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CN110589794A - A kind of preparation method of large size porous carbon material - Google Patents

A kind of preparation method of large size porous carbon material Download PDF

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CN110589794A
CN110589794A CN201910844404.1A CN201910844404A CN110589794A CN 110589794 A CN110589794 A CN 110589794A CN 201910844404 A CN201910844404 A CN 201910844404A CN 110589794 A CN110589794 A CN 110589794A
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carbon
nitrogen composite
composite material
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silicon dioxide
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张展
穆春丰
张大奎
贾楠楠
张馨予
姚君
王晓楠
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Anshan Chemical Technology Co Ltd
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    • B82NANOTECHNOLOGY
    • B82YSPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
    • B82Y40/00Manufacture or treatment of nanostructures
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    • C01B32/05Preparation or purification of carbon not covered by groups C01B32/15, C01B32/20, C01B32/25, C01B32/30

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Abstract

本发明涉及一种大尺寸多孔碳材料的制备方法,1)将二氧化硅磨成粉末,烘干;2)加入表面活性剂聚乙烯吡咯烷酮PVP和正硅酸乙酯TEOS,充分搅拌,二氧化硅粉末完全浸润液体后取出,干燥将表面活性剂蒸干,形成碳氮复合小球;3)将碳氮复合小球加入反应釜中,以乙二醇为溶剂,聚合生成小球聚合物;4)将小球聚合物和氨腈混合,形成碳氮复合材料前驱体,煅烧,形成碳氮复合材料;5)在碳氮复合材料中加入溶剂乙醇,在负压条件下进行搅拌,使二氧化硅为核心的碳氮复合小球脱离碳氮复合材料,碳氮复合小球抽滤排出,抽滤后的残留物干燥去除乙醇,完成大尺寸多孔碳材料的制备。本发明保证碳材料结构强度的基础上,降低碳材料15%以上的重量。

The present invention relates to a kind of preparation method of large-size porous carbon material, 1) grind silicon dioxide into powder, dry; After the powder is completely soaked in the liquid, take it out, dry and evaporate the surfactant to dryness to form a carbon-nitrogen composite pellet; 3) Add the carbon-nitrogen composite pellet to the reaction kettle, use ethylene glycol as a solvent, and polymerize to form a pellet polymer; 4 ) mixing the pellet polymer and cyanamide to form a carbon-nitrogen composite material precursor, calcining to form a carbon-nitrogen composite material; 5) adding solvent ethanol to the carbon-nitrogen composite material, and stirring under negative pressure to make the carbon dioxide The carbon-nitrogen composite balls with silicon as the core are separated from the carbon-nitrogen composite material, and the carbon-nitrogen composite balls are discharged by suction filtration, and the residue after suction filtration is dried to remove ethanol, and the preparation of large-size porous carbon materials is completed. On the basis of ensuring the structural strength of the carbon material, the invention reduces the weight of the carbon material by more than 15%.

Description

一种大尺寸多孔碳材料的制备方法A kind of preparation method of large size porous carbon material

技术领域technical field

本发明涉及炼焦领域,特别涉及一种大尺寸多孔碳材料的制备方法。The invention relates to the field of coking, in particular to a method for preparing a large-size porous carbon material.

背景技术Background technique

碳纤维材料最早从上世纪70年代开始应用,一直作为高性能材料应用于航空航天和奢侈品行业。近年来,随着航空航天技术的商用化和民众消费水平的提高,通用级碳纤维(聚丙烯腈基碳纤维)广泛应用于家用汽车、高端运动产品和传统工业。但是,高性能碳纤维一直受困于性能和成本的两方面影响,商用化进程缓慢。Carbon fiber materials were first used in the 1970s and have been used as high-performance materials in aerospace and luxury industries. In recent years, with the commercialization of aerospace technology and the improvement of public consumption, general-purpose carbon fibers (polyacrylonitrile-based carbon fibers) are widely used in household cars, high-end sports products and traditional industries. However, high-performance carbon fiber has been suffering from two aspects of performance and cost, and the commercialization process is slow.

