CN107335456A - 一种碳掺杂修饰石墨相氮化碳光催化剂及其制备方法 - Google Patents
一种碳掺杂修饰石墨相氮化碳光催化剂及其制备方法 Download PDFInfo
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- 239000003054 catalyst Substances 0.000 title claims abstract description 22
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 18
- 229910052799 carbon Inorganic materials 0.000 title claims abstract description 10
- 229910002804 graphite Inorganic materials 0.000 title claims abstract description 9
- 239000010439 graphite Substances 0.000 title claims abstract description 9
- JMANVNJQNLATNU-UHFFFAOYSA-N oxalonitrile Chemical compound N#CC#N JMANVNJQNLATNU-UHFFFAOYSA-N 0.000 title claims abstract description 9
- 238000002360 preparation method Methods 0.000 title claims abstract description 9
- 238000012986 modification Methods 0.000 title claims abstract description 8
- 230000004048 modification Effects 0.000 title claims abstract description 7
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- 238000010438 heat treatment Methods 0.000 claims abstract description 21
- 239000004202 carbamide Substances 0.000 claims abstract description 20
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Chemical compound NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 claims abstract description 19
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims abstract description 16
- 239000000463 material Substances 0.000 claims abstract description 16
- 239000004570 mortar (masonry) Substances 0.000 claims abstract description 16
- 239000002131 composite material Substances 0.000 claims abstract description 12
- MTPVUVINMAGMJL-UHFFFAOYSA-N trimethyl(1,1,2,2,2-pentafluoroethyl)silane Chemical compound C[Si](C)(C)C(F)(F)C(F)(F)F MTPVUVINMAGMJL-UHFFFAOYSA-N 0.000 claims abstract description 12
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- 238000000034 method Methods 0.000 claims abstract description 8
- 239000002245 particle Substances 0.000 claims abstract description 8
- 230000008569 process Effects 0.000 claims abstract description 8
- 229910052719 titanium Inorganic materials 0.000 claims abstract description 7
- 239000010936 titanium Substances 0.000 claims abstract description 7
- -1 titanium carbides Chemical class 0.000 claims abstract description 7
- 239000000126 substance Substances 0.000 claims abstract description 3
