Preparation of 8-hydroxy-quinoline modified polyacrylonitrile fiber

Abstract

A process for preparing 8-hydroxy quinoline modified polyacrylontirile fibre includes such steps as proportionally loading hollow polyacrylonitrile fibre and hydrazine hydrate in reactor, reacting at 60-100 deg.c for 2-16 hr, reacting on diethylene triamine at 80-100 deg.C for 2-16 hr, proportionally mixing with sodium nitrite, reacting in acidic acid at -5-10 deg.C for 1-4 hr, filtering, washing with water at 0 deg.C, and reacting on the solution of 8-hydroxy quinoline in alcohol for 1-16 hr.

Description

technical field

[0001] The invention relates to a preparation method of a chelating fiber, in particular to a polyacrylonitrile fiber modified by 8-hydroxyquinoline. Background technique

[0002] In the detection process of metal elements in natural water, separation and enrichment technology is indispensable. This is because the metal content in general natural water is much lower than the detection limit of many analytical instruments (such as: flame atomic absorption, plasma spectroscopy, graphite furnace atomic absorption, etc.) and cannot be directly analyzed. At the same time, some natural water bodies such as seawater contain more salt and complex matrix, which limits the use of plasma mass spectrometers with the highest sensitivity today.

[0003] 8-Hydroxyquinoline is a kind of organic ligand with good performance. It can combine with more than 60 kinds of metal ions under different conditions. At the same time, it can separate transition elements, heavy metal elem...

Examples

Embodiment 1

[0018] Embodiment 1, put the polyacrylonitrile hollow fiber and hydrazine hydrate in the ratio of 1:20 in the reactor, and react at 100°C for 2 hours to obtain the product (1); mix the product (1) with diethylenetriamine Put it into the reactor at a ratio of 1:50, and react at 80°C for 10 hours to obtain the product (2); mix the product (2) with sodium nitrite at a ratio of 1:1, and in acetic acid medium, -5 ℃ for 4 hours to obtain the product (3); after the product (3) was filtered and washed with water at 0 ℃, it was reacted with the ethanol solution of 8-hydroxyquinoline in a ratio of 2:1 for 6 hours to produce 8-hydroxyquinoline Quinoline chelated polyacrylonitrile fibers.

Embodiment 2

[0019] Embodiment 2, put polyacrylonitrile hollow fiber and hydrazine hydrate in the ratio of 1:60 in the reactor, react at 60 ℃ for 16 hours, and make product (1); product (1) is mixed with diethylenetriamine Put it into the reaction kettle at a ratio of 1:80, and react at 100°C for 2 hours to obtain the product (2); mix the product (2) with sodium nitrite at a ratio of 1:10, in acetic acid medium, 10°C The product (3) was reacted at lower temperature for 1 hour to obtain the product (3); after the product (3) was filtered and washed with water at 0°C, it was reacted with the ethanol solution of 8-hydroxyquinoline in a ratio of 2:4 for 1 hour to make 8-hydroxyquinoline Phenyl chelated polyacrylonitrile fibers.

Embodiment 3

[0020] Embodiment 3, put polyacrylonitrile hollow fiber and hydrazine hydrate in the ratio of 1:100 in the reactor, react at 60 ℃ for 8 hours, and obtain product (1); product (1) is mixed with diethylenetriamine Put it into the reaction kettle at a ratio of 1:20, and react at 80°C for 16 hours to obtain the product (2); mix the product (2) with sodium nitrite at a ratio of 1:5, in acetic acid medium, 5°C The product (3) was reacted at lower temperature for 4 hours to obtain the product (3); after the product (3) was filtered and washed with water at 0°C, it was reacted with the ethanol solution of 8-hydroxyquinoline in a ratio of 2:2 for 16 hours to make 8-hydroxyquinoline Phenyl chelated polyacrylonitrile fibers.

[0021] Through following test example, can know the performance of the 8-hydroxyquinoline chelate fiber that above-mentioned embodiment makes.

technical field

[0001] The invention relates to a preparation method of a chelating fiber, in particular to a polyacrylonitrile fiber modified by 8-hydroxyquinoline. Background technique

[0002] In the detection process of metal elements in natural water, separation and enrichment technology is indispensable. This is because the metal content in general natural water is much lower than the detection limit of many analytical instruments (such as: flame atomic absorption, plasma spectroscopy, graphite furnace atomic absorption, etc.) and cannot be directly analyzed. At the same time, some natural water bodies such as seawater contain more salt and complex matrix, which limits the use of plasma mass spectrometers with the highest sensitivity today.

[0003] 8-Hydroxyquinoline is a kind of organic ligand with good performance. It can combine with more than 60 kinds of metal ions under different conditions. At the same time, it can separate transition elements, heavy metal elem...

Examples

Embodiment 1

[0018] Embodiment 1, put the polyacrylonitrile hollow fiber and hydrazine hydrate in the ratio of 1:20 in the reactor, and react at 100°C for 2 hours to obtain the product (1); mix the product (1) with diethylenetriamine Put it into the reactor at a ratio of 1:50, and react at 80°C for 10 hours to obtain the product (2); mix the product (2) with sodium nitrite at a ratio of 1:1, and in acetic acid medium, -5 ℃ for 4 hours to obtain the product (3); after the product (3) was filtered and washed with water at 0 ℃, it was reacted with the ethanol solution of 8-hydroxyquinoline in a ratio of 2:1 for 6 hours to produce 8-hydroxyquinoline Quinoline chelated polyacrylonitrile fibers.

Embodiment 2

[0019] Embodiment 2, put polyacrylonitrile hollow fiber and hydrazine hydrate in the ratio of 1:60 in the reactor, react at 60 ℃ for 16 hours, and make product (1); product (1) is mixed with diethylenetriamine Put it into the reaction kettle at a ratio of 1:80, and react at 100°C for 2 hours to obtain the product (2); mix the product (2) with sodium nitrite at a ratio of 1:10, in acetic acid medium, 10°C The product (3) was reacted at lower temperature for 1 hour to obtain the product (3); after the product (3) was filtered and washed with water at 0°C, it was reacted with the ethanol solution of 8-hydroxyquinoline in a ratio of 2:4 for 1 hour to make 8-hydroxyquinoline Phenyl chelated polyacrylonitrile fibers.

Embodiment 3

[0020] Embodiment 3, put polyacrylonitrile hollow fiber and hydrazine hydrate in the ratio of 1:100 in the reactor, react at 60 ℃ for 8 hours, and obtain product (1); product (1) is mixed with diethylenetriamine Put it into the reaction kettle at a ratio of 1:20, and react at 80°C for 16 hours to obtain the product (2); mix the product (2) with sodium nitrite at a ratio of 1:5, in acetic acid medium, 5°C The product (3) was reacted at lower temperature for 4 hours to obtain the product (3); after the product (3) was filtered and washed with water at 0°C, it was reacted with the ethanol solution of 8-hydroxyquinoline in a ratio of 2:2 for 16 hours to make 8-hydroxyquinoline Phenyl chelated polyacrylonitrile fibers.

[0021] Through following test example, can know the performance of the 8-hydroxyquinoline chelate fiber that above-mentioned embodiment makes.

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