CN107413326A - 一种碳纤维支撑液膜燃烧制备高活性CQDs/BiVO4复合纳米光催化材料的方法 - Google Patents
一种碳纤维支撑液膜燃烧制备高活性CQDs/BiVO4复合纳米光催化材料的方法 Download PDFInfo
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Abstract
本发明涉及一种碳纤维支撑液膜燃烧制备高活性CQDs/BiVO4复合纳米光催化材料的方法,以改性后碳纤维为支撑体,采用液膜燃烧法(LFC),通过将反应原料溶液附着于改性后的碳纤维,在一定温度下煅烧2h后,用去离子水或乙醇或甲醇清洗后,高速离心烘干,一步合成CQDs/BiVO4复合纳米材料。该材料晶体粒径小,并具有高光催化活性。本方法可以批量制备CQDs/BiVO4复合纳米材料,合成方法简单,重复性好,在光分解水、光催化氧化环境污染物等领域具有广泛的应用前景。且该方法还可以推广用于其他多金属氧化物的合成。
Description
技术领域
本发明属于环境污染治理技术领域,涉及ー种钒酸铋可见光光催化材料的制备方法。
背景技术
随着社会不断发展,环境污染治理是人类社会面临和急需解决的重大课题。在众多的环境污染治理技术中,半导体多相光催化技术,因其能室温条件下反应、可直接利用太阳光作为光源来驱动氧化-还原反应等优点而成为ー种理想的环境污染治理技木。BiVO4作为ー类新型可见光半导体光催化材料,因其带隙较窄(约2.4eV),波长响应范围扩展到520nm左右,光化学性能稳定,氧化还原能力强,无毒、价廉等优点正在成为可见光光催化研究領域的热点。研究报道BiVO4主要有3种晶体结构,包括四方晶系白钨矿型(高温相)、四方晶系硅酸锆型和单斜晶系变形白钨矿型(褐钇铌矿型)。其中单晶·白钨矿结构的单体BiVO4光催化活性相对最高。然而,BiVO4的导带边位于0V,其光生电子不容易被空气中的氧气捕获而在催化剂表面积累,増加了电子与空穴的复合几率,致使在可见光下降解有机物的能力较差。因此在这种情况下快速捕获光激发电子,抑制其与高能空穴的复合,对提高此类光催化剂可见光催化降解污染物的效率至关重要。为此,研究者采取了多种手段对其进行修饰与改性,其中复合碳量子点(CQDs)能有效抑制光生电子-空穴复合,延长光载流子寿命,是提高光催化活性的一种有效方法。CQDs是一种粒子尺寸小于20nm的新型碳纳米材料,具有成本低廉、低毒、化学惰性、导电性良好、快速转移和存储电子的特性。如Wu等采用水热法和电化学法分别制备BiVO4和CQDs,然后将两者按照一定比例与环己烷混合,40℃下回流3h,然后在85℃下将环己烷蒸发干得到CQDs/BiVO4量子点,分解水制氢能力是单独BiVO4量子点的4倍。Nan等制备了CQDs与反蛋白石BiVO4复合,CQDs对可见光的强吸收能力以及对光生电子的捕获,复合CQDs后,分解水制氢效率提高了五倍。但目前制备CQDs与光催化材料掺杂基本都需分步法,本发明采用碳纤维支撑液膜燃烧法(LFC),通过碳纤维表面改性,改变表面浸润性和引入特征官能团,调节反应前驱溶液在纤维表面成膜状态,能一步实现BiVO4与CQDs的原位复合,降低电子-空穴的复合率,有效提高BiVO4的可见光催化活性。目前尚未见采用此种简易方法,实现BiVO4与CQDs原位复合的相关报到。
发明内容
本发明涉及一种高活性碳量子点(CQDs)/BiVO4光催化材料的制备方法,
一种碳纤维支撑液膜燃烧制备高活性CQDs/BiVO4复合纳米光催化材料的方法,制备步骤如下:
