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Preparation method of magnetic fullerene molecularly-imprinted nano-composite material

A nanocomposite material, magnetic fullerene technology, applied in chemical instruments and methods, alkali metal compounds, alkali metal oxides/hydroxides, etc., can solve the problem of molecularly imprinted polymers with small adsorption capacity, poor selectivity, and cumbersome operation and other problems, to achieve the effect of efficient selective separation and purification, saving processing time and cost, and increasing specific surface area

Active Publication Date: 2016-12-14
安徽出入境检验检疫局检验检疫技术中心 +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] In order to overcome the disadvantages of poor selectivity and serious matrix interference in the pretreatment of traditional sulfonylurea herbicides, as well as the disadvantages of traditional molecularly imprinted polymers such as small adsorption capacity, slow adsorption speed, cumbersome operation, and low removal efficiency, high selectivity is achieved. Adsorption and separation to improve the sensitivity and accuracy of the detection method

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0026] 1. Fullerene (C 60 ) / Fe 3 o 4 Preparation of magnetic nanoparticles:

[0027] Take 0.5 g fullerene, 1.0 g diethyl malonate, 2.3 g carbon tetrabromide and 2.0 mL diazabicyclo (DBU) in 25 mL o-dichlorobenzene for two days at room temperature, pass through a silica gel column Purification yields the hexa-substituted fullerene ester product. The hexa-substituted fullerene ester product was dissolved in 25 mL of o-dichlorobenzene, and then 25 mL of 10% sodium hydroxide aqueous solution was added for hydrolysis to obtain carboxylated fullerene (C 60 -COOH).

[0028] Magnetic fullerenes were prepared by hydrothermal synthesis. Weigh 1.6 g ferric chloride hexahydrate (FeCl 3 ·6H 2 O) Dissolve in 40 mL ethylene glycol. Then 400 mg carboxylated fullerene (C 60 -COOH), ultrasonically dispersed for 3 h. Next, 5.0 g of sodium acetate (NaAc) and 2.0 g of polyethylene glycol (PEG) were added and stirred for 30 min. The mixture was sealed in an autoclave, reacted at 200 °C...

Embodiment 2

[0034] 1. Fullerene (C 60 ) / Fe 3 o 4 Preparation of magnetic nanoparticles:

[0035] Take 0.5 g fullerene, 1.0 g diethyl malonate, 2.3 g carbon tetrabromide and 2.0 mL diazabicyclo (DBU) in 25 mL o-dichlorobenzene for two days at room temperature, pass through a silica gel column Purification yields the hexa-substituted fullerene ester product. The hexa-substituted fullerene ester product was dissolved in 25 mL of o-dichlorobenzene, and then 25 mL of 10% sodium hydroxide aqueous solution was added for hydrolysis to obtain carboxylated fullerene (C 60 -COOH).

[0036] Magnetic fullerenes were prepared by hydrothermal synthesis. Weigh 1.6 g ferric chloride hexahydrate (FeCl 3 ·6H 2 O) Dissolve in 40 mL ethylene glycol. Then 400 mg carboxylated fullerene (C 60 -COOH), ultrasonically dispersed for 3 h. Next, 5.0 g of sodium acetate (NaAc) and 2.0 g of polyethylene glycol (PEG) were added and stirred for 30 min. The mixture was sealed in an autoclave, reacted at 200 °C...

Embodiment 3

[0042] 1. Fullerene (C 60 ) / Fe 3 o 4 Preparation of magnetic nanoparticles:

[0043] Take 0.5 g fullerene, 1.0 g diethyl malonate, 2.3 g carbon tetrabromide and 2.0 mL diazabicyclo (DBU) in 25 mL o-dichlorobenzene for two days at room temperature, pass through a silica gel column Purification yields the hexa-substituted fullerene ester product. The hexa-substituted fullerene ester product was dissolved in 25 mL of o-dichlorobenzene, and then 25 mL of 10% sodium hydroxide aqueous solution was added for hydrolysis to obtain carboxylated fullerene (C 60 -COOH).

[0044] Magnetic fullerenes were prepared by hydrothermal synthesis. Weigh 1.6 g ferric chloride hexahydrate (FeCl 3 ·6H 2 O) Dissolve in 40 mL ethylene glycol. Then 400 mg carboxylated fullerene (C 60 -COOH), ultrasonically dispersed for 3 h. Next, 5.0 g of sodium acetate (NaAc) and 2.0 g of polyethylene glycol (PEG) were added and stirred for 30 min. The mixture was sealed in an autoclave, reacted at 200 °C...

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Abstract

The invention discloses a preparation method of a magnetic fullerene molecularly-imprinted nano-composite material. The preparation method comprises the specific operation steps that firstly, polycarboxylation-substituted fullerene (C60-COOH) is synthesized; secondly, magnetic fullerene nano-particles are prepared through a hydrothermal synthesis method, and the surfaces of the magnetic fullerene nano-particles are covered with a layer of silicon dioxide to prepare silicon dioxide-coated magnetic fullerene nano-particles; lastly, the magnetic fullerene molecularly-imprinted nano-composite material is prepared through a molecular imprinting technique. According to the magnetic fullerene molecularly-imprinted nano-composite material, fullerene is taken as a carrier, and therefore the specific surface area of an imprinted polymer is greatly increased; magnetic Fe3O4 is used, and therefore the operation steps of column packing, centrifuging, filtering and the like in the purification process are simplified; specific identification on sulfonylurea herbicides is achieved through the molecular imprinting technique, and therefore the sulfonylurea herbicides are efficiently and selectively separated and purified.

Description

technical field [0001] The invention relates to a preparation method of a magnetic fullerene molecularly imprinted nanocomposite material. Background technique [0002] Sulfonylurea herbicides are currently one of the most widely used herbicides in the world, and have the advantages of high efficiency and low toxicity. However, because it remains in the soil for a long time, a small amount of residue can cause damage to sensitive crops. Therefore, it is necessary to monitor the residues of sulfonylurea herbicides in food, and pretreatment materials and technologies with high selective enrichment ability have become a research hotspot. [0003] Commonly used pretreatment methods for such herbicides include supercritical fluid extraction, immunoaffinity chromatography, and solid-phase extraction. These methods generally have disadvantages such as poor selectivity and serious matrix interference, which seriously affect the sensitivity and accuracy of the method. . Molecularl...

Claims

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Application Information

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IPC IPC(8): B01J20/26B01J20/28B01J20/30
CPCB01J20/06B01J20/103B01J20/20B01J20/26B01J20/28009
Inventor 周典兵宋伟韩芳吕亚宁丁磊胡艳云郑平盛旋
Owner 安徽出入境检验检疫局检验检疫技术中心
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