CN106964381B - 一种高浓度纳米红磷光催化剂分散液的制备方法 - Google Patents
一种高浓度纳米红磷光催化剂分散液的制备方法 Download PDFInfo
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Abstract
本发明公开了一种高浓度纳米红磷光催化剂分散液的制备方法。首先,将市售红磷置于水中研磨,筛网筛分后获得微米级红磷颗粒,对微米级红磷颗粒进行溶剂热处理后,离心、洗涤、干燥、退火获得纳米红磷光催化剂,再将其分散于水中进行超声处理可获得高浓度纳米红磷光催化剂分散液。该分散液制备方法简单,稳定性好,可长期稳定储存;所得纳米红磷光催化剂具有层状孔道结构,比较面积高,重复利用性能好,具有较好的光解水制氢及光降解有机污染物性能。
Description
技术领域
本发明属于光催化剂制备技术领域,具体涉及一种高浓度纳米红磷光催化剂分散液的制备方法。
背景技术
半导体光催化技术作为一种绿色催化技术,已经成为解决能源和环境问题的重要技术之一,在光解水制氢、光催化还原CO2、污染物降解等领域展示出良好的应用前景。纵观光催化技术的发展历程,实际上就是高效光催化剂的研发过程,高效、稳定、廉洁的光催化剂的开发一直是光催化技术的研究核心。以二氧化钛(TiO2)为代表的经典半导体和石磨相氮化碳(g-C3N4)为代表的新型非金属光催化材料,因二者物理化学性质稳定、廉价易得、环境友好一直是光催化领域研究的热点。但是受能带结构的限制,可见光利用率仍然很低,而且,光生电子和空穴极易复合,很难迁移至催化剂表面参与氧化还原反应,进一步导致量子效率降低,阻碍了光催化技术的发展。当前,开发光谱响应范围宽、量子效率高的新型光催化剂仍是当前光催化领域的重要研究方向。
Wang等首次报道单质红磷作为光催化剂可实现光解水制氢,引起了广泛关注。研究发现,RP带隙较窄(Eg≈1.8eV)与太阳光匹配度好,能够吸收长达700nm的可见光,而且其导带电势位置比H+/H2还原电势更负,价带电势位置比O2/H2O的氧化电势更正,具有分解水产氢气和氧气的能力,成为新型可见光光催化剂中的一颗新星。虽然红磷常温下化学性质稳定(不溶于水,空气中不自燃),但高温易着火,加工时要避免受热、摩擦和撞击,使得红磷的制备方法几乎均采用水热法或机械研磨法(需要惰性介质保护),很难得到纳米颗粒,产物多为微米或亚微米颗粒,比表面积小,不利于表面催化反应的进行。
发明内容
针对现有制备技术的缺陷和不足,本发明提供了一种高浓度纳米红磷光催化剂分散液的制备方法,获得的纳米红磷具有层状结构,孔道发达,比较面积高,重复利用性能好。
为了解决上述技术问题,本发明采用如下技术方案予以实现:
一种高浓度纳米红磷光催化剂分散液的制备方法,包括以下步骤:
步骤一:将红磷置于水中研磨,筛分后获得微米级红磷颗粒;
步骤二:将获得微米级红磷颗粒在溶剂中进行热处理,热处理温度为160~220℃,时间3~72h;
所述的溶剂为水、乙二醇或丙三醇和NaOH的混合溶液,其中:水与乙二醇或丙三醇的体积比为11:1~3:1,NaOH浓度为0.05~0.20mol/L;
步骤三:将热处理后的红磷进行离心、洗涤、干燥、退火处理,得到纳米级红磷;
步骤四:将获得的纳米级红磷分散于水中,超声处理,获得纳米红磷光催化剂分散液;
进一步的,所述的步骤三中,离心转速为8000~12000r/min;采用真空干燥,温度为50~80℃。
进一步的,所述的退火处理工艺为:在温度350~380℃下保温1~2h,在氩气气氛进行。
