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A kind of synthetic method of macromonomer

A technology of macromonomer and synthesis method, which is applied in the field of macromonomer preparation, and achieves the effects of rich structure, mild reaction conditions and broadened application.

Inactive Publication Date: 2017-10-20
CHANGZHOU UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] The present invention is aimed at the shortcomings and deficiencies of the current macromonomer synthesis method, and provides a simple method for synthesizing macromolecular initiators

Method used

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  • A kind of synthetic method of macromonomer

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0029] Add 0.34 g (3 mmol) caprolactone, 0.15 g (0.3 mmol) p-vinylbenzyl alcohol, and 0.1 g THF to a dry 50 mL reaction flask. The reaction system, after three times of "vacuumizing-nitrogen", added 300 mu L (0.3 mmol) t -BuP 4 n-hexane solution. at -30 o After reacting for 48 h under the condition of C, 2 mL of 10 wt% hydrochloric acid solution was added dropwise to terminate the above reaction. Then use 2 × 100 mL methanol to fully wash the polymer under rapid stirring to remove unreacted monomer and solvent, filter, 50 o C under vacuum for 12 h, the calculated yield was 80%, and the molecular weight was 1500 g / mol.

Embodiment 2

[0031] Add 34 g (300 mmol) of caprolactone and 0.15 g (0.3 mmol) of p-vinylbenzyl alcohol into a dry 250 mL reaction flask. The reaction system, after three times of "vacuumizing-nitrogen", added 300 mu L (0.3mmol) t -BuP 4 n-hexane solution. at 200 o After reacting at C for 0.5 h, 2 mL of 10 wt% hydrochloric acid solution was added dropwise to terminate the above reaction, and 50 mL of THF was added to dissolve the polymer. Then use 3 × 200 mL methanol to fully wash the polymer under rapid stirring to remove unreacted monomers, filter, 50 o C under vacuum for 12 h, the calculated yield was 84%, and the molecular weight was 134200 g / mol.

Embodiment 3

[0033] Add 0.34 g (3 mmol) caprolactone, 0.15 g (0.3 mmol) p-vinylbenzyl alcohol, and 1.0 g THF to a dry 50 mL reaction flask. The reaction system, after three times of "vacuumizing-nitrogen", added 0.01g (0.3 mmol) NaOH solution in n-hexane under the protection of nitrogen. at 25 o After reacting for 48 h under the condition of C, 2 mL of 10 wt% hydrochloric acid solution was added dropwise to terminate the above reaction. at -30 o After 48 h of reaction under C conditions, 2 mL of 10 wt% hydrochloric acid solution was added dropwise to terminate the above reaction. Then use 2 × 100 mL methanol to fully wash the polymer under rapid stirring to remove unreacted monomers and solvents, filter, 50 o C under vacuum for 12 h, the calculated yield was 60%, and the molecular weight was 1600 g / mol.

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Abstract

The invention relates to a method for synthesizing a macromonomer, which belongs to the technical field of macromonomer preparation. The method uses a strong base and a compound containing double bonds and active hydrogen as an initiating system to initiate homopolymerization or copolymerization of vinyl monomers or cyclic monomers, and synthesize macromonomers containing terminal double bonds in one step. The polymerization reaction conditions of the present invention are mild, and the raw materials used have industrial products, which are suitable for industrial production, and the prepared macromonomer structure is rich, which not only has the physical characteristics of polymers, but also has chemical reactivity. Polymers, degradable polymers and nano-polymer particle materials are widely used.

Description

technical field [0001] The invention relates to a method for synthesizing a macromonomer, and belongs to the technical field of macromonomer preparation. Background technique [0002] A macromonomer is a linear low molecular weight polymer with a functional group at the end of the molecule that can participate in the polymerization reaction. Such polymers can be copolymerized with small molecular monomers to form graft or comb-shaped polymers with small molecular monomers as the main chain. Therefore, macromonomers are widely used in polymer modification, and their application prospects are very broad. However, at present, macromonomers are mostly synthesized by anionic polymerization, cationic polymerization, group transfer polymerization, free radical polymerization and other methods. The preparation process of these methods is cumbersome, and the types of available monomers are limited, and the reaction conditions are harsh, which is not conducive to the industrializati...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08G63/08C08G65/28C08G77/14C08G79/04C08F120/14C08F120/34C08F126/06C08F120/54C08G63/64
Inventor 杨宏军蒋必彪黄文艳薛小强
Owner CHANGZHOU UNIV
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