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Preparing method of calixarene modified magnetic material

A technology of calixarene and magnetic zeolite is applied in the field of preparation of magnetic materials, which can solve the problems of complicated operation steps, long time consumption, easy oxidation of ferromagnetic particles, etc., and achieves the advantages of improving enrichment efficiency, stable material performance and excellent application potential. Effect

Inactive Publication Date: 2015-09-02
JILIN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] The invention provides a method for preparing a carboxylated calixarene-modified magnetic zeolite material, which solves the technical problems that ferromagnetic particles are easily oxidized, or the operation steps are cumbersome and time-consuming in the preparation process of existing magnetic materials.

Method used

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  • Preparing method of calixarene modified magnetic material
  • Preparing method of calixarene modified magnetic material

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Experimental program
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Effect test

Embodiment 1

[0015] (1) Take 5.0g of mesoporous silica gel and 4.0g of ferric nitrate as reaction monomers, mix and stir them evenly in ethanol solution, and dry at 35°C to powder; add 2mL of ethylene glycol as a reducing agent, and the powder Place in a tube furnace, under the protection of nitrogen, react at 230°C for 5 hours, the in situ reduction method will produce ferric oxide silicon dioxide dark brown powder; with 0.05g sodium hydroxide as alkali source, 3.5g tetrapropyl hydrogen Ammonium oxide was used as a structure-directing agent, 0.05g of sodium metaaluminate was used as a reaction monomer, and 16mL of deionized water was used as a reaction medium. 4.0g of dark brown powder was injected into the reaction kettle and reacted at 160°C for 20 After cooling, magnetic zeolite was obtained;

[0016] (2) With 7.0mL ethanol as the reaction medium, 6.0mL deionized water as the hydrolysis initiator, and 1.0mL 3-aminopropyltriethoxysilane as the silylating agent, the magnetic zeolite is c...

Embodiment 2

[0019] (1) Take 5.0g of mesoporous silica gel and 5.0g of ferric nitrate as reaction monomers, mix and stir them evenly in an ethanol solution, and dry them at 50°C until they are powdery; after adding 5mL of ethylene glycol as a reducing agent, the powder Put it in a tube furnace, under the protection of nitrogen, react at 280°C for 7 hours, the in situ reduction method will generate ferric oxide silicon dioxide dark brown powder; with 0.2g sodium hydroxide as alkali source, 5.0g tetrapropyl hydrogen Ammonium oxide was used as a structure-directing agent, 0.2g of sodium metaaluminate was used as a reaction monomer, and 20mL of deionized water was used as a reaction medium. 4.0g of dark brown powder was injected into the reaction kettle and reacted at 200°C for 30 After cooling, magnetic zeolite was obtained;

[0020] (2) With 10.0mL ethanol as the reaction medium, 7.0mL deionized water as the hydrolysis initiator, and 3.0mL 3-aminopropyltriethoxysilane as the silylating agent...

Embodiment 3

[0023] (1) Take 5.0g of mesoporous silica gel and 4.0g of ferric nitrate as reaction monomers, mix and stir them evenly in an ethanol solution, and dry them at 40°C until they are powdery; after adding 4mL of ethylene glycol as a reducing agent, the powder Placed in a tube furnace, under the protection of nitrogen, reacted at 250°C for 6 hours, and the in-situ reduction method produced iron ferric oxide and silicon dioxide dark brown powder; with 0.1g sodium hydroxide as the alkali source, 4.1g tetrapropyl hydrogen Ammonium oxide was used as a structure-directing agent, 0.1g of sodium metaaluminate was used as a reaction monomer, and 19mL of deionized water was used as a reaction medium. 4.0g of dark brown powder was injected into the reaction kettle and reacted at 180°C for 24 After cooling, magnetic zeolite was obtained;

[0024] (2) With 9.5mL ethanol as the reaction medium, 6.4mL deionized water as the hydrolysis initiator, and 1.5mL 3-aminopropyltriethoxysilane as the si...

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Abstract

The invention discloses a preparing method of calixarene modified magnetic material. The preparing method includes: mixing well mesoporous silica and ferric nitrate in ethyl alcohol before drying; allowing mixture and reducing agent to reaction by means of in-situ reduction using ethylene glycol as the reducing agent; adding a reaction product, sodium hydroxide, tetrapropylammonium hydroxide, sodium metaaluminate and water into a reactor, and allowing hydrothermal reaction to generate magnetic zeolite; using 3-triethoxysilylpropylamine as silylating reagent to allow surface silylation for the magnetic zeolite; and using 1-(3-dimethyl aminopropyl)-3-ethylcarbodiimide hydrochloride and n-hydroxysuccinimide as activating reagents to allow coupled reaction of carboxylic calixarene and the magnetic zeolite so as to obtain carboxylic calixarene modified magnetic material. The calixarene modified magnetic material as magnetic hybrid material has the advantages in organic macrocycle molecules and inorganic magnetic materials, the preparing method is reliable, the calixarene modified magnetic material is good in stability, the introduction of the macrocycle molecules is good for separating identification, the calixarene modified magnetic material is very suitable for analyzing phenolic antioxidants in milk and juice samples and has great application potential in the field of organics separation and magnetic solid-phase extraction.

Description

technical field [0001] The invention provides a method for preparing a calixarene-modified magnetic material, which is an improvement on the existing magnetic solid-phase extraction method, is a new method for preparing a magnetic material, and belongs to the technical field of magnetic material synthesis. Background technique [0002] Magnetic solid-phase extraction (MSPE) is based on the characteristic adsorption capacity of solid-phase adsorption materials and the recyclability of magnetic particles, and realizes and optimizes the enrichment and extraction of analytes by changing test parameters such as solution pH and ionic strength separate technology. Since the magnetic adsorption material enriches the analyte during the separation process, it can quickly realize the separation from the mother liquor under the action of an external magnetic field, reducing the use of volatile organic solvents, so it has high enrichment efficiency, large enrichment factor, and recycling...

Claims

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Application Information

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IPC IPC(8): B01J20/22B01J20/30B01J20/28H01F1/11
Inventor 贾琼周绍岩宋乃忠马玖彤吕学举郑海娇王荟琪江丹丹武明雪周玉凤
Owner JILIN UNIV
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