碳纤维与普通碳素材料相比的的优点是强度高、重量轻,缺点是价格昂贵,生产工艺复杂。如果能在保持普通碳材料强度的基础上,尽可能的降低碳材料的重量,即可实现碳材料商用化的目标。目前最主流的技术方案是在碳素材料中构造孔洞,降低碳素材料的整体质量。Compared with ordinary carbon materials, carbon fiber has the advantages of high strength and light weight, but the disadvantage is that it is expensive and the production process is complicated. If the weight of carbon materials can be reduced as much as possible while maintaining the strength of ordinary carbon materials, the goal of commercialization of carbon materials can be achieved. At present, the most mainstream technical solution is to construct holes in carbon materials to reduce the overall quality of carbon materials.

目前流行的工艺技术主要采用物理加工方式,物理打孔或者球磨方式容易破坏现有碳材料的微观结构,造成整体强度下降。因此如果能开发一种化学加工方式,在不影响微观结构的基础上,降低碳材料重量,将快速实现碳材料商用化的目标。The current popular technology mainly adopts physical processing methods. Physical drilling or ball milling methods are easy to damage the microstructure of existing carbon materials, resulting in a decrease in overall strength. Therefore, if a chemical processing method can be developed to reduce the weight of carbon materials without affecting the microstructure, the goal of commercialization of carbon materials will be quickly realized.

专利CN201710247691.9一种小尺寸多孔碳纳米球的制备方法,将表面活性剂、有机烃类和氨水混合成澄清透明的溶液,加入间苯二酚和甲醛水溶液的混合物,搅拌形成反相微乳液体系;将该体系转入含聚四氟乙烯内衬的水热釜内密封,在80~120℃下热处理10~24h;降温后向反应液中加入破乳剂,超声、离心、洗涤、干燥、研磨、惰性气氛下高温焙烧后得到碳纳米球。本发明所述小尺寸碳纳米球的制备方法,工艺简单、经济,并且可以通过改变反应条件控制碳纳米球的尺寸。该专利采用化学和物理方法结合的方式,最后采用研磨的方式进行造型。研磨影响材料的结构强度,与纯化学处理工艺不同。Patent CN201710247691.9 A preparation method of small-sized porous carbon nanospheres, mixing surfactants, organic hydrocarbons and ammonia water into a clear and transparent solution, adding a mixture of resorcinol and formaldehyde aqueous solution, and stirring to form an inverse microemulsion system; transfer the system into a hydrothermal kettle with a polytetrafluoroethylene liner and seal it, heat treatment at 80-120°C for 10-24 hours; add a demulsifier to the reaction solution after cooling down, ultrasonication, centrifugation, washing, drying, The carbon nanospheres are obtained after grinding and high-temperature calcination under an inert atmosphere. The preparation method of the small-sized carbon nanosphere of the present invention has a simple and economical process, and the size of the carbon nanosphere can be controlled by changing the reaction conditions. The patent uses a combination of chemical and physical methods, and finally uses grinding to shape. Grinding affects the structural strength of the material, unlike purely chemical processing.

专利CN201510563597.5一种黑二氧化钛纳米棒可见光光催化剂的制备方法,本发明是要解决现有方法制备的二氧化钛对太阳光的利用率低及二氧化钛作为催化剂的电荷传输效率低的技术问题。方法:一、制备混合液;二、制备反应液;三、洗涤干燥;四、球磨;五、煅烧;六、洗涤干燥,得到黑二氧化钛纳米棒可见光光催化剂。优点:本发明制备的黑二氧化钛纳米棒可见光催化剂降解罗明丹B的降解率大于94%;本发明制备的黑二氧化钛纳米棒可见光光催化剂为棒状,尺寸为150nm~300nm。该专利采用球磨的方式进行加工,物理加工最终会影响材料的结构强度。Patent CN201510563597.5 is a preparation method of black titanium dioxide nanorod visible light photocatalyst. The present invention is to solve the technical problems of low utilization rate of sunlight by titanium dioxide prepared by the existing method and low charge transfer efficiency of titanium dioxide as a catalyst. Methods: 1. Preparation of mixed liquid; 2. Preparation of reaction liquid; 3. Washing and drying; 4. Ball milling; 5. Calcination; Advantages: the visible light photocatalyst of black titanium dioxide nanorods prepared by the present invention has a degradation rate of more than 94% for degrading rhomboid B; the visible light photocatalyst of black titanium dioxide nanorods prepared by the present invention is rod-shaped with a size of 150nm to 300nm. The patent uses ball milling for processing, and physical processing will eventually affect the structural strength of the material.

