CN106732732A - 一种抗堆叠氮掺杂的三维石墨烯及其制备方法 - Google Patents
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Abstract
本发明公开一种抗堆叠氮掺杂的三维石墨烯及其制备方法。用三聚氰胺和37wt%甲醛水溶液和氧化石墨烯水溶液水热制备抗堆叠氧化石墨烯;将所制的抗堆叠氧化石墨烯在氮气气氛下煅烧即可得到抗堆叠氮掺杂的三维石墨烯;在可见光光照下,该催化剂负载质量比为10%的贵金属Pt之后,具有很好地曙红Y敏化光解水产氢活性;由于制备方法简单易行,催化剂廉价可方便回收重复利用,该复合型光催化材料在材料制备技术领域和光解水产氢领域具有广泛地实用价值和应用前景。
Description
技术领域
本发明属于光催化材料制备和光催化技术领域,具体涉及一种抗堆叠氮掺杂的三维石墨烯及其制备方法,。
背景技术
近年来,石墨烯,这种具有独特的二维形貌、优异的导电性能以及极大的理论比表面积的材料在光催化领域得到了广泛的关注和应用。在光催化领域,石墨烯常用的制备方法是改性的Hummers方法。这种石墨烯的制备方法实验操作则相对简单,石墨烯的产量也相对较高,而且可以在石墨烯表面引入一定量的含氧官能团,有利于增加石墨烯在不同溶剂(水相和有机相)中的分散性。
但是,这种方法所制备的石墨烯通常都会带有许多的缺陷,并且存在着严重的堆叠现象,而这些都会显著的影响石墨烯的导电性能,从而难以充分发挥出石墨烯的优异的导电性能。我们知道,石墨烯的导电性能又会直接影响到石墨烯基光催化剂的催化活性,因此,优化所制备的石墨烯的导电性对于制备高效的石墨烯基光催化材料意义重大。
为了减少石墨烯堆叠和缺陷带来的导电性能降低对石墨烯基光催化剂的催化活性的影响,研究者们通过制备具有3D形貌的石墨烯来抑制石墨烯的堆叠,或者是引入其他杂原子(如,B、N、S和P等)来减小石墨烯的表面缺陷,以期获得导电性能更好的石墨烯来提高石墨烯基光催化剂的催化活性。但是这两种策略分别使用时对石墨烯的导电性能改善能力有限,如何同时将两种策略应用在石墨烯上来进一步提高石墨烯的导电性能仍然是一个研究难点。
发明内容
本发明的目的在于提供一种抗堆叠氮掺杂的3D石墨烯及其制备方法,以解决石墨烯堆叠和缺陷对石墨烯基光催化材料的性能带来的影响,所制备的抗堆叠氮掺杂的3D石墨烯负载质量比为10%的贵金属Pt的情况下,可以实现高效的曙红Y敏化光解水产氢。
为实现上述目的,本发明采用如下技术方案:
一种制备如上所述的抗堆叠氮掺杂的3D石墨烯的制备方法,包括以下步骤:
(1)抗堆叠氧化石墨烯的制备:
将三聚氰胺、37wt%甲醛加入到氧化石墨烯水溶液混合搅拌后,在180 ℃下水热10 h,然后离心、洗涤、干燥得到抗堆叠3D氧化石墨烯;
(2)抗堆叠氮掺杂的3D石墨烯的制备:
将步骤(1)制得的抗堆叠3D氧化石墨烯放入管式炉中,在氮气气氛保护下750 ℃煅烧5h,然后自然降温,得到抗堆叠氮掺杂的3D石墨烯。
步骤(1)中,氧化石墨烯水溶液的浓度为10 mg/mL。
步骤(2)中,升温速度为5 ℃每分钟;
曙红Y敏化光解水产氢的具体步骤如下:
(1)将10mg的抗堆叠氮掺杂的3D石墨烯和40mg曙红Y加入到70 mL水溶液中混合超声,加入0.50 mL 10mM的H2PtCl6和10 mL的三乙醇胺作为光解水反应牺牲剂;
(2)在保持温度恒定为5 ℃时,对反应体系进行脱气,以便获得良好的真空反应条件;
(3)用波长大于420 nm的可见光照射反应体系,先光照30min作为光沉积Pt的时间;
(4)光沉积Pt完成后,对体系脱气,保持良好的真空反应条件,然后光照2 h检测体系中的产氢量;
(4)将光催化产物气体进气相色谱分析,以氩气为载气,通过保留时间和峰面积定性定量。
本发明的显著优点在于:
(1)本发明将贵金属Pt原位光沉积到抗堆叠氮掺杂的3D石墨烯并将其用于曙红Y敏化分解水制氢反应,具有高催化效率,稳定性好等优点;
(2)开发高效的可见光驱动的光解水制氢催化剂,有利于环境和能源的可持续发展。
附图说明
图1是抗堆叠氮掺杂的3D石墨烯的SEM图。
图2是抗堆叠氮掺杂的3D石墨烯N 1S的XPS图。
