CN112694491A - 一种由双氰胺钠与嘧啶甲酸共同构筑的镝金属配合物及其制备方法 - Google Patents
一种由双氰胺钠与嘧啶甲酸共同构筑的镝金属配合物及其制备方法 Download PDFInfo
- Publication number
- CN112694491A CN112694491A CN201911015011.6A CN201911015011A CN112694491A CN 112694491 A CN112694491 A CN 112694491A CN 201911015011 A CN201911015011 A CN 201911015011A CN 112694491 A CN112694491 A CN 112694491A
- Authority
- CN
- China
- Prior art keywords
- pyrimidinecarboxylic acid
- dicyandiamide
- sodium
- sodium dicyandiamide
- constructed
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 title claims abstract description 22
- QGBSISYHAICWAH-UHFFFAOYSA-N dicyandiamide Chemical compound NC(N)=NC#N QGBSISYHAICWAH-UHFFFAOYSA-N 0.000 title claims abstract description 22
- ZFCHNZDUMIOWFV-UHFFFAOYSA-N pyrimidine-2-carboxylic acid Chemical compound OC(=O)C1=NC=CC=N1 ZFCHNZDUMIOWFV-UHFFFAOYSA-N 0.000 title claims abstract description 22
- 229910052708 sodium Inorganic materials 0.000 title claims abstract description 22
- 239000011734 sodium Substances 0.000 title claims abstract description 22
- KBQHZAAAGSGFKK-UHFFFAOYSA-N dysprosium atom Chemical compound [Dy] KBQHZAAAGSGFKK-UHFFFAOYSA-N 0.000 title claims abstract description 13
- 238000002360 preparation method Methods 0.000 title claims abstract description 7
- 239000003446 ligand Substances 0.000 claims abstract description 16
- 238000003756 stirring Methods 0.000 claims abstract description 8
- 238000006243 chemical reaction Methods 0.000 claims abstract description 7
- 239000012153 distilled water Substances 0.000 claims abstract description 4
- BOXVSFHSLKQLNZ-UHFFFAOYSA-K dysprosium(iii) chloride Chemical compound Cl[Dy](Cl)Cl BOXVSFHSLKQLNZ-UHFFFAOYSA-K 0.000 claims abstract description 4
- 238000001914 filtration Methods 0.000 claims abstract description 4
- 239000011259 mixed solution Substances 0.000 claims abstract description 4
- 239000002244 precipitate Substances 0.000 claims abstract description 4
- 239000000047 product Substances 0.000 claims abstract description 4
- 239000002904 solvent Substances 0.000 claims abstract description 4
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 4
- 239000000203 mixture Substances 0.000 claims abstract description 3
- 239000000126 substance Substances 0.000 claims abstract description 3
- 238000000034 method Methods 0.000 claims description 5
- 238000002329 infrared spectrum Methods 0.000 claims description 4
- 238000010521 absorption reaction Methods 0.000 claims description 2
- 238000002156 mixing Methods 0.000 claims description 2
- 239000000243 solution Substances 0.000 claims 1
- 230000015572 biosynthetic process Effects 0.000 abstract description 2
