CN102225330B - 光催化法制备光催化剂/石墨烯一维核壳复合结构的方法 - Google Patents
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Abstract
光催化法制备光催化剂/石墨烯一维核壳复合结构的方法。将氧化石墨烯分散在溶剂中,配制氧化石墨烯胶体;将一维结构的光催化剂分散在溶剂中,配置光催化剂悬浮液;将上述溶液混合搅拌,置于开口容器中光照;反应结束后,在将产物离心分离,干燥。制备出的光催化剂/石墨烯产物具有新颖的纳米核壳结构和新颖的物理化学性质;反应体系未添加任何有机物作为表面活性剂,产物纯净,无需复杂的分离、提纯过程;可以在可见光、紫外光照条件下进行反应,因此可以利用自然光进行生产;制备方法中无任何有毒有害试剂,对环境友好,无污染;方法快速便捷、简单易学,重现性好,并且制造成本低,工艺简单,效率高。
Description
技术领域
本发明属于光催化剂/石墨烯复合纳米材料技术领域,尤其涉及一种制备光催化剂/石墨烯一维核壳复合结构的制备方法。
背景技术
现有技术:石墨烯(GE)是一种由碳原子以sp2杂化轨道组成六角型呈蜂巢晶格的二维平面材料,其基本重复结构单元为有机材料中最稳定的苯六元环,单层石墨烯理论比表面积高达2630 m2/g。最常用的制备方法是化学还原法。但是由氧化石墨烯还原为石墨烯的过程中,碳原子由sp3杂化转变为sp2杂化,导致石墨烯发生不可逆团聚,产物比表面积下降至仅有1 m2/g([1] 柏嵩,沈小平. 石墨烯基无机纳米复合材料. 化学进展 2010, 22, 2010-2118; [2] 徐超,陈胜,汪信. 基于石墨烯的材料化学进展. 应用化学 2011, 28, 1-9.)。
将无机材料(如金属和半导体纳米粒子)分散到石墨烯中制备石墨烯/无机纳米复合材料,由于无机纳米粒子的存在,可以大大减少石墨烯片层之间的相互作用,一定程度上防止石墨烯的团聚。因此,采用无机纳米粒子修饰石墨烯片是一种有效阻止石墨烯团聚的方法。目前,人们已经制备的石墨烯/无机氧化物(GE/TiO2、GE/Li4Ti5O12、GE/SnO2、GE/Co3O4、GE/ZnO、GE/Fe3O4、GE/Al2O3、GE/LiFePO4等)、石墨烯/金属(GE/Ag、GE/Au、GE/Pt、GE/Pd、GE/Co等)、石墨烯/高分子(GE/聚苯乙烯、GE/聚乙酸乙烯酯)的复合纳米颗粒。在已报道的文献、专利中,金属、金属氧化物均为三维的纳米颗粒([1] 柏嵩,沈小平. 石墨烯基无机纳米复合材料. 化学进展 2010, 22, 2010-2118)。
发明内容
技术问题:本发明提供一种光催化法制备光催化剂/石墨烯一维核壳复合结构的方法,利用一维光催化剂光催化特性,将氧化石墨烯还原为石墨烯,生成新颖的具有核壳结构的光催化剂/石墨烯一维核壳复合纳米材料。
技术方案:光催化法制备光催化剂/石墨烯一维核壳复合结构的方法,制备步骤为:将氧化石墨烯分散在溶剂中,配制浓度为0.01-10 mg/mL的氧化石墨烯胶体;将一维结构的光催化剂分散在溶剂中,配置浓度为0.01-1000 mg/mL的光催化剂悬浮液;将上述溶液按质量比100:1-1:100混合搅拌,置于开口容器中光照0.5-1000 h;反应结束后,在将产物离心分离,干燥。
所述氧化石墨烯分散溶剂为水或者乙醇。
所述一维结构为纳米纤维、纳米管或纳米棒。
所述光催化剂为TiO2、ZnO、ZrO2、SnO2、N掺杂TiO2、S掺杂TiO2、N和S共掺杂TiO2或N掺杂ZnO。
所述光催化剂分散溶剂为水或者乙醇。
