CN116408045A - 一种基于氧化石墨烯和多孔植物粉末的多孔复合材料及其制备方法和应用 - Google Patents
一种基于氧化石墨烯和多孔植物粉末的多孔复合材料及其制备方法和应用 Download PDFInfo
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Abstract
本发明涉及一种基于氧化石墨烯和多孔植物粉末的多孔复合材料及其制备方法和应用。所述基于氧化石墨烯和多孔植物粉末的多孔复合材料的制备方法包括:(1)选用多孔天然轻木木屑粉末置于含有腺嘌呤的过氧化氢/磷酸混合溶液中浸泡处理,再经清洗和干燥,得到纤维素;(2)将氧化石墨烯水溶液和纤维素混合,通过预冻和真空冷冻干燥,得到复合气凝胶;(3)将所得复合气凝胶进行高温碳化,得到基于氧化石墨烯和多孔植物粉末的多孔复合材料。
Description
技术领域
本发明涉及一种基于氧化石墨烯和多孔植物粉末的多孔复合材料及其制备方法和应用,属于复合材料及其制备技术领域。
背景技术
石墨烯具有优异的力学特性,被认为是一种未来革命性的材料。因此,石墨烯复合材料能够兼备各方面的优点,具有研究开发潜力。石墨烯是具有较大比表面积的多孔结构碳材料,可通过调控组装形成不同的空间构型,使其在多种领域中得到应用。以石墨烯为基础的复合材料对吸附有害物质能力很强。然而,石墨烯基多孔材料的韧性往往不足以承受挤压过程中的大压缩变形和坍塌和断裂,因此,在保证吸附容量的前提下提高材料的压缩性能对于吸附材料的应用和发展非常重要。
纤维素是广泛存在于自然界中的天然高分子材料。纤维素气凝胶具备环保可再生优点,以及多孔结构特性。由于其优异的生物相容性和降解性,在多种领域极为有用。虽然应用发展前景广阔,但简单的纤维素气凝胶无法充分发挥其独特的性能。
发明内容
针对上述问题,本发明的目的在于提供一种基于氧化石墨烯和多孔植物粉末的多孔复合材料及其制备方法和应用。
第一方面,本发明提供了一种基于氧化石墨烯和多孔植物粉末的多孔复合材料的制备方法,包括:
(1)选用多孔天然轻木木屑粉末置于含有腺嘌呤的过氧化氢/磷酸混合溶液中浸泡处理,再经清洗和干燥,得到纤维素;
(2)将氧化石墨烯水溶液和纤维素混合,通过预冻和真空冷冻干燥,得到复合气凝胶;
(3)将所得复合气凝胶进行高温碳化,得到基于氧化石墨烯和多孔植物粉末的多孔复合材料。
在本发明中,选用天然轻木木屑粉末,经处理得到纤维素后与氧化石墨烯均匀混合,在液氮预冷以及冷冻干燥获得混合气凝胶,再使其高温碳化得到氧化石墨烯/木屑的多孔复合材料。该方法制备的多孔复合材料具有很低的密度,较好的压缩性能和自回复性,同时具有一定的亲疏水性,可用于吸收烟气中的有害物质。此方法操作简单,重现性好,具有广阔的应用前景。具体地,本发明通过将多孔天然木屑粉末加入至该含有腺嘌呤的过氧化氢/磷酸混合溶液中,目的是引入P与N元素,生成双杂原子多孔复合材料。其中H2O2是为了分解木屑制备纤维素,腺嘌呤提供N元素,磷酸提供P元素。而且,发明选择氧化石墨烯进行复合,由于羟基、羧基和碳氧官能团附着在氧化石墨烯表面,使之具有良好的亲水性,会对共辄分子、碱基、叶啾和座酮分子等具有很好的选择性作用。
较佳的,所述多孔天然轻木木屑粉末的粒径≤6mm;将纵向厚度≤3mm的多孔天然轻木切片进行打碎处理,得到多孔天然轻木木屑粉末;所述多孔天然轻木木屑粉末的材质为轻木、乔木、桐木和楸木中的至少一种。
较佳的,含有腺嘌呤的过氧化氢/磷酸混合溶液包括:浓度为30wt%的过氧化氢溶液50~150mL、浓度≥85.0wt%的磷酸溶液50~150mL、腺嘌呤15g~25g,三者混合得到。
较佳的,所述浸泡处理的温度为60~100℃,浸泡时间为6~10小时。
较佳的,所述清洗为在去离子水中浸泡数次以去除溶解的化学物质。
