CN109179376A - 乳胶海绵制备多孔碳纳米材料的方法 - Google Patents
乳胶海绵制备多孔碳纳米材料的方法 Download PDFInfo
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- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 56
- 229910052799 carbon Inorganic materials 0.000 title claims abstract description 54
- 239000002086 nanomaterial Substances 0.000 title claims abstract description 49
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- 238000000034 method Methods 0.000 title claims abstract description 15
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 45
- 235000019441 ethanol Nutrition 0.000 claims abstract description 24
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- 238000001354 calcination Methods 0.000 claims description 9
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 8
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 8
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 4
- 229910052757 nitrogen Inorganic materials 0.000 claims description 4
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- 238000002484 cyclic voltammetry Methods 0.000 description 10
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- 244000043261 Hevea brasiliensis Species 0.000 description 1
- 240000000599 Lentinula edodes Species 0.000 description 1
- HBBGRARXTFLTSG-UHFFFAOYSA-N Lithium ion Chemical compound [Li+] HBBGRARXTFLTSG-UHFFFAOYSA-N 0.000 description 1
- 240000007594 Oryza sativa Species 0.000 description 1
- 235000007164 Oryza sativa Nutrition 0.000 description 1
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Abstract
本发明公开了一种乳胶海绵制备多孔碳纳米材料的方法。所述方法按乳胶海绵、KOH与乙醇的质量比为1:1:1~2:1:2,将乳胶海绵粉末和KOH加入乙醇中,均匀混合后,100~150℃下加热除去乙醇,然后在惰性气体的保护下,将乳胶海绵进行分段煅烧,产物用盐酸洗涤去除杂质,再水和乙醇洗至中性,得到多孔碳纳米材料。本发明以丰富易得的乳胶海绵为原料,降低成本,不仅实现了乳胶海绵废料的回收利用,而且降低了废料对环境的污染,制备的多孔碳纳米材料比表面积高,其作电极材料组装的超级电容器具有较高的比电容,在1mol.L‑1H2SO4中比电容达460F.g‑1。
Description
技术领域
本发明属于能源材料制备技术领域,涉及一种乳胶海绵制备多孔碳纳米材料的方法。
背景技术
乳胶海绵是一种以天然橡胶为主要原料的具有多泡孔结构的海绵制品,具有高弹性,高透气性、绿色环保等特点,广泛应用于座椅、沙发、床垫等家居产品和体育器材。目前乳胶海绵的处理方法都比较粗糙,大多是将其作为填充物处理。如果将海绵废料制备成具有良好电化学性能的多孔碳材料并应用于超级电容器以及锂离子电池中,将会使乳胶海绵废料的价值得到最大化开发利用。
目前多采用生物质材料制备多孔碳纳米材料,例如:Ping Cheng等人将香菇分别用H3PO4以及KOH活化来制备多孔碳纳米材料,该材料在水系以及有机电解质分别表现出优异的电化学性能,分别为306F.g-1和149F.g-1(Cheng Ping,et al.Hierarchically porouscarbon by activation of shiitake mushroom for capacitive en ergystorage.Carbon 93(2015):315-324.);Yuhe Cao等人将玉米秸秆芯用KOH活化之后在管式炉中煅烧制备的多孔碳纳米材料在6mol.L-1的KOH中具有323F.g-1的比电容(Cao,Yuhe,etal."Hierarchical porous activated carbon for supercapacitor derived from cornstalk core by potassium hydroxide activation."Electrochimica Acta 212(2016):839-847.);Lijing Xie等人将柳絮用KOH活化后高温煅烧制备多孔碳纳米材料,制备的多孔碳纳米材料在6mol.L-1的KOH中具有优异的电化学性能为292F.g-1(Xie Lijing,et al."Hierarchical Porous Carbon Microtubes Derived from Willow Catkins forSupercapacitor Application."Journal of Materials Chemistry A 4.5(2015):1637-1646.)。