所述光照为可见光照或者紫外光照。
所述搅拌速度为不超过800 rpm/min。
所述离心速度为500-13000 rpm/min,离心时间为1-60 min。
在光照条件下,氧化石墨烯被光催化剂还原为石墨烯,在还原反应发生过程中,光催化剂的位阻效应可以有效防止石墨烯的团聚,并且二维的片状氧化石墨烯发生卷曲包裹在一维的光催化剂表面,形成新颖的光催化剂/石墨烯核壳结构。
有益效果:
利用光催化还原法制备一维半导体/石墨烯复合纳米纤维,方法简便;采用光催化反应法还原氧化石墨烯,可以克服氧化石墨烯在还原过程中出现不可逆团聚的现象,产物具有良好的分散性。制备出的光催化剂/石墨烯产物是一种新的复合材料,具有新颖的纳米核壳结构和新颖的物理化学性质;反应体系未添加任何有机物作为表面活性剂,产物纯净,无需复杂的分离、提纯过程;以水或乙醇作为反应溶剂,来源广泛、价格低廉;可以在可见光、紫外光照条件下进行反应,因此可以利用自然光进行生产;制作过程在常温常压下进行,无烧结工艺,节约生产能耗;制备方法中无任何有毒有害试剂,对环境友好,无污染;方法快速便捷、简单易学,重现性好,并且制造成本低,工艺简单,效率高。
附图说明
图1为光催化制备半导体/石墨烯核壳复合一维结构的设备。1、光源;2、容器;3、反应溶液;4、磁子;5、磁力搅拌器;6、载物台。
图2为二氧化钛/石墨烯核壳复合纳米纤维透射电镜(TEM)照片。
图3为二氧化钛/石墨烯核壳复合纳米纤维高分辨率透射电镜(HRTEM)照片。
具体实施方式
实施例1:
a、将氧化石墨分散在乙醇中,浓度为1 mg/mL。
b、将TiO2纳米纤维分散在水中,浓度为2 mg/mL。
c、将上述溶液按照氧化石墨烯/TiO2纳米纤维质量比为1:4进行混合,置于烧杯中,进行磁力搅拌,转速为50 rpm/min,用紫外灯照射21 h。
d、反应结束后,在8000 rpm/min转速下离心3 min,将产物分离出来,室温干燥。
反应产物见图2、3。
实施例2:
a、将氧化石墨烯分散在去离子水中,浓度为2 mg/mL。
b、将TiO2纳米管分散在乙醇中,配置浓度为0.01 mg/mL。
c、上述溶液按照氧化石墨烯/TiO2纳米管质量比为10:1进行混合,置于烧杯中,磁力搅拌,转速为500 rpm/min,用紫外灯照射4 h。
d、反应结束后,在将复合纤维在13000 rpm/min转速下进行离心1 min,将产物分离出来,室温干燥。
实施例3:
a、将氧化石墨烯分散在去离子水中,浓度为0.05 mg/mL。
b、将ZnO纳米纤维分散在去离子水中,浓度为100 mg/mL。
c、将上述溶液混合,氧化石墨烯/ZnO纳米纤维质量比为100:1,置于烧杯中,磁力搅拌,转速为100 rpm/min,用紫外灯照射1000 h。
d、反应结束后,在将复合纤维在15000 rpm/min转速下进行离心1 min,将产物分离出来,室温干燥。
实施例4:
a、将氧化石墨烯分散在去离子水中,配置浓度为10 mg/mL。
b、将ZnO纳米棒分散在乙醇中,配置浓度为100 mg/mL。
c、将上述溶液混合,氧化石墨烯/ZnO纳米棒质量比为20:1,置于烧杯中,磁力搅拌,转速为800 rpm/min,用紫外灯照射4 h。
d、反应结束后,在将复合纤维在15000 rpm/min转速下进行离心1 min,将产物分离出来,室温干燥。
实施例5:
a、将氧化石墨烯分散在蒸馏水中,配置浓度为5 mg/mL。
b、将ZrO2纳米纤维分散在乙醇中,配置浓度为0.1 mg/mL。
c、将上述溶液混合,氧化石墨烯/ZrO2纳米纤维质量比为1:100,置于烧杯中,转速为300 rpm/min,在紫外光下连续照射0.5 h。
