CN111943199A - Method for preparing sulfur-nitrogen co-doped porous carbon material by using potassium hydroquinone sulfate as activating agent - Google Patents
Method for preparing sulfur-nitrogen co-doped porous carbon material by using potassium hydroquinone sulfate as activating agent Download PDFInfo
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- 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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Abstract
The invention provides a method for preparing a sulfur-nitrogen co-doped porous carbon material by using potassium hydroquinone sulfate as an activating agent. Grinding potassium hydroquinone sulfate and a glucosamine hydrochloride hot carbonization product or chitosan, and then carbonizing at high temperature, wherein co-doping of sulfur and nitrogen in the carbon material is realized by utilizing a sulfur element in the potassium hydroquinone sulfate and a nitrogen element in a carbon source material; meanwhile, a porous structure is formed in the carbon material through one-step high-temperature treatment by utilizing the chemical activation of potassium element in the reaction mixture. The preparation method provided by the invention avoids the use of strong corrosive activators such as potassium hydroxide and the like, and only one-step high-temperature treatment is needed to complete the activation and sulfur/nitrogen doping processes, so that the preparation method is simpler than the traditional carbonization-activation two-step preparation process; meanwhile, the prepared sulfur-nitrogen co-doped carbon material has high specific surface area and high pore volume and shows good adsorption property on carbon dioxide.
Description
Technical Field
The invention belongs to the technical field of preparation and application of porous carbon materials, and particularly relates to a method for preparing a sulfur-nitrogen co-doped porous carbon material by using hydroquinone potassium sulfate as an activating agent.
Background
Fossil energy such as coal and petroleum is a current main energy form, and a large amount of carbon dioxide is consumed and formed, resulting in a continuous increase in the concentration of carbon dioxide in the atmosphere. Although a great deal of manpower and material resources are invested at home and abroad at present to develop novel clean and environment-friendly energy, the leading position of fossil energy is still difficult to change in a short time. In this context, it is of great importance to control the continuous rise in carbon dioxide concentration using carbon capture and sequestration techniques. The absorption treatment of carbon dioxide by using an organic amine solution is the most mature carbon capture mode at present, but the regeneration process of the amine solution needs to consume a large amount of energy, and has potential safety hazards such as corrosivity and toxicity (environ, sci, technol, 47(2013) 11960-11975). The adsorption capture of Carbon dioxide by using porous Carbon material is another method with great potential, because the porous Carbon material has abundant porous structure types, good thermal stability and chemical stability, and low production cost, and is very suitable for the adsorption research of Carbon dioxide (Carbon 148(2019) 164-186).
Carbon materials can be endowed with more functionality by doping, and most of the doping elements are mainly studied to be sulfur, nitrogen, phosphorus, boron and the like (Energy environ. Sci.6(2013) 2839-2855). The carbon dioxide adsorption performance of sulfur and nitrogen doped carbon materials has also been the focus of research. The existing research results show that the doped sulfur element existing in oxidation states of thiophene and the like has stronger interaction with Carbon dioxide molecules, and can effectively improve the Carbon dioxide adsorption performance (Carbon 66(2014)320-326) of the porous Carbon material; and nitrogen doping can form basic adsorption sites in the carbon material, can selectively adsorb carbon dioxide and enhance the interaction with carbon dioxide molecules (J.Mater.chem.A. 4(2016) (17299) -17307). The sulfur/nitrogen doped porous carbon material is generally prepared by two methods: firstly, directly carrying out carbonization or activation treatment by using sulfur/nitrogen-containing organic matters as raw materials; secondly, sulfur dioxide/ammonia gas and other sulfur/nitrogen containing compounds are used to react with carbon at high temperature to complete doping. The second preparation method has better universality, but the first method has simpler requirements on preparation processes and equipment.
The most common method of forming porous structures in carbon materials is activation. In general, the raw material is carbonized and then activated with phosphoric acid, potassium hydroxide, or the like. In addition to the need for this preparation method to undergo two temperature ramp-down processes, the corrosiveness of the activator must also be addressed. The selection of proper materials as the raw materials for preparation, the simplification of the preparation process and the saving of the production cost are still the key points of the research on the preparation of the porous carbon material.
Disclosure of Invention
The invention aims to provide a method for preparing a sulfur-nitrogen co-doped porous carbon material by using hydroquinone potassium sulfate as an activating agent, which completes the doping and activating processes of sulfur and nitrogen elements to carbon by one-step high-temperature treatment. Meanwhile, the prepared carbon material has high specific surface area and shows good carbon dioxide adsorption performance.