较佳的,所述干燥的温度为60~120℃,时间为6~12小时。
较佳的,所述纤维素和氧化石墨烯的质量比为10:(1~6)。
较佳的,所述预冻为将所述混合液冷冻结晶至固态;优选地,所述预冻的温度≤-10℃,预冻的时间≥3小时。
较佳的,所述真空冷冻干燥的温度为-60~-80℃,时间为6~10小时,真空度为1~10Pa
较佳的,所述高温碳化为:先升温至400~600℃保温1~3后,再升温至800~1000℃并保温1~3小时;所述高温碳化的气氛为惰性气氛。
第二方面,本发明提供了一种根据上述制备方法制备得到的基于氧化石墨烯和多孔植物粉末的多孔复合材料,所述基于氧化石墨烯和多孔植物粉末的多孔复合材料由排列整齐的细孔道壁组成,相邻孔道之间的间隙是具有连续导向的多通道结构。
优选地,所述基于氧化石墨烯和多孔植物粉末的多孔复合材料的平均孔径为300nm~700nm;
优选地,所述基于氧化石墨烯和多孔植物粉末的多孔复合材料的比表面积为60~550m2/g,更优选为400~450m2 g-1;
优选地,所述基于氧化石墨烯和多孔植物粉末的多孔复合材料能压缩至20~80%体积后回弹至原状;
优选地,所述基于氧化石墨烯和多孔植物粉末的多孔复合材料的亲水角为0~40°。
第三方面,本发明提供了一种基于氧化石墨烯和多孔植物粉末的多孔复合材料在烟草过滤嘴中的应用。
有益效果:
本发明中,基于氧化石墨烯和多孔植物粉末的多孔复合材料具有很低的密度,较好的压缩性能和自回复性,同时具有一定的亲疏水性,可用于吸收烟气中的有害物质。此方法操作简单,重现性好,具有广阔的应用前景。
附图说明
图1为实施例2制备的基于氧化石墨烯和多孔植物粉末的多孔复合材料的SEM图,从图中可知经改性后的复合材料呈现呈管腔状结构;
图2为实施例2制备的基于氧化石墨烯和多孔植物粉末的多孔复合材料的XRD图,从图中可知,复合材料没有其他杂质峰。
具体实施方式
以下通过下述实施方式进一步说明本发明,应理解,下述实施方式仅用于说明本发明,而非限制本发明。
在本发明中,基于氧化石墨烯和多孔天然植物粉末的多孔复合材料,是由排列整齐的细孔道壁组成,相邻孔道之间的间隙是具有连续导向的多通道结构。所得氧化石墨烯/植物粉末复合材料具有亲疏水多孔结构,可用于烟草过滤嘴,吸收烟气中有害物质。
本发明中基于氧化石墨烯和多孔天然植物粉末的多孔复合材料的原料就地取材,制备工业流程简单,符合环境友好型的设计理念。
以下示例性地说明基于氧化石墨烯和多孔天然植物粉末的多孔复合材料的制备方法。
通过浸泡处理天然多孔轻木木屑粉末,获得纤维素。其中,浸泡所用混合溶液为含有腺嘌呤(C5H5N5,99%)的氧化氢(H2O2,30%)和磷酸(H3PO4,≥85.0%)混合溶液。该浸泡所用混合溶液中过氧化氢用量50~150mL、磷酸溶液用量50~150mL及腺嘌呤15~25g。所述浸泡可为在60~100℃下保持6~10h。优选,在浸泡处理后,在去离子水中浸泡数次(例如3-5次)以去除溶解的化学物质。
在可选的实施方式中,将沿纵向典型厚度为2-6mm(优选3mm)的多孔天然轻木木屑,进行打碎处理形成天然多孔轻木木屑粉末。
将氧化石墨烯水溶液(例如,1-6mg/mL)与纤维素均匀混合后,经预冻、真空干燥,得到氧化石墨烯和纤维素复合气凝胶。或者,将氧化石墨烯水溶液与纤维素水溶液混合均匀,液氮预冻、冷冻干燥,获得氧化石墨烯和纤维素复合气凝胶。其中,预冻为将所述混合液冷冻结晶至固态;优选地,所述预冻温度≤-10℃,预冻时间≥3h(例如,液氮预冻不低于3h)。真空冷冻干燥的温度为-50至-80℃,时间为6-12小时,真空度可为1~10Pa。优选,真空冷冻干燥的温度可为-60至-80℃,时间可为6-10小时,真空度可为1~3Pa
