CN105001270A - Ba/Fe/Na金属和羧酸席夫碱配合物的制备方法 - Google Patents
Ba/Fe/Na金属和羧酸席夫碱配合物的制备方法 Download PDFInfo
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Abstract
本发明属于化学技术领域,具体涉及一种基于Ba/Fe/Na金属和羧酸席夫碱配合物的制备方法与应用,配合物为下述化学式:[BaNa(Fe-L)2(<i>μ2</i>-OH)(H2O)]·DMF·2H2O,其中L为去四个质子的1,2-环己烷二氨基-N,Nˊ-二(3-甲基-5-羧基水杨醛)阴离子。配合物采用溶剂热方法制备。配合物的光催化降解有机污染物研究表明该材料能够在可见光照射下降解2-氯酚,3-氯酚和4-氯酚,其中对4-氯酚的光降解效能最好,有望作为光降解有机污染物的催化剂在材料科学领域得到应用。
Description
技术领域
本发明属于化学技术领域,具体涉及一种过渡金属配合物制备方法及其应用。
背景技术
杂金属有机框架结构由于在磁性、气体吸附和异相催化等方面具有潜在的应用而被化学工作者广泛关注(T. Senapati, C. Pichon, R.
Ababei, C. Mathonière, R. Clérac, Inorg. Chem. 2012, 51, 3796)。官能化的席夫碱是制备杂金属配合物的极佳配体,原因是席夫碱内部的空腔和外部的官能团可以与不同的金属分别配位(K. Bhattacharya, S. M. T.
Abtab, M. C. Majee, A. Endo, M. Chaudhury, Inorg. Chem. 2014, 53, 8287)。
光催化也是当前的一个研究热点,此技术被广泛应用于气体与水的净化和分离等领域(H. Zhang, L.-H. Guo, L.
Zhao, B. Wan, Y. Yang, J. Phys. Chem. Lett. 2015, 6, 958)。近期的研究表明,几种含铁的杂金属配合物具有光降解有机污染物的性能(D. S. Nesterov, E. N.
Chygorin, V. N. Kokozay, V. V. Bon, R. Boca, Y. N. Kozlov, L. S.
Shul’pina, J. Jezierska, A.
Ozarowski, A. J. L. Pombeiro, G. B. Shul’pin, Inorg. Chem. 2012, 51,
9110)。但是,基于羧酸功能化席夫碱配体的三杂金属配合物至今还无人报导。
发明内容
本发明要解决的技术问题是公开一种基于Ba/Fe/Na三种金属和羧酸席夫碱配体的杂金属配合物。
本发明同时还公开了这种杂金属配合物的制备方法及其应用。
杂金属配合物具有下述化学式,即:[BaNa(Fe-L)2(µ2 -OH)(H2O)]·DMF·2H2O,其中L为去四个质子的1,2-环己烷二氨基-N,N'-二(3-甲基-5-羧基水杨醛)阴离子配体。
配合物晶体属于正交晶系,空间群为F222,晶胞参数为a = 31.955(3) Å,b = 65.386(2) Å,c = 12.9570(16) Å,α= 90°,β= 90°,γ = 90°,V = 27072(4) Å3,基本结构是含孔道的三维框架结构。
所述的杂金属配合物的制备方法,包括如下步骤:
取BaCl2·2H2O 0.12 mmol,1,2-环己烷二氨基-N,N'-二(3-甲基-5-羧基水杨醛)(H4L配体)0.03 mmol,FeCl3·6H2O 0.03 mmol,NaCl 0.06 mmol,二甲基甲酰胺1 mL,乙醇4 mL和水2 mL混合,得到棕色悬浊液。将混合物放入15 mL聚四氟乙烯反应釜中,放置在烘箱中,加热到100 ℃恒温72小时,然后缓慢降到室温得到棕色晶体,产率31%。
本发明晶体样品对可见光照射下的2-氯酚,3-氯酚和4-氯酚均表现出光催化降解能力,其中对4-氯酚的光催化降解能力最强,可以作为光降解催化剂在材料科学领域得到应用。
本发明杂金属配合物通过溶剂热合成得到,具有制备方法简单、产品性能稳定、重复性强等特点。
附图说明
图1是配合物中金属的配位环境图;
图2是三维孔道结构图;
图3是不同pH值时,配合物光催化降解2-氯酚随时间变化的曲线图;
图4是不同pH值时,配合物光催化降解3-氯酚随时间变化的曲线图;
