CN108126684B - 一种花状碳球的制备方法 - Google Patents
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Abstract
本发明涉及一种花状碳球的制备方法，包括：将柠檬酸和尿素溶于溶剂中，转移至水热反应釜中反应，冷却，干燥，超声，离心，分散于溶剂中，离心，得到花状碳球。本发明采用有机小分子化合物柠檬酸和尿素为原料制备花状碳球，制备方法简单快速，经济，可以大量制备，制备得到的花状碳球具有比表面积大的三维花状结构，能够高效地应用于染料废水的光催化脱色，在发展新型碳基催化剂材料中具有重要应用前景。
Description
技术领域
本发明属于碳材料制备领域，特别涉及一种花状碳球的制备方法。
背景技术
近年来碳材料在电池等能源转换材料方面的应用前景备受关注。由于复杂三维形貌结构具有更大的比表面积，因此制备复杂结构的碳材料在催化剂材料应用中尤其备受青睐。目前由有机小分子自组装制备的碳材料结构一般相对简单，多为光滑圆球，也有棒状和片状。而且制备条件一般要求比较苛刻，需要高温高压，甚至需要金属催化剂，这亦导致所得碳材料纯化困难。因此，发展一种简单经济的制备方法来合成具有大比表面积的复杂三维结构碳材料，是一个亟待解决的问题。
发明内容
本发明所要解决的技术问题是提供一种花状碳球的制备方法，该方法简单快速，制备得到的花状碳球具有复杂的三维花状形貌结构，可直接作为光催化剂用于染料废水脱色处理，在发展新型碳基催化剂材料中具有重要应用前景。
本发明的一种花状碳球的制备方法，具体步骤如下：
将柠檬酸和尿素以质量比为1:1-1:3溶于溶剂中，转移至水热反应釜中反应，冷却，干燥，超声，离心，分散于溶剂中，离心，得到花状碳球，其中柠檬酸溶液的浓度为0.05-0.1g/mL。
所述溶剂均为水。
所述反应温度为150-170℃，反应时间为5-7h。
所述干燥为冷冻干燥。
所述超声为依次用乙醇和水超声。
所述花状碳球的直径为500-900nm。
所述花状碳球用于光催化染料废水脱色。
所述光催化染料废水脱色包括：将光催化剂超声分散在染料水溶液中，搅拌下通过氙灯照射，并记录不同光照射时间下溶液的吸光度来评价光催化脱色性能。
所述染料为罗丹明B，浓度为50mg/L。
所述花状碳球的加入量为每10mL染料溶液中加入30mg。
所述光催化染料废水脱色的方法为：将花状碳球超声分散在罗丹明B染料水溶液中，暗吸附30min后，置于氙灯下照射，每间隔1h测量吸光度来测试光催化染料脱色性能，其中花状碳球用量30mg，染料浓度50mg/L。
有益效果
本发明采用有机小分子化合物柠檬酸和尿素为原料制备花状碳球，制备方法简单快速，经济，可以大量制备，制备得到的花状碳球具有比表面积大的三维花状结构，可直接作为光催化剂用于染料废水脱色处理，在发展新型碳基催化剂材料中具有重要应用前景。
附图说明
图1为实施例1中花状碳球的透射电镜图。
图2为实施例2中罗丹明B染料光催化降解曲线图。
具体实施方式
下面结合具体实施例，进一步阐述本发明。应理解，这些实施例仅用于说明本发明而不用于限制本发明的范围。此外应理解，在阅读了本发明讲授的内容之后，本领域技术人员可以对本发明作各种改动或修改，这些等价形式同样落于本申请所附权利要求书所限定的范围。
冷冻干燥机为左乐ZL-10TD，透射电镜为日本电子JEM-2100F。
实施例1
将1g柠檬酸和2g尿素溶于10mL水中，然后将溶液转移至50mL水热反应釜中，并将反应釜置于烘箱中160℃恒温加热反应6h。将反应液冷却至室温并转移至烧杯中，快速冷冻干燥除去溶剂；分别用乙醇和水超声洗涤并离心分离得到固体；再将所得固体超声分散于水中，离心分离得到固体，即得到花状碳球。该花状碳球的直径为500-900nm。
图1表明：花状碳球具有花状形貌结构。
实施例2
以罗丹明B作为典型染料，考察了本发明花状碳球的光催化活性。取30mg实施例1制备的花状碳球，加入到10mL浓度为50mg/L的罗丹明B溶液中，超声振荡10min，置于暗箱中吸附30min后，搅拌下开启于氙灯照射；每隔1h移取一次混合液，离心，取上清液用紫外可见分光光度计测量吸光度，从而计算出罗丹明B的浓度，并通过不同照射时间下染料实际浓度与其初始浓度的比值计算脱色率，另取相同的罗丹明B溶液不加花状碳球做相同的处理作为对照，如图2所示。
图2表明：在有实施例1制备的花状碳球存在下，在3小时内对罗丹明B的脱色率可达90％以上，而无花状碳球存在下则小于5％，说明花状碳球具有良好的光催化活性。
Claims (2)
1.一种花状碳球的制备方法，具体步骤如下：
将1g柠檬酸和2g尿素溶于10mL水中，然后将溶液转移至50mL水热反应釜中，并将反应釜置于烘箱中160℃ 恒温加热反应6h，将反应液冷却至室温并转移至烧杯中，快速冷冻干燥除去溶剂；分别用乙醇和水超声洗涤并离心分离得到固体；再将所得固体超声分散于水中，离心分离得到固体，即得到花状碳球。
2.按照权利要求1所述的一种花状碳球的制备方法，其特征在于，所述花状碳球直接应用于染料废水光催化脱色处理。
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| CN103045242A (zh) * | 2013-01-21 | 2013-04-17 | 吉林大学 | 高荧光量子产率碳点的制备方法 |
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| N掺杂石墨烯量子点的制备及其光催化降解性能;李冬辉 等;《新型炭材料》;20151231;第30卷(第6期);第2.1节,第3.3节 * |
| 荧光氮掺杂碳点的制备及其在Hg2+检测中的应用;张漪;《中国博士学位论文全文数据库 工程科技Ⅰ辑》;20160715(第07期);第2.1.3节 * |
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