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Preparation of polymethyl tert-butyl acrylate large molecular monomer by atom transfer radial

A technology of poly-tert-butyl methacrylate and macromonomers, which is applied in the field of preparation of macromolecular monomers, and achieves the effects of mild reaction conditions, high reactivity and precise structure

Inactive Publication Date: 2006-11-29
JIANGNAN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

There is no literature report on the preparation of poly tert-butyl methacrylate macromonomer by atom transfer radical polymerization (ATRP)

Method used

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  • Preparation of polymethyl tert-butyl acrylate large molecular monomer by atom transfer radial
  • Preparation of polymethyl tert-butyl acrylate large molecular monomer by atom transfer radial
  • Preparation of polymethyl tert-butyl acrylate large molecular monomer by atom transfer radial

Examples

Experimental program
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Effect test

Embodiment 1

[0030] Add bipyridine, CuCl, tert-butyl methacrylate (predetermined amount, added according to the molecular weight requirement) into a 100mL three-necked flask in sequence according to the formula at room temperature, stir to make them fully mixed, freeze and thaw the mixed solution and repeat three times Circulation, continuously feed high-purity nitrogen for 30 minutes, add p-chloromethyl styrene, and then seal the three-necked flask. Place the three-necked flask in an oil bath at 80-90°C, stir it with magnetic force, and react for a predetermined time (6-8 hours). The three-necked flask was taken out, cooled naturally, and tetrahydrofuran was added to the reaction liquid to fully dissolve the reaction product, and the above solution was filtered through an alumina glass column to remove residual CuCl therein. Under stirring, add methanol / water (V methanol / V water ≈ 1:1) mixed solvent dropwise to the filtrate to completely precipitate the polymer in the filtrate, filter wit...

Embodiment 2

[0032] Step 1: Add bipyridine or PMDETA (1mmol), CuCl (0.5mmol), tert-butyl methacrylate (predetermined amount, 10-100mmol according to the required molecular weight) in sequence in a 100mL three-necked flask at room temperature, and stir Make it fully mixed, repeat three cycles of freezing and thawing the mixed solution, continuously feed high-purity nitrogen for 30 minutes, add ethyl α-bromopropionate (0.5 mmol), and then seal the three-necked flask. Place the three-necked flask in an oil bath at 80-90°C, stir it with magnetic force, and react for a predetermined time (6-8 hours). The three-necked flask was taken out, cooled naturally, and tetrahydrofuran was added to the reaction liquid to fully dissolve the reaction product, and the above solution was filtered through an alumina glass column to remove residual CuCl therein. Under stirring state, dropwise add methanol / water (V methanol / V water ≈ 1: 1) mixed solvent to the filtrate, the polymer in the filtrate is precipitate...

Embodiment 3

[0035]The reaction was carried out according to the steps described in Example 2, but the second step of the nucleophilic substitution reaction was to replace methacrylic acid with acrylic acid, and the reaction conditions were the same as in Example 2, to prepare acrylic acid-terminated polytert-butyl methacrylate macromer.

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Abstract

This is a preparation of polytert-butyl methacrylic (PBMA) macromolecule monomer through atom transfer free radical polymerization (ATRP), belonging to macromolecule monomer preparation technology field. The invention provides the PBMA macromolecule monomer, including the styrene end-sealed one and crylic acid or methacrylic acid (MAA) end-sealed one. This kind of macromolecule monomer has the physical property and chemical reactive property, so it is very suitable for the structure design of macromolecule, and is widely used in the preparation of stem grafting macromolecule, segment embedded macromolecule and nanometer macromolecule grain material system. ATRP is a kind of active / controllable free radical polymerization., which has wide suitable monomers, simple operation, mild reaction condition, and can obtain high polymers of accurate structure and equably distributed molecular weights(Mw / Mn < 1.20). Applying the ATRP method can synthesize macromolecule monomers of uniformly distributed molecular weight.

Description

technical field [0001] Atom transfer radical polymerization is used to prepare poly(tert-butyl methacrylate) macromonomers. Polymethacrylate, a functional macromonomer with precise structure and high reactivity, can be prepared by atom transfer radical polymerization or by continuing nucleophilic substitution reaction. The invention discloses tert-butyl acrylate, which belongs to the technical field of macromonomer preparation. Background technique [0002] At present, there are many methods for the preparation of macromonomers: anionic polymerization, cationic polymerization, group transfer polymerization and so on. However, most of them are limited in the range of applicable monomers, and the reaction conditions are relatively harsh. The Atom Transfer Radical Polymerization (ATRP) method is suitable for many types of monomers, a wide range, mild reaction conditions, and can obtain polymers with a narrow molecular weight distribution, and the molecular weight is easy to co...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08F120/16C08F8/00C08F265/04
Inventor 陈明清杨伟刘晓亚倪忠斌杨成
Owner JIANGNAN UNIV
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