In order to achieve the purpose, the technical scheme adopted by the invention is as follows;
a method for preparing a sulfur-nitrogen co-doped porous carbon material by using potassium hydroquinone sulfate as an activating agent comprises the following steps:
(1) dissolving glucosamine hydrochloride in 50mL of water, adding the formed solution into a 100mL hydrothermal reaction kettle, and carrying out hydrothermal carbonization treatment at 200 ℃;
(2) repeatedly washing the product obtained in the step (1) by using deionized water, and drying at 100 ℃;
(3) taking chitosan or the product dried in the step (2), grinding and mixing with hydroquinone potassium sulfate, placing the formed mixture in a tube furnace, introducing inert gas for protection, heating the tube furnace to high temperature for treatment, and naturally cooling to room temperature under the protection of inert atmosphere;
(4) and (4) adding hydrochloric acid into the product prepared in the step (3) for treatment, repeatedly washing with deionized water, and drying to obtain the sulfur-nitrogen co-doped porous carbon material.
Preferably, in the step (1), the addition amount of the glucosamine hydrochloride is 5.0g, and the hydrothermal carbonization treatment time is 6 hours;
preferably, in the step (3), the mass ratio of the potassium hydroquinone sulfate to the thermal carbonization product of the chitosan or the glucosamine hydrochloride is 2-4:1, the nitrogen flow is 60mL/min, the high-temperature treatment temperature is 700-
Preferably, in the step (4), the hydrochloric acid is used at a concentration of 10% by mass, the drying temperature is 100 ℃, and the drying time is 4 hours.
Compared with the prior art, the invention grinds the potassium hydroquinone sulfate and the glucosamine hydrochloride hot carbonization product or chitosan and then carries out carbonization treatment at high temperature, and realizes the co-doping of sulfur and nitrogen to the carbon material by utilizing the sulfur element in the potassium hydroquinone sulfate and the nitrogen element in the carbon source material; meanwhile, a porous structure is formed in the carbon material through one-step high-temperature treatment by utilizing the chemical activation of potassium element in the reaction mixture. The preparation method provided by the invention avoids the use of strong corrosive activators such as potassium hydroxide and the like, and only one-step high-temperature treatment is needed to complete the activation and sulfur/nitrogen doping processes, so that the preparation method is simpler than the traditional carbonization-activation two-step preparation process; meanwhile, the prepared sulfur-nitrogen co-doped carbon material has high specific surface area and high pore volume and shows good adsorption property on carbon dioxide. The invention has the advantages that:
(1) the potassium hydroquinone sulfate is used as a sulfur source and an activating agent, and the doping and activating processes are simultaneously completed at high temperature;
(2) nitrogen doping of the carbon material is realized by using nitrogen elements contained in chitosan and glucosamine hydrochloride, and a sulfur-nitrogen co-doped carbon material is prepared;
(3) the doping, carbonizing and activating processes are completed in one step, and the traditional carbonization-reactivation two-step preparation process is simplified.
Drawings
Fig. 1 is a scanning electron micrograph of a sulfur-nitrogen co-doped porous carbon material according to embodiment 1 of the present invention;
FIG. 2 shows N of the sulfur-nitrogen co-doped porous carbon material at 77K in embodiment 1 of the present invention2Adsorption and desorption isotherms;
fig. 3 is an X-ray photoelectron spectrum N1s of the sulfur-nitrogen co-doped porous carbon material according to embodiment 2 of the present invention;
FIG. 4 is a S2p spectrum of an X-ray photoelectron spectrum of the sulfur-nitrogen co-doped porous carbon material in the embodiment 2 of the present invention;
FIG. 5 shows N of the sulfur-nitrogen co-doped porous carbon material at 77K in embodiment 2 of the present invention2Adsorption and desorption isotherms;
FIG. 6 shows CO of the S-N CO-doped porous carbon material at 298K according to embodiment 3 of the present invention2Adsorption isotherms;
FIG. 7 shows N of the S-N co-doped porous carbon material at 298K according to embodiment 3 of the present invention2Adsorption isotherms;
FIG. 8 shows CO of the S-N CO-doped porous carbon material in embodiment 3 of the present invention2/N2A schematic diagram of adsorption selectivity results;
FIG. 9 is a schematic view of a preparation process of the sulfur-nitrogen co-doped porous carbon material of the present invention.
Detailed Description
The method for preparing the sulfur-nitrogen co-doped porous carbon material by using potassium hydroquinone sulfate as an activator according to the present invention will be described in more detail with reference to the preparation flow diagram, wherein preferred embodiments of the present invention are shown, but not limited thereto.
