CN112897505B - A kind of preparation method of mesoporous carbon material - Google Patents

A kind of preparation method of mesoporous carbon material Download PDF

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CN112897505B
CN112897505B CN202110317875.4A CN202110317875A CN112897505B CN 112897505 B CN112897505 B CN 112897505B CN 202110317875 A CN202110317875 A CN 202110317875A CN 112897505 B CN112897505 B CN 112897505B
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phenolic resin
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曹学飞
王鹏飞
孙少超
孙少妮
袁同琦
孙润仓
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Beijing Forestry University
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Abstract

本发明涉及一种介孔炭材料的制备方法。包括以下步骤:(1)酚醛树脂前驱体溶液的制备;(2)前驱体与模板剂共混;(3)固化;(4)炭化;(5)后处理。将酚醛树脂前驱体与模板剂按照一定比例混合并固化后,将其置于惰性气体氛围下程序升温,除去模板剂并使酚醛树脂炭化,炭化产物经粉碎,清洗、除杂、过滤、烘干,得介孔炭材料。本发明所用模板剂来源广泛且廉价易得,制备方法简单,制备的介孔炭具有孔径尺寸可控、孔道均匀、结构稳定等优点,可广泛应用于储能、催化、吸附等领域。The present invention relates to a preparation method of mesoporous carbon material. It includes the following steps: (1) preparation of a phenolic resin precursor solution; (2) blending of the precursor and a template agent; (3) curing; (4) carbonization; (5) post-treatment. After mixing and curing the phenolic resin precursor and the template agent in a certain proportion, it is placed in an inert gas atmosphere to program the temperature to remove the template agent and carbonize the phenolic resin. The carbonized product is pulverized, washed, removed, filtered and dried. , to obtain mesoporous carbon materials. The template agent used in the invention has wide sources, is cheap and easy to obtain, the preparation method is simple, and the prepared mesoporous carbon has the advantages of controllable pore size, uniform pore channel, stable structure, etc.

Description

一种介孔炭材料的制备方法A kind of preparation method of mesoporous carbon material

技术领域technical field

本发明属于炭材料领域,涉及一种介孔炭材料的制备方法。The invention belongs to the field of carbon materials, and relates to a preparation method of a mesoporous carbon material.

背景技术Background technique

近年来,人们对炭纳米材料的研究及其在工业中的应用产生了很大的兴趣。炭纳米材料在光学特性、硬度、耐腐蚀性、耐热性、耐化学药品特性、耐辐射特性、电绝缘特性、导电性、表面与界面特性等方面性能优异,因此炭纳米材料在储氢、二次电池、超级电容器、传感器、催化剂载体等领域都有广泛的应用。In recent years, there has been a great deal of interest in the study of carbon nanomaterials and their application in industry. Carbon nanomaterials have excellent performance in optical properties, hardness, corrosion resistance, heat resistance, chemical resistance properties, radiation resistance properties, electrical insulation properties, electrical conductivity, surface and interface properties, etc. Secondary batteries, supercapacitors, sensors, catalyst carriers and other fields have a wide range of applications.

多孔炭材料是一种具有多种孔道结构的炭材料。由国际纯粹应用化学联合会的规定:直径在0.8nm以下的孔为亚微孔,介于0.8-2nm间的称为微孔,介于2-50nm间的称为介孔,大于50nm的称为大孔。所以,根据孔径的大小可以将多孔材料分为微孔材料、介孔材料、大孔材料。制备介孔炭材料的方法包括有机凝胶炭化法、催化气化法和模板法。但是,有机凝胶炭化法和催化气化法由于无法精确的控制孔道结构、尺寸和孔径的分布,因此在合成介孔炭材料的方法中使用较少。而模板法由于能够精确控制孔径尺寸及其分布,并且能够合成具有规整孔道结构的介孔炭材料,所以近年来被广泛应用于介孔炭材料的制备。Porous carbon material is a carbon material with various pore structures. According to the regulations of the International Federation of Pure Applied Chemistry: pores with a diameter below 0.8nm are called submicropores, those between 0.8-2nm are called micropores, those between 2-50nm are called mesopores, and those greater than 50nm are called mesopores. for large holes. Therefore, according to the size of the pore size, porous materials can be divided into microporous materials, mesoporous materials, and macroporous materials. Methods for preparing mesoporous carbon materials include organogel carbonization, catalytic gasification and template methods. However, organogel carbonization and catalytic gasification are rarely used in the synthesis of mesoporous carbon materials because they cannot precisely control the pore structure, size, and pore size distribution. The template method has been widely used in the preparation of mesoporous carbon materials in recent years because it can precisely control the pore size and distribution, and can synthesize mesoporous carbon materials with regular pore structure.

