CN106478694B - 一种锶的配合物及其制备方法 - Google Patents
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- 229910052712 strontium Inorganic materials 0.000 title claims abstract description 25
- CIOAGBVUUVVLOB-UHFFFAOYSA-N strontium atom Chemical compound [Sr] CIOAGBVUUVVLOB-UHFFFAOYSA-N 0.000 title claims abstract description 21
- 238000002360 preparation method Methods 0.000 title claims abstract description 16
- JUJWROOIHBZHMG-UHFFFAOYSA-N Pyridine Chemical compound C1=CC=NC=C1 JUJWROOIHBZHMG-UHFFFAOYSA-N 0.000 claims abstract description 17
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 17
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N EtOH Substances CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 16
- 239000002244 precipitate Substances 0.000 claims abstract description 14
- AHBGXTDRMVNFER-UHFFFAOYSA-L strontium dichloride Chemical compound [Cl-].[Cl-].[Sr+2] AHBGXTDRMVNFER-UHFFFAOYSA-L 0.000 claims abstract description 13
- 229910001631 strontium chloride Inorganic materials 0.000 claims abstract description 9
- 239000002253 acid Substances 0.000 claims abstract description 5
- 238000010438 heat treatment Methods 0.000 claims abstract description 5
- 239000000126 substance Substances 0.000 claims abstract description 4
- WJJMNDUMQPNECX-UHFFFAOYSA-N dipicolinic acid Chemical class OC(=O)C1=CC=CC(C(O)=O)=N1 WJJMNDUMQPNECX-UHFFFAOYSA-N 0.000 claims description 15
- 239000000460 chlorine Substances 0.000 claims description 12
- 238000006243 chemical reaction Methods 0.000 claims description 9
- 239000003446 ligand Substances 0.000 claims description 9
- 239000000047 product Substances 0.000 claims description 7
- 239000007787 solid Substances 0.000 claims description 7
- 125000001309 chloro group Chemical group Cl* 0.000 claims description 5
- 239000013078 crystal Substances 0.000 claims description 5
- 238000005406 washing Methods 0.000 claims description 5
- 229910052801 chlorine Inorganic materials 0.000 claims description 3
- 125000004430 oxygen atom Chemical group O* 0.000 claims description 3
- 150000003222 pyridines Chemical class 0.000 claims description 3
- 125000004433 nitrogen atom Chemical group N* 0.000 claims description 2
- KAESVJOAVNADME-UHFFFAOYSA-N Pyrrole Chemical compound C=1C=CNC=1 KAESVJOAVNADME-UHFFFAOYSA-N 0.000 claims 2
- -1 SrII Ion Chemical class 0.000 claims 2
- 230000001476 alcoholic effect Effects 0.000 claims 1
- SQDFHQJTAWCFIB-UHFFFAOYSA-N n-methylidenehydroxylamine Chemical compound ON=C SQDFHQJTAWCFIB-UHFFFAOYSA-N 0.000 claims 1
- 239000013049 sediment Substances 0.000 claims 1
- 150000001991 dicarboxylic acids Chemical class 0.000 abstract description 7
- 239000000463 material Substances 0.000 abstract description 5
- UMJSCPRVCHMLSP-UHFFFAOYSA-N pyridine Natural products COC1=CC=CN=C1 UMJSCPRVCHMLSP-UHFFFAOYSA-N 0.000 abstract 2
- 150000002500 ions Chemical class 0.000 description 4
- 125000004429 atom Chemical group 0.000 description 3
