CN103880871B - A kind of synthetic method by the double interpenetrating structure cadmium coordination polymer of 0D → 2D - Google Patents
A kind of synthetic method by the double interpenetrating structure cadmium coordination polymer of 0D → 2D Download PDFInfo
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- CN103880871B CN103880871B CN201410133763.3A CN201410133763A CN103880871B CN 103880871 B CN103880871 B CN 103880871B CN 201410133763 A CN201410133763 A CN 201410133763A CN 103880871 B CN103880871 B CN 103880871B
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Abstract
By a synthetic method for the double interpenetrating structure cadmium coordination polymer of 0D → 2D, it relates to a kind of cadmium coordination polymer and preparation method thereof.The object of the invention is to be subject to additive factors impact when ligand polymer is synthesized and the cadmium coordination polymer that do not synthesize two-dirnentional structure to solve, and in building-up process, additive cost is high, the problem that products collection efficiency is low.A kind of molecular formula with the double interpenetrating structure cadmium coordination polymer of 2D of the present invention is [Cd (C
10h
7n
2o
2)
2]
n.Synthetic method of the present invention is: on the synthesis condition basis of 0D cadmium complex, add oxalic acid molecule as additive, serve the effect of induced product structural changes, obtain the double interpenetrating structure cadmium coordination polymer of 2D, but oxalic acid is not present among product.The double interpenetrating structure cadmium coordination polymer of this 2D of the present invention can be used as metal organic blue luminescent material and uses.The present invention is applied to luminous organic material preparation field.
Description
Technical field
The present invention relates to a kind of cadmium coordination polymer and preparation method thereof.
Background technology
Metal organic coordination polymer is paid close attention to widely because it receives people in the potential using value of the various fields such as gas storage and catalysis.Numerous research shows, numerous aspect is depended in the synthesis of this kind of material, as the shape of part, reaction solvent, template and additive etc.When forming ligand polymer, the general skeleton expecting the high dimension of formation.Because the skeleton of 1D or 0D is unfavorable for when piling up forming large duct.And the skeleton of high dimension is also better than the skeleton of low dimension in stability.Therefore adding some ion and molecule when synthesizing ligand polymer, ligand polymer structure can be induced to change, but mechanism wherein and reaction rule need to explore.Additive to crystal formation shock absorption and inducing action report be not also a lot, we attempt additive to be incorporated in the synthetic system of ligand polymer, be conducive to exploring the impact of additive on ligand polymer structure further, thus the synthesis ligand polymer with high dimension novel structure more.
Summary of the invention
The object of the invention is to be subject to additive factors impact when ligand polymer is synthesized and the cadmium coordination polymer that do not synthesize two-dirnentional structure to solve, and in building-up process, additive cost is high, the problem that products collection efficiency is low.And provide a kind of synthetic method by the double interpenetrating structure cadmium coordination polymer of 0D → 2D.
One of the present invention is subject to additive factors impact by the double interpenetrating structure cadmium coordination polymer of 0D → 2D, and the one of present embodiment is subject to additive factors impact by the double interpenetrating structure cadmium coordination polymer of 0D → 2D, and its molecular formula is [Cd (C
10h
7n
2o
2)
2]
n, wherein said polymer formulae is:
wherein said n is positive integer.
The 4-imidazolyl phenylformic acid cadmium complex of 0D of the present invention is with [Cd (C
10h
7n
2o
2)
2(H
2o)
4]
nfor structural unit, be in distortion octahedral coordination environment by cadmium ion, the atom N in part participates in coordination.
In the 4-imidazolyl phenylformic acid cadmium coordination polymer of 2D of the present invention, be connected to form 1D " undaform " chain-like structure by the coordinating oxygen atoms of a 4-imidazolyl phenylformic acid part and nitrogen-atoms between two adjacent cadmium ions, be connected to form another 1D " undaform " chain-like structure by the coordinating oxygen atoms of another 4-imidazolyl phenylformic acid part and nitrogen-atoms between two cadmium ions simultaneously.Interconnection formation 2D net grid structure between adjacent chain, its duct size is
because its duct is large and without free small molecules, in order to keep the stability of skeleton, make 2D cadmium coordination polymer define double interpenetrating structure.