A method for preparing a sulfur-nitrogen co-doped porous carbon material by using potassium hydroquinone sulfate as an activating agent, as shown in fig. 9, comprises the following steps:
(1) dissolving 5.0g of glucosamine hydrochloride into 50mL of water, adding the formed solution into a 100mL hydrothermal reaction kettle, and carrying out hydrothermal carbonization reaction for 6h at 200 ℃;
(2) repeatedly washing the product obtained in the step (1) by using deionized water, and drying at 100 ℃;
(3) taking chitosan or the product dried in the step (2), grinding and mixing with hydroquinone potassium sulfate, placing the formed mixture in a tube furnace, introducing nitrogen for protection (60mL/min), heating the tube furnace to 700-900 ℃, keeping the temperature for 1-2 hours, and naturally cooling to room temperature under the protection of inert atmosphere;
(4) and (4) adding 10% hydrochloric acid into the product prepared in the step (3) for treatment, repeatedly washing with deionized water, and drying at 100 ℃ for 4 hours to obtain the sulfur-nitrogen co-doped porous carbon material.
The carbon dioxide adsorption characteristic test of the obtained sulfur-nitrogen co-doped porous carbon material is carried out according to the following steps:
(1) adding about 100mg of carbon material into a test sample chamber, heating to 250 ℃, and carrying out vacuum degassing treatment for 3 hours;
(2) setting the environment temperature of the test sample chamber, gradually increasing the pressure of carbon dioxide, and testing a complete carbon dioxide adsorption isotherm;
(3) after the carbon dioxide adsorption test is finished, heating the sample chamber to 100 ℃ and carrying out vacuum treatment for 1h to finish carbon dioxide desorption;
(4) a similar method was used to test the nitrogen adsorption isotherm of the carbon material and calculate the adsorption selectivity.
Example 1
The preparation steps of the sulfur-nitrogen co-doped porous carbon material of the embodiment are as follows: 5.0g of glucosamine hydrochloride was dissolved in 50mL of water, and the resulting clear solution was put into a 100mL stainless steel hydrothermal reaction vessel and subjected to hydrothermal carbonization at 200 ℃ for 6 hours. The resulting product was filtered and washed repeatedly with deionized water and finally dried at 100 ℃ for 4 h. 1.0g of the dried hydrothermal carbonized product is uniformly ground with 3.0g of potassium hydroquinone sulfate, and the formed mixture is placed in a tube furnace and is protected by nitrogen (60 mL/min). The temperature of the tube furnace is raised from room temperature to 900 ℃ at the speed of 5 ℃/min and is kept constant for 2 hours. And after natural cooling, treating the product by using 10% hydrochloric acid, repeatedly washing the product by using deionized water, and drying the product for 4 hours at 100 ℃ to obtain the final product.
As shown in FIG. 1, a scanning electron micrograph of the sulfur-nitrogen co-doped porous carbon material prepared from glucosamine hydrochloride and potassium hydroquinone sulfate according to this example shows that the carbon material has irregular shape and size, and forms particles with different sizes on the surfaceAnd (4) large pores. The nitrogen adsorption-desorption isotherm of the carbon material at 77K is shown in FIG. 2, and the specific surface area is 1303m2The use of potassium hydroquinone sulphate demonstrated that a rich porous structure could be formed in the carbon material, i.e. could act as an activator.
Example 2
The preparation steps of the sulfur-nitrogen co-doped porous carbon material of the embodiment are as follows: 1.0g of chitosan and 4.0g of potassium hydroquinone sulfate are ground, the ground mixture is placed in a tube furnace, the furnace temperature is increased from room temperature to 800 ℃ at the speed of 5 ℃/min under the protection of nitrogen (60mL/min), and the mixture is heated at the constant temperature of 800 ℃ for 2 hours. And after natural cooling, treating the product by using 10% hydrochloric acid, repeatedly washing by using deionized water, and drying for 4 hours at 100 ℃ to obtain the final product.
The spectrogram of an X-ray photoelectron spectrum N1s of the sulfur-nitrogen co-doped porous carbon material prepared from chitosan and potassium hydroquinone sulfate according to the embodiment is shown in FIG. 3, wherein the nitrogen content is 4.49 wt%, which proves that nitrogen doping can be carried out by using nitrogen elements contained in the raw materials; the spectrogram of the carbon material X-ray photoelectron spectrum S2p is shown in FIG. 4, the sulfur content of the carbon material is 6.70 wt%, and the sulfur doping of the carbon material by using the sulfur element contained in the potassium hydroquinone sulfate is proved. The nitrogen adsorption/desorption isotherm of this carbon material 77K is shown in FIG. 5, and its specific surface area is 1186m2Per g, pore volume of 0.889cm3And/g shows that the sulfur-nitrogen co-doped porous carbon material with high specific surface area can be prepared by using potassium hydroquinone sulfate as an activating agent.