- 238000003756 stirring Methods 0.000 description 3
- 229910001427 strontium ion Inorganic materials 0.000 description 3
- 230000015572 biosynthetic process Effects 0.000 description 2
- 238000000034 method Methods 0.000 description 2
- 229910052760 oxygen Inorganic materials 0.000 description 2
- 238000003786 synthesis reaction Methods 0.000 description 2
- 229910052784 alkaline earth metal Inorganic materials 0.000 description 1
- 150000001342 alkaline earth metals Chemical class 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 238000013459 approach Methods 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 238000012512 characterization method Methods 0.000 description 1
- 238000004891 communication Methods 0.000 description 1
- 239000011365 complex material Substances 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 150000004696 coordination complex Chemical class 0.000 description 1
- 239000013256 coordination polymer Substances 0.000 description 1
- 229920001795 coordination polymer Polymers 0.000 description 1
- 238000002425 crystallisation Methods 0.000 description 1
- 230000008025 crystallization Effects 0.000 description 1
- 238000013461 design Methods 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000001506 fluorescence spectroscopy Methods 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 238000004020 luminiscence type Methods 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
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- 230000003287 optical effect Effects 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 238000000634 powder X-ray diffraction Methods 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 239000000523 sample Substances 0.000 description 1
- PWYYWQHXAPXYMF-UHFFFAOYSA-N strontium(2+) Chemical compound [Sr+2] PWYYWQHXAPXYMF-UHFFFAOYSA-N 0.000 description 1
- 238000007039 two-step reaction Methods 0.000 description 1
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- C07F—ACYCLIC, CARBOCYCLIC OR HETEROCYCLIC COMPOUNDS CONTAINING ELEMENTS OTHER THAN CARBON, HYDROGEN, HALOGEN, OXYGEN, NITROGEN, SULFUR, SELENIUM OR TELLURIUM
- C07F3/00—Compounds containing elements of Groups 2 or 12 of the Periodic Table
- C07F3/003—Compounds containing elements of Groups 2 or 12 of the Periodic Table without C-Metal linkages
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- C07D213/00—Heterocyclic compounds containing six-membered rings, not condensed with other rings, with one nitrogen atom as the only ring hetero atom and three or more double bonds between ring members or between ring members and non-ring members
- C07D213/02—Heterocyclic compounds containing six-membered rings, not condensed with other rings, with one nitrogen atom as the only ring hetero atom and three or more double bonds between ring members or between ring members and non-ring members having three double bonds between ring members or between ring members and non-ring members