- 238000003786 synthesis reaction Methods 0.000 abstract description 2
- 229910052761 rare earth metal Inorganic materials 0.000 description 12
- 150000002910 rare earth metals Chemical class 0.000 description 6
- KAESVJOAVNADME-UHFFFAOYSA-N Pyrrole Chemical compound C=1C=CNC=1 KAESVJOAVNADME-UHFFFAOYSA-N 0.000 description 5
- -1 rare earth metal ions Chemical class 0.000 description 5
- 230000000694 effects Effects 0.000 description 3
- IJGRMHOSHXDMSA-UHFFFAOYSA-N nitrogen Substances N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 3
- XYFCBTPGUUZFHI-UHFFFAOYSA-N Phosphine Chemical compound P XYFCBTPGUUZFHI-UHFFFAOYSA-N 0.000 description 2
- JUJWROOIHBZHMG-UHFFFAOYSA-N Pyridine Chemical compound C1=CC=NC=C1 JUJWROOIHBZHMG-UHFFFAOYSA-N 0.000 description 2
- 150000001638 boron Chemical class 0.000 description 2
- 229910052799 carbon Inorganic materials 0.000 description 2
- 238000003379 elimination reaction Methods 0.000 description 2
- 229910052751 metal Inorganic materials 0.000 description 2
- 239000002184 metal Substances 0.000 description 2
- 229910021645 metal ion Inorganic materials 0.000 description 2
- 229910052757 nitrogen Inorganic materials 0.000 description 2
- 125000002524 organometallic group Chemical group 0.000 description 2
- 229910052723 transition metal Inorganic materials 0.000 description 2
- 150000003624 transition metals Chemical class 0.000 description 2
- ROFVEXUMMXZLPA-UHFFFAOYSA-N Bipyridyl Chemical group N1=CC=CC=C1C1=CC=CC=N1 ROFVEXUMMXZLPA-UHFFFAOYSA-N 0.000 description 1
- UGFAIRIUMAVXCW-UHFFFAOYSA-N Carbon monoxide Chemical compound [O+]#[C-] UGFAIRIUMAVXCW-UHFFFAOYSA-N 0.000 description 1
- 229910052693 Europium Inorganic materials 0.000 description 1
- 239000002841 Lewis acid Substances 0.000 description 1
- VVQNEPGJFQJSBK-UHFFFAOYSA-N Methyl methacrylate Chemical compound COC(=O)C(C)=C VVQNEPGJFQJSBK-UHFFFAOYSA-N 0.000 description 1
- 101100518501 Mus musculus Spp1 gene Proteins 0.000 description 1
- ZLMJMSJWJFRBEC-UHFFFAOYSA-N Potassium Chemical class [K] ZLMJMSJWJFRBEC-UHFFFAOYSA-N 0.000 description 1
- 229910052771 Terbium Inorganic materials 0.000 description 1
- 230000004913 activation Effects 0.000 description 1
- 150000001336 alkenes Chemical class 0.000 description 1
- 150000001412 amines Chemical class 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 229910002091 carbon monoxide Inorganic materials 0.000 description 1
- 238000006555 catalytic reaction Methods 0.000 description 1
- 239000011365 complex material Substances 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 150000004678 hydrides Chemical class 0.000 description 1
