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Preparation and application methods of lignin-based flame retardant

A technology based on lignin and an application method is applied in the field of preparing lignin-based flame retardant polyurethane, which can solve the problems of small impact on material mechanical properties, human health and environmental hazards, etc., and achieves improved compatibility, good impact resistance, and mechanical properties. The effect of improved performance

Active Publication Date: 2017-10-13
CHANGCHUN UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Traditional halogen-based flame retardants have the advantages of good flame-retardant effect, low addition amount, and little impact on the mechanical properties of materials. However, when halogen-based flame retardants burn, they will release a large amount of toxic gases, which will cause great harm to human health and the environment. hazards, so halogenated flame retardants have been banned

Method used

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  • Preparation and application methods of lignin-based flame retardant
  • Preparation and application methods of lignin-based flame retardant
  • Preparation and application methods of lignin-based flame retardant

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0035] (1) Preparation of phosphorus-containing lignin-based flame retardant

[0036] Weigh 1.36g of lignin, disperse it in 2ml of N,N-dimethylformamide (DMF), stir to disperse the lignin evenly, then add 4.2g of hexamethylene diisocyanate (HDI) and stir until it is evenly dispersed , put it into an oil bath at 80°C and keep stirring, react for 12 minutes until the system becomes viscous, set the oil bath temperature to 125°C, add 21.6g DOPO, continue stirring for 20 minutes until the system is viscous, take out the reaction product, and dry it at 80°C 12 hours, pulverized to obtain phosphorus-containing lignin-based flame retardant L5-2, its FTIR characterization results are as follows figure 1 shown.

[0037] (2) Preparation of flame retardant polyurethane

[0038] Add 15ml of N,N-dimethylformamide (DMF), 10g of polyethylene glycol (PEG200), and 10g of hexamethylene diisocyanate (HDI) into a 250ml three-necked flask, and stir until uniform. Put it in an oil bath, react at...

Embodiment 2

[0040] (1) Preparation of phosphorus-containing lignin-based flame retardant

[0041] Weigh 1.43g of lignin and disperse it in 3ml of N,N-dimethylformamide (DMF). Stir to disperse the lignin evenly. Then add 5.55g of hexamethylene diisocyanate (HDI) and stir until dispersed. Evenly, put it in an oil bath at 80°C and keep stirring, react for 15 minutes until the system becomes viscous, set the temperature of the oil bath at 125°C, add 21.6g DOPO, continue stirring for 12 minutes until the system is viscous, take out the reaction product, and bake at 80°C Dry for 24 hours and pulverize to obtain phosphorus-containing lignin-based flame retardant L5-1.5, and its FTIR characterization results are as follows: figure 1 shown.

[0042] (2) Preparation of flame retardant polyurethane

[0043] Add 15ml of N,N-dimethylformamide (DMF), 10g of polyethylene glycol (PEG200), and 10g of hexamethylene diisocyanate (HDI) into a 250ml three-necked flask, and stir until uniform. Put it in an ...

Embodiment 3

[0045] (1) Preparation of phosphorus-containing lignin-based flame retardant

[0046] Weigh 1.58g of lignin and disperse it in 4ml of N,N-dimethylformamide (DMF). Stir to disperse the lignin evenly, then add 8.41g of hexamethylene diisocyanate (HDI) and stir until evenly dispersed. , placed in an oil bath at 80°C and continuously stirred, and reacted for 18 minutes. When the system becomes viscous, set the oil bath temperature to 120°C, add 21.6g DOPO, continue to react for 12 minutes and stir until the system is viscous, take out the reaction product, dry at 80°C for 20 hours, and pulverize to obtain phosphorus-containing lignin-based flame retardant L5- 1. The FTIR characterization results are as follows figure 1 shown.

[0047] (2) Preparation of flame retardant polyurethane

[0048] Add 15ml of N,N-dimethylformamide (DMF), 10g of polyethylene glycol (PEG200), and 10g of hexamethylene diisocyanate (HDI) into a 250ml three-necked flask, and stir until uniform. Put it in ...

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Abstract

The invention provides preparation and application methods of a lignin-based flame retardant, and relates to a flame retardant. The flame retardant is prepared from the following raw materials: lignin, isocyanate, 9,10-dihydro-9-oxa-phenanthrene-10-oxide (DOPO). The preparation method specifically comprises the following steps: performing reaction on the lignin and the isocyanate at certain temperature; performing reaction with the DOPO at certain temperature; finally, drying the obtained product in a vacuum drying box, and smashing the product, thus obtaining the flame retardant. According to the flame retardant, hydroxyl on the lignin is reacted with the isocyanate; meanwhile, with a phosphate structure, the flame retardant has a good flame retarding effect; benzene ring structures contained in the lignin and the DOPO can enhance the mechanical property of the material. The invention further provides a preparation method of flame retarding polyurethane. The method comprises the steps of performing reaction on polyatomic alcohol and the isocyanate at certain temperature till the system is sticky, adding the phosphorus-containing lignin-based flame retardant and other auxiliaries, and performing thermal curing and molding. The obtained flame retarding polyurethane can be used as an adhesive, a coating, a foaming material, a terrace coating material and the like.

Description

technical field [0001] The invention belongs to the technical field of preparation and application of organic phosphine flame retardants, and in particular relates to the preparation of a phosphorus-containing lignin-based flame retardant and its application in polyurethane to prepare lignin-based flame-retardant polyurethane. Background technique [0002] Lignin is bound together with cellulose and hemicellulose to form the main support structure of plants. It is the second most abundant natural polymer material in the plant kingdom after cellulose and the only natural polymer material containing an aromatic ring structure. Lignin is a three-dimensional network polymer connected by carbon-carbon bonds and ether bonds with phenylpropane as the structural unit; according to the number and position of methoxy groups, it can be divided into p-hydroxyphenyl type (H), Guaiac-based (G) and syringyl-based (S). Due to its natural renewable, biodegradable, non-toxic and other advant...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G18/64C08G18/65C08G18/32C08G18/73C08L75/04
CPCC08G18/3206C08G18/6492C08G18/65C08G18/73C08L75/04
Inventor 呼微张玉美韩爽闫茹赵麒倪闯将张明耀
Owner CHANGCHUN UNIV OF TECH
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