CN109485606B - 纳米管结构的吡唑啉酮锌配合物及其制备方法和应用 - Google Patents
纳米管结构的吡唑啉酮锌配合物及其制备方法和应用 Download PDFInfo
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- -1 Pyrazolone zinc Chemical compound 0.000 title claims abstract description 34
- 239000002071 nanotube Substances 0.000 title claims abstract description 25
- 238000002360 preparation method Methods 0.000 title abstract description 10
- ONDPHDOFVYQSGI-UHFFFAOYSA-N zinc nitrate Chemical compound [Zn+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O ONDPHDOFVYQSGI-UHFFFAOYSA-N 0.000 claims abstract description 26
- 239000011701 zinc Substances 0.000 claims abstract description 20
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 claims abstract description 19
- 229910052725 zinc Inorganic materials 0.000 claims abstract description 17
- RBTBFTRPCNLSDE-UHFFFAOYSA-N 3,7-bis(dimethylamino)phenothiazin-5-ium Chemical compound C1=CC(N(C)C)=CC2=[S+]C3=CC(N(C)C)=CC=C3N=C21 RBTBFTRPCNLSDE-UHFFFAOYSA-N 0.000 claims abstract description 12
- 229960000907 methylthioninium chloride Drugs 0.000 claims abstract description 12
- 230000003197 catalytic effect Effects 0.000 claims abstract description 7
- 239000003446 ligand Substances 0.000 claims description 28
- ZMXDDKWLCZADIW-UHFFFAOYSA-N N,N-Dimethylformamide Chemical compound CN(C)C=O ZMXDDKWLCZADIW-UHFFFAOYSA-N 0.000 claims description 24
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- 125000004430 oxygen atom Chemical group O* 0.000 claims description 4
- 125000002915 carbonyl group Chemical group [*:2]C([*:1])=O 0.000 claims description 2
- RKTYLMNFRDHKIL-UHFFFAOYSA-N copper;5,10,15,20-tetraphenylporphyrin-22,24-diide Chemical compound [Cu+2].C1=CC(C(=C2C=CC([N-]2)=C(C=2C=CC=CC=2)C=2C=CC(N=2)=C(C=2C=CC=CC=2)C2=CC=C3[N-]2)C=2C=CC=CC=2)=NC1=C3C1=CC=CC=C1 RKTYLMNFRDHKIL-UHFFFAOYSA-N 0.000 claims description 2
- 125000004185 ester group Chemical group 0.000 claims description 2
