Anion receptor based on nitro phenylhydrazone and phenolic hydroxyl and preparation of anion test paper and use thereof

A technology of nitrophenylhydrazone and anion, which is applied in the field of chemistry and can solve the problems of inconvenient carrying and storage of solutions

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

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Problems solved by technology

However, the colorimetric detection of anions in the solution still

Method used

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  • Anion receptor based on nitro phenylhydrazone and phenolic hydroxyl and preparation of anion test paper and use thereof
  • Anion receptor based on nitro phenylhydrazone and phenolic hydroxyl and preparation of anion test paper and use thereof
  • Anion receptor based on nitro phenylhydrazone and phenolic hydroxyl and preparation of anion test paper and use thereof

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Experimental program
Comparison scheme
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Embodiment 1

[0042] Embodiment 1, the synthesis of anion acceptor K1 (corresponding to the product of X=H)

[0043] 1. Synthesis of intermediate 2,6-dimethylol-4-chlorophenol (M1): 15 grams of p-chlorophenol, 7.8 grams of paraformaldehyde and 1.2 grams of sodium hydroxide were mixed, slowly heated to 60 ° C, 4 -Chlorophenol melts, paraformaldehyde is suspended in it, and the reactant is stirred at 60-65°C for 1 hour. Caking, the reaction is terminated. The agglomerated reaction mixture was dissolved in 100 mL of hot methanol at 70°C, and the pH was adjusted to about 2-3 with hydrochloric acid. After cooling to room temperature, the product precipitated, and was filtered to collect the product. Part of the solvent was evaporated from the filtrate and then cooled to room temperature, the product was precipitated again, and the product was combined after filtration. It was recrystallized with methanol to obtain light khaki crystals. Yield 51.0%.

[0044] 2, Synthesis of 2,6-diformyl-4-ch...

Embodiment 2、K1

[0047] The preparation of embodiment 2, K1 detection test paper

[0048] Cut the filter paper into a square of 8cm×8cm, and use 0.5mol·L -1 Soak in dilute hydrochloric acid for 1 hour. After washing with distilled water several times, filter with suction on the Buchner funnel while washing with distilled water until the filtrate is neutral. Remove the water by suction filtration, and dry the washed filter paper in a vacuum oven. Dissolve the main compound K1 in DMSO solution to prepare a concentration of 2.0×10 -2 mol L -1 DMSO solution. Put the treated filter paper flat on a 10cm plate, add the prepared DMSO solution of K1 dropwise to the center of the filter paper with a dropper, control the dropping speed, add the second drop after the first drop spreads on the filter paper, until The filter paper evenly absorbs the DMSO solution of K1. Place the test paper that has absorbed the solution in a vacuum oven to dry. After thorough drying, cut the filter paper adsorbed wi...

Embodiment 3

[0049] Embodiment 3, detect the F in DMSO solution with K1 detection test paper - 、AcO - and H 2 PO 4 -

[0050] will be prepared to a concentration of 1 x 10 -2 mol L -1 the F - , Cl - , Br - , I- , CH 3 COO - , HSO 4 - , H 2 PO 4 - , ClO 4 - The DMSO solution of tetrabutylammonium salt of the anion is added dropwise to the K1 detection test paper with a dropper, and the color of the test paper changes from yellow to deep red, which is F - 、AcO - or H 2 PO 4 - solution.

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Abstract

The invention provides an anion receptor based on nitrophenylhydrazone and phenolic hydroxyl groups. The anion receptor is prepared by the following steps: 2, 6-diformyl-4-irgasan and paranitrophenylhydrazine are added into a reactor according to the quantity ratio of between 1 to 2 and 1 to 2.5, paratoluenesulfonic acid which accounts for 0.001 to 0.01 percent of the total mass of reactants is added as a catalyst, absolute ethyl alcohol which is 20 to 40 times of the total mass of the reactants is added as a solvent, and the reflux is performed for 3 to 6 hours at a temperature of between 70 and 100 DEG C to generate an orange precipitate; and the mixture is cooled to room temperature, and then the precipitate is filtered, is scrubbed by the absolute ethyl alcohol, and is recrystallized by DMSO to obtain the anion receptor. The anion receptor has the colorimetric identification ability to fluoride ions, acetates and dihydrogen phosphates in a DMSO solution, and has the selective colorimetric detection ability to acetate ions in DMSO/H2O solution. Anion detection test paper prepared by absorbing the anion receptor on the pretreated filter paper and drying the filter paper is used for colorimetric detection of the fluoride ions, the acetates and the dihydrogen phosphates, and has the characteristics of convenience for carrying, convenient use, high detection sensitivity and so on.

Description

technical field [0001] The invention belongs to the field of chemistry, and relates to a class of anion receptors based on nitrophenylhydrazone and phenolic hydroxyl groups and a preparation method thereof; meanwhile, it also relates to the preparation and application of the anion receptor detection test paper. 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 fluorosis can cause fluoride-i...

Claims

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Application Information

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IPC IPC(8): C07C251/86C07C249/16G01N21/78
Inventor 张有明林奇王丹丹李艳魏太保
Owner NORTHWEST NORMAL UNIVERSITY
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