图5是不同pH值时,配合物光催化降解4-氯酚随时间变化的曲线图;
图6是配合物的粉末衍射图。
具体实施方式
杂金属配合物的合成:
实施例1
取二水合氯化钡 0.12 mmol,六水合氯化铁 0.03 mmol,氯化钠0.06 mmol和H4L配体0.03 mmol,放入15 mL聚四氟乙烯反应釜中,以1 mL二甲基甲酰胺,4 mL乙醇和2 mL水为混合溶剂,放置在烘箱中,加热到100 ℃恒温72小时,然后缓慢降到室温得到棕色晶体,产率31%。
实施例2
取二水合氯化钡 0.12 mmol,六水合氯化铁 0.03 mmol,氯化钠0.06 mmol和H4L配体0.03 mmol,放入15 mL聚四氟乙烯反应釜中,以3 mL二甲基甲酰胺,2 mL乙醇和2 mL水为混合溶剂,放置在烘箱中,加热到110 ℃恒温72小时,然后缓慢降到室温得到棕色晶体,产率10%。
主要的红外吸收峰为:3394 (m),2932 (w),2858 (w),1607 (w),1565 (w),1388 (w),1308 (w),1286 (w),1217 (w),1122 (m),1027 (s),978 (s),952 (s),919 (s),861 (s),794 (m),760 (m),712 (m),582 (m),558 (m),525 (m),502 (s),466 (m),421 (s)。
配合物的相关表征
(1)配合物的晶体结构测定
配合物的衍射数据是在Oxford Diffraction Gemini R Ultra衍射仪上收集,293 K,Mo Kα射线 (λ = 0.71069 Å)。使用技术扫描进行校正。晶体结构是通过SHELEXL-97程序以直接法解出,用全矩阵最小二乘法SHELEXL-97进行精修。非氢原子的温度因子用各向异性进行修正。详细的晶体测定数据见表1;重要的键长和键角数据见表2;晶体结构见图1和图2。
发明的配合物其特征在于所述配合物晶体属于正交晶系,空间群为F222,晶胞参数为a = 31.955(3) Å,b = 65.386(2) Å,c = 12.9570(16) Å,α= 90°,β= 90°,γ = 90°,V = 27072(4) Å3。单胞中包含两个独立的 Fe (III)离子(Fe1和Fe2 都为一半占有率,五配位构型),三个独立的Ba(II)离子(其中Ba1和Ba2 为四分之一占有率,八配位构型;Ba3为一半占有率,六配位构型),两个Na (I)离子(Na1和Na2 为一半占有率,四配位构型),两个个L4-阴离子,两个一半占有率的µ 2-OH阴离子,两个一半占有率的配位水分子,一个游离的DMF 分子和两个游离的水分子。两个铁离子分别嵌于两个L4-阴离子内部的N2O2中,被一个µ 2-OH阴离子连接为(Fe-L)2(μ 2-OH)二聚体。两个L4-阴离子分别与(三个Ba离子/两个Na离子)和(两个Ba离子/两个Na离子)配位。配合物的整体结构为含孔道的三维框架。
(2)配合物的光催化2-氯酚,3-氯酚和4-氯酚研究(30m long × 0.25mm i.d.,WondaCAP 17毛细管色谱,GC-2014C,Shimadzu,FID探测器)。
在可见光照射下,配合物对溶液中三种氯酚的浓度均起到明显的降解作用。在pH = 3的条件下,对2-氯酚光降解的能力为55.5%(图3);在pH = 4的条件下,对3-氯酚光降解的能力为40.3%(图4);在pH = 3的条件下,对4-氯酚光降解的能力为71%(图5)。
(3)配合物的XPRD相纯度表征(Rigaku Dmax 2000 X-射线衍射器)。
通过粉末X-射线衍射来检测配合物晶体及作为催化剂后的相纯度。通过比较发现主要PXRD峰的位置相同,说明作为催化剂后配合物保持了结晶性及结构的完整性,见图6。
表1为配合物的主要晶体学数据
formula | C51H51N5O17Fe2BaNa |
Mr | 1277.34 |
crystal system | orthographic |
space group | F222 |
a (Å) | 31.955(3) |
b (Å) | 65.386(2) |
c (Å) | 12.9570(16) |
α(°) | 90 |
β(°) | 90 |
γ(°) | 90 |
V (Å3) | 27072(4) |
Z | 16 |
D calc (g cm-3) | 1.116 |
