CN111153393A - 一种聚苯胺基炭材料及其孔隙结构的调控方法和应用 - Google Patents
一种聚苯胺基炭材料及其孔隙结构的调控方法和应用 Download PDFInfo
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Abstract
本发明公开了一种聚苯胺基炭材料及其孔隙结构的调控方法和应用,属于纳米材料和能源科学技术领域,包括以下步骤:制备聚苯胺基炭前驱体;将聚苯胺基炭前驱体在不同压力条件下进行加压处理,之后进行碳化处理,冷却,制得不同孔隙结构的聚苯胺基炭材料;本发明在给定前驱体和碳化处理条件下,通过简单物理方法实现了给定前驱体炭材料孔隙结构的调控,与传统方法相比,无需借助超高的碳化温度,极大降低工艺能耗,节约成本,所制得的聚苯胺基炭材料用作钠离子电池负极材料,循环性能稳定,在储能等领域拥有广泛的应用前景。
Description
技术领域
本发明属于纳米材料和能源科学技术领域,具体涉及一种聚苯胺基炭材料及其孔隙结构的调控方法和应用。
背景技术
纳米孔炭材料由于具有丰富可调的孔结构、良好的导电性和优异的机械性能等特点,在能源储存、吸附分离、催化等领域有广泛的应用。纳米孔炭材料的孔结构对材料的性能发挥着重要的作用,例如,具有微孔骨架和高比表面积的炭有助于增加双电层电容;而低孔隙/低缺陷炭有利于提高锂/钠离子电池首次库伦效率以及插层容量。炭材料骨架微孔结构与所选择的前驱体以及碳化工艺有很大的关系。例如,利用蔗糖、酚醛树脂、聚苯胺等碳化得到微孔骨架,而利用一些含有大π平面结构的前驱体往往可获得不含微孔或微孔较低的炭材料。研究人员也通过改变碳化温度来改变微孔孔隙,比如提高碳化温度可以降低硬炭的比表面积、孔隙度以及骨架内缺陷。因此,要实现炭材料骨架在微孔和无孔之间的转换,需要使用不同的前驱体或者不同的碳化/活化条件。在给定前驱体和碳化处理条件下,如何调控给定前驱体炭材料的孔隙结构还需要进一步研究。
发明内容
为了克服上述现有技术的缺点,本发明提供一种聚苯胺基炭材料及其孔隙结构的调控方法和应用。
本发明的第一个目的是提供一种聚苯胺基炭材料孔隙结构的调控方法,包括以下步骤:
制备聚苯胺基炭前驱体;将聚苯胺基炭前驱体在不同压力条件下进行加压处理,之后进行碳化处理,冷却,制得不同孔隙结构的聚苯胺基炭材料。
优选地,在压力为0.1-10MPa下进行加压处理。
优选地,所述碳化处理具体为氮气保护下,400-800℃碳化处理3h。
优选地,所述碳化处理的升温速率为2℃/min,氮气流速为80mL/min。
优选地,所述聚苯胺基炭前驱体为聚苯胺或苯胺-吡咯共聚物。
优选地,所述聚苯胺具体是通过以下步骤制得:
将苯胺和过硫酸铵在1mol/L盐酸溶液中混合溶解,静置反应1.5-2.5h后,过滤、洗涤、干燥,制得聚苯胺;所述过硫酸铵:苯胺用量比为0.6-0.65g:1mL,盐酸与苯胺用量比为0.06-0.08mol:1mL。
优选地,所述苯胺-吡咯共聚物具体是通过以下步骤制得:
将苯胺和吡咯依次加至Triton X-100的水溶液中,混合均匀,制得分散液,将过硫酸铵在0-5℃加至分散液中,冰水浴条件下静置反应12h后过滤、洗涤、干燥,制得苯胺-吡咯共聚物;苯胺:吡咯:Triton X-100的用量比为8.1-8.3mL:6.1-6.5mL:1g;Triton X-100:水用量比为0.001g:1mL;过硫酸铵:苯胺用量比为5g:1mL。
本发明的第二个目的是提供由上述调控方法制得的聚苯胺基炭材料。
本发明的第三个目的是提供上述聚苯胺基炭材料在钠离子电池负极材料中的应用。
与现有技术相比,本发明的有益效果在于:
本发明在给定前驱体和碳化处理条件下,通过简单物理方法实现了给定前驱体炭材料孔隙结构的调控,与传统方法相比,无需借助超高的碳化温度(大于1000℃),极大降低工艺能耗,节约成本,所制得的聚苯胺基炭材料用作钠离子电池负极材料,循环性能稳定,在储能等领域拥有广泛的应用前景。
附图说明
图1为实施例1制得的聚苯胺基炭材料的氮气吸附-脱附曲线;
