Color-changing organic-inorganic hybrid material, and preparation method and application of material

A hybrid material and inorganic technology, applied in the field of color-changing organic-inorganic hybrid materials and their preparation, can solve the problems of high detection cost, insufficient sensitivity, and complicated operation, and achieve the effects of high sensitivity, simple raw materials, and simple operation

Inactive Publication Date: 2018-09-04
山西师范大学
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  • Abstract
  • Description
  • Claims
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AI Technical Summary

Problems solved by technology

[0003] The above-mentioned methods for analyzing and detecting oxygen content all need the assistance of relevant instruments. At present, some traditional sensors for detecting oxygen include Clark type electrodes and optical devices, but the sensitivity of Clark type oxygen sensors to detect oxygen is not enough, and optical oxygen sensors need the help of a fluorometer In the detection process, it is judged that the luminescence performance of the material will be strengthened or quenched with the concentration of oxygen. This kind of fluorescence instrument is expensive, the detection cost is high, and the operation is relatively complicated.

Method used

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  • Color-changing organic-inorganic hybrid material, and preparation method and application of material
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  • Color-changing organic-inorganic hybrid material, and preparation method and application of material

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preparation example Construction

[0032] The preparation method of the color-changing organic-inorganic hybrid material of the present invention includes the following steps:

[0033] S1. Weigh cadmium nitrate, terephthalic acid and monochloro-3-benzoic acid-4,4'-bipyridine according to a certain molar ratio and mix, add the mixture to the solvent, and stir under air atmosphere The solvothermal reaction is carried out after 30 minutes, the reaction temperature is 100°C, and the reaction time is 5-10 days. After the reaction is completed, it is cooled at a rate of 5-10°C / h, filtered and washed to obtain yellow block crystals;

[0034] S2. Put the crystal material obtained from S1 into a Shrek tube, evacuate until the oxygen content does not exceed 0.06ppm, and then irradiate the sample with a high-pressure mercury lamp. The sample in the tube turns from yellow to light blue, which is a color-changing organic Inorganic hybrid materials.

[0035] Furthermore, the synthetic route of monochloro-3-benzoic acid-4,4'-bipyri...

Embodiment 1

[0044] First, 2,4-dinitrochlorobenzene (16.16g, 78mmol) and 4,4'-bipyridine (12.40g, 78mmol) were dissolved in 80ml of acetone, and heated and stirred for 24h at 75℃ to obtain a light gray product Monochloro-1-(2,4-dinitrophenyl)-4,4'-bipyridine; followed by 5.0g monochloro-1-(2,4-dinitrophenyl)-4 Add 200ml ethanol to 4'-bipyridine, then add 2.8ml triethylamine, stir for 30 minutes, add 1.50g m-aminobenzoic acid, and react at 93°C for 48h. The solvent was removed by rotary evaporation, then water was added, stirred for 1 hour, and vacuum filtered. After suction filtered, water was added to dissolve, drop acetone to the solid powder, vacuum filtered, and the solid powder obtained was monochloro-3-benzoic acid. -4,4'-Bipyridine.

[0045] Then cadmium nitrate (0.155g, 0.5mmol), terephthalic acid (0.082g, 0.5mmol) and chloro-3-benzoic acid group-4,4'-bipyridine (0.056g, 0.2mmol) were dissolved in In a solvent prepared by mixing ethanol (2mL), water (1mL) and N,N'-dimethylformamide ...

Embodiment 2

[0047] The preparation method is the same as in Example 1, except that the reaction time of cadmium nitrate, terephthalic acid and monochloro-3-benzoyl-4,4'-bipyridine in the solvent is 10 days, and the cooling rate is 10°C / h.

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Abstract

The invention discloses a color-changing organic-inorganic hybrid material, and a preparation method and an application of the material. A chemical formula of the material is [Cd3(CPBPY)2(BDC)3], wherein CPBPY is 3-benzoic acid-4,4'-dipyridyl; and BDC is p-benzene dicarbonic acid. The preparation method of the material comprises the steps of dissolving cadmium nitrate, terephthalic acid and monochlorated-3-benzoxy-4,4'-dipyridyl in a mixed solvent prepared from ethanol, water and N,N'-dimethylformamide proportionally under a solvothermal condition, heating for 5-10 days at 100 DEG C, cooling at a speed of 5-10 DEG C / h, performing filtration and washing to form a yellow blocky crystal, putting the crystal in a Shrek tube, performing vacuumizing till an oxygen content not exceeding 0.06ppm,irradiating a sample with a high-pressure mercury lamp, and obtaining a target product when the sample in the tube is changed to light blue from yellow. The crystal is stable in structure under a vacuum condition; the synthesis is simple; conditions are mild; the operation is convenient; low-concentration oxygen is detected quickly under a room temperature condition; the sensitivity is high; the testing cost is low; and the material has good application prospects in an aspect of oxygen molecule detection.

Description

Technical field [0001] The invention relates to the technical field of chemistry and chemical engineering, in particular to a color-changing organic-inorganic hybrid material and a preparation method and application thereof. Background technique [0002] With the rapid development of science and technology in my country, the detection of molecular oxygen has received widespread attention, and it is also playing an increasingly important role in many scientific fields such as life sciences, biology, meteorology, oceanography, medicine, and the environment. In the detection of molecular oxygen technology, oxygen content is an important control index. Choosing suitable oxygen content analysis and testing methods and equipment according to actual conditions is an important prerequisite for ensuring accurate oxygen content determination. At present, the main methods of oxygen content analysis are: 1. Chemical methods, including chemical colorimetry and chemical volumetric method, whic...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07F3/08C09K9/02G01N21/64G01N21/78
CPCC07B2200/13C07F3/003C09K9/02C09K2211/1029C09K2211/188G01N21/6447G01N21/783
Inventor 李士利王杰
Owner 山西师范大学
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