Anion receptor based on nitrofuran formyl hydrazone and phenolic hydroxyl and preparation and use of organagel thereof

A technology of nitrofuroylhydrazone and organogel, which is applied in organic chemistry, analyzing materials through chemical reactions, and analyzing materials through observing the impact on chemical indicators, etc., which can solve the inconvenience of carrying and storing solutions And other issues

Inactive Publication Date: 2009-04-29
NORTHWEST NORMAL UNIVERSITY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the colorimetric detection of anions in the solution still needs to prepare a solution, which is inconvenient to carry and store

Method used

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  • Anion receptor based on nitrofuran formyl hydrazone and phenolic hydroxyl and preparation and use of organagel thereof
  • Anion receptor based on nitrofuran formyl hydrazone and phenolic hydroxyl and preparation and use of organagel thereof
  • Anion receptor based on nitrofuran formyl hydrazone and phenolic hydroxyl and preparation and use of organagel thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0040] Embodiment 1, the synthesis of anion acceptor compound

[0041] (1) Synthesis of intermediate 2,6-diformyl-4-chlorophenol:

[0042] a. Preparation of 2,6-dimethylol-4-chlorophenol

[0043] Slowly heat the mixture of 15 grams of p-chlorophenol, 7.8 grams of paraformaldehyde and 1.2 grams of sodium hydroxide to 60 ° C, 4-chlorophenol is melted, paraformaldehyde is suspended in it, and the reaction is stirred at 60 ~ 65 ° C for 1 h , the reaction solution was khaki and then purple-red, and the reaction mixture was stirred at about 65°C for 3.5h, the reactant was agglomerated, and the reaction was terminated; the agglomerated reaction mixture was dissolved in 100mL of hot methanol, and the Adjust the pH to about 2-3; cool to room temperature, precipitate 2,6-dimethylol-4-chlorophenol, filter and collect the product. It was recrystallized with methanol to obtain light khaki crystals. Yield 65%.

[0044] b. Preparation of 2,6-diformyl-4-chlorophenol

[0045] Add 3.8 g (0...

Embodiment 2

[0050] Embodiment 2, the preparation of anion acceptor organogel

[0051] Add 0.015 g of the above-prepared anion acceptor compound into 1 mL of DMF, heat to 70-120° C. to dissolve, form a DMF solution with a mass percentage of 1.5%, and form a stable anionic organic gel after cooling to room temperature.

Embodiment 3

[0052] Embodiment 3, detect anion with anion acceptor organogel

[0053] Take a small amount of anion acceptor organogels, place them on a white drip plate, and drop F on the organogels respectively. - , Cl - , Br - , I - , CH 3 COO - , HSO 4 - , H 2 PO 4 - , ClO 4- Anionic tetrabutylammonium salt in DMSO solution (0.01mol / L); organic gel changes from yellow to orange, then it is F-solution; organic gel changes from yellow to red, then it is CH 3 COO - solution; organogel changes from yellow to orange, then H 2 PO 4 - solution; if the organic gel does not change color, it is a solution of other ions.

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Abstract

The invention provides an anion receptor based on 5-nitrofuran formyl hydrazone and phenolic hydroxyl. The anion receptor is obtained by mixing 2, 6-dimethylacyl-4-chlorophenol and 5-(4-nitro)-phenyl-2-benzoyl diazanyl furan according to certain proportion, stirring and refluxing the mixture for 3 to 8 hours at a temperature of between 70 and 100 DEG C by using anhydrous ethanol as a solvent and p-toluene sulfonic acid as a catalyst, distilling out most of the solvent through reducing the pressure, performing suction filtration after cooling, and performing recrystalization on the solid product by using DMSO-EtOH. The anion receptor has color comparison recognizing ability on fluorion, acetic acid radical and phosphoric acid dihydrogen radical in a DMSO solution. The anion receptor is dissolved in DMF to be prepared into 0.5 to 2.0 percent of solution which is cooled to room temperature to be prepare into stable anion receptor organic gel used for performing colorimetric detection on the fluorion, and the acetic acid radical and phosphoric acid dihydrogen radical ions in the DMSO solution. The anion receptor has the advantages of convenience for carrying, convenient use, high detection sensitivity and the like.

Description

technical field [0001] The invention belongs to the technical field of chemical industry, and relates to an anion acceptor based on nitrofuroylhydrazone and phenolic hydroxyl group and a preparation method thereof. The invention also relates to the preparation of the anion acceptor organic gel and its application in anion detection. Background technique [0002] Anions play a fundamental role in life systems, environmental systems and chemical production. Especially in living systems, anions play an important role in the realization of life processes. Therefore, the detection of anions is a very necessary work. For example, fluoride ion is an anion that has an important impact on living systems. It is well known that the human body can prevent dental caries and prevent osteoporosis by taking an appropriate amount of fluoride ions. However, excessive intake of fluoride ions can lead to fluorosis. Mild fluorosis can harm the ameloblasts of human tooth germs. Severe fluorosi...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D307/68G01N21/78
Inventor 张有明林奇秦霄萍魏太保
Owner NORTHWEST NORMAL UNIVERSITY
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