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Preparation method of magnetic attapulgite molecularly imprinted material

A technology of attapulgite and molecular imprinting, applied in chemical instruments and methods, alkali metal oxides/hydroxides, inorganic chemistry, etc., can solve the problems of time-consuming and complicated operation, difficulty in realizing rapid separation and continuous production, etc. The effect of high reuse times, improved stability and reusability, and reduced false positive problems

Inactive Publication Date: 2017-12-12
DONGGUAN LIANZHOU INTPROP OPERATION MANAGEMENT CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0003] Traditional molecularly imprinted materials are often used as adsorbents for solid-phase extraction in practical applications to enrich, purify, and separate actual samples. The operation is relatively time-consuming and complicated, and column packing and column passage usually require supporting equipment. The use of reagents also requires suction filtration or centrifugation, so it is difficult to achieve rapid separation and continuous production. Therefore, magnetic molecular imprinting technology using magnetic nanoparticles as carriers is becoming more and more popular.

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  • Preparation method of magnetic attapulgite molecularly imprinted material

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Embodiment 1

[0026] (1) 2.7g ferric chloride and 7.2g sodium acetate are dissolved in 100mL ethylene glycol, form uniform yellow solution, according to the mol ratio of ferric chloride, carboxylated carbon nanotubes and attapulgite is 2: 0.5:4, add carboxylated carbon nanotubes and attapulgite, ultrasonically disperse under the protection of nitrogen, transfer to a polytetrafluoroethylene-lined autoclave, react at 200 ° C for 8 h, cool naturally to room temperature, wash with ethanol Wash with deionized water and dry in vacuum at 60°C to obtain magnetic particles.

[0027] (2) Disperse 0.1 g of magnetic particles in 90 mL of ethanol aqueous solution, mix ultrasonically, add 10 mL of ammonia water and 5 mL of tetraethyl orthosilicate dropwise in sequence, stir at room temperature for 24 h, wash and separate, and disperse in purified toluene after vacuum drying. Under nitrogen protection, 4 mL of alkenyl silane modifier and 6 mL of triethylamine were added, refluxed for 24 hours, washed and ...

Embodiment 2

[0030] (1) The ferric chloride of 2.7g and 7.2g sodium acetate are dissolved in 100mL ethylene glycol, form uniform yellow solution, be 5 according to the mol ratio of ferric chloride, carboxylated carbon nanotube and attapulgite: 1:8, add carboxylated carbon nanotubes and attapulgite, ultrasonically disperse under nitrogen protection, transfer to a polytetrafluoroethylene-lined autoclave, react at 200°C for 8 hours, cool naturally to room temperature, and wash with ethanol Wash with deionized water and dry in vacuum at 60°C to obtain magnetic particles.

[0031] (2) Disperse 0.1 g of magnetic particles in 90 mL of ethanol aqueous solution, mix ultrasonically, add 10 mL of ammonia water and 5 mL of tetraethyl orthosilicate dropwise in sequence, stir at room temperature for 24 h, wash and separate, and disperse in purified toluene after vacuum drying. Under nitrogen protection, 4 mL of alkenyl silane modifier and 6 mL of triethylamine were added, refluxed for 24 hours, washed a...

Embodiment 3

[0034] (1) The ferric chloride of 2.7g and 7.2g sodium acetate are dissolved in 100mL ethylene glycol, form uniform yellow solution, be 3 according to the mol ratio of ferric chloride, carboxylated carbon nanotube and attapulgite: 0.6:6, add carboxylated carbon nanotubes and attapulgite, ultrasonically disperse under nitrogen protection, transfer to a polytetrafluoroethylene-lined autoclave, react at 200°C for 8 hours, cool naturally to room temperature, and wash with ethanol Wash with deionized water and dry in vacuum at 60°C to obtain magnetic particles.

[0035] (2) Disperse 0.1 g of magnetic particles in 90 mL of ethanol aqueous solution, mix ultrasonically, add 8 mL of ammonia water and 2 mL of tetraethyl orthosilicate dropwise in sequence, stir at room temperature for 24 h, wash and separate, and disperse in purified toluene after vacuum drying. Under nitrogen protection, 5 mL of alkenyl silane modifier and 6 mL of triethylamine were added, refluxed for 24 hours, washed ...

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Abstract

The invention provides a method for preparing a magnetic attapulgite molecularly imprinted material, which comprises the following steps: dissolving ferric chloride and sodium acetate in ethylene glycol, adding carboxylated carbon nanotubes and attapulgite, ultrasonically dispersing, and using high pressure React in the reactor to obtain magnetic particles; disperse the magnetic particles in ethanol aqueous solution, add ammonia water and tetraethyl orthosilicate dropwise in turn, stir at room temperature, wash, separate and dry, then disperse in purified toluene, under nitrogen protection, add alkenyl silane modifier and triethylamine, reflux reaction, washing and drying to obtain silane-modified magnetic silica particles; 4,4-methylene-two-(2-chloroaniline) and vinylpyridine were added to toluene, mixed and pre- Assemble, add silane-modified magnetic silica gel particles and ethylene glycol dimethacrylate, then add azobisisobutyronitrile, heat the reaction, separate under the action of an external magnetic field, wash repeatedly, and dry in vacuum to obtain a magnetic attapulgite Soil Molecularly Imprinted Materials.

Description

technical field [0001] The invention belongs to the technical field of magnetic molecular imprinting materials, and in particular relates to a preparation method of magnetic attapulgite molecular imprinting materials. Background technique [0002] Molecular imprinting technology, also known as molecular template technology, refers to the use of template molecules, imprinted molecules or imprinted molecules as templates to copolymerize with functional monomers and cross-linking agents under certain conditions to obtain molecularly imprinted polymers. When using physical or chemical methods After the template molecule is removed, the imprinted hole that is complementary to the template molecule in shape, size and chemical group, that is, the recognition site, remains in the highly cross-linked polymer network, which can selectively re-recognize the template molecule and its analog molecular imprinted polymerization Therefore, molecularly imprinted polymers have three character...

Claims

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Application Information

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IPC IPC(8): B01J20/26B01J20/28B01J20/30
CPCB01J20/268B01J20/28009
Inventor 陈东进
Owner DONGGUAN LIANZHOU INTPROP OPERATION MANAGEMENT CO LTD
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