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A kind of bio-based flame retardant magnolol epoxy monomer and its preparation method and application in flame retardant epoxy resin

An epoxy resin and bio-based technology, applied in the field of polymer chemistry, can solve the problems of relatively few studies on flame retardancy, and achieve the effect of simple and efficient curing process, wide sources, and high compatibility

Active Publication Date: 2021-10-22
NANJING TECH UNIV
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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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  • A kind of bio-based flame retardant magnolol epoxy monomer and its preparation method and application in flame retardant epoxy resin
  • A kind of bio-based flame retardant magnolol epoxy monomer and its preparation method and application in flame retardant epoxy resin
  • A kind of bio-based flame retardant magnolol epoxy monomer and its preparation method and application in flame retardant epoxy resin

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0077] Example 1: Biologically flame retardant phenol epoxy monomer system:

[0078] First, in a clean three-neck bottle, a thick mougol (9.98 g, 37.5 mmol), sodium hydride (1.98 g, 82.5 mmol), add excess tetrahydrofuran (200 ml) under ice bath, so that it is fully dissolved and responding system The mixture was filled with nitrogen and held under ice bath for 15 min, slowly added diphenyl phosphon chloride (19.52 g, 82.5 mmol), stirring at room temperature for 3 h, and at room temperature, ethyl acetate and deionized water The solution ratio of 1: 1 (60 mL) was added to the reaction solution cooled under an ice bath, allowed for 30 min, add a small amount of saturated brine, ethyl acetate extraction reaction liquid, combined with organic phase, sodium anhydrous sodium sulfate Organic phase, filtration, discharilization of intermediate DBDBD; elution crude eluting elution (PE: EA, 2 / 1 to 1 / 2) using silica gel column chromatography (PE: EA, 2 / 1 to 1 / 2), and finally gave a white int...

Embodiment 2

[0081] DGEBA monomers (0.1 g, 0.29 mmol), epoxy resin monomer BOBDB (0.037 g, 0.053 mmol), that is, 2% by weight of the total mass of the reaction system in the epoxy monomer BOBDB (0.037 g, 0.053 mmol), i.e. After nitrogen, after removal of oxygen components, the nitrogen atmosphere is added, and Menganentalamine (0.025 g, 0.145 mmol) is added, and the air is further removed, and the temperature is warmed to 55 ° C, which is melted (the molten process is transparently one) and mixed uniform , Cured from 200 ° C for 3 h to give a pale yellow transparent epoxy polymer. The minimum thermal release rate of the micro-combustion amount heat method (MCC) experiment was 431.95 W / g.

Embodiment 3

[0083] DGEBA monomers (0.1 g, 0.29 mmol), epoxy resin monomer BOBDB (0.11 g, 0.016 mmol), i.e., the epoxy monomer BOBDB (0.11 g, 0.016 mmol), that is, 4% by weight of the total mass of the C element in the epoxy resin monomer BOBDB, After nitrogen, after removal of the oxygen component, the nitrogen atmosphere is perhemened, and Menganentalamine (0.025 g, 0.145 mmol) is added, and the air is further removed, and the temperature is increased to 65 ° C to make both melt (molten transparent uniform) and mix well Curing from 200 ° C, cured 3 h, resulting in a pale yellow transparent epoxy resin polymer. The minimum thermal release rate of the experimental results of the micro-combustion amount (MCC) experiment was 303.24 W / g.

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Abstract

The invention discloses a bio-based flame-retardant magnolol epoxy monomer, a preparation method and an application in flame-retardant epoxy resin. The preparation method of the bio-based flame-retardant magnolol epoxy monomer comprises the following steps: (1) stirring the mixed solution of magnolol, sodium hydride and tetrahydrofuran under the protection of an inert gas; Acyl chloride reaction, obtains the intermediate shown in formula II; (2) the solution of intermediate shown in formula II is reacted with m-chloroperoxybenzoic acid, obtains the bio-based flame-retardant magnolol epoxy resin shown in formula I monomer. The invention prepared the bio-based flame-retardant magnolol epoxy monomer shown in formula I for the first time, which is a new type of bio-based phosphorus-containing epoxy structure, and is also a good flame-retardant additive with low usage. At the same time, It has excellent compatibility in epoxy resin, no phosphorous removal after participating in curing, high safety, and great market application value.

Description

Technical field [0001] The present invention belongs to the field of polymer chemistry, and more particularly to a biologically flame-fired phenolic oxygen monomer and a preparation method and an application in flame retardant epoxy resin. Background technique [0002] Biological high molecular materials are mainly based on starch, protein, cellulose, chin, vegetable oils, etc. It includes both degradable or compost of plastics, including non-degradation plastics; or both thermoplastic materials, but also a thermosetting resin. Such polymer materials are mainly raw materials in renewable resources, while reducing the dependence on petrochemical products, it also reduces CO 2 Emissions are an important development direction of current polymer materials. At present, research on biological high molecular materials is mainly limited to starch plastics, cellulose-based materials, bioeramics, etc., some natural polymers or thermoplastic materials, and relatively small for biological th...

Claims

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Application Information

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