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Preparation method of high performance foam carbon

A foamed carbon, high-performance technology, used in carbon preparation/purification, chemical instruments and methods, carbon compounds, etc., can solve the problems of graphene dispersibility, mechanical properties and thermal conductivity, and achieve accelerated thermal polycondensation process, The effect of improving the interface bonding strength and shortening the time

Active Publication Date: 2019-10-18
HUNAN UNIV
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Problems solved by technology

[0004] In order to solve the problem of the dispersion of graphene in carbon foam and overcome the defects of insufficient mechanical properties and thermal conductivity of existing carbon foam, the present invention proposes a method for preparing high-performance carbon foam

Method used

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  • Preparation method of high performance foam carbon
  • Preparation method of high performance foam carbon
  • Preparation method of high performance foam carbon

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0030] 步骤1:将氧化石墨烯加入到乙醇溶液中超声处理1h得到分散液,接着往分散液中滴加十八胺单体,在60℃下回流反应8h,经过抽滤洗涤后得到十八胺接枝功能化石墨烯材料。

[0031] 步骤2:将十八胺接枝石墨烯材料加入乙醇中,然后将该混合溶液超声1h,得到分散的功能化石墨烯悬浮液,接着将占总质量0.2%的功能化石墨烯悬浮液与精制纯化的FCC油浆进行磁力搅拌混合并超声分散,随后通过减压蒸馏的方式除去多余的乙醇溶剂得到混合物。

[0032] 步骤3:将步骤2得到的混合物原料置于高压反应釜内进行直接热缩聚,在N 2 气氛和500r / min的搅拌速率下,将所述混合物以2°C / min的速率从室温升至420℃,然后调控釜内压力至3.5MPa,并在恒压条件下保温8小时,冷却后得到软化点为260°C的前躯体。

[0033] 步骤4:将前躯体研磨后过200目筛,放入可拆卸不锈钢模具中,在N 2 气体保护下,在高压反应釜中发泡,维持釜内恒压到6MPa,以1℃ / min 的升温速率升温至350℃,保温4h,保温结束后再以1℃ / min的升温速率升温至500℃,保温2h,冷却后获得石墨烯 / 泡沫碳生料。

[0034] 步骤5:将石墨烯 / 泡沫碳生料放入炭化炉内,以5℃ / min的升温速率升温至1000℃,保温3h;再将其放入高温石墨化炉中,以5℃ / min的升温速率升温至2800℃,保温1h,保温结束后自然冷却至室温,得到石墨烯增强高性能泡沫碳复合材料。

[0035] 所制得石墨烯增强高性能泡沫碳复合材料的密度为 0.51 g / cm 3 ,压缩强度为8.1 MPa,导热率为125 W / m·K。

Embodiment 2

[0037] 步骤1:将氧化石墨烯加入到N, N-二甲基甲酰胺溶液中超声处理3h得到分散液,在氮气气氛保护下往分散液中滴加异氰酸酯单体,在30°C下搅拌反应8h,经过抽滤洗涤后得到异氰酸酯接枝功能化石墨烯材料。

[0038] 步骤2:将异氰酸酯接枝石墨烯加入甲苯中,然后将该混合溶液超声2h,得到分散的异氰酸酯接枝石墨烯悬浮液,接着将占总质量0.5%的功能化石墨烯悬浮液与精制纯化的FCC油浆进行磁力搅拌混合并超声分散,随后通过减压蒸馏的方式除去多余的甲苯溶剂得到混合物。

[0039] 步骤3:将步骤2得到的混合物原料置于高压反应釜内进行直接热缩聚,在N 2 气氛和400r / min的搅拌速率下,将所述混合物以3°C / min的速率从室温升至400℃,然后调控釜内压力至5.0MPa,并在恒压条件下保温10小时,冷却后得到软化点为254°C的前躯体。

[0040] 步骤4:将前躯体研磨后过200目筛,放入可拆卸不锈钢模具中,在N 2Under the protection of gas, foam in a high-pressure reactor, maintain a constant pressure in the kettle to 4MPa, raise the temperature to 360°C at a heating rate of 3°C / min, keep it for 3 hours, and then raise the temperature at a heating rate of 3°C / min to 530°C, heat preservation for 1h, and obtain graphene / foamed carbon raw material after cooling.

[0041] Step 5: Put the graphene / foam carbon raw material into the carbonization furnace, raise the temperature to 800°C at a heating rate of 3°C / min, and keep it warm for 1h; then put it into a high-temperatur...

