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Preparation method and application of magnetic carboxymethyl-beta-cyclodextrin polymer

A technology of cyclodextrin polymer and carboxymethyl, which is applied in the direction of alkali metal compounds, chemical instruments and methods, water pollutants, etc., can solve problems such as loss and recycling difficulties, and achieve good regeneration performance, easy operation, and convenience The effect of recycling

Active Publication Date: 2018-12-18
NANJING UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, β-cyclodextrin has a certain solubility in water, making its recycling difficult and loss

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0027] Preparation of magnetic carboxymethyl β-cyclodextrin polymer:

[0028] 1) Dissolve 9g of β-cyclodextrin and 7.14g of NaOH in 20ml of deionized water, heat and stir at 90°C for 5min, then drop chloroacetic acid solution (17.46 in 20ml of deionized water) into a three-necked flask (dropping is completed within 5min); After 3 hours, cool to room temperature, adjust the system to PH = 5 with hydrochloric acid, add an appropriate amount of methanol to form a white precipitate, continue to add methanol until the white precipitate no longer occurs, filter and dry the precipitate in vacuum at 80°C;

[0029] 2) 3g carboxymethyl β-cyclodextrin, 1.5g tetrafluoroterephthalonitrile, 4g K 2 CO 3 Add to a 100ml pressure bottle, add 55ml tetrahydrofuran and 5.5ml N,N-dimethylformamide, and ultrasonicate the mixture;

[0030] 3) Vacuumize the pressure bottle for 1 minute and fill it with nitrogen for 1 minute alternately for 3 times, so that the reaction is carried out in a nitrogen e...

Embodiment 2

[0036] Preparation of magnetic carboxymethyl β-cyclodextrin polymer:

[0037] 1) Dissolve 9g of β-cyclodextrin and 7.14g of NaOH in 20ml of deionized water, heat and stir at 90°C for 5min, then drop chloroacetic acid solution (17.46 in 20ml of deionized water) into a three-necked flask (dropping is completed within 5min); After 3 hours, cool to room temperature, adjust the system to PH = 5 with hydrochloric acid, add an appropriate amount of methanol to form a white precipitate, continue to add methanol until the white precipitate no longer occurs, filter and dry the precipitate in vacuum at 80°C;

[0038] 2) 3g carboxymethyl β-cyclodextrin, 1.5g tetrafluoroterephthalonitrile, 4g K 2 CO 3 Add to a 100ml pressure bottle, add 55ml tetrahydrofuran and 5.5ml N,N-dimethylformamide, and ultrasonicate the mixture;

[0039] 3) Vacuumize the pressure bottle for 1 minute and fill it with nitrogen for 1 minute alternately for 3 times, so that the reaction is carried out in a nitrogen e...

Embodiment 3

[0045] The magnetic carboxymethyl β-cyclodextrin polymer (MNP-P-CDP) prepared in Example 1 adsorbs estriol:

[0046] Mix 100 mg of the magnetic carboxymethyl β-cyclodextrin polymer MNP-P-CDP obtained in Example 1 with 50 ml of 0.1 mmol estriol solution, take out the sample with a syringe, filter it with a filter membrane, and measure the sample by high performance liquid chromatography The remaining concentration of estriol in the solution can remove 90% of the estriol in the solution within 10 minutes.

[0047] The ultrasonic magnetic β-cyclodextrin polymer was soaked in ethanol to regenerate it, and the adsorption experiment was continued for three cycles, with almost no loss in sample performance.

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Abstract

The invention provides a preparation method and an application of a magnetic carboxymethyl-beta-cyclodextrin polymer. The preparation method comprises the following steps: carboxylating beta-cyclodextrin, reacting the obtained carboxymethyl-beta-cyclodextrin with a crosslinking agent and a catalyst in a solvent to obtain a carboxymethyl-beta-cyclodextrin polymer, adding the carboxymethyl-beta-cyclodextrin polymer, trisodium citrate, tin(II) bis(2-ethylhexanoate), methanol, FeCl2.4H2O and FeCl3.6H2O into a three-necked flask according to a certain molar ratio, selecting 25% NH3.H20 as an alkalisource, and reacting obtained the system under the protection of nitrogen to obtain the magnetic carboxymethyl-beta-cyclodextrin polymer after the reaction is finished. Ferroferric oxide is successfully connected to the carboxymethyl-beta-cyclodextrin polymer by a coprecipitation technology, so the obtained polymer is magnetic, and can rapidly adsorb endocrine disrupting substances in the environment.

Description

technical field [0001] The invention relates to the technical field of environmental protection materials, in particular to a method for preparing magnetic carboxymethyl β-cyclodextrin polymer and its application. Background technique [0002] Endocrine disruptors are chemical substances that interfere with the endocrine system exogenously. They enter water bodies through precipitation, surface runoff, sewage discharge, etc., causing water environment pollution. The concentration of endocrine disruptors in the environment is very low (ng / L), but they can cause high biological toxicity. At present, advanced oxidation and adsorption are mostly used for the removal of endocrine disruptors, but advanced oxidation technology has many influencing factors and high cost; the commonly used adsorbent is activated carbon, but the regeneration cost of activated carbon is high, and there are certain problems. limitation. At the same time, the concentration of endocrine disruptors in th...

Claims

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Application Information

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IPC IPC(8): B01J20/26B01J20/28B01J20/30C02F1/28C02F101/30
CPCC02F1/285B01J20/265B01J20/28009C02F2101/305
Inventor 谢显传胡月许贵洲
Owner NANJING UNIV
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