CN106215975A - 一步合成碳点/聚1,4‑二苯基丁二炔杂化光催化材料的方法 - Google Patents
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Abstract
本发明公开了一步合成碳点/聚1,4‑二苯基丁二炔杂化光催化材料的方法，该方法中1,4‑二苯基丁二炔分子既充当了形成聚1,4‑二苯基丁二炔的单体，又充当了碳点形成的碳源，通过混合、密封、保温冷却等3个步骤得到导电聚1,4‑二苯基丁二炔与碳点的杂化光催化材料。本发明公开的一步合成碳点/聚1,4‑二苯基丁二炔杂化光催化材料方法无需软模板和引发剂，合成的聚1,4‑二苯基丁二炔与碳点的杂化结构具有更优异的可见光吸收能力及更优异的光催化性能；且无复杂的提纯过程，合成方法更加简单易于控制，有利于工业大规模生产。
Description
技术领域
本发明属于纳米材料技术领域，具体涉及一种一步合成碳点/聚1,4-二苯基丁二炔杂化光催化材料的方法。
背景技术
碳点是一类新型零维碳纳米材料，除了碳元素外，它还常含有氢、氧、氮元素。它不仅具有类似传统半导体量子点的诸多优异特性，还能够作为电子给体和受体与其它纳米结构或材料杂化，从而提升材料的综合性能。一类制备碳点的有效方法是利用有机分子碳化过程来实现的，即在合适的温度下，有机分子中的氢与分子中或者外界提供的氧反应形成水，原分子结构被破坏发生重结晶的过程。
导电聚合物是指通过掺杂等手段，使得电导率在半导体和导体范围内的聚合物，这一类聚合物主链上含有交替的单键和双键，从而形成了大的共轭π体系，π电子的流动产生了导电的可能性。聚合物聚1,4-二苯基丁二炔是导电聚合物的一种，通常由单体1,4-二苯基丁二炔在引发剂安息香甲醚存在的情况下，使用软模板法在紫外光照下发生聚合反应而形成。聚1,4-二苯基丁二炔在可见光照射下能够产生大量的光生电子和空穴，氧化还原有机物，其在光催化降解有机染料方面具有十分优异的效果。然而该方法制备条件苛刻，产物产量十分低，且仅能够在实验室操作，无法工业大规模生产，使其成为当今科学界一难以克服的问题。
发明内容
本发明的目的旨在解决现有聚1,4-二苯基丁二炔难以量产等难题，提供一种一步合成碳点/聚1,4-二苯基丁二炔杂化光催化材料的方法。该方法合成的聚1,4-二苯基丁二炔与碳点的杂化结构表现出了更优异的可见光吸收能力及更优异的光催化性能；同时，与现有合成单一导电聚1,4-二苯基丁二炔的方法相比，本发明所提供的一步合成导电聚1,4-二苯基丁二炔与碳点杂化的方法更简单易于控制，且无复杂的提纯过程，更有利于工业大规模生产。
为解决上述技术问题，本发明采用的技术方案是：
一步合成碳点/聚1,4-二苯基丁二炔杂化光催化材料的方法，采用以下步骤：
(1)将1,4-二苯基丁二炔固体粉均匀分散到水热反应釜内衬罐底部，使其厚度为2～7mm；
(2)把装好1,4-二苯基丁二炔固体粉的内衬罐放入钢罐后抽真空，使内部压力小于0.1个大气压，然后充入氧气与氮气的混合气体至1个大气压，最后密封，其中，氧气与氮气的体积比为2～3；
(3)把密封好的反应釜放入鼓风烘箱，在95～135℃下保温50～150min，然后冷却至室温，即可得到导电聚1,4-二苯基丁二炔与碳点的杂化光催化材料。
本发明提出了一种一步合成聚1,4-二苯基丁二炔与碳点的杂化光催化材料的方法，与现有技术相比，无需软模板和引发剂，合成的聚1,4-二苯基丁二炔与碳点的杂化结构具有更优异的可见光吸收能力及更优异的光催化性能；且无复杂的提纯过程，合成方法更加简单易于控制，有利于工业大规模生产。
附图说明
图1为聚1,4-二苯基丁二炔与碳点杂化光催化材料的扫描电镜照片。
图2为聚1,4-二苯基丁二炔与碳点杂化光催化材料的透射电镜照片。
图3为聚1,4-二苯基丁二炔及其与碳点杂化光催化材料的紫外-可见吸收光谱。
图4为在可见光照射下，聚1,4-二苯基丁二炔与碳点杂化光催化材料降解亚甲基蓝染料效率随光照时间的对应关系。
具体实施方式
以下结合附图和实施例对本发明作进一步的详细描述：
一步合成碳点/聚1,4-二苯基丁二炔杂化光催化材料的方法，采用以下步骤：
(1)将1,4-二苯基丁二炔固体粉均匀分散到水热反应釜内衬罐底部，使其厚度为2～7mm；
