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Two-dimensional dinuclear zinc coordination polymer and preparation method and application thereof

A technology of zinc coordination polymer and polytetrafluoroethylene tube, which is applied in the field of coordination polymers, can solve problems such as use restrictions, and achieve the effect of simple preparation process and high purity

Active Publication Date: 2018-08-14
SHANXI UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Among these fluorescent probes, some probes cannot exist stably in aqueous solution, which greatly limits their use.

Method used

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  • Two-dimensional dinuclear zinc coordination polymer and preparation method and application thereof
  • Two-dimensional dinuclear zinc coordination polymer and preparation method and application thereof
  • Two-dimensional dinuclear zinc coordination polymer and preparation method and application thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0020] Preparation of Zinc Coordination Polymer

[0021] Weigh 0.2mmol H 3 L1, 0.2mmol L2 and 0.1mmol Zn(NO 3 ) 2 ·6H 2 O was added containing 6mL H 2 In a 13 mL polytetrafluoroethylene tube with O, slowly add KOH with a concentration of 0.2 mol / l dropwise into the stirring mixture to adjust the pH to 5, and continue stirring for 30 minutes. Seal the polytetrafluoroethylene tube in a stainless steel reaction kettle, heat it at 413K for three days, then cool it down to room temperature by 10°C every hour, and a colorless blocky crystal can be precipitated, washed with water and dried in vacuum, with a yield of 80%. Elemental analysis: theoretical value: C 57.47, H 3.19, N 4.97%; experimental value: C 57.93, H 3.39, N 5.14%.

[0022] Zinc coordination polymer crystal structure determination:

[0023] The crystal structure was determined by X-ray diffraction, using Bruker D8Venture detector to monochromatize Mo-Kα rays through graphite monochromator, scanning mode ω, and th...

Embodiment 2

[0031] Example 2 The zinc coordination polymer of the present invention selectively recognizes dichromate ions and chromate ions in water.

[0032] First, prepare 10mL concentration of 5×10 -3 mol / L of different anion solutions, (anion=F - , Cl - ,Br - ,I - , SO 4 2- ,SCN - ,CH 3 COO - ,ClO 4 - ,CO 3 2- ,HPO 4 2-,MoO 4 2- ,CrO 4 2- and Cr 2 o 7 2- ). 2 mg of the zinc coordination polymers were added to 10 mL of different anion solutions, treated with ultrasound for 30 minutes, and sedimented for three days to form a suspension of zinc coordination polymers incorporated with inorganic anions. Get the supernatant, under the condition that the excitation wavelength is 290nm, and the slit width is 10nm, measure its fluorescence emission spectrum intensity, as Figure 4 As shown, the coordination polymer has unique fluorescence selectivity for dichromate ion and chromate ion.

Embodiment 3

[0033] Example 3 The sensitivity of the zinc coordination polymer of the present invention to recognize dichromate ions and chromate ions in water.

[0034] Add 2 mg of the coordination polymer to 10 mL of water, ultrasonicate for 30 minutes, and settle for three days to form a uniform suspension of the zinc coordination polymer. Take 2mL of the supernatant, and gradually add dropwise to a concentration of 1×10 -3 mol / L of dichromate ion or acid ion, from Figure 4 It can be seen that under the excitation wavelength of 290nm, the suspension of the zinc coordination polymer shows very strong fluorescence at 370nm. Such as Figure 5 The titration curve shows that with the dichromate ion in the system ( Figure 5 a) or chromate ion ( Figure 5 b) As the concentration increases, the fluorescence of the solution decreases significantly. In addition, if Figure 6 As shown, at low concentrations, the quenching effect can be dealt with by the Stern-Volmer equation: I 0 / I=1+K ...

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Abstract

The invention provides a two-dimensional dinuclear zinc coordination polymer which has a simple chemical formula as shown in [Zn(HL1)L2]n.nH2O, wherein H3L1 is o-(p-carboxylbenzene)oxy-terephthalic acid, and L2 is phenanthroline. The coordination polymer is prepared through a hydrothermal method, that is, the coordination polymer is prepared by adding Zn(NO3)2.6H2O, phenanthroline, o-(p-carboxylbenzene)oxy-terephthalic acid and water in a polytetrafluoroethylene tube at a mole ratio of 2:2:1:(300 to 350), regulating the pH with 0.2 mmol / L KOH to 5, performing a reaction for 3 days in a hydrothermal reaction kettle at 413 K after stirring for 30 mins, cooling to a room temperature and then collecting white block crystals, washing with distilled water, and performing vacuum drying. The zinccoordination polymer has a two-dimensional structure with dinuclear zinc secondary structure units. The dinuclear zinc coordination polymer has a good selectivity detection to dichromate ions and chromate ions in a water solution, can be at least repeatedly used for five times or more, and can be used as a chemical sensor for efficiently detecting hexavalent chromium ions.

Description

technical field [0001] The present invention relates to a coordination polymer, in particular to a coordination polymerization with a two-dimensional structure formed based on transition metal zinc (II), o-(p-carboxyphenyl)oxy terephthalic acid and o-phenanthroline Compound and its preparation method, and the application of the coordination polymer as a chemical sensor for detecting hexavalent chromium ions in aqueous solution. Background technique [0002] Chromium mainly occurs in three forms: metallic chromium, trivalent chromium and hexavalent chromium. Among them, hexavalent chromium ions can cause skin allergies and ulcers, rhinitis, lung cancer, skin allergies, kidney failure and induce gene mutations after concentration. Therefore, the analysis and detection of hexavalent chromium in the environment has attracted much attention in recent years. Currently, methods for detecting hexavalent chromium ions include ion mobility spectrometry (IMS), inductively coupled pla...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G83/00C09K11/06G01N21/64
CPCC08G83/008C09K11/06C09K2211/188G01N21/6428G01N2021/6432
Inventor 李少东卢丽萍朱苗力
Owner SHANXI UNIV
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