图2为实施例1制得的聚苯胺基炭材料的扫描电镜图;
图3为实施例1制得的聚苯胺基炭材料的透射电镜图;
图4为实施例1制得的聚苯胺基炭材料的钠离子电池循环性能图。
具体实施方式
为了使本领域技术人员更好地理解本发明的技术方案能予以实施,下面结合附图以及具体实施例对本发明作进一步说明,但所举实施例不作为对本发明的限定。
下面各实施例中未注明具体条件的试验方法,均按照本领域的常规方法和条件进行,所用的材料若无特殊说明均为市售。
实施例1
一种聚苯胺基炭材料孔隙结构的调控方法,包括以下步骤:
S1,在250mL中烧杯中加入100mL 1mol/L HCl溶液,加入2.9mL苯胺单体,磁力搅拌均匀,将其命名为A液;在250mL烧杯中加入100mL 1mol/L HCl溶液,加入1.82g过硫酸铵,磁力搅拌均匀,将其命名为B液;将B液迅速倒入A液中磁力搅拌,混合均匀后停止搅拌;停止搅拌后,翡翠绿的聚苯胺会迅速出现,静置2h反应;结束后,使用减压抽滤洗涤至滤液接近无色,于60℃烘箱中干燥12h,得到苯胺共轭高分子纳米线;
S2,将干燥后的苯胺共轭高分子纳米线取60mg加入直径为8mm的圆形不锈钢模具中,然后用压力机进行机械压力处理,在2MPa下加压1min,将加压后线性聚苯胺共轭高分子片取出,放入氧化铝坩埚中,在流速为80mL/min的氮气气氛下进行碳化处理,升温条件为2℃/min升温至800℃,保温3h,炉内自然冷却到室温,得到聚苯胺基炭材料。
实施例2
一种聚苯胺基炭材料孔隙结构的调控方法,包括以下步骤:
S1,在100mL烧瓶中加入60mL超纯水和0.06g Triton X-100,然后依次加入0.49mL苯胺单体和0.38mL吡咯单体,室温下电磁力搅拌30min,室温下超声30min,再置入预先冷却到0℃低温恒温反应浴30min;将预先冷却至5℃的过硫酸铵水溶液(其中,将2.465g过硫酸铵溶解于5mL超纯水中)加入反应瓶中磁力搅拌,混合均匀后停止搅拌,置于0℃冰水浴中反应12h,反应结束后,使用超纯水减压抽滤至滤液无色后真空干燥12h,制备得到苯胺-吡咯共轭高分子纳米球;
S2,将干燥后的苯胺-吡咯共轭高分子纳米球取60mg加入直径为8mm的圆形不锈钢模具中,然后用压力机进行机械压力处理,在2MPa下加压1min,在流速为80mL/min的氮气气氛下进行碳化处理,升温条件为2℃/min升温至800℃,保温3h,炉内自然冷却到室温,得到聚苯胺基炭材料。
实施例3
一种聚苯胺基炭材料孔隙结构的调控方法,包括以下步骤:
S1,按照实施例1中的步骤S1制得苯胺共轭高分子纳米线;
S2,将干燥后的苯胺共轭高分子纳米线取60mg加入直径为8mm的圆形不锈钢模具中,然后用压力机进行机械压力处理,在2MPa下加压1min。在流速为80mL/min的氮气气氛下进行碳化处理,升温条件为2℃/min升温至400℃,保温3h,炉内自然冷却到室温,得到聚苯胺基炭材料。
实施例4
一种聚苯胺基炭材料孔隙结构的调控方法,包括以下步骤:
S1,按照实施例1中的步骤S1制得苯胺共轭高分子纳米线;
S2,将干燥后的苯胺共轭高分子纳米线取60mg加入直径为8mm的圆形不锈钢模具中,然后用压力机进行机械压力处理,在2MPa下加压1min,在流速为80mL/min的氮气气氛下进行碳化处理,升温条件为2℃/min升温至600℃,保温3h,炉内自然冷却到室温,得到聚苯胺基炭材料。
实施例5
一种聚苯胺基炭材料孔隙结构的调控方法,包括以下步骤:
S1,按照实施例1中的步骤S1制得苯胺共轭高分子纳米线;
S2,将干燥后的苯胺共轭高分子纳米线取60mg加入直径为8mm的圆形不锈钢模具中,然后用压力机进行机械压力处理,在5MPa下加压1min,在流速为80mL/min的氮气气氛下进行碳化处理,升温条件为2℃/min升温至800℃,保温3h,炉内自然冷却到室温,得到聚苯胺基炭材料。
实施例6
一种聚苯胺基炭材料孔隙结构的调控方法,包括以下步骤:
S1,按照实施例1中的步骤S1制得苯胺共轭高分子纳米线;
