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Flame-retardant polylactic acid and preparation method thereof

A technology of polylactic acid and prepolymer, which is applied in the field of preparation of flame-retardant polylactic acid, and can solve problems such as restricted application, melt dripping, and flammability

Pending Publication Date: 2022-03-04
ZHEJIANG HISUN BIOMATERIALS
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

As an aliphatic polyester, polylactic acid has the disadvantage of being extremely flammable due to its organic characteristics, and there is serious molten dripping during the combustion process, which seriously restricts the application of polylactic acid and its products in the fields of electronic appliances, home decoration, etc. Applications

Method used

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  • Flame-retardant polylactic acid and preparation method thereof
  • Flame-retardant polylactic acid and preparation method thereof
  • Flame-retardant polylactic acid and preparation method thereof

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preparation example Construction

[0098] On the other hand, the present invention also relates to the preparation method of flame-retardant polylactic acid, it comprises the following steps at least:

[0099] Step (1): reacting lactide with a dihydric alcohol end-capping agent, the lactide undergoes ring-opening polymerization to obtain a polylactic acid prepolymer with double-terminated hydroxyl groups;

[0100] Step (2): The polylactic acid prepolymer with double-terminal hydroxyl groups prepared in step (1) is esterified with a flame retardant containing double carboxyl groups to obtain a flame-retardant polylactic acid prepolymer containing double-terminal carboxyl groups ;

[0101] Step (3): reacting the flame-retardant polylactic acid prepolymer prepared in step (2) with a chain extender to prepare the flame-retardant polylactic acid.

[0102] Step (1): react lactide with a dihydric alcohol end-capping agent, and the lactide undergoes ring-opening polymerization to prepare a polylactic acid prepolymer w...

Embodiment 1

[0191] Example 1 was prepared by the following preparation method:

[0192] (1) Take 300g of L-lactide in a three-necked flask, replace nitrogen, raise the temperature to 150°C, add 10g of ethylene glycol and 0.3g of stannous octoate after 0.5h, and react for 5h to obtain a polylactic acid prepolymer.

[0193] (2) Take 200g of the polylactic acid prepolymer obtained in step (1), 15g of bis(4-carboxyphenyl)phenylphosphine oxide, and 0.2g of antimony trioxide in a three-necked flask, replace nitrogen, and heat up to 180°C. Vacuumize for 3.5 hours and maintain a vacuum degree of 100 Pa to obtain a flame-retardant polylactic acid prepolymer.

[0194] (3) After the reaction in step (2), keep the temperature at 180°C, add 10g of 2,2'-bis(2-oxazoline), and react for 30min to prepare high molecular weight halogen-free flame-retardant polylactic acid.

Embodiment 2

[0196] Example 2 was prepared by the following preparation method:

[0197] (1) Take 300g of L-lactide in a three-necked flask, replace nitrogen, raise the temperature to 170°C, add 5g of ethylene glycol and 0.5g of stannous octoate after 0.5h, and react for 4h to obtain a polylactic acid prepolymer.

[0198] (2) Take 200g of the polylactic acid prepolymer obtained in step (1), 10g of bis(4-carboxyphenyl)phenylphosphine oxide, and 0.4g of antimony trioxide in a three-necked flask, replace nitrogen, and heat up to 160°C. Vacuumize for 2 hours and maintain a vacuum degree of 200 Pa to obtain a flame-retardant polylactic acid prepolymer.

[0199] (3) After the reaction in step (2), keep the temperature at 160°C, add 5g of 2,2'-bis(2-oxazoline), and react for 45min to prepare high molecular weight halogen-free flame-retardant polylactic acid.

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Abstract

The invention relates to flame-retardant polylactic acid and a preparation method thereof.The flame-retardant polylactic acid comprises a polymer obtained through a reaction of a flame-retardant polylactic acid prepolymer and a chain extender, the flame-retardant polylactic acid prepolymer comprises a structure shown in the formula (I), n is an integer selected from 5-500, n is an integer selected from 1-10, and n is an integer selected from 1-10. L and L'are independently selected from linear or branched hydrocarbon chains containing 2-20 carbon atoms, and the hydrocarbon chains are optionally and independently substituted by one or more substituents selected from alkyl, cycloalkyl, alkoxy, cyano, aryl and heteroaryl; f and F'are structural fragments with flame retardant property, and the chain extender contains more than two functional groups independently selected from oxazoline group, amino group, hydroxyl group and combination of the oxazoline group, the amino group, the hydroxyl group and the combination of the oxazoline group, the amino group and the hydroxyl group.

Description

technical field [0001] The invention belongs to the technical field of polymer materials, and in particular relates to a preparation method of flame-retardant polylactic acid. Background technique [0002] Polylactic acid (PLA) is a fully degradable and environmentally friendly thermoplastic aliphatic polyester material derived from renewable resource crops. It has good biocompatibility and biodegradability, and can be used clinically for medical sutures and orthopedic fixation , Drug controlled release, tissue repair, etc., are globally recognized as the most promising biomedical materials and new packaging materials in the new century. As an aliphatic polyester, polylactic acid has the disadvantage of being extremely flammable due to its organic characteristics, and there is serious molten dripping during the combustion process, which seriously restricts the application of polylactic acid and its products in the fields of electronic appliances, home decoration, etc. Appli...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G63/692C08G63/685C08G63/78
CPCC08G63/6922C08G63/6852C08G63/78
Inventor 裴承度陈志明王良波徐宁林秀锦金洁
Owner ZHEJIANG HISUN BIOMATERIALS