模板法又分为硬模板法和软模板法。硬模板法是指使用预先制备的具有某种特定孔道结构的介孔硅分子筛为模板,先将炭前驱体填充到分子筛的孔道中去,然后用氢氧化钠或者氢氟酸除去硅模板,得到介孔炭材料;软模板法是指直接使用表面活性剂作为结构导向剂,通过氢键的作用与炭前驱体结合,经过交联和炭化过程,使得原来表面活性剂占有的位置变为介孔,炭前驱体经过炭化后成为孔的骨架。虽然模板法具有精准控制孔径尺寸和孔分布的优点,但同时也存在一定的缺点。硬模板法在制备介孔炭材料时往往需要先合成出硬模板,最后通过腐蚀出去模板,该法对硬模板的消耗十分严重,成本极高。此外硬模板法对炭材料的要求往往较高,例如前驱体和硬模板之间相溶性要好,孔道间要有相互支撑的结构,避免经过洗除模板后造成炭材料结构发生错位。软模板法相对于硬模板法来说,不需要硅源的参与和硅模板的脱除,避免了步骤的繁琐和资源的浪费,但软模板法一般需要以价格昂贵的嵌段共聚物作为软模板,模板剂用量高且仅在特定情况下才能形成介孔材料所需的相分布,对制备工艺要求高。因此,探索制备过程简便且能精确合成介孔炭材料的方法显得非常重要。Template method is divided into hard template method and soft template method. The hard template method refers to using a pre-prepared mesoporous silicon molecular sieve with a specific pore structure as a template, first filling the carbon precursor into the pores of the molecular sieve, and then removing the silicon template with sodium hydroxide or hydrofluoric acid to obtain Mesoporous carbon materials; the soft template method refers to the direct use of surfactants as structure-directing agents, which are combined with carbon precursors through the action of hydrogen bonds. , the carbon precursor becomes the skeleton of the pores after carbonization. Although the template method has the advantages of precisely controlling the pore size and pore distribution, it also has certain disadvantages. In the preparation of mesoporous carbon materials, the hard template method often needs to synthesize a hard template first, and then remove the template by etching. This method consumes a lot of hard templates and costs extremely high. In addition, the hard template method often has high requirements on carbon materials, such as better compatibility between the precursor and the hard template, and a mutually supporting structure between the pores to avoid the dislocation of the carbon material structure after the template is washed away. Compared with the hard template method, the soft template method does not require the participation of the silicon source and the removal of the silicon template, which avoids the cumbersome steps and waste of resources, but the soft template method generally requires an expensive block copolymer as a soft template. , the amount of template agent is high and the phase distribution required for mesoporous materials can be formed only under certain circumstances, which requires high preparation process. Therefore, it is very important to explore methods for facile preparation and accurate synthesis of mesoporous carbon materials.

