CN106732711B - 一种氮化碳和铁酸镧复合光催化材料及其制备方法 - Google Patents
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
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- B01J23/70—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper
- B01J23/76—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper combined with metals, oxides or hydroxides provided for in groups B01J23/02 - B01J23/36
- B01J23/83—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper combined with metals, oxides or hydroxides provided for in groups B01J23/02 - B01J23/36 with rare earths or actinides
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- B01J35/39—
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- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/30—Treatment of water, waste water, or sewage by irradiation
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
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- C02F2101/34—Organic compounds containing oxygen
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
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- C02F2101/38—Organic compounds containing nitrogen
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- C—CHEMISTRY; METALLURGY
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- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2305/00—Use of specific compounds during water treatment
- C02F2305/10—Photocatalysts
Abstract
本发明提供一种氮化碳和铁酸镧复合光催化材料及其制备方法，该复合材料中，氮化碳与铁酸镧的质量比为100:1～100:80。制备步骤为：先制备g‑C3N4，而后，称取g‑C3N4粉末，加硝酸铁和硝酸镧，研磨使之充分混合均匀，g‑C3N4粉末、硝酸铁、硝酸镧的质量比为400:6.8:7.2～400：544：576；置于马弗炉中升温至350～550℃煅烧处理1～3h，得到氮化碳和铁酸镧复合光催化材料。以解决现有光催化剂制备方法复杂，对设备要求高，且稳定性及催化活性较为一般的问题。本发明属于半导体光催化制备领域。
Description
技术领域
本发明属于半导体光催化制备领域，具体涉及一种氮化碳/铁酸镧复合光催化材料的制备方法。
背景技术
氮化碳是一种新型可见光响应的非金属光催化剂。主要由碳和氮组成，是一种有机聚合物。理论计算表明，石墨相氮化碳(g-C3N4)在室温下最为稳定，具有半导体特性。g-C3N4是由三-s-三嗪通过叔胺氮相连形成的二维片状结构。与传统的金属催化剂相比，石墨型氮化碳具有稳定性高、耐酸碱和便于改性等优点，在催化领域有广阔的应用前景。已发现g-C3N4可以催化Friedel-Crafts反应、CO2的活化反应、烯烃和腈的环化反应等一些重要的有机反应。尽管对g-C3N4光催化剂的研究已取得较大进展，但还有很多问题亟待解决。如比表面积小、对可见光响应范围窄、光生电子-空穴对快速复合、光量子效率低等缺陷，所以其光催化效率很低。单纯的g-C3N4常与金属氧化物、金属磷化物等半导体复合形成异质结，能有效促进光生电子和空穴的分离，抑制电子-空穴的复合，提高光催化效率。
铁酸镧(LaFeO3)具有稳定的晶体结构、独特的电磁、催化和气敏性等特点，在电学、磁学和传感器等领域都有着广泛的应用前景。铁酸镧属p型稀土复合半导体金属氧化物，具有钙钛矿结构，其带隙较窄，具备可见光响应等优点，因此在光催化领域具有传统TiO2无法比拟的优势，展现出良好的可见光催化性能。
发明内容
本发明的目的在于：提供一种氮化碳和铁酸镧复合光催化材料及其制备方法，得到的复合光催化剂稳定性好、光催化活性高，制备方法简单易行，设备要求低，以解决现有光催化剂制备方法复杂，对设备要求高，且稳定性及催化活性较为一般的问题。
为解决上述问题，提供一种氮化碳和铁酸镧复合光催化材料，该复合材料中，氮化碳与铁酸镧的质量比为100:1～100:80。
优选地，氮化碳与铁酸镧的质量比为100:2～100:40；
其制备步骤如下：
步骤一，制备g-C3N4，称取三聚氰胺并放于半封闭的坩埚中，置于马弗炉中程序升温至550℃煅烧2小时，冷却至室温，研钵研磨成粉末；
