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Preparation method of compatible polylactic acid fire retardant

A polylactic acid and compatibility technology, applied in the field of preparation of compatible polylactic acid flame retardants, can solve problems such as poor compatibility and poor heat resistance, and achieve the effects of rapid synthesis, easy product and simple process

Inactive Publication Date: 2014-02-05
SOUTH CHINA NORMAL UNIVERSITY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Small-molecule flame retardants that have been used in PLA blends mainly include nitrogen-based flame retardants such as metal hydroxides, phosphates, and melamine [Zhan J, Song L, Nie S B, Hu Y. Polym Degrad Stab, 2009 , 94(3): 291-296; Matsuno Y, Mitsunaga M, Oda J, Doteguchi M, Shibata Y, Kitamura T, Toyohara K, Iwai M. JP 2010111737, 2010-05-20; Matsuno Y, Mitsunaga M, Oda N, Doteguchi M, Kitamura T, Toyohara K. JP 2011032432, 2011-02-17], and halogenated flame retardants, which are generally rich in resources, many in variety, and low in price, but poor in heat resistance and compatibility

Method used

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  • Preparation method of compatible polylactic acid fire retardant
  • Preparation method of compatible polylactic acid fire retardant

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0030] Using D, L-LA, o-phenylenediamine analogue F (that is, biphenyltetramine, see the aforementioned structural formula F) as raw materials, according to the ratio of substances n (D,L-LA): n (Biphenyltetramine) = 200:1 mixed evenly, after 120°C, 4000Pa, 5h of pre-polymerization and water removal treatment to obtain intermediate I, adding catalyst zinc oxide (0.5% by mass of intermediate I), at temperature Melt polycondensation at 160°C and pressure 70Pa for 5h. After the reaction, the product was dissolved in chloroform at normal temperature, purified by methanol precipitation, and vacuum-dried to obtain a white powdery benzimidazole-based compatible polylactic acid flame retardant. The structure of the polymer was confirmed by infrared spectroscopy (see figure 1 ), H NMR spectrum (see figure 2 ), gel permeation chromatography and other polymer characterization methods confirmed that the intrinsic viscosity [η] is 0.5049 dL / g, and the nitrogen-containing compatible pol...

Embodiment 2

[0036] Using D, L-LA, o-phenylenediamine analogue E (see the aforementioned structural formula E) as raw materials, according to the ratio of substances n (D,L-LA): n (o-phenylenediamine analogue E) = 160:1 mixed evenly, after prepolymerization at 140°C, 4000Pa, 8h to get intermediate I, add catalyst stannous oxide (mass percentage is 0.7% of intermediate I ), control the temperature at 160°C and the pressure at 80Pa, and react for 6h. After the reaction, the product was dissolved in chloroform, purified by methanol precipitation, and vacuum-dried to obtain a white powdery benzimidazole-based compatible polylactic acid flame retardant. In the same way as in Example 1, the structure of the polymer is confirmed by polymer characterization methods such as infrared spectroscopy, hydrogen nuclear magnetic resonance spectroscopy, and gel permeation chromatography. The intrinsic viscosity [η] is 1.0977 dL / g, and the nitrogen-containing base phase synthesized by this method The cap...

Embodiment 3

[0038] Take L-LA, o-phenylenediamine D 1 (R 2 = H, see the aforementioned structural formula D) as raw material, according to the ratio of substance n (L-LA): n (o-phenylenediamine D 1 ) = 50:1 mixed evenly, after 130°C, 4000Pa, 10h of pre-polymerization treatment to remove water, intermediate I was obtained, and the catalyst stannous octoate (0.5% by mass of intermediate I) was added at a temperature of 165°C and a pressure of 90Pa Next, melt polycondensation for 3h. After the reaction, the product is dissolved, precipitated and purified, and vacuum-dried to obtain a white powdery benzimidazole-based compatible polylactic acid flame retardant. In the same way as in Example 1, the structure of the polymer is confirmed by polymer characterization methods such as infrared spectroscopy, hydrogen nuclear magnetic resonance spectroscopy, and gel permeation chromatography. The intrinsic viscosity [η] is 0.6842 dL / g, and the nitrogen-containing base phase synthesized by this me...

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Abstract

The invention relates to a preparation method of a compatible polylactic acid fire retardant, which adopts amino compounds and lactic acid as raw materials, and synthesizes nitrogen-based polylactic acid with fire retardant performance through a simple and practical direct melt polymerization method; the invention provides a synthetic route of the compatible nitrogen-based polylactic acid fire retardant for the first time, and preferably selects technical conditions such as the polymerization monomer ratio, the polymerization temperature and time, the catalyst, and the like; the operation is simple; the prepared compatible polylactic acid fire retardant can be used in the polylactic acid fire retardant processing of biodegradable materials, facilitates the low-cost synthesis of biodegradable polymers and the wide applications of fire retardant processing in related fields.

Description

technical field [0001] The invention relates to a preparation method of a flame retardant, in particular to a preparation method of a compatible polylactic acid flame retardant which can be used for flame retardant processing of biodegradable material polylactic acid. Background technique [0002] Biodegradable material Polylactic acid (PLA) is a non-toxic, fully biodegradable polymer synthesized from lactic acid (LA), which has good mechanical properties, biocompatibility, etc. However, PLA itself has poor thermal stability and flame retardant properties. There is only UL-94 HB grade, the limiting oxygen index (LOI) is 20%, and there is a droplet phenomenon when burning. With the increasing application of PLA in textiles, packaging, daily necessities, electronic appliances, automobiles, aviation and other fields, it is imminent to modify it for flame retardancy. [0003] Usually, the flame retardant modification of PLA is mainly realized by physical blending. The flame re...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08G63/685
Inventor 汪朝阳熊金锋
Owner SOUTH CHINA NORMAL UNIVERSITY
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