- 150000002466 imines Chemical class 0.000 description 1
- 150000007517 lewis acids Chemical class 0.000 description 1
- 239000000696 magnetic material Substances 0.000 description 1
- 230000005389 magnetism Effects 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 125000004433 nitrogen atom Chemical group N* 0.000 description 1
- JRZJOMJEPLMPRA-UHFFFAOYSA-N olefin Natural products CCCCCCCC=C JRZJOMJEPLMPRA-UHFFFAOYSA-N 0.000 description 1
- 239000013110 organic ligand Substances 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 125000004430 oxygen atom Chemical group O* 0.000 description 1
- 229910000073 phosphorus hydride Inorganic materials 0.000 description 1
- 229920000642 polymer Polymers 0.000 description 1
- 229910052700 potassium Inorganic materials 0.000 description 1
- 239000011591 potassium Substances 0.000 description 1
- 125000002924 primary amino group Chemical group [H]N([H])* 0.000 description 1
- UMJSCPRVCHMLSP-UHFFFAOYSA-N pyridine Natural products COC1=CC=CN=C1 UMJSCPRVCHMLSP-UHFFFAOYSA-N 0.000 description 1
- 150000003233 pyrroles Chemical class 0.000 description 1
- 239000000758 substrate Substances 0.000 description 1
- 238000009475 tablet pressing Methods 0.000 description 1
Images
Classifications
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07F—ACYCLIC, CARBOCYCLIC OR HETEROCYCLIC COMPOUNDS CONTAINING ELEMENTS OTHER THAN CARBON, HYDROGEN, HALOGEN, OXYGEN, NITROGEN, SULFUR, SELENIUM OR TELLURIUM
- C07F5/00—Compounds containing elements of Groups 3 or 13 of the Periodic Table
- C07F5/003—Compounds containing elements of Groups 3 or 13 of the Periodic Table without C-Metal linkages
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
Abstract
本发明涉及一种由双氰胺钠与嘧啶甲酸共同构筑的镝金属配合物及其制备方法。配合物的化学组成含有双氰胺钠与嘧啶甲酸(Hpmc)配体。合成方案为按计量比分别将双氰胺钠与DyCl3·6H2O溶于蒸馏水,常温搅拌30min,然后再按照计量比加入嘧啶甲酸配体,常温搅拌1h,将反应后的混合溶液过滤,去除沉淀,挥发溶剂,大约3天后可以析出目标产品。双氰胺钠与嘧啶甲酸、DyCl3·6H2O的质量之比为:1∶4.10∶2.88。
Description
技术领域
本发明涉及一种由双氰胺钠与嘧啶甲酸共同构筑的镝金属配合物及其制备方法,属于金属配合物科学及技术领域。
技术背景
由金属离子和有机配体构筑的金属-有机配合物材料因其结构多样,性质独特,在气体存储、光电子材料、磁性材料及催化等领域具有广泛的应用前景。相对于d族过渡金属有机配合物及主族金属有机配合物,稀土金属有机配合物的性质有明显的差异,这是由于稀土金属离子具有半径大、配位数高的特点,更有利于底物的配位及活化。4f轨道由于受到极强的屏蔽作用不参与成键,d族的18电子规则在稀土金属有机化学中不适用,也不易发生d族过渡金属有机配合物化学中常见的氧化加成和还原消除反应。稀土元素虽属于副族元素,但稀土-碳σ键、稀土-氮σ键却具有较强的离子性,有好的反应活性。稀土离子属于硬Lewis酸,易于和含N、O原子的硬碱配体配位,表现出强的亲氧性,而与有机膦、烯烃及一氧化碳等软碱配位作用弱[钱长涛等.化学学报,2014,72(8):883-905.]。