进一步的,所述的超声频率为20KHz,超声功率300~800W,超声时间2~10h,在空气中进行。
进一步的,所述的纳米红磷光催化剂分散液中红磷的浓度可达2g/L。
与现有技术相比,本发明的有益效果是:
(1)本发明采用的溶剂热法和超声分散法制备纳米红磷的方法简单,所得纳米红磷具有层状孔道结构,比表面积高,可达54m2/g,有利于提供更多活性位点。
(2)本发明的纳米红磷分散液在作为光催化剂使用过程中,能与反应助剂良好接触,实现光生电子与空穴的快速分离。
(3)本发明的纳米红磷光催化剂分散液在避免了纳米红磷粉体在制备和使用过程中的分离、干燥、称量等过程,可进行稀释获得不同浓度纳米红磷分散液,避免了称量纳米材料所引起的误差,储存、使用安全方便。
附图说明
图1是本发明实施例1所得纳米红磷样品不同浓度分散液的宏观照片。
图2是本发明实施例1所得纳米红磷样品的TEM图。
图3是本发明纳米红磷样品的吸收光谱图。
图4是本发明所得纳米红磷样品的氮气吸附-脱附曲线。
图5是本发明实施例1所得纳米红磷分散液稀释后光解水制氢的性能图。
图6是本发明实施例2所得纳米红磷分散液稀释后光解水制氢的性能图。
图7是本发明实施例3所得纳米红磷光催化降解罗丹明B吸收光谱图。
以下结合实施例对本发明的具体内容作进一步详细解释说明。
具体实施方式
本发明的高浓度纳米红磷光催化剂分散液的制备方法,包括以下步骤:
步骤一:将红磷置于水中研磨,筛分后获得微米级红磷颗粒;
步骤二:将获得微米级红磷颗粒在溶剂中进行热处理,热处理温度为160~220℃,时间3~72h;
所述的溶剂为水、乙二醇或丙三醇和NaOH的混合溶液,其中:水与乙二醇或丙三醇的体积比为11:1~3:1,NaOH浓度为0.05~0.20mol/L;
步骤三:将热处理后的红磷进行离心、洗涤、干燥、退火处理,得到纳米级红磷;
步骤四:将获得的纳米级红磷分散于水中,超声处理,获得纳米红磷光催化剂分散液;
其中,步骤三中,离心转速为8000~12000r/min;采用真空干燥,温度为50~80℃。
退火处理工艺为:在温度350~380℃下保温1~2h,在氩气气氛进行。
超声频率为20KHz,超声功率300~800W,超声时间2~10h,在空气中进行。
纳米红磷光催化剂分散液中红磷的浓度可达2g/L。
纳米红磷具有较大的比表面积能为表面反应提供更多空间场所,反应物吸附、脱附、传质扩散过程可得到有效强化,同时光生电子与空穴的迁移距离将大幅缩短,表现出高的光催化活性。
本发明的退火处理可使得红磷原子排布稳定,有利于去除表面杂质。
以下给出本发明的具体实施例,需要说明的是本发明并不局限于以下具体实施例,凡在本申请技术方案基础上做的等同变换均落入本发明的保护范围。
实施例1
在室温条件下,将市售红磷置于水中研磨,用120目筛网筛分后干燥获得微米级红磷颗粒,称取3g分散于由55mL水、5mL乙二醇、0.12gNaOH组成的反应液中,搅拌30min,转移至100mL具有聚四氟乙烯内衬的水热合成反应罐中,密封后置于鼓风干燥箱,以5℃/min升温至200℃保温24h,反应完成后自然冷却至室温,将产物用蒸馏水、无水乙醇反复冲洗、离心(12000rmp/min),将产物在80℃干燥后,在氩气保护下于380℃退火处理1h,最后,将1.0g产物分散于500mL水中,采用300W、20KHz超声10h得到高浓度纳米红磷光催化剂分散液。取纳米红磷分散液6mL加入到94mL水溶液中(含4mL三乙醇胺作为牺牲剂),将其置于光催化反应器中(Labsolar-III AG光催化系统),密封并抽真空后,开启300W氙灯在反应器顶部垂直照射反应液,每隔1h通过气相色谱检测氢气产量,测试结果如图5所示,在最初反应阶段,制氢速率可达到862.8μmol·h-1·g-1。