- 239000011229 interlayer Substances 0.000 claims description 2
- 239000002105 nanoparticle Substances 0.000 claims description 2
- 238000013019 agitation Methods 0.000 claims 1
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 abstract description 10
- 238000003756 stirring Methods 0.000 abstract description 7
- 238000001816 cooling Methods 0.000 abstract description 6
- 238000004519 manufacturing process Methods 0.000 abstract description 3
- 231100000252 nontoxic Toxicity 0.000 abstract description 3
- 230000003000 nontoxic effect Effects 0.000 abstract description 3
- 238000009413 insulation Methods 0.000 abstract 1
- 229910052739 hydrogen Inorganic materials 0.000 description 8
- 239000001257 hydrogen Substances 0.000 description 8
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 7
- 238000007146 photocatalysis Methods 0.000 description 7
- GSEJCLTVZPLZKY-UHFFFAOYSA-N Triethanolamine Chemical compound OCCN(CCO)CCO GSEJCLTVZPLZKY-UHFFFAOYSA-N 0.000 description 6
- 239000000919 ceramic Substances 0.000 description 5
- 239000003795 chemical substances by application Substances 0.000 description 5
- 229910052593 corundum Inorganic materials 0.000 description 5
- 239000010431 corundum Substances 0.000 description 5
- 230000001699 photocatalysis Effects 0.000 description 4
- 238000006303 photolysis reaction Methods 0.000 description 4
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 4
- 239000007864 aqueous solution Substances 0.000 description 3
- 238000006555 catalytic reaction Methods 0.000 description 3
- 230000015843 photosynthesis, light reaction Effects 0.000 description 3
- 229910052724 xenon Inorganic materials 0.000 description 3
- FHNFHKCVQCLJFQ-UHFFFAOYSA-N xenon atom Chemical compound [Xe] FHNFHKCVQCLJFQ-UHFFFAOYSA-N 0.000 description 3
- 230000003197 catalytic effect Effects 0.000 description 2
- 150000001875 compounds Chemical class 0.000 description 2
- 239000000356 contaminant Substances 0.000 description 2
- 238000003912 environmental pollution Methods 0.000 description 2
- 239000004065 semiconductor Substances 0.000 description 2
- 238000003786 synthesis reaction Methods 0.000 description 2
- 230000001154 acute effect Effects 0.000 description 1