- C07D213/04—Heterocyclic compounds containing six-membered rings, not condensed with other rings, with one nitrogen atom as the only ring hetero atom and three or more double bonds between ring members or between ring members and non-ring members having three double bonds between ring members or between ring members and non-ring members having no bond between the ring nitrogen atom and a non-ring member or having only hydrogen or carbon atoms directly attached to the ring nitrogen atom
- C07D213/60—Heterocyclic compounds containing six-membered rings, not condensed with other rings, with one nitrogen atom as the only ring hetero atom and three or more double bonds between ring members or between ring members and non-ring members having three double bonds between ring members or between ring members and non-ring members having no bond between the ring nitrogen atom and a non-ring member or having only hydrogen or carbon atoms directly attached to the ring nitrogen atom with hetero atoms or with carbon atoms having three bonds to hetero atoms with at the most one bond to halogen, e.g. ester or nitrile radicals, directly attached to ring carbon atoms
- C07D213/78—Carbon atoms having three bonds to hetero atoms, with at the most one bond to halogen, e.g. ester or nitrile radicals
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Abstract
本发明公开了一种锶的配合物及其制备方法，涉及配合物荧光材料领域，其特征在于：锶的配合物的化学式为：[HSr3(pda)3(H2O)3Cl]n，其中pda2‑为吡啶‑2,6‑二羧酸酸根。所述配合物的制备方法：第一步，在2‑吡啶甲醛肟乙醇溶液加入固态吡啶‑2,6‑二羧酸、氯化锶，加热得到白色沉淀，第二步，加水，白色沉淀转化为目标配合物。本发明配合物具有良好的荧光性能，热稳定性好，制备方法简单。
Description
技术领域
本发明属于金属配合物荧光材料领域，具体涉及到一种锶的配合物及其制备方法。
技术背景
高发光性能的荧光配合物在通讯、卫星、雷达、光学计算机和生物分子探针等领域具有巨大的应用前景，因此，这类功能性配合物的分子设计、合成及性质研究具有重要意义。其中碱土金属-有机配位聚合物由于其具有良好的荧光性能得到了广泛的关注。
锶的配合物材料已经被报道，锶离子是一种碱土金属，有非常大的离子半径，可以与配体形成高配合数的配体，锶与配合物复杂的结合，并由不同的结构呈现出不同的性质，展现出优良的潜在性能。吡啶-2,6-二羧酸酸根是一种配体，可以与金属桥连。目前，利用锶、吡啶-2,6-二羧酸制备锶的配合物尚未见报道。
发明内容
本发明的目的就是为市场提供了一种具有良好的荧光性能，热稳定性好，制备方法简单的锶的配合物及其制备方法。
本发明的技术方案是：将氯化锶和吡啶-2,6-二羧酸通过直接混合反应制作而成，锶的配合物的化学式为：[HSr3(pda)3(H2O)3Cl]n，其中pda2-为吡啶-2,6-二羧酸酸根。所述的配合物的结构为氯桥连的三维结构，属于R-3空间群，三方晶系。在不对称单元中，有三个SrII离子，三个pda2-阴离子，三个配位水分子，一个Cl-离子。每一个SrII离子连接着四个pda2-配体中的六个氧原子和一个N原子，一个水分子和C1-离子。SrII离子的构型是一个扭曲的单帽四方反棱柱体。Sr-O的键长从2.623(4)到2.745(4) Å。Sr-N的键长是2.687(5) Å。所有Sr-O和Sr-N键长都与参考文献一致，Cl-与三个锶离子组成三角锥结构，每一个Sr-Cl距离是2.9860(13) Å，Sr-Cl-Sr的键角是114.87(7)o。SrII离子通过两个氧原子连接到相邻的三个SrII离子上，Sr与Sr的距离在4.439到5.095 Å之间。在晶体结构中，pda2-配体连接4个SrII离子形成一个三维网状结构。
上述锶的配合物制备方法的第一步是在2-吡啶甲醛肟乙醇溶液中加入固体吡啶-2,6-二羧酸、氯化锶，加热，得到白色沉淀。第二步，加水，白色沉淀转化为目标配合物，过滤，洗涤，获得产品[HSr3(pda)3(H2O)3Cl]n。合成分成两步，第二步加水是重要的，如果在第一步中直接加水，不能获得目标化合物。两步反应均是将原料混合之后直接反应，操作简便易实施。
上述制备方法中，第一步中的2-吡啶甲醛肟乙醇溶液的浓度为0.08-0.12 mol/L，加入比例为1L的2-吡啶甲醛肟乙醇溶液中加入0.025-0.035 mol吡啶-2,6-二羧酸和0.045-0.055mol化锶，反应温度控制在80～100℃范围内，第二步的加水量为0.35-0.45 L。
进一步的，步骤一中的2-吡啶甲醛肟乙醇溶液的浓度为0.10 mol/L，加入比例为1L 2-吡啶甲醛肟乙醇溶液中加入0.03 mol吡啶-2,6-二羧酸和0.05 mol氯化锶，反应温度控制在90℃，第二步中加水量为0.4 L。
产物样品的荧光光谱数据显示，本发明制备的配合物具有良好的荧光性能，与配体的荧光最大发射波长接近，可以作为荧光材料在材料领域得到应用。其热分析数据显示，该配合物加热后可失去结晶水和侨联的Cl-离子，但骨架直到520左右仍保持稳定，说明其具有良好的热稳定性，为其作为荧光材料的进一步开发应用提供了保证。