纤维素作为地球上最丰富的天然可再生资源,是自然界分布最广的一种生物高分子。而纳米纤维素是由天然纤维素经过机械作用或水解获得的一种纳米级纤维素,主要包括纤维素纳米晶和纤维素纳米纤维两类。纳米纤维素一般具有较高的长径比,它的直径分布一般分布在3-50nm,符合介孔的直径范围。此外,纳米纤维素的热降解温度一般要低于炭材料的热降解温度,因此以纳米纤维素作为模板剂可以十分方便地合成出介孔炭材料。As the most abundant natural renewable resource on earth, cellulose is the most widely distributed biopolymer in nature. Nanocellulose is a kind of nano-scale cellulose obtained by mechanical action or hydrolysis of natural cellulose, mainly including cellulose nanocrystals and cellulose nanofibers. Nanocellulose generally has a high aspect ratio, and its diameter distribution is generally 3-50 nm, which is in line with the diameter range of mesopores. In addition, the thermal degradation temperature of nanocellulose is generally lower than that of carbon materials, so it is very convenient to synthesize mesoporous carbon materials using nanocellulose as a template.

发明内容SUMMARY OF THE INVENTION

本发明针对上述现有技术存在的缺陷,提供了一种以纳米纤维素为模板制备介孔炭材料的方法,该方法简单可靠,可以根据所用模板剂的尺寸和用量精准的控制炭材料孔径的尺寸和分布,为介孔炭材料的制备提供了一种新的简便的方法。Aiming at the defects of the above-mentioned prior art, the present invention provides a method for preparing mesoporous carbon materials by using nanocellulose as a template. size and distribution, providing a new and facile method for the preparation of mesoporous carbon materials.

本发明采用的技术方案如下:The technical scheme adopted in the present invention is as follows:

一种介孔炭材料的制备方法,其特征在于,包括以下步骤:A method for preparing a mesoporous carbon material, comprising the following steps:

(1)酚醛树脂前驱体溶液的制备:将苯酚、甲醛溶液和碱溶液混合,升至反应温度,反应一段时间,降至室温,得酚醛树脂前驱体溶液;(1) preparation of phenolic resin precursor solution: mix phenol, formaldehyde solution and alkaline solution, raise the temperature to reaction temperature, react for a period of time, and then drop to room temperature to obtain phenolic resin precursor solution;

(2)前驱体与模板剂共混:将步骤(1)得到的酚醛树脂前驱体溶液与模板剂共混,超声处理一段时间;(2) Blending the precursor and the templating agent: blending the phenolic resin precursor solution obtained in step (1) with the templating agent, and ultrasonically treating it for a period of time;

(3)固化:将步骤(2)得到的混合物加热至固化温度,固化一段时间;(3) curing: the mixture obtained in step (2) is heated to the curing temperature, and cured for a period of time;

(4)炭化:将步骤(3)得到的固化产物在惰性气体氛围下程序升温炭化一段时间;(4) carbonization: the solidified product obtained in step (3) is carbonized for a period of time by temperature-programmed heating under an inert gas atmosphere;

(5)后处理:对步骤(4)得到的炭化产物进行粉碎,清洗、除杂、过滤、烘干,得介孔炭材料;(5) post-treatment: pulverize the carbonized product obtained in step (4), clean, remove impurities, filter and dry to obtain mesoporous carbon material;

所述步骤(1)中碱溶液为氢氧化钠溶液、氢氧化钾溶液、氨水中的至少一种;所述的苯酚、甲醛溶液和碱溶液中苯酚:甲醛:碱的摩尔比为1:0.5~3:0.1~0.5;所述反应温度为50~100℃;所述反应时间为0.5~4小时;In the described step (1), the alkali solution is at least one of sodium hydroxide solution, potassium hydroxide solution, and ammonia; in the described phenol, formaldehyde solution and alkali solution, the mol ratio of phenol: formaldehyde: alkali is 1:0.5 ~3: 0.1 to 0.5; the reaction temperature is 50 to 100°C; the reaction time is 0.5 to 4 hours;

