CN111253584A - Preparation method of d-f heteronuclear bimetallic organic framework material based on single metal coordination polymer - Google Patents

Preparation method of d-f heteronuclear bimetallic organic framework material based on single metal coordination polymer Download PDF

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CN111253584A
CN111253584A CN202010124165.5A CN202010124165A CN111253584A CN 111253584 A CN111253584 A CN 111253584A CN 202010124165 A CN202010124165 A CN 202010124165A CN 111253584 A CN111253584 A CN 111253584A
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杨国平
刘姣
靳晶
张文彦
王尧宇
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Abstract

The invention provides a preparation method of a d-f heteronuclear bimetallic organic framework material based on a single metal coordination polymer; the method comprises the following steps: synthesizing two cases of Ni-and Dy-based single metal coordination polymers MOFs (metal-organic frameworks) respectively MOF1 and MOF2 by using a hydrothermal method; MOF1 and MOF2 are used as precursors and react with dysprosium nitrate and nickel nitrate respectively to successfully prepare two d-f heteronuclear bimetallic organic frameworks HMOF3 and HMOF 4. The method takes monometal MOFs as a precursor to prepare the d-f heteronuclear bimetallic organic framework material HMOFs; the HMOFs material prepared by the method has coordination unsaturated bimetallic nodes and larger porosity, and is expected to be applied in the field of gas adsorption and organic catalysis.