将氧化石墨烯和纤维素复合气凝胶,通过高温碳化,获得多孔复合材料。作为高温碳化的示例,在惰性气氛(例如,氮气、氩气或氦气等)下以1-5℃/min(例如3℃/min)的加热速率加热至400-600℃并保温1-3h,然后将样品以1-10℃/min(例如5℃/min)加热至800-1000℃保温1-3h,完成高温碳化。
本发明中,采用BET测试所得基于氧化石墨烯和多孔植物粉末的多孔复合材料的平均孔径为300nm~700nm。采用BET测试所得基于氧化石墨烯和多孔植物粉末的多孔复合材料的比表面积为60~550m2/g;基于氧化石墨烯和多孔植物粉末的多孔复合材料的能压缩20~80%体积后回弹至原体积,具有较好的压缩性能和自回复性。采用BET测试亲水性测试仪所得基于氧化石墨烯和多孔植物粉末的多孔复合材料的亲疏水性。
本发明中,基于氧化石墨烯和多孔植物粉末的多孔复合材料具有亲疏水性,可用于烟草过滤嘴,吸收烟气中有害物质。
下面进一步例举实施例以详细说明本发明。同样应理解,以下实施例只用于对本发明进行进一步说明,不能理解为对本发明保护范围的限制,本领域的技术人员根据本发明的上述内容作出的一些非本质的改进和调整均属于本发明的保护范围。下述示例具体的工艺参数等也仅是合适范围中的一个示例,即本领域技术人员可以通过本文的说明做合适的范围内选择,而并非要限定于下文示例的具体数值。
实施例1
将沿纵向典型厚度为2mm的天然轻木切片,打碎成粉末,得到木屑粉末;
将木屑粉末浸泡在80mL过氧化氢(H2O2、30%)、80mL磷酸溶液(H3PO4、≥85.0%)以及15g腺嘌呤(C5H5N5、99%)的混合溶液中,在60℃下浸泡6h。然后在去离子水中浸泡3次以去除溶解的化学物质,包括多余的H3PO4和腺嘌呤,得到纤维素;
将氧化石墨烯水溶液(1mg/m)与纤维素均匀混合后,在液氮预冷后,冷冻干燥(-50℃、2Pa、6h),得到改性后的混合气凝胶;其中,氧化石墨烯与纤维素的质量比为1:10;将复合气凝胶,以3℃/min的加热速率加热至400℃保温1h,然后将样品以5℃/min加热至800℃保温1h进行碳化,获得基于氧化石墨烯和植物粉末的多孔复合材料。
实施例2
将沿纵向典型厚度为3mm的天然轻木切片,打碎成粉末,得到木屑粉末;
将木屑粉末浸泡在100mL过氧化氢(H2O2、30%)、100mL磷酸溶液(H3PO4、≥85.0%)以及20g腺嘌呤(C5H5N5、99%)的混合溶液中,在80℃下浸泡8h;然后在去离子水中浸泡4次以去除溶解的化学物质,包括多余的H3PO4和腺嘌呤,得到纤维素;
将氧化石墨烯水溶液(2mg/mL)与纤维素均匀混合后,在液氮预冷后,冷冻干燥(-60℃、2Pa、8h),得到改性后的复合气凝胶。其中,氧化石墨烯与纤维素的质量比为2:10;
将复合气凝胶,以3℃/min的加热速率加热至500℃保温2h,然后将样品以5℃/min加热至900℃保温2h进行碳化,获得基于氧化石墨烯和植物粉末的多孔复合材料。
实施例3
将沿纵向典型厚度为4mm的天然轻木切片,打碎成粉末,得到木屑粉末;
将木屑粉末浸泡在120mL过氧化氢(H2O2、30%)、120mL磷酸溶液(H3PO4、≥85.0%)以及30g腺嘌呤(C5H5N5、99%)混合溶液中,在100℃下浸泡10h。然后在去离子水中浸泡5次以去除溶解的化学物质,包括多余的H3PO4和腺嘌呤,得到纤维素;
将氧化石墨烯水溶液(3mg/mL)与纤维素均匀混合后,在液氮预冷后,冷冻干燥(-70℃、2Pa、10h),得到改性后的复合气凝胶。其中,氧化石墨烯与纤维素的质量比为3:10;
将复合气凝胶,以3℃/min的加热速率加热至600℃保温3h,然后将样品以5℃/min加热至1000℃保温3h进行碳化,获得基于氧化石墨烯和植物粉末的多孔复合材料。
实施例4