From topological angle analysis, if the organic ligand in 2D structure to be reduced to a node, each 4-imidazolyl phenylformic acid part connects two metals, each central metal connects four 4-imidazolyl phenylformic acid parts, infinitely repeat in this way, define the 2D interpenetrating structure that has double IPN (4,4)-connection.
Of the present invention a kind of be subject to additive factors impact realized by following steps by 0D → 2D double interpenetrating structure cadmium coordination polymer synthetic method:
4-imidazolyl phenylformic acid, oxalic acid and four nitric hydrate cadmiums are placed in solvent, stirred at ambient temperature is to mixing, put into the stainless steel cauldron that liner is tetrafluoroethylene, react at temperature is 100 ~ 180 DEG C after 2 ~ 6 days and be down to room temperature, obtain light brown bulk crystals, be 0D cadmium complex; Wherein, the mol ratio of four nitric hydrate cadmiums, 4-imidazolyl phenylformic acid and oxalic acid is 1:(0.5 ~ 3): (0.5 ~ 2); Solvent is 1mL:(0.0008 ~ 0.0063 with the volume mass ratio of oxalic acid) g.
The present invention includes following effective income:
1, the productive rate of preparation method of the present invention is 60% ~ 70%.
2, the present invention adds oxalic acid molecule as additive on the synthesis condition basis of 0D cadmium complex, serves the effect of induced product structural changes, obtain the double interpenetrating structure cadmium coordination polymer of 2D, but oxalic acid is not present among product.Oxalic acid molecule is not only cheap, and as the sensual pleasure group of luminescence, can regulate and control the light emitting region of ligand polymer well.
3, the 2D double interpenetrating structure cadmium coordination polymer that the present invention obtains has good blue luminescent properties, gathers around and has broad application prospects.Under room temperature solid, take 332nm as excitation wavelength, the strongest emission peak is positioned at 463nm, and the double interpenetrating structure cadmium coordination polymer of 2D presents blue-fluorescence clearly to utilize XYZ chromaticity diagram to determine, color is pure.In the present invention, the solid state fluorescence attenuation process of the double interpenetrating structure cadmium coordination polymer of 2D comprises two component τ
1and τ
2, its value is 1.09 μ s and 10.90 μ s respectively.
4, the present invention uses containing N, the organic ligand 4-imidazolyl phenylformic acid of O heterocycle and four nitric hydrate cadmiums are under hydrothermal conditions, with the addition of inexpensive additive oxalic acid molecule to react, successfully prepare the double interpenetrating structure cadmium coordination polymer of a routine 2D, preparation method is simple, synthesis cost is low, and products collection efficiency is high.
Accompanying drawing explanation
Fig. 1 is the basic structural unit figure of the 0D cadmium complex of test synthesis;
Fig. 2 is the molecular structural formula of the double interpenetrating structure cadmium coordination polymer of 2D of test synthesis;
Fig. 3 is the one-dimensional chain structure iron of the double interpenetrating structure cadmium coordination polymer of 2D of test synthesis;
Fig. 4 is the two-dimentional interpenetrating structure figure of the 2D double interpenetrating structure cadmium coordination polymer of test synthesis;
Fig. 5 be test synthesis 2D double interpenetrating structure cadmium coordination polymer two-dimentional interpenetrating structure topological diagram (tie point 1 represent be central metal cadmium ion, tie point 2 represent be 4-imidazolyl phenylformic acid part);
Fig. 6 is the solid state fluorescence spectrogram of the double interpenetrating structure cadmium coordination polymer of 2D of test synthesis;
Fig. 7 is the solid state fluorescence chromaticity diagram of the double interpenetrating structure cadmium coordination polymer of 2D of test synthesis; Wherein, 1 is green; 2 is blue-greenish colour; 3 is blue; 4 is pink colour; 5 is red; 6 is orange; 7 is yellow; 8 is white;
Fig. 8 is the solid state fluorescence life curve figure of the double interpenetrating structure cadmium coordination polymer of 2D of test synthesis.
Embodiment
Technical solution of the present invention is not limited to following cited embodiment, also comprises the arbitrary combination between each embodiment.
Embodiment one: the one of present embodiment is subject to additive factors impact by the double interpenetrating structure cadmium coordination polymer of 0D → 2D, the one of present embodiment is subject to additive factors impact by the double interpenetrating structure cadmium coordination polymer of 0D → 2D, and its molecular formula is [Cd (C
10h
7n
2o
2)
2]
n, wherein said polymer formulae is:
wherein said n is positive integer.
