CN106311306B - 一种制备锂掺杂石墨相氮化碳材料的方法 - Google Patents
一种制备锂掺杂石墨相氮化碳材料的方法 Download PDFInfo
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- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 title claims abstract description 37
- 229910052744 lithium Inorganic materials 0.000 title claims abstract description 37
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 34
- JMANVNJQNLATNU-UHFFFAOYSA-N oxalonitrile Chemical compound N#CC#N JMANVNJQNLATNU-UHFFFAOYSA-N 0.000 title claims abstract description 33
- 229910002804 graphite Inorganic materials 0.000 title claims abstract description 32
- 239000010439 graphite Substances 0.000 title claims abstract description 32
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- 229910003002 lithium salt Inorganic materials 0.000 claims abstract description 6
- 159000000002 lithium salts Chemical class 0.000 claims abstract description 6
- 238000006068 polycondensation reaction Methods 0.000 claims abstract description 6
- 238000001816 cooling Methods 0.000 claims abstract description 5
- 238000001035 drying Methods 0.000 claims abstract description 4
- 239000007864 aqueous solution Substances 0.000 claims abstract description 3
- 239000003125 aqueous solvent Substances 0.000 claims abstract description 3
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- 238000001354 calcination Methods 0.000 claims description 7
- 239000000843 powder Substances 0.000 claims description 6
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- 229920000877 Melamine resin Polymers 0.000 claims description 4
- XIXADJRWDQXREU-UHFFFAOYSA-M lithium acetate Chemical compound [Li+].CC([O-])=O XIXADJRWDQXREU-UHFFFAOYSA-M 0.000 claims description 4
- JDSHMPZPIAZGSV-UHFFFAOYSA-N melamine Chemical compound NC1=NC(N)=NC(N)=N1 JDSHMPZPIAZGSV-UHFFFAOYSA-N 0.000 claims description 4
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- XGZVUEUWXADBQD-UHFFFAOYSA-L lithium carbonate Chemical compound [Li+].[Li+].[O-]C([O-])=O XGZVUEUWXADBQD-UHFFFAOYSA-L 0.000 claims description 2
- 229910052808 lithium carbonate Inorganic materials 0.000 claims description 2
- 229940071264 lithium citrate Drugs 0.000 claims description 2
- WJSIUCDMWSDDCE-UHFFFAOYSA-K lithium citrate (anhydrous) Chemical compound [Li+].[Li+].[Li+].[O-]C(=O)CC(O)(CC([O-])=O)C([O-])=O WJSIUCDMWSDDCE-UHFFFAOYSA-K 0.000 claims description 2
- QJGQUHMNIGDVPM-UHFFFAOYSA-N nitrogen group Chemical group [N] QJGQUHMNIGDVPM-UHFFFAOYSA-N 0.000 claims description 2