发明内容
针对乳胶海绵废料回收再利用技术中的不足,本发明提供一种乳胶海绵制备多孔碳纳米材料的方法。该方法利用乳胶海绵废料制备具有高比表面积和较高比电容的多孔碳纳米材料。
本发明的技术方案如下:
乳胶海绵制备多孔碳纳米材料的方法,具体步骤如下:
按乳胶海绵、KOH与乙醇的质量比为1:1:1~2:1:2,将乳胶海绵粉末和KOH加入乙醇中,均匀混合后,100~150℃下加热除去乙醇,然后在惰性气体的保护下,将乳胶海绵进行分段煅烧,第一段煅烧温度为300~500℃,煅烧保温时间为1~3h,第二段煅烧温度为600~900℃,煅烧保温时间为1~3h,煅烧结束后,自然冷却,产物用盐酸洗涤去除杂质,再水和乙醇洗至中性,烘干,得到多孔碳纳米材料。
优选地,所述的乙醇浓度为95%。
优选地,所述的盐酸浓度为10~50%。通过盐酸洗涤去除材料中的杂质。不同浓度的盐酸腐蚀性不同,选择该浓度既可以去除杂质又不破坏制备出材料的性能,从而制备出最佳形貌以及最佳电化学性能的复合材料。
优选地,所述的惰性气体为氮气或氩气,惰性气体保护下能够防止材料制备过程中的氧化,并降低生产成本。
优选地,所述的分段煅烧过程中,升温速率为3~10℃/min。
与现有技术相比,本发明具有以下优点:
(1)以丰富易得的乳胶海绵为原料,降低成本,不仅实现了乳胶海绵废料的回收利用,而且降低了废料对环境的污染;
(2)本发明通过控制乳胶海绵、KOH与乙醇的质量比,以及水和乙醇的去除方式,使KOH与乳胶海绵充分混合,制备具有良好的多孔性和电容性能的多孔碳材料,比电容达460F.g-1,在超级电容器领域具有重要的实用价值和良好的应用前景。
附图说明
图1为实施例1制得的多孔碳纳米材料的扫描电镜图。
图2为实施例1制得的多孔碳纳米材料的循环伏安曲线。
图3为实施例1制得的多孔碳纳米材料的充放电曲线图。
图4为实施例2制得的多孔碳纳米材料的扫描电镜图。
图5为实施例2制得的多孔碳纳米材料的循环伏安曲线。
图6为实施例2制得的多孔碳纳米材料的充放电曲线图。
图7为对比例1制得的多孔碳纳米材料的扫描电镜图。
图8为对比例1制得的多孔碳纳米材料的循环伏安曲线。
图9为对比例1制得的多孔碳纳米材料的充放电曲线图。
图10为对比例2制得的多孔碳纳米材料的扫描电镜图。
图11为对比例2制得的多孔碳纳米材料的循环伏安曲线。
图12为对比例2制得的多孔碳纳米材料的充放电曲线图。
图13为对比例3制得的多孔碳纳米材料的扫描电镜图。
图14为对比例3制得的多孔碳纳米材料的循环伏安曲线。
图15为对比例3制得的多孔碳纳米材料的充放电曲线图。
具体实施方式
下面结合实施例和附图对本发明作进一步详述。
实施例1
将1g乳胶海绵粉末和1g KOH加入1g95%乙醇中,超声混合均匀后,将混合溶液在油浴中以110℃加热,去除水和乙醇,然后在氮气保护下置于管式炉中煅烧,先在300℃煅烧2.0h,再在900℃煅烧0.5h,升温速率为5℃/min;将制得的产物用1mol/L的HCl洗涤去除杂质,用水和乙醇多次离心洗涤,在60℃烘箱中干燥,得到多孔碳纳米材料。
图1为实施例1制得的多孔碳纳米材料的扫描电镜图,从图中可以看出多孔碳纳米片为薄片状多孔结构。图2为实施例1制得的多孔碳纳米材料的循环伏安曲线。图3为实施例1制得的多孔碳纳米材料的充放电曲线图。从曲线可知,多孔碳纳米材料的比电容为460F/g,具有较高的比电容量。
实施例2
将2g乳胶海绵粉末和1g KOH加入2g95%乙醇中,超声混合均匀后,将混合溶液在油浴中以110℃加热,去除水和乙醇,然后在氮气保护下置于管式炉中煅烧,先在300℃煅烧2.0h,再在900℃煅烧0.5h,升温速率为5℃/min;将制得的产物用1mol/L的HCl洗涤去除杂质,用水和乙醇多次离心洗涤,在60℃烘箱中干燥,得到多孔碳纳米材料。
图4为实施例2制得的多孔碳纳米材料的扫描电镜图。图5为实施例2制得的多孔碳纳米材料的循环伏安曲线。图6为实施例2制得的多孔碳纳米材料的充放电曲线图。从曲线中可知所制备材料的比电容为418F/g,具有高的比电容量。
对比例1
本对比例与实施例1基本相同,唯一不同的是不加入KOH,即乳胶海绵、KOH与乙醇水溶液的质量比为1:0:1。
图7为对比例1制得的多孔碳纳米材料的扫描电镜图,从图中可以看出纳米颗粒结构。图8为对比例1制得的多孔碳纳米材料的循环伏安曲线。图9为对比例1制得的多孔碳纳米材料的充放电曲线图。从曲线中可知所制备材料的比电容为32F/g,比电容量较低。
对比例2
本对比例与实施例1基本相同,唯一不同的是乳胶海绵、KOH与乙醇水溶液的质量比为3:1:1。
图10为对比例2制得的多孔碳纳米材料的扫描电镜图。图11为对比例2制得的多孔碳纳米材料的循环伏安曲线。图12为对比例2制得的多孔碳纳米材料的充放电曲线图。从曲线中可知所制备材料的比电容为130F/g。
对比例3
本对比例与实施例1基本相同,唯一不同的是乳胶海绵、KOH与乙醇水溶液混合后,采用冷冻干燥的方式除去水和乙醇。
图13为对比例3制得的多孔碳纳米材料的扫描电镜图。图14为对比例3制得的多孔碳纳米材料的循环伏安曲线。图15为对比例3制得的多孔碳纳米材料的充放电曲线图。从曲线中可知所制备材料的比电容为141F/g,具有较高的比电容量。
Claims (5)
1.乳胶海绵制备多孔碳纳米材料的方法,其特征在于,具体步骤如下:
按乳胶海绵、KOH与乙醇的质量比为1:1:1~2:1:2,将乳胶海绵粉末和KOH加入乙醇中,均匀混合后,100~150℃下加热除去乙醇,然后在惰性气体的保护下,将乳胶海绵进行分段煅烧,第一段煅烧温度为300~500℃,煅烧保温时间为1~3h,第二段煅烧温度为600~900℃,煅烧保温时间为1~3h,煅烧结束后,自然冷却,产物用盐酸洗涤去除杂质,再水和乙醇洗至中性,烘干,得到多孔碳纳米材料。
2.根据权利要求1所述的方法,其特征在于,所述的乙醇浓度为95%。
3.根据权利要求1所述的方法,其特征在于,所述的盐酸浓度为10~50%。
4.根据权利要求1所述的方法,其特征在于,所述的惰性气体为氮气或氩气。
5.根据权利要求1所述的方法,其特征在于,所述的分段煅烧过程中,升温速率为3~10℃/min。
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