The 4-imidazolyl phenylformic acid cadmium complex of the 0D of present embodiment is with [Cd (C
10h
7n
2o
2)
2(H
2o)
4]
nfor structural unit, be in distortion octahedral coordination environment by Cd (II) ion, the atom N in part participates in coordination.
Be connected to form 1D " undaform " chain-like structure by the coordinating oxygen atoms of a 4-imidazolyl phenylformic acid part and nitrogen-atoms between two adjacent cadmium ions, be connected to form another 1D " undaform " chain-like structure by the coordinating oxygen atoms of another 4-imidazolyl phenylformic acid part and nitrogen-atoms between two cadmium ions simultaneously.Interconnection formation 2D net grid structure between adjacent chain, its duct size is
because its duct is large and without free small molecules, in order to keep the stability of skeleton, make 2D cadmium coordination polymer define double interpenetrating structure.
From topological angle analysis, if the organic ligand in 2D structure to be reduced to a node, each 4-imidazolyl phenylformic acid part connects two metals, each central metal connects four 4-imidazolyl phenylformic acid parts, infinitely repeat in this way, define the 2D interpenetrating structure that has double IPN (4,4)-connection.
Present embodiment comprises following effective income:
1, present embodiment adds oxalic acid molecule as additive on the synthesis condition basis of 0D cadmium complex, serves the effect of induced product structural changes, obtain the double interpenetrating structure cadmium coordination polymer of 2D, but oxalic acid is not present among product.Oxalic acid molecule is not only cheap, and as the sensual pleasure group of luminescence, can regulate and control the light emitting region of ligand polymer well.
2, the 2D double interpenetrating structure cadmium coordination polymer that present embodiment obtains has good blue luminescent properties, gathers around and has broad application prospects.Under room temperature solid, take 332nm as excitation wavelength, the strongest emission peak is positioned at 463nm, and the double interpenetrating structure cadmium coordination polymer of 2D presents blue-fluorescence clearly to utilize XYZ chromaticity diagram to determine, color is pure.In the present invention, the solid state fluorescence attenuation process of the double interpenetrating structure cadmium coordination polymer of 2D comprises two component τ
1and τ
2, its value is 1.09 μ s and 10.90 μ s respectively.
Embodiment two: present embodiment and embodiment one unlike: containing a central metal cadmium ion in described polymkeric substance basic structural unit, two 4-imidazolyl phenylformic acid parts; Wherein, central metal cadmium ion presents hexa-coordinate octoploids structure, and from the Sauerstoffatom of two 4-imidazolyl phenylformic acid parts and nitrogen-atoms coordination Cheng Jian.Other is identical with embodiment one.
Embodiment three: present embodiment and embodiment one or two unlike: described central metal cadmium ion presents hexa-coordinate octoploids structure.Other is identical with embodiment one or two.
Embodiment four: the one of present embodiment is subject to additive factors impact and is carried out according to the following steps by 0D → 2D double interpenetrating structure cadmium coordination polymer synthetic method:
4-imidazolyl phenylformic acid, oxalic acid and four nitric hydrate cadmiums are placed in solvent, stirred at ambient temperature is to mixing, put into the stainless steel cauldron that liner is tetrafluoroethylene, react at temperature is 100 ~ 180 DEG C after 2 ~ 6 days and be down to room temperature, obtain light brown bulk crystals, be 0D cadmium complex; Wherein, the mol ratio of four nitric hydrate cadmiums, 4-imidazolyl phenylformic acid and oxalic acid is 1:(0.5 ~ 3): (0.5 ~ 2); Solvent is 1mL:(0.0008 ~ 0.0063 with the volume mass ratio of oxalic acid) g.
Present embodiment comprises following beneficial effect:
1, the productive rate of the preparation method of present embodiment is about 65%.
2, present embodiment adds oxalic acid molecule as additive on the synthesis condition basis of 0D cadmium complex, serves the effect of induced product structural changes, obtain the double interpenetrating structure cadmium coordination polymer of 2D, but oxalic acid is not present among product.Oxalic acid molecule is not only cheap, and as the sensual pleasure group of luminescence, can regulate and control the light emitting region of ligand polymer well.
