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Composite epoxy resin composition and preparation method thereof

A technology of epoxy resin and composition, applied in the field of polymer compounds, can solve the problems of limited application of epoxy resin, flame retardancy and temperature resistance of epoxy resin, etc., and achieves simple and fast preparation method, excellent flame retardancy, and good flame retardancy. Effect

Pending Publication Date: 2022-08-05
SHANGHAI UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0006] In order to overcome the defects in the prior art, a composite epoxy resin composition and its preparation method are now provided to solve the problem of flame retardancy and temperature resistance of epoxy resin, which greatly limits the application of epoxy resin

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  • Composite epoxy resin composition and preparation method thereof
  • Composite epoxy resin composition and preparation method thereof
  • Composite epoxy resin composition and preparation method thereof

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preparation example Construction

[0030] The preparation of the modified titanium oxide powder includes fully stirring and mixing the titanium oxide powder with anhydrous ethanol and a modifier to carry out a modification reaction.

[0031] The flame retardant curing agent is a DOPO derivative. The flame retardant curing agent is DOPO derivative DOPO-DDS, and the structural formula of said DOPO-DDS is as follows:

[0032]

[0033] A common curing agent is 4,4'-diaminodiphenylmethane (DDM).

[0034] In the present invention, the mixture of titanium oxide powder, flame retardant curing agent and common curing agent is sequentially pre-cured and secondary-cured to obtain a composite epoxy resin composition.

[0035] Wherein, the temperature of pre-curing is 90℃~110℃, the time of pre-curing is 1h~2h; the temperature of secondary curing is 140℃~160℃, and the time of secondary curing is 2~4h.

[0036] The present invention also provides a preparation method of the composite epoxy resin composition, comprising t...

Embodiment 1

[0046] With the volume ratio of ethanol:water=1:9, 100 mL of ethanol was prepared, and 2 g of γ-aminopropyltriethoxysilane was added to the ethanol solution, and the solution was stirred until uniform. 20g of nano-titanium oxide was pre-dried at 120°C for 6h, and then added to the above solution. The solution system was mechanically stirred in nitrogen for 1-2h, followed by ultrasonication for 30min, and the reaction temperature was controlled at about 50°C. After the reaction, the system was cooled to room temperature, and washed with acetone solution by centrifugation for 3 to 5 times. Finally, the product was dried in an oven at 80°C for 12 hours to obtain the modified nano-titanium oxide powder.

[0047] In a 500mL three-necked round bottom flask equipped with magnetic stirring, dropping funnel and reflux device, add 0.1mol (19.826g) 4,4'-diaminodiphenylsulfone (DDS), 0.2mol (24.4g) p-hydroxybenzene formaldehyde and 200 mL of tetrahydrofuran (THF). The mixture was stirre...

Embodiment 2

[0050] With the volume ratio of ethanol:water=1:9, 100 mL of ethanol was prepared, and 2 g of γ-aminopropyltriethoxysilane was added to the ethanol solution, and the solution was stirred until uniform. 20g of nano-titanium oxide was pre-dried at 120°C for 6h, and then added to the above solution. The solution system was mechanically stirred in nitrogen for 1-2h, followed by ultrasonication for 30min, and the reaction temperature was controlled at about 50°C. After the reaction, the system was cooled to room temperature, and washed with acetone solution by centrifugation for 3 to 5 times. Finally, the product was dried in an oven at 80°C for 12 hours to obtain the modified nano-titanium oxide powder.

[0051] In a 500mL three-necked round bottom flask equipped with magnetic stirring, dropping funnel and reflux device, add 0.1mol (19.826g) 4,4'-diaminodiphenylsulfone (DDS), 0.2mol (24.4g) p-hydroxybenzene formaldehyde and 200 mL of tetrahydrofuran (THF). The mixture was stirre...

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Abstract

The invention discloses a composite epoxy resin composition and a preparation method thereof, and the composite epoxy resin composition is composed of 100 parts by weight of epoxy resin, 1-5 parts by weight of titanium oxide powder, 15-20 parts by weight of a flame-retardant curing agent and 17-21 parts by weight of a common curing agent. The titanium oxide powder is nano titanium oxide powder modified by gamma-aminopropyltriethoxysilane, and the flame-retardant curing agent is a DOPO (9, 10-dihydro-9-oxa-10-phosphaphenanthrene-10-oxide) derivative; the mixture of the titanium oxide powder, the flame-retardant curing agent and the common curing agent is sequentially subjected to pre-curing and secondary curing to prepare the composite epoxy resin composition, the pre-curing temperature is 90-110 DEG C, the pre-curing time is 1-2 hours, the secondary curing temperature is 140-160 DEG C, and the secondary curing time is 2-4 hours. The problems of flame retardance and temperature resistance of the epoxy resin are solved, and the application of the epoxy resin is greatly limited.

Description

technical field [0001] The invention relates to the technical field of polymer compounds, in particular to a composite epoxy resin composition and a preparation method thereof. Background technique [0002] Epoxy resin has excellent properties such as adhesion, chemical resistance, electrical insulation and high strength. However, the flame retardancy and temperature resistance of epoxy resin have not been solved, which greatly limits the application of epoxy resin. If the flame retardant is simply added to the epoxy resin, although the flame retardant performance of the epoxy resin will be improved, its glass transition temperature Tg will be reduced at the same time. When the ambient temperature exceeds Tg, the adhesive properties of epoxy resin will be greatly reduced, resulting in the loss of its reinforcement effect, which restricts the application scenarios of epoxy resin. [0003] At the same time, although the traditional halogen-based flame retardants have high fl...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08L63/00C08K9/06C08K3/22C08K5/5313
CPCC08K9/06C08K3/22C08K5/5313C08K2201/011C08K2003/2241C08L2201/02C08L63/00
Inventor 肖依赵子敬任慕苏俞鸣明
Owner SHANGHAI UNIV