Description

Preparation method of d-f heteronuclear bimetallic organic framework material based on single metal coordination polymer
Technical Field
The invention relates to the field of metal organic frameworks, in particular to a preparation method of a d-f heteronuclear bimetallic organic framework material based on a single metal coordination polymer.
Background
The Heteronuclear Metal Organic Frameworks (HMOFs) are formed by assembling two or more metal ions and organic ligands, and can exert more excellent optical, electric, magnetic and other properties through the interaction between different metal ions. However, most of the reported work to date has focused on the assembly of monometallic coordination polymers constructed from simple lanthanide ions (Ln) or transition metal ions (Tm), and still presents significant challenges for the construction of HMOFs. According to the principle of soft and hard acids and bases (HSAB), lanthanide ions (Ln) and transition metal ions (Tm) have different coordination behaviors, Ln being hard acids and more prone to coordinate with oxygen atoms, and Tm (e.g. ni (ii)) being a fringing acid and prone to coordinate with both N and O atoms, which results in greater competition of different metal ions in HMOFs for the same donor. Therefore, the patent takes 2-imidazolyl-terephthalic acid as a ligand and takes monometal MOFs as a precursor to construct two different types of HMOFs. The two HMOFs have a large number of Lewis acid active sites in the structures, so that the two HMOFs have large application potential in the aspects of organic catalysis and gas adsorption.
Disclosure of Invention
The invention aims to provide a synthesis method for preparing a d-f heteronuclear bimetallic organic framework material by taking 2-imidazolyl-terephthalic acid as a ligand and taking monometal MOFs as a precursor.
The invention is realized by the following technical scheme:
the invention relates to a preparation method of a d-f heteronuclear bimetallic organic framework material based on a single metal coordination polymer, which comprises the following steps: synthesizing two cases of Ni-and Dy-based single metal coordination polymers MOFs (metal-organic frameworks) respectively MOF1 and MOF2 by using a hydrothermal method; MOF1 and MOF2 are used as precursors and react with dysprosium nitrate and nickel nitrate respectively to successfully prepare two d-f heteronuclear bimetallic organic frameworks HMOF3 and HMOF 4.
Preferably, the MOFs 1, MOF2, HMOF3, HMOF4 are of the respective formulae:
MOF1：[Ni(HL)2(H2O)2]，
MOF2：[Dy2(L)3(H2O)2]·4H2O，
HMOF3：[Dy2Ni(L)4(H2O)6]·DMA·H2O，
HMOF4：[Dy2Ni(L)4(H2O)4]·DMA·H2o, wherein the MOF1, the MOF2, the HMOF3 and the HMOF4 belong to a triclinic system, P-1 space group, and the unit cell parameters are shown in Table 1.
TABLE 1
Figure RE-GDA0002451794940000021
Preferably, the MOF1 is specifically: the asymmetric unit comprises 0.5 Ni (II), 1 HL-Ligand and 1 coordinated water molecule; six-coordinate central ion Ni (II) located in distorted octahedron [ NiN ]2O4]In coordination environment, four oxygen atoms are in horizontal direction and respectively come from two coordinated water molecules and carboxyl oxygen atoms in ligand, two nitrogen atoms are in axial position and come from two HL-Ligand molecules in which the Ni (II) ions are all bridged by HL-The ligands form a 1D chain structure parallel to the b-axis.
Preferably, the MOF2 is specifically: the asymmetric unit comprises 1 Dy (III) ion and 1.5 deprotonations L2-Ligand, 1 coordinated water molecule and 2 free water molecules; nine-coordinated Dy1(III) ion in distorted triangular prism [ DyNO8]In the geometric configuration, the eight oxygen atoms are all from 4L2-Carboxyl groups on the ligands, and the carboxyl groups are η1μ1χ1,η3μ2χ3,η2μ2χ2And η2μ1χ2The coordination mode connects two adjacent Dy (III) ions to form a secondary building unit [ Dy (III) ] of the MOF2(COO)6(H2O)2]These adjacent secondary building units then form a 3D network by spatial extension of the ligands.
Preferably, the HMOF3 is, in particular, one whose asymmetric unit comprises 1 dy (iii) ion, 0.5 ni (ii) ion, 2 fully deprotonated L2-Ligand, 3 coordinated water molecules, 0.5 free DMA molecules and 0.5 free waterA molecule; the octadentate Dy (III) ions form a distorted dodecahedron [ DyO ]8]Geometric configuration in which 6 oxygen atoms are from 4L2-The carboxyl group of the ligand, the other 2 oxygen atoms coming from coordinated water molecules; the hexa-coordinated Ni (II) ion is in a distorted octahedron [ NiN ]4O2]In the geometrical configuration, four nitrogen atoms are in horizontal positions, and two oxygen atoms are in axial positions; the two types of metal centers are connected through completely deprotonated ligands to form a three-dimensional porous framework structure with pore channels of the size
Figure RE-GDA0002451794940000032
The porosity was calculated to be 27% using the Platon program.
Preferably, the HMOF4 is specifically: the asymmetric unit consists of1 dy (iii) ion, 0.5 ni (ii) ion, 2 fully deprotonated ligands, 2 coordinated water molecules, 0.5 free DMA molecules and 0.5 free water molecules. HMOF4 differs from HMOF3 in that the Dy (III) ion of HMOF is in nine coordination [ DyO9]And a binuclear metal cluster SBU, namely [ Dy2(COO)6(H2O)2]. Similarly, HMOF4 is an example of a 3D porous frame structure with cell channels of a size of
Figure RE-GDA0002451794940000031
The porosity was 31.5%.
Preferably, the method specifically comprises the following steps:
step 1, synthesizing two monometallic MOF1 and MOF2 by a hydrothermal method;
step 2, weighing 0.05 mmol of MOF1 and 0.1 mmol of dysprosium nitrate, dissolving into 6 ml of DMA solution, and stirring at normal temperature;
and 3, filtering the solution, adding 2 ml of distilled water into the filtrate, stirring again to uniformly mix the solution, transferring the mixture into a small glass bottle, reacting in a constant-temperature oven at 95 ℃ for three days, naturally cooling to room temperature to obtain light green blocky crystals, washing with distilled water, and drying in vacuum to obtain HMOF 3.
And 4, replacing MOF1 with MOF2, replacing the metal salt with cobalt nitrate, and repeating the operation to prepare HMOF 4.
Preferably, in step 2, the stirring time is 0.5 hour.
Preferably, in step 2, the time for stirring again is 0.5 hour.
The invention takes monometal MOFs as a precursor to prepare the d-f heteronuclear bimetallic organic framework material. The HMOFs material has coordination unsaturated bimetallic nodes and larger porosity, and is expected to be applied to the fields of gas adsorption and organic catalysis.