- 230000005540 biological transmission Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 230000015556 catabolic process Effects 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 238000006731 degradation reaction Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 150000002431 hydrogen Chemical class 0.000 description 1
- 229920000620 organic polymer Polymers 0.000 description 1
- 239000002957 persistent organic pollutant Substances 0.000 description 1
- 238000000634 powder X-ray diffraction Methods 0.000 description 1
- 230000006798 recombination Effects 0.000 description 1
- 238000005215 recombination Methods 0.000 description 1
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Abstract
一种碳掺杂修饰石墨相氮化碳光催化剂,它的化学成分质量百分比为:C‑TiO2 0.1‑0.8、其余为g‑C3N4;上述碳掺杂修饰石墨相氮化碳光催化剂的制备方法主要是按取每30g尿素加入0.5‑6mg碳化钛的比例,将尿素和碳化钛置于玛瑙研钵中,充分研磨、搅动、混合10min;将混合均匀的尿素和碳化钛混合物装入容器中,然后放到马弗炉里进行热处理,其升温程序为:从室温以5‑30℃/min的升温速率,升到500‑600℃,并保温1‑2h,随后随炉冷却,整个热处理过程均在空气气氛下进行;将得到的复合材料倒入玛瑙研钵中,充分研磨成粒径为2‑10μm的物质,制得C‑TiO2/g‑C3N4光催化剂。本发明制备方法简单,成本低廉,物理化学性质稳定,无毒,环境友好有利于实际应用和工业化生产。
Description
技术领域
本发明属于材料技术领域,特别涉及一种光催化材料及其制备方法。
背景技术
近年来,能源危机和环境污染已成为全球性尖锐问题。半导体催化剂能够有效地将太阳能转化为清洁能源并且降解有机污染物,从而缓解能源危机和减少环境污染,被广泛重视。非金属有机聚合物石墨相g-C3N4材料具有廉价易得,很好的化学及热稳定性,合适的能带结构,可见光响应等性质,在光解水制氢,有机物合成和污染物降解领域有潜在应用,能够很好的实现太阳能到化学能的转化。光催化材料技术的目的是制备成本低廉,高效稳定的催化剂。然而,纯g-C3N4仍在高效性及稳定性上存在不足,如对可见光利用效率低;光生电子空穴对容易复合,较低的量子效率;抗光腐蚀性差,催化稳定性不好。为了满足光催化技术的要求,需对g-C3N4改性处理,提高其光催化活性及稳定性。
TiO2作为半导体催化材料,同g-C3N4一样具有良好的物理化学性质,成本低,无毒,对环境友好等。但是,TiO2的带隙宽,只能吸收紫外光能量,同时光生电子空穴对复合速度快,量子效率偏低,不利于TiO2催化剂实用化和工业化应用。
发明内容
本发明的目的在于提供一种高催化活性、高稳定性、能工业化应用的碳掺杂修饰石墨相氮化碳光催化剂及其制备方法。本发明主要是在空气气氛下热处理TiC和尿素的混合物,合成有少量C-TiO2复合g-C3N4材料,使其能有效利用太阳光能,同时提高光解水制氢效率。
本发明的碳掺杂修饰石墨相氮化碳光催化剂的化学成分质量百分比(wt%)为:C-TiO2为0.1-0.8,其余为g-C3N4,C-TiO2/g-C3N4材料形貌为C-TiO2纳米颗粒分布在层状g-C3N4表面或者插入到g-C3N4层间。
上述碳掺杂修饰石墨相氮化碳光催化剂的制备方法:
(1)按取每30g尿素加入0.5-6mg碳化钛的比例,将尿素和碳化钛置于玛瑙研钵中,充分研磨、搅动、混合10min;
(2)将混合均匀的尿素和碳化钛混合物装入容器中,然后放到马弗炉里进行热处理,其升温程序为:从室温以5-30℃/min的升温速率,升到500-600℃,并保温1-2h,随后随炉冷却,整个热处理过程均在空气气氛下进行;
(3)将得到的复合材料倒入玛瑙研钵中,充分研磨成粒径为2-10μm的物质,制得C-TiO2/g-C3N4光催化剂。
本发明与现有技术相比具有如下优点:
1、制备方法简单,有利于实际应用和工业化生产。
2、制备的C-TiO2/g-C3N4光催化剂保留了纯的g-C3N4和TiO2的诸多优点,即成本低廉,物理化学性质稳定,无毒,环境友好等。
3、该光催化剂可应用于光解水制氢和环境污染物降解,其五小时光催化产氢量可达5.728mmol/g,相比纯的g-C3N4和TiO2分别为2.278mmol/g、0.010mmol/g,均比单相g-C3N4和TiO2高。
附图说明
图1为实施例1制得的C-TiO2/g-C3N4光催化剂的X射线粉末衍射图(XRD);
图2为实施例1制得的C-TiO2/g-C3N4光催化剂的透射电子显微镜图(TEM);
图3为实施例1、2、4所得的C-TiO2/g-C3N4复合材料及纯g-C3N4和TiO2的光解水制氢图。
具体实施方式
实施例1
