Hydrophilic modification method for PS-DVB (polystyrene-divinyl benzene) crosslinked microspheres grafted and bonded with PVA (polyvinyl alcohol)

A technology of divinylbenzene and polystyrene, applied in the field of hydrophilic modification of PVA graft-bonded polystyrene-divinylbenzene cross-linked microspheres, which can solve phase collapse, unfavorable biological protein separation, and reaction conditions Harsh and other issues

Inactive Publication Date: 2017-03-08
扬州倍赛德生物科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Common polymers that can be used for bonding include PVA, PEG, and β-cyclodextrin, etc., mainly through the benzyl chloride or acetyl chloride (bromine) on the surface of functionalized PS-DVB microspheres and PVA (ZL200710177704.6, 2009 ), PEG (Journal of biomedicalmaterials research, 1992, 26, 779-790) and β-cyclodextrin (Journal of Functional Polymers, 1997, 10, 25-212) react under alkaline conditions, but benzyl chloride or ethyl Acyl chloride (bromine) has only 1-2 C atoms away from the benzene ring on the surface of PS-DVB microspheres. It reacts with large molecular weight polymers, and its benzyl chloride or acetyl chloride (bromine) has low degrees of freedom, and the reaction needs to It can only react under alkaline conditions, the reaction conditions are harsh, and the activity is low; in addition, Ma Guang

Method used

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  • Hydrophilic modification method for PS-DVB (polystyrene-divinyl benzene) crosslinked microspheres grafted and bonded with PVA (polyvinyl alcohol)
  • Hydrophilic modification method for PS-DVB (polystyrene-divinyl benzene) crosslinked microspheres grafted and bonded with PVA (polyvinyl alcohol)

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0028] Step (a) introduction of epoxy groups on the surface of PS-DVB microspheres

[0029] Weigh 0.5g of N-bromosuccinimide in a 50mL beaker, measure 20mL of acetone and 4mL of deionized water in the above beaker with a graduated cylinder, and stir until the N-bromosuccinimide Dissolve completely; add this solution into a 50mL round-bottomed flask with 1.0g of dry PS-DVB microspheres (cross-linking degree 1%, non-porous), stir evenly, add 0.2g of ammonium acetate, and react at room temperature 3h, after the reaction was completed, sand core was filtered, washed with 10 times the amount of ethanol and deionized water respectively, and drained; the microspheres were transferred to a 50mL round bottom flask, and 15mL of deionized water and 3mL of NaOH ( 3mol / L) solution, reacted at 40°C for 6h; after the reaction, filtered through a sand core, washed with 10 times the amount of deionized water, and drained for later use.

[0030] Step (b) bonding and post-crosslinking of PVA on...

Embodiment 2

[0034] Step (a) introduction of epoxy groups on the surface of PS-DVB microspheres

[0035] Weigh 1g of N-chlorosuccinimide in a 50mL beaker, measure 15mL of acetone and 4mL of deionized water in the above beaker with a graduated cylinder, and stir until the N-chlorosuccinimide is completely Dissolve; add this solution into a 50mL round-bottomed flask with 1.0g of dry PS-DVB microspheres (30% cross-linking degree, with holes), stir evenly, add 0.3g of sodium acetate, and react at room temperature for 3h , after the reaction, sand core filter, wash with 10 times the amount of ethanol and deionized water respectively, and drain; transfer the microspheres to a 50mL round bottom flask, add 15mL of deionized water and 3mL of NaOH (3mol / L) solution, react at 40° C. for 6 h; after the reaction, filter through a sand core, wash with 10 times the amount of deionized water, and drain for later use.

[0036] Step (b) bonding and post-crosslinking of PVA on the surface of PS-DVB microsp...

Embodiment 3

[0040] Step (a) introduction of epoxy groups on the surface of PS-DVB microspheres

[0041] Weigh 1g of N-bromosuccinimide in a 50mL beaker, measure 15mL of acetone and 4mL of deionized water in the above beaker with a graduated cylinder, and stir until the N-bromosuccinimide is completely Dissolve; add this solution into a 50mL round-bottomed flask with 1.0g of dry PS-DVB microspheres (30% cross-linking degree, with holes), stir evenly, add 0.3g of sodium acetate, and react at room temperature for 3h , after the reaction, sand core filter, wash with 10 times the amount of ethanol and deionized water respectively, and drain; transfer the microspheres to a 50mL round bottom flask, add 15mL of deionized water and 3mL of NaOH (3mol / L) solution, react at 40° C. for 6 h; after the reaction, filter through a sand core, wash with 10 times the amount of deionized water, and drain for later use.

[0042] Step (b) bonding and post-crosslinking of PVA on the surface of PS-DVB microsphe...

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Abstract

The invention relates to a hydrophilic modification method for PS-DVB (polystyrene-divinyl benzene) crosslinked microspheres grafted and bonded with PVA (polyvinyl alcohol). The method comprises steps as follows: epoxy groups with high reaction activity are introduced into surfaces of PS-DVB crosslinked microspheres and subjected to a reaction with hydroxyl in PVA, bonded PVA is subjected to a post-crosslinking reaction with a cross-linking agent, compact hydrophilic PS-DVB crosslinked microspheres wrapped with PVA are obtained, and hydrophobicity caused by benzene ring residues and pendent double bonds on the surfaces of the PS-DVB crosslinked microspheres is eliminated; furthermore, PVA is subjected to the post-crosslinking reaction, so that the phase collapse phenomenon of PVA long chains on the surfaces of the PS-DVB crosslinked microspheres in the field of bioseparation under the high-salt condition is avoided, further derivatization of a large amount of hydroxyl in PVA can be facilitated, chromatography separation media meeting different requirements can be prepared, and the method belongs to the field of modification of functional polymer microspheres.

Description

technical field [0001] The invention relates to a method for hydrophilic modification of PVA graft-bonded polystyrene-divinylbenzene crosslinked microspheres (PS-DVB microspheres), which is introduced on the surface of PS-DVB microspheres with high reactivity The epoxy group of the epoxy group reacts with the hydroxyl group in PVA, and the bonded PVA passes through the post-crosslinking reaction of the crosslinking agent to obtain PVA-coated compact hydrophilic PS-DVB microspheres, which eliminates the PS-DVB microsphere surface factor. The hydrophobicity caused by the residual benzene ring and the hanging double bond; and the post-crosslinking reaction of PVA can avoid the phase collapse phenomenon of the long chain of PVA on the surface of the hydrophilic PS-DVB microsphere under the high salt condition in the field of biological separation, and A large number of hydroxyl groups in PVA can facilitate further derivatization, and can be prepared into chromatographic separation...

Claims

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Application Information

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IPC IPC(8): C08J7/12C08J3/24C08G81/02C08L25/08
CPCC08J7/12C08G81/021C08J3/24C08J2325/08
Inventor 仲玉
Owner 扬州倍赛德生物科技有限公司
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