在稀土金属有机配合物中,稀土元素与含氮杂环配体形成的配合物是种重要研究方向。例如以吡啶及其衍生物为配体,首都师范大学的杨晓东等[杨晓东.首都师范大学学报.2009,No2,21-24.]选择铕离子及铽离子合成了具有较高量子效率的含联吡啶单元结构的八配位荧光性稀土配合物;以吡咯为配体,Arnold等采用取代吡咯双齿配体合成了亚胺吡咯基稀土烷基配合物,两个配体中的四个氮原子均以η1模式与金属离子配位,该配合物单组分高活性高选择性催化甲基丙烯酸甲酯聚合,聚合物的等规度高达94.8%[Cui,C.Etc.Organometallics 2003,22,3357.];以三吡唑硼盐(Tp)作为三齿氮配体,Takats等通过合成得到了一系列含Tp配体的两价稀土配合物,三价稀土烷基配合物,胺基配合物和氢化物。与此同时,Takats和Anwander等通过Tp钾盐与La(AlMe3)3反应合成了镧桥联碳卡宾配合物[Litlabo,R.Etc.Angew.Chem.Int.Ed.2008,47,9560.],通过胺消除反应合成了异双金属配合物(Tp)Yb(II)(AlR4)(R=Me,Et)[Litlabo,R.Etc.Organometallics 2009,28,6750.]。
目前以双氰胺钠与嘧啶甲酸为配体的稀土金属配合物研究较少,因而具有很大的发展空间。
发明内容
本发明的目的在于提供了一种由双氰胺钠与嘧啶甲酸共同构筑的镝金属配合物及其制备方法,在荧光、磁性等方面有很好的应用前景。
本发明提供的镝金属配合物的化学组成中含有双氰胺钠与2-嘧啶甲酸(Hpmc)配体。
本发明公开的镝金属配合物的红外光谱如图1所示,其特征在于它的红外光谱的特征吸收峰如下:3222(s)cm-1,2291(m)cm-1,2224(w)cm-1,2163(s)cm-1,1635(s)cm-1,1575(m)cm-1,1559(m)cm-1,1451(w)cm-1,1383(s)cm-1,1357(m)cm-1,1284(w)cm-1,1264(w)cm-1,1219(w)cm-1,1192(w)cm-1,1019(w)cm-1,873(w)cm-1。
本发明的制备方法如下:
按计量比分别将双氰胺钠与DyCl3·6H2O溶于蒸馏水,常温搅拌30min,然后再按照计量比加入嘧啶甲酸配体,常温搅拌1h,将反应后的混合溶液过滤,去除沉淀,挥发溶剂,大约3天后可以析出目标产品。
双氰胺钠与嘧啶甲酸、DyCl3·6H2O的质量之比为:1∶4.10∶2.88。
附图说明
图1:配合物的红外光谱图;
具体实施方式
实施例1配合物的合成:
按计量比分别将双氰胺钠(0.0089g,0.1mmol)与DyCl3·6H2O(0.0365g,0.1mmol)溶于蒸馏水,常温搅拌30min,然后再按照计量比加入嘧啶甲酸配体(0.0248g,0.2mmol),常温搅拌1h,将反应后的混合溶液过滤,去除沉淀,挥发溶剂,大约3天后可以析出目标产品。双氰胺钠与嘧啶甲酸、DyCl3·6H2O的质量之比为:1∶4.10∶2.88。
实施例2配合物的红外光谱测定:
配合物的红外光谱测定采用KBr压片法,用Nicolet330FT-IR红外光谱仪在4000~500cm-1范围内录得,具体峰值见图1。
Claims (5)
1.一种由双氰胺钠与嘧啶甲酸共同构筑的镝金属配合物及其制备方法,该配合物的化学组成中含有双氰胺钠与2-嘧啶甲酸(Hpmc)配体。
2.根据权利要求1所述的由双氰胺钠与嘧啶甲酸共同构筑的镝金属配合物,其特征在于它的红外光谱的特征吸收峰如下:3222(s)cm-1,2291(m)cm-1,2224(w)cm-1,2163(s)cm-1,1635(s)cm-1,1575(m)cm-1,1559(m)cm-1,1451(w)cm-1,1383(s)cm-1,1357(m)cm-1,1284(w)cm-1,1264(w)cm-1,1219(w)cm-1,1192(w)cm-1,1019(w)cm-1,873(w)cm-1。
3.根据权利要求1所述的双氰胺钠与嘧啶甲酸共同构筑的镝金属配合物的制备方法,其特征在于它包括以下步骤:
1)按计量比分别将双氰胺钠与DyCl3·6H2O溶于蒸馏水,常温搅拌30min;
2)然后再按照计量比加入嘧啶甲酸配体,常温搅拌1h;
3)将反应后的混合溶液过滤,去除沉淀,挥发溶剂,大约3天后可以析出目标产品。
4.根据权利要求3所述的由双氰胺钠与嘧啶甲酸共同构筑的镝金属配合物的制备方法,其特征在于所述的双氰胺钠与嘧啶甲酸、DyCl3·6H2O的质量之比为:1∶4.10∶2.88。
5.根据权利要求3所述的由双氰胺钠与嘧啶甲酸共同构筑的镝金属配合物的制备方法,其特征在于所述的反应条件是在常温条件下,溶液挥发。
Priority Applications (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
CN201911015011.6A CN112694491A (zh) | 2019-10-22 | 2019-10-22 | 一种由双氰胺钠与嘧啶甲酸共同构筑的镝金属配合物及其制备方法 |
Applications Claiming Priority (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
CN201911015011.6A CN112694491A (zh) | 2019-10-22 | 2019-10-22 | 一种由双氰胺钠与嘧啶甲酸共同构筑的镝金属配合物及其制备方法 |
Publications (1)
Publication Number | Publication Date |
---|---|
CN112694491A true CN112694491A (zh) | 2021-04-23 |
Family
ID=75505389
Family Applications (1)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
CN201911015011.6A Pending CN112694491A (zh) | 2019-10-22 | 2019-10-22 | 一种由双氰胺钠与嘧啶甲酸共同构筑的镝金属配合物及其制备方法 |
Country Status (1)
Country | Link |
---|---|
CN (1) | CN112694491A (zh) |
-
2019
- 2019-10-22 CN CN201911015011.6A patent/CN112694491A/zh active Pending
Similar Documents
Publication | Publication Date | Title |
---|---|---|
Hümmer et al. | Uranium Tetrakis-Aryloxide Derivatives Supported by Tetraazacyclododecane: Synthesis of Air-Stable, Coordinatively-Unsaturated U (IV) and U (V) Complexes | |
Huang et al. | From dinuclear, chain to sheet: Synthesis, structural characterization and luminescence properties of silver (I) complexes based on rigid and flexible pyridyl-containing ligands | |
Carlucci et al. | Nanoporous three-dimensional networks topologically related to Cooperite from the self-assembly of copper (I) centres and the “square-planar” building block 1, 2, 4, 5-tetracyanobenzene | |
Anga et al. | Synthesis, structure and reactivity study of magnesium amidinato complexes derived from carbodiimides and N, N′-bis (2, 6-diisopropylphenyl)-1, 4-diaza-butadiene ligands | |
CN112694494A (zh) | 一种由呋喃四酸构筑的铽金属配合物及其制备方法 | |
Joshi et al. | Cu–tetracatechol metallopolymer catalyst for three component click reactions and β-borylation of α, β-unsaturated carbonyl compounds | |
CN112694491A (zh) | 一种由双氰胺钠与嘧啶甲酸共同构筑的镝金属配合物及其制备方法 | |
CN112694496A (zh) | 一种由双氰胺钠与嘧啶甲酸共同构筑的铽金属配合物及其制备方法 | |
CN110615804A (zh) | 一种由双氰胺钠与嘧啶甲酸共同构筑的铕金属配合物及其制备方法 | |
CN110615806A (zh) | 一种由双氰胺钠与嘧啶甲酸共同构筑的钐金属配合物及其制备方法 | |
CN108069910A (zh) | 一种由嘧啶甲酸构筑的铕金属配合物及其制备方法 | |
CN108069990A (zh) | 一种由嘧啶甲酸构筑的钐金属配合物及其制备方法 | |
CN107417740A (zh) | 一种一维钴配合物及其制备方法和应用 | |
Evans et al. | Synthesis of di-and trinuclear methyl osmium complexes via cis-hydridomethyltetracarbonylosmium | |
CN108069988A (zh) | 一种由嘧啶甲酸构筑的钕金属配合物及其制备方法 | |
Chen et al. | A new anionic metal–organic framework showing tunable emission by lanthanide (III) doping and highly selective CO 2 adsorption properties | |
CN108373477B (zh) | 一种双核镉有机骨架配合物及其制备方法和应用 | |
CN112694493A (zh) | 一种由嘧啶甲酸构筑的钆金属配合物及其制备方法 | |
CN112694495A (zh) | 一种由呋喃四酸构筑的钐金属配合物及其制备方法 | |
CN110615805A (zh) | 一种由2-氨基嘧啶-4,6-二甲酸构筑的铽金属配合物及其制备方法 | |
CN112694492A (zh) | 一种由呋喃四酸构筑的铕金属配合物及其制备方法 | |
CN110615760A (zh) | 一种由2-氨基嘧啶-4,6-二甲酸构筑的钬金属配合物及其制备方法 | |
CN110615761A (zh) | 一种由2-氨基嘧啶-4,6-二甲酸构筑的钐金属配合物及其制备方法 | |
Chen et al. | Tripodal bis (imidazole)-based ligands and their chelation to copper (II) | |
Huang et al. | Synthesis, structure, and catalytic performance of heterobimetallic coordination polymers with β-diketone containing imidazole group |
Legal Events
Date | Code | Title | Description |
---|---|---|---|
PB01 | Publication | ||
PB01 | Publication | ||
WD01 | Invention patent application deemed withdrawn after publication | ||
WD01 | Invention patent application deemed withdrawn after publication |
Application publication date: 20210423 |