CN114700101B - 一种具有高可见光催化活性的富缺陷g-C3N4纳米材料的制备方法 - Google Patents
一种具有高可见光催化活性的富缺陷g-C3N4纳米材料的制备方法 Download PDFInfo
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Abstract
本发明公布了一种具有高可见光催化活性的富缺陷g‑C3N4纳米材料的制备方法。首先采用物理搅拌混合制备了富氮前驱体溶液,然后经低温处理、引入碳酸氢铵制得富氮前驱体碱混合液;再经冷冻干燥、热缩聚反应制得具有高可见光催化活性的富缺陷g‑C3N4纳米材料。本发明充分利用铵盐碱蚀和内源性气体热剥离作用,使g‑C3N4被原位剥离和造孔,有效解决了体相g‑C3N4片层易堆积、比表面积小、活性位暴露不足的问题;本发明易操控,适合于工业批量生产,在处理有机污染物领域具有良好的应用前景。
Description
技术领域
本发明属于光催化材料制备领域,具体涉及一种具有高可见光催化活性的富缺陷g-C3N4纳米材料的制备方法。
背景技术
近年来,随着工业的飞速发展,有机污染问题也日益突出。光催化降解有机物从而解决有机污染物问题作为一种绿色的方法被广泛研究,以期未来投入广泛应用。到目前为止,已有大量半导体材料被证明可作为光催化剂用于降解有机污染物。而石墨相氮化碳(g-C3N4)作为一种具有可见光响应的材料,因其无毒、优异的化学稳定性和独特的电子能带结构而成为极具前景的光催化剂。但是,受限于g-C3N4的固有缺陷如聚合产物为密实块体物质、比表面积低、光致电荷复合高,极大地限制了其光催化应用性能。为了解决这些问题,目前研究多采用构建特定的纳米结构,元素掺杂和半导体复合异质结等,用于提高g-C3N4的光催化活性。
中国专利《一种石墨相氮化碳-硫化镉复合光催化剂的制备方法》(授权公告号:CN113134382A)利用硬模板法,制备出负载有石墨相氮化碳的二氧化钛-石墨相氮化碳复合微球,再使氯化镉与二甲基亚砜生成的硫化镉纳米颗粒生长在复合微球上,最后利用碱液消除复合微球中的二氧化钛微球,从而制备得到石墨相氮化碳-硫化镉异质结复合光催化剂。中国专利《磷掺杂氮化碳/氮化碳同型异质结光催化剂及其制备方法和应用》(授权公告号:CN108380233B)提供了一种磷掺杂氮化碳/氮化碳同型异质结光催化剂,以磷杂原子为修饰剂,改变氮化碳原有的能带结构,形成与氮化碳导带与价带位置不同的磷掺杂氮化碳。进而利用磷掺杂氮化碳与原始氮化碳结合,形成磷掺杂氮化碳/氮化碳同型异质结光催化剂。虽然构建异质结构、元素掺杂的方法能够提高氮化碳的光催化效果,但外来物质与氮化碳在理化性质上往往存在明显的差异,这可能会极大地影响所得异质结的相容性、均匀性和稳定性,也削弱了无金属氮化碳的固有优势。
发明内容
本发明的目的在于提供一种具有高可见光催化活性的富缺陷g-C3N4纳米材料的方法。该方法通过在过饱和富氮前驱体水溶液体系中引入碳酸氢铵,以及采用冷冻手段使体系中的分子和原子充分键合(包括分子间作用力),在调控热缩聚过程中热触发产生内源性气体(H2O、NH3和CO2),同时伴有碱蚀作用,从而在原子级对体相g-C3N4制造缺陷位、原位剥离和造孔,最后通过急冷方式保持其富缺陷结构,实现了一步热法原位制备富缺陷g-C3N4纳米材料。本发明解决了以往g-C3N4比表面积小、片层易堆积等问题,极大提高了其光催化性能。所制备富缺陷g-C3N4纳米材料片层剥离程度高,片层孔隙度高,比表面积大,缺陷丰富,对罗丹明B、甲基橙、靛蓝有机物具有高可见光催化降解能力。
具体步骤如下:
(1)按照1~2:1质量比称量富氮前驱体和去离子水,在室温下充分搅拌混合20~30min,获得富氮前驱体溶液。所述富氮前驱体是指尿素、双缩脲、三聚氰胺的一种或几种。
(2)将步骤(1)获得的富氮前驱体溶液置于2~5℃低温处理20~30min,获得富氮前驱体过饱和溶液。
(3)按照碳酸氢铵与富氮前驱体质量比为1.6~2.4:100称量碳酸氢铵,然后将其与步骤(2)获得的富氮前驱体过饱和溶液混合,获得富氮前驱体碱混合液。
(4)将步骤(3)获得的富氮前驱体碱混合液于-40℃冷冻干燥2~3h,然后将其转移至带盖坩埚并置于马弗炉中,于550~580℃条件下保温2~5h。反应结束后立即取出并加入去离子水冷却至室温,经离心洗涤后,于70℃干燥24h,制得富缺陷g-C3N4纳米材料。
