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Preparation method for illite magnetic composite surface imprinting temperature-sensitive adsorbent

A magnetic composite material, surface imprinting technology, applied in chemical instruments and methods, adsorption water/sewage treatment, alkali metal compounds, etc., can solve problems such as allergies, joint lesions, antibiotics, and human health threats

Active Publication Date: 2015-09-09
陕西三水环境技术有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, often due to unreasonable use and abuse, a large amount of antibiotic residues enter the water body and soil through the excretion of humans and animals. After ingestion by the human body, adverse reactions such as diarrhea, nausea, allergies, and joint lesions may occur.
The accumulation of antibiotic residues represented by ciprofloxacin in the environment has posed a potential threat to human health, and it is difficult to target, separate and quantitatively detect them by general treatment methods

Method used

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  • Preparation method for illite magnetic composite surface imprinting temperature-sensitive adsorbent
  • Preparation method for illite magnetic composite surface imprinting temperature-sensitive adsorbent
  • Preparation method for illite magnetic composite surface imprinting temperature-sensitive adsorbent

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0023] (1) Preparation of magnetic illite composites

[0024] The massive illite is ground by a ball mill and passed through a 100-mesh sieve, calcined at 150°C for 22 hours, then the illite is refluxed at 70°C for 12 hours in concentrated sulfuric acid and concentrated nitric acid with a volume ratio of 1:3, and the product is washed with distilled water until neutral , dried at 60°C to obtain activated illite powder;

[0025]According to the proportion of activated illite, ferric chloride hexahydrate, sodium acetate and ethylene glycol: 1.0:0.3:2.5:70 (g / g / g / mL), add activated illite, ferric chloride hexahydrate to the flask (FeCl.6H 2 O), sodium acetate (NaAc), ethylene glycol, and the mixed solution were ultrasonically 3.0h under the protection of nitrogen, and the mixed solution was uniformly dispersed. Then, polyethylene glycol (PEG-1500) and polyethylene glycol were added to the dispersion. The amount of alcohol added is according to the mass ratio of activated illite...

Embodiment 2

[0034] Take 25ml of CIP solutions with initial concentrations of 5, 10, 20, 30, 50, 60, 80, 100, 150, and 200 μmol / L and add them to centrifuge tubes, add 10 mg of imprinted adsorbent and non-imprinted adsorbent respectively, and test The solution was placed in a water bath at 25°C for 12 hours, the supernatant was separated and collected by a Nd-Fe-B permanent magnet, and the molecular concentration of unadsorbed ciprofloxacin was measured with a UV-visible spectrophotometer, and the adsorption capacity was calculated. figure 2 The results show that the imprinted adsorbent has a saturated adsorption capacity of 58.25umol / g, which is higher than that of the non-imprinted adsorbent, which is 26.50umol / g, which proves that the imprinted adsorbent has a large number of imprinted holes and shows a good imprinting effect.

Embodiment 3

[0036] Take 25ml of CIP solution with an initial concentration of 100μmol / L and add it to a centrifuge tube, add 10mg of imprinted adsorbent and non-imprinted adsorbent, and place the test solution in a water bath at 25°C for 2, 5, 10, 30, 45 , 60, 90, 120 and 150min, after standing still, the supernatant was separated and collected by Nd-Fe-B permanent magnet, the molecular concentration of unadsorbed ciprofloxacin was measured by UV-Vis spectrophotometer, and the adsorption capacity was calculated ,From image 3 It can be seen from the figure that at the beginning, with the increase of adsorption time, the adsorption capacity increased rapidly, and the adsorption reached equilibrium after 30 min. In the whole adsorption time range, the adsorption capacity of magnetic molecularly imprinted adsorbent to ciprofloxacin was greater than that of non-imprinted adsorbent to ciprofloxacin. Profloxacin adsorption capacity, showing good adsorption performance.

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Abstract

The present invention relates to a preparation method for an illite magnetic composite surface imprinting temperature-sensitive adsorbent. The method comprises that: magnetic illite is prepared through solvothermal synthesis; the surface of magnetic illite undergoes ethylene functionalized modification performed by using KH570 and is used as a matrix material; ciprofloxacin is used as a template, hydroxyethyl methacrylate and methacrylic acid are used as a functional monomer; N-isopropyl acrylamide is used as a temperature-sensitive monomer; polyethylene glycol dimethacrylate and N,N'-methylene bisacrylamide are used as a crosslinking agent; copper bromide, N,N,N',N",N"-pentamethyldiethylene triamine and 2-bromoisobutyrate are used as a initiator; the illite magnetic composite surface imprinting temperature-sensitive adsorbent is prepared in a mixed system of methanol and water, and the adsorbent is used for selectively identifying and separating ciprofloxacin in an aqueous environment. The preparation method for illite magnetic composite surface imprinting temperature-sensitive adsorbent provided by the present invention is low in cost and simple in preparation, and the adsorbent is high in accuracy in identifying a target molecule, high in selectivity and excellent in the separation and enrichment capability.

Description

technical field [0001] The invention relates to a method for preparing a temperature-sensitive adsorbent imprinted on the surface of an illite magnetic composite material, and belongs to the technical field of preparation of environmental functional materials. Background technique [0002] Molecularly imprinted polymers are polymers that can specifically recognize and selectively adsorb target molecules (template molecules) synthesized by molecular imprinting technology. Surface molecular imprinting technology, by establishing molecular recognition sites on the surface of matrix materials, solves the problems of incomplete removal of template molecules, low binding capacity, slow mass transfer, and over-embedding of active sites caused by high cross-linking in traditional bulk polymerization. Deep, poor adsorption-desorption kinetics and other shortcomings. [0003] Illite is a silicate clay mineral with a layered structure. Due to its large specific surface area, low cost,...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08F292/00C08F220/28C08F220/06C08F220/54C08F222/14C08F222/38C08J9/26B01J20/26B01J20/30B01J20/28C02F1/28
Inventor 毛艳丽罗世田王红强牛云峰焦学然陈爱玖刘海成郭一飞王增欣陈松涛
Owner 陕西三水环境技术有限公司
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