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Crosslinking polylactic acid and preparation method thereof

A polylactic acid and cross-linked technology, applied in the field of cross-linked polylactic acid and its preparation, can solve the problems of inconvenient composite material molding, poor heat resistance of polylactic acid, low cross-linking density, etc. Melt viscosity, easy processing effect

Inactive Publication Date: 2011-07-13
TONGJI UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, because these two methods directly use commercialized linear polylactic acid and cross-linking agent to melt blend, not only the cross-linking density is low, but also the high melt viscosity is not convenient for the molding of composite materials.
[0005] In view of the above situation, the present invention provides a cross-linked polylactic acid and its preparation method, by synthesizing multi-armed star-shaped polylactic acid and modifying it, and then triggering the cross-linking of the modified star-shaped polylactic acid by appropriate means Curing by reaction to improve the disadvantage of poor heat resistance of polylactic acid

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0029] (1) Add 0.92g of glycerol, 10.8g of dry L-lactide and 0.0012g of stannous octoate into a reaction vessel with an inert gas, stir and heat to 120°C, and react for 5 hours to obtain star shaped polylactic acid.

[0030] (2) Add 0.055 g of hydroquinone to the product obtained in step (1), then add 0.036 mol of methacrylic anhydride, stir and heat to 110°C, and react for 5 hours under an inert gas environment to obtain the terminal group modified Sexual star polylactic acid.

[0031] (3) Add 0.14 g of cumene hydroperoxide to the modified product melt obtained in step (2) at 100° C., keep warm and stir for 5 minutes. Subsequently, the resin is poured into the mold and kept at 160°C for 2 hours, and finally post-cured at 200°C for 1 hour.

[0032] T of cured product g The temperature is 69°C, the sample can keep its original shape without deformation at 200°C, the temperature for 5% weight loss is 248°C, and the temperature for the maximum weight loss rate is 318°C.

Embodiment 2

[0034] (1) Add 1.36g of pentaerythritol, 14.4g of dry D,L-lactide and 0.0027g of stannous octoate into a reaction vessel with an inert gas, stir and heat to 130°C, and react for 4 hours to obtain star shaped polylactic acid.

[0035] (2) Add 0.080 g of hydroquinone to the product obtained in step (1), then add 0.050 mole of methacrylic anhydride, stir and heat to 120°C, and react for 4 hours under an inert gas environment to obtain the terminal group modified Sexual star polylactic acid.

[0036] (3) Add 0.20 g of tert-butyl peroxybenzoate to the melt of the modified product obtained in step (2) at 110° C., keep warm and stir for 7 minutes. Subsequently, the resin is poured into the mold and kept at 130°C for 1 hour, and finally post-cured at 180°C for 1 hour.

[0037] T of cured product g The temperature is 78°C, the sample can keep its original shape without deformation at 200°C, the temperature for 5% weight loss is 263°C, and the temperature for the maximum weight loss ...

Embodiment 3

[0039] (1) Add 2.54 grams of dipentaerythritol, 43.2 grams of dry L-lactide and 0.0071 grams of stannous octoate into a reaction vessel with an inert gas, stir and heat to 160 ° C, and react for 2 hours to obtain a star polylactic acid.

[0040] (2) Add 0.088 g of hydroquinone to the product obtained in step (1), then add 0.072 moles of methacrylic anhydride, stir and heat to 130°C, and react for 3 hours under an inert gas environment to obtain the terminal group modified Sexual star polylactic acid.

[0041] (3) At 120°C, add 0.85 g of tert-butyl hydroperoxide to the melt of the modified product obtained in step (2), keep warm and stir for 10 minutes. Subsequently, the resin is poured into the mold and kept at 170°C for 2 hours, and finally post-cured at 200°C for 2 hours.

[0042] T of cured product g The temperature is 71°C, the sample can keep its original shape without deformation at 200°C, the temperature for 5% weight loss is 253°C, and the temperature for the maximum ...

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Abstract

The invention relates to a crosslinking polylactic acid and a preparation method thereof. The preparation method comprises the following steps of: in the presence of a coinitiator, synthesizing starlike polylactic acid through ring-opening polymerization of lactide; modifying a terminal group by using unsaturated anhydride; initiating C=C double-bond free radical polymerization reaction by a proper method; and crosslinking and curing to obtain the product. The crosslinking polylactic acid and the preparation method thereof have the following advantages that: under the condition of the same molecular weight, the starlike polylactic acid has lower melting viscosity compared with that of linear molecules, so that a composite material is easy to process; crosslinking density of a curing product can be changed by adjusting the arm number and the arm length of the starlike polylactic acid; and various initiating methods can be selected, so that different requirements of a polylactic acid body and the composite material of the polylactic acid body during formation are met.

Description

technical field [0001] The invention relates to a cross-linked polylactic acid and a preparation method thereof. Background technique [0002] The growing awareness of environmental protection and energy shortage have aroused people's attention to the research, development and application of biodegradable materials. Among the many biodegradable polymer materials that have been developed, the research on the synthesis, preparation, processing and application of polylactic acid is the most active. Polylactic acid (PLA) is derived from renewable non-food crops (such as cassava, sugarcane, sweet sorghum, etc.), and its most prominent advantage is biodegradability. Pollution of the environment is very beneficial to the protection of the environment. So far, polylactic acid has been able to perform various molding processes like ordinary polymers. After secondary processing such as thermoforming and spinning, various films, sheets, and fibers prepared by it can be used in textil...

Claims

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Application Information

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IPC IPC(8): C08G63/91C08G63/08C08J3/28C08J3/24
Inventor 任杰常少坤曾超
Owner TONGJI UNIV
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