附图说明
图1为本发明实施例1制得的富缺陷g-C3N4纳米材料的扫描电子显微镜图。
图2为本发明实施例1制得的富缺陷g-C3N4纳米材料光催化降解罗丹明B有机溶液后,不同时间下有机溶液的紫外吸收光谱图。
具体实施方式
下面的实施例将进一步说明本发明,但对本发明没有限制。
实施例1:
(1)称取20g尿素,加入坩埚中,量取20mL去离子水作为分散剂。在室温下充分搅拌混合20min,获得充分溶解的尿素水溶液。
(2)将步骤(1)获得的尿素溶液置于2℃低温冷藏20min,使尿素低温下形成过饱和溶液。
(3)称取0.316g碳酸氢铵,加入步骤(2)获得的过饱和尿素溶液,充分溶解混合,获得尿素碱混合液。
(4)将步骤(3)获得的尿素碱混合液于-40℃冷冻干燥2h,然后将其转移至带盖坩埚并置于马弗炉中,于550℃条件下保温2h。反应结束后立即取出并加入去离子水冷却至室温,经离心洗涤后,于70℃干燥24h,制得富缺陷g-C3N4纳米材料。
经扫描电子显微镜观察发现该富缺陷g-C3N4纳米材料片层剥离程度高,孔隙丰富,比表面积达45.5m2/g。
称取10mg的上述g-C3N4,添加到50mL、浓度为50mg/L的罗丹明B(RhB)模拟有机污染物溶液中,在暗处磁力搅拌30min达到动态吸附平衡。然后在可见光(λ≥400nm)(300W氙灯)下光催化反应45min,结果显示其对RhB的去除率达99%;同理分别以甲基橙、靛蓝为目标污染物,其降解率分别为94%和86%。
实施例2:
(1)称取20g尿素,加入坩埚中,量取10mL去离子水作为分散剂。在室温下充分搅拌混合30min,获得充分溶解的尿素水溶液。
(2)将步骤(1)获得的尿素溶液置于5℃低温冷藏30min,使尿素低温下形成过饱和溶液。
(3)称取0.474g碳酸氢铵,加入步骤(2)获得的过饱和尿素溶液,充分溶解混合,获得尿素碱混合液。
(4)将步骤(3)获得的尿素碱混合液于-40℃冷冻干燥3h,然后将其转移至带盖坩埚并置于马弗炉中,于580℃条件下保温5h。反应结束后立即取出并加入去离子水冷却至室温,经离心洗涤后,于70℃干燥24h,制得富缺陷g-C3N4纳米材料。
经扫描电子显微镜观察发现该富缺陷g-C3N4纳米材料片层剥离程度高,孔隙丰富,比表面积达41.6m2/g。
参照实施例1评价光催化性能的方法,结果显示所制备的纳米材料对RhB、甲基橙、靛蓝的去除率分别为96%、91%和81%。
实施例3
(1)称取20g双缩脲,加入坩埚中,量取18mL去离子水作为分散剂。在室温下充分搅拌混合30min,获得充分溶解的双缩脲水溶液。
(2)将步骤(1)获得的双缩脲溶液置于4℃低温冷藏25min,使双缩脲低温下形成过饱和溶液。
(3)称取0.350g碳酸氢铵,加入步骤(2)获得的过饱和双缩脲溶液,充分溶解混合,获得双缩脲碱混合液。
(4)将步骤(3)获得的双缩脲碱混合液于-40℃冷冻干燥2h,然后将其转移至带盖坩埚并置于马弗炉中,于560℃条件下保温2h。反应结束后立即取出并加入去离子水冷却至室温,经离心洗涤后,于70℃干燥24h,制得富缺陷g-C3N4纳米材料。
经扫描电子显微镜观察发现该富缺陷g-C3N4纳米材料片层剥离程度高,孔隙丰富,比表面积达37.9m2/g。
参照实施例1评价光催化性能的方法,结果显示所制备的纳米材料对RhB、甲基橙、靛蓝的去除率分别为92%、87%和76%。
Claims (2)
1.一种具有高可见光催化活性的富缺陷g-C3N4纳米材料的制备方法,其特征在于具体步骤为:
(1)按照1~2:1质量比称量富氮前驱体和去离子水,在室温下充分搅拌混合20~30min,获得富氮前驱体溶液;所述富氮前驱体是指尿素、双缩脲、三聚氰胺的一种或几种;
(2)将步骤(1)获得的富氮前驱体溶液置于2~5℃低温处理20~30min,获得富氮前驱体过饱和溶液;
(3)按照碳酸氢铵与富氮前驱体质量比为1.6~2.4:100称量碳酸氢铵,然后将其与步骤(2)获得的富氮前驱体过饱和溶液混合,获得富氮前驱体碱混合液;
(4)将步骤(3)获得的富氮前驱体碱混合液于-40℃冷冻干燥2~3h,然后将其转移至带盖坩埚并置于马弗炉中,于550~580℃条件下保温2~5h;反应结束后立即取出并加入去离子水冷却至室温,经离心洗涤后,于70℃干燥24h,制得富缺陷g-C3N4纳米材料。
