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High-effective bio-based flame-retarding agent containing furan ring, and synthesis method and application of the flame-retarding agent

A furan ring and bio-based technology, which is applied in the field of high-efficiency furan ring-containing bio-based flame retardants and their synthesis, can solve the problems of low flame retardant efficiency, high toxicity, and environmental hazards, and achieve high flame retardant efficiency and improved mechanical properties. , the effect of high purity

Active Publication Date: 2019-01-29
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

[0004] One purpose of the present invention is to solve the problems of traditional flame retardants such as dependence on petrochemical resources, low flame retardant efficiency, high toxicity, and environmental hazards. Bio-based flame retardants are prepared by combining bio-based materials with flame-retardant element phosphorus, providing A high-efficiency bio-based flame retardant containing furan ring

Method used

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  • High-effective bio-based flame-retarding agent containing furan ring, and synthesis method and application of the flame-retarding agent
  • High-effective bio-based flame-retarding agent containing furan ring, and synthesis method and application of the flame-retarding agent
  • High-effective bio-based flame-retarding agent containing furan ring, and synthesis method and application of the flame-retarding agent

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0051] 1) In a 250mL three-necked round-bottomed flask equipped with magnetic stirring, disperse 0.30mol of methylfurylamine and 0.40mol of triethylamine into 100ml of acetonitrile solution and stir evenly;

[0052] 2) Add 0.10mol of phosphorus oxychloride to 50mL of acetonitrile solution and stir evenly;

[0053] 3) Slowly drop the acetonitrile solution containing phosphorus oxychloride into the acetonitrile solution containing furanmethylamine and triethylamine in an ice-water bath and nitrogen atmosphere with a constant pressure dropping funnel, and the dropping time is controlled within 2 hours. After the dropwise addition, react at room temperature for 2 h, then raise the temperature to 50° C. and continue to react for 6 h.

[0054] 4) After the reaction, remove the white precipitate by filtration, remove the solvent by rotary evaporation, add ethyl acetate for dissolution, wash 5 times with deionized water, and remove the ethyl acetate by rotary evaporation to obtain a y...

Embodiment 2

[0059] In an ice-water bath and a nitrogen atmosphere, add 0.30 mol of methylfuranamine and 0.60 mol of triethylamine in chloroform to a 250 mL three-necked round-bottomed flask equipped with magnetic stirring. After stirring evenly, use a constant pressure dropping funnel to The chloroform solution of 0.50mol phosphorus oxychloride was slowly dropped into the flask, and the dropping time was controlled at 0.5h. After the dropwise addition, react at room temperature for 4 h, then raise the temperature to 80° C. and continue to react for 4 h. After the reaction was completed, it was washed with deionized water for 5 times, and the solvent was removed by rotary evaporation to obtain a light yellow solid product, the structural formula of which was shown in Formula 1.

Embodiment 3

[0061] In an ice-water bath and a nitrogen atmosphere, add 0.30 mol of furan methanol and 0.30 mol of pyridine in a 1,4-dioxane solution into a 250 mL three-neck round bottom flask equipped with magnetic stirring. The 1,4-dioxane solution of phosphorus oxychloride (0.1mol) was slowly dropped into the flask through the funnel, and the dropping time was controlled at 1.5h. After the dropwise addition, react at room temperature for 2 h, then raise the temperature to 50° C. and continue to react for 6 h.

[0062] After the reaction, the white precipitate was removed by filtration, the solvent was removed by rotary evaporation, washed 5 times with deionized water, and vacuum-dried to obtain the dark brown target product, whose structural formula is shown in formula 2:

[0063]

[0064] The compound prepared above can prove that the structure shown in the above formula has been obtained by proton nuclear magnetic spectrum, phosphorous nuclear spectrum and infrared spectrum. The ...

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Abstract

The invention discloses a high-effective bio-based flame-retarding agent containing furan ring, and a synthesis method and an application of the flame-retarding agent. In the invention, with a bio-based compound containing furan ring and a phosphorus-containing compound being raw materials, the bio-based flame-retarding agent containing furan ring is prepared under protection by inert gas. The flame-retarding agent is very low in influence on thermo-stability of a resin matrix and can effectively improve crystallization property of the resin matrix, thereby improving mechanical strength and modulus of the material. When being applied to polymers, the flame-retarding agent has outstanding flame-retarding effect and can achieve flame retarding just by a less addition amount. The flame-retarding agent can alleviate thermal performance loss of a flame-retarding composite material and significantly improve crystallization and increase crystallization speed of the polymer matrix, thus significantly enhancing mechanical performance of the composite material. The flame-retarding agent can catalyze degradation of polylactic acid mainly in the manner of breaking molecular chains to form low-molecular-weight oligomers, then heat generated during combustion is released in the form of molten drops, thus achieving the flame retarding object.

Description

technical field [0001] The invention relates to the technical field of flame retardant synthesis and application, in particular to a high-efficiency furan ring-containing bio-based flame retardant and its synthesis method and application. Background technique [0002] Due to their excellent performance, polymer materials are widely used in the fields of electronic communication, construction industry, machinery manufacturing, aerospace and daily life. However, polymer materials are mostly flammable due to their own structure and other factors, which can easily cause fires and cause heavy losses of personal property. Therefore, the development and research of flame retardants for polymer materials is imminent. [0003] At present, the development and application of flame retardants have been greatly developed, and a variety of flame retardant technologies have been formed. The development of early flame retardants was mainly based on the development of inorganic flame retar...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08K5/5377C08L67/04C07F9/655C07F9/6574
CPCC07F9/65515C07F9/657172C08K5/5377C08L2201/02C08L67/04
Inventor 李娟孙晋皓
Owner NINGBO INST OF MATERIALS TECH & ENG CHINESE ACADEMY OF SCI
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