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- GWEVSGVZZGPLCZ-UHFFFAOYSA-N titanium dioxide Inorganic materials O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 4
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- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical group [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 2
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 2
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- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 description 1
- 239000005864 Sulphur Substances 0.000 description 1
- 238000002835 absorbance Methods 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
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- 229910052724 xenon Inorganic materials 0.000 description 1
- FHNFHKCVQCLJFQ-UHFFFAOYSA-N xenon atom Chemical compound [Xe] FHNFHKCVQCLJFQ-UHFFFAOYSA-N 0.000 description 1
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- B01J27/00—Catalysts comprising the elements or compounds of halogens, sulfur, selenium, tellurium, phosphorus or nitrogen; Catalysts comprising carbon compounds
- B01J27/24—Nitrogen compounds
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Abstract
本发明公开一种锂掺杂石墨相氮化碳(g‑C3N4)材料的制备方法。制备步骤:将锂盐分散于富碳氮材料的水溶液中,充分混合,然后加热除去溶剂水;在充分干燥后经程序升温并恒温加热发生缩聚反应;缩聚反应产物自然冷却、研磨得到锂掺杂石墨相氮化碳。其优点在于:制备方法简单,成本低廉、周期短、制备过程中人为因素对实验结果影响小,制备过程中无需昂贵的设备,适用于工业化大规模生产;相较于纯g‑C3N4,制备的锂掺杂的g‑C3N4的带隙明显窄化,其吸收带边可延伸到620nm;锂掺杂的g‑C3N4具有较窄的带隙,可以极大提高可见光利用率,同时能有效抑制光生电子–空穴对的复合,因此具有优异的光催化性能。
Description
技术领域
本发明涉及一种制备锂掺杂石墨相氮化碳(g-C3N4)材料的方法,属于材料制备领域。
背景技术
上世纪70年代Fujishima和Honda发现TiO2能够用于光催化分解水制氢,揭开了人们对于光催化半导体材料研究的序幕。1977年Bard发现了在紫外光辐照下,TiO2对CN–向OCN–转变具有催化氧化活性,从而拓宽了光催化反应的应用范围,并首次提出光催化技术可应用于污水处理领域。光催化技术是一种直接将光能转化为化学能的绿色新技术,与传统水污染处理方法相比具有诸多优点,如:在常温常压下进行反应,条件温和;可以将污染物彻底氧化分解为二氧化碳和水等无机小分子,避免二次污染等。但是目前光催化技术在污染物降解应用中的实际效果仍不理想,原因包括如TiO2、ZnO等传统光催化材料只能吸收紫外光,而紫外光只占太阳光中的大约4%,其他47%的可见光得不到利用,并且在催化过程中存在光生电子–空穴对分离效率低等弊端。因此设计研发新型、高效且具有可见光响应的光催化半导体材料是一个重要的研究方向。
石墨相氮化碳(简称g-C3N4)是具有类石墨烯结构的二维片层状聚合物半导体材料,物质本身只含有地球上富含的碳和氮两种元素,其独特的半导体光催化特性已在太阳能利用上展现出很大的潜力。虽然g-C3N4作为新型催化剂具有稳定、耐高温、合适的能带结构等优点,但由于其存在比表面积小(10m2/g)、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。研究者尝试用不同的方法对其改性,包括共聚合改性、硫介质调控、形貌调控和掺杂改性等。研究表明,这些方法都可以在一定程度上提高g-C3N4的光催化活性,而掺杂改性又是其中比较有效的方法。在g-C3N4中掺入一定量的其它元素,不仅可以扩大g-C3N4的可见光响应范围,还可以抑制光生电子–空穴对的复合,从而显著提高其光催化性能。到目前为止,对g-C3N4进行掺杂改性的绝大部分是非金属元素,比如F、S、P等,但是它们对g-C3N4的吸收带边调节都很有限,比如F掺杂只能将其带边从460nm调节到470nm(Chem.Mater.2010,22,5119),S掺杂只能将其带边从460nm调节到475nm(J.Mater.Chem.,2012,22,15006),P掺杂只能将其带边从460nm调节到477nm(RSCAdv.,2014,4,21657)。