Embodiment 3

[0044] Step 1: Add graphene oxide to the cyclohexane solution and ultrasonically treat it for 0.5h to obtain a dispersion, then add stearic acid monomer dropwise to the dispersion, reflux at 80°C for 4h, and obtain hard Fatty acid grafted functionalized graphene materials.

[0045] Step 2: Add stearic acid grafted graphene to acetone, then ultrasonicate the mixed solution for 1h to obtain a dispersed stearic acid grafted graphene suspension, and then add the functionalized graphene suspension that accounts for 0.01% of the total mass It is magnetically stirred and mixed with refined and purified FCC oil slurry and dispersed ultrasonically, and then excess acetone solvent is removed by vacuum distillation to obtain a mixture.

[0046] Step 3: the mixture raw material that step 2 obtains is placed in autoclave and carries out direct heat polycondensation, under N 2 Atmosphere and a stirring rate of 300r / min, the mixture was raised from room temperature to 450°C at a rate of 5°C...

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Abstract

The invention belongs to the technical field of carbon matrix composite preparation, and particularly relates to a preparation method of a high performance foam carbon.Functionalized grapheme is addedto refined and purified catalytic cracking (FCC) oilslurry to prepare high dispersion graphene modified FCC oil slurry; a precursor is prepared by heating and quality modifying treatment; the precursor is spontaneously bubbled and pyrolyzed to obtain graphene / foam carbon raw materials under a high temperature and high pressure;and the raw materials are carbonized and graphitized to obtain the graphene enhanced high performance foam carbon.Compared with pure foamed carbon, the graphene reinforced foamed carbon material prepared by the preparation method can increase thermal conductivity by 5%~20% and compression strength by 10%~30%.

Description

technical field [0001] 本发明属于碳基复合材料制备技术领域,具体涉及一种高性能泡沫碳的制备方法。 Background technique [0002] 泡沫碳是一种具有三维网状孔道结构的功能型碳材料,其孔结构主要是由微米级的孔泡和相互连接的韧带结构组成。经过石墨化处理后,固体碳骨架由沿孔壁方向呈网状排列的石墨韧带构成,其孔隙率高达70~80%。这种独特的结构与基体碳的特性,使得泡沫碳具有低密度、高导电性、低热膨胀系数、高强度、高导热系数、低吸水率、耐高温、耐酸碱、抗氧化、无挥发性物质、不产生有毒气体,且具有良好的可加工和可成型性能的优点。因此,作为一种轻质功能结构材料,泡沫碳在航空航天、化工、能源、环境、电子等领域具有很好的发展前景。然而,由中间相沥青作为原料制备的高导热泡沫碳由于在石墨化过程中易产生较多的裂纹,使泡沫碳强度明显降低,热导率比理论热导率低,制约了其大规模的应用,因此有必要对其进行增强处理。 [0003] 目前,对泡沫碳进行掺杂增强的研究大多是直接将增强体与中间相沥青进行混合得到的泡沫碳前驱体,对泡沫碳的力学性能和导热性能改善效果不明显,改善幅度有限。 Contents of the invention [0004] 为了解决石墨烯在泡沫碳中的分散性问题,克服现有泡沫碳力学性能和导热性能不足的缺陷,本发明提出了一种高性能泡沫碳的制备方法。 [0005] 一种高性能泡沫碳的制备方法,包括以下步骤: [0006] (1)向精制纯化的催化裂化(FCC)油浆中加入功能化石墨烯,制得石墨烯改性的FCC油浆; [0007] (2)对步骤(1)的石墨烯改性的FCC油浆,加热改质,制得前驱体; [0008] (3)高温、高压下,步骤(2)的前驱体经过自发泡热解而得到石墨烯 / 泡沫碳生料; [0009] (4)将步骤(3)的生料经碳化、石墨化得到石墨烯增强高性能泡沫碳。 [0010] 所述步骤(1)中功能化石墨烯的制备方法:将氧化石墨烯加入到有机溶液1中超声处理0.5~3h得到分散液,接着加入小分子单体,在气氛条件下于30~80℃下回流反应4~8h,经过抽滤洗涤后得到功能化石墨烯材料。 [0011] 优选地,所述的有机溶剂1为乙醇、异丙醇、丙酮、苯、甲苯、二甲苯、氯仿、...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B32/05C01B32/194
CPCC01B32/05C01B32/194
Inventor 韩飞叶崇刘金水张福全朱圣林
Owner HUNAN UNIV