3, the 2D double interpenetrating structure cadmium coordination polymer that present embodiment obtains has good blue luminescent properties, gathers around and has broad application prospects.Under room temperature solid, take 332nm as excitation wavelength, the strongest emission peak is positioned at 463nm, and the double interpenetrating structure cadmium coordination polymer of 2D presents blue-fluorescence clearly to utilize XYZ chromaticity diagram to determine, color is pure.In the present invention, the solid state fluorescence attenuation process of the double interpenetrating structure cadmium coordination polymer of 2D comprises two component τ
1and τ
2, its value is 1.09 μ s and 10.90 μ s respectively.
4, present embodiment uses containing N, the organic ligand 4-imidazolyl phenylformic acid of O heterocycle and four nitric hydrate cadmiums are under hydrothermal conditions, with the addition of inexpensive additive oxalic acid molecule to react, successfully prepare the double interpenetrating structure cadmium coordination polymer of a routine 2D, preparation method is simple, synthesis cost is low, and products collection efficiency is high.
Embodiment five: present embodiment and embodiment four unlike: four described nitric hydrate cadmiums and 4-imidazolyl phenylformic acid mol ratio are 2:1.Other parameter is identical with embodiment four.
Embodiment six: present embodiment and embodiment four or five unlike: described reacts 6 days under the condition of temperature 120 DEG C.Other parameter is identical with embodiment four or five.
Embodiment seven: one of present embodiment and embodiment four to six unlike: described solvent is distilled water.Other step and parameter identical with one of embodiment four to six.
Embodiment eight: one of present embodiment and embodiment four to seven unlike: the mol ratio of described four nitric hydrate cadmiums, 4-imidazolyl phenylformic acid and oxalic acid is 1:(0.5 ~ 2.5): (0.5 ~ 1.5).Other parameter is identical with one of embodiment four to seven.
Embodiment nine: one of present embodiment and embodiment four to eight unlike: the mol ratio of described four nitric hydrate cadmiums, 4-imidazolyl phenylformic acid and oxalic acid is 1:(0.5 ~ 2): (0.5 ~ 1).Other parameter is identical with one of embodiment four to eight.
Embodiment ten: one of present embodiment and embodiment four to nine unlike: the mol ratio of described four nitric hydrate cadmiums, 4-imidazolyl phenylformic acid and oxalic acid is 1:(0.5 ~ 1.5): (0.5 ~ 0.8).Other step and parameter identical with one of embodiment four to nine.
Embodiment 11: one of present embodiment and embodiment four to ten unlike: the mol ratio of described four nitric hydrate cadmiums, 4-imidazolyl phenylformic acid and oxalic acid is 1:(0.5 ~ 1): (0.5 ~ 0.6).Other step and parameter identical with one of embodiment four to ten.
Embodiment 12: one of present embodiment and embodiment four to ten one unlike: the mol ratio of described four nitric hydrate cadmiums, 4-imidazolyl phenylformic acid and oxalic acid is 1:0.5:0.5.Other step and parameter identical with one of embodiment four to ten one.
Embodiment 13: one of present embodiment and embodiment four to ten two unlike: the mol ratio of described four nitric hydrate cadmiums, 4-imidazolyl phenylformic acid and oxalic acid is 1:0.5:0.5.Other step and parameter identical with one of embodiment four to ten two.
Embodiment 14: one of present embodiment and embodiment four to ten three unlike the volume mass of: described solvent and oxalic acid than being 1mL:(0.0008 ~ 0.005) g.Other step and parameter identical with one of embodiment four to ten three.
Embodiment 15: one of present embodiment and embodiment four to ten four unlike the volume mass of: described solvent and oxalic acid than being 1mL:(0.0008 ~ 0.004) g.Other step and parameter identical with one of embodiment four to ten four.
Embodiment 16: one of present embodiment and embodiment four to ten five unlike the volume mass of: described solvent and oxalic acid than being 1mL:(0.0008 ~ 0.003) g.Other step and parameter identical with one of embodiment four to ten five.
Embodiment 17: one of present embodiment and embodiment four to ten six unlike the volume mass of: described solvent and oxalic acid than being 1mL:(0.0008 ~ 0.002) g.Other step and parameter identical with one of embodiment four to ten six.
Embodiment 18: one of present embodiment and embodiment four to ten seven unlike the volume mass of: described solvent and oxalic acid than being 1mL:0.0015g.Other step and parameter identical with one of embodiment four to ten seven.