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- 125000003226 pyrazolyl group Chemical group 0.000 claims description 2
- 230000035484 reaction time Effects 0.000 claims description 2
- 230000001699 photocatalysis Effects 0.000 abstract description 7
- 239000000126 substance Substances 0.000 abstract description 3
- 239000011365 complex material Substances 0.000 abstract description 2
- 125000001495 ethyl group Chemical group [H]C([H])([H])C([H])([H])* 0.000 abstract 1
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- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 2
- PTFCDOFLOPIGGS-UHFFFAOYSA-N Zinc dication Chemical compound [Zn+2] PTFCDOFLOPIGGS-UHFFFAOYSA-N 0.000 description 2
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- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 1
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Abstract
本发明属于配合物材料技术领域,具体涉及一种纳米管结构的吡唑啉酮锌配合物及其制备方法和应用,所述的锌配合物化学表达式为{[Zn(Hpyc)2]·H2O}n,n为正整数,式中H2pyz为5‑吡唑啉酮‑4‑甲酸乙酯。锌配合物是利用5‑吡唑啉酮‑4‑甲酸乙酯和硝酸锌在溶剂热条件下合成,产物稳定性高,有优良的催化活性。该锌配合物具有光催化性质,尤其能高效的催化光降解亚甲基蓝,并且可以循环利用。
Description
技术领域
本发明属于配合物材料技术领域,具体涉及一种纳米管结构的吡唑啉酮锌配合物及其制备方法和应用。
背景技术
近年来随着印染工业的迅速发展,染料废水引起的水体污染日益严重,科学工作者也通过不断努力来治理和保护水体环境。目前处理染料废水的方法主要有物化法、生化法以及光催化技术。光催化技术是一种新兴的有机染料处理技术,是指有机染料在光和催化剂同时作用下所进行的化学反应,即利用光能进行物质转化的一种方式。大量研究表明,光催化技术可以高效降解水体中有机染料,并达到脱色、去毒的效果。传统的TiO2、WO3及CdS等无机光催化材料在催化过程中量子产率和太阳能转换率比较低,制约了其实际应用。因此,开发新型高效光催化剂对于治理和保护水体环境具有重要意义。
金属有机配合物是一种由金属离子和有机配体自组装形成的新型功能材料。这类功能材料具有良好的热化学稳定性、高的比表面积、结构可调性和光学活性等性能,广泛应用于催化、气体储存、气体分离及污染物的去除等领域,尤其是催化领域,吸引了人们越来越多的关注。因为金属有机配合物存在着配体与金属之间的电荷跃迁行为,配合物中的每一个金属位点都可以视为独立的无机半导体量子点,在催化过程中量子产率和太阳能转换率都比传统无机材料高,因此可以通过改变配体和金属的种类来获得具有高效光响应的光催化材料。
发明内容
本发明主要提供了一种纳米管结构的吡唑啉酮锌配合物及其制备方法和应用,所述吡唑啉酮锌配合物能高效催化光降解亚甲基蓝,并且吡唑啉酮锌配合物可循环利用,为催化光降解有机染料提供了新选择。其技术方案如下:
一种纳米管结构的吡唑啉酮锌配合物,该配合物的分子式为{[Zn(Hpyc)2]·H2O}n,H2pyc为5-吡唑啉酮-4-甲酸乙酯,所述锌配合物分子结构如下所示:
其中,n为正整数。
