CN107099287B - 一种用作可见光催化光敏剂碳量子点的水热制备方法 - Google Patents
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Abstract
一种用作可见光催化光敏剂碳量子点的水热制备方法，其特征在于：以落叶松为原料，经高温高压水热法处理后，离心过滤除去深棕色固体产物，得到浅黄色液体产物，将液体产物高速离心，控制离心转速和时间，除去不溶小颗粒杂质，用一定分子量的透析袋透析除去未反应糖，盐分等，后经浓缩得到目标产物‑水溶性荧光碳量子点。将其与TiO2复合制备光催化复合体系，以抗生素为模型物，考察复合体系对模型物的光催化降解性能，碳点作为光敏剂的作用效率。本操作工艺的主要特点为利用黑龙江省资源丰富的落叶松为原料，环保廉价易得，水热反应低温低压，无需添加酸碱盐等钝化剂，产物为水溶性的且具有一定荧光效应，反应过程操作简单，成本低廉。
Description
所属技术领域：
本发明涉及纳米材料制备领域，特别是涉及一种用作可见光催化光敏剂碳量子点的水热制备方法
背景技术：
抗生素类药品广泛用于医疗处置、医疗用药及农业领域，但通常情况下人类及动物对抗生素的吸收能力很低，50％～80％的抗生素最终被排除冰进入水生环境，引起土壤毒性、耐抗生素病原体产生等威胁人类身体健康的情况发生。四环素是全球使用量第二大的抗生素，目前为止对于四环素的去除仍然缺乏有效、全面、系统的技术支持。相比于传统的吸附、微生物降解法，光催化降解能有效去除水相溶液中的大分子有机组分，将其降解成小分子，抑制毒性及进一步在水溶液中的传播。
炭量子点的制备和应用引起学者们的广泛关注，量子效应能赋予炭点独特的性质，尺寸限域进一步引起小尺寸效应、宏观的量子隧道效应及表面效应，表现出不同于大尺寸颗粒的物理化学性质，广泛的用作金属探针，生物标记，光传感器等方面。炭量子点是一类由碳元素构成的纳米尺寸的粒子，由SP2杂化和不饱和SP3杂化碳原子组成的共轭体系。表面丰富的官能团易于与半导体催化剂复合，拓展半导体催化剂对光的响应范围，制备的复合体系催化剂能有效响应可将光照射，拓展了其使用价值。
公开号为CN103011126的中国专利介绍了水溶性荧光炭量子点制备工艺，该法将葡萄糖与丙二酸二已酯混合，140-160℃回流后冷却至室温，产物100-120℃真空干燥2h后溶于蒸馏水中，经离心分离冷冻干燥后得到目标荧光碳点，产物粒径2～4nm，荧光效率达24％。此法虽提高了量子效率，但反应中应用有机溶剂，且过程较繁琐。
公开号为CN103480353A的中国专利介绍了一种用水热法合成碳量子点溶液制备复合纳米光催化剂的方法，该法将以维生素C作为碳源，无水乙醇和去离子水混合液为溶剂，水热反应后向产物中加入二氯甲烷，萃取上清液透析后得到目标产物，将其与溶胶凝胶法制备的TiO2复合得到复合纳米光催化剂，本法操作简单，成本低，但反应产物的萃取剂为有机试剂且对产率影响较大。
公开号为CN104201357的中国专利介绍了一种石墨烯量子点-石墨烯复合材料及其制备方法与用途。将卤代苯、碱金属单质和取代芳烃化合物放入高压密闭的反应釜中搅拌反应，后离心分离得到干燥样品，惰性气体保护下高温处理得到石墨烯量子点-石墨烯复合材料，有优异的电化学性能，反应中三种原料的配比对材料的性质有较大影响，反应条件要求高。
公开号为CN102127431的中国专利介绍了碳量子点的制法及应用该量子点制备光催化剂的方法，该法将乙醇与蒸馏水按一定体积比混合后加入无机强碱得到电解液放入电解槽，以石墨碳棒作为电极，在10～200mA/cm2的电流密度下进行电化学反应2～4h，最后加入干燥剂，通过柱层析分离得到碳量子点，该法进行两步操作，一次电解一次柱层析分离，反应复杂且对仪器损害较大。
综上所述，传统的燃烧，电解，冷冻干燥，超声等制备碳点的方法高损耗，反应复杂，需强酸碱等钝化剂，有些虽然性能优异，但缺乏相关实际应用方面的指导。本专利提出以水热法制备荧光碳纳米粒子，反应以水为溶剂，条件温和，设备操作简单，将其与TiO2复合，能作为光敏剂，能将TiO2光响应范围有效拓展至可见光范围，对抗生素有优异的光催化降解性能。
发明内容：
本发明的目的在于提供一种用作可见光催化光敏剂碳量子点的水热制备方法。
为了达到上述目的，本发明采用的技术方案包括：一种用作可见光催化光敏剂碳量子点的水热制备方法，其特征在于：以落叶松为原料，经高温高压水热法处理后，离心过滤除去深棕色固体产物，得到浅黄色液体产物，将液体产物高速离心，控制离心转速和时间，除去不溶小颗粒杂质，用一定分子量的透析袋透析除去未反应糖，盐分等，后经浓缩得到目标产物-水溶性荧光碳量子点。将其与TiO2复合制备光催化复合体系，以抗生素为模型物，考察复合体系对模型物的光催化降解性能，碳点作为光敏剂的作用效率。本操作工艺的主要特点为利用黑龙江省资源丰富的落叶松为原料，环保廉价易得，水热反应低温低压，无需添加酸碱盐等钝化剂，产物为水溶性的且具有一定荧光效应，反应过程操作简单，成本低廉。
