Epoxy resin composition containing vanillic aldehyde-based phosphorus containing flame retardant and application thereof

A technology of epoxy resin and vanillin, which is applied in the fields of compounds of group 5/15 elements of the periodic table, organic chemistry, chemical instruments and methods, etc., can solve problems such as complex preparation process, and achieve simple preparation process and high mechanical properties Excellent, the effect of alleviating the oil crisis

Active Publication Date: 2017-08-04
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

[0003] Phosphorus-containing compounds based on Schiff base have a very good carbon-forming effect and contain nitrogen, which can act as a gas source, but the existing phosphorus-containing compounds are usually made of petrochemical products as raw materials, and often Complex process

Method used

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  • Epoxy resin composition containing vanillic aldehyde-based phosphorus containing flame retardant and application thereof
  • Epoxy resin composition containing vanillic aldehyde-based phosphorus containing flame retardant and application thereof
  • Epoxy resin composition containing vanillic aldehyde-based phosphorus containing flame retardant and application thereof

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Experimental program
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preparation example Construction

[0028] Further, the preparation method may further include: uniformly mixing the vanillin-based phosphorus-containing bisphenol, epichlorohydrin and alkaline substances, and then reacting at 20-120° C. for 0.2-48 hours to obtain the vanillin-based phosphorus-containing bisphenol An epoxy compound, the vanillin-based phosphorus-containing epoxy compound has a structure shown in formula (3) or formula (4);

[0029]

[0030] Among them, R 1 include

[0031] R 2 Including straight-chain alkanes or aromatic hydrocarbons or alicyclic alkanes with more than 2 to 20 carbon atoms, 0≤n≤10.

[0032] As one of the preferred embodiments, the mass ratio of vanillin, diamine compound, phosphorus-containing compound, catalyst and organic solvent is 100: (15-100): (20-300): (0-15): (50 ~500).

[0033] As one of the preferred embodiments, the mass ratio of the vanillin-based phosphorus-containing bisphenol, epichlorohydrin and alkaline substance is 100:(20-500):(30-300).

[0034] As o...

Embodiment 1

[0050] (1) React 100g of vanillin, 36g of p-phenylenediamine, and 500mL of ethanol at 40°C for 1 hour, then add 2.5g of zinc chloride and 72g of dimethyl phosphite, heat up to 80°C and react for 3 hours, petroleum ether precipitates, After washing with ethanol, the vanillin-based phosphorus-containing bisphenol represented by the following formula (5) was obtained. According to the hydrogen nuclear magnetic resonance spectrum figure of this vanillin-based phosphorus-containing bisphenol, it can be known that in 1 In H nuclear magnetic resonance (d6-DMSO is the solvent), 6.7-7.1ppm represents the proton peak on the benzene ring of the vanillin structure, 6.5ppm represents the proton peak on the benzene ring of the p-phenylenediamine structure, and 3.8ppm is the methyl group of the vanillin structure proton peak on the .

[0051]

[0052] (2) Mix 100g of bisphenol-A epoxy resin (E-51), 15g of ammonium polyphosphate and 0.5g of vanillin-based phosphorus-containing bisphenol s...

Embodiment 2

[0059] (1) React 100g of vanillin, 36g of p-cyclohexanediamine, and 500mL of ethanol at 40°C for 1 hour, then add 2.5g of zinc chloride and 154g of diphenyl phosphite, raise the temperature to 90°C for 2 hours, and precipitate petroleum ether , after washing with ethanol, obtain the vanillin-based phosphorus-containing bisphenol shown in the following formula (6). According to the hydrogen nuclear magnetic resonance spectrum figure of this vanillin-based phosphorus-containing bisphenol, it can be known that in 1 In H NMR (d6-DMSO is a solvent), 6.6-7.4ppm represents the proton peak on the benzene ring of diphenyl phosphite and vanillin structure, and 2.6ppm represents the proton peak on the carbon connected to the imine group on the alicyclic ring, 1.2-1.8ppm is the chemical shift of the proton on the methylene group of the 1,4-cyclohexanediamine structure, and 3.7ppm is the proton peak on the methyl group of the vanillin structure.

[0060]

[0061] (2) Mix 100 g of glyci...

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Abstract

The invention discloses an epoxy resin composition containing a vanillic aldehyde-based phosphorus containing flame retardant. The epoxy resin composition comprises epoxy resin, a curing agent, a curing accelerant, a primary flame retardant and a flame retardant additive and etc. The flame retardant additive is the vanillic aldehyde-based phosphorus containing flame retardant The invention also discloses an application of the epoxy resin composition, for example, an application of the epoxy resin composition or a cured product thereof as a flame retardant material. When the epoxy resin composition disclosed by the invention is cured and used as a flame retardant material, compared with an existing intumescent fire retardant epoxy system, the epoxy resin composition not only is more excellent in flame retardant property and mechanical property, but also has double functions of saving resources and protecting the environment as the flame retardant additive uses sustainable vanillic aldehyde as a raw material.

Description

technical field [0001] The invention relates to an epoxy resin composition, in particular to an epoxy resin composition containing the formulation of the vanillin-based phosphorus-containing flame retardant and its application, such as the use as a flame-retardant material, belonging to the technical field of polymer materials . Background technique [0002] Epoxy resin 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. Flammability is a common problem of epoxy resins and even most polymer materials. In order to achieve the purpose of flame retardancy, the current common method is to introduce flame retardants into the epoxy resin system. With the EU's two major environmental directives on flame retardants, "West Electrical and Electronic Equipment Directive, WEEE" (effective in March 2003) and "Restriction of Wit...

Claims

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Application Information

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