实施例2
在室温条件下,将市售红磷置于水中研磨,用120目筛网筛分后干燥获得微米级红磷颗粒,称取3g分散于由45mL水、15mL乙二醇、0.48gNaOH组成的反应液中,搅拌30min,转移至100mL具有聚四氟乙烯内衬的水热合成反应罐中,密封后置于鼓风干燥箱,以5℃/min升温至160℃保温12h,反应完成后自然冷却至室温,将产物用蒸馏水、无水乙醇反复冲洗、离心(8000rmp/min),将产物在50℃干燥后,在氩气保护下于350℃退火处理2h,最后,将1.0g产物分散于500mL水中,采用800W,20KHz超声2h得到高浓度纳米红磷光催化剂分散液。取纳米红磷分散液6mL加入到94mL水溶液中(含4mL三乙醇胺作为牺牲剂),将其置于光催化反应器中(Labsolar-III AG光催化系统),密封并抽真空后,开启300W氙灯在反应器顶部垂直照射反应液,每隔1h通过气相色谱检测氢气产量,测试结果如图6所示,在最初反应阶段,制氢速率可达到115.2μmol·h-1·g-1。
实施例3
在室温条件下,将市售红磷置于水中研磨,用120目筛网筛分后干燥获得微米级红磷颗粒,称取1g分散于由45mL水、15mL丙三醇、0.12gNaOH组成的反应液中,搅拌30min,转移至100mL具有聚四氟乙烯内衬的水热合成反应罐中,密封后置于鼓风干燥箱,以5℃/min升温至180℃保温6h,反应完成后自然冷却至室温,将产物用蒸馏水、无水乙醇反复冲洗、离心(8000rmp/min),将产物在60℃干燥后,在氩气保护下于350℃退火处理1h,最后,将1.0g产物分散于500mL水,采用500W,20KHz超声6h得到高浓度纳米红磷光催化剂分散液。取纳米红磷分散液6mL加入到50mL浓度为50mg/L的罗丹明B溶液中,先置于黑暗中搅拌30min,使反应体系达到吸附平衡。随后开启反应光源,每隔10min采集悬浮液,离心分离,用UV/VIS/NIR分光光度计测定上清液中罗丹明B的吸光度。由图7所示,在40min以内光降解效率可以达到91.96%。
Claims (5)
1.一种高浓度纳米红磷光催化剂分散液的制备方法,其特征在于:包括以下步骤:
步骤一:将红磷置于水中研磨,筛分后获得微米级红磷颗粒;
步骤二:将获得微米级红磷颗粒在溶剂中进行热处理,热处理温度为160~220℃,时间3~72h;
所述的溶剂为水、乙二醇或丙三醇和NaOH的混合溶液,其中:水与乙二醇或丙三醇的体积比为11:1~3:1,NaOH浓度为0.05~0.20mol/L;
步骤三:将热处理后的红磷进行离心、洗涤、干燥、退火处理,得到纳米级红磷;
步骤四:将获得的纳米级红磷分散于水中,超声处理,获得纳米红磷光催化剂分散液。
2.如权利要求1所述的高浓度纳米红磷光催化剂分散液的制备方法,其特征在于:所述的步骤三中,离心转速为8000~12000r/min;采用真空干燥,温度为50~80℃。
3.如权利要求1所述的高浓度纳米红磷光催化剂分散液的制备方法,其特征在于:所述的退火处理工艺为:在温度350~380℃下保温1~2h,在氩气气氛进行。
4.如权利要求1所述的高浓度纳米红磷光催化剂分散液的制备方法,其特征在于:所述的超声频率为20KHz,超声功率300~800W,超声时间2~10h,在空气中进行。
5.如权利要求1所述的高浓度纳米红磷光催化剂分散液的制备方法,其特征在于:所述的纳米红磷光催化剂分散液中红磷的浓度可达2g/L。
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