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Preparation method of substituted polyacetylene type water-phase bivalent copper ion detection probe as well as product and application thereof

A technology of divalent copper ions and detection probes, which can be applied in the measurement of color/spectral properties, etc., can solve the problems of difficult development, limitations, and difficulty in the synthesis of water-soluble substituted polyalkynes, and achieve the effect of reducing synthesis costs.

Pending Publication Date: 2020-05-08
ZHEJIANG SCI-TECH UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The most difficult of these is that the application is still limited to organic solvent systems and difficult to carry out in aqueous phase
The root cause of this problem is that the synthesis of water-soluble substituted polyynes is still difficult (Chem. Mater. 2018, 30, 6908-6914)

Method used

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  • Preparation method of substituted polyacetylene type water-phase bivalent copper ion detection probe as well as product and application thereof
  • Preparation method of substituted polyacetylene type water-phase bivalent copper ion detection probe as well as product and application thereof
  • Preparation method of substituted polyacetylene type water-phase bivalent copper ion detection probe as well as product and application thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0056]The first step is to prepare the substituted alkyne monomer M-Gly-Boc, as follows: Dissolve 1.75 g of N-Boc-glycine (N-tert-butoxycarbonyl-glycine; CAS: 4530-20-5) in 50 mL of tetrahydrofuran, Then add 1.3mL of isobutyl chloroformate and 1.1mL of N-methylmorpholine, after a constant temperature reaction for 15min, then add 0.7mL of propargylamine, and react in a water bath at 30°C for 4h to obtain the M-Gly-Boc solution; Ethyl acetate was used as the extractant, and the resulting solution was washed three times with 30 mL of hydrochloric acid solution (2M), twice with 30 mL of saturated sodium bicarbonate solution, and once with 80 mL of deionized water, then dried by adding anhydrous magnesium sulfate, and then rotary evaporated , purified by freeze crystallization in a THF / n-hexane volume ratio system of 1 / 5. After 5 hours, it was filtered and dried at 30° C. for 24 hours to 48 hours to obtain a solid product of M-Gly-Boc with a yield of 82.1%.

[0057] The second ste...

Embodiment 2

[0076] The first step is to prepare the substituted alkyne monomer M-Gly-Boc, as follows: dissolve 1.75 g of N-Boc-glycine in 50 mL of tetrahydrofuran, then add 1.3 mL of isobutyl chloroformate and 1.1 mL of N-methyl mol After reacting at constant temperature for 15 minutes, add 1.05 mL of propargylamine and react for 4 hours at 30°C in a water bath to obtain the M-Gly-Boc solution; use ethyl acetate as the extraction agent, and use 30 mL of hydrochloric acid solution (2M) Wash three times, wash twice with 30mL saturated sodium bicarbonate solution, wash once with 80mL deionized water, then add anhydrous magnesium sulfate for drying treatment, rotary evaporation, and freeze crystallization in a system with a THF / n-hexane volume ratio of 1 / 5 for purification . After 5 hours, filter and dry at 30° C. for 24 hours to 48 hours to obtain a solid product of M-Gly-Boc.

[0077] The second step is to prepare the substituted polyalkyne P-Gly-Boc, the specific method is as in Example 1...

Embodiment 3

[0081] The first step is to prepare the substituted alkyne monomer M-Gly-Boc, as follows: dissolve 1.75 g of N-Boc-glycine in 50 mL of tetrahydrofuran, then add 1.3 mL of isobutyl chloroformate and 1.1 mL of N-methyl mol After reacting at constant temperature for 15 minutes, add 0.35 mL of propargylamine and react for 4 hours at 30°C in a water bath to obtain the M-Gly-Boc solution; use ethyl acetate as the extractant, and use 30 mL of hydrochloric acid solution (2M) Wash three times, wash twice with 30mL saturated sodium bicarbonate solution, wash once with 80mL deionized water, then add anhydrous magnesium sulfate for drying treatment, rotary evaporation, and freeze crystallization in a system with a THF / n-hexane volume ratio of 1 / 5 for purification . After 5 hours, filter and dry at 30° C. for 24 hours to 48 hours to obtain a solid product of M-Gly-Boc.

[0082] The second step is to prepare the substituted polyalkyne P-Gly-Boc, the specific method is as in Example 1.

[...

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Abstract

The invention belongs to the field of functional polymer materials, and particularly discloses a substituted polyacetylene type water-phase bivalent copper ion detection probe as well as a preparationmethod and application thereof. The preparation method comprises the following steps: taking N-Boc-glycine and propargylamine as raw materials and carrying out amidation reaction to synthesize M-Gly-Boc; initiating M-Gly-Boc to polymerize under the catalysis of an organic rhodium complex, so as to prepare P-Gly-Boc; finally, removing Boc groups through trifluoroacetic acid, and obtaining a substituted polyacetylene type water-phase bivalent copper ion detection probe P-Gly-NH2 with excellent water solubility. The probe prepared by the method disclosed by the invention has specificity on detection of Cu <2+> and high anti-interference capability on other metal ions and anions, and the detection limit is determined to be 0.128 mg / L. According to the method, the practical application value of substituted polyacetylene in the field of recognition and detection is remarkably improved, and a simple, convenient and feasible solution is provided for special detection of Cu <2+> in drinking water.

Description

technical field [0001] The invention belongs to the field of functional polymer materials, and in particular relates to a preparation method of a polyacetylene-type water-phase divalent copper ion detection probe and its product and application. Background technique [0002] Copper is one of the most common metal elements in nature and plays a very important role in life activities. When the living body Cu 2+ Concentrations above or below the concentration range required by cells can cause severe copper metabolism disorder diseases, so its directional detection in aqueous solution has received great attention. [0003] Currently, Cu 2+ There are mainly two types of detection methods: direct method and indirect method. Direct methods include atomic absorption / emission spectrometry, ion selective electrode method, etc., which have the advantages of strong selectivity and high sensitivity but require expensive test equipment. Most of the indirect methods use organic small m...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N21/33
CPCG01N21/33
Inventor 黄骅隽段慧敏戚栋明陈智杰殷丽杰
Owner ZHEJIANG SCI-TECH UNIV
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