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A rare earth organic framework material for trace water fluorescence detection and its preparation method

A framework material, rare earth organic technology, applied in luminescent materials, material analysis by optical means, 3/13 groups of organic compounds without C-metal bonds, etc., can solve the problem of in-situ detection and real-time monitoring, reaction rate Slow, complex process and other problems, to achieve the effect of self-calibration detection, low detection limit, simple preparation method

Active Publication Date: 2018-04-20
ZHEJIANG UNIV
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  • Claims
  • Application Information

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Problems solved by technology

The commonly used chemical analysis method for the determination of water content in organic solvents is the classic Karl Fischer method, which was proposed in 1935. Although it has been greatly improved, it still has slow reaction rate, easy interference, poor precision, and high toxicity. and other shortcomings
Other methods for determining water content include spectrophotometry, gas chromatography, liquid chromatography and infrared spectroscopy, etc., but these detection methods are expensive and complicated, and cannot achieve in-situ detection and real-time monitoring

Method used

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  • A rare earth organic framework material for trace water fluorescence detection and its preparation method
  • A rare earth organic framework material for trace water fluorescence detection and its preparation method
  • A rare earth organic framework material for trace water fluorescence detection and its preparation method

Examples

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Effect test

example 1

[0022] A highly stable rare-earth organic framework material EuBDC-NH was synthesized by solvothermal method using europium nitrate hexahydrate and 2-aminoterephthalic acid 2 , its specific synthetic route is as follows:

[0023] Dissolve 0.725 mmol of 2-aminoterephthalic acid, 0.725 mmol of europium nitrate hexahydrate, and 5.8 mmol of o-fluorobenzoic acid in 36.5 mL of N,N-dimethylformamide, and then add 3 mL of deionized water and 2mL of nitric acid, stirred evenly, put into a closed 100mL reaction kettle, reacted in a constant temperature oven at 110°C for 60 hours, cooled to room temperature with the furnace, centrifuged to separate solid and liquid, and used N,N-dimethyl formaldehyde for solid Rare-earth organic framework material crystal EuBDC-NH obtained by amide washing three times 2 , the crystal is a colorless and transparent octahedron with a size of about 0.5mm×0.5mm×0.5mm, and the yield is 75%.

[0024] Its structural formula was determined by Oxford Xcalibur G...

example 2

[0028] A highly stable rare-earth organic framework material EuBDC-NH was synthesized by solvothermal method using europium nitrate hexahydrate and 2-aminoterephthalic acid 2 , its specific synthetic route is as follows:

[0029] Dissolve 0.725 mmol of 2-aminoterephthalic acid, 0.725 mmol of europium nitrate hexahydrate, and 5.8 mmol of o-fluorobenzoic acid in 36.5 mL of N,N-dimethylformamide, and then add 3 mL of deionized water and 2mL of nitric acid, stirred evenly, put into a closed 100mL reaction kettle, reacted in a constant temperature oven at 110°C for 60 hours, cooled to room temperature with the furnace, centrifuged to separate solid and liquid, and used N,N-dimethyl formaldehyde for solid Rare-earth organic framework material EuBDC-NH obtained by amide cleaning three times 2 , the yield was 75%.

[0030] EuBDC-NH 2 Dispersed in ethanol, the quantum efficiency is 5.3%, with the increase of water content, Eu 3+ The characteristic emission intensity (at 614nm) of t...

example 3

[0033] A highly stable rare-earth organic framework TbBDC-NH was synthesized by solvothermal method using terbium nitrate hexahydrate and 2-aminoterephthalic acid 2 , its specific synthetic route is as follows:

[0034] Dissolve 0.725 mmol of 2-aminoterephthalic acid, 0.725 mmol of terbium nitrate hexahydrate, and 5.8 mmol of o-fluorobenzoic acid in 36.5 mL of N,N-dimethylformamide, and then add 3 mL of deionized water and 2mL of nitric acid, stirred evenly, put into a closed 100mL reaction kettle, reacted in a constant temperature oven at 110°C for 60 hours, cooled to room temperature with the furnace, centrifuged to separate solid and liquid, and used N,N-dimethyl formaldehyde for solid Rare-earth organic framework material TbBDC-NH obtained by amide cleaning three times 2 , the yield was 70%.

[0035] Powder X-ray diffraction showed that TbBDC-NH 2 with EuBDC-NH 2 Isomorphic, also belongs to the crystal of face-centered cubic structure, the appearance is octahedral, can...

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Abstract

The invention discloses a rare earth organic framework material for fluorescence detection of trace water and a preparation method of the rare earth organic framework material. The rare earth organic framework material is an orderly microporous crystalline material, and the general structural formula of the material is [(CH3)2NH2]2[Ln6(mu3-OH)8(L-NH2)6(H2O)6]*(G)7, wherein Ln in the formula is Eu<3+>, Tb<3+> or Gd<3+>, L-NH2 is a chainlike phthalic acid organic ligand with an amino group function group and G represents a solvent in pores. The rare earth organic framework material is synthesized with a solvothermal method, the synthesis method adopts a simple process, the condition is mild, the yield is higher, and the product stability is good. The rare earth organic framework material has the properties of characteristic emission of rare earth and fluorescence of the ligand, the specific value of two emission peaks and the content of water in the solvent are in a better linear relation, and ratio type detection of trace water can be realized; the light color remarkably changes with the change of the water content, and the material can be used for colorimetric type detection of trace water. The sensitivity of a probe is high, the response speed is high, the detection limit is low, and the material can be recycled and is expected to be used practically in fields of detection and monitoring of trace water.

Description

technical field [0001] The invention relates to a rare earth organic framework material and a preparation method thereof, in particular to a rare earth organic framework material for trace water fluorescence detection and a preparation method thereof. Background technique [0002] Typically, water is the main impurity in organic solvents. The water content in an organic solvent is an important indicator of the quality of the organic solvent. It directly affects the performance of the organic solvent. It is very important for precise synthesis and separation testing. It greatly affects the progress and yield of the chemical reaction, and even determines the reaction. product type. In addition, the water content index in the petroleum industry is also extremely important. The presence of water will not only reduce the performance of the engine, but even emulsification and phase separation will occur when the temperature drops, which will block the fuel pipeline and cause fata...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07F5/00C09K11/06G01N21/64
CPCC07F5/003C09K11/06C09K2211/1007G01N21/643
Inventor 崔元靖夏体锋朱逢亮郁建灿杨雨钱国栋
Owner ZHEJIANG UNIV
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