Wulff type phenylboronic acid (AABOB) functionalized magnetic nanometer microspheres and preparation method and applications thereof

A magnetic nano-type phenylboronic acid technology, applied in biochemical equipment and methods, chemical instruments and methods, nanotechnology and other directions, can solve the problems of poor reuse ability and low solid load, and achieve the effect of rapid separation

Inactive Publication Date: 2018-09-25
JIANGSU UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] The purpose of the present invention is to overcome some disadvantages of the current immobilized horseradish peroxidase, such as low immobilization cap

Method used

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  • Wulff type phenylboronic acid (AABOB) functionalized magnetic nanometer microspheres and preparation method and applications thereof
  • Wulff type phenylboronic acid (AABOB) functionalized magnetic nanometer microspheres and preparation method and applications thereof
  • Wulff type phenylboronic acid (AABOB) functionalized magnetic nanometer microspheres and preparation method and applications thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0072] Embodiment 1: Preparation of Fe3O4@p(AABOB-co-AIM) microspheres

[0073] (1) Synthesis of NBOB:

[0074] Add 5 mL of fuming nitric acid dropwise to 1 g of 2-(hydroxymethyl)phenylboronic acid cyclic monoester (BOB) at -40 °C while stirring, and continue stirring for 20 min after the addition is complete. After completion of the reaction as determined by TLC spot plate, the mixture was transferred to ice water and stirred vigorously for 1.5 h. After the reaction, the product was separated by suction filtration, washed several times with deionized water, and then vacuum-dried at 40° C. overnight.

[0075] (2) Synthesis of ABOB:

[0076] Dissolve 3 g of NBOB and 2 g (50%) Raney nickel in 90 mL of methanol, then add 5 mL of hydrazine hydrate to the mixture under nitrogen protection while stirring, and control the temperature of the system throughout the reaction process is 0°C. After the completion of the reaction was determined by TLC, the mixture was suction-filtered t...

Embodiment 2

[0085] Embodiment 2: Preparation of Fe3O4@p(AABOB-co-AIM) microspheres

[0086] (1) Synthesis of NBOB:

[0087] 15 mL of fuming nitric acid was added dropwise to 2.2 g of 2-(hydroxymethyl)phenylboronic acid cyclic monoester (BOB) at -40 °C while stirring, and the stirring reaction was continued for 20 min after the addition was completed. After completion of the reaction as determined by TLC spot plate, the mixture was transferred to ice water and stirred vigorously for 2.5 h. After the reaction, the product was separated by suction filtration, washed several times with deionized water, and then vacuum-dried at 40° C. overnight.

[0088] (2) Synthesis of ABOB:

[0089] Dissolve 3.8 g of NBOB and 4 g (50%) Raney nickel in 90 mL of methanol, then add 8.2 mL of hydrazine hydrate to the mixture under nitrogen protection, and control the temperature of the system during the entire reaction process is 0°C. After the completion of the reaction was determined by TLC, the mixture w...

Embodiment 3

[0098] Embodiment 3: Preparation of Fe3O4@p(AABOB-co-AIM) microspheres

[0099] (1) Synthesis of NBOB:

[0100] 10 mL of fuming nitric acid was added dropwise to 1.6 g of 2-(hydroxymethyl)phenylboronic acid cyclic monoester (BOB) at -40 °C while stirring, and the reaction was stirred for 20 min after the addition was completed. After completion of the reaction as determined by TLC spot plate, the mixture was transferred to ice water and stirred vigorously for 2 h. After the reaction, the product was separated by suction filtration, washed several times with deionized water, and then vacuum-dried at 40° C. overnight.

[0101] (2) Synthesis of ABOB:

[0102] Dissolve 3.4 g of NBOB and 3 g (50%) Raney nickel in 90 mL of methanol, then add 6.6 mL of hydrazine hydrate to the mixture under nitrogen protection while stirring, and control the temperature of the system throughout the reaction process is 0°C. After the completion of the reaction was determined by TLC, the mixture wa...

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Abstract

The invention belongs to the technical field of inorganic materials and analysis, and relates to Wulff-type phenylboronic acid (AABOB) functionalized magnetic nanometer microspheres and a preparationmethod and applications thereof. Firstly, Fe3O4@MPS microspheres and acetonitrile are mixed and ultrasonically dispersed; then AABOB, N-allyl imidazole, a crosslinking agent MBAA and an initiator thatis azobisisobutyronitrile are added; the mixture is heated to initiate polymerization; a product obtained is washed repeatedly and dried in vacuum; then the product is subjected to synergistic actionof nickel ions and is used for horseradish peroxidase immobilization; and the obtained immobilized enzyme is used for degradation of phenolic pollutants. The immobilized enzyme synthesized from the magnetic nanometer microspheres has good recyclability, the relative enzyme activity can still be 83% after five times of reutilization, which is far higher than that reported in present literatures, and the immobilized enzyme has pH stability, temperature stability and storage stability which are significantly improved that those of materials not immobilized.

Description

technical field [0001] The invention belongs to the technical field of inorganic materials and analysis, and relates to a Wulff-type phenylboronic acid AABOB functionalized magnetic nano-microsphere and a preparation method and application thereof. Background technique [0002] Phenolic wastewater is one of the most serious industrial wastewater pollution problems in the world. Phenol-containing wastewater mainly comes from the iron and steel industry, paper industry and plastic processing industry. If this wastewater is discharged directly into rivers and the environment without treatment, it will cause very serious pollution and bring harm to human body, water body, fish body and crops. to serious harm. At present, the methods for treating phenolic wastewater mainly include three categories: physical method, chemical method and biochemical method. Physical treatment requires very high treatment conditions, and the treatment process is expensive; chemical treatment may ca...

Claims

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Application Information

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IPC IPC(8): C02F3/34C12N11/14C12N11/02C12N9/08B82Y40/00B82Y30/00C02F101/34
CPCC02F3/342B82Y30/00B82Y40/00C02F2101/345C12N9/0065C12N11/02C12N11/14C12Y111/01007
Inventor 蔡云凤韩娟罗鹏李颖范美美姬治宇谭朝林王赟顾磊李春梅倪良张文莉
Owner JIANGSU UNIV
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