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Method for preparing protein adsorption-resistant ceramic composite film

A ceramic composite membrane, anti-protein adsorption technology, applied in chemical instruments and methods, membrane technology, semi-permeable membrane separation and other directions, to achieve excellent anti-protein adsorption effect, simplify membrane cleaning process, prolong the effect of membrane cleaning cycle

Active Publication Date: 2013-02-06
NANJING TECH UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, in the actual application system, the ceramic membrane used for the separation and purification of the protein system is a porous microfiltration ultrafiltration membrane. When the ceramic membrane is grafted and modified from the surface, the molecular size of the reactants in the reaction solution It is very small and can penetrate the membrane into the pores of the membrane and react on the surface of the membrane and in the pores, resulting in changes in the pore structure and pore size of the membrane

Method used

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  • Method for preparing protein adsorption-resistant ceramic composite film
  • Method for preparing protein adsorption-resistant ceramic composite film
  • Method for preparing protein adsorption-resistant ceramic composite film

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0032] Example 1: Preparation of anti-protein adsorption ceramic membrane by grafting onto the surface, the mechanism diagram is shown in Image 6

[0033] (1) Cool the mixed solution of 3.5ml of 3-aminopropyltriethoxysilane, 3.35ml of triethylamine and 30ml of dichloromethane to 0°C in an ice bath under the protection of nitrogen, and then slowly add 3ml of 2-bromopropionyl bromide to it solution and 15ml of dichloromethane mixed solution, reacted for 6h, and dried under vacuum at 45°C.

[0034] (2) 9.5gOEGMA, 0.143gCuBr, 0.0223gCuBr 2 , 0.344g2,2-bipyridine and 15ml of isopropanol were heated to 40°C under nitrogen protection, and then 0.37g (1) of the prepared silanized initiator 2-bromo-2-methyl-N was added thereto -React a mixed solution of (3-triethoxysilyl-propyl)propanamide and 25ml of isopropanol for 6h to obtain a solution containing silylated POEGMA molecular brushes.

[0035](3) Mix and stir 50ml of absolute ethanol and 5ml of deionized water for 30min, add glac...

Embodiment 2

[0044] (1) Mix and stir 1.75ml of 3-aminopropyltriethoxysilane, 3.35ml of triethylamine and 15ml of tetrahydrofuran under the protection of nitrogen and lower to 5°C, then slowly add 3ml of 2-bromopropionyl bromide solution and 15ml of After the tetrahydrofuran mixed solution was reacted at 5° C. for 4 h, it was vacuum-dried at 50° C.

[0045] (2) 19gOEGMA, 0.286gCuBr, 0.614g2, 2-bipyridine and 40ml methanol were mixed and stirred under nitrogen protection and heated to 60°C, and then 0.37g (1) of the silanized initiator 2- A mixed solution of bromo-2-methyl-N-(3-triethoxysilyl-propyl)propanamide and 30ml of methanol was reacted for 4h to obtain a solution containing silylated POEGMA molecular brushes.

[0046] (3) 100ml of absolute ethanol and 5ml of deionized water were mixed and stirred for 30min, then hydrochloric acid was added to adjust the pH value to 1, and then the mixed solution was added to the POEGMA molecular brush solution prepared above, and the mixed solution w...

Embodiment 3

[0049] (1) Mix and stir 3ml of 4-aminobutyltriethoxysilane, 4.5ml of triethylamine and 50ml of dichloromethane under the protection of argon to -5°C, then slowly add 3.3ml of 2-chloropropionyl chloride dropwise to it After mixing the solution with 35ml of dichloromethane, reacted for 10h, and dried in vacuum at 30°C.

[0050] (2) 28.5gOEGMA, 0.099gCuCl, 0.027gCuCl 2 , 0.413g of 2,2-bipyridine and 15ml of ethanol were mixed and stirred, heated in a water bath to 80°C, and then 0.51g of the silanized initiator 2-chloro-2-methyl-N- A mixed solution of (3-triethoxysilyl-butyl) propionamide and 15ml of ethanol was reacted for 10h.

[0051] (3) Mix and stir 50ml of absolute ethanol and 2ml of deionized water for 30min, add glacial acetic acid to adjust the pH value to 4, then add the mixed solution to the polymer molecular brush solution prepared above, and use a pump to drive the mixed solution to make it 200nmAl in 10cm length 2 o 3 The surface of the 19-channel ceramic membra...

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Abstract

The invention relates to a method for preparing a protein adsorption-resistanting ceramic composite film. In the method, methylacrylic acid oligomerization gylcol ester (OEGMA) is adopted as a functional monomer, and initiates polymerization through a silylanized initiator to prepare a silanizated poly(oligo(ethylene glycol) methacrylate) (POEGMA) molecular brush; alkylalkoxylsilane is formed on one end of the molecular brush, and can react with hydroxyl on the surface of a ceramic film; and the POEGMA molecular brush is grafted on the film surface to prepare the protein adsorption resistance ceramic composite film. The method realizes that the polymer molecular brush is only grafted on the surface of the ceramic film by adopting a method of grafting to surface, only changes the surface property of the film, and does not influence the property of the film pores. By the method, the protein adsorption resistance polymer molecular brush can be grafted on the surface of the porous ceramic film of 4 to 500nm.

Description

technical field [0001] The invention relates to a preparation method of an anti-protein adsorption ceramic composite film, in particular to a method for preparing an anti-protein adsorption ceramic film by grafting and modifying a silanized POEGMA (polyethylene glycol methacrylate) molecular brush, This method is especially suitable for surface grafting modification of porous ceramic membranes. Background technique [0002] In the process of protein separation and purification, membrane separation technology, as a new type of separation technology, has attracted increasing attention due to its advantages of low energy consumption, simple equipment, normal temperature operation, high selectivity, no phase change and no chemical change. However, in the process of separating proteins with ceramic membranes, protein molecules are easily adsorbed on the surface of the membrane and in the pores to form membrane fouling, which reduces the separation performance and flux, and the us...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01D71/02B01D71/78B01D69/12B01D67/00
Inventor 景文珩何华婷邢卫红徐南平
Owner NANJING TECH UNIV
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