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Phosphor-containing halogen-free flame-retardant polylactic acid, preparation thereof and flame-retardant material blended therewith

A polylactic acid, flame retardant technology, applied in the field of flame retardant polylactic acid and its preparation, can solve the problems of easy precipitation, poor flame retardant compatibility, etc., to overcome easy precipitation, overcome poor compatibility, and avoid material mechanical properties. worsening effect

Active Publication Date: 2009-05-27
SICHUAN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] The primary purpose of the present invention is to provide a new phosphorus-containing halogen-free flame-retardant polylactic acid for the defects of the existing additive flame-retardant polylactic acid. The flame-retardant element phosphorus in the polylactic acid is linked to the polylactic acid On the main chain of the lactic acid molecule, it can increase the molecular weight while endowing the flame retardant properties of the polylactic acid itself, and overcome the shortcomings of the additive flame retardant, such as poor compatibility and easy precipitation.

Method used

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  • Phosphor-containing halogen-free flame-retardant polylactic acid, preparation thereof and flame-retardant material blended therewith
  • Phosphor-containing halogen-free flame-retardant polylactic acid, preparation thereof and flame-retardant material blended therewith
  • Phosphor-containing halogen-free flame-retardant polylactic acid, preparation thereof and flame-retardant material blended therewith

Examples

Experimental program
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Effect test

Embodiment 1

[0049] Dissolve 50ml (0.546mol) of phosphorus oxychloride in diethyl ether first, then cool in an ice bath to below 5°C, then add 51.3g (0.546mol) of phenol dropwise into the system through a constant pressure dropping funnel, and the dropwise addition is complete After reacting for 2 hours, the temperature was raised to 10°C and kept at a constant temperature for 10 minutes. Finally, diethyl ether was evaporated under normal pressure, and the phenoxyphosphoryl dichloride fraction was collected by distillation under reduced pressure for future use.

[0050] First, 30g (0.024mol) of hydroxyl-terminated polylactic acid prepolymer with a molecular weight of 1250g / mol and 0.03g of stannous chloride were protected under nitrogen, mechanically stirred and heated to 140°C, and after it melted, 2.53g (0.012 mol) phenoxyphosphoryl dichloride was added to the reaction system with a syringe, and after 10 minutes of normal pressure reaction, the pressure was reduced to 100Pa, and the react...

Embodiment 2

[0052] First, 30g (0.0097mol) of hydroxyl-terminated polylactic acid prepolymer with a molecular weight of 3100g / mol and 0.09g of stannous chloride were protected under nitrogen, mechanically stirred and heated to 150°C, and after it was melted, 2.05g (0.0097 mol) phenoxyphosphoryl dichloride (because its preparation is the same as in Example 1, so it is omitted.) was added to the reaction system with a syringe, after 30 minutes of normal pressure reaction, the pressure was reduced to 10Pa, and the product was obtained after 1 hour of reaction. Its intrinsic viscosity is 0.44dl / g.

Embodiment 3

[0054] Dissolve 50ml (0.546mol) of phosphorus oxychloride in ether first, then cool in an ice bath to below 5°C, then add 32.0ml (0.546mol) of ethanol dropwise into the system through a constant pressure dropping funnel, and the dropwise addition is complete After reacting for 1 hour, the temperature was raised to 10°C, and the temperature was kept constant for 20 minutes. Finally, diethyl ether was evaporated under normal pressure, and the ethoxyphosphoryl dichloride fraction was collected by distillation under reduced pressure for future use.

[0055] First, 30g (0.0066mol) of hydroxyl-terminated polylactic acid prepolymer with a molecular weight of 4520g / mol and 0.15g of stannous chloride were protected under nitrogen, mechanically stirred and heated to 160°C, and after melting, 0.94ml (0.0080 mol) ethoxyphosphoryl dichloride was added into the reaction system with a syringe, and after 90 minutes of normal pressure reaction, the pressure was reduced to 20Pa, and the product ...

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Abstract

The invention discloses a phosphorus-containing halogen-free flame-retardant polylactic acid, which is obtained by leading phosphorus element with flame retardant function into a molecular backbone through a chain extending method or a coupling method. The phosphorus content of the polylactic acid is between 0.1 and 5 weight percent, and the vertical combustion level of the polylactic acid is V-0. The invention also discloses a method for preparing the halogen-free flame-retardant polylactic acid, and a flame retardant material formed by blending the phosphorus-containing halogen-free flame-retardant polylactic acid with common industrial polylactic acid. The phosphorus-containing flame-retardant polylactic acid provided by the invention leads flame-retardant element into the molecular backbone of the polylactic acid through chain extending or coupling reaction, thereby improving the molecular weight of the polylactic acid, endowing a polylactic acid body and the blended flame retardant material with good flame retardant property and overcoming the disadvantages of poor compatibility, precipitation easiness and the like caused by the application of additive flame retardant. In addition, as no halogen component is contained, no halogen-containing gas can be released during application, thereby particularly preventing the release of harmful gas from polluting environment and harming human bodies during combustion.

Description

technical field [0001] The invention belongs to the technical field of flame-retardant polylactic acid (PLA) and its preparation, and in particular relates to a phosphorus-containing halogen-free flame-retardant polylactic acid, a preparation method thereof, and a flame-retardant material blended with ordinary polylactic acid. technical background [0002] With the improvement of people's living standards, more and more polymer materials are used in building decoration, decorative materials and furniture. However, most polymer materials are flammable (B3 grade) or combustible (B2 grade) materials. When encountering high temperature during use, they will decompose and burn, causing fire and releasing toxic gases, which will bring serious damage to people's lives and property safety. threaten. [0003] As an aliphatic polyester, PLA is a bio-based polymer synthesized from renewable biological resources rather than petroleum resources. The load is small, coupled with its cert...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G63/692C08G63/78C08L67/04
Inventor 王德义宋艳朋汪秀丽袁小亚王玉忠
Owner SICHUAN UNIV
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