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Method for preparing monodisperse photoactive polymer microspheres

A photoactive polymer, monodisperse technology, applied in the field of preparing monodisperse photoactive polymer microspheres, can solve the problems of microsphere function limitation, influence effect, complicated operation, etc.

Pending Publication Date: 2022-03-29
SUN YAT SEN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

It can be seen that the current preparation method of polymer microspheres has defects such as complicated operation, limited content of functional groups, and inability to effectively ensure that enough functional groups are located on the surface of the microspheres, resulting in the limitation of the functions of the microspheres.
Therefore, it is necessary to develop a simple and efficient preparation method of photoactive polymer microspheres, so that the functional groups can fully extend to the outside of the microspheres, and avoid affecting the effect due to being inside the microspheres or covered by stabilizers

Method used

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  • Method for preparing monodisperse photoactive polymer microspheres
  • Method for preparing monodisperse photoactive polymer microspheres
  • Method for preparing monodisperse photoactive polymer microspheres

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0059] Example 1 Preparation of a small molecule RAFT agent (BMS-DDMAT) containing a benzophenone derivative photoinitiator at one end and a RAFT active group at one end

[0060] The synthetic reaction formula is as follows:

[0061]

[0062] The specific preparation method is as follows:

[0063] Add BMS-OH (1g, 3mmol), DDMAT (2.2g, 6mmol), 4-dimethylaminopyridine (DMAP) (0.076g, 0.6mmol) and anhydrous dichloromethane (CH 2 CI 2 ) (60mL), stirred and dissolved in an ice-water bath, and when the temperature dropped to about 0°C, anhydrous dichloromethane solution containing dicyclohexylcarbodiimide (DCC) (1.3g, 6mmol) was added dropwise ( 10 mL) for more than 15 min, and continued to react for 1 h in an ice-water bath. Then transfer to room temperature and react for 48h. After the reaction, remove the insoluble matter DCU generated in the reaction solution by filtration in a suction filter bottle, then add 100mL of 5% sodium hydroxide aqueous solution to dissolve the rem...

Embodiment 2

[0064] Embodiment 2 prepares the macromolecular RAFT agent (BMS-PAA) that one end contains benzophenone derivative photoinitiator, one end contains RAFT active group 267 -DDMAT)

[0065] The synthetic reaction formula is as follows:

[0066]

[0067] In the formula, the value of n depends on the amount of acrylic acid (AA), and n=267 in this embodiment.

[0068] BMS-PAA 267 The specific preparation method of -DDMAT is as follows:

[0069] In a 100 mL one-necked flask, BMS-DDMAT (0.25 g, 0.375 mmol), acrylic acid (AA) (7.2 g, 100 mmol), AIBN (azobisisobutyronitrile, 0.0062 g, 0.00375 mmol) and anhydrous 1,4 - Dioxane (30 mL), blowing nitrogen gas for 30 min, and then putting the flask into a preheated oil bath at 70° C. for 4 hours to react. After the reaction, the product was precipitated with ether. In order to purify the product, it was necessary to repeat the operation many times, that is, first dissolve it with anhydrous 1,4-dioxane, then precipitate it with ether, ...

Embodiment 3

[0070] Embodiment 3 prepares photoactive polymer microsphere

[0071] In a 25mL round bottom flask, add 18g of absolute ethanol and water mixed solvent (w / w=40 / 60), 2g of monomer MMA (10% relative to the system), 0.2g of stable dispersant BMS-PAA n -DDMAT (10% with respect to MMA monomer), the chain transfer agent DDMAT of 0.005g (0.5% with respect to MMA monomer), feed nitrogen 30min after stirring and dissolving, then add 0.08g hydrogen peroxide and ascorbic acid mixture (4wt% With respect to the MMA monomer, wherein the molar ratio of hydrogen peroxide and ascorbic acid is 1:1), a stable emulsion product, namely monodisperse photoactive polymer microspheres, is obtained after reaction at room temperature for 1 hour. Scanning electron micrographs of the product as figure 1 shown. From figure 1 It can be seen that the photoactive polymer microspheres prepared by this method exhibit a monodisperse distribution.

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Abstract

The invention belongs to the technical field of surface functional polymer microspheres, and particularly relates to a method for preparing monodisperse photoactive polymer microspheres. The preparation method comprises the following steps: firstly, carrying out esterification reaction on a hydroxyl-containing benzophenone derivative photoinitiator and a carboxyl-containing reversible addition-fragmentation chain transfer reagent to synthesize a small-molecule RAFT reagent containing the benzophenone derivative photoinitiator and an RAFT active group, and then carrying out RAFT solution polymerization reaction to synthesize a macromolecular RAFT reagent. Then, the macromolecular RAFT reagent is used as a stable dispersing agent, and monodisperse photoactive polymer microspheres are synthesized through a dispersion polymerization reaction. The monodisperse polymer microspheres grafted with photo-initiation active groups on the surfaces are efficiently synthesized through a one-step method, the content of functional groups on the surfaces of the microspheres can be controlled by adjusting the amount of the stabilizer, and the situation that the effect is affected due to the fact that the photo-initiation active groups are located in the microspheres or covered by the stabilizer can be avoided.

Description

technical field [0001] The invention belongs to the technical field of surface functional polymer microspheres, in particular to a method for preparing monodisperse photoactive polymer microspheres. Background technique [0002] Monodisperse surface functional polymer microspheres have a wide range of applications in many fields, such as biological detection, protein separation and drug release, due to the surface has a certain amount of active groups. Different application fields have different requirements for the functional properties of microspheres. Therefore, if a microsphere with active groups that can be flexibly modified on the surface can be synthesized and used as the matrix of functional microspheres, the microspheres can be modified according to different application requirements and used in different occasions. For example, the introduction of photoactive groups on the surface of microspheres can conveniently and rapidly modify the surface of microspheres thro...

Claims

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Application Information

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IPC IPC(8): C08F120/06C08F2/48C08F2/38C08F293/00
CPCC08F120/06C08F2/48C08F2/38C08F293/005C08F2438/03
Inventor 曾兆华袁世彬谢刚杨建文
Owner SUN YAT SEN UNIV
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