图3是堆叠石墨烯、3D石墨烯和抗堆叠氮掺杂的3D石墨烯的曙红Y敏化光解水产氢活性图。
具体实施方式
本发明用下列实施例来进一步说明本发明,但本发明的保护范围并不限于下列实施例。
实施例1
将80 mL 1 mg/mL 氧化石墨烯水溶液加入到反应釜中,而后在180 ℃下水热10 h,然后所得到的固体离心洗涤3遍,在60 ℃烘干12 h,得到堆叠石墨烯;
取10 mg 所制的堆叠石墨烯和40 mg 曙红Y固体加入到70 mL水溶液中,超声30 min,加入0.50 mL 10mM的H2PtCl6和10 mL的三乙醇胺,在保持5 ℃恒温条件下,对反应体系进行脱气。而后,用波长大于420 nm的可见光照射反应体系30 min。之后对体系进行脱气,保持体系真空状态。用波长大于420 nm的可见光照射反应体系,通过气相色谱在线检测氢气产量,以氩气作为载气。光照2 h后,检测体系中氢气产量。
实施例2
将15 mL 10 mg/mL 氧化石墨烯水溶液加入到反应釜中,而后在180 ℃下水热10 h,然后所得到的柱状石墨烯冷冻干燥,得到3D石墨烯;
取10 mg 所制的3D石墨烯和40 mg 曙红Y固体加入到70 mL溶液中,超声30 min,加入0.50 mL 10mM的H2PtCl6和10 mL的三乙醇胺,在保持5 ℃恒温条件下,对反应体系进行脱气。而后,用波长大于420 nm的可见光照射反应体系30 min。之后对体系进行脱气,保持体系真空状态。用波长大于420 nm的可见光照射反应体系,通过气相色谱在线检测氢气产量,以氩气作为载气。光照2 h后,检测体系中氢气产量。
实施例3
将350 mg三聚氰胺、1.5 mL 37wt%甲醛加入到15 mL 10 mg/mL氧化石墨烯水溶液中,在180 ℃下水热10 h,然后离心、洗涤、干燥得到抗堆叠氧化石墨烯。将抗堆叠氧化石墨烯放入管式炉中,在氮气气氛保护下750 ℃煅烧5 h(升温速率为5 ℃每分钟),然后自然降温,得到抗堆叠氮掺杂的3D石墨烯;
取10 mg 所制的抗堆叠氮掺杂的3D石墨烯和40 mg 曙红Y固体加入到70 mL溶液中,超声30 min,加入0.50 mL 10mM的H2PtCl6和10 mL的三乙醇胺,在保持5 ℃恒温条件下,对反应体系进行脱气。而后,用波长大于420 nm的可见光照射反应体系30 min。之后对体系进行脱气,保持体系真空状态。用波长大于420 nm的可见光照射反应体系,通过气相色谱在线检测氢气产量,以氩气作为载气。光照2 h后,检测体系中氢气产量。
以上所述仅为本发明的较佳实施例,凡依本发明申请专利范围所做的均等变化与修饰,皆应属本发明的涵盖范围。
Claims (6)
1.一种抗堆叠氮掺杂的三维石墨烯,其特征在于:所述石墨烯是一种含有氮掺杂,而且具有抗堆叠3D形貌的石墨烯。
2.一种制备如权利要求1所述的一种抗堆叠氮掺杂的三维石墨烯的方法,其特征在于:包括以下步骤:
(1)抗堆叠氧化石墨烯的制备:
将350 mg 三聚氰胺、1.5 mL 37wt%甲醛加入到15 mL 10 mg/mL氧化石墨烯水溶液混合搅拌后,在180 ℃下水热10 h,然后离心、洗涤、干燥得到抗堆叠氧化石墨烯;
(2)抗堆叠氮掺杂的3D石墨烯的制备:
将步骤(1)制得的抗堆叠氧化石墨烯放入管式炉中,在氮气气氛保护下煅烧,然后自然降温,得到抗堆叠氮掺杂的三维石墨烯。
3. 根据权利要求2所述的抗堆叠氮掺杂的三维石墨烯的制备方法,其特征在于:步骤(1)中,氧化石墨烯水溶液的浓度为10 mg/mL。
4. 根据权利要求2所述的抗堆叠氮掺杂的三维石墨烯的制备方法,其特征在于:步骤(2)中,煅烧温度为750 ℃,煅烧时间为5 h。
5.一种如权利要求1所述的抗堆叠氮掺杂的三维石墨烯的应用,其特征在于:所述抗堆叠氮掺杂的三维石墨烯应用于曙红Y敏化光解水产氢。
6. 根据权利要求5所述的抗堆叠氮掺杂的三维石墨烯的应用,其特征在于:抗堆叠氮掺杂的3D石墨烯在原位光沉积质量比为10%的Pt之后,在波长>420 nm的可见光下照射2 h,曙红Y敏化光解水产氢量为778 μmol。
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