The method of the invention has the following advantages:
(1) the method takes monometal MOFs as a precursor to prepare the d-f heteronuclear bimetallic organic framework material HMOFs; the HMOFs material prepared by the method has coordination unsaturated bimetallic nodes and larger porosity, and is expected to be applied in the field of gas adsorption and organic catalysis.
(2) The method has the advantages of low raw material cost, simple steps, high repetition rate and obvious effect.
(3) The synthesis method adopted by the invention is simple to operate and high in yield, and is expected to be applied to the fields of gas adsorption and organic catalysis.
Drawings
FIG. 1 is a diagram of the coordination environment of a MOF1 material of the invention;
FIG. 2 is a diagram of the coordination environment of a MOF2 material of the invention;
FIG. 3 is a diagram of the coordination environment of the HMOF3 material of the present invention;
FIG. 4 is a three-dimensional stacking diagram of the HMOF3 material of the present invention;
FIG. 5 is a diagram of the coordination environment of the HMOF4 material of the present invention;
FIG. 6 is a three-dimensional stacking view of the HMOF4 material of the present invention;
FIG. 7 is an enlarged three-dimensional packing of the HMOF4 material of the present invention;
FIG. 8 is a powder diffraction diagram of four MOFs of the present invention.
Detailed Description
The present invention will be described in detail with reference to specific examples. It should be noted that the following examples are only illustrative of the present invention, but the scope of the present invention is not limited to the following examples.
The following examples of the present invention relate to a method for preparing a d-f heteronuclear bimetallic organic framework material based on a monometallic coordination polymer, the method comprising: two examples of Ni-and Dy-based single metal coordination polymers MOFs are synthesized by a hydrothermal method, and the powder diffraction patterns of the MOFs are shown in FIG. 8 and are MOF1 and MOF2 respectively; MOF1 and MOF2 are used as precursors and react with dysprosium nitrate and nickel nitrate respectively to successfully prepare two d-f heteronuclear bimetallic organic frameworks HMOF3 and HMOF 4.
Example 1
Step 1, weigh 0.1 mmoles of nickel nitrate and 0.05 mmoles of H2L was dissolved in a mixed solution of3 ml of DMA solution and 2 ml of distilled water, and stirred for 0.5 hour to mix them uniformly.
Step 2, transferring the mixture obtained in the step 1 into a 25 ml stainless steel reaction kettle with a polytetrafluoroethylene lining, reacting for four days at 120 ℃, and cooling to room temperature by a program to obtain green blocky crystals, wherein the green blocky crystals are MOF1 of single metal and have a molecular formula of [ Ni (HL)2(H2O)2]The coordination environment diagram is shown in figure 1.
Step 3, 0.05 mmol of MOF1 and 0.1 mmol of dysprosium nitrate are weighed and dissolved in 6 ml of DMA solution, and the mixture is stirred for 0.5 hour at normal temperature.
And 4, filtering the solution in the step 3, adding 2 ml of distilled water into the filtrate, stirring for 0.5 hour again to uniformly mix the solution, transferring the solution into a 10 ml small glass bottle, putting the small glass bottle into a constant-temperature oven at 95 ℃ for reacting for three days, naturally cooling to room temperature to obtain light green blocky crystals, washing the crystals with distilled water, and performing vacuum drying to prepare HMOF3, wherein the coordination environment diagram is shown in figure 3, and the three-dimensional stacking diagram is shown in figure 4.
Example 2
(1) Weigh 0.1 mmoles of dysprosium nitrate and 0.05 mmoles of H2L was dissolved in a mixed solution of3 ml of DMA solution and 2 ml of distilled water, and stirred for 0.5 hour to mix them uniformlyAnd (4) homogenizing.
(2) Transferring the mixture obtained in the step (1) into a 25 ml stainless steel reaction kettle with a polytetrafluoroethylene lining, reacting for four days at 120 ℃, and carrying out programmed cooling to room temperature to obtain green blocky crystals, wherein the blocky crystals are MOF2 of single metal and have a molecular formula of [ Dy [ ]2(L)3(H2O)2]·4H2And O, the coordination environment diagram of which is shown in figure 2.
(3) 0.05 mmol of MOF2 and 0.1 mmol of nickel nitrate were weighed out and dissolved in 6 ml of DMA solution, and the mixture was stirred at room temperature for 0.5 hour.
(4) And (3) filtering the solution in the step (3), adding 2 ml of distilled water into the filtrate, stirring for 0.5 hour again to uniformly mix the solution, transferring the solution into a 10 ml small glass bottle, putting the small glass bottle into a constant-temperature oven at 95 ℃ for reacting for three days, naturally cooling to room temperature to obtain light green blocky crystals, washing the crystals with distilled water, and performing vacuum drying to prepare HMOF4, wherein the coordination environment diagram is shown in figure 5, and the three-dimensional stacking diagram is shown in figures 6 and 7.
The invention takes monometal MOFs as a precursor to prepare the d-f heteronuclear bimetallic organic framework material. The HMOFs material has coordination unsaturated bimetallic nodes and larger porosity, and is expected to be applied to the fields of gas adsorption and organic catalysis.
The method of the invention has the following advantages: the method takes monometal MOFs as a precursor to prepare the d-f heteronuclear bimetallic organic framework material HMOFs; the HMOFs material prepared by the method has coordination unsaturated bimetallic nodes and larger porosity, and is expected to be applied in the field of gas adsorption and organic catalysis. The method has the advantages of low raw material cost, simple steps, high repetition rate and obvious effect. The synthesis method adopted by the invention is simple to operate and high in yield, and is expected to be applied to the fields of gas adsorption and organic catalysis.
The foregoing description of specific embodiments of the present invention has been presented. It is to be understood that the present invention is not limited to the specific embodiments described above, and that various changes or modifications may be made by one skilled in the art within the scope of the appended claims without departing from the spirit of the invention.