所述步骤(2)中模板剂为纤维素纳米晶和纤维素纳米纤维中的至少一种;所述的酚醛树脂前驱体溶液和模板剂的质量比为1:0.05~2,所述的超声时间为5~60分钟;In the step (2), the templating agent is at least one of cellulose nanocrystals and cellulose nanofibers; the mass ratio of the phenolic resin precursor solution and the templating agent is 1:0.05-2, and the ultrasonic The time is 5 to 60 minutes;

所述步骤(3)中固化温度为120~180℃;所述反应时间为5~60分钟;In the step (3), the curing temperature is 120-180° C.; the reaction time is 5-60 minutes;

所述步骤(4)中惰性气体为氮气、氩气中的至少一种;所述的程序升温为以1~10℃/min的速率升温至300~400℃,保温0.5~2小时,继续以1~10℃/min的速率升温至600~900℃,保温0.5~4小时,然后自然降至室温。In the step (4), the inert gas is at least one of nitrogen gas and argon gas; the temperature program is to heat up to 300 to 400 ° C at a rate of 1 to 10 ° C/min, keep the temperature for 0.5 to 2 hours, and continue to use The temperature is raised to 600-900°C at a rate of 1-10°C/min, kept for 0.5-4 hours, and then naturally lowered to room temperature.

本发明的显著优点在于:The significant advantages of the present invention are:

本发明利用纳米纤维素为模板制备介孔炭材料,相比于其他介孔炭材料制备方法,该操作方法简单易行,生产成本低,制备出的介孔炭材料具有孔径尺寸可控、孔道均匀、结构稳定等优点。Compared with other preparation methods of mesoporous carbon materials, the operation method is simple and feasible, and the production cost is low, and the prepared mesoporous carbon material has controllable pore size and pore channels. Uniform and stable structure.

具体实施方式Detailed ways

下面结合实施例,对发明作进一步详细说明,但本发明的实施方式不限于此。The invention will be described in further detail below with reference to the examples, but the embodiments of the present invention are not limited thereto.

实施例1Example 1

(1)酚醛树脂前驱体溶液的制备:称取9.4克苯酚、16.2克甲醛溶液和2.8克20%的氢氧化钾溶液混合,在70℃的恒温水浴锅中加热,反应时间为1小时,降至室温,得到酚醛树脂前驱体溶液。(1) Preparation of phenolic resin precursor solution: 9.4 grams of phenol, 16.2 grams of formaldehyde solution and 2.8 grams of 20% potassium hydroxide solution were weighed and mixed, and heated in a constant temperature water bath at 70°C. The reaction time was 1 hour. to room temperature to obtain a phenolic resin precursor solution.

(2)前驱体与模板剂共混:称取步骤(1)制得的酚醛树脂4.75克和0.25克纤维素纳米晶混合,超声5分钟。(2) Blending the precursor and the template agent: Weigh 4.75 g of the phenolic resin obtained in step (1) and 0.25 g of cellulose nanocrystals, mix, and ultrasonicate for 5 minutes.

(3)固化:将步骤(2)所得的产物加热至150℃,固化1小时。(3) Curing: The product obtained in step (2) is heated to 150° C. and cured for 1 hour.

(4)炭化:将步骤(3)所得的固化产物在氮气的氛围下程序升温炭化一段时间,所述的程序升温为3℃/min升温至300℃,保温1小时,继续2℃/min升温至700℃,保温2小时,然后自然降至室温。(4) carbonization: the solidified product obtained in step (3) is temperature-programmed and carbonized for a period of time under the atmosphere of nitrogen, and the temperature-programmed temperature is 3°C/min to be warmed to 300°C, maintained for 1 hour, and continued to heat up at 2°C/min to 700°C, incubated for 2 hours, and then cooled to room temperature naturally.

(5)后处理:对步骤(4)得到的炭化产物进行粉碎、清洗、除杂、过滤、烘干,得到介孔炭材料。(5) Post-treatment: pulverizing, washing, removing impurities, filtering and drying the carbonized product obtained in step (4) to obtain a mesoporous carbon material.