By following verification experimental verification beneficial effect of the present invention:
It is carry out according to the following steps by 0D → 2D double interpenetrating structure cadmium coordination polymer synthetic method that this test one is subject to additive factors impact:
Oxalic acid, 4-imidazolyl phenylformic acid and four nitric hydrate cadmiums are placed in 8mL distilled water, stirred at ambient temperature is to mixing, put into the stainless steel cauldron that liner is tetrafluoroethylene, react at temperature is 120 DEG C after 6 days and be down to room temperature, obtain yellow bulk crystals, productive rate 60 ~ 70%, wherein, the mol ratio of four nitric hydrate cadmiums, 4-imidazolyl phenylformic acid and oxalic acid is 2:1:1, and gained crystal is the double interpenetrating structure cadmium coordination polymer of 2D.
The 2D double interpenetrating structure cadmium coordination polymer productive rate of the synthetic method of this test is 60% ~ 70%.
The basic structural unit figure of the double interpenetrating structure cadmium coordination polymer of 2D of this test synthesis as shown in Figure 1;
The molecular structural formula of the double interpenetrating structure cadmium coordination polymer of 2D of this test synthesis as shown in Figure 2;
The one-dimensional chain structure iron of the double interpenetrating structure cadmium coordination polymer of 2D of this test synthesis as shown in Figure 3;
The two-dimentional interpenetrating structure figure of the 2D double interpenetrating structure cadmium coordination polymer of this test synthesis as shown in Figure 4;
This test synthesis 2D double interpenetrating structure cadmium coordination polymer two-dimentional interpenetrating structure topological diagram (tie point 1 represent be central metal cadmium ion, tie point 2 represent be 4-imidazolyl phenylformic acid part) as shown in Figure 5;
Utilize FLSP920 built-up type stable state transient state fluorescent/phosphorescent spectrograph to carry out fluorescence spectrum and fluorescence lifetime test to the double interpenetrating structure cadmium coordination polymer of 2D that this test is synthesized, obtain the solid state fluorescence spectrogram of the double interpenetrating structure cadmium coordination polymer of 2D of this test synthesis as shown in Figure 6; Obtain the solid state fluorescence chromaticity diagram of the double interpenetrating structure cadmium coordination polymer of 2D of this test synthesis as shown in Figure 7; Obtain the solid state fluorescence life curve figure of the double interpenetrating structure cadmium coordination polymer of 2D of this test synthesis as shown in Figure 8; As can be seen from Figure 6, under room temperature solid, take 332nm as excitation wavelength, 2D double interpenetrating structure cadmium coordination polymer maximum emission wavelength is 463nm, can determine that the XYZ chromaticity diagram of Fig. 7 the double interpenetrating structure cadmium coordination polymer of 2D presents blue-fluorescence clearly, color is pure.As can be seen from Figure 8, the fluorescence decay profile of the double interpenetrating structure cadmium coordination polymer of 2D comprises two-pack, fluorescence life τ time solid-state
1and τ
21.09 μ s and 10.90 μ s respectively.
Claims (1)
1., by a synthetic method for the double interpenetrating structure cadmium coordination polymer of 0D → 2D, it is characterized in that it carries out according to the following steps:
Oxalic acid, 4-imidazolyl phenylformic acid and four nitric hydrate cadmiums are placed in 8mL distilled water, stirred at ambient temperature is to mixing, put into the stainless steel cauldron that liner is tetrafluoroethylene, react at temperature is 120 DEG C after 6 days and be down to room temperature, obtain yellow bulk crystals, wherein, the mol ratio of four nitric hydrate cadmiums, 4-imidazolyl phenylformic acid and oxalic acid is 2:1:1, and gained crystal is the double interpenetrating structure cadmium coordination polymer of 2D;
Described polymer molecule formula is [Cd (C
10h
7n
2o
2)
2]
n, wherein said polymer formulae is:
wherein said n is positive integer;
Containing a central metal cadmium ion in described polymkeric substance basic structural unit, two 4-imidazolyl phenylformic acid parts; Wherein, central metal cadmium ion with from the Sauerstoffatom of two 4-imidazolyl phenylformic acid parts and nitrogen-atoms coordination Cheng Jian;
Described central metal cadmium ion presents hexa-coordinate octoploids structure.
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