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Starlike polymyrcene-polylactic acid block copolymer and preparation method thereof

A technology of block copolymer and myrcene is applied in the field of star-shaped polymyrcene-polylactic acid block copolymer and its preparation. Low cost, excellent elastic deformation recovery performance, and the effect of improving physical and mechanical properties

Active Publication Date: 2019-01-11
DALIAN UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The strength and rigidity of PLA are high, but the disadvantages of poor toughness and elastic deformation recovery performance seriously restrict the wide application of PLA.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0025] Synthesis of star-shaped hydroxyl-terminated polymyrcene macroinitiators: Add 10 g of myrcene monomer, 100 mL of cyclohexane and 0.72 g of anhydrous tetrahydrofuran into a 250 mL single-necked round-bottom flask, and then add 3.0×10 -3 mol tert-butyldimethylsiloxypropyllithium ((CH 3 ) 3 C-Si(CH 3 ) 2 -O-(CH 2 ) 3 -Li) initiates polymerization, reacts at 50°C for 3 hours, then lowers the temperature to room temperature, and adds 3.0×10 -3 mol divinylbenzene (DVB) coupling (measured according to the molar ratio of DVB to tert-butyldimethylsilyloxybutyllithium as 1), react at 0°C for 1 hour, and then add excess isopropanol to terminate. The product was washed with water until neutral, dried in vacuum at room temperature, and finally hydrolyzed with concentrated hydrochloric acid to obtain a hydroxyl-terminated star polymyrcene macromolecular initiator, which was dried in vacuum at room temperature. The product was tested by GPC, and its number average molecular weig...

Embodiment 2

[0027]Synthesis of star-shaped hydroxyl-terminated polymyrcene macroinitiators: 10 g of myrcene monomer, 100 mL of toluene and 0.72 g of anhydrous tetrahydrofuran were added to a 250 mL single-necked round-bottom flask, and then 2.1×10 -3 mol tert-butyldimethylsiloxybutyllithium ((CH 3 ) 3 C-Si(CH 3 ) 2 -O-(CH 2 ) 4 -Li) initiates polymerization, reacts at 40°C for 4h, then lowers the temperature to room temperature, and adds 2.1×10 -2 mol divinylbenzene (DVB) coupling (measured according to the molar ratio of DVB to lithium initiator is 10), reacted at 15°C for 30 minutes and then terminated by adding excess isopropanol. The product was washed with water until neutral, dried in vacuum at room temperature, and finally hydrolyzed with concentrated hydrochloric acid to obtain a hydroxyl-terminated star polymyrcene macromolecular initiator, which was dried in vacuum at room temperature. The product was tested by GPC, and its number average molecular weight before coupling w...

Embodiment 3

[0029] Synthesis of star-shaped hydroxyl-terminated polymyrcene macroinitiators: 10 g of myrcene monomer, 100 mL of cyclohexane and 0.72 g of tetramethylethylenediamine were added to a 250 mL single-necked round-bottom flask, and then 2.0×10 -3 mol tert-butyldimethylsiloxybutyllithium ((CH 3 ) 3 C-Si(CH 3 ) 2 -O-(CH 2 ) 4 -Li) initiates polymerization, after 5 hours of reaction at 30 ° C, the temperature is lowered to room temperature, and 0.04 mol of divinylbenzene (DVB) is added for coupling (measured according to the molar ratio of DVB to lithium initiator of 20), and after 6 minutes of reaction at 30 ° C Add excess isopropanol to terminate. The product was washed with water until neutral, dried in vacuum at room temperature, then hydrolyzed with concentrated hydrochloric acid to obtain a hydroxyl-terminated star polymyrcene macromolecular initiator, and dried in vacuum at room temperature. The product was tested by GPC, and its number average molecular weight before ...

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Abstract

The invention relates to a starlike polymyrcene-polylactic acid block copolymer and a preparation method thereof and belongs to the technical field of synthesis and preparation of high molecular materials. The polymer is the starlike polymyrcene-polylactic acid block copolymer, with a (PM-PLA)n-C structure, synthesized by polymerizing myrcene and lactide, wherein PM is polymyrcene, PLA is polylactic acid, C is a residue of a coupling agent, and n refers to an average coupling arm number of the starlike polymyrcene-polylactic acid block copolymer and is greater than or equal to 3. Based on thetotal amount of the copolymer being 100%, the polymyrcene blocks account for 10-55% by mass and the balance is polylactic acid blocks. The copolymer has a micro-phase separation structure and has highstrength, high elasticity and excellent elastic deformation restoring property. The preparation process of the copolymer is simple and efficient in flow, and relatively low in cost. An initiator doesnot contain metals, and the polymer is free of metal residues.

Description

technical field [0001] The invention belongs to the technical field of polymer material synthesis and preparation, and relates to a star-shaped polymyrcene-polylactic acid block copolymer and a preparation method thereof, which is characterized in that the star-shaped polymyrcene-polylactic acid block copolymer has a high molecular weight , narrow distribution, highly branched structure, with excellent elastic deformation recovery performance. Background technique [0002] Polylactic acid (PLA) is a thermoplastic aliphatic polyester prepared by chemical synthesis from renewable plant resources (lactic acid). Due to its biodegradability and excellent physical and mechanical properties, it is known as the most potential in the future. substitutes for petroleum-based polymers. Polylactic acid products can be decomposed into carbon dioxide and water by microorganisms after being discarded, and will not pollute the environment. Therefore, it is a completely natural cycle biodegr...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G81/02
CPCC08G81/024
Inventor 李杨魏志勇周城王艳色冷雪菲
Owner DALIAN UNIV OF TECH
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