CN109317096B - 一种膨胀石墨/多孔六方氮化硼复合材料及其制备方法和作为苯气体吸附剂的应用 - Google Patents
一种膨胀石墨/多孔六方氮化硼复合材料及其制备方法和作为苯气体吸附剂的应用 Download PDFInfo
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Abstract
本发明属于气体吸附材料领域,公开了一种膨胀石墨复合多孔六方氮化硼吸附剂及其制备方法和应用,包括以下步骤:a)依次将三聚氰胺,硼酸和膨胀石墨加入去离子水中,搅拌5min,混合物;b)将所得混合物倒入反应釜中,150℃‑300℃,反应6‑8h,得产物;d)将产物过滤、烘干,得到膨胀石墨和氮化硼前驱体的复合材料,e)将前驱体复合材料在N2氛围中升温至1000‑1200℃碳化1‑2h,得到膨胀石墨/多孔六方氮化硼复合吸附材料。本发明充分利用多孔六方氮化硼的高比表面积和丰富的孔结构,结合膨胀石墨高孔容的的特性,对苯气体具有良好的吸附性。
Description
技术领域
本发明属于新型碳材料领域,具体涉及一种膨胀石墨/多孔六方氮化硼复合材料及其制备方法和作为苯气体吸附剂的应用。
背景技术
随着工业化的不断发展,苯气体的排放量逐年提高。苯气体是存在于许多工业应用中的污染物,即使在非常低的浓度下,它们对人体健康和环境的危害都非常大。
因此需要有效的针对苯气体的去除手段,如吸附,催化氧化,冷凝和膜分离。在多样性技术中,吸附被认为是去除苯的最具成本效益和环境友好的技术之一。目前,市面上使用的吸附材料存在吸附容量有限,且在低浓度下对苯气体吸附性能不佳等缺点。
膨胀石墨是近几十年来发展起来的新型碳质吸附材料,通常由天然鳞片石墨通过顺序插层、洗涤、干燥和膨化来制备,具有微米级的孔结构、较大的吸附容量,通透性良好,非常适合于流动介质的吸附,但其不适合应用于气相吸附研究,需要对其的孔结构进行修饰。
多孔六方氮化硼(p-BN)具有独特的物理和化学性质,包括高比表面积,低密度,高导热性,优异的化学稳定性和抗氧化性,这些特性使p-BN具有广泛的应用前景,尤其是与吸附相关的应用。此外,芳环分子体系中广泛存在一种π-π堆积的非共价相互作用,这种相互作用是范德华作用和静电作用相结合产生的,是分子自组装的主要动力。p-BN是具有芳环的六边型结构,能够和苯的芳环发生面面堆积和边面堆积的π-π相互作用,因此可以达到选择性吸附的目的。制得p-BN的BET比表面积为1018m2/g,平均孔径约为1.41nm,根据吸附理论,该孔径对挥发性有机污染物有极高的吸附能力。
发明内容
有鉴于此,本发明提供了膨胀石墨/多孔六方氮化硼复合吸附材料,该复合材料对苯气体等挥发性有机物有良好的吸附性能,且具有很强的热稳定性,化学稳定性,应用广泛。
本发明是通过以下技术方案实现的:
一种膨胀石墨复合多孔六方氮化硼的吸附剂的制备方法,包括如下步骤:
a.将鳞片石墨氧化、插层,在700℃-900℃温度下加热膨胀,膨化时间10-30s,制成膨胀石墨;
b.将膨胀石墨,三聚氰胺和硼酸按质量比1-5:1:1混合加入100mL去离子水初步搅拌5min,得混合物;
c.将所得混合物倒入反应釜中,在150℃-300℃条件下,反应6-8h;
d.反应后将产物过滤、烘干,得到膨胀石墨和氮化硼前驱体的复合材料;
e.将前驱体复合材料在N2氛围下高温碳化1-2h,得到膨胀石墨/多孔六方氮化硼复合吸附材料。