本实施例4中基于氧化石墨烯和植物粉末的多孔复合材料的制备过程参照实施例1,区别在于:氧化石墨烯与纤维素的质量比为4:10。
实施例5
本实施例5中基于氧化石墨烯和植物粉末的多孔复合材料的制备过程参照实施例1,区别在于:氧化石墨烯与纤维素的质量比为5:10。
实施例6
本实施例6中基于氧化石墨烯和植物粉末的多孔复合材料的制备过程参照实施例1,区别在于:氧化石墨烯与纤维素的质量比为6:10。
对比例1
本对比例1中基于氧化石墨烯和植物粉末的多孔复合材料的制备过程参照实施例1,区别在于:不加入氧化石墨烯。
表1为制备的多孔复合材料的性能
尽管已经示出和描述了本发明的实施例,对于本领域的普通技术人员而言,可以理解在不脱离本发明的原理和精神的情况下可以对这些实例进行多种变化、修改、替换和变型,本发明的范围由所附权利要求及其等同物限定。
Claims (10)
1.一种基于氧化石墨烯和多孔植物粉末的多孔复合材料的制备方法,其特征在于,包括:
(1)选用多孔天然轻木木屑粉末置于含有腺嘌呤的过氧化氢/磷酸混合溶液中浸泡处理,再经清洗和干燥,得到纤维素;
(2)将氧化石墨烯水溶液和纤维素混合,通过预冻和真空冷冻干燥,得到复合气凝胶;
(3)将所得复合气凝胶进行高温碳化,得到基于氧化石墨烯和多孔植物粉末的多孔复合材料。
2.根据权利要求1所述的制备方法,其特征在于,所述多孔天然轻木木屑粉末的粒径≤6mm;将纵向厚度≤3mm的多孔天然轻木切片进行打碎处理,得到多孔天然轻木木屑粉末;所述多孔天然轻木木屑粉末的材质为轻木、乔木、楸木和桐木中的至少一种。
3.根据权利要求1所述的制备方法,其特征在于,含有腺嘌呤的过氧化氢/磷酸混合溶液包括:浓度为30wt%的过氧化氢溶液50~150mL、浓度≥85.0wt%的磷酸溶液50~150mL、腺嘌呤15g~25g,三者混合得到。
4.根据权利要求1所述的制备方法,其特征在于,所述浸泡处理的温度为60~100 ℃,浸泡时间为6~10 小时;所述清洗为在去离子水中浸泡数次以去除溶解的化学物质;所述干燥的温度为60~120℃,时间为6~12小时。
5.根据权利要求1所述的制备方法,其特征在于,所述纤维素和氧化石墨烯的质量比为10:(1~6)。
6.根据权利要求1所述的制备方法,其特征在于,所述预冻为将所述混合液冷冻结晶至固态;优选地,所述预冻的温度≤-10℃,预冻的时间≥3小时。
7.根据权利要求1所述的制备方法,其特征在于,所述真空冷冻干燥的温度为-60~-80℃,时间为6~10小时,真空度为1~10Pa。
8.根据权利要求1-7中任一项所述的制备方法,其特征在于,所述高温碳化为:先升温至400~600℃保温1~3后,再升温至800~1000℃并保温1~3小时;所述高温碳化的气氛为惰性气氛。
9.一种根据权利要求1-8中任一项所述的制备方法制备得到的基于氧化石墨烯和多孔植物粉末的多孔复合材料,其特征在于,所述基于氧化石墨烯和多孔植物粉末的多孔复合材料由排列整齐的细孔道壁组成,相邻孔道之间的间隙是具有连续导向的多通道结构;
优选地,所述基于氧化石墨烯和多孔植物粉末的多孔复合材料的平均孔径为300 nm~700 nmμm;
优选地,所述基于氧化石墨烯和多孔植物粉末的多孔复合材料的比表面积为60~550m2/g;更优选地,所述基于氧化石墨烯和多孔植物粉末的多孔复合材料的比表面积为400~450 m2 g-1;
优选地,所述基于氧化石墨烯和多孔植物粉末的多孔复合材料能压缩至20~80%体积后回弹至原状;
优选地,所述基于氧化石墨烯和多孔植物粉末的多孔复合材料的亲水角为0~40°。
10.一种权利要求9所述的基于氧化石墨烯和多孔植物粉末的多孔复合材料在烟草过滤嘴中的应用。
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