发明内容
针对目前g-C3N4进行掺杂改性的绝大部分是非金属元素,且带隙调节很有限,本发明提出一种制备锂掺杂石墨相氮化碳(g-C3N4)材料的方法。这种方法简单易行,具体包括如下步骤:
a.将锂盐分散于富碳氮材料的水溶液中,充分搅拌使其混合均匀,然后于40-80℃加热除去溶剂水,得到白色粉末;
b.将步骤a所述的白色粉末于管式炉中进行煅烧使其发生缩聚反应,具体煅烧过程为:从室温经3-6小时程序升温到550-600℃并在此温度下保持2-6小时;
c.将步骤b所述的缩聚反应产物自然冷却,用去离子水洗涤后,于40-80℃干燥,产物经研磨得到锂掺杂石墨相氮化碳。
进一步地,步骤a中所述锂盐为醋酸锂、碳酸锂、柠檬酸锂。
进一步地,步骤a中所述富碳氮材料为尿素、双氰胺、氰胺、三聚氰胺。
进一步地,步骤a中锂盐与富碳氮材料的重量比为1:4~1:20;优选1:5~1:10;更优选1:6.5~1:9。
进一步地,步骤b中煅烧氛围为氮气和氩气氛围。
本发明提出在g-C3N4中掺入Li元素,这是对g-C3N4进行掺杂改性的一个突破,其典型特征是极大地扩大了g-C3N4的可见光响应范围,将其从460nm调节到620nm,且有效抑制了光生电子–空穴对的复合,显著提高了其可见光催化性能。这是其它掺杂元素所无法比拟的。这种制备方法简单,成本低廉、周期短、制备过程中无需昂贵的设备,人为因素对实验结果影响小,适用于工业化大规模生产。
附图说明
本发明附图6幅,
图1是实施例1制备的锂掺杂石墨相氮化碳的XRD图;
图2是实施例1制备的锂掺杂石墨相氮化碳的XPS图;
图3是实施例1制备的锂掺杂石墨相氮化碳的DRS图;
图4是实施例1制备的锂掺杂石墨相氮化碳的PL图;
图5是实施例2制备的锂掺杂石墨相氮化碳的DRS图;
图6是应用例5的光催化降解率曲线。
具体实施方式
下述非限定性实施例可以使本领域的普通技术人员更全面地理解本发明,但不以任何方式限制本发明。
实施例1
将0.10g醋酸锂和1g三聚氰胺分散于10mL去离子水中,充分搅拌使其混合均匀,然后于50℃加热除去水,得到白色粉末。将此白色粉末于管式炉中在氮气氛围下进行煅烧。具体煅烧过程为:从室温经4小时程序升温到550℃并在此温度下保持4小时。煅烧产物自然冷却,用去离子水洗涤后,于60℃干燥,最后经研磨得到锂掺杂石墨相氮化碳。
图1所示为实施例1制备的锂掺杂石墨相氮化碳的XRD图;图中位于13.1o和27.3o的衍射峰分别归属于石墨相氮化碳的(100)和(002)晶面(JCPDS 87-1526),且图中并未显示任何锂的化合物的衍射峰。
图2所示为实施例1制备的锂掺杂石墨相氮化碳的XPS-Li(1s)图;图中位于55.3eV的峰归属于锂,说明锂成功掺入石墨相氮化碳中。
图3所示为实施例1制备的锂掺杂石墨相氮化碳的DRS图;图中显示掺入锂后,其光吸收带边由460nm红移到500nm,说明掺入锂可使其光吸收范围增大。
图4所示为是实施例1制备的锂掺杂石墨相氮化碳的PL图;图中显示相较于未掺杂的石墨相氮化碳,其PL发光强度明显降低,说明掺入锂可有效抑制光生电子-空穴对的复合。
实施例2
实验方法同实施例1,不同之处在于将醋酸锂的用量提高到0.25g,得到锂掺杂石墨相氮化碳。
图5所示为实施例2制备的锂掺杂石墨相氮化碳的DRS图;图中显示掺入锂后,其光吸收带边由460nm红移到620nm,说明掺入锂可使其光吸收范围增大。
实施例3
实验方法同实施例1,不同之处在于煅烧氛围为氩气。
实施例4
实验方法同实施例1,不同之处在于煅烧温度为580℃。
应用例5
将实施例1得到的锂掺杂石墨相氮化碳和未掺杂的石墨相氮化碳按照如下方法进行光催化降解罗丹明B溶液。
使用300W的氙灯(CEL-HXF300)作为可见光源,其光波长λ>420nm。
向石英反应器内加入50mL浓度为10mg/L的罗丹明B溶液,以及20mg的光催化剂。将反应器在磁力搅拌下避光暗反应20分钟后,开灯持续搅拌继续反应40分钟,反应过程使用回流水冷却装置维持室温条件,过程中每10分钟用注射器取4mL的样品悬浮液分别放入离心管内。在离心机9500转/分钟条件下离心10分钟,完成后取上清液,经过漏斗过滤,将滤液放入紫外分光光度仪测量其554nm处的吸光度,计算出降解率。
图6所示为应用例5的光催化降解率曲线,表明实施例1制备的锂掺杂石墨相氮化碳光催化活性明显高于未掺杂的石墨相氮化碳。
未掺杂的石墨相氮化碳的制备:
将1g三聚氰胺于管式炉中在氮气氛围下进行煅烧。具体煅烧过程为:从室温经4小时程序升温到550℃并在此温度下保持4小时。煅烧产物自然冷却,研磨得到石墨相氮化碳。
Claims (4)
1.一种制备锂掺杂石墨相氮化碳材料的方法,其特征在于具体包括如下步骤:
a.将锂盐分散于富碳氮材料的水溶液中,充分搅拌使其混合均匀,然后于40-80℃加热除去溶剂水,得到白色粉末;
b.将步骤a所述的白色粉末于管式炉中进行煅烧使其发生缩聚反应,具体煅烧过程为:从室温经3-6小时程序升温到550-600℃并在此温度下保持2-6小时;
c.将步骤b所述的缩聚反应产物自然冷却,用去离子水洗涤后、于40-80℃干燥,产物经研磨得到锂掺杂石墨相氮化碳;
步骤a中所述锂盐为醋酸锂、碳酸锂、柠檬酸锂。
2.根据权利要求1所述制备锂掺杂石墨相氮化碳材料的方法,其特征在于:步骤a中所述富碳氮材料为尿素、双氰胺、氰胺、三聚氰胺。
3.根据权利要求1所述制备锂掺杂石墨相氮化碳材料的方法,其特征在于:步骤a中锂盐与富碳氮材料的重量比为1:4~1:20。
4.根据权利要求1所述制备锂掺杂石墨相氮化碳材料的方法,其特征在于:步骤b中煅烧氛围为氮气和氩气氛围。
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