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One-step synthesis of silane-modified copper nanoclusters and their application to detect trace water content in organic solvents

A copper nanocluster and organic solvent technology, applied in the field of preparation and application of functional nano ions, can solve problems such as inability to detect trace water, instability, interference, etc., and achieve the effects of easy promotion, fast reaction speed and low toxicity

Active Publication Date: 2019-07-26
ZHEJIANG NORMAL UNIVERSITY
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  • Summary
  • 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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  • One-step synthesis of silane-modified copper nanoclusters and their application to detect trace water content in organic solvents
  • One-step synthesis of silane-modified copper nanoclusters and their application to detect trace water content in organic solvents
  • One-step synthesis of silane-modified copper nanoclusters and their application to detect trace water content in organic solvents

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0030] Embodiment 1: One-step method for synthesizing copper nanoclusters modified by mercaptopropyltrimethoxysilane

[0031] Such as figure 1 As shown, 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 copper 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, well dispersed, and free from agglomeration, and the particle size is mainly distributed in the range of 2 to 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 340nm, the fluoresce...

Embodiment 2

[0032] Embodiment 2: One-step method for synthesizing copper nanoclusters modified by mercaptoethyltriethoxysilane

[0033] Such as figure 1 as shown in figure 1As 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 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 6nm. The elements are mainly composed of five elements: carbon, oxygen, silicon, copper and sulfur. Around 700nm.

Embodiment 3

[0034] Example 3: One-step synthesis of copper nanoclusters modified by mercaptopropylmethyldiethoxysilane

[0035] 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 mercaptopropylmethyldiethoxysilane Ethoxysilane-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 6nm. The elements are mainly composed of five elements: carbon, oxygen, silicon, copper and sulfur. The peak is around 700nm.

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Abstract

The invention discloses a method for one-step synthesis of silane-modified copper nano-clusters and its application in detecting trace water content in organic solvents. The preparation method is as follows: taking copper salt and placing it in anhydrous acetonitrile, then adding mercapto-substituted silane, and stirring for 20-40 minutes under airtight room temperature condition to obtain silane-modified copper nano-clusters. Sensitive detection of trace amounts of water in organic solvents is achieved by the on-mode of the fluorescent signal. The method has the characteristics of low operation cost, simple preparation process equipment, mild reaction conditions, fast reaction speed and easy popularization.

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 Patents(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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