CN106944029A - 一种碳量子点/凹凸棒纳米复合材料及其制备方法和应用 - Google Patents
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Abstract
本发明属于化工新材料领域,特别涉及一种碳量子点/凹凸棒纳米复合材料及其制备方法和应用。本发明将柠檬酸、双氧水和凹凸棒混合进行水热反应,再经过离心、洗涤、烘干得到碳量子点/凹凸棒纳米复合材料,再将此复合材料用于光催化脱硫。
Description
技术领域
本发明属于化工新材料领域,特别涉及一种碳量子点/凹凸棒纳米复合材料及其制备方法和应用。
背景技术
燃料中的含硫化合物转化为SOx逐渐导致空气污染和酸雨形成。为了减少对人类健康和环境的危害性影响,因此迫切需要降低燃料中的硫含量。
传统加氢脱硫虽已广泛应用,但是其需要高温高压和昂贵的氢气。另外,由于二苯并噻吩及其衍生物如4,6-二甲基二苯并噻吩在加氢条件下是强稳定性的,因此难以满足深度脱硫的要求,包括氧化脱硫,萃取脱硫,生物脱硫和吸附脱硫等的替代方法已被用于从燃料油中去除含硫物质,其中氧化脱硫由于其低成本和高效率而备受关注。因此,光催化氧化脱硫新材料由于其成本低,操作简单,无需氢耗,脱硫效率高的优点而受到广泛的关注。
发明内容
本发明旨在提供一种碳量子点/凹凸棒纳米复合材料及其制备方法和应用,该复合材料是以凹凸棒为载体,将凹凸棒与碳量子点复合后得到的纳米复合材料,本发明复合材料的组成通式表示为:CQDs/ATP。
本发明的制备方法为:将柠檬酸、双氧水和凹凸棒混合进行水热反应,再经过离心、洗涤、烘干得到碳量子点/凹凸棒纳米复合材料,
控制柠檬酸的用量,使碳量子点相对于凹凸棒的质量分数为10%-40%,
双氧水中过氧化氢的浓度为0.9mol·L-1,控制双氧水中过氧化氢和柠檬酸的摩尔比为0.3~0.6:1,
水热温度为120-180℃,水热时间为6-24h。
本发明还提供了一种上述复合材料的应用,即将该复合材料用于光催化脱硫。
现有的制备工艺所得到的碳量子点往往粒径过大,对此,本发明在柠檬酸碳源水热过程中加入双氧水,发现以此为水热体系提供了羟基环境后,有效控制了所生成的碳量子点的粒径小于5nm。同时,本发明中碳量子点被可见光激发后产生光生电子与空穴,电子被注入凹凸棒导带,大大降低了与碳量子点上余留的空穴重新复合的几率,提高了光响应范围,此时该电子与O2、H2O2生成·O2 —、·OH,用以氧化二苯并噻吩实现脱硫。
附图说明
图1为实施例1所制备的CQDs/ATP的XRD图。
图2为实施例1中原料ATP的TEM图。
图3为实施例1所制备的CQDs/ATP的TEM图。
图4为对比例1所制备的CQDs/ATP的TEM图。
具体实施方式
实施例1:
称取柠檬酸0.32g、0.9mol·L-1的双氧水1mL和凹凸棒1g加入10ml去离子水中超声充分搅拌,然后将混合溶液转移至水热反应釜中,在160℃下反应8h,用水和无水乙醇充分洗涤之后,在80℃的烘箱中烘干,再经过研磨即可得到CQDs/ATP纳米复合材料。
对所得CQDs/ATP纳米复合材料进行X射线粉末衍射,如图1所示,复合材料的XRD中分别出现了碳量子点、凹凸棒的特征峰,说明碳量子点与凹凸棒成功复合;
利用透射电子显微镜观察CQDs/ATP纳米复合材料的形貌:ATP的TEM图如图2所示,凹凸棒呈现纳米棒状结构;本实施例中所得CQDs/ATP的TEM图如图3所示,碳量子点颗粒均一,粒径小于5nm,均匀地负载在凹凸棒上,与XRD结果一致。
本发明还提供了将上述复合材料用于光催化脱硫的方法:称取二苯并噻吩0.40g溶解于500ml正辛烷中用来制备200ppm的模拟汽油,在光催化反应装置中加入该复合材料和模拟油(质量比1:1000),暗吸附30min后以300W的氙灯作为模拟光源进行照射,滤去420nm以下的紫外光,确保仅有可见光存在,每隔半小时收集一次样品,加入N-N,二甲基甲酰胺萃取上层清液,用紫外荧光定硫仪测定硫含量,脱硫率(%)根据下列公式计算:
D=(1-Ct/C0)*100%