Example 3
The preparation steps of the sulfur-nitrogen co-doped porous carbon material of the embodiment are as follows: 1.0g of chitosan and 3.0g of potassium hydroquinone sulfate are ground, the ground mixture is placed in a tube furnace, the furnace temperature is increased from room temperature to 900 ℃ at the speed of 5 ℃/min under the protection of nitrogen (60mL/min), and the mixture is heated at the constant temperature of 900 ℃ for 2 hours. And after natural cooling, treating the product by using 10% hydrochloric acid, repeatedly washing by using deionized water, and drying for 4 hours at 100 ℃ to obtain the final product.
The steps for testing the carbon dioxide adsorption performance of the sulfur-nitrogen co-doped porous carbon material prepared in the embodiment are as follows: 100mg of carbon material was added to a test sample chamber and subjected to vacuum heating at 250 ℃ for 3 hours to remove impurities such as water adsorbed on the surface. And (3) placing the test sample chamber in a constant-temperature water bath at 25 ℃, gradually increasing the equilibrium adsorption pressure of the carbon dioxide to obtain a complete adsorption isotherm, and calculating the equilibrium adsorption quantity of the carbon dioxide. And changing the used test gas into nitrogen, testing the nitrogen adsorption isotherm of the prepared nitrogen-doped porous carbon material, and calculating the nitrogen adsorption capacity and the adsorption selectivity.
The carbon dioxide adsorption isotherm of the sulfur-nitrogen co-doped porous carbon material prepared from chitosan and potassium hydroquinone sulfate at 298K according to the present example is shown in FIG. 6, where the carbon dioxide adsorption amount is 1.3mmol/g under one atmosphere and 11.5mmol/g under 20bar pressure. FIG. 7 shows the nitrogen adsorption isotherm at 298K of this carbon material, and the nitrogen adsorption amount at one atmosphere was 0.2 mmol/g. Fig. 8 is a graph showing adsorption selectivity values calculated from the results of carbon dioxide and nitrogen adsorption tests, and the adsorption selectivity at 1 atmosphere was 9.1.
Claims (5)
1. The method for preparing the sulfur-nitrogen co-doped porous carbon material by using potassium hydroquinone sulfate as an activating agent is characterized by comprising the following preparation steps of:
(1) dissolving glucosamine hydrochloride in water, adding the formed solution into a hydrothermal reaction kettle, and carrying out hydrothermal carbonization treatment;
(2) repeatedly washing the product obtained in the step (1) by using deionized water, and drying;
(3) grinding and mixing chitosan or the product dried in the step (2) with hydroquinone potassium sulfate, placing the formed mixture in a tube furnace, introducing inert gas for protection, heating the tube furnace to a high temperature for treatment, and naturally cooling to room temperature;
(4) and (4) adding hydrochloric acid into the product obtained in the step (3) for treatment, repeatedly washing with deionized water, and drying to obtain the sulfur-nitrogen co-doped porous carbon material.
2. The method for preparing the sulfur-nitrogen co-doped porous carbon material by using potassium hydroquinone sulfate as an activating agent according to claim 1, wherein in the step (3), the mass ratio of the potassium hydroquinone sulfate to the glucosamine hydrochloride hot carbonization product or chitosan is 2-4: 1.
3. The method for preparing the S-N co-doped porous carbon material by using potassium hydroquinone sulfate as the activator in claim 1, wherein the temperature of the high-temperature treatment in the step (3) is 700-900 ℃, and the treatment time is 1-2 h.
4. The method for preparing the sulfur-nitrogen co-doped porous carbon material by using potassium hydroquinone sulfate as an activating agent according to claim 1, wherein in the step (1), the hydrothermal carbonization treatment is performed at 200 ℃.
5. The method for preparing the sulfur-nitrogen co-doped porous carbon material by using potassium hydroquinone sulfate as an activator according to claim 1, wherein the drying temperature in the step (2) is 100 ℃.
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| CN113060720A (en) * | 2021-04-07 | 2021-07-02 | 福州大学 | Preparation method and application of ZiF-8 derived P and N co-doped 3D porous carbon adsorbent |
| CN113893821A (en) * | 2021-10-14 | 2022-01-07 | 安徽元琛环保科技股份有限公司 | Nitrogen-sulfur-doping-based porous carbon material noble metal adsorbent and preparation method thereof |
| CN113912057A (en) * | 2021-12-02 | 2022-01-11 | 山东建筑大学 | Preparation method of super-capacitor activated carbon |
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| CN115304061A (en) * | 2022-09-01 | 2022-11-08 | 江西省科学院应用化学研究所 | Sulfur-nitrogen co-doped carbon material and preparation method and application thereof |
| CN115490232A (en) * | 2022-11-02 | 2022-12-20 | 江西省科学院应用化学研究所 | Nitrogen-sulfur co-doped or sulfur-doped porous carbon material and preparation method and application thereof |
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