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Polylactic acid segmented copolymer and modified polylactic acid preparation method

A technology of block copolymer and polylactic acid, which is applied in the field of preparation of polylactic acid block copolymer and modified polylactic acid, can solve the problems of low reaction efficiency, prolonged blending time, unstable samples, etc.

Active Publication Date: 2014-05-21
CHANGCHUN INST OF APPLIED CHEMISTRY - CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] At present, there have been some reports on the research on PLA modification. The Chinese patent with the publication number CN101597374A discloses a preparation method of long-branched polylactic acid. The long-branched polylactic acid is prepared by reacting polylactic acid with an epoxy monomer with a trifunctionality or more. Branched polylactic acid improves the melt strength, but because the ends of commercialized polylactic acid are mostly capped, the reaction efficiency with epoxy groups is low, and the blending time needs to be prolonged, which increases the production cost; the Chinese patent with the publication number CN102010583 Disclosed are high-molecular-weight long-chain branched crystalline polylactic acid materials and a preparation method thereof. By adding a protonic acid into an aqueous lactic acid solution as a catalyst, dehydration, and reacting with a dibasic acid or an anhydride to obtain a carboxyl-terminated product, and then acting on the catalyst Lewis acid Down polycondensation, finally add crosslinking agent diglycidyl ester and crystallization accelerator to obtain long-chain branched crystalline polylactic acid, but diglycidyl ester is a small molecule, unreacted diglycidyl ester will migrate to the surface of the product, causing the sample unstable

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  • Polylactic acid segmented copolymer and modified polylactic acid preparation method
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  • Polylactic acid segmented copolymer and modified polylactic acid preparation method

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preparation example Construction

[0033] The invention provides a method for preparing a polylactic acid block copolymer, comprising the following steps: A) reacting branched polylactic acid and a halogenated acid halide under the action of a first catalyst to obtain a macromolecular initiator, the halogenated acid halide The acyl halide is a halogenated isobutyryl halide and / or a halogenated propionyl halide; B) the macroinitiator is mixed with glycidyl methacrylate under the action of cuprous halide and N-containing ligands, in a solvent The reaction was carried out to obtain a polylactic acid block copolymer.

[0034] The branched polylactic acid described in the present invention is preferably prepared according to the following steps: react lactide and polyhydric alcohol under the action of the second catalyst by heating to obtain branched polylactic acid, the number of hydroxyl groups of the polyhydric alcohol is ≥3, preferably 3~20, more preferably 3~10.

[0035] Wherein, the molar ratio of lactide to ...

Embodiment 1

[0061] A 500mL reaction bottle with two vents was vacuum-baked and degassed, and after repeated argon filling three times, 200g (1.4mol) lactide, 0.13g (1.4×10 -3 mol) glycerol with 0.28g (7×10 -4 mol) stannous octoate, sealed system, heated to 120°C, stirred and reacted for 24 hours to obtain a white crystalline polymer, dissolved in chloroform, precipitated with excess ethanol to obtain a white solid, dried in vacuum to constant weight, and obtained branched polylactic acid , the relative weight average molecular weight is 180.0kg / mol, the relative molecular weight distribution is 1.50, and the relative molecular weight distribution is a relatively narrow peak.

[0062] Utilize nuclear magnetic resonance to analyze the branched polylactic acid obtained in embodiment 1, obtain its hydrogen nuclear magnetic resonance spectrum figure, as figure 1 , where a and b are the displacements of different hydrogens in the polymer, respectively.

[0063] The branched polylactic acid ob...

Embodiment 2

[0065] A 500mL reaction bottle with two vents was vacuum-baked and degassed, and after repeated argon filling three times, 200g (1.4mol) lactide, 0.26g (2.8×10 -3 mol) glycerol with 0.28g (7×10 -4 mol) stannous octoate, sealed system, heated to 120°C, stirred and reacted for 24 hours to obtain a white crystalline polymer, dissolved in chloroform, precipitated with excess ethanol to obtain a white solid, dried in vacuum to constant weight, and obtained branched polylactic acid , the relative weight average molecular weight is 92.0kg / mol, the relative molecular weight distribution is 1.48, and the relative molecular weight distribution is a relatively narrow peak.

[0066] The branched polylactic acid obtained in Example 2 was analyzed by nuclear magnetic resonance, and the number of branched chains was 3 through analytical calculation.

[0067] The branched polylactic acid obtained in Example 2 was analyzed by differential scanning calorimetry (DSC), and its melting point was ...

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Abstract

The invention provides a polylactic acid segmented copolymer and modified polylactic acid preparation method. The method includes: reacting branched polyactic acid with halogenated acid halide to obtain macroinitiator to further react with glycidyl methacrylate to obtain the polylactic acid segmented copolymer; and finally, blending the branched polyactic acid, the polylactic acid segmented copolymer and polylactic acid to obtain the modified polylactic acid. Compared with the prior art which using bis-glycidyl ester for modifying the polylactic acid, the method has the advantages that firstly, the polylactic acid-polyglycidyl methacrylate segmented copolymer is a macromolecular compound and can be in cross-linking reaction with the branched polylactic acid and the polylactic acid to form polymer with higher molecular weight and higher branching degree, so that the problems of proneness to migration and osmosis of micromolecular branched cross-linking agent are solved, and stability of the modified polylactic acid is improved; and secondly, the polylactic acid-polyglycidyl methacrylate segmented copolymer with an intrinsic branched polylactic acid structure unit has high compatibility to the branched polylactic acid and the polylactic acid.

Description

technical field [0001] The invention belongs to the field of polymer materials, in particular to a polylactic acid block copolymer and a preparation method of modified polylactic acid. Background technique [0002] Plastic products are indispensable in people's lives, but traditional plastic products generally take hundreds of years or even longer to degrade completely, resulting in serious "white pollution"; at the same time, traditional plastic raw materials are derived from petroleum and other unavailable Renewable resources, with the depletion of petrochemical resources, the traditional plastic industry is also threatened. Therefore, vigorously developing environmentally friendly biodegradable polymers to replace petroleum-based plastic products has become a hot spot in current research and development. [0003] Among them, polylactic acid (PLA) is a very important biodegradable plastic. It is a new type of biodegradable polymer material chemically synthesized from lact...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08F293/00C08G63/08C08L67/04C08L53/00
Inventor 陈学思张宝李杲黄绍永庄秀丽
Owner CHANGCHUN INST OF APPLIED CHEMISTRY - CHINESE ACAD OF SCI
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