F(0 0 0) | 9112 |
R int | 0.0437 |
GOF on F 2 | 1.026 |
R1 [I>2σ(I)] | 0.0818 |
wR2 (all data) | 0.2554 |
表2为配合物的主要键长(Å)和键角[°]*
Fe(1)-O(2) | 1.7718(19) | Fe(1)-O(8) | 1.908(5) |
Fe(1)-O(7) | 1.934(6) | Fe(2)-O(1) | 1.7665(14) |
Fe(2)-O(5) | 1.899(5) | Fe(2)-O(6) | 1.898(5) |
Fe(1)-N(4) | 2.067(6) | Fe(1)-N(3) | 2.133(6) |
Fe(2)-N(2) | 2.095(6) | Fe(2)-N(1) | 2.103(5) |
Ba(1)-O(13)#1 | 2.697(12) | Ba(1)-O(13)#2 | 2.697(12) |
Ba(1)-O(13) | 2.697(12) | Ba(1)-O(13)#3 | 2.697(12) |
Ba(1)-O(11)#3 | 2.752(6) | Ba(1)-O(11)#2 | 2.752(6) |
Ba(1)-O(11) | 2.752(6) | Ba(1)-O(11)#1 | 2.752(6) |
Ba(2)-O(4)#4 | 2.719(11) | Ba(2)-O(4)#5 | 2.719(11) |
Ba(2)-O(4)#6 | 2.719(11) | Ba(2)-O(4)#3 | 2.719(11) |
Ba(2)-O(10)#7 | 2.861(11) | Ba(2)-O(10)#8 | 2.861(11) |
Ba(2)-O(10) | 2.861(11) | Ba(2)-O(10)#9 | 2.861(11) |
Ba(3)-O(3) | 2.445(15) | Ba(3)-O(9)#11 | 2.535(11) |
Ba(3)-O(3)#10 | 2.566(15) | Ba(3)-O(2W)#10 | 2.658(14) |
Ba(3)-O(9)#12 | 2.816(11) | Ba(3)-O(2W) | 2.860(15) |
Ba(3)-O(4) | 2.992(11) | Ba(3)-O(4)#10 | 3.039(11) |
Na(1)-O(14) | 2.678(16) | Na(1)-O(14)#2 | 2.678(16) |
Na(1)-O(12)#2 | 2.683(10) | Na(1)-O(12) | 2.683(10) |
Na(2)-O(1W) | 2.477(18) | Na(2)-O(9)#11 | 2.746(10) |
Na(2)-O(4) | 2.936(11) | Na(2)-O(10)#3 | 2.984(13) |
O(2)-Fe(1)-O(8) | 117.15(19) | O(2)-Fe(1)-O(8) | 106.3(3) |
O(8)-Fe(1)-O(7) | 89.9(2) | O(2)-Fe(1)-N(4) | 107.8(2) |
O(8)-Fe(1)-N(4) | 133.8(2) | O(7)-Fe(1)-N(4) | 87.3(2) |
O(2)-Fe(1)-N(3) | 85.1(2) | O(7)-Fe(1)-N(3) | 153.7(2) |
N(4)-Fe(1)-N(3) | 77.8(3) | O(1)-Fe(2)-O(6) | 113.4(2) |
O(1)-Fe(2)-O(5) | 112.4(3) | O(6)-Fe(2)-O(5) | 89.1(2) |
O(1)-Fe(2)-N(2) | 100.8(2) | O(6)-Fe(2)-N(2) | 85.5(2) |
O(5)-Fe(2)-N(2) | 145.6(3) | O(1)-Fe(2)-N(1) | 100.9(2) |
O(6)-Fe(2)-N(1) | 143.9(2) | O(5)-Fe(2)-N(1) | 87.9(2) |
N(2)-Fe(2)-N(1) | 77.1(3) | O(13)#1-Ba(1)-O(13)#2 | 110.0(5) |
O(13)#1-Ba(1)-O(13) | 134.3(5) | O(13)#2-Ba(1)-O(13) | 87.7(5) |