Claims (10)

1. A preparation method of a d-f heteronuclear bimetallic organic framework material based on a single metal coordination polymer is characterized by comprising the following steps: synthesizing two cases of Ni-and Dy-based single metal coordination polymers MOFs (metal-organic frameworks) respectively MOF1 and MOF2 by using a hydrothermal method; MOF1 and MOF2 are used as precursors and react with dysprosium nitrate and nickel nitrate respectively to successfully prepare two d-f heteronuclear bimetallic organic frameworks HMOF3 and HMOF 4.
2. The method for preparing a monometallic coordination polymer-based d-f heteronuclear bimetallic organic framework material of claim 1, wherein the MOFs 1, MOF2, HMOF3 and HMOF4 have the respective formulae:
MOF1：[Ni(HL)2(H2O)2]，
MOF2：[Dy2(L)3(H2O)2]·4H2O，
HMOF3：[Dy2Ni(L)4(H2O)6]·DMA·H2O，
HMOF4：[Dy2Ni(L)4(H2O)4]·DMA·H2O。
3. the method for preparing a monometallic coordination polymer-based d-f heteronuclear bimetallic organic framework material of claims 1 or 2, wherein the MOFs 1, MOFs 2, HMOF3 and HMOF4 all belong to the triclinic system, P-1 space group.
4. The method for preparing a d-f heteronuclear bimetallic organic framework material based on a monometallic coordination polymer according to claim 2, wherein the MOF1 is in particular: the asymmetric unit comprises 0.5 Ni and 1 HL-Ligand and 1 coordinated water molecule; the hexa-coordinated central ion Ni is located in a distorted octahedral coordination environment, with four oxygen atoms in the horizontal direction from two coordinated water molecules and the carboxyloxygen atom in the ligand, respectively, and two nitrogen atoms in the axial position from two HL-Ligand molecule in which Ni is dissociatedAll through bridged HL-The ligands form a 1D chain structure parallel to the b-axis.
5. The method for preparing a d-f heteronuclear bimetallic organic framework material based on a monometallic coordination polymer according to claim 2, wherein the MOF2 is in particular: the asymmetric unit comprises 1 Dy ion and 1.5 deprotonations L2-Ligand, 1 coordinated water molecule and 2 free water molecules; the nine-coordinated Dy1 ion is located in a distorted triangular prism geometry with eight oxygen atoms each from 4L2-Carboxyl groups on the ligands, and the carboxyl groups are η1μ1χ1,η3μ2χ3,η2μ2χ2And η2μ1χ2And the coordination mode connects two adjacent Dy ions to form a secondary building unit of the MOF, and the adjacent secondary building units form a 3D network structure through the spatial extension of the ligand.
6. The method of claim 2, wherein the HMOF3 is HMOF3 comprising 1 Dy ion, 0.5 Ni ion, 2 completely deprotonated L ions2-Ligand, 3 coordinated water molecules, 0.5 free DMA molecules and 0.5 free water molecules; the octadentate Dy ion forms a distorted dodecahedral geometry with 6 oxygen atoms from 4L2-The carboxyl group of the ligand, the other 2 oxygen atoms coming from coordinated water molecules; the hexa-coordinated Ni ions are in a distorted octahedral geometric configuration, four nitrogen atoms of the hexa-coordinated Ni ions are in horizontal positions, and two oxygen atoms of the hexa-coordinated Ni ions are in axial positions; the two types of metal centers are connected through completely deprotonated ligands to form a 3D porous framework structure, and the size of the pore channel of the porous framework structure is
Figure FDA0002393908730000021
The porosity was 27%.
7. The preparation method of the d-f heteronuclear bimetallic organic framework material based on the monometallic coordination polymer as claimed in claim 2, characterized in that the HMOF4 is specifically: the asymmetric unit consists of1 Dy ion, 0.5 Ni ion, 2 completely deprotonated ligands, 2 coordinated water molecules, 0.5 free DMA molecules and 0.5 free water molecules.
8. The method of preparing a monometallic coordination polymer-based d-f heteronuclear bimetallic organic framework material of claim 1, comprising the steps of:
step 1, synthesizing two monometallic MOF1 and MOF2 by a hydrothermal method;
step 2, weighing 0.05 mmol of MOF1 and 0.1 mmol of dysprosium nitrate, dissolving into 6 ml of DMA solution, and stirring at normal temperature;
and 3, filtering the solution, adding 2 ml of distilled water into the filtrate, stirring again to uniformly mix the solution, transferring the mixture into a small glass bottle, reacting in a constant-temperature oven at 95 ℃ for three days, naturally cooling to room temperature to obtain light green blocky crystals, washing with distilled water, and drying in vacuum to obtain HMOF 3.
And 4, replacing MOF1 with MOF2, replacing the metal salt with cobalt nitrate, and repeating the operation to prepare HMOF 4.
9. The method of claim 1, wherein the stirring time in step 2 is 0.5 hours.
10. The method for preparing a d-f heteronuclear bimetallic organic framework material based on a monometallic coordination polymer of claim 1, wherein in step 2, the re-stirring time is 0.5 hour.
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