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Method for synthesizing copper nano-clusters modified by silane in one step and application of copper nano-clusters modified by silane in detecting trace water-content in organic solvent

A technology of copper nano-clusters and organic solvents, applied in the preparation and application of functional nano-ions, can solve problems such as interference, inapplicability to trace water detection, instability, etc., and achieve fast reaction speed, easy promotion, stability and light resistance good sex effect

Active Publication Date: 2017-11-21
ZHEJIANG NORMAL UNIVERSITY
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, these molecular probes are easily affected by the polarity of organic solvents and are unstable, and these fluorescent molecular probes are only suitable for the determination of a few organic solvents, especially for trace amounts in protic solvents such as ethanol and methanol. water detection
More importantly, most fluorescent molecular probes detect water content based on the quenching mechanism of the fluorescent signal, and the mode of signal reduction is not an ideal detection mode, and is often interfered by other quenchers

Method used

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  • Method for synthesizing copper nano-clusters modified by silane in one step and application of copper nano-clusters modified by silane in detecting trace water-content in organic solvent
  • Method for synthesizing copper nano-clusters modified by silane in one step and application of copper nano-clusters modified by silane in detecting trace water-content in organic solvent
  • Method for synthesizing copper nano-clusters modified by silane in one step and application of copper nano-clusters modified by silane in detecting trace water-content in organic solvent

Examples

Experimental program
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Effect test

Embodiment 1

[0031] Embodiment 1: One-step method for synthesizing copper nanoclusters modified by mercaptopropyltrimethoxysilane

[0032] Such as figure 1 As indicated, weigh 6 mg of copper nitrate, place it in 20 mL of anhydrous acetonitrile, add 25 μL of mercaptopropyltrimethoxysilane, and stir for 20 to 40 minutes under airtight room temperature conditions to obtain mercaptopropyltrimethoxysilane-modified Cu nanoclusters with a calculated yield of 95%. Such as figure 2 The TEM imaging results in A show that the prepared mercaptopropyltrimethoxysilane-modified copper nanoclusters are approximately spherical in shape, uniform in size, good in dispersion, and free from agglomeration, and the particle size is mainly distributed in the range of 2-6 nm. Such as figure 2 The XPS pattern in B shows that the copper nanoclusters are mainly composed of five elements: carbon, oxygen, silicon, copper, and sulfur. Such as image 3 As shown, at the excitation wavelength of 340 nm, the fluores...

Embodiment 2

[0033] Embodiment 2: One-step method for synthesizing copper nanoclusters modified by mercaptoethyltriethoxysilane

[0034] Such as figure 1 as shown in figure 1 As shown, weigh 6 mg of copper sulfate, place it in 20 mL of anhydrous acetonitrile, add 34.5 μL of mercaptoethyltriethoxysilane, and stir for 20 to 40 minutes under airtight room temperature conditions to obtain mercaptoethyltriethoxysilane Silane-modified copper nanoclusters with a calculated yield of 90%. Characterized by TEM, XPS and fluorescence spectra, the copper nanoclusters modified by mercaptoethyltriethoxysilane and the copper nanoclusters modified by mercaptopropyltrimethoxysilane are similar in shape, size, elemental composition and fluorescence emission. They are all approximately spherical in shape, with a size between 2 and 6 nm. The elements are mainly composed of five elements: carbon, oxygen, silicon, copper and sulfur. They emit faint red light under ultraviolet light, and the fluorescence spectr...

Embodiment 3

[0035] Example 3: One-step synthesis of copper nanoclusters modified by mercaptopropylmethyldiethoxysilane

[0036] Such as figure 1 As shown, weigh 60 mg of copper chloride, place it in 100 mL of anhydrous acetonitrile, add 422 μL of mercaptopropylmethyldiethoxysilane, and stir for 20 to 40 minutes under airtight room temperature conditions to obtain mercaptopropyl methyl Diethoxysilane-modified copper nanoclusters with a calculated yield of 90%. Characterized by TEM, XPS and fluorescence spectra, the copper nanoclusters modified with mercaptopropylmethyldiethoxysilane and the copper nanoclusters modified with mercaptopropyltrimethoxysilane have different properties such as morphology, elemental composition and fluorescence emission. Similar, they are all approximately spherical in shape, with a size between 2 and 6 nm. The elements are mainly composed of five elements: carbon, oxygen, silicon, copper, and sulfur. They emit faint red light under ultraviolet light, and their...

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Abstract

The invention discloses a method for synthesizing copper nano-clusters modified by silane in one step and application of the copper nano-clusters modified by the silane in detecting trace water-content in an organic solvent. The preparation method for the synthesizing copper nano-clusters modified by silane comprises the step that copper salt is placed in anhydrous acetonitrile, then the silane substituted by mercapto groups is added, stirring is conducted for 20-40 min under a sealed room-temperature condition, and the copper nano-clusters modified by the silane are obtained. Ultrasensitive detection of trace water in the organic solvent is achieved through the open pattern of a fluorescence signal. The method for synthesizing the copper nano-clusters modified by the silane in one step and the application of the copper nano-clusters modified by the silane in detecting the trace water-content in the organic solvent has the characteristics that the operating cost is low, preparation process equipment is simple, the reaction condition is gentle, the reaction speed is high, and popularization is easy.

Description

technical field [0001] The invention belongs to the technical field of preparation and application of functional nanometer ions, and specifically relates to a method for one-step synthesis of silane-modified copper nanoclusters and its application in detecting trace water content in organic solvents. Background technique [0002] The determination and control of water content in organic solvents is of great significance to the fields of organic synthesis, drug production, food processing and biomedical monitoring. Water is one of the most common impurities in organic solvents. The existence of a small amount of water will greatly affect the progress of chemical reactions, and even change the products of the reactions. Therefore, the determination of water content in organic solvents is the most important and important part of chemical reactions. One of the most common analysis problems. The commonly used chemical analysis method for the determination of water content in org...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B22F9/24B22F1/00G01N21/64B82Y30/00B82Y40/00
CPCG01N21/6428B82Y30/00B82Y40/00B22F9/24B22F1/07B22F1/054B22F1/102
Inventor 钱兆生丰慧赵美芝
Owner ZHEJIANG NORMAL UNIVERSITY
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