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Preparation method and application of amidoxime-modified para-aramid adsorption material

A technology based on para-aramid and amidoxime, which is applied in the field of preparation of adsorption materials, can solve the problems of poor metal ion chelation performance, practical application limitations, and small adsorption capacity, and achieve large adsorption capacity of metal ions and long-term reduction Pollution, improve the effect of comprehensive utilization

Active Publication Date: 2017-05-17
LUDONG UNIVERSITY +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, amide bonds have poor chelating properties for metal ions
In previous studies, materials with adsorption properties were obtained by introducing nitro groups and amino groups on the surface of para-aramid fiber, and its effect on Hg 2+ , Cu 2+ , Pb 2+ The results show that although the adsorption performance of modified PPTA on metal ions is higher than that of unmodified fibers, the adsorption capacity is still small, and its practical application is greatly limited.

Method used

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  • Preparation method and application of amidoxime-modified para-aramid adsorption material

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preparation example Construction

[0024] The preparation method of the para-aramid adsorption material modified by amidoxime group comprises the following steps:

[0025] 1) Wash the para-aramid powder with toluene, acetone, and deionized water for 3-6 hours respectively, and then vacuum-dry it at 60°C to obtain pretreated para-aramid powder;

[0026] 2) Under the protection of nitrogen, mix sodium hydride and anhydrous dimethyl sulfoxide at a molar ratio of 1:125, stir mechanically, wait until the temperature rises to 70°C, continue the reaction for 40-60min, then cool down to 30°C, to obtain a mixed solution;

[0027] 3) Slowly add the pretreated para-aramid powder obtained in step 1) to the mixed solution obtained by the reaction in step 2) several times, the amide bond in the aramid powder and the mole of sodium hydride The ratio is 1:1, the reaction is at 25-40°C for 16-72h, and an orange-red solution is obtained; the temperature is raised to 50°C, and redistilled acrylonitrile is slowly dropped into the...

Embodiment 1

[0031] 1) Wash the waste para-aramid powder with toluene, acetone, and deionized water in sequence for 3 hours, and then vacuum-dry it at 60°C to obtain pretreated para-aramid powder;

[0032] 2) After purging the dry 250mL three-necked flask with nitrogen for 10min, at 30°C, add 0.4034g of sodium hydride (0.017mol) and 150mL of anhydrous dimethyl sulfoxide (2.112mol), stir mechanically, and heat up to 70°C, keep warm for 40min, then cool down to 30°C to obtain a mixed solution;

[0033] 3) Slowly add 2 g of the pretreated para-aramid powder obtained in step 1) to the mixed solution obtained in step 2), and mechanically stir at 30° C. for 48 hours to obtain an orange-red solution; raise the temperature to 50° C. 11 mL of redistilled acrylonitrile (0.168 mol) was slowly dropped into the orange-red solution, and the reaction was continued for 16 hours to obtain a purple-red solution;

[0034] 4) Add 500mL of 0.1mol / L dilute hydrochloric acid to the purple-red solution obtained ...

Embodiment 2

[0037] 1) Wash the waste para-aramid powder with toluene, acetone, and deionized water for 6 hours, and then vacuum-dry it at 60°C to obtain pretreated para-aramid powder;

[0038] 2) After purging the dry 250mL three-necked flask with nitrogen for 10min, at 30°C, add 0.4034g of sodium hydride (0.017mol) and 150mL of anhydrous dimethyl sulfoxide (2.112mol), stir mechanically, and heat up to 70°C, keep warm for 60min, then cool down to 30°C to obtain a mixed solution;

[0039] 3) Slowly add 2 g of the pretreated para-aramid powder obtained in step 1) to the mixed solution in step 2), and mechanically stir for 72 hours at 25° C. to obtain an orange-red solution; raise the temperature to 50° C. Slowly drop 33 mL of redistilled acrylonitrile (0.504 mol) into the orange-red solution, and continue the reaction at 50°C for 16 hours to obtain a purple-red solution;

[0040] 4) Add 700 mL of 0.1 mol / L dilute hydrochloric acid to the purple-red solution obtained in step 3), precipitate...

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Abstract

The invention relates to a preparation method of an amidoxime group modified p-aramid adsorption material and application of the amidoxime group modified p-aramid adsorption material in the adsorption of metal ions. The preparation method has advantages of simplicity in preparation and high efficiency. The preparation method comprises the following steps: (1) as waste p-aramid powder is used as a research target, anhydrous dimethylsulfoxide is adopted as a solvent, modifying the p-aramid (PPTA) by utilizing acrylonitrile, wherein the molar ratio of an amido group to the acrylonitrile is (1 to 10) to (1 to 50), introducing a cyano group onto the surface of PPTA to obtain acrylonitrile modified p-aramid (PPTA-AN); and (2) reacting the PPTA-AN with hydroxylamine hydrochloride under the condition that anhydrous methanol is used as a solvent, converting the cyano group in the PPTA-AN to an amidoxime group to obtain the amidoxime group modified p-aramid adsorption material (PPTA-AO). The adsorption material prepared by adopting the method is high in capacity of adsorbing the metal ions, can be used for treating heavy metal ion waste water and has a unique advantage in the real application process.

Description

technical field [0001] The invention relates to the field of preparation of adsorption materials, in particular to a para-aramid adsorption material modified with amidoxime groups and its application in metal ion adsorption. Background technique [0002] Aramid (PPTA) is a new type of synthetic polymer material. Due to its high performance, it has been widely used in cables, insulating paper, helmets, body armor, and aircraft shells. With the continuous expansion of the production scale and demand of aramid products, the amount of waste has also increased dramatically. The stability of high temperature resistance and chemical corrosion resistance prevents it from being recycled by reheating and melting. Relying on traditional landfill or incineration can no longer meet the requirements of sustainable development. As countries around the world have higher and higher requirements for the utilization rate of waste resources, it is imperative to develop environmentally friendly...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01J20/26B01J20/30C02F1/28C02F1/62
Inventor 曲荣君李沙沙张盈马千里宋西全徐长洲孙昌梅高静静
Owner LUDONG UNIVERSITY