S2,将干燥后的苯胺共轭高分子纳米线取60mg加入直径为8mm的圆形不锈钢模具中,然后用压力机进行机械压力处理,在10MPa下加压1min,在流速为80mL/min的氮气气氛下进行碳化处理,升温条件为2℃/min升温至800℃,保温3h,炉内自然冷却到室温,得到聚苯胺基炭材料。
实施例7
一种聚苯胺基炭材料孔隙结构的调控方法,包括以下步骤:
S1,按照实施例1中的步骤S1制得苯胺共轭高分子纳米线;
S2,将干燥后的苯胺共轭高分子纳米线取60mg加入直径为8mm的圆形不锈钢模具中,然后不使用压力机处理直接在流速为80mL/min的氮气气氛下进行碳化处理,升温条件为2℃/min升温至800℃,保温3h,炉内自然冷却到室温,得到聚苯胺基炭材料。
下面对实施例1-7不同条件下制得的聚苯胺基炭材料进行检测,其比表面积结果如表1所示:
表1不同条件制得的聚苯胺基炭材料比表面积
各实施例比表面积结果如表1所示,由表1可得,实施例7在碳化处理之前没有采用加压处理,其比表面积最大,而采用加压处理之后,可改变炭材料的孔隙结构。通过氮气吸附-脱附仪测得实施例1聚苯胺基炭材料的比表面积,如图1所示,聚苯胺基炭材料的孔结构可由氮气吸附-脱附仪测得,在各压力区间均几乎无氮气吸附,其比表面积为40m2/g,这说明加压处理后,可改变炭材料孔隙;图2为实施例1中制备的聚苯胺基炭材料微观形貌的扫描电镜图,可见呈现出紧密纠缠的纳米纤维形貌;图3为实施例1中制备的聚苯胺基炭材料TEM图,显示其石墨微晶由3-4层叠层的石墨片堆叠形成。
以实施例1制得的聚苯胺基炭材料为例,将其作为钠离子电池负极材料,图4为在20mA/g电流密度下的循环性能图,如图4所示,其在循环130圈后容量仍稳定在217mAh/g,展现出良好的电化学性能。
显然,本领域的技术人员可以对本发明进行各种改动和变型而不脱离本发明的精神和范围。这样,倘若本发明的这些修改和变型属于本发明权利要求及其等同技术的范围之内也意图包含这些改动和变型在内。
Claims (9)
1.一种聚苯胺基炭材料孔隙结构的调控方法,其特征在于,包括以下步骤:
制备聚苯胺基炭前驱体;将聚苯胺基炭前驱体在不同压力条件下进行加压处理,之后进行碳化处理,冷却,制得不同孔隙结构的聚苯胺基炭材料。
2.根据权利要求1所述的聚苯胺基炭材料孔隙结构的调控方法,其特征在于,在压力为0.1-10MPa下进行加压处理。
3.根据权利要求1所述的聚苯胺基炭材料孔隙结构的调控方法,其特征在于,所述碳化处理具体为氮气保护下,400-800℃碳化处理3h。
4.根据权利要求3所述的聚苯胺基炭材料孔隙结构的调控方法,其特征在于,所述碳化处理的升温速率为2℃/min,氮气流速为80mL/min。
5.根据权利要求1所述的聚苯胺基炭材料孔隙结构的调控方法,其特征在于,所述聚苯胺基炭前驱体为聚苯胺或苯胺-吡咯共聚物。
6.根据权利要求5所述的聚苯胺基炭材料孔隙结构的调控方法,其特征在于,所述聚苯胺具体是通过以下步骤制得:
将苯胺和过硫酸铵在1mol/L盐酸溶液中混合溶解,静置反应1.5-2.5h后,过滤、洗涤、干燥,制得聚苯胺;所述过硫酸铵:苯胺用量比为0.6-0.65g:1mL,盐酸与苯胺用量比为0.06-0.08mol:1mL。
7.根据权利要求5所述的聚苯胺基炭材料孔隙结构的调控方法,其特征在于,所述苯胺-吡咯共聚物具体是通过以下步骤制得:
将苯胺和吡咯依次加至Triton X-100的水溶液中,混合均匀,制得分散液,将过硫酸铵在0-5℃加至分散液中,冰水浴条件下静置反应12h后过滤、洗涤、干燥,制得苯胺-吡咯共聚物;苯胺:吡咯:Triton X-100的用量比为8.1-8.3mL:6.1-6.5mL:1g;Triton X-100:水用量比为0.001g:1mL;过硫酸铵:苯胺用量比为5g:1mL。
8.根据权利要求1-7任一项调控方法制得的聚苯胺基炭材料。
9.根据权利要求8所述的聚苯胺基炭材料在钠离子电池负极材料中的应用。
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