其中:C0为初始溶液的硫含量,Ct为反应t时间后的硫含量。
本实施例制备的CQDs/ATP在3h光照后的脱硫率达到了94%。
对比例1
将0.9mol·L-1的双氧水1mL和凹凸棒1g加入10ml去离子水中超声充分搅拌后,再向其中加入柠檬酸0.32g并分散均匀,然后将混合溶液转移至水热反应釜中,在160℃下反应8h,用水和无水乙醇充分洗涤之后,在80℃的烘箱中烘干,再经过研磨即可得到CQDs/ATP纳米复合材料。
本对比例中所得CQDs/ATP的TEM图如图3所示:碳量子点颗粒粒径明显大于实施例1的产物,且粒径分布均匀度下降。这是由于本对比例中过氧化氢先对凹凸棒发生了改性反应,从而水中的羟基数量大大减少了,在后续的水热反应中不足以控制所生成碳量子点的粒径大小。
光催化脱硫检测如实施例1,对比例1中制备的CQDs/ATP在3h光照后的脱硫率仅达到78%。
实施例2:
称取柠檬酸0.12g、0.9mol·L-1的双氧水0.375mL和凹凸棒1g加入10ml去离子水中超声充分搅拌,然后将混合溶液转移至水热反应釜中,在120℃下反应24h,用水和无水乙醇充分洗涤之后,在80℃的烘箱中烘干,再经过研磨即可得到CQDs/ATP纳米复合材料。后续检测如实施例1。
实施例3:
称取柠檬酸0.21g、0.9mol·L-1的双氧水0.66mL和凹凸棒1g加入10ml去离子水中超声充分搅拌,然后将混合溶液转移至水热反应釜中,在140℃下反应20h,用水和无水乙醇充分洗涤之后,在80℃的烘箱中烘干,再经过研磨即可得到CQDs/ATP纳米复合材料。后续检测如实施例1。
实施例4:
称取柠檬酸0.43g、0.9mol·L-1的双氧水1.34mL和凹凸棒1g加入10ml去离子水中超声充分搅拌,然后将混合溶液转移至水热反应釜中,在180℃下反应6h,用水和无水乙醇充分洗涤之后,在80℃的烘箱中烘干,再经过研磨即可得到CQDs/ATP纳米复合材料。后续检测如实施例1。
Claims (6)
1.一种碳量子点/凹凸棒纳米复合材料,其特征在于:所述的复合材料是以凹凸棒为载体,将凹凸棒与碳量子点复合后得到的纳米复合材料。
2.一种如权利要求1所述的碳量子点/凹凸棒纳米复合材料的制备方法,其特征在于:所述的制备方法为,将柠檬酸、双氧水和凹凸棒混合进行水热反应,再经过离心、洗涤、烘干得到碳量子点/凹凸棒纳米复合材料。
3.如权利要求2所述的碳量子点/凹凸棒纳米复合材料的制备方法,其特征在于:所述的双氧水中过氧化氢的浓度为0.9mol·L-1,控制双氧水中过氧化氢和柠檬酸的摩尔比为0.3~0.6:1。
4.如权利要求2所述的碳量子点/凹凸棒纳米复合材料的制备方法,其特征在于:控制柠檬酸的用量,使碳量子点相对于凹凸棒的质量分数为10%-40%。
5.如权利要求2所述的碳量子点/凹凸棒纳米复合材料的制备方法,其特征在于:水热温度为120-180℃,水热时间为6-24h。
6.一种如权利要求1所述的碳量子点/凹凸棒纳米复合材料的应用,其特征在于:将所述的复合材料用于光催化脱硫。
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CN107661745A (zh) * | 2017-10-20 | 2018-02-06 | 常州大学盱眙凹土研发中心 | 一种凹凸棒石/碳分子筛复合脱硫吸附材料的制备方法 |
CN110882713A (zh) * | 2019-11-22 | 2020-03-17 | 常州纳欧新材料科技有限公司 | 一种导电凹凸棒石/氧化钛/氮化碳量子点复合材料及其制备方法和在光催化脱硫中的应用 |
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CN114854394A (zh) * | 2022-05-25 | 2022-08-05 | 甘肃政法大学 | 一种荧光碳点纳米复合材料的制备及在潜指纹显现中应用 |
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