Synthesis and surface modification of polyglycidyl methacrylate microspheres

A technology of polymethacrylic acid and glycidol, which is applied in the field of surface modification of solid-phase carriers, can solve problems such as inconvenient operation and environmental pollution, and achieve the effects of simple operation, simple post-processing operation, and low reaction cost

Active Publication Date: 2017-07-18
厦门圣科环保科技股份有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

When carrying out ATRP reaction, the process of introducing the initiator needs to be protected from light, and CuBr, etc. need to be weighed in the glove box, which causes inconvenient operation and pollutes the environment

Method used

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  • Synthesis and surface modification of polyglycidyl methacrylate microspheres
  • Synthesis and surface modification of polyglycidyl methacrylate microspheres
  • Synthesis and surface modification of polyglycidyl methacrylate microspheres

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0034] (1) Weigh 0.5 g of polyvinylpyrrolidone (PVP), dissolve it in 20 mL of 8.5:1 mixed solvent of ethanol and water, and transfer it to a four-neck flask after dissolving.

[0035] (2) Weigh 0.05 g of azobisisobutyronitrile (AIBN) and 2.5 g of glycidyl methacrylate (GMA) monomers, and transfer them to a four-neck flask after ultrasonic dissolution.

[0036] (3) After ultrasonicating the four-neck flask for 10 min, one mouth of the four-necked flask was sealed with a rubber stopper, one was connected to a vacuum line tube for vacuuming and nitrogen filling, the other was connected to a reflux condenser, and the middle mouth was used to fix a stirring rod. After the installation is completed, vacuumize, fill with nitrogen, repeat several times, and reflux and condense in a water bath at 72°C for more than 8 hours at a stirring speed of 180r / min.

[0037] (4) After the reaction, the white emulsion in the four-neck flask was taken out, centrifuged to remove the supernatant, and...

Embodiment 2

[0040] 1) Weigh 1 g of the white solid powder of PGMA microspheres obtained in Example 1 into a 100 mL flask, add 20 mL of water and 30 mL of ethylenediamine.

[0041] 2) A reflux condenser was connected to the mouth of the flask, and the reaction was carried out with magnetic stirring for 12 hours in a water bath at 80°C.

[0042] 3) After the reaction is over, transfer the white emulsion to a centrifuge tube and centrifuge to remove the supernatant, then centrifuge and wash with deionized water for more than 3 times. Finally, the supernatant was removed, and the white precipitate was vacuum-dried to obtain PGMA-NH 2 Microsphere white solid powder.

[0043] From image 3 It can be seen that the PGMA-NH2 microspheres obtained by this method have very little morphology damage, and still keep well dispersed microspheres; from Figure 5 It can be seen from the infrared spectrum that after ethylenediamine treats PGMA microspheres, the characteristic absorption peak of the epoxy...

Embodiment 3

[0045] 1) Weigh 0.4 g of the PGMA-NH microspheres obtained in Example 2 in a 25 mL round bottom flask, add 0.16 g of carboxybetaine (CBAA) and 12 mL of methanol solvent.

[0046] 2) Stir with magnetic force and react at room temperature for 3 days.

[0047] 3) After the reaction, transfer the white emulsion to a centrifuge tube, centrifuge to remove the supernatant, and wash with deionized water by centrifugation, repeating more than 3 times. Finally, the supernatant was removed, and the white precipitate was vacuum-dried to obtain PGMA-NH2-CBAA microspheres.

[0048] From Figure 4 It can be seen that the PGMA-NH obtained by this method 2 -CBAA microspheres, the shape is very small, and the microspheres are still well dispersed and uniform; from Figure 5 It can be seen from the infrared spectrum that after the Michael addition reaction between PGMA-NH2 and carboxybetaine, the microspheres appeared the –C(=O)-N(-H)-characteristic peak of CBAA, indicating that CBAA was on the...

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Abstract

The invention provides a poly glycidyl methacrylate microsphere synthesis and surface modification method, and relates to a solid phase carrier surface modification method. The method comprises: 1) adding polyvinylpyrrolidone, azobisisobutyronitrile and a monomer GMA to a container filled with an ethanol and water mixing solvent, vacuumizing, introducing nitrogen gas, and carrying out a reflux reaction to obtain a milky white liquid; 2) carrying out centrifugation washing on the milky white liquid obtained in the step 1), and drying to obtain the white solid powder PGMA microspheres; 3) adding the PGMA microspheres obtained in the step 2) to ethylene diamine and deionized water, carrying out a reflux reaction, carrying out centrifugation washing, and drying to white solid powder PGMA-NH2 microspheres; and 4) adding the PGMA-NH2 microspheres obtained in the step 3) to a methanol solvent of zwitterionic carboxy betaine, carrying out a reaction, carrying out centrifugation washing, and drying to the solid powder poly glycidyl methacrylate microspheres. According to the present invention, the poly glycidyl methacrylate microspheres have good dispersion property, the reaction conditions are mild, the influence on the morphology of the microspheres is low, the operation is simple, and the reaction cost is low.

Description

technical field [0001] The invention relates to a method for modifying the surface of a solid-phase carrier, in particular to a method for synthesizing and modifying the surface of polyglycidyl methacrylic acid (PGMA) microspheres. Background technique [0002] Compared with styrene (St), glycidyl methacrylate (GMA) has better hydrophilicity and biocompatibility, is easy to polymerize into balls, and contains epoxy groups that are easy to be functionalized, which is convenient for its modification. It can form groups such as amino, carboxyl or sulfhydryl, which can directly participate in various reactions and modifications, and can be used for the detection of biomedical targets. [0003] Nonspecific adsorption on solid surfaces is mainly caused by electrostatic and hydrophobic interactions. Polyethylene glycol and its derivatives are the most widely used anti-nonspecific adsorption materials, but it is a polyether substance that is particularly sensitive to aerobic enviro...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08F120/32C08F8/44C08F8/32
Inventor 周雷激刘芳毛瑜杨朝勇
Owner 厦门圣科环保科技股份有限公司
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