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Bio-based flame-retardant magnolol epoxy monomer, preparation method thereof and application of monomer in flame-retardant epoxy resin

An epoxy resin, bio-based technology, applied in the field of polymer chemistry, can solve the problem of relatively little research on flame retardant properties, and achieve the effects of simple and efficient curing process, low usage, and high biological safety.

Active Publication Date: 2021-06-01
NANJING UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] In recent years, the preparation of bio-based epoxy resins has been developed rapidly, but there are relatively few studies on their flame retardant properties as a whole.

Method used

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  • Bio-based flame-retardant magnolol epoxy monomer, preparation method thereof and application of monomer in flame-retardant epoxy resin
  • Bio-based flame-retardant magnolol epoxy monomer, preparation method thereof and application of monomer in flame-retardant epoxy resin
  • Bio-based flame-retardant magnolol epoxy monomer, preparation method thereof and application of monomer in flame-retardant epoxy resin

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0077] Embodiment 1: Preparation of bio-based flame retardant magnolol epoxy monomer:

[0078] First, add magnolol (9.98g, 37.5mmol) and sodium hydride (1.98g, 82.5mmol) successively in a clean three-necked flask, and add excess tetrahydrofuran (200mL) under ice bath to fully dissolve it, and the reaction system Filled with nitrogen and kept stirring under ice bath conditions for 15min, slowly added diphenylphosphinoyl chloride (19.52g, 82.5mmol) with a 50mL syringe, stirred at room temperature for 3h, when the reaction was complete, mixed ethyl acetate and deionized water Add the solution with a volume ratio of 1:1 (each 60 mL) into the reaction solution cooled in an ice bath, let it stand for 30 minutes, add a small amount of saturated saline, extract the reaction solution with ethyl acetate, combine the organic phases, and dry over anhydrous sodium sulfate The organic phase was filtered and distilled under reduced pressure to obtain the crude product of intermediate DBDBD; ...

Embodiment 2

[0081] Take by weighing DGEBA monomer (0.1g, 0.29mmol) in the sample bottle, epoxy resin monomer BOBDB (0.037g, 0.053mmol), promptly the P element content accounts for 2wt% of reaction system gross mass in the epoxy resin monomer BOBDB, Introduce nitrogen to remove oxygen components, add menthanediamine (0.025g, 0.145mmol) under nitrogen atmosphere, further remove air, heat up to 55°C to melt the two (melting process is transparent and uniform) and mix well , Cured at 200°C for 3h to obtain light yellow transparent epoxy resin polymer. Micro-combustion calorimetry (MCC) experiment results show that the maximum heat release rate is 431.95W / g.

Embodiment 3

[0083] Take by weighing DGEBA monomer (0.1g, 0.29mmol) in the sample bottle, epoxy resin monomer BOBDB (0.11g, 0.016mmol), promptly the P element content accounts for 4wt% of reaction system gross mass in the epoxy resin monomer BOBDB, Introduce nitrogen to remove oxygen components, add menthanediamine (0.025g, 0.145mmol) under nitrogen atmosphere, further remove air, heat up to 65°C to melt the two (melting process is transparent and uniform) and mix well , 200 ° C curing, curing 3h, to obtain light yellow transparent epoxy resin polymer. Micro-combustion calorimetry (MCC) experiment results show that the maximum heat release rate is 303.24W / g.

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Abstract

The invention discloses a bio-based flame-retardant magnolol epoxy monomer, a preparation method thereof and application of the monomer in flame-retardant epoxy resin. The preparation method of the bio-based flame-retardant magnolol epoxy monomer comprises the following steps: (1) stirring a mixed solution of magnolol, sodium hydride and tetrahydrofuran under the protection of inert gas, and reacting an obtained mixture with diphenyl phosphinyl chloride to obtain an intermediate as shown in a formula II; and (2) reacting the solution of the intermediate as shown in the formula II with m-chloroperoxybenzoic acid to obtain the bio-based flame-retardant magnolol epoxy monomer as shown in the formula I. The bio-based flame-retardant magnolol epoxy monomer as shown in the formula I is prepared for the first time, is a novel bio-based phosphorus-containing epoxy structure, is also a good flame-retardant aid, is low in use amount, has excellent compatibility in epoxy resin, is free of phosphorus removal after participating in curing, is high in safety and has great market application value.

Description

technical field [0001] The invention belongs to the field of polymer chemistry, and in particular relates to a bio-based flame-retardant magnolol epoxy monomer, a preparation method and an application in flame-retardant epoxy resin. Background technique [0002] Bio-based polymer materials mainly use some natural renewable resources such as starch, protein, cellulose, chitin, and vegetable oil as starting materials, and pay attention to the biological origin and renewability of raw materials. It includes both degradable or compostable plastics and non-degradable plastics; both thermoplastics and thermosetting resins. This type of polymer material uses renewable resources as the main raw material, while reducing dependence on petrochemical products, it also reduces CO 2 It is an important development direction of current polymer materials. At present, the research on bio-based polymer materials is mainly limited to some natural polymers or thermoplastic materials such as st...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07F9/655C08G59/30C08G59/22C08G59/50
CPCC07F9/65505C08G59/304C08G59/226C08G59/5026
Inventor 郭凯张杰孟晶晶
Owner NANJING UNIV OF TECH
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