实施例2Example 2

(1)酚醛树脂前驱体溶液的制备:称取9.4克苯酚、11.9克甲醛溶液和2.8克20%的氢氧化钾溶液混合,在70℃的恒温水浴锅中加热,反应时间为1小时,降至室温,得到酚醛树脂前驱体溶液。(1) Preparation of phenolic resin precursor solution: 9.4 grams of phenol, 11.9 grams of formaldehyde solution and 2.8 grams of 20% potassium hydroxide solution were weighed and mixed, heated in a constant temperature water bath at 70°C, the reaction time was 1 hour, and the reaction time was 1 hour. to room temperature to obtain a phenolic resin precursor solution.

(2)前驱体与模板剂共混:称取步骤(1)制得的酚醛树脂4.5克和0.5克纤维素纳米晶混合,超声15分钟。(2) Blending the precursor and the template agent: Weigh 4.5 g of the phenolic resin obtained in step (1) and 0.5 g of cellulose nanocrystals, mix, and ultrasonicate for 15 minutes.

(3)固化:将步骤(2)所得的产物加热至160℃,固化1小时。(3) Curing: The product obtained in step (2) is heated to 160° C. and cured for 1 hour.

(4)炭化:将步骤(3)所得的固化产物在氮气的氛围下程序升温炭化一段时间,所述的程序升温为3℃/min升温至350℃,保温1小时,继续2℃/min升温至750℃,保温2小时,然后自然降至室温。(4) carbonization: the solidified product obtained in step (3) is temperature-programmed and carbonized for a period of time under the atmosphere of nitrogen, and the temperature-programmed temperature is 3°C/min to be warmed to 350°C, maintained for 1 hour, and continued to heat up at 2°C/min to 750°C, incubated for 2 hours, and then naturally cooled to room temperature.

(5)后处理:对步骤(4)得到的炭化产物进行粉碎、清洗、除杂、过滤、烘干,得到介孔炭材料。(5) Post-treatment: pulverizing, washing, removing impurities, filtering and drying the carbonized product obtained in step (4) to obtain a mesoporous carbon material.

实施例3Example 3

(1)酚醛树脂前驱体溶液的制备:称取9.4克苯酚、17.8克甲醛溶液和2.8克20%的氢氧化钾溶液混合,在80℃的恒温水浴锅中加热,反应时间为0.5小时,降至室温,得到酚醛树脂前驱体溶液。(1) Preparation of phenolic resin precursor solution: Weigh 9.4 grams of phenol, 17.8 grams of formaldehyde solution and 2.8 grams of 20% potassium hydroxide solution, mix them, and heat them in a constant temperature water bath at 80°C. The reaction time is 0.5 hours. to room temperature to obtain a phenolic resin precursor solution.

(2)前驱体与模板剂共混:称取步骤(1)制得的酚醛树脂4克和1克纤维素纳米晶混合,超声30分钟。(2) Blending the precursor and the template agent: Weigh 4 grams of the phenolic resin obtained in step (1) and 1 gram of cellulose nanocrystals and mix, and sonicate for 30 minutes.

(3)固化:将步骤(2)所得的产物加热至170℃,固化1小时。(3) Curing: The product obtained in step (2) was heated to 170° C. and cured for 1 hour.

(4)炭化:将步骤(3)所得的固化产物在氮气的氛围下程序升温炭化一段时间,所述的程序升温为5℃/min升温至400℃,保温1.5小时,继续5℃/min升温至800℃,保温2小时,然后自然降至室温。(4) carbonization: the solidified product obtained in step (3) is temperature-programmed and carbonized for a period of time under the atmosphere of nitrogen, and the temperature-programmed temperature is 5°C/min to be warmed to 400°C, maintained for 1.5 hours, and continued to heat up at 5°C/min to 800°C, incubated for 2 hours, and then cooled to room temperature naturally.