发明内容Contents of the invention

本发明所要解决的技术问题是提供一种大尺寸多孔碳材料的制备方法,不影响碳材料结构强度的基础上,降低碳材料15%以上的重量。为实现上述目的,本发明采用以下技术方案实现:The technical problem to be solved by the present invention is to provide a method for preparing a large-size porous carbon material, which can reduce the weight of the carbon material by more than 15% without affecting the structural strength of the carbon material. To achieve the above object, the present invention adopts the following technical solutions:

一种大尺寸多孔碳材料的制备方法,具体包括以下步骤:A method for preparing a large-scale porous carbon material, specifically comprising the following steps:

(1)将二氧化硅磨成直径5-8μm的粉末,在80-100℃的范围内烘干2-4h,完全排出水分;(1) Grind silicon dioxide into a powder with a diameter of 5-8 μm, and dry it in the range of 80-100 ° C for 2-4 hours to completely discharge the water;

(2)在二氧化硅粉末中加入表面活性剂聚乙烯吡咯烷酮PVP和正硅酸乙酯TEOS,三者的质量比为1:0.3-0.8:2-3,充分搅拌,二氧化硅粉末完全浸润液体后取出,在100-120℃的条件下干燥6-8h,将聚乙烯吡咯烷酮PVP蒸干,正硅酸乙酯TEOS包覆在二氧化硅表面,形成碳氮复合小球;(2) Add the surfactant polyvinylpyrrolidone PVP and ethyl tetrasilicate TEOS to the silicon dioxide powder, the mass ratio of the three is 1:0.3-0.8:2-3, stir well, the silicon dioxide powder is completely soaked in the liquid Then take it out, dry it at 100-120°C for 6-8 hours, evaporate the polyvinylpyrrolidone PVP to dryness, and coat the silica surface with TEOS to form carbon-nitrogen composite pellets;

(3)将碳氮复合小球加入反应釜中,以乙二醇为溶剂,乙二醇加入量为氮复合小球质量的4-6倍,温度控制在180-220℃之间,搅拌速率控制在45-60r/min之间,聚合反应持续2-4h,生成小球聚合物;(3) Put the carbon-nitrogen composite pellets into the reaction kettle, use ethylene glycol as the solvent, the amount of ethylene glycol added is 4-6 times the mass of the nitrogen composite pellets, the temperature is controlled between 180-220°C, and the stirring rate is Controlled between 45-60r/min, the polymerization reaction lasts for 2-4h to generate small spherical polymers;

(4)将小球聚合物和氨腈混合,氨腈加入量为小球聚合物质量的2-3倍,在60-80℃下进行搅拌,使氨腈完全浸润小球聚合物,形成碳氮复合材料前驱体,然后在1800-2000℃进行煅烧,去除乙二醇和残留的聚乙烯吡咯烷酮PVP,形成碳氮复合材料;(4) Mix the bead polymer and cyanamide, the amount of cyanamide added is 2-3 times the mass of the bead polymer, and stir at 60-80°C, so that the bead polymer is completely infiltrated with cyanamide to form carbon The nitrogen composite material precursor is then calcined at 1800-2000°C to remove ethylene glycol and residual polyvinylpyrrolidone PVP to form a carbon-nitrogen composite material;

(5)在碳氮复合材料中加入溶剂乙醇,乙醇加入量为碳氮复合材料质量的8-10倍,在负压条件下进行搅拌,使二氧化硅为核心的碳氮复合小球脱离碳氮复合材料,并随溶剂在负压条件下抽滤排出,抽滤后的残留物在60-80℃的条件下进行干燥去除乙醇,完成大尺寸多孔碳材料的制备。(5) Add solvent ethanol to the carbon-nitrogen composite material, the amount of ethanol added is 8-10 times of the mass of the carbon-nitrogen composite material, stir under negative pressure conditions, so that the carbon-nitrogen composite pellets with silicon dioxide as the core are separated from carbon Nitrogen composite material, and the solvent is discharged under negative pressure by suction filtration, and the residue after suction filtration is dried at 60-80°C to remove ethanol, and the preparation of large-scale porous carbon material is completed.

