises the following steps of (a) carrying out,
s1: respectively weighing Pluronic F127 and potassium chloride with certain mass, dissolving in hydrochloric acid solution, adding 1,3, 5-trimethylbenzene and ethanol after complete dissolution, stirring uniformly, adding formaldehyde solution and 3-aminophenol, and reacting at a certain temperature;
s2: and after the reaction in the step S1 is completed, transferring the solution obtained by the reaction into a high-pressure reaction kettle, carrying out hydrothermal treatment, cooling to room temperature, and carrying out centrifugal drying on the solution to obtain the aminophenol formaldehyde resin (APF) polymer.
S3: and drying the APF obtained in the step S2, grinding the dried APF, then placing the APF in a tubular furnace, and annealing under the protection of nitrogen to obtain the mesoporous carbon material with developed pores.
2. The method for preparing the cationic pi-acting synergistic mesoporous carbon material according to claim 1, wherein the method comprises the following steps: the weight of the Pluronic F127, the potassium chloride, the 1,3, 5-trimethylbenzene and the 3-aminophenol is as follows;
Pluronic F127 4～6g；
4-6 g of potassium chloride;
4-6 g of 1,3, 5-trimethylbenzene;
2-4 g of 3-aminophenol.
3. The method for preparing the cationic pi-effect synergistic mesoporous carbon material according to claim 2, wherein the method comprises the following steps:
the concentration of the hydrochloric acid solution is 2Mmol/L, and the formaldehyde solution contains 5-15% by mass of methanol and 37% by mass of formaldehyde;
the volumes of the hydrochloric acid solution, the formaldehyde solution and the ethanol are as follows:
300ml of hydrochloric acid solution;
2-4 ml of formaldehyde solution;
100-300 ml of ethanol.
4. The method for preparing the cationic pi-acting synergistic mesoporous carbon material according to claim 3, wherein the method comprises the following steps: the weight of the Pluronic F127, the potassium chloride, the 1,3, 5-trimethylbenzene and the 3-aminophenol is as follows;
pluronic F1275 g; 5g of potassium chloride; 5g of 1,3, 5-trimethylbenzene; 3g of 3-aminophenol;
the volumes of the hydrochloric acid solution, the formaldehyde solution and the ethanol are as follows: 300ml of hydrochloric acid solution; 3ml of formaldehyde solution; 200ml of ethanol.
5. The method for preparing the cationic pi-acting synergistic mesoporous carbon material according to claim 1, wherein the method comprises the following steps: the reaction temperature in the S1 is 20-40 ℃, and the reaction time is 40-60 min.
6. The method for preparing the cationic pi-acting synergistic mesoporous carbon material according to claim 1, wherein the method comprises the following steps: and the hydrothermal temperature in the S2 is 80-120 ℃, and the hydrothermal time is 12-36 h.
7. The method for preparing the cationic pi-acting synergistic mesoporous carbon material according to claim 1, wherein the method comprises the following steps: the nitrogen flow is 100-300 ml/min, and the annealing temperature is 400-500 ℃.
8. The application of the mesoporous carbon material prepared by the preparation method according to any one of claims 1 to 7 is characterized in that: the mesoporous carbon material is applied to deep desalination water quality treatment.
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| US20110134585A1 (en) * | 2009-12-07 | 2011-06-09 | Shen Bo-Jiun | Mesoporous carbon material, fabrication method thereof and supercapacitor |
| CN102634054A (en) * | 2012-04-12 | 2012-08-15 | 沁园集团股份有限公司 | Preparation method of modified polymer film material for effectively removing trace heavy metal ions in water body |
| CN102976305A (en) * | 2012-12-03 | 2013-03-20 | 张鸿涛 | Preparation method of mesoporous carbon material with aperture regulated by using template method |
| CN110950317A (en) * | 2019-12-15 | 2020-04-03 | 复旦大学 | Ordered mesoporous carbon and hydrothermal preparation method thereof |
Non-Patent Citations (5)
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