(5)后处理:对步骤(4)得到的炭化产物进行粉碎、清洗、除杂、过滤、烘干,得到介孔炭材料。(5) Post-treatment: pulverizing, washing, removing impurities, filtering and drying the carbonized product obtained in step (4) to obtain a mesoporous carbon material.

实施例4Example 4

(1)酚醛树脂前驱体溶液的制备:称取9.4克苯酚、16.2克甲醛溶液和14克20%的氢氧化钠溶液混合,在70℃的恒温水浴锅中加热,反应时间为1小时,降至室温,得到酚醛树脂前驱体溶液。(1) Preparation of phenolic resin precursor solution: 9.4 grams of phenol, 16.2 grams of formaldehyde solution and 14 grams of 20% sodium hydroxide solution were weighed and mixed, and heated in a constant temperature water bath at 70°C. The reaction time was 1 hour. to room temperature to obtain a phenolic resin precursor solution.

(2)前驱体与模板剂共混:称取步骤(1)制得的酚醛树脂4.75克和0.25克纤维素纳米纤维并混合,超声40分钟。(2) Blending the precursor and the template agent: Weigh 4.75 g of the phenolic resin and 0.25 g of the cellulose nanofibers obtained in step (1) and mix, and sonicate for 40 minutes.

(3)固化:将步骤(2)所得的产物加热至150℃,固化1小时。(3) Curing: The product obtained in step (2) is heated to 150° C. and cured for 1 hour.

(4)炭化:将步骤(3)所得的固化产物在氮气的氛围下程序升温炭化一段时间,所述的程序升温为3℃/min升温至350℃,保温1小时,继续2℃/min升温至700℃,保温2小时,然后自然降至室温。(4) carbonization: the solidified product obtained in step (3) is temperature-programmed and carbonized for a period of time under the atmosphere of nitrogen, and the temperature-programmed temperature is 3°C/min to be warmed to 350°C, maintained for 1 hour, and continued to heat up at 2°C/min to 700°C, incubated for 2 hours, and then cooled to room temperature naturally.

(5)后处理:对步骤(4)得到的炭化产物进行粉碎、清洗、除杂、过滤、烘干,得到介孔炭材料。(5) Post-treatment: pulverizing, washing, removing impurities, filtering and drying the carbonized product obtained in step (4) to obtain a mesoporous carbon material.

实施例5Example 5

(1)酚醛树脂前驱体溶液的制备:称取9.4克苯酚、16.2克甲醛溶液和2.8克氨水溶液混合,在70℃的恒温水浴锅中加热,反应时间为1小时,降至室温,得到酚醛树脂前驱体溶液。(1) Preparation of phenolic resin precursor solution: Weigh 9.4 grams of phenol, 16.2 grams of formaldehyde solution and 2.8 grams of ammonia solution and mix, heat in a constant temperature water bath at 70°C, and the reaction time is 1 hour, and it is lowered to room temperature to obtain phenolic Resin precursor solution.

(2)前驱体与模板剂共混:称取步骤(1)制得的酚醛树脂4克和1克纤维素纳米纤维并混合,超声60分钟。(2) Blending of precursor and template agent: 4 grams of phenolic resin and 1 gram of cellulose nanofibers obtained in step (1) were weighed and mixed, and sonicated for 60 minutes.

(3)固化:将步骤(2)所得的产物加热至150℃,固化1小时。(3) Curing: The product obtained in step (2) is heated to 150° C. and cured for 1 hour.

(4)炭化:将步骤(3)所得的固化产物在氮气的氛围下程序升温炭化一段时间,所述的程序升温为3℃/min升温至350℃,保温1小时,继续2℃/min升温至700℃,保温2小时,然后自然降至室温。(4) carbonization: the solidified product obtained in step (3) is temperature-programmed and carbonized for a period of time under the atmosphere of nitrogen, and the temperature-programmed temperature is 3°C/min to be warmed to 350°C, maintained for 1 hour, and continued to heat up at 2°C/min to 700°C, incubated for 2 hours, and then cooled to room temperature naturally.