所述的大尺寸多孔碳材料的孔径直径大于50nm。The pore diameter of the large-size porous carbon material is larger than 50nm.

与现有的技术相比,本发明的有益效果是:Compared with prior art, the beneficial effect of the present invention is:

本发明为化学方法制备大尺寸多孔碳材料,不影响碳材料结构强度的基础上,降低碳材料15%以上的重量。The invention prepares the large-size porous carbon material by chemical method, and reduces the weight of the carbon material by more than 15% on the basis of not affecting the structural strength of the carbon material.

本发明碳材料成孔原理:以二氧化硅为核心,通过包覆材料使其聚合,形成二氧化硅粉末的聚合物,微观下为小球聚集体。利用氨腈填满小球聚集体中的空隙,之后去除小球,小球原位置形成孔洞。The pore-forming principle of the carbon material of the present invention is as follows: silicon dioxide is used as the core, and the coating material is polymerized to form a polymer of silicon dioxide powder, which is a microscopic aggregate of small balls. Cyanamide is used to fill the gaps in the bead aggregates, and then the bead is removed to form a hole in its original position.

附图说明Description of drawings

图1为本发明的制备工艺流程图。Fig. 1 is the preparation process flowchart of the present invention.

具体实施方式Detailed ways

下面结合实施例对本发明进一步说明:Below in conjunction with embodiment the present invention is further described:

以下实施例对本发明进行详细描述。这些实施例仅是对本发明的最佳实施方案进行描述,并不对本发明的范围进行限制。The following examples describe the present invention in detail. These examples are only to describe the best embodiment of the present invention, and do not limit the scope of the present invention.

实施例1Example 1

一种大尺寸多孔碳材料的制备方法,具体包括:A method for preparing a large-scale porous carbon material, specifically comprising:

1)取二氧化硅20g,磨成平均粒径6μm的粉末,在90℃的条件下烘干3h,完全排出水分。1) Take 20g of silicon dioxide, grind it into a powder with an average particle size of 6μm, and dry it at 90°C for 3 hours to completely discharge the water.

2)在二氧化硅中加入表面活性剂聚乙烯吡咯烷酮8g和正硅酸乙酯30g,充分搅拌,二氧化硅粉末完全浸润液体后取出,在110℃的条件下干燥7h,将溶剂聚乙烯吡咯烷酮蒸干。使正硅酸乙酯包覆在二氧化硅表面,形成碳氮复合小球24g。2) Add 8 g of surfactant polyvinylpyrrolidone and 30 g of tetraethyl orthosilicate to silicon dioxide, stir well, take out the silicon dioxide powder after completely infiltrating the liquid, dry at 110°C for 7 hours, distill the solvent polyvinylpyrrolidone Dry. Coat the surface of silicon dioxide with tetraethyl orthosilicate to form 24 g of carbon-nitrogen composite pellets.

3)将碳氮复合小球加入反应釜中,加入120g乙二醇为溶剂,温度控制在190℃,搅拌速率控制在50r/min,聚合反应持续3h,生成小球的聚合物18g。3) Add carbon-nitrogen composite pellets into the reaction kettle, add 120g of ethylene glycol as a solvent, control the temperature at 190°C, control the stirring rate at 50r/min, and continue the polymerization reaction for 3 hours to form 18g of polymer pellets.