所述的高温碳化温度为1000℃-1200℃。选择在该温度下煅烧是由于温度较低时产物是菱方氮化硼和六方氮化硼的混合物,随着温度的提高,菱方氮化硼逐渐消失,直到1000℃以上产物为纯六方氮化硼。
本发明与现有技术相比较,具有如下显著的优点:
(1)本发明所制备的膨胀石墨/多孔六方氮化硼复合吸附材料,是利用多孔六方氮化硼具有芳环的六边型结构,能够和苯的芳环发生面面堆积和边面堆积的π-π相互作用,因此可以达到选择性吸附的目的。将高孔容的膨胀石墨的作为骨架支撑p-BN,使多孔六方氮化硼(p-BN)嵌于膨胀石墨孔壁,两者之间产生相互协同作用,可以极大提高对苯气体的吸附量和吸附能力,最终复合材料对苯的吸附量能达到945mg/g;
(2)本发明选用膨胀石墨为多孔六方氮化硼(p-BN)的骨架支撑,是因为制得的膨胀石墨在具有较大比表面积的同时其孔径是以中孔和大孔为主,而其他高孔容的物质(如活性炭,活性氧化铝,沸石等)孔径以微孔为主,与p-BN复合效果较差,不能满足p-BN骨架的要求,所以膨胀石墨和p-BN制备的复合吸附材料对苯气体选择吸附性好,吸附容量高,结构稳定,并制备方法简单,快速,重复性高,具有很好的应用前景。
附图说明
图1为实施例1-3分别制备的EG/p-BN吸附材料的吸脱附等温线图;
图2为实施例1-3制备的EG/p-BN吸附材料的孔径分布图;
图3为EG,p-BN,和实施例一制得的EG/p-BN的XRD衍射谱图;
图4为EG 30k倍下的SEM照片;
图5为EG/p-BN复合材料30k倍下的SEM照片。
具体实施方式
下面给出实施例以对本发明进行具体的描述,但不限于此。
实施例一
a.将鳞片石墨氧化、插层,在900℃温度下加热膨胀,膨化时间30s,制成膨胀石墨;
b.将膨胀石墨,三聚氰胺和硼酸按质量比2:1:1混合加入100mL去离子水初步搅拌5min,得混合物;
c.将所得混合物倒入反应釜中,在180℃条件下,反应6h;
d.反应后将产物过滤、烘干,得到膨胀石墨和氮化硼前驱体的复合材料;
e.将前驱体复合材料于N2氛围下升温至1050℃碳化1h,得到膨胀石墨/多孔六方氮化硼复合吸附材料。
本实例中制备的膨胀石墨/多孔六方氮化硼复合材料作为吸附剂用来吸附苯气体,采用氮气吸脱附测得BET比表面积为1145m2/g,平均孔径为2.15nm,采用静态保干器法测量对苯气体的吸附量,测得吸附量为945mg/g。
实施例二
本实施例与实施例一基本相同,特别之处在于“将膨胀石墨,三聚氰胺和硼酸按质量比1:1:1混合”。具体方案如下:
a.将鳞片石墨氧化、插层,在900℃温度下加热膨胀,膨化时间30s,制成膨胀石墨;
b.将膨胀石墨,三聚氰胺和硼酸按质量比1:1:1混合后加入100mL去离子水初步搅拌5min,得混合物;
c.将所得混合物倒入反应釜中,在180℃条件下,反应6h;
d.将产物过滤、烘干,得到膨胀石墨和氮化硼前驱体的复合材料;
e.将复合材料于N2氛围下升温至1050℃碳化1h,得到膨胀石墨/多孔六方氮化硼复合吸附材料。
本实例中制备的膨胀石墨/多孔六方氮化硼复合材料作为吸附剂用来吸附苯气体,采用氮气吸脱附测得BET比表面积为930m2/g,平均孔径为2.29nm,采用静态保干器法测量对苯气体的吸附量,测得吸附量为762mg/g。
实施例三
本实施例与实施例一基本相同,特别之处在于“将复合材料于N2氛围气氛下升温至750℃碳化1h”。具体方案如下:
