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Preparation method of thermosetting polylactic acid

A polylactic acid and thermosetting technology, applied in the field of preparation of thermosetting polylactic acid, can solve the problems of uncontrollable cross-linking structure regularity and uniformity, inconvenience in forming composite materials, large melt viscosity, etc., and achieves a safe and environmentally friendly synthesis process, and is easy to industrialize. production, effect of low melt viscosity

Active Publication Date: 2013-03-13
TONGJI UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, because these methods directly use commercialized thermoplastic polylactic acid and crosslinking agent to melt blend and initiate crosslinking by irradiation or only use crosslinked polylactic acid as a reinforcing phase, not only the crosslinking density is low, the regularity of the crosslinking structure and The uniformity is uncontrollable, and the large melt viscosity is not convenient for the molding of composite materials
In addition, the above methods only introduce a partial crosslinking structure into thermoplastic polylactic acid to improve its performance, and the real thermosetting polylactic acid has not been reported yet.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0019] (1) Add 100 grams of L-lactic acid with a purity of 88% to a 250ml three-necked bottle with a stirrer, heat to 110°C, and stir and dehydrate for 3 hours under a vacuum of 70mmHg.

[0020] (2) Add 0.0088 g of stannous octoate and 6.66 g of pentaerythritol to the dehydrated lactic acid, first raise the temperature of the reaction system to 160 °C at a rate of 10 °C / h, and then react at 160 °C for another 12 hours, and the vacuum degree of the polycondensation reaction is 10mmHg.

[0021] (3) Add 33.18 g of methacrylic anhydride to the polycondensation product, control the reaction temperature at 130° C., and react for 3 hours under nitrogen atmosphere.

[0022] (4) To the synthesized resin was added 1.92 g of tert-butyl peroxybenzoate at 100°C and predispersed by stirring for 10 minutes. Pour the resin into the mold and keep it warm at 140°C for 3 hours, and finally post-cure at 180°C for 0.5 hours.

[0023] T of cured product g The temperature is 86.9°C, the sample ca...

Embodiment 2

[0025] (1) Add 100 grams of L-lactic acid with a purity of 88% to a 250ml three-necked bottle with a stirrer, heat to 90°C, and stir and dehydrate for 4 hours under a vacuum of 30mmHg.

[0026] (2) Add 0.0440 g of zinc chloride and 5.00 g of glycerol to the dehydrated lactic acid, first raise the temperature of the reaction system to 150°C at a rate of 10°C / h, and then react at 150°C for another 10h, and the polycondensation reaction takes place in a vacuum The degree is 5mmHg.

[0027] (3) Add 24.90 g of acrylic anhydride to the polycondensation product, control the reaction temperature to 120° C., and react for 4 hours under nitrogen atmosphere.

[0028] (4) At 80°C, 1.53 g of dicumyl peroxide was added to the synthesized resin and predispersed by stirring for 5 minutes. Pour the resin into the mold and keep it warm at 150°C for 2 hours, and finally post-cure at 180°C for 1 hour.

[0029] T of cured product g The temperature is 69.4°C, the sample can keep its original sha...

Embodiment 3

[0031] (1) Add 100 grams of L-lactic acid with a purity of 88% to a 250ml three-necked bottle with a stirrer, heat to 120°C, and stir and dehydrate for 2 hours under a vacuum of 80mmHg.

[0032] (2) Add 0.0616 g of aluminum chloride and 5.18 g of dipentaerythritol to the dehydrated lactic acid, first raise the temperature of the reaction system to 170°C at a rate of 10°C / h, and then react at 170°C for another 14h, and the vacuum degree of polycondensation reaction It is 1mmHg.

[0033] (3) Add 22.65 g of methacrylic anhydride to the polycondensation product, control the reaction temperature to 140° C., and react for 3.5 hours under nitrogen atmosphere.

[0034] (4) At 120°C, 2.32 g of cumene hydroperoxide was added to the synthesized resin and predispersed by stirring for 10 minutes. Pour the resin into the mold and keep it warm at 160°C for 2 hours, and finally post-cure at 200°C for 1.5 hours.

[0035] T of cured product g The temperature is 88.4°C, the sample can keep it...

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PUM

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Abstract

The invention relates to a preparation method of thermosetting polylactic acid. The preparation method comprises the following steps: using lactic acid to perform direct polycondensation in the presence of a coinitiator and prepare star-shaped polylactic acid, performing terminal group modification, and adding a proper initiator to initiate the crosslinking of the system and curing the system. The preparation method has a simple process; no waste is generated, no organic solvent is used, the synthetic process is safe and environmentally-friendly; lactic acid is used to perform a direct polycondensation process, thus industrial production is more easier to realize compared with the lactide ring-opening polymerization; the star-shaped product has lower melt viscosity and is convenient for the processing of the composite material; and the product and many kinds of unsaturated monomers such as styrene and divinylbenzene are used to realize copolymerization. Therefore, the preparation method has a wider application prospect.

Description

technical field [0001] The invention relates to a preparation method of thermosetting polylactic acid. Background technique [0002] The huge production and consumption of synthetic polymer materials has created two major issues: the massive consumption of limited petroleum resources and the environmental pollution caused by waste polymers. In this case, environmentally friendly biodegradable polymer materials have emerged and developed vigorously. Among the many biodegradable polymer materials that have been developed, polylactic acid (PLA) is due to its complete biodegradability and other Renewable resources attract attention for the plant origin of raw materials. At the same time, as a thermoplastic polymer, polylactic acid is suitable for various methods such as extrusion, injection, melt spinning, solution spinning, blow molding, and biaxial stretching due to its good mechanical properties, thermoplasticity, fiber formation, and high transparency. Processing, its appl...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08G63/91C08G63/06C08G63/78C08J3/24C08F290/06
Inventor 任杰常少坤曾超
Owner TONGJI UNIV
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