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Preparation method of halloysite surface initiated boron affinity imprinted polymer adsorbent

An imprinted polymer, surface-initiated technology, applied in chemical instruments and methods, other chemical processes, etc., can solve the problems of inability to quickly identify and separate luteolin, poor regeneration performance, etc., and achieve good chemical stability and rapid adsorption of materials. Effects of kinetics, good specific adsorption capacity

Inactive Publication Date: 2016-12-21
JIANGSU UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0004] At present, materials for adsorbing luteolin are rarely studied. Recently, graphene molecularly imprinted materials with dual recognition functions are used to adsorb luteolin (Shucheng Liu, Jianming Pan, Hengjia Zhu, GuoqingPan, Fengxian Qiu, Minjia Meng, Juntong Yao, Dong Yuan, Graphene oxide based molecularly imprinted polymers with double recognition abilities: The combination of covalent boronic acid and traditional non-covalent monomers, Chemical Engineering Journal 290 (2016) 220–231.), but they cannot quickly identify and isolate and has poor regenerative properties

Method used

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  • Preparation method of halloysite surface initiated boron affinity imprinted polymer adsorbent
  • Preparation method of halloysite surface initiated boron affinity imprinted polymer adsorbent
  • Preparation method of halloysite surface initiated boron affinity imprinted polymer adsorbent

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0049] (1) Preparation of vinyl fluorophenylboronic acid (F-BA):

[0050] In an ice-water bath, add 2 g of fluorophenylboronic acid (4-(aminoethylcarbamoyl)-3-fluorophenylboronic acid) to 100 mL of sodium carbonate solution, then add 3 mL of acryloyl chloride to the above solution, and then add 0.1 mol / L of sodium hydroxide The pH of the solution was adjusted to neutrality for 12 hours, and finally vacuum-dried at 60°C.

[0051] (2) Activation of halloysite nanotubes (HNTs):

[0052] Grinding and pulverizing 0.1g block halloysite nanotubes through 100 sieves, calcining at 100°C for 24h,

[0053] The calcined 0.1g of HNTs was placed in 50mL of a mixed solution of sulfuric acid and hydrochloric acid (v:v, 1:3), and stirred at 80°C for 6h; Dry at ℃.

[0054] (3) Preparation of dopamine loaded on halloysite nanotubes (HNTs@PDA):

[0055] 100mg of activated halloysite nanotubes were put into 40mL of ethanol and water solution (v:v, 1:1), and then 50mg of dopamine hydrochloride ...

Embodiment 2

[0072] (1) Preparation of vinyl fluorophenylboronic acid (F-BA):

[0073] In an ice-water bath, add 3 g of fluorophenylboronic acid (4-(aminoethylcarbamoyl)-3-fluorophenylboronic acid) to 150 mL of sodium carbonate solution, then add 4 mL of acryloyl chloride to the above solution, and then use 0.1 mol / L of sodium hydroxide solution Adjust the pH to neutral and react for 12 hours, and finally dry it under vacuum at 60°C.

[0074] (2) Activation of halloysite nanotubes (HNTs):

[0075] 0.2g block halloysite nanotubes were ground and crushed through 100 sieves, and calcined at a high temperature of 100°C for 24h. The calcined 0.2g HNTs were placed in a mixed solution of 60mL sulfuric acid and hydrochloric acid, (v:v, 1 :3) Stir at 80°C for 6h. Then rinse with a large amount of distilled water until neutral, and finally dry it under vacuum at 60°C.

[0076] (3) Preparation of dopamine loaded on halloysite nanotubes (HNTs@PDA):

[0077] Put 150mg of activated halloysite nanotube...

Embodiment 3

[0089] (1) Preparation of vinyl fluorophenylboronic acid (F-BA):

[0090] In an ice-water bath, add 4 g of fluorophenylboronic acid (4-(aminoethylcarbamoyl)-3-fluorophenylboronic acid) to 200 mL of sodium carbonate solution, then add 5 mL of acryloyl chloride to the above solution, and then add 0.1 mol / L of sodium hydroxide The pH of the solution was adjusted to neutrality for 12 hours, and finally vacuum-dried at 60°C.

[0091] (2) Activation of halloysite nanotubes (HNTs):

[0092] Grind and crush 0.3g massive halloysite nanotubes through a 100 sieve, and calcined at 100°C for 24h. The calcined 0.3g of HNTs was placed in 70mL of a mixed solution of sulfuric acid and hydrochloric acid (v:v, 1:3 ), stirred at 80°C for 6h. Then rinse with a large amount of distilled water until neutral, and finally dry it under vacuum at 60°C.

[0093] (3) Preparation of dopamine loaded on halloysite nanotubes (HNTs@PDA):

[0094] 200mg of activated halloysite nanotubes were put into 60mL o...

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Abstract

The invention relates to a preparation method of a halloysite surface initiated boron affinity imprinted polymer adsorbent, and belongs to the technical field of preparation of environmental functional materials. The method comprises the following steps: purifying halloysite (HNTs), and wrapping the surface of halloysite with a layer of dopamine to form HNTs@PDA; connecting a bromine initiator to the surface of the HNTs@PDA to obtain HNTs@PDA@Br; connecting vinyl imidazole to the HNTs@PDA@Br through an atom free radical polymerization technology to obtain HNTs@PDA@Br@VLD; and adsorbing zinc ions, adsorbing luteolin, introducing fluorophenylboronic acid, and carrying out ATRP polymerization in order to obtain the imprinted polymer. Imprinted polymer microspheres prepared through the method have the advantages of good chemical stability, high adsorption capacity, good acid-alkali effect, realization of reversible adsorption / release functional luteolin with the acid-base value, and specific and high selective identification performance.

Description

technical field [0001] The invention relates to a preparation method of a boron affinity imprinted polymer adsorbent induced on the surface of halloysite, which belongs to the technical field of preparation of environmental functional materials. Background technique [0002] Molecular imprinting technology was proposed by Wulff of Germany in 1972. Molecularly imprinted polymers are three-dimensional cross-linked polymers with predetermined recognition function binding sites, and the prepared molecularly imprinted polymers (MIPs) can produce specific adsorption on template molecules. Molecular imprinting technology has the characteristics of predetermined structure and activity, specific recognition and wide practicability. ATRP (atom radical polymerization), as a form of molecular imprinting technology, uses simple organic halides as initiators and transition metal complexes as halogen atom carriers to achieve control of the reaction through redox reactions. Halloysite nano...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08F292/00C08F226/06C08F230/06C08J9/26B01J20/26B01J20/30
CPCB01J20/268C08F292/00C08J9/26C08F226/06C08F230/06
Inventor 刘树成潘建明刘金鑫黄伟张文莉
Owner JIANGSU UNIV
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