d、反应结束后,将复合纤维在1000 rpm/min转速下离心5 min,将产物分离出来,室温真空干燥。
实施例6:
a、以氧化石墨烯作为碳源,超声分散在蒸馏水中,配置浓度为1 mg/mL。
b、将SnO2纳米纤维分散在水中,配置浓度为10 mg/mL。
c、将上述溶液混合,其中氧化石墨烯/SnO2纳米纤维质量比为2:1,置于烧杯中,磁力搅拌,转速为50 rpm/min,在紫外光下连续照射96 h。
d、反应结束后,在将复合纤维在1000 rpm/min转速下离心10 min,室温干燥。
实施例7:
a、以氧化石墨烯作为碳源,超声分散在蒸馏水中,配置浓度为1 mg/mL。
b、将静电纺丝制备的N掺杂TiO2纳米纤维分散在水中,配置浓度为0.1 mg/mL。
c、将上述溶液混合,其中氧化石墨烯/SnO2纳米纤维质量比为10:1置于烧杯中,在可见光下连续照射96 h。
d、反应结束后,在将复合纤维在1000 rpm/min转速下离心10 min,室温干燥。
实施例8:
a、以氧化石墨烯作为碳源,超声分散在蒸馏水中,配置浓度为1 mg/mL。
b、将静电纺丝制备的S掺杂TiO2纳米纤维分散在水中,配置浓度为0.1 mg/mL。
c、将上述溶液混合,其中氧化石墨烯/S掺杂TiO2纳米纤维质量比为5:1置于烧杯中,磁力搅拌,转速为400 rpm/min,在可见光下连续照射24 h。
d、反应结束后,在将复合纤维在500 rpm/min转速下离心60 min,将产物分离出来,室温干燥。
实施例9:
a、以氧化石墨烯作为碳源,超声分散在蒸馏水中,配置浓度为1 mg/mL。
b、将静电纺丝制备的N和S共掺杂TiO2纳米纤维分散在水中,配置浓度为0.1 mg/mL。
c、将上述溶液混合,置于烧杯中,在可见光下连续照射1 h。
d、反应结束后,在将复合纤维在8000 rpm/min转速下进行离心,将产物分离出来,室温干燥。
其中氧化石墨烯/N和S共掺杂TiO2纳米纤维质量比为1:10。
实施例10:
a、以氧化石墨烯作为碳源,超声分散在蒸馏水中,配置浓度为1 mg/mL。
b、将S掺杂的ZnO纳米棒分散在水中,配置浓度为0.1 mg/mL。
c、将上述溶液混合,置于烧杯中,磁力搅拌,转速为500 rpm/min,在可见光下连续照射120 h。
d、反应结束后,在将复合纤维在8000 rpm/min转速下进行离心,将产物分离出来,室温干燥。
其中氧化石墨烯/S掺杂的ZnO纳米棒质量比为20:1。
Claims (1)
1.光催化法制备光催化剂/石墨烯一维核壳复合结构的方法,其特征在于制备步骤为:
a. 将氧化石墨烯分散在溶剂中,配制浓度为0.01-10 mg/mL的氧化石墨烯胶体;所述氧化石墨烯分散溶剂为水或者乙醇;
b. 将一维结构的光催化剂分散在溶剂中,配置浓度为0.01-1000 mg/mL的光催化剂悬浮液;所述一维结构为纳米纤维、纳米管或纳米棒;所述光催化剂为TiO2、ZnO、ZrO2、SnO2、N掺杂TiO2、S掺杂TiO2、N和S共掺杂TiO2或N掺杂ZnO;所述光催化剂分散溶剂为水或者乙醇;
c. 将上述溶液按质量比100:1-1:100混合搅拌,置于开口容器中光照0.5-1000 h;所述光照为可见光照或者紫外光照;搅拌速度为不超过800 rpm/min;
d. 反应结束后,再将产物离心分离,干燥;离心速度为500-13000 rpm/min,离心时间为1-60 min。
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