4)将小球聚合物和36g氨腈混合,在80℃下进行搅拌,使氨腈完全浸润小球聚合物,形成碳氮复合材料前驱体26g。然后在1900℃进行煅烧,去除乙二醇和残留的聚乙烯吡咯烷酮PVP,形成碳氮复合材料23g。4) Mix the pellet polymer and 36 g of cyanamide, and stir at 80° C. to completely infiltrate the pellet polymer with cyanamide to form 26 g of carbon-nitrogen composite material precursor. Calcination was then carried out at 1900° C. to remove ethylene glycol and residual polyvinylpyrrolidone PVP to form 23 g of carbon-nitrogen composite materials.

5)在碳氮复合材料中加入190g乙醇,在负压条件下进行搅拌,使二氧化硅为核心的碳氮复合小球脱离碳氮复合材料,并随溶剂在负压条件下抽滤排出。抽滤后的残留物在60℃的条件下进行干燥,形成大尺寸多孔碳材料7.4g。5) Add 190 g of ethanol to the carbon-nitrogen composite material, and stir under negative pressure to make the carbon-nitrogen composite pellets with silicon dioxide as the core separate from the carbon-nitrogen composite material, and discharge them by suction filtration with the solvent under negative pressure. The residue after suction filtration was dried at 60° C. to form 7.4 g of a large-sized porous carbon material.

经测量,上述材料真密度1.63g/m3,与市场主流碳材料国标(真密度大于2.12g/m3)相比,降低23.1%,抗拉强度3400MPa,与同等级T700碳纤维相同。After measurement, the true density of the above material is 1.63g/m3, which is 23.1% lower than the national standard of mainstream carbon materials in the market (true density greater than 2.12g/m3), and the tensile strength is 3400MPa, which is the same as that of T700 carbon fiber of the same grade.

实施例2Example 2

一种大尺寸多孔碳材料的制备方法,具体包括:A method for preparing a large-scale porous carbon material, specifically comprising:

1)取二氧化硅10g,磨成平均粒径7μm的粉末,在80℃的条件下烘干2h,完全排出水分。1) Take 10g of silicon dioxide, grind it into a powder with an average particle size of 7μm, and dry it at 80°C for 2 hours to completely discharge the water.

2)在氧化硅中加入表面活性剂聚乙烯吡咯烷酮3g和正硅酸乙酯15g,充分搅拌,二氧化硅粉末完全浸润液体后取出,在100℃的条件下干燥6h,将溶剂全部蒸干。使正硅酸乙酯包覆在二氧化硅表面,形成碳氮复合小球13g。2) Add 3 g of surfactant polyvinylpyrrolidone and 15 g of tetraethyl orthosilicate to silicon oxide, stir well, take out the silicon dioxide powder after completely infiltrating the liquid, dry at 100°C for 6 hours, and evaporate all the solvent to dryness. Coat the surface of silicon dioxide with ethyl orthosilicate to form 13 g of carbon-nitrogen composite pellets.

3)将碳氮复合小球加入反应釜中,加入55g乙二醇为溶剂,温度控制在180℃,搅拌速率控制在45r/min,聚合反应持续2h,生成小球的聚合物12g。3) Add carbon-nitrogen composite pellets into the reaction kettle, add 55g of ethylene glycol as a solvent, control the temperature at 180°C, control the stirring rate at 45r/min, and continue the polymerization reaction for 2 hours to form 12g of polymer pellets.

4)将小球聚合物和25g氨腈混合,在70℃下进行搅拌,使氨腈完全浸润小球聚合物,形成碳氮复合材料前驱体17g。然后在1900℃进行煅烧,去除乙二醇和残留的聚乙烯吡咯烷酮PVP,形成碳氮复合材料15g。4) Mix the pellet polymer and 25 g of cyanamide, and stir at 70° C., so that the pellet polymer is completely infiltrated with cyanamide to form 17 g of carbon-nitrogen composite material precursor. Calcination was then carried out at 1900° C. to remove ethylene glycol and residual polyvinylpyrrolidone PVP to form 15 g of carbon-nitrogen composite materials.

5)在碳氮复合材料中加入120g乙醇,在负压条件下进行搅拌,使二氧化硅为核心的小球脱离碳氮复合材料,并随溶剂在负压条件下抽滤排出。抽滤后的残留物在70℃的条件下进行干燥,形成大尺寸多孔碳材料4.3g。5) Add 120 g of ethanol to the carbon-nitrogen composite material, and stir under negative pressure to separate the silica-cored balls from the carbon-nitrogen composite material, and discharge them by suction filtration with the solvent under negative pressure. The residue after suction filtration was dried at 70° C. to form 4.3 g of large-sized porous carbon material.