优选的,所述锌配合物的不对称结构单元由一个中心金属Zn、两个5-吡唑啉酮-4-甲酸乙酯配体、一个晶格水组成;配合物中配体为三齿配位模式,配体一端通过酯基上的氧原子和羰基上的氧原子螯合一个锌原子,另一端则通过吡唑环上的氮原子与另一个锌原子连接,四个配体将四个锌原子桥连成一个四核结构单元,每个四核结构单元再通过四个配体连接,形成一个纳米管状结构,晶格水处于纳米孔道中。
上述纳米管结构的吡唑啉酮锌配合物的制备方法如下:将5-吡唑啉酮-4-甲酸乙酯配体溶于N,N-二甲基甲酰胺溶剂、硝酸锌溶于蒸馏水,然后将两种溶液混合均匀,于密闭烘箱加热反应,反应结束后,冷却至室温,得纳米管结构的吡唑啉酮锌配合物。
优选的,5-吡唑啉酮-4-甲酸乙酯与硝酸锌的摩尔比为1:(1-1.5)。
优选的,N,N-二甲基甲酰胺溶剂与蒸馏水的体积比为1:(1-2)。
优选的,烘箱温度为80~90℃,反应时间为1~2天。
所述锌配合物在催化光降解染料中的应用,该锌配合物能高效催化光降解亚甲基蓝,且吡唑啉酮锌配合物稳定性高,可循环利用。
采用上述方案,本发明具有以下优点:
本发明所述的纳米管结构的吡唑啉酮锌配合物,合成方法简单、能耗低,为基于吡唑衍生物有机配体合成金属配合物提供了一定的依据。所述的纳米管结构的吡唑啉酮锌配合物能高效催化光降解亚甲基蓝,并且吡唑啉酮锌配合物可循环利用,为催化光降解有机染料提供了新选择。
附图说明
图1是本发明的一种纳米管结构的吡唑啉酮锌配合物的锌属离子配位环境图;
图2为本发明的一种纳米管结构的吡唑啉酮锌配合物的空间构型图;
图3是本发明的一种纳米管结构的吡唑啉酮锌配合物催化光降解亚甲基蓝的紫外吸收光谱图;
图4是本发明的一种纳米管结构的吡唑啉酮锌配合物催化光降解亚甲基蓝的浓度变化速率图;
图5是本发明的一种纳米管结构的吡唑啉酮锌配合物催化光降解亚甲基蓝5次循环浓度变化速率图;
图6是本发明的一种纳米管结构的吡唑啉酮锌配合物催化光降解亚甲基蓝的PXRD图。
具体实施方式
以下实施例中的实验方法如无特殊规定,均为常规方法,所涉及的实验试剂及材料如无特殊规定均为常规生化试剂和材料。
实施例1
本实施例纳米管结构的吡唑啉酮锌配合物的制备方法如下:
称取5-吡唑啉酮-4-甲酸乙酯配体(0.1mmol,0.0156g)溶于1mL N,N-二甲基甲酰胺溶剂,制得配体溶液。称取硝酸锌(0.1mmol,0.0298g)溶于2mL蒸馏水,将配体溶液倒入硝酸锌溶液中,混合均匀,于80℃烘箱反应1天;反应结束后,冷却至室温,过滤,洗涤,风干,得目标化合物。产率:62%。对产物进行红外表征,具体结果为:IR(KBr,cm-1):3330(m),2994(w),1645(s),1536(m),1454(m),1329(m),1279(m),1141(m),1066(w),1020(w),931(m),786(m),671(w),603(w)。
实施例2
本实施例纳米管结构的吡唑啉酮锌配合物的制备方法如下:
称取5-吡唑啉酮-4-甲酸乙酯配体(0.1mmol,0.0156g)溶于2mL N,N-二甲基甲酰胺溶剂,制得配体溶液。称取硝酸锌(0.15mmol,0.0446g)溶于2mL蒸馏水,将配体溶液倒入硝酸锌溶液中,混合均匀,于80℃烘箱反应2天;反应结束后,冷却至室温,过滤,洗涤,风干,得目标化合物。产率:53%。对产物进行红外表征,具体结果为:IR(KBr,cm-1):3333(m),2991(w),1646(s),1534(m),1455(m),1330(m),1281(m),1143(m),1064(w),1022(w),931(m),788(m),672(w),601(w)。
红外测试结果表明,本实施例的产物与实施例1的产物相同。
实施例3
本实施例纳米管结构的吡唑啉酮锌配合物的制备方法如下:
称取5-吡唑啉酮-4-甲酸乙酯配体(0.1mmol,0.0156g)溶于1mL N,N-二甲基甲酰胺溶剂,制得配体溶液。称取硝酸锌(0.1mmol,0.0298g)溶于2mL蒸馏水,将配体溶液倒入硝酸锌溶液中,混合均匀,于90℃烘箱反应1天;反应结束后,冷却至室温,过滤,洗涤,风干,得目标化合物。产率:75%。对产物进行红外表征,具体结果为:IR(KBr,cm-1):3331(m),2992(w),1643(s),1538(m),1457(m),1327(m),1277(m),1144(m),1068(w),1020(w),932(m),786(m),670(w),602(w)。
红外测试结果表明,本实施例的产物与实施例1的产物相同。