本发明的优点是：
1、以资源丰富的落叶松为反应原料，充分利用天然生物质，原料丰富廉价易得，含有丰富的纤维素、半纤维素及木质素，原料环保天然无污染，经水热处理后炭化率较高。
2、本发明克服了现有技术中的不足，改变了传统的生产工艺，使用水热反应，以水为溶剂，原料不需预处理，反应过程操作简单，生产成本低，得率高。
3、本发明制备的液体产物为水溶性，且具有良好的荧光效应，可以有效作为光催化复合体系的光敏剂。
4、本发明反应中不添加酸碱盐等钝化剂，无需额外处理，产物为水溶性，表现出对PH的敏感性，以硫酸奎宁做标准物质为参比，量子效率可达22％。
附图说明：
图1为本发明实施例1制备得到的碳纳米粒子的透射电镜(TEM)照片；
图2为本发明实施例1制备得到的碳纳米粒子水溶液在紫外光(365nm)照射下的吸收曲线和照片；
图3为本发明实施例1制备得到的碳纳米粒子水溶液在荧光照射下的发射和激发光谱；
图4为本发明实施例1制备得到的碳纳米粒子水溶液在不同激发波长下得到的发射光谱。
具体实施方式：
下面对本发明实施作进一步详细描述：
一种用作可见光催化光敏剂碳量子点的水热制备方法，其特征在于：以落叶松为原料，经高温高压水热法处理后，离心过滤除去深棕色固体产物，得到浅黄色液体产物，将液体产物高速离心，控制离心转速和时间，除去不溶小颗粒杂质，用一定分子量的透析袋透析除去未反应糖，盐分等，后经浓缩得到目标产物-水溶性荧光碳量子点。将其与TiO2复合制备光催化复合体系，以抗生素为模型物，考察复合体系对模型物的光催化降解性能，碳点作为光敏剂的作用效率。
下面，本发明将用实施例进行进一步的说明，但是它并不限于这些实施例的任一个或类似实例。
实施例1：
购买商品落叶松木粉，选取40-60目木粉，称取10g，放入容积500ml的聚四氟乙烯反应釜中，放入一定体积的水作为溶剂，保证溶液体积与釜容积为7:10，10℃/min升温速率升温至目标温度260℃，恒温9.5h，冷却降至室温，过滤，收集得到的淡黄色液体，以12000r/min的转速离心分离20分钟，去除小颗粒沉淀物，液体用截留量1500的透析袋透析3天，除去未反应糖，盐分等，浓缩后即得水溶性荧光碳量子点，平均粒径为6.5nm。其紫外吸收光谱图、TEM图，荧光发射光谱图分别如图1-图4所示。
将其与溶胶凝胶法制备的TiO2复合制备光催化复合体系，以四环素为目标模型物，可见光照射下3h该复合体系对四环素的降解效率达到93.8％。
实施例2：
购买商品落叶松木粉，选取40-60目木粉，称取8g，放入容积500ml的聚四氟乙烯反应釜中，放入一定体积的水作为溶剂，保证溶液体积与釜容积为9:10，10℃/min升温速率升温至目标温度230℃，恒温12h，冷却降至室温，过滤，收集得到的淡黄色液体，以11000r/min的转速离心分离15分钟，去除小颗粒沉淀物，液体用截留量1000的透析袋透析3天，除去未反应糖，盐分等，浓缩后即得水溶性荧光碳量子点，平均粒径为38.2nm。
将其与溶胶凝胶法制备的TiO2复合制备光催化复合体系，以四环素为目标模型物，可见光照射下3h该复合体系对四环素的降解效率达到91.3％。
Claims (2)
1.一种用作可见光催化光敏剂碳量子点的水热制备方法，其特征在于：以落叶松为原料，经高温高压水热法处理后，离心过滤除去深棕色固体产物，得到浅黄色液体产物，将液体产物高速离心，控制离心转速和时间，除去不溶小颗粒杂质，用一定分子量的透析袋透析除去未反应糖，盐分等，后经浓缩得到目标产物-水溶性荧光碳量子点， 将其与TiO2复合制备光催化复合体系，以抗生素为模型物，考察复合体系对模型物的光催化降解性能，碳点作为光敏剂的作用效率；
水热反应原料浓度为1％～15％，溶剂容量与反应釜容量比为3:5～9:10，水热反应温度在210～260℃，反应时间8～12小时，所述的液体产物离心速率为6000-13000rpm，离心时间为15-30min，透析袋的分子截流量为1000-5000，所述的水溶性碳纳米点粒径分布为5～45nm，所述的光催化复合体系中碳点与TiO2比为1:10～1:1。
2.按照权利要求1所述的一种用作可见光催化光敏剂碳量子点的水热制备方法，其特征在于：所述的光催化复合体系对抗生素类模型物的降解效率达到90～95％。
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