(2)把装好1,4-二苯基丁二炔固体粉的内衬罐放入钢罐后抽真空，使内部压力小于0.1个大气压，然后充入氧气与氮气的混合气体至1个大气压，最后密封，其中，氧气与氮气的体积比为2～3；
(3)把密封好的反应釜放入鼓风烘箱，在95～135℃下保温50～150min，然后冷却至室温，即可得到导电聚1,4-二苯基丁二炔与碳点的杂化光催化材料。
本发明中1,4-二苯基丁二炔分子既充当了形成聚1,4-二苯基丁二炔的单体，又充当了碳点形成的碳源，单体1,4-二苯基丁二炔在热引发下，发生聚合反应形成聚1,4-二苯基丁二炔的同时，反应釜内的有机物作为碳源，碳化脱氢制备得到了碳点，使得碳点与聚1,4-二苯基丁二炔杂化在了一起。
实施例1
一步合成碳点/聚1,4-二苯基丁二炔杂化光催化材料的方法，采用以下步骤：
(1)取1克1,4-二苯基丁二炔固体粉，将其均匀分散到具有250毫升的水热反应釜内衬罐底部，且厚度为3mm；
(2)把装好1,4-二苯基丁二炔固体粉的内衬罐放入钢罐后抽真空，使内部压力小于0.1个大气压，然后充入氧气与氮气的混合气体至1个大气压，最后密封，其中，氧气与氮气的体积比为2；
(3)把密封好的反应釜放入鼓风烘箱，在95℃下保温50min，然后冷却至室温，即可得到导电聚1,4-二苯基丁二炔与碳点的杂化光催化材料。
对合成的碳点/聚1,4-二苯基丁二炔杂化光催化材料进行了性能测试及表征。图1为聚1,4-二苯基丁二炔与碳点杂化光催化材料的扫描电镜照片；图2为聚1,4-二苯基丁二炔与碳点杂化光催化材料的透射电镜照片，表明碳点颗粒分散在了无定型聚1,4-二苯基丁二炔结构中，获得了杂化结构；图3为聚1,4-二苯基丁二炔及其与碳点杂化光催化材料的紫外-可见吸收光谱，表明聚1,4-二苯基丁二炔与碳点杂化光催化材料的可见光吸收能力优于单一的聚1,4-二苯基丁二炔光催化材料；图4为在可见光照射下，聚1,4-二苯基丁二炔与碳点杂化光催化材料降解亚甲基蓝染料效率随光照时间的对应关系，表明聚1,4-二苯基丁二炔与碳点杂化光催化材料光降解染料的效率高于S.Ghosh等人提出的现有方法制备的单一聚1,4-二苯基丁二炔光解效率。
实施例2
一步合成碳点/聚1,4-二苯基丁二炔杂化光催化材料的方法，采用以下步骤：
(1)取1.5克1,4-二苯基丁二炔固体粉，将其均匀分散到具有250毫升的水热反应釜内衬罐底部，厚度为5mm；
(2)把装好1,4-二苯基丁二炔固体粉的内衬罐放入钢罐后抽真空，使内部压力小于0.1个大气压，然后充入氧气与氮气的混合气体至1个大气压，最后密封，其中，氧气与氮气的体积比为3；
(3)把密封好的反应釜放入鼓风烘箱，在135℃下保温150min，然后冷却至室温，即可得到导电聚1,4-二苯基丁二炔与碳点的杂化光催化材料。
实施例3
一步合成碳点/聚1,4-二苯基丁二炔杂化光催化材料的方法，采用以下步骤：
(1)取2克1,4-二苯基丁二炔固体粉，将其均匀分散到具有250毫升的水热反应釜内衬罐底部，厚度为7mm；
(2)把装好1,4-二苯基丁二炔固体粉的内衬罐放入钢罐后抽真空，使内部压力小于0.1个大气压，然后充入氧气与氮气的混合气体至1个大气压，最后密封，其中，氧气与氮气的体积比为2；
(3)把密封好的反应釜放入鼓风烘箱，在120℃下保温100min，然后冷却至室温，即可得到导电聚1,4-二苯基丁二炔与碳点的杂化光催化材料。
Claims (1)
1.一步合成碳点/聚1,4-二苯基丁二炔杂化光催化材料的方法，其特征在于：采用以下步骤：
(1)取1～2克1,4-二苯基丁二炔固体粉，将其均匀分散到具有250毫升的水热反应釜内衬罐底部，且厚度为2～7mm；
(2)把装好1,4-二苯基丁二炔固体粉的内衬罐放入钢罐后抽真空，使内部压力小于0.1个大气压，然后充入氧气与氮气的混合气体至1个大气压，最后密封，其中，氧气与氮气的体积比为2～3；
(3)把密封好的反应釜放入鼓风烘箱，在95～135℃下保温50～150min，然后冷却至室温，即可得到导电聚1,4-二苯基丁二炔与碳点的杂化光催化材料。
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