实施例4
本实施例纳米管结构的吡唑啉酮锌配合物的制备方法如下:
称取5-吡唑啉酮-4-甲酸乙酯配体(0.1mmol,0.0156g)溶于2mL N,N-二甲基甲酰胺溶剂,制得配体溶液。称取硝酸锌(0.15mmol,0.0446g)溶于2mL蒸馏水,将配体溶液倒入硝酸锌溶液中,混合均匀,于90℃烘箱反应2天;反应结束后,冷却至室温,过滤,洗涤,风干,得目标化合物。产率:60%。对产物进行红外表征,具体结果为:IR(KBr,cm-1):3330(m),2993(w),1643(s),1535(m),1453(m),1331(m),1276(m),1140(m),1068(w),1023(w),929(m),785(m),669(w),604(w)。
红外测试结果表明,本实施例的产物与实施例1的产物相同。
实施例5
图1为实施例1制备的锌配合物的锌属离子配位环境图,图2为该锌配合物的空间构型图。
表2 Zn配合物的晶体键角(°)
O4B-Zn1-O1A | 87.88(19) | N1-Zn1-O5B | 94.72(16) |
O4B-Zn1-N1 | 92.01(17) | N3-Zn1-O5B | 92.46(19) |
O1A-Zn1-N1 | 86.19(15) | O4B-Zn1-O2A | 86.21(16) |
O4B-Zn1-N3 | 173.33(17) | O1A-Zn1-O2A | 88.05(14) |
O1A-Zn1-N3 | 89.3(2) | N1-Zn1-O2A | 174.03(16) |
N1-Zn1-N3 | 93.81(17) | N3-Zn1-O2A | 87.67(16) |
90.30(19) | 90.30(19) | O5B-Zn1-O2A | 90.99(14) |
O1A-Zn1-O5B | 177.99(13) |
表3Zn配合物的晶体学数据
实施例6
吡唑啉酮锌配合物催化光降解亚甲基蓝实验:
采用氙灯作为紫外光源,采用实施例1获得的吡唑啉酮锌配合物进行催化光降解亚甲基蓝的反应。
取50mL浓度为5mg/L的亚甲基蓝水溶液于石英反应罐中,加入30mg实施例1获得的吡唑啉酮锌配合物,在黑暗环境下搅拌30min。达到吸附-解吸平衡后,取样一次。然后以氙灯作为紫外光源进行催化光降解反应,每隔20min取样一次,共取样10次,取出的悬浊液经10000r/min的转速离心4min后取上层清液测其紫外可见吸收光谱(图3)。结果表明,200min后,吡唑啉酮锌配合物对亚甲基蓝的降解率为86.87%(图4)。PXRD测试结果显示,经过5次循环后,吡唑啉酮锌配合物结构没有发生变化(图5),且催化效果基本不发生变化(图6),说明该配合物具有高稳定性以及很好的光化学活性,可循环利用。
对本领域的技术人员来说,可根据以上描述的技术方案以及构思,做出其它各种相应的改变以及形变,而所有的这些改变以及形变都应该属于本发明权利要求的保护范围之内。
Claims (8)
3.根据权利要求1所述的纳米管结构的吡唑啉酮锌配合物,其特征在于:所述锌配合物的不对称结构单元由一个中心金属Zn、两个5-吡唑啉酮-4-甲酸乙酯配体、一个晶格水组成;配合物中配体为三齿配位模式,配体一端通过酯基上的氧原子和羰基上的氧原子螯合一个锌原子,另一端则通过吡唑环上的氮原子与另一个锌原子连接,四个配体将四个锌原子桥连成一个四核结构单元,每个四核结构单元再通过四个配体连接,形成一个纳米管状结构,晶格水处于纳米孔道中。
4.一种如权利要求1所述的纳米管结构的吡唑啉酮锌配合物的制备方法,其特征在于:将5-吡唑啉酮-4-甲酸乙酯配体溶于N,N-二甲基甲酰胺溶剂、硝酸锌溶于蒸馏水,然后将两种溶液混合均匀,于密闭烘箱加热反应,反应结束后,冷却至室温,得纳米管结构的吡唑啉酮锌配合物。
5.根据权利要求4所述的纳米管结构的吡唑啉酮锌配合物的制备方法,其特征在于:5-吡唑啉酮-4-甲酸乙酯与硝酸锌的摩尔比为1:(1-1.5)。
6.根据权利要求4所述的纳米管结构的吡唑啉酮锌配合物的制备方法,其特征在于:N,N-二甲基甲酰胺溶剂与蒸馏水的体积比为1:(1-2)。
7.根据权利要求4所述的纳米管结构的吡唑啉酮锌配合物的制备方法,其特征在于:烘箱温度为80~90℃,反应时间为1~2天。
8.权利要求1所述的锌配合物在催化光降解亚甲基蓝中的应用。
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