经测量,上述材料真密度1.72g/m3,与市场主流碳材料国标(真密度大于2.12g/m3)相比,降低18.9%,抗拉强度3400MPa,与同等级T700碳纤维相同。After measurement, the true density of the above-mentioned material is 1.72g/m3, which is 18.9% lower than the national standard of mainstream carbon materials in the market (true density greater than 2.12g/m3), and the tensile strength is 3400MPa, which is the same as that of T700 carbon fiber of the same grade.

实施例3Example 3

1)取二氧化硅100g,磨成平均粒径5μm的粉末,在100℃的条件下烘干4h,完全排出水分。1) Take 100g of silicon dioxide, grind it into a powder with an average particle size of 5 μm, and dry it at 100°C for 4 hours to completely discharge the water.

2)在氧化硅中加入表面活性剂聚乙烯吡咯烷酮40g和正硅酸乙酯300g,充分搅拌,二氧化硅粉末完全浸润液体后取出,在120℃的条件下干燥8h,将溶剂全部蒸干。使正硅酸乙酯包覆在二氧化硅表面,形成碳氮复合小球136g。2) Add 40g of surfactant polyvinylpyrrolidone and 300g of tetraethyl orthosilicate to the silicon oxide, stir well, take out the silicon dioxide powder completely soaked in the liquid, dry at 120°C for 8 hours, and evaporate all the solvent to dryness. Ethyl orthosilicate was coated on the surface of silicon dioxide to form 136 g of carbon-nitrogen composite pellets.

3)将碳氮复合小球加入反应釜中,加入800g乙二醇为溶剂,温度控制在220℃,搅拌速率控制在60r/min,聚合反应持续4h,生成小球的聚合物122g。3) Add carbon-nitrogen composite pellets into the reactor, add 800g of ethylene glycol as a solvent, control the temperature at 220°C, control the stirring rate at 60r/min, and continue the polymerization reaction for 4 hours to form 122g of polymer pellets.

4)将小球聚合物和366g氨腈混合,在80℃下进行搅拌,使氨腈完全浸润小球聚合物,形成碳氮复合材料前驱体154g。然后在2000℃进行煅烧,去除乙二醇和残留的聚乙烯吡咯烷酮PVP,形成碳氮复合材料143g。4) The pellet polymer and 366g of cyanamide were mixed, and stirred at 80° C. to completely infiltrate the pellet polymer with cyanamide to form 154 g of carbon-nitrogen composite material precursor. Calcination was then carried out at 2000° C. to remove ethylene glycol and residual polyvinylpyrrolidone PVP to form 143 g of carbon-nitrogen composite materials.

5)在碳氮复合材料中加入1100g乙醇,在负压条件下进行搅拌,使二氧化硅为核心的小球脱离碳氮复合材料,并随溶剂在负压条件下抽滤排出。抽滤后的残留物在80℃的条件下进行干燥,形成大尺寸多孔碳材料28.6g。5) Add 1100 g of ethanol to the carbon-nitrogen composite material, and stir under negative pressure to make the silica-cored pellets separate from the carbon-nitrogen composite material, and then discharge it by suction filtration with the solvent under negative pressure. The residue after suction filtration was dried at 80° C. to form 28.6 g of a large-sized porous carbon material.

经测量,上述材料真密度1.67g/m3,与市场主流碳材料国标(真密度大于2.12g/m3)After measurement, the true density of the above material is 1.67g/m3, which is in line with the national standard of mainstream carbon materials in the market (true density greater than 2.12g/m3)

相比,降低20.9%,抗拉强度3400MPa,与同等级T700碳纤维相同。Compared with that, it is 20.9% lower, and the tensile strength is 3400MPa, which is the same as that of T700 carbon fiber of the same grade.