O(13)#1-Ba(1)-O(13)#3 | 87.7(5) | O(13)#2-Ba(1)-O(13)#3 | 134.3(5) |
O(13)#1-Ba(1)-O(13)#3 | 110.0(5) | O(13)#1-Ba(1)-O(11)#3 | 73.5(3) |
O(13)#2-Ba(1)-O(11)#3 | 149.2(3) | O(13)-Ba(1)-O(11)#3 | 71.2(3) |
O(13)#3-Ba(1)-O(11)#3 | 75.4(3) | O(13)#1-Ba(1)-O(11)#2 | 71.2(3) |
O(13)#2-Ba(1)-O(11)#2 | 75.4(3) | O(13)-Ba(1)-O(11)#2 | 73.5(3) |
O(13)#3-Ba(1)-O(11)#2 | 149.2(3) | O(11)#3-Ba(1)-O(11)#2 | 77.1(4) |
O(13)#1-Ba(1)-O(11) | 149.2(3) | O(13)#2-Ba(1)-O(11) | 73.5(13) |
O(13)-Ba(1)-O(11) | 75.4(3) | O(13)#3-Ba(1)-O(11) | 71.2(3) |
O(11)#3-Ba(1)-O(11) | 120.0(4) | O(11)#2-Ba(1)-O(11) | 136.3(4) |
O(13)#1-Ba(1)-O(11)#1 | 75.4(3) | O(13)#2-Ba(1)-O(11)#1 | 71.2(3) |
O(13)-Ba(1)-O(11)#1 | 149.2(3) | O(13)#3-Ba(1)-O(11)#1 | 73.5(3) |
O(11)#3-Ba(1)-O(11)#1 | 136.3(4) | O(11)#2-Ba(1)-O(11)#1 | 120.0(4) |
O(11)-Ba(1)-O(11)#1 | 77.1(4) | O(4)#4-Ba(2)-O(4)#5 | 99.0(4) |
O(4)#4-Ba(2)-O(4)#6 | 150.6(4) | O(4)#5-Ba(2)-O(4)#6 | 88.4(4) |
O(4)#4-Ba(2)-O(4)#3 | 88.4(4) | O(4)#5-Ba(2)-O(4)#3 | 150.6(4) |
O(4)#6-Ba(2)-O(4)#3 | 99.0(4) | O(4)#4-Ba(2)-O(10)#7 | 72.3(3) |
O(4)#5-Ba(2)-O(10)#7 | 70.7(3) | O(4)#6-Ba(2)-O(10)#7 | 83.7(3) |
O(4)#3-Ba(2)-O(10)#7 | 138.1(3) | O(4)#4-Ba(2)-O(10)#8 | 83.7(3) |
O(4)#5-Ba(2)-O(10)#8 | 138.1(3) | O(4)#6-Ba(2)-O(10)#8 | 72.3(3) |
O(4)#3-Ba(2)-O(10)#8 | 70.7(3) | O(10)#7-Ba(2)-O(10)#8 | 70.5(5) |
O(4)#4-Ba(2)-O(10) | 138.1(3) | O(4)#5-Ba(2)-O(10) | 83.7(3) |
O(4)#6-Ba(2)-O(10) | 70.7(3) | O(4)#3-Ba(2)-O(10) | 72.3(3) |
O(10)#7-Ba(2)-O(10) | 144.3(5) | O(10)#8-Ba(2)-O(10) | 121.5(4) |
O(4)#4-Ba(2)-O(10)#9 | 70.7(3) | O(4)#5-Ba(2)-O(10)#9 | 72.3(3) |
O(4)-Ba(2)-O(10)#9 | 138.1(3) | O(4)-Ba(2)-O(10)#9 | 83.7(3) |
O(10)-Ba(2)-O(10)#9 | 121.5(4) | O(10)-Ba(2)-O(10)#9 | 144.3(5) |
O(10)-Ba(2)-O(10)#9 | 70.5(5) | O(3)-Ba(3)-O(9)#11 | 79.4(4) |
O(3)-Ba(3)-O(3)#10 | 161.8(6) | O(9)#11-Ba(3)-O(3)#10 | 97.1(4) |
