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Preparation method and application of cyclodextrin-citric acid graft loaded ceramic ball

A cyclodextrin, citric acid technology, applied in chemical instruments and methods, water pollutants, water/sludge/sewage treatment, etc., can solve unreasonable use, triazole pesticide residue restrictions, human health and environmental pollution, etc. problem, to achieve the effect of high adsorption and good recycling rate

Active Publication Date: 2021-05-28
WENZHOU UNIVERSITY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0002] Triazole pesticides (fluorotriol, diniconazole, penconazole, hexazole, tebuconazole, difenoconazole) are widely used as fungicides in the world to control lawn grass, vegetables, citrus, Field crops, ornamental plants and other diseases, although these triazole pesticides have played an important role in agricultural production, but their irrational use, potential threats to human health and environmental pollution have attracted more and more attention (C.L. Sanchez, C.L. Souders II, C.J. Pena-Delgado, K.T. Nguyen, N. Kroyter, N.E. Ahmadie, J.J. Aristizabal-Henao, J.A. Bowden, C.J. Martyniuk. NeuroToxicology. 80 (2020) 76-86; C.Y. Ezirimzie, P.C. Chike K.M. Iheanacho, N.R. Nwachukwu. J. Pollut. Eff. Cont, 5 (2017) 185; W. Yan, X. Wang, K. Li, T. Li, J. Wang, K. Yao, L. Cao, S. Zhao, Y. Ye. Pestic. Biochem. Phys., 156(2019) 160-169.)
Therefore, in many countries, the residues of triazole pesticides in vegetables and fruits are strictly limited, and the maximum residue limit is 0.010 mg / kg; therefore, how to remove triazole pesticides in water is also more and more concerned by people, but At present, there is no adsorbent that can effectively adsorb triazole pesticides in water.

Method used

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  • Preparation method and application of cyclodextrin-citric acid graft loaded ceramic ball
  • Preparation method and application of cyclodextrin-citric acid graft loaded ceramic ball
  • Preparation method and application of cyclodextrin-citric acid graft loaded ceramic ball

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Effect test

Embodiment 1

[0021] A preparation method of cyclodextrin-citric acid graft loaded ceramic balls, comprising the following steps:

[0022] Step 1: Add 10g of citric acid and 3.39g of sodium dihydrogen phosphate into a 100mL three-neck flask filled with 20mL of deionized water, stir and dissolve at room temperature, then add 10g of β-cyclodextrin to further stir and mix, and mix well reacting at a temperature of 60° C. for 1 h to obtain the first mixture;

[0023] Step 2: Add 40 g of porous ceramic balls into the first mixture and stir to mix. After mixing evenly, react at a temperature of 170° C. for 3 hours to obtain a second mixture. At this time, the second mixture is light yellow;

[0024] Step 3: Then continue to react the second mixture at a temperature of 75° C. for 35 minutes. At this time, the second mixture is yellow and dissolved with deionized water to obtain yellow insoluble matter; centrifuged and washed 5 times with deionized water, Separation until pH = 5; finally drying at...

Embodiment 2

[0026] A preparation method of cyclodextrin-citric acid graft loaded ceramic balls, comprising the following steps:

[0027] Step 1: Add 10g of citric acid and 4.44g of sodium dihydrogen phosphate into a 100mL three-necked flask filled with 30mL of deionized water, stir and dissolve at room temperature, and then add 10g of γ-cyclodextrin to further stir and mix. After mixing evenly reacting at a temperature of 40° C. for 3 hours to obtain the first mixture;

[0028] Step 2: Add 35g of porous ceramic balls into the first mixture and stir to mix. After mixing evenly, react at a temperature of 105° C. for 6 hours to obtain a second mixture. At this time, the second mixture is light yellow;

[0029] Step 3: Then continue to react the second mixture for 20 minutes at a temperature of 80° C. At this time, the second mixture is yellow and dissolved with deionized water to obtain a yellow insoluble matter; centrifuged, washed 5 times with deionized water, Separation until pH = 5; fin...

Embodiment 3

[0031] A preparation method of cyclodextrin-citric acid graft loaded ceramic balls, comprising the following steps:

[0032] Step 1: Add 3.4g of citric acid and 6.25g of disodium hydrogen phosphate into a 100mL three-neck flask filled with 20mL of deionized water, stir and dissolve at room temperature, then add 10g of β-cyclodextrin and stir to mix evenly Then react for 2.5 hours at a temperature of 45° C. to obtain the first mixture;

[0033] Step 2: Add 40g of porous ceramic balls into the first mixture and stir to mix. After mixing evenly, react at a temperature of 150°C. The reaction time is 2.5h to obtain the second mixture. At this time, the second mixture is light yellow ;

[0034] Step 3: Then continue to react the second mixture at a temperature of 75° C. for 25 minutes. At this time, the second mixture is yellow, and is dissolved in deionized water to obtain a yellow insoluble matter; centrifuged, washed 5 times with deionized water, Separation until pH = 5; finall...

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Abstract

The invention discloses a preparation method and application of a cyclodextrin-citric acid graft loaded ceramic ball. Cyclodextrin, citric acid and a porous ceramic ball are used as reactants, a catalyst is also added, the reactants react in deionized water, the cyclodextrin is any one of alpha-cyclodextrin, beta-cyclodextrin and gamma-cyclodextrin, and the catalyst is any one of sodium hypophosphite, sodium dihydrogen phosphate and disodium hydrogen phosphate; the cyclodextrin-citric acid graft loaded ceramic ball can be used as an adsorbent to adsorb triazole pesticides in water, is good in adsorption stability, is good in stability at different pH values and different temperatures, and has a relatively high adsorption effect on the triazole pesticides; and the cyclodextrin-citric acid graft loaded ceramic ball as an adsorbent has a good cyclic utilization rate on triazole pesticides, and the initial capacity of the cyclodextrin-citric acid graft loaded ceramic ball still reaches 80.1% even when the cyclodextrin-citric acid graft loaded ceramic ball is recycled for the tenth time, so that the cyclodextrin-citric acid graft loaded ceramic ball is beneficial to reuse and has high economic value.

Description

technical field [0001] The invention relates to the technical field of organic synthesis, in particular to a preparation method and application of cyclodextrin-citric acid graft-loaded porcelain balls. Background technique [0002] Triazole pesticides (fluorotriol, diniconazole, penconazole, hexazole, tebuconazole, difenoconazole) are widely used as fungicides in the world to control lawn grass, vegetables, citrus, Field crops, ornamental plants and other diseases, although these triazole pesticides have played an important role in agricultural production, but their irrational use, potential threats to human health and environmental pollution have attracted more and more attention (C.L. Sanchez, C.L. Souders II, C.J. Pena-Delgado, K.T. Nguyen, N. Kroyter, N.E. Ahmadie, J.J. Aristizabal-Henao, J.A. Bowden, C.J. Martyniuk. NeuroToxicology. 80 (2020) 76-86; C.Y. Ezirimzie, P.C. Chike K.M. Iheanacho, N.R. Nwachukwu. J. Pollut. Eff. Cont, 5 (2017) 185; W. Yan, X. Wang, K. Li, T....

Claims

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Application Information

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IPC IPC(8): B01J20/24B01J20/30C02F1/28C02F101/30C02F101/34C02F101/36C02F101/38
CPCB01J20/24C02F1/286C02F2101/306C02F2101/36C02F2101/34C02F2101/38
Inventor 高文霞陈洁李兴伟刘妙昌吴华悦黄小波
Owner WENZHOU UNIVERSITY
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