a.将鳞片石墨氧化、插层,在900℃温度下加热膨胀,膨化时间30s,制成膨胀石墨;
b.将膨胀石墨,三聚氰胺和硼酸按2:1:1混合加入100mL去离子水初步搅拌5min,得混合物;
c.将所得混合物倒入反应釜中,在180℃条件下,反应6h;
d.将反应产物过滤、烘干,得到膨胀石墨和氮化硼前驱体的复合材料;
e.将复合材料于N2氛围下升温至750℃碳化1h,得到膨胀石墨/多孔六方氮化硼复合吸附材料。
本实例中制备的膨胀石墨/多孔六方氮化硼复合材料作为吸附剂用来吸附苯气体,采用氮气吸脱附测得BET比表面积为823m2/g,平均孔径为2.64nm,采用静态保干器法测量对苯气体的吸附量,测得吸附量为638mg/g。
对比例一
制备膨胀石墨:
将鳞片石墨氧化、插层,在900℃温度下加热膨胀,膨化时间30s,制成膨胀石墨。
将制备的膨胀石墨,采用静态保干器法测量对苯气体的吸附量,测得吸附量为112mg/g
对比例二
制备多孔六方氮化硼:
将三聚氰胺和硼酸按1:1混合加入100mL去离子水;
将混合物倒入反应釜中,180℃,反应6h;
将反应产物过滤、烘干,于N2氛围碳化1h,得到多孔六方氮化硼。
将制备的多孔六方氮化硼,采用静态保干器法测量对苯气体的吸附量,测得吸附量为430mg/g。
对比例三
将膨胀石墨和多孔六方氮化硼按1:1进行物理混合;采用静态保干器法测量对苯气体的吸附量,测得吸附量为354mg/g。
图1为实施例1-3制备的EG/p-BN吸附材料的吸脱附等温线图,具有I型等温线的特征,说明材料微孔分布范围较广,是具有较小外表面的微孔材料,吸附能很快达到饱和;图2为实施例1-3制备的EG/p-BN吸附材料的孔径分布图。可以看出,实施例一制备的EG/p-BN比表面积最大,达到了1145m2/g,各个实施例的孔径集中在2nm以下,说明各个实施例制备的吸附材料均具有良好的孔结构。
图3为EG,p-BN,和实施例一制得的EG/p-BN的XRD衍射谱图。在2θ=26.3°处的特征峰对应(002)平面(六方氮化硼的标准峰)。另一个衍射峰出现在2θ=42.4°,对应六方氮化硼的(100)和(101)面叠加的一个峰。EG/p-BN除了在与EG相同的位置上有明显的衍射峰,同时在26.3°处出现了(002)面的不规则峰,表明EG/p-BN复合材料中同时存在EG和p-BN。
图4为EG 30k倍下的SEM照片,图5为EG复合p-BN 30k倍下的SEM照片。由图可以看出复合后材料结构疏松,有大量的微孔,比表面积大幅提升。
Claims (2)
1.一种膨胀石墨/多孔六方氮化硼复合材料作为苯气体吸附剂的应用,其特征在于:所述复合材料是以膨胀石墨为基体,在膨胀石墨上复合多孔六方氮化硼(p-BN);
所述膨胀石墨/多孔六方氮化硼复合材料的制备方法为:
a.依次将三聚氰胺,硼酸和膨胀石墨加入去离子水中,搅拌,得混合物;所述的三聚氰胺、硼酸、膨胀石墨的质量比为1:1:1-5;
b.将所得混合物倒入反应釜中,在150℃-300℃条件下,反应6-8h;
c.反应后将产物过滤、烘干,得到膨胀石墨和氮化硼前驱体复合材料;
d.将前驱体复合材料在N2氛围下高温碳化1-2h,得到膨胀石墨/多孔六方氮化硼复合吸附材料。
2.根据权利要求1所述膨胀石墨/多孔六方氮化硼复合材料作为苯气体吸附剂的应用,其特征在于:步骤d中所述的高温碳化温度为1000℃-1200℃。
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