(5)后处理:对步骤(4)得到的炭化产物进行粉碎、清洗、除杂、过滤、烘干,得到介孔炭材料。(5) Post-treatment: pulverizing, washing, removing impurities, filtering and drying the carbonized product obtained in step (4) to obtain a mesoporous carbon material.

Claims (1)

1.一种介孔炭材料的制备方法,其特征在于,包括以下步骤:1. a preparation method of mesoporous carbon material, is characterized in that, comprises the following steps: (1)酚醛树脂前驱体溶液的制备:将苯酚、甲醛溶液和碱溶液混合,升至反应温度,反应一段时间,降至室温,得酚醛树脂前驱体溶液;(1) preparation of phenolic resin precursor solution: mix phenol, formaldehyde solution and alkaline solution, raise the temperature to reaction temperature, react for a period of time, and then drop to room temperature to obtain phenolic resin precursor solution; (2)前驱体与模板剂共混:将步骤(1)得到的酚醛树脂前驱体溶液与模板剂共混,超声处理一段时间;(2) Blending the precursor and the templating agent: blending the phenolic resin precursor solution obtained in step (1) with the templating agent, and ultrasonically treating it for a period of time; (3)固化:将步骤(2)得到的混合物加热至固化温度,固化一段时间;(3) curing: the mixture obtained in step (2) is heated to the curing temperature, and cured for a period of time; (4)炭化:将步骤(3)得到的固化产物在惰性气体氛围下程序升温炭化一段时间;(4) carbonization: the solidified product obtained in step (3) is carbonized for a period of time by temperature-programmed heating under an inert gas atmosphere; (5)后处理:对步骤(4)得到的炭化产物进行粉碎,清洗、除杂、过滤、烘干,得介孔炭材料;(5) post-treatment: pulverize the carbonized product obtained in step (4), clean, remove impurities, filter and dry to obtain mesoporous carbon material; 所述步骤(1)中碱溶液为氢氧化钠溶液、氢氧化钾溶液、氨水中的至少一种;所述的苯酚、甲醛溶液和碱溶液中苯酚:甲醛:碱的摩尔比为1:0.5~3:0.1~0.5;所述反应温度为50~100℃;所述反应时间为0.5~4小时;In the described step (1), the alkali solution is at least one of sodium hydroxide solution, potassium hydroxide solution, and ammonia; in the described phenol, formaldehyde solution and alkali solution, the mol ratio of phenol: formaldehyde: alkali is 1:0.5 ~3: 0.1 to 0.5; the reaction temperature is 50 to 100°C; the reaction time is 0.5 to 4 hours; 所述步骤(2)中模板剂为纤维素纳米晶和纤维素纳米纤维中的至少一种;所述的酚醛树脂前驱体溶液和模板剂的质量比为1:0.05~0.25,所述的超声时间为5~60分钟;In the step (2), the templating agent is at least one of cellulose nanocrystals and cellulose nanofibers; the mass ratio of the phenolic resin precursor solution and the templating agent is 1:0.05-0.25, and the ultrasonic The time is 5 to 60 minutes; 所述步骤(3)中固化温度为120~180℃;所述反应时间为5~60分钟;In the step (3), the curing temperature is 120-180° C.; the reaction time is 5-60 minutes; 所述步骤(4)中惰性气体为氮气、氩气中的至少一种;所述的程序升温为以1~10℃/min的速率升温至300~400℃,保温0.5~2小时,继续以1~10℃/min的速率升温至600~900℃,保温0.5~4小时,然后自然降至室温。In the step (4), the inert gas is at least one of nitrogen gas and argon gas; the temperature program is to heat up to 300 to 400 ° C at a rate of 1 to 10 ° C/min, keep the temperature for 0.5 to 2 hours, and continue to use The temperature is raised to 600-900°C at a rate of 1-10°C/min, kept for 0.5-4 hours, and then naturally lowered to room temperature.
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