步骤二，称取g-C3N4粉末，加硝酸铁和硝酸镧，研磨使之充分混合均匀，g-C3N4粉末、硝酸铁、硝酸镧的质量比为400:6.8:7.2～400：544：576；
步骤三，g-C3N4粉末、硝酸铁和硝酸镧于马弗炉中升温至350～550℃煅烧处理1～3h，得到氮化碳和铁酸镧复合光催化材料。
优选地，所制得复合光催化材料中，氮化碳与铁酸镧的质量比为100:2～100:40；
优选地，步骤二中，加入的硝酸铁和硝酸镧的摩尔比为1:1；
优选地，步骤二中的研磨时间为30min。
与现有技术相比，本发明将g-C3N4与铁酸镧复合形成异质结构，所得光催化剂稳定性好、光催化活性高，制备方法简单易行，设备要求低，具有很好的应用前景。
附图说明
图1是所制备质量比为5％的氮化碳/铁酸镧复合光催化材料，在300W氙灯照射下光降解亚甲基蓝光谱图。；
图2是所制备不同质量比的氮化碳/铁酸镧复合光催化材料，在3W LED灯照射下光降解亚甲基蓝光谱图。
具体实施方式
为使本发明的目的、技术方案和优点更加清楚，下面将对本发明作进一步地详细描述，
实施例1：
本实施例提供一种氮化碳和铁酸镧复合光催化材料，该复合材料中，氮化碳与铁酸镧的质量比为20:1。
同时提供一种氮化碳和铁酸镧复合光催化材料的制备方法：
1.石墨相氮化碳(g-C3N4)制备，称取10.00g三聚氰胺于半封闭的坩埚中，马弗炉中以5℃min-1的速度程序升温至550℃，于550℃煅烧2小时，冷却至室温，研钵研磨成粉末。
2.称取g-C3N4粉末4.00g、硝酸铁0.34g和硝酸镧0.36g，马弗炉中以5℃min-1的速度程序升温至450℃，于450℃煅烧3小时，冷却至室温，研钵研磨成粉末。得到氮化碳/铁酸镧复合光催化材料。
实施例2：
本实施例提供一种氮化碳和铁酸镧复合光催化材料，该复合材料中，氮化碳与铁酸镧的质量比为10:1。
同时提供一种氮化碳和铁酸镧复合光催化材料的制备方法：
1.石墨相氮化碳(g-C3N4)制备，称取10.00g三聚氰胺于半封闭的坩埚中，马弗炉中以5℃min-1的速度程序升温至550℃，于550℃煅烧2小时，冷却至室温，研钵研磨成粉末。
2.称取g-C3N4粉末4.00g、硝酸铁0.68g和硝酸镧0.72g，马弗炉中以5℃min-1的速度程序升温至500℃，于500℃煅烧2小时，冷却至室温，研钵研磨成粉末。得到氮化碳/铁酸镧复合光催化材料。
实施例3：
本实施例提供一种氮化碳和铁酸镧复合光催化材料，该复合材料中，氮化碳与铁酸镧的质量比为5：2。
同时提供一种氮化碳和铁酸镧复合光催化材料的制备方法：
1.石墨相氮化碳(g-C3N4)制备，称取10.00g三聚氰胺于半封闭的坩埚中，马弗炉中以5℃min-1的速度程序升温至550℃，于550℃煅烧2小时，冷却至室温，研钵研磨成粉末。
2.称取g-C3N4粉末4.00g、硝酸铁2.72g和硝酸镧2.88g，马弗炉中以5℃min-1的速度程序升温至550℃，于550℃煅烧1小时，冷却至室温，研钵研磨成粉末。得到氮化碳/铁酸镧复合光催化材料。
实施例4：
本实施例提供一种氮化碳和铁酸镧复合光催化材料，氮化碳与铁酸镧的质量比为5：3。
同时提供一种氮化碳和铁酸镧复合光催化材料的制备方法：
1.石墨相氮化碳(g-C3N4)制备，称取10.00g三聚氰胺于半封闭的坩埚中，马弗炉中以5℃min-1的速度程序升温至550℃，于550℃煅烧2小时，冷却至室温，研钵研磨成粉末。
2.称取g-C3N4粉末4.00g、硝酸铁4.08g和硝酸镧4.32g，马弗炉中以5℃min-1的速度程序升温至550℃，于550℃煅烧2小时，冷却至室温，研钵研磨成粉末。得到氮化碳/铁酸镧复合光催化材料。
光催化降解活性评估：
以300W氙灯为光源，对含有光催化剂和亚甲基蓝的样品溶液进行照射，一定时间后取出一定体积的溶液，离心分离除去光催化剂，通过紫外可见分光光度计测量溶液吸光度。
具体为：将50mg复合光催化剂分散于100mL浓度为50mg L-1的亚甲基蓝溶液中，以300W氙灯为光源，对溶液照射，每隔5min，取出5mL溶液，以5000rpm离心10min分离除去光催化剂，在波长665nm处测量溶液吸光度。
图1是所制备质量比为5％的氮化碳/铁酸镧复合光催化材料，在300W氙灯照射下光降解亚甲基蓝光谱图。从图中可见以300W氙灯为光源对含有光催化剂和亚甲基蓝的样品溶液照射5min后，亚甲基蓝的降解率达到85％。
图2所制备不同质量比的氮化碳/铁酸镧复合光催化材料，在3W LED灯照射下光降解亚甲基蓝光谱图。从图中可见以3W LED灯为光源对含有光催化剂和亚甲基蓝的样品溶液进行光照，质量比为20％的氮化碳/铁酸镧复合光催化剂，光降解效率最高。
Claims (4)
1.一种氮化碳和铁酸镧复合光催化材料的制备方法，其特征在于，步骤如下：
步骤一，制备g-C3N4，称取三聚氰胺并放于半封闭的坩埚中，置于马弗炉中程序升温至550℃煅烧2小时，冷却至室温，研钵研磨成粉末；
步骤二，称取g-C3N4粉末，加硝酸铁和硝酸镧，研磨使之充分混合均匀，g-C3N4粉末、硝酸铁、硝酸镧的质量比为400:(6.8～544):(7.2～576)；
步骤三，g-C3N4粉末、硝酸铁和硝酸镧于马弗炉中升温至350～550℃煅烧处理1～3h，得到氮化碳和铁酸镧复合光催化材料。
2.根据权利要求1所述一种氮化碳和铁酸镧复合光催化材料的制备方法，其特征在于：所制得复合光催化材料中，氮化碳与铁酸镧的质量比为100:2～100:40。
3.根据权利要求1所述一种氮化碳和铁酸镧复合光催化材料的制备方法，其特征在于：步骤二中，加入的硝酸铁和硝酸镧的摩尔比为1:1。
4.根据权利要求1所述一种氮化碳和铁酸镧复合光催化材料的制备方法，其特征在于：步骤二中的研磨时间为30min。
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