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Hydrophilic modification method and modified material of polyglycidyl methacrylate or its copolymer

A technology of polymethacrylic acid and methacrylic acid, which is applied in the hydrophilic modification of polyglycidyl methacrylate or its copolymer, and the field of modified obtained materials, can solve the problems of easy loosening of the coating layer and the like

Active Publication Date: 2020-12-01
INST OF PROCESS ENG CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0005] The applicant has previously studied the hydrophilic modification of the surface of cross-linked polyacrylate materials (CN102617869A), and bonded a single layer of hydrophilic polysaccharide molecules to the surface of polyacrylate materials by chemical coupling, thereby endowing The surface of the material has a certain degree of hydrophilicity, but this method has certain limitations, mainly because the coating layer coupled with a layer of hydrophilic polysaccharide molecules is easy to loosen, and the unpolymerized residue in the microsphere material after multiple uses Hydrophobic sites such as vinyl double bonds are gradually exposed, and a certain proportion of non-specific adsorption properties are restored

Method used

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  • Hydrophilic modification method and modified material of polyglycidyl methacrylate or its copolymer
  • Hydrophilic modification method and modified material of polyglycidyl methacrylate or its copolymer
  • Hydrophilic modification method and modified material of polyglycidyl methacrylate or its copolymer

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Effect test

Embodiment 1

[0067] Preparation and pretreatment of embodiment 1 polyglycidyl methacrylate (PGMA) linear powder

[0068] Since the epoxy group of glycidyl methacrylate (GMA) is prone to ring-opening reaction at high temperature, the atom transfer radical polymerization of GMA is carried out in this embodiment under low temperature conditions. Add GMA monomer 6.6mL (50mmol) in the 100mL reactor of polytetrafluoroethylene liner, CuBr 2 55mg (0.25mmol), 2,2'-bipyridine (bpy) 78.1mg (0.5mmol), initiator azobisisobutyronitrile (AIBN) 2mL, THF 15mL, pass into N 2 to remove O from the reaction system 2 , placed in an oven, and reacted at the set temperature for 8h (take out the ice bath to cool to terminate the reaction). With tetrahydrofuran (THF) or CH 2 Cl 2 As a solvent, methanol or n-hexane as a precipitant to purify the polymer, and vacuum-dried at 45°C for 24 hours to obtain PGMA as a white powder. Such as figure 1 The residual double bond treatment method shown is to take 10 g of t...

Embodiment 2

[0069] Preparation and pretreatment of embodiment 2 cross-linked polyglycidyl methacrylate (PGMA-DVB) microspheres

[0070] Add a certain proportion of GMA monomer, crosslinking agent (DVB), diluent, surfactant and initiator (BPO) into the beaker to form an oil phase, and stir until the BPO is completely dissolved. A certain amount of stabilizer (PVA), anhydrous Na 2 SO 4 , SDS and HQ were dissolved in deionized water to form a water phase, and the oil phase was dispersed in the water phase under stirring (200r / min) to form an O / W emulsion. After passing nitrogen for 1 hour, the temperature was raised to 75° C., and polymerization was carried out under nitrogen atmosphere for 20 hours. The obtained polymer microspheres were washed three times with water and ethanol, respectively. Unpolymerized substances in the microspheres, such as surfactants, diluents, etc., were removed with acetone extraction for 24 hours. After vacuum drying at room temperature, PGMA microspheres were ...

Embodiment 3

[0071] Embodiment 3 graft monolayer dextran

[0072] Under normal temperature, 30L dimethyl sulfoxide (DMSO) is injected in the 50L reactor, start stirring, 100rpm, then take by weighing 1kg dextran powder and 12g 4-dimethylaminopyridine (DMAP) powder and put into large beaker, by Pour the beaker directly into the kettle, and keep stirring until it is completely dissolved and transparent. It takes 4 hours; after it is completely dissolved, add 2 kg of dried PGMA microspheres prepared in Example 2 to the reaction kettle, stir at room temperature for 1 hour, and then set at 100 rpm; Start to heat up to 37 degrees, start timing after the temperature rise, and keep the reaction for 3 days. During the reaction, the color of the reaction solution will deepen to 12h and become dark yellow, and the color will not change until the end of the reaction. After discharging, after filtering, wash the coated microspheres with deionized water. Cross-linked reinforced coating: prepare water p...

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Abstract

A hydrophilic modification method for crosslinked polyglycidyl methacrylates or copolymers thereof and materials obtained by modification are disclosed. The method includes performing a plurality of times of covalent cross-linking of natural polysaccharide molecules by utilizing active epoxy groups on the surface of the crosslinked polyglycidyl methacrylates or copolymers thereof so as to achieve hydrophilic modification to obtain hydrophilic modified materials of the polyglycidyl methacrylates or copolymers thereof. The method is simple to operate and mild in reaction conditions, and the obtained polyglycidyl methacrylates or copolymers thereof modified with a plurality of layers of hydrophilic modification groups have high saccharide hydroxyl contents and stable platings. Non-specific protein adsorption of polymer microspheres is eliminated. A hydrophilic layer can be coupled to other ligands or functional groups directly or through further derivation. The obtained materials have a high application prospect in the field of biochemical engineering, especially the field of biochemical separation.

Description

technical field [0001] The invention relates to the technical field of polymer material modification, in particular to a method for hydrophilic modification of polyglycidyl methacrylates or copolymers thereof (that is, glycidyl methacrylate copolymers) and modified products. Material. Background technique [0002] There are three main types of substrates used as chromatography fillers: 1. Natural polysaccharide polymers represented by cellulose, dextran and agarose; 2. Polystyrene / divinylbenzene (PS / DVB), polyacrylic acid (PAA ), polyglycidyl methacrylate (PGMA) and other synthetic polymers; 3, silica gel, hydroxyapatite, glass and other inorganic substrates. As a chromatographic separation medium, polymer microspheres have the advantages of stable chemical properties, high mechanical strength, good acid and alkali resistance, and can be operated under high pressure, etc., and have broad application prospects. However, some characteristics of the polymer itself limit its a...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08J7/12C08F220/32C08F212/36C08F8/08
CPCC08F8/08C08J7/12C08J2333/14C08F220/325C08F212/36
Inventor 马光辉李强张坤赵岚黄永东周炜清吴学星朱凯
Owner INST OF PROCESS ENG CHINESE ACAD OF SCI
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