取30g尿素(天津市凯通化学试剂有限公司)和1mg碳化钛(三河市海特科技有限公司,40nm)置于玛瑙研钵中,充分研磨、搅动、混合10min;将混合均匀的尿素和碳化钛混合物装入刚玉瓷方舟中,然后放到马弗炉里进行热处理,其升温程序为:从室温以5℃/min的升温速率升到500℃,并保温2h,随后随炉冷却,整个热处理过程均在空气气氛下进行。将得到的复合材料倒入玛瑙研钵中,充分研磨成粒径为2-10μm的物质,制得C-TiO2/g-C3N4光催化剂。
C-TiO2/g-C3N4复合材料光催化性能测试,其条件为:300W氙灯作为光源,催化剂用量为50mg,80ml三乙醇胺水溶液,三乙醇胺占10vol.%,其五小时产氢量达到了5.8mmol/g,相比纯的g-C3N4和TiO2分别为2.2mmol/g、0.01mmol/g。
实施例2
取30g尿素(天津市凯通化学试剂有限公司)和0.5mg碳化钛(三河市海特科技有限公司,40nm)置于玛瑙研钵中,充分研磨、搅动、混合10min;将混合均匀的尿素和碳化钛混合物装入刚玉瓷方舟中,然后放到马弗炉里进行热处理,其升温程序为:从室温以30℃/min的升温速率升到500℃,并保温1h,随后随炉冷却,整个热处理过程均在空气气氛下进行。将得到的复合材料倒入玛瑙研钵中,充分研磨成粒径为2-10μm的物质,制得C-TiO2/g-C3N4光催化剂。
C-TiO2/g-C3N4复合材料光催化性能测试,其条件为:300W氙灯作为光源,催化剂用量为50mg,80ml三乙醇胺水溶液,三乙醇胺占10vol.%。其五小时产氢量达到了3.5mmol/g,相比纯的g-C3N4和TiO2分别为2.2mmol/g、0.01mmol/g。
实施例3
取30g尿素(天津市凯通化学试剂有限公司)和2mg碳化钛(三河市海特科技有限公司,40nm)置于玛瑙研钵中,充分研磨、搅动、混合10min。将混合均匀的尿素和碳化钛混合物装入刚玉瓷方舟中,然后放到马弗炉里进行热处理。其升温程序为:从室温以10℃/min的升温速率升到550℃,并保温2h,随后随炉冷却,整个热处理过程均在空气气氛下进行。将得到的复合材料倒入玛瑙研钵中,充分研磨成粒径为2-10μm的物质,制得C-TiO2/g-C3N4光催化剂。
实施例4
取30g尿素(天津市凯通化学试剂有限公司)和4mg碳化钛(三河市海特科技有限公司,40nm)置于玛瑙研钵中,充分研磨、搅动、混合10min。将混合均匀的尿素和碳化钛混合物装入刚玉瓷方舟中,然后放到马弗炉里进行热处理。其升温程序为:从室温以10℃/min的升温速率升到600℃,并保温2h,随后随炉冷却,整个热处理过程均在空气气氛下进行。将得到的复合材料倒入玛瑙研钵中,充分研磨成粒径为2-10μm的物质,制得C-TiO2/g-C3N4光催化剂。
C-TiO2/g-C3N4复合材料光催化性能测试,其条件为:300W氙灯作为光源,催化剂用量为50mg,80ml三乙醇胺水溶液,三乙醇胺占10vol.%。其五小时产氢量达到了4.2mmol/g,相比纯的g-C3N4和TiO2分别为2.2mmol/g、0.01mmol/g。
实施例5
取30g尿素(天津市凯通化学试剂有限公司)和6mg碳化钛(三河市海特科技有限公司,40nm)置于玛瑙研钵中,充分研磨、搅动、混合10min。将混合均匀的尿素和碳化钛混合物装入刚玉瓷方舟中,然后放到马弗炉里进行热处理。其升温程序为:从室温以20℃/min的升温速率升到600℃,并保温2h,随后随炉冷却,整个热处理过程均在空气气氛下进行。将得到的复合材料倒入玛瑙研钵中,充分研磨成粒径为2-10μm的物质,制得C-TiO2/g-C3N4光催化剂。
Claims (2)
1.一种碳掺杂修饰石墨相氮化碳光催化剂,其特征在于:它的化学成分质量比wt%为:C-TiO2 0.1-0.8,其余为g-C3N4,C-TiO2/g-C3N4材料形貌为C-TiO2纳米颗粒分布在层状g-C3N4表面或者插入到g-C3N4层间。
2.权利要求1的碳掺杂修饰石墨相氮化碳光催化剂的制备方法,其特征在于:
(1)按取每30g尿素加入0.5-6mg碳化钛的比例,将尿素和碳化钛置于玛瑙研钵中,充分研磨、搅动、混合10min;
(2)将混合均匀的尿素和碳化钛混合物装入容器中,然后放到马弗炉里进行热处理,其升温程序为:从室温以5-30℃/min的升温速率,升到500-600℃,并保温1-2h,随后随炉冷却,整个热处理过程均在空气气氛下进行;
(3)将步骤(2)得到的复合材料倒入玛瑙研钵中,充分研磨成粒径为2-10μm的物质,制得C-TiO2/g-C3N4光催化剂。
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CN108499588A (zh) * | 2018-03-02 | 2018-09-07 | 东华大学 | 一种g-C3N4/MXene复合材料的制备方法 |
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CN112076777A (zh) * | 2020-09-23 | 2020-12-15 | 湖南大学 | 一种用于co2还原的光催化剂及其制备方法 |
CN112076777B (zh) * | 2020-09-23 | 2022-02-08 | 湖南大学 | 一种用于co2还原的光催化剂及其制备方法 |
CN114100664A (zh) * | 2021-12-02 | 2022-03-01 | 塔里木大学 | C-TiO2/g-C3N4复合光催化材料及其合成方法 |
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