2.根据权利要求1所述的一种具有高可见光催化活性的富缺陷g-C3N4纳米材料的制备方法,其特征在于:所制备富缺陷g-C3N4纳米材料可用于提高对罗丹明B、甲基橙、靛蓝有机物的可见光催化降解能力。
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Citations (7)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
WO2011049085A1 (ja) * | 2009-10-20 | 2011-04-28 | 独立行政法人産業技術総合研究所 | 窒化炭素を含む光触媒及びその製造方法並びに該光触媒を用いた空気浄化方法 |
CN105126893A (zh) * | 2015-08-31 | 2015-12-09 | 中国科学院过程工程研究所 | 一种石墨相氮化碳材料、其制备方法和用途 |
CN110479350A (zh) * | 2019-09-12 | 2019-11-22 | 哈尔滨工业大学 | 一种薄层多孔氮化碳光催化剂的制备方法 |
CN110975917A (zh) * | 2019-12-11 | 2020-04-10 | 中南林业科技大学 | 一种缺陷态氮化碳材料及其制备方法与用途 |
CN112058298A (zh) * | 2020-09-03 | 2020-12-11 | 上海工程技术大学 | 一种高浓度碱溶液改性氮化碳的制备方法 |
CN113731464A (zh) * | 2021-08-20 | 2021-12-03 | 山东大学 | 一种含氮空位氮化碳光催化剂及其制备方法和应用 |
CN114130387A (zh) * | 2021-11-26 | 2022-03-04 | 合肥智慧环境研究院 | 一种氮缺陷g-C3N4表面掺杂纳米锰催化剂及其制备方法和应用 |
-
2022
- 2022-04-02 CN CN202210357502.4A patent/CN114700101B/zh active Active
Patent Citations (7)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
WO2011049085A1 (ja) * | 2009-10-20 | 2011-04-28 | 独立行政法人産業技術総合研究所 | 窒化炭素を含む光触媒及びその製造方法並びに該光触媒を用いた空気浄化方法 |
CN105126893A (zh) * | 2015-08-31 | 2015-12-09 | 中国科学院过程工程研究所 | 一种石墨相氮化碳材料、其制备方法和用途 |
CN110479350A (zh) * | 2019-09-12 | 2019-11-22 | 哈尔滨工业大学 | 一种薄层多孔氮化碳光催化剂的制备方法 |
CN110975917A (zh) * | 2019-12-11 | 2020-04-10 | 中南林业科技大学 | 一种缺陷态氮化碳材料及其制备方法与用途 |
CN112058298A (zh) * | 2020-09-03 | 2020-12-11 | 上海工程技术大学 | 一种高浓度碱溶液改性氮化碳的制备方法 |
CN113731464A (zh) * | 2021-08-20 | 2021-12-03 | 山东大学 | 一种含氮空位氮化碳光催化剂及其制备方法和应用 |
CN114130387A (zh) * | 2021-11-26 | 2022-03-04 | 合肥智慧环境研究院 | 一种氮缺陷g-C3N4表面掺杂纳米锰催化剂及其制备方法和应用 |
Non-Patent Citations (1)
Title |
---|
Metal-free carbon nitride with boosting photo-redox ability realized by the controlled carbon dopants;Zhihao Li et al.;《Chemical Engineering Journal》;第382卷;文献码122657 * |
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