O(3)-Ba(3)-O(2W)#10 | 82.5(4) | O(9)#11-Ba(3)-O(2W)#10 | 91.1(5) |
O(3)#10-Ba(3)-O(2W)#10 | 115.5(4) | O(3)-Ba(3)-O(9)#12 | 92.9(4) |
O(9)#11-Ba(3)-O(9)#12 | 115.6(4) | O(3)#10-Ba(3)-O(9)#12 | 72.3(4) |
O(2W)#10-Ba(3)-O(9)#12 | 151.7(4) | O(3)-Ba(3)-O(2W) | 112.6(4) |
O(9)#1-Ba(3)-O(2W) | 159.3(4) | O(3)#10-Ba(3)-O(2W) | 76.6(4) |
O(2W)#10-Ba(3)-O(2W) | 74.6(8) | O(9)#12-Ba(3)-O(2W) | 81.6(4) |
O(3)-Ba(3)-O(4) | 43.6(4) | O(3)-Ba(3)-O(4) | 65.4(3) |
O(9)#11-Ba(3)-O(4) | 118.7(4) | O(3)#10-Ba(3)-O(4) | 122.6(4) |
O(9)#12-Ba(3)-O(4) | 66.1(3) | O(3)-Ba(3)-O(4) | 134.9(3) |
O(3)-Ba(3)-O(4)#10 | 121.1(4) | O(9)#11-Ba(3)-O(4)#10 | 68.7(3) |
O(3)#10-Ba(3)-O(4)#10 | 42.6(4) | O(2W)#10-Ba(3)-O(4)#10 | 143.0(3) |
O(9)#12-Ba(3)-O(4)#10 | 61.8(3) | O(2W)-Ba(3)-O(4)#10 | 114.4(4) |
O(4)-Ba(3)-O(4)#10 | 77.9(4) | O(14)-Na(1)-O(14)#2 | 138.5(7) |
O(14)-Na(1)-O(12)#2 | 68.1(4) | O(14)#2-Na(1)-O(12)#2 | 85.0(4) |
O(14)-Na(1)-O(12) | 85.0(4) | O(14)#2-Na(1)-O(12) | 68.1(4) |
O(12)#2-Na(1)-O(12) | 99.1(5) | O(1W)-Na(2)-O(9)#11 | 92.9(6) |
O(1W)-Na(2)-O(4) | 118(1) | O(9)#11-Na(2)-O(4) | 63.9(3) |
O(1W)-Na(2)-O(10)#3 | 59.5(8) | O(9)#11-Na(2)-O(10)#3 | 97.1(3) |
O(4)-Na(2)-O(10)#3 | 67.5(3) |
对称代码:#1 x, -y-1/2, -z+1/2;#2 -x-1/2, -y-1/2, z;#3 -x-1/2, y, -z+1/2;#4 x+1/2, -y, -z+1/2;#5 -x-1/2, -y, z+1/2;#6 x+1/2, y, z+1/2;#7 -x, -y, z;#8 -x, y, -z+1;#9 x, -y, -z+1;#10 -x-1, -y, z;#11 -x-1/2, -y, z-1/2;#12 x-1/2, y, z-1/2。
Claims (3)
1.Ba/Fe/Na金属和羧酸席夫碱配合物的制备方法,其特征在于包括如下步骤:
杂金属配合物的合成:取二水合氯化钡 0.12 mmol,六水合氯化铁 0.03 mmol,氯化钠0.06 mmol和H4L配体0.03 mmol,放入15 mL聚四氟乙烯反应釜中,以1 mL二甲基甲酰胺,4 mL乙醇和2 mL水为混合溶剂,放置在烘箱中,加热到100 ℃恒温72小时,然后缓慢降到室温即得。
2.按照权利要求1所述的制备方法制备的配合物,其特征在于其化学式为[BaNa(Fe-L)2(µ2 -OH)(H2O)]·DMF·2H2O,它的晶体属于正交晶系,空间群为F222,晶胞参数为a = 31.955(3) Å,b =
65.386(2) Å,c = 12.9570(16) Å,α= 90°,β= 90°,γ = 90°,V =
27072(4) Å3,基本结构是含孔道的三维框架结构。
3.按照权利要求2所述的配合物作为光降解催化剂在材料科学领域中的应用。
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