Claims (2)

1.一种大尺寸多孔碳材料的制备方法,其特征在于,具体包括以下步骤:1. A preparation method of a large-scale porous carbon material, characterized in that, specifically comprising the following steps: (1)将二氧化硅磨成直径5-8μm的粉末,在80-100℃的范围内烘干2-4h,完全排出水分;(1) Grind silicon dioxide into a powder with a diameter of 5-8 μm, and dry it in the range of 80-100 ° C for 2-4 hours to completely discharge the water; (2)在二氧化硅粉末中加入表面活性剂聚乙烯吡咯烷酮PVP和正硅酸乙酯TEOS,三者的质量比为1:0.3-0.8:2-3,充分搅拌,二氧化硅粉末完全浸润液体后取出,在100-120℃的条件下干燥6-8h,将聚乙烯吡咯烷酮PVP蒸干,正硅酸乙酯TEOS包覆在二氧化硅表面,形成碳氮复合小球;(2) Add the surfactant polyvinylpyrrolidone PVP and ethyl tetrasilicate TEOS to the silicon dioxide powder, the mass ratio of the three is 1:0.3-0.8:2-3, stir well, the silicon dioxide powder is completely soaked in the liquid Then take it out, dry it at 100-120°C for 6-8 hours, evaporate the polyvinylpyrrolidone PVP to dryness, and coat the silica surface with TEOS to form carbon-nitrogen composite pellets; (3)将碳氮复合小球加入反应釜中,以乙二醇为溶剂,乙二醇加入量为氮复合小球质量的4-6倍,温度控制在180-220℃之间,搅拌速率控制在45-60r/min之间,聚合反应持续2-4h,生成小球聚合物;(3) Put the carbon-nitrogen composite pellets into the reaction kettle, use ethylene glycol as the solvent, the amount of ethylene glycol added is 4-6 times the mass of the nitrogen composite pellets, the temperature is controlled between 180-220°C, and the stirring rate is Controlled between 45-60r/min, the polymerization reaction lasts for 2-4h to generate small spherical polymers; (4)将小球聚合物和氨腈混合,氨腈加入量为小球聚合物质量的2-3倍,在60-80℃下进行搅拌,使氨腈完全浸润小球聚合物,形成碳氮复合材料前驱体,然后在1800-2000℃进行煅烧,去除乙二醇和残留的聚乙烯吡咯烷酮PVP,形成碳氮复合材料;(4) Mix the bead polymer and cyanamide, the amount of cyanamide added is 2-3 times the mass of the bead polymer, and stir at 60-80°C, so that the bead polymer is completely infiltrated with cyanamide to form carbon The nitrogen composite material precursor is then calcined at 1800-2000°C to remove ethylene glycol and residual polyvinylpyrrolidone PVP to form a carbon-nitrogen composite material; (5)在碳氮复合材料中加入溶剂乙醇,乙醇加入量为碳氮复合材料质量的8-10倍,在负压条件下进行搅拌,使二氧化硅为核心的碳氮复合小球脱离碳氮复合材料,并随溶剂在负压条件下抽滤排出,抽滤后的残留物在60-80℃的条件下进行干燥去除乙醇,完成大尺寸多孔碳材料的制备。(5) Add solvent ethanol to the carbon-nitrogen composite material, the amount of ethanol added is 8-10 times of the mass of the carbon-nitrogen composite material, stir under negative pressure conditions, so that the carbon-nitrogen composite pellets with silicon dioxide as the core are separated from carbon Nitrogen composite material, and the solvent is discharged under negative pressure by suction filtration, and the residue after suction filtration is dried at 60-80°C to remove ethanol, and the preparation of large-scale porous carbon materials is completed. 2.根据权利要求1所述的一种大尺寸多孔碳材料的制备方法,其特征在于,所述的大尺寸多孔碳材料的孔径直径大于50nm。2. The preparation method of a large-size porous carbon material according to claim 1, characterized in that, the pore diameter of the large-size porous carbon material is greater than 50 nm.
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CN104418333A (en) * 2013-09-10 2015-03-18 中国科学院大连化学物理研究所 Method for preparing mesoporous silica hollow spheres
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Application publication date: 20191220