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Method for modifying heat-proof plasticizing methyl nadic anhydride

A technology of tough methyl nadic anhydride and methyl nadic anhydride, which is applied in organic chemistry and other fields, can solve the problems of low bending strength and low bending strength, and achieve improved heat resistance and toughness, outstanding cost performance, and convenient use Effect

Inactive Publication Date: 2008-04-23
朱新干 +2
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0008] The object of the present invention is to provide a kind of modification method of heat-resistant and toughened methyl nadic acid anhydride, the modification method of described heat-resistant toughened methyl nadic acid anhydride will solve the problem of methyl nadic acid anhydride in the prior art The technical problem that the bending strength is lower than that of ordinary methylnadic anhydride and epoxy resin cured product

Method used

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  • Method for modifying heat-proof plasticizing methyl nadic anhydride
  • Method for modifying heat-proof plasticizing methyl nadic anhydride
  • Method for modifying heat-proof plasticizing methyl nadic anhydride

Examples

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Effect test

Embodiment 1

[0036] Add 200g of methylnadic acid anhydride, 1.0g of sulfuric acid, 1.0g of phenylphosphonic acid, 50g of pyromellitic anhydride, and 40g of diethylene glycol glycidyl ether in a container equipped with a flow condenser, feeder and agitator , heated to 160°C under stirring, reacted for 1 hour, and then flashed under vacuum at -0.09Mpa to obtain a dark red transparent liquid with a yield of 92%.

[0037] Curing test E51: Modified methyl nadic anhydride: 2-ethyl-4-methylimidazole=100:80.5:1

[0038] Curing temperature 80°C Degassing for half an hour 100°C / 2h+130°C / 3h+150°C / 3h+180°C / 3h (The ratio of curing temperature refers to "Epoxy Resin and Epoxy Coatings" 2003 edition, Chemical Industry Press, P216 -P218 page)

[0039] Glass transition temperature: 175°C

[0040] The glass transition temperature is the temperature at which an amorphous or semi-crystalline polymer transitions from a viscous or highly elastic state to a glass state (or vice versa), and it indicat...

Embodiment 2

[0043] In the above device, add 200g of methyl nadic acid anhydride, 1.0g of polyphosphoric acid, 1.0g of phenylphosphonic acid, 30g of hydroxy-terminated nitrile rubber, 50g of pyromellitic anhydride, heat to 170°C under stirring, and react for 1.5 hours. Then it was flash evaporated under vacuum at -0.09Mpa to obtain a reddish-brown liquid with a yield of 92.5%.

[0044] Curing test E51: Modified methyl nadic anhydride: 2-ethyl-4-methylimidazole = 100:80:1

[0045] Curing temperature 80°C Degassing for half an hour 100°C / 2h+130°C / 3h+150°C / 3h+180°C / 3h

[0046] Glass transition temperature: 170℃ Impact strength: 35KJ / m 2

Embodiment 3

[0048] In the above device, add 200g of methyl nadic acid anhydride, 1.5g of sulfuric acid, 0.5g of tetramethylphosphonium hydroxide, 40g of polypropylene glycol diglycidyl ether, 50g of trimellitic anhydride, heat to