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A kind of oxime-based multi-layer polyimide microsphere adsorption material and preparation method thereof

A polyimide microsphere, polyimide technology, applied in chemical instruments and methods, adsorption water/sewage treatment, inorganic chemistry, etc., to achieve the effect of high uranium adsorption capacity, high adsorption efficiency, easy recovery and reuse

Active Publication Date: 2022-08-02
HARBIN ENG UNIV
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, there is no report on the preparation of uranium adsorption materials by introducing oxime groups into polyimide.

Method used

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  • A kind of oxime-based multi-layer polyimide microsphere adsorption material and preparation method thereof

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Effect test

Embodiment 1

[0021] 1. Preparation process of multi-layer polyimide microspheres: under nitrogen atmosphere, 4 mmol of DAAQ was dissolved in 16 mL of N-methylpyrrolidone. After magnetic stirring for 30 min, 4 mmol BTDA was added to the above solution in 6 times within 1 h for the reaction, the reaction temperature was 20 °C, and the stirring was continued for 12 h. After the reaction, it was transferred to the reaction kettle for solvothermal reaction, the reaction temperature was 180°C, and the reaction time was 10h. After the reaction, the solid material was filtered, washed with deionized water and ethanol in turn, and dried at 60° C. for 12 h to prepare multi-layer polyimide microspheres.

[0022] 2. The preparation process of oxime-based multi-lamellar polyimide microspheres: Disperse 0.1 g of multi-lamellar polyimide microspheres in 15 mL of a mixture of deionized water and ethanol with a volume ratio of 1:4, add 0.6g of hydroxylamine hydrochloride, ultrasonically dispersed for 30s;...

Embodiment 2

[0026] 1. Preparation process of multi-layer polyimide microspheres: under nitrogen atmosphere, 4 mmol of DAAQ was dissolved in 25 mL of N-methylpyrrolidone. After magnetic stirring for 30 min, 4 mmol BTDA was added to the above solution in 6 times within 1 h for the reaction, the reaction temperature was 20 °C, and the stirring was continued for 12 h. After the reaction, it was transferred to the reaction kettle for solvothermal reaction, the reaction temperature was 180°C, and the reaction time was 12h. After the reaction, the solid matter was filtered, washed with deionized water and ethanol in turn, and dried at 70° C. for 12 h to prepare multi-layer polyimide microspheres.

[0027] 2. Preparation process of oxime-based multi-lamellar polyimide microspheres: Disperse 0.1 g of multi-lamellar polyimide microspheres in 13 mL of a mixture of deionized water and ethanol with a volume ratio of 1:4, add 0.7g of hydroxylamine hydrochloride, ultrasonically dispersed for 30s; use 1...

Embodiment 3

[0031] 1. Preparation process of multi-layer polyimide microspheres: under nitrogen atmosphere, 4 mmol of DAAQ was dissolved in 10 mL of N-methylpyrrolidone. After magnetic stirring for 30 min, 4 mmol BTDA was added to the above solution in 6 times within 1 h for the reaction, the reaction temperature was 18 °C, and the stirring was continued for 12 h. After the reaction, it was transferred to the reaction kettle for solvothermal reaction, the reaction temperature was 180°C, and the reaction time was 12h. After the reaction, the solid material was filtered, washed with deionized water and ethanol in turn, and dried at 60° C. for 12 h to prepare multi-layer polyimide microspheres.

[0032] 2. The preparation process of oxime-based multi-lamellar polyimide microspheres: Disperse 0.1 g of multi-lamellar polyimide microspheres in 10 mL of a mixture of deionized water and ethanol with a volume ratio of 1:4, add 0.6g of hydroxylamine hydrochloride, ultrasonically dispersed for 30s;...

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Abstract

The invention provides an oxime-based multi-layer polyimide microsphere adsorption material and a preparation method thereof. Firstly, using 2,6-diaminoanthraquinone (DAAQ) and 3,3',4,4'-benzophenone tetraacid dianhydride (BTDA) as raw materials, multi-lamellar polyimide microstructures were prepared by solvothermal method. ball. Hydroxylamine hydrochloride (NH 2 OH . HCl) and oxime-modified it to prepare oxime-based multi-layer polyimide microspheres. The prepared oxime-based multi-layer polyimide microsphere adsorption material has stable chemical properties and good adsorption performance, especially high uranium adsorption capacity under weak acid conditions. The multi-layer polyimide microsphere adsorption material and the preparation method thereof provided by the invention have the advantages of high adsorption efficiency, fast adsorption rate, simple preparation steps, short period, low cost, etc., and have broad application prospects, especially in the treatment of weak It has obvious advantages in acidic uranium-containing wastewater.

Description

technical field [0001] The invention belongs to the field of adsorption material preparation, and mainly relates to an oxime-based multi-layer polyimide microsphere adsorption material and a preparation method thereof, in particular to an oxime-based multi-layer polyimide microsphere with high-efficiency uranium adsorption capacity Ball adsorption material and preparation method thereof. Background technique [0002] The continuous progress and development of society have put forward an urgent need for low-carbon energy. As a low-carbon energy, nuclear energy has been developed and utilized by countries all over the world. Uranium is an important element in the nuclear energy industry and is an efficient nuclear fuel, but it is radioactive and toxic. If the uranium-containing wastewater produced by the nuclear energy industry is directly discharged into the natural environment without treatment, it can exist in soil and water bodies for a long time and stably, posing a ser...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01J20/26B01J20/28B01J20/30C02F1/28
CPCB01J20/265B01J20/28021B01J20/28035C02F1/285C02F2101/006
Inventor 张春红朱立恩马福秋朱睿琪秦非凡刘立佳董红星
Owner HARBIN ENG UNIV
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