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Vanillin-based high-heat-resistant flame-retardant epoxy resin rich in benzene rings and its preparation method and application

A technology of epoxy resin and vanillin, which is applied in the field of high heat-resistant and high-efficiency flame-retardant epoxy resin, its preparation, and the field of flame-retardant epoxy resin, can solve the problems of comprehensive performance such as heat resistance to be improved, and achieve industrialization Large-scale production, good controllability, and the effect of overcoming poor thermal stability

Active Publication Date: 2019-09-27
NINGBO INST OF MATERIALS TECH & ENG CHINESE ACADEMY OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

For example, a class of vanillin-based phosphorus-containing flame-retardant epoxy resins developed by the inventors of this case has also been reported, which has shown good flame-retardant properties, but its comprehensive properties such as heat resistance (glass transition temperature and Thermal stability) still needs to be improved

Method used

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  • Vanillin-based high-heat-resistant flame-retardant epoxy resin rich in benzene rings and its preparation method and application
  • Vanillin-based high-heat-resistant flame-retardant epoxy resin rich in benzene rings and its preparation method and application
  • Vanillin-based high-heat-resistant flame-retardant epoxy resin rich in benzene rings and its preparation method and application

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Embodiment example

[0039] Wherein, as a more specific embodiment of the present invention, the preparation method may include the following steps:

[0040] (1) Mix 100 parts by mass of vanillin, 10 to 100 parts by mass of diamine compounds, 20 to 300 parts by mass of phosphine reagent and 0 to 15 parts by mass of catalyst in 50 to 500 parts by mass of organic solvent. ℃ reaction for 0.5 to 24 hours, after the reaction is completed, distill, wash, dry and remove the solvent to obtain the phosphorus-containing bisphenol with vanillin group rich in benzene ring as shown in formula (2);

[0041] (2) Mix 100 parts by mass of the above vanillin-based phosphorous-containing bisphenol rich in benzene rings, 40-600 parts by mass of epichlorohydrin, and 30-300 parts by mass of basic substances, and then react at 20-130°C for 0.5 ~ 72 hours, after the reaction is finished, wash with water and distill to obtain a high heat-resistant and flame-retardant epoxy resin with vanillin group rich in benzene rings. ...

Embodiment 1

[0047] Example 1: Vanillin 100g, toluene 200g, 4,4'-biphenylenediamine 35g, 9,10-dihydro-9-oxa-10-phosphaphenanthrene-10-oxide 80g, pentachloride After mixing 10 g of niobium evenly, heat up to 30° C. for 24 hours, distill, wash with ethanol, and dry to obtain phosphorus-containing bisphenol with vanillin group rich in benzene rings as shown in the following formula (3). Then, 100 g of phosphorus-containing bisphenol rich in benzene ring in the vanillin group obtained above, 40 g of epichlorohydrin, and 80 g of lithium hydroxide aqueous solution of 20% (wt%, the same below) were mixed and reacted at 20° C. for 72 hours, After washing with water and distillation, the vanillin group-rich benzene ring-rich high heat-resistant and high-efficiency flame-retardant epoxy resin shown in the following formula (4) was obtained. According to the hydrogen nuclear magnetic resonance spectrum of the high heat-resistant and high-efficiency flame-retardant epoxy resin rich in benzene rings in...

Embodiment 2

[0050] Example 2: Oxidation of vanillin 100g, dimethylformamide 500g, 4,4'-diaminodiphenylmethane 10g, 9,10-dihydro-9-oxa-10-phosphaphenanthrene-10- After mixing 20 g of the mixture evenly, heat up to 120° C. for 0.5 hour reaction, distill, wash with ethanol, and dry to obtain phosphorus-containing bisphenol rich in benzene rings in the vanillin group shown in the following formula (5). Then, 100 g of phosphorus-containing bisphenols rich in benzene rings in the vanillin group obtained above, 500 g of epichlorohydrin, 5 g of tetrabutylammonium bromide, and 295 g of 15% NaOH aqueous solution were mixed and reacted at 130° C. for 0.5 hour, and then reacted for 0.5 hours at 130° C. Washing with water and distillation obtains the high heat-resistant and high-efficiency flame-retardant epoxy resin rich in benzene rings in the vanillin group shown in the following formula (6). According to the hydrogen nuclear magnetic resonance spectrum of the high heat-resistant and high-efficienc...

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Abstract

The invention discloses vanillic aldehyde-based high heat-resistant flame-retardant epoxy resin rich in benzene rings. The epoxy resin has a structure as shown in a formula (1), wherein R1 comprises a formula as shown in the description and R2 comprises a formula as shown in the description, and n is greater than or equal to 0 but less than or equal to 10. A preparation method comprises the following steps: uniformly mixing vanillic aldehyde, a diamine compound, a phosphorus hydrogen reagent, a catalyst and an organic solvent to react to form vanillic aldehyde-based phosphorus-containing bisphenol rich in benzene rings; and uniformly mixing the vanillic aldehyde-based phosphorus-containing bisphenol, epoxy chloropropane and an alkaline substance to react to obtain the vanillic aldehyde-based high heat-resistant flame-retardant epoxy resin rich in benzene rings. The invention also provides the preparation method of the epoxy resin. The epoxy resin disclosed by the invention is biological high heat-resistant efficient flame-retardant epoxy resin which not only has an excellent flame-retardant property if being cured, but also has excellent thermal stability, high glass-transition temperature and the like. Meanwhile, the preparation method is high in operability, good in controllability and easy to implement, and thus industrial production on a large scale is facilitated.

Description

technical field [0001] The invention relates to a flame-retardant epoxy resin, in particular to a vanillin-based benzene-ring-rich high-heat-resistant and high-efficiency flame-retardant epoxy resin, its preparation method and application, and belongs to the technical field of polymer materials. Background technique [0002] Epoxy resin is one of the most widely used polymer materials. It has excellent mechanical properties, high temperature resistance, corrosion resistance, adhesion and electrical insulation, and is widely used in automobiles, construction, electronics, aviation and other fields. With the advancement of science and technology and the continuous improvement of people's requirements for various products, epoxy resin as a matrix resin is also facing the pressure of high-performance development. Among them, improving the flame retardancy and heat resistance of epoxy resin is an important development direction of high performance epoxy resin. Among them, a lot ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08G59/06C08L63/00C08G59/30C07F9/40C07F9/6574
Inventor 马松琪朱锦王胜
Owner NINGBO INST OF MATERIALS TECH & ENG CHINESE ACADEMY OF SCI
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