(1)碳纤维改性:采用无胶碳纤维,将其剪为10cm长,先依次采用丙酮、乙醇和去离子水超声清洗,然后将其在至少含有硝酸或硫酸的酸性条件下浸泡24-72小时,再经去离子水超声清洗,40℃下烘干;
(2)BiVO4反应溶液制备:将一定量的硝酸铋和偏钒酸铵以1:1摩尔比,分别溶于溶剂 (去离子水或乙二醇)后混合,并分别加入柠檬酸或尿素或乙二胺四乙酸等,再将两溶液混合,然后用氨水调节混合溶液pH值为5-6,在80℃下持续搅拌蒸发反应原料溶液至一定粘度,将一定量烘干的碳纤维等体积浸渍于反应溶液;
(3)将步骤(2)附有一层反应溶液液膜的碳纤维,置于马弗炉中于400-450℃下煅烧1h;
(4)将步骤(3)所得负有BiVO4的碳纤维于去离子水或乙醇或甲醇中清洗,然后将清洗液置于高速离心机中5000rpm离心20分钟,将浓缩沉淀液于烘箱中30-40℃干燥至恒重,得到CQDs/BiVO4复合纳米材料。
本发明以改性后碳纤维为支撑体,采用液膜燃烧法(LFC),通过将反应原料溶液附着于改性后的碳纤维,在一定温度下煅烧2h后,用去离子水或乙醇或甲醇清洗后,高速离心烘干,一步合成CQDs/BiVO4复合纳米材料。该材料晶体粒径小,并具有高光催化活性。本方法可以批量制备CQDs/BiVO4复合纳米材料,合成方法简单,重复性好,在光分解水、光催化氧化环境污染物等领域具有广泛的应用前景,而且该方法还可以推广用于其他多金属氧化物的合成。
附图说明
图1 CQDs/BiVO4复合纳米材料1-4以及纯BiVO4降解罗丹明效率变化曲线。
图2 CQDs/BiVO4复合材料2的XRD图谱。
图3 CQDs/BiVO4复合材料2的TEM图谱。
图4 CQDs/BiVO4复合材料2的XPS图谱。
具体实施方式
下面通过实例对本发明所述的方法和技术加以说明,实际应用中,不限于此。
实例1:(1)碳纤维改性:将无胶碳纤维剪为10cm长,依次采用丙酮、乙醇和去离子水超声清洗,然后将其浸泡于浓硝酸中72小时,再经去离子水超声清洗,40℃下烘干;(2)BiVO4反应溶液制备:将0.01mol的硝酸铋和偏钒酸铵分别溶于80℃25mL去离子水中,然后分别于两溶液中加入0.02mol柠檬酸,再将两反应溶液混合,再用氨水调节混合溶液pH值为6,然后在80℃持续搅拌蒸发反应原料溶液至余下20mL,将15g改性碳纤维等体积浸渍于反应溶液;(3)将步骤(2)负有一层反应溶液液膜的碳纤维,置于马弗炉中于450℃下煅烧 1h;(4)将步骤(3)所得负有BiVO4的碳纤维于去离子水中清洗,然后将清洗液置于高速离心机中5000rpm离心20分钟,将浓缩沉淀液于烘箱中30℃干燥至恒重,得到CQDs/BiVO4复合纳米材料1。
实例2:(1)碳纤维改性:将无胶碳纤维剪为10cm长,依次采用丙酮、乙醇和去离子水超声清洗,然后将其浸泡于浓硝酸中48小时,再经去离子水超声清洗,40℃下烘干;(2)BiVO4反应溶液制备:将0.01mol的硝酸铋和偏钒酸铵分别溶于80℃25mL去离子水中,然后分别于两溶液中加入0.02mol柠檬酸,再将两反应溶液混合,再用氨水调节混合溶液pH值为6,然后在80℃持续搅拌蒸发反应原料溶液至余下10mL,将10g改性碳纤维等体积浸渍于反应溶液;(3)将步骤(2)负有一层反应溶液液膜的碳纤维,置于马弗炉中于400℃下煅烧 1h;(4)将步骤(3)所得负有BiVO4的碳纤维于去离子水中清洗,然后将清洗液置于高速离心机中5000rpm离心20分钟,将浓缩沉淀液于烘箱中30℃干燥至恒重,得到CQDs/BiVO4复合纳米材料2。
