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Preparation method and application of lignin-based intumescent flame retardant

An intumescent flame retardant, lignin-based technology, applied in the field of flame retardant preparation technology and polymer material modification, can solve the problems of easy precipitation, poor compatibility of matrix materials, poor thermal stability and mechanical strength, etc. Achieve the effect of good compatibility, good flame retardancy and improved mechanical properties

Active Publication Date: 2015-02-25
NANJING FORESTRY UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

In the prior art, there is little research and development of lignin-based flame retardants. Some people use phosphorus oxychloride and imidazole to react with lignin to prepare lignin-based flame retardants. However, phosphorus oxychloride is highly toxic and the reaction conditions are very strict. Harsh and expensive raw materials, it is difficult to have industrial application value
[0005]Biopolyester P(3,4)HB is a degradable polyester material, which is very flammable and has poor thermal stability and mechanical strength. Commonly used APP flame retardants, etc., are difficult to play a good flame retardant effect on P(3,4)HB materials. Usually, the matrix material has begun to degrade before the flame retardant is degraded during combustion, and ordinary APP flame retardants generally have the problem of poor compatibility with matrix materials and easy precipitation

Method used

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  • Preparation method and application of lignin-based intumescent flame retardant
  • Preparation method and application of lignin-based intumescent flame retardant
  • Preparation method and application of lignin-based intumescent flame retardant

Examples

Experimental program
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Effect test

Embodiment 1

[0029] Add 10g of lignin and 70mL of DMF into a reaction kettle equipped with a stirring device and a reflux device, stir and dissolve, add 15g of phosphorus pentoxide, and react at 100°C for 2 hours; dissolve 26.6g of melamine in 54mL of DMF and add to the above reaction system During the process, the temperature was raised to 130°C, the reaction was continued for 5 hours, and then the reaction was stopped. After the reaction kettle was cooled to room temperature, after washing and suction filtration, the filter cake was dried at 60°C for 24 hours to obtain 45.7 g of a brown powder product. Yield 88.6%.

Embodiment 2

[0031] Add 10g of lignin and 60mL of DMF into a reaction kettle equipped with a stirring device and a reflux device, stir and dissolve, add 20g of phosphorus pentoxide, and react at 120°C for 3 hours; dissolve 29.3g of melamine in 62mL of DMF and add to the above reaction system During the process, the temperature was raised to 130°C, the reaction was continued for 3 hours, and then the reaction was stopped. After the reaction kettle was cooled to room temperature, after washing and suction filtration, the filter cake was dried at 60°C for 24 hours to obtain 54.2 g of a brown powder product. Yield 91.4%.

Embodiment 3

[0033] Add 10g of lignin and 75mL of DMSO into a reaction kettle equipped with a stirring device and a reflux device, stir and dissolve, add 25g of phosphorus pentoxide, and react at 120°C for 3 hours; dissolve 22.2g of melamine in 55mL of DMSO and add to the above reaction system During the process, the temperature was raised to 120°C, the reaction was continued for 3 hours, and then the reaction was stopped. After the reaction kettle was cooled to room temperature, after washing and suction filtration, the filter cake was dried at 60°C for 24 hours to obtain 50.8 g of a brown powder product. Yield 88.8%.

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Abstract

The invention discloses a preparation method of a lignin-based intumescent flame retardant. The preparation method comprises the steps of carrying out esterification reaction on phosphoric anhydride and lignin through optimizing reaction temperature, reaction time, reactant ratio and solvent selecting ratio and other process conditions; then, enabling the reaction product to react with melamine to obtain the lignin-based intumescent flame retardant which is integrated with an acid source, a carbon source and an air source and is high in char formation quantity and good in flame retardance. When the lignin-based intumescent flame retardant is independently applied to a P(3,4)HB biopolyester material or is applied to the P(3,4)HB biopolyester material after being compounded with other flame retardants, the compatibility of the lignin-based intumescent flame retardant and a matrix is good, so that the flame retardance of the material can be remarkably improved, meanwhile, the mechanical property of the material can also be improved, and a P(3,4)HB flame-retardant composite material with excellent comprehensive properties can be prepared. By using the preparation method disclosed by the invention, the yield is high; a reactant is basically nontoxic; the process conditions are easy to control; the operation process is simple; the lignin serving as a main raw material is an abundant regenerative resource, so that the price is low; and therefore, the lignin-based intumescent flame retardant is favorable in application prospect.

Description

technical field [0001] The invention belongs to the field of flame retardant preparation technology and polymer material modification technology, and specifically relates to a preparation method of a lignin-based intumescent flame retardant, and the flame retardant alone or compounded with other flame retardants in poly( 3-hydroxybutyrate-co-4-hydroxybutyrate) [P(3,4)HB] material application. Background technique [0002] With the increasing application range of polymer materials and the increasing awareness of global safety and environmental protection, people have higher and higher requirements for flame retardancy of polymer material products. Halogen-free, low toxicity, low smoke, and high heat resistance environmental resistance Combustion agent has begun to become the target that people pursue. [0003] Intumescent flame retardants (IFR) originated in the 1930s and are mainly composed of three parts, namely acid sources (mainly phosphorus-containing compounds), gas so...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08H7/00C08L67/04C08L97/00
Inventor 张蕤王坚剑苏天翔
Owner NANJING FORESTRY UNIV
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