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Preparation method and application of magnetic porous supermolecular cyclodextrin-adsorbing material

An adsorption material, cyclodextrin technology, applied in chemical instruments and methods, adsorption water/sewage treatment, alkali metal oxides/hydroxides, etc., to achieve good stability and dispersibility, improve separation efficiency, and simple operation. Effect

Inactive Publication Date: 2018-08-17
JIANGSU GUOCHUANG ENVIRO PROTECTION TECH CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] Aiming at the shortcomings of existing adsorbents used in water pollution, the present invention provides a preparation method and application of a magnetic porous supramolecular cyclodextrin adsorption material

Method used

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  • Preparation method and application of magnetic porous supermolecular cyclodextrin-adsorbing material
  • Preparation method and application of magnetic porous supermolecular cyclodextrin-adsorbing material
  • Preparation method and application of magnetic porous supermolecular cyclodextrin-adsorbing material

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Effect test

Embodiment 1

[0025] A method for preparing a magnetic porous supramolecular cyclodextrin adsorption material, comprising the steps of:

[0026] 1) Under nitrogen protection, add 10g of β-cyclodextrin, 5g of tetrafluoroterephthalonitrile and 10g of potassium carbonate into the flask, then add 100ml of anhydrous tetrahydrofuran into the flask, heat up to 80°C for reaction, and stir at a speed of 500rpm After 25 hours, the reaction was complete, cooled to room temperature, and the product was washed several times with 10 wt% hydrochloric acid until potassium carbonate was removed (the filtrate was detected by barium chloride without precipitation), and then freeze-dried to obtain orange powder PBCD;

[0027] 2) Weigh 5g FeCl 3 ·6H 2 0.2g FeCl 2 4H 2 0 and 15g of the PBCD obtained in step 1) were placed in a reactor, and 120ml of water was added to the reactor, and then the reactor was heated to 80°C under nitrogen protection and stirring, kept for 5 minutes, and then concentrated ammonia w...

Embodiment 2

[0030] A method for preparing a magnetic porous supramolecular cyclodextrin adsorption material, comprising the steps of:

[0031] 1) Under nitrogen protection, add 20g of β-cyclodextrin, 8g of tetrafluoroterephthalonitrile and 10g of potassium carbonate into the flask, then add 250ml of anhydrous tetrahydrofuran into the flask, heat up to 70°C for reaction, and stir at a speed of 800rpm Reaction was complete after 20 hours, cooled to room temperature, and the product was washed several times with 10wt% nitric acid until potassium carbonate was removed (the filtrate was detected by barium chloride without precipitation), and then freeze-dried to obtain orange powder PBCD;

[0032] 2) Weigh 8g FeCl 3 ·6H 2 0.3g FeCl 2 4H 20 and 40g of the PBCD obtained in step 1) were placed in a reactor, and 220ml of water was added to the reactor, and then the reactor was heated to 100°C under nitrogen protection and stirring, kept for 15 minutes, and concentrated ammonia water was added d...

Embodiment 3

[0035] A method for preparing a magnetic porous supramolecular cyclodextrin adsorption material, comprising the steps of:

[0036] 1) Under nitrogen protection, add 8g of β-cyclodextrin, 2.2g of tetrafluoroterephthalonitrile and 15g of potassium carbonate in the flask, then add 80ml of anhydrous tetrahydrofuran into the flask, heat up to 90°C and react at a speed of 1000rpm After stirring for 40 hours, the reaction was complete, cooled to room temperature, and the product was washed several times with 10 wt% nitric acid until potassium carbonate was removed (the filtrate was detected by barium chloride without precipitation), and then freeze-dried to obtain orange powder PBCD;

[0037] 2) Weigh 5g FeCl 3 ·6H 2 0.2g FeCl 2 4H 2 0 and 50 g of the PBCD obtained in step 1) were placed in a reactor, and 100 ml of water was added to the reactor, and then the reactor was heated to 80° C. under nitrogen protection and stirring, kept for 30 minutes, and concentrated ammonia water wa...

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Abstract

The invention relates to a preparation method of a magnetic porous supermolecular cyclodextrin-adsorbing material, which comprises the following steps of 1) preparation of porous supermolecular cyclodextrin: in an inert atmosphere, adding an organic solvent into a mixture of beta-cyclodextrin, tetrafluoroterephthalonitrile and potassium carbonate, heating to 70 to 90 DEG C under the condition of stirring, then reacting at constant temperature for 20 to 40h, cooling to room temperature after the reaction is finished, then performing aftertreatment to obtain the porous supermolecular cyclodextrin; 2) preparation of magnetic porous supermolecular cyclodextrin: putting FeCl3.6H20, FeCl2.4H20 and the porous supermolecular cyclodextrin in a reactor, adding water, heating to 80 to 100 DEG C whilestirring in an inert atmosphere, reacting at constant temperature for 5 to 30min, then regulating the pH of reaction liquid to be 9 to 11, continuously stirring and reacting for 2 to 5h, cooling a product to room temperature, performing hysteresis separation to obtain black brown precipitate, washing the precipitate to be neutral, then performing vacuum drying to obtain the magnetic porous supermolecular cyclodextrin.

Description

technical field [0001] The invention relates to a preparation method of an adsorption material, in particular to a preparation method and application of a magnetic porous supramolecular cyclodextrin adsorption material, and belongs to the technical field of adsorption materials. Background technique [0002] Due to their unique properties, magnetic nanoparticles have good applications in magnetic storage, magnetic adsorbents, and magnetic fluids. Loading magnetic functions on nanomaterials with certain functions can greatly expand the functions of magnetic nanomaterials, which can be widely used in biomedicine, microelectronics, new energy, information, catalysis and other fields. The functional groups of magnetic nanoparticles and targeted positioning have injected new vitality into the research and become one of the hottest research fields at present. [0003] In the face of the increasingly serious water pollution in the environment, the most difficult to solve is the or...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J20/24B01J20/28B01J20/30C02F1/28C02F101/20C02F101/22
CPCB01J20/24B01J20/28009C02F1/286C02F2101/20C02F2101/22
Inventor 姚志建焦伟王伟莉李文涛仰凡甘萍
Owner JIANGSU GUOCHUANG ENVIRO PROTECTION TECH CO LTD
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