实例3:(1)碳纤维改性:将无胶碳纤维剪为10cm长,依次采用丙酮、乙醇和去离子水超声清洗,然后将其浸泡于浓硝酸中48小时,再经去离子水超声清洗,40℃下烘干;(2)BiVO4反应溶液制备:将0.01mol的硝酸铋和偏钒酸铵分别溶于80℃25mL乙二醇中,然后分别于两溶液中加入0.01mol尿素,再将两反应溶液混合,再用氨水调节混合溶液pH值为 6,然后在80℃持续搅拌蒸发反应原料溶液至余下12mL,将10g改性碳纤维等体积浸渍于反应溶液;(3)将步骤(2)负有一层反应溶液液膜的碳纤维,置于马弗炉中于400℃下煅烧1h;(4)将步骤(3)所得负有BiVO4的碳纤维于去离子水中清洗,然后将清洗液置于高速离心机中5000rpm离心20分钟,将浓缩沉淀液于烘箱中30℃干燥至恒重,得到CQDs/BiVO4复合纳米材料3。
实例4:(1)碳纤维改性:将无胶碳纤维剪为10cm长,依次采用丙酮、乙醇和去离子水超声清洗,然后将其浸泡于浓酸中48小时,再经去离子水超声清洗,40℃下烘干;(2)BiVO4反应溶液制备:将0.01mol的硝酸铋和偏钒酸铵分别溶于80℃25mL去离子水中,然后分别于两溶液中加入0.02mol乙二胺四乙酸,再将两反应溶液混合,再用氨水调节混合溶液pH值为6,然后在80℃持续搅拌蒸发反应原料溶液至余下20mL,将15g改性碳纤维等体积浸渍于反应溶液;(3)将步骤(2)负有一层反应溶液液膜的碳纤维,置于马弗炉中于400℃下煅烧 1h;(4)将步骤(3)所得负有BiVO4的碳纤维于去离子水中清洗,然后将清洗液置于高速离心机中5000rpm离心20分钟,将浓缩沉淀液于烘箱中30℃干燥至恒重,得到CQDs/BiVO4复合纳米材料4。
对以上所得CQDs/BiVO4复合纳米材料1-4进行光催化活性测试实验,同时为了对比,在同样条件下也测定了纯BiVO4的光催化活性。光催化活性测试过程如下:将初始浓度为 5mg·L-1罗丹明B(RhB)溶液50ml作为目标降解物置于250ml烧杯中,称取0.01g光催化剂并使其均匀分布于罗丹明B(RhB)溶液中,光催化剂在溶液中呈悬浮状态,加入0.1ml浓度为10%的H2O2。为了达到溶解-吸附平衡,将此悬浮液在磁力搅拌条件下暗反应30min,将其置于距液面14cm的可见光光源(250W金卤灯)下进行光催化实验,每隔一段时间取上清液在罗丹明B(RhB)的最大吸收波长处(554nm)测其吸光度,共光照反应50min,所得结果如附图1所示。
Claims (1)
1.一种碳纤维支撑液膜燃烧制备高活性CQDs/BiVO4复合纳米光催化材料的方法,制备步骤如下:
(1)碳纤维改性:采用无胶碳纤维,将其剪为10cm长,先依次采用丙酮、乙醇和去离子水超声清洗;然后将其在至少含有硝酸或硫酸的酸性条件下浸泡24-72小时,再经去离子水超声清洗,40℃下烘干;
(2)BiVO4反应溶液制备:将硝酸铋和偏钒酸铵以1:1摩尔比,分别溶于溶剂后混合,并分别加入柠檬酸、尿素或乙二胺四乙酸;再将两溶液混合,然后用氨水调节混合溶液pH值为5-6,在80℃下持续搅拌蒸发反应原料溶液至一定粘度,将烘干的碳纤维等体积浸渍于反应溶液;
(3)将步骤(2)附有一层反应溶液液膜的碳纤维,置于马弗炉中于400-450℃下煅烧1h;
(4)将步骤(3)所得负有BiVO4的碳纤维于去离子水、乙醇或甲醇中清洗,然后将清洗液置于高速离心机中5000rpm离心20分钟,将浓缩沉淀液于烘箱中30-40℃干燥至恒重,得到CQDs/BiVO4复合纳米材料。
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