A polylactic acid/starch intumescent flame-retardant composite material and its preparation method

A technology of intumescent flame retardant and composite material, which is applied in the field of polylactic acid/starch intumescent flame retardant composite material and its preparation, and can solve the problems of poor compatibility between starch and matrix plastic, poor thermal stability of starch, and inability to meet application requirements. , to achieve the effect of promoting carbon forming ability, high phosphorus content and high phosphorus content

Active Publication Date: 2019-02-15
NINGBO INST OF MATERIALS TECH & ENG CHINESE ACADEMY OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

At present, there are many reports on the application of natural starch in plastics such as polylactic acid and polypropylene, but there are obvious defects: first, the thermal stability of starch is not good, it is easy to degrade during processing, and yellowing occurs, resulting in unsightly products. Beautiful; Secondly, the compatibility between starch and base plastic is very poor, which limits the filling amount of starch, and the mechanical properties of the material are very poor, which cannot meet the requirements of practical applications

Method used

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  • A polylactic acid/starch intumescent flame-retardant composite material and its preparation method
  • A polylactic acid/starch intumescent flame-retardant composite material and its preparation method
  • A polylactic acid/starch intumescent flame-retardant composite material and its preparation method

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0061] In a 250mL three-necked flask, 20g of 9,10-dihydro-9-oxa-10-phosphaphenanthrene-10-oxide (DOPO) and 15g of maleic anhydride (MA) were dissolved in 50mL of toluene and 20mL of dioxygen Hexacyclic, heated to 40 ° C, nitrogen protection, reflux reaction for 12 hours. After the reaction, the solvent was removed by rotary evaporation, and the product 1 was obtained after vacuum drying, which was set aside.

[0062] In a 250mL three-necked flask, 20g of starch (corn starch) and 40mL of pyridine were heated to 65°C and refluxed for 2h under nitrogen protection. After the temperature dropped to 50°C, 20g of the product 1 (dissolved in DMSO) was added to the catalyst 4-dimethylaminopyridine, protected by nitrogen, and refluxed at 50°C for 12h. After the reaction is finished, it is washed, purified, and vacuum-dried to obtain bio-based phosphorus-containing starch, ie, modified starch.

Embodiment 2

[0064] In a 250mL three-necked flask, 20g DOPO and 18g maleic anhydride (MA) were respectively dissolved in 50mL xylene and 20mL THF (tetrahydrofuran), heated to 50°C, under nitrogen protection, and refluxed for 24h. After the reaction, the solvent was removed by rotary evaporation, and the product 1 was obtained after vacuum drying, which was set aside.

[0065] In a 250mL three-necked flask, 20g of starch (corn starch) and 60mL of pyridine were heated to 75°C and refluxed for 4h under nitrogen protection. After the temperature dropped to 50°C, 25g of the product 1 (dissolved in DMSO) was added to the catalyst 4-dimethylaminopyridine, protected by nitrogen, and refluxed for 24h. After the reaction is finished, it is washed, purified, and vacuum-dried to obtain bio-based phosphorus-containing starch, ie, modified starch.

Embodiment 3

[0067] In a 250mL three-necked flask, 20g DOPO and 21g maleic anhydride (MA) were dissolved in 70mL xylene, heated to 60°C, under nitrogen protection, and refluxed for 24h. After the reaction, the solvent was removed by rotary evaporation, and the product 1 was obtained after vacuum drying, which was set aside.

[0068] In a 250mL three-necked flask, 20g of starch (corn starch) and 80mL of pyridine were heated to 85°C and refluxed for 8h under nitrogen protection. After the temperature dropped to 65°C, 35g of the product 1 (dissolved in DMSO) was added to the catalyst 4-dimethylaminopyridine, protected by nitrogen, and refluxed for 24h. After the reaction is finished, it is washed, purified, and vacuum-dried to obtain bio-based phosphorus-containing starch, ie, modified starch.

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Abstract

The invention discloses a polylactic acid / starch expansion flame-resistant composite material with excellent flame resistance, and a preparation method thereof. The polylactic acid / starch expansion flame-resistant composite material is composed of, by weight, 60 to 89% of polylactic acid, 5 to 30% of an acid source, 5 to 30% of a modified starch, and 1 to 15% of a gas source. In a preferred embodiment, the modified starch is phosphorized maleic anhydride grafting modified starch (bio-based phosphorus containing starch). According to the preparation method, polylactic acid possesses excellent compatibility with the modified starch; synergistic effect of the acid source, the carbon source (the modified starch), and the gas source is capable of improving charring forming capability of the polylactic acid matrix, and improving high temperature stability and flame resistance of polylactic acid greatly. According to the preparation method, adoption of an existing double-screw extruder is enough for production; preparation is simple and convenient; and the preparation method is convenient for industrial production.

Description

technical field [0001] The invention relates to the technical field, in particular to a polylactic acid / starch swelling flame-retardant composite material and a preparation method thereof. Background technique [0002] With the increasingly severe environmental problems and the oil crisis, people's research on sustainable materials has gradually increased. Bio-based materials, as fully biodegradable green materials, fully meet the current development needs and have received widespread attention. Among them, polylactic acid (PLA), as the bioplastic with the most development potential, has excellent mechanical properties and good processing performance, and is widely used in the automotive industry, electrical facilities and other fields. However, its flammability has greatly limited its promotion in these fields. At present, due to the advantages of low toxicity, environmental protection and smoke suppression, intumescent flame retardant has replaced the traditional halogen-...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08L67/04C08L3/06C08K3/32C08K5/3492C08B31/04
CPCC08B31/04C08L67/04C08L2201/02C08L2201/08C08L3/06C08K2003/323C08K5/34922
Inventor 孙晋皓汤兆宾朱锦
Owner NINGBO INST OF MATERIALS TECH & ENG CHINESE ACADEMY OF SCI
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