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Cadmium organic framework compound and preparation method thereof

A technology of organic frameworks and complexes, applied in the field of transition metal complexes, can solve problems such as no reports, and achieve the effects of simple preparation method, low cost and high yield

Active Publication Date: 2017-12-01
SHANXI UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

So far, complexes of transition metals and 2,5-bis(1,2,4-triazolyl)terephthalic acid have not been reported

Method used

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  • Cadmium organic framework compound and preparation method thereof
  • Cadmium organic framework compound and preparation method thereof
  • Cadmium organic framework compound and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0020] Embodiment 1. Complex of the present invention [Cd (L) (H 2 O) 2 ] n preparation method

[0021] Weigh 0.05mmol H 2 L with 0.1mmolCd(NO 3 ) 2 4H 2 O was placed in a 15ml teflon tube, and 8ml H was added 2 O and 2ml DMF, stirred at room temperature for 30 minutes. Then the polytetrafluoroethylene tube was sealed in a stainless steel reaction kettle, the temperature was controlled at 120°C and heated for 72 hours, and it was naturally lowered to room temperature to obtain a colorless diamond-shaped crystal, which was washed three times with distilled water and dried in vacuum. The yield of the obtained cadmium complex was was 76%. Infrared spectrum (wave number, cm -1 ): 3446(m), 3134(m), 2309(w), 1837(w), 1764(w), 1588(s), 1534(s), 1442(m), 1410(m), 1362(s ),1335(s),1282(s),1233(m),1216(m),1142(s),1075(m),1000(w),980(s),914(m),886(m ), 814(s), 671(m), 653(m), 567(w).

Embodiment 2

[0022] Embodiment 2. Complexes of the present invention [Cd(L)(H 2 O) 2 ] n crystal structure of

[0023] Select a single crystal of a suitable size under a microscope, use X-ray diffraction, use Bruker Smart Apex II detector to monochromatize Mo-Kα rays through a graphite monochromator, scan mode ω, and collect diffraction data at room temperature. All diffraction data were subjected to semi-empirical absorption correction using the SADABS program after SAINT reduction. The crystal structure was solved by SHELXL-97 direct method. The detailed crystal determination data are shown in Table 1; the crystal structure is as figure 1 As shown, each Cd(II) adopts a hexacoordinated mode, L 2- Four coordination atoms are provided to coordinate with four central ions Cd(II), thereby forming a three-dimensional network structure.

[0024] Crystallographic data of the complexes in Table 1

[0025]

[0026]

Embodiment 3

[0027] Embodiment 3. Complexes of the present invention [Cd(L)(H 2 O) 2 ] n Infrared Spectrum

[0028] Take a small amount of [Cd(L)(H 2 O) 2 ] n Solid powder, pressed with KBr, recorded in infrared spectrometer at 4000-400cm -1 absorb, see figure 2 . Complex characteristic absorption peak (cm -1 ) and the corresponding vibration modes are: the complex at 3134cm -1 The broadband absorption of corresponds to the O–H stretching vibration of water molecules. Complex at 1700cm -1 The characteristic band at is very weak compared with the ligand, indicating that the carboxyl group reacts with Cd(II) ion to completely deprotonate.

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Abstract

The invention discloses a cadmium organic framework compound and a preparation method thereof. A chemical formula of the compound is [Cd(L)(H2O)2]n, wherein H2L is 2,5-di(1H-1,2,4-triazolyl)terephthalic acid. The preparation method comprises the following steps: adding the H2L and cadmium nitrate with the mol ratio of 1 to 2 into H2O and DMF (Dimethyl Formamide) with the volume ratio of 4 to 1; after stirring the components at the room temprature for 30min, enabling a mixture to react at 120 DEG C for 72h in a closed reaction kettle, so as to obtain a colorless rhombus-shaped crystal, with the yield of 76 percent. The compound disclosed by the invention has a three-dimensional framework structure; a cadmium ion adopts a six-coordinated octahedral coordination mode. When the solid-state compound is stimulated by light with the wavelength of 320nm, the compound has an emission peak at a the part with the wavelength of 414nm and a CIE chromaticity coordinate is (0.15, 0.0439) and is located in a blue-ray region; the compound can be used as an optical material.

Description

technical field [0001] The invention relates to a transition metal complex, specifically a cadmium organic framework complex, especially a cadmium (II) ion and 2,5-bis(1H-1,2,4-triazolyl) terephthalate A cadmium complex with luminescent properties constructed by formic acid and a preparation method thereof. Background technique [0002] Transition metal complexes have broad application prospects in the fields of magnetism, luminescence, and adsorption due to their optical, electrical, and magnetic properties. Among them, d 10 Compared with traditional inorganic light-emitting materials, electronic transition metal organic complexes as photoluminescent materials, on the one hand, because of their special molecular rigid structure, the molecular radiation transition probability is greatly enhanced, that is, they have high fluorescence quantum efficiency; on the other hand, they also have The high stability of inorganic substances guarantees its application as a functional mat...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07F3/08C07D249/08C09K11/06
CPCC07B2200/13C07D249/08C07F3/003C09K11/06C09K2211/1059C09K2211/188
Inventor 卢丽萍孟丽朱苗力冯思思
Owner SHANXI UNIV
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