附图说明
图1为实施例1制备的Sr-吡啶2,6二羧酸配合物的配位环境图；
图2为实施例1制备的Sr-吡啶2,6二羧酸配合物的粉末X-射线衍射图；
图3为实施例1制备的Sr-吡啶2,6二羧酸配合物的热重曲线图；
图4为实施例1制备的Sr-吡啶2,6二羧酸配合物的固态荧光光谱图；
图5为实施例1制备的Sr-吡啶2,6二羧酸配合物的红外光谱图。
具体实施方式
一种锶的配合物及其制备方法是将氯化锶和吡啶-2,6-二羧酸直接混合反应制作而成，制得锶的配合物的化学式为：[HSr3(pda)3(H2O)3Cl]n，其中pda2-为吡啶-2,6-二羧酸酸根；结构为氯桥连的三维结构，属于R-3空间群，三方晶系；在不对称单元中，有三个SrII离子，三个pda2-阴离子，三个配位水分子，一个Cl-离子；每一个SrII离子连接着四个pda2-配体中的六个氧(O1, O1B, O2C, O3, O3A, O4A)原子和一个N（N1）原子，一个水分子（O5）和C11原子，所述SrII离子的构型是一个扭曲的单帽四方反棱柱体；Sr-O的键长从2.623(4)到2.745(4) Å，Sr-N的键长是2.687(5) Å； Cl-与三个锶离子组成三角锥结构，每一个Sr-Cl距离是2.9860(13) Å，Sr-Cl-Sr的键角是114.87(7)o；SrII离子通过O1和O3原子连接到相邻的三个SrII离子上，Sr与Sr的距离在4.439到5.095 Å之间；在晶体结构中，pda2-配体显示µ 4-η 1:η 2:η 1:η 1:η 1配位模式，并且连接4个SrII离子形成一个三维网状结构。
其制备方法包括两步：第一步是在浓度为0.08～0.12 mol/L的2-吡啶甲醛肟乙醇的1L溶液中加入0.025～0.035 mol固体吡啶-2,6-二羧酸和0.045～0.055 mol氯化锶，加热（反应温度控制在80～100℃范围内），得到白色沉淀；第二步是上述白色沉淀液中加水0.35～0.45 L，白色沉淀即转化为锶的配合物。
实施例一：
第一步，在100 ml浓度为0.1 mol/L的2-吡啶甲醛肟乙醇溶液，加入固体吡啶-2,6-二羧酸0.003 mol、氯化锶0.005 mol，加热，在90℃条件下搅拌，得到白色沉淀；第二步，加水40 mL，白色沉淀转化为目标配合物，过滤，洗涤，获得产品[HSr3(pda)3(H2O)3Cl]n。
表一：产物的主要晶体学数据
表2 重要的键长键角
对称代码: A: y+1/3,-x+y+2/3,-z+2/3; B: -x+1,-y,-z+1; C: y+1,-x+y+1,-z+1; D: x-y,x-1,-z+1; E: -y+1,x-y,z; F: -x+y+1,-x+1,z; G: x-y+1/3,x-1/3,-z+2/3。
晶体结构见图1；
XRD表征见图2；
热重见图3；
荧光见图4；
红外见图5。
实施例二：
第一步，在100 ml浓度为0.08 mol/L的2-吡啶甲醛肟乙醇溶液加入固体吡啶-2,6-二羧酸0.0025 mol、氯化锶0.0045 mol，加热，在温度80℃条件下搅拌，得到白色沉淀；第二步，加水35 mL，白色沉淀转化为目标配合物，过滤，洗涤，获得产品[HSr3(pda)3(H2O)3Cl]n。
实施例三：
第一步，在100 ml浓度为0.12 mol/L的2-吡啶甲醛肟乙醇溶液加入固体吡啶-2,6-二羧酸0.0035 mol、氯化锶0.0055 mol，加热至温度100℃，搅拌，得到白色沉淀，第二步，加水45 mL，白色沉淀转化为目标配合物，过滤，洗涤，获得产品[HSr3(pda)3(H2O)3Cl]n。
Claims (4)
1.一种锶的配合物，其特征在于：锶的配合物的化学式为：[HSr3(pda)3(H2O)3Cl]n，其中pda2-为吡啶-2,6-二羧酸酸根；结构为氯桥连的三维结构，属于R-3空间群，三方晶系；在不对称单元中，有三个SrII离子，三个pda2-阴离子，三个配位水分子，一个Cl-离子；每一个SrII离子连接着四个pda2-配体中的六个氧原子和一个N原子，一个水分子和C1-离子，所述SrII离子的构型是一个扭曲的单帽四方反棱柱体；在晶体结构中，pda2-配体连接4个SrII离子形成一个三维网状结构。
2.如权利要求1所述的一种锶的配合物的制备方法，其特征在于：它是将氯化锶和吡啶-2,6-二羧酸直接混合反应制作而成，其制备方法包括两步：第一步是在2-吡啶甲醛肟乙醇溶液中加入固体吡啶-2,6-二羧酸、氯化锶，加热，得到白色沉淀；第二步是加水，白色沉淀即转化为目标配合物，过滤，洗涤，获得产品[HSr3(pda)3(H2O)3Cl]n。
3. 根据权利要求2所述的一种锶的配合物的制备方法，其特征在于：第一步的2-吡啶甲醛肟乙醇溶液的浓度为0.08～0.12 mol/L，加入比例为1L的2-吡啶甲醛肟乙醇溶液中加入0.025～0.035 mol吡啶-2,6-二羧酸和0.045～0.055 mol氯化锶，反应温度控制在80～100℃范围内；第二步中的加水量为0.35～0.45 L。
4. 根据权利要求2或3所述的一种锶的配合物的制备方法，其特征在于： 第一步中2-吡啶甲醛肟乙醇溶液的浓度为0.10 mol/L，加入比例为1L的2-吡啶甲醛肟乙醇溶液中加入0.03 mol吡啶-2,6-二羧酸和0.05 mol氯化锶，反应温度为90℃，在第二步中加水量为0.4L。
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| KR101251367B1 (ko) * | 2011-01-27 | 2013-04-05 | 중앙대학교 산학협력단 | 열적 안정성이 우수한 신규한 알칼리토금속-유기골격구조 화합물 |
| CN105283445A (zh) * | 2013-07-26 | 2016-01-27 | 昭和电工株式会社 | 金属配位化合物、吸附材、分离材以及1,3-丁二烯的分离方法 |
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| CN105283445A (zh) * | 2013-07-26 | 2016-01-27 | 昭和电工株式会社 | 金属配位化合物、吸附材、分离材以及1,3-丁二烯的分离方法 |
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| Synthesis, Structure, and Luminescent Property of a 3-D Strontium Complex [Sr3（pda）2（Hpda）2（H2O）2]n·2nH2O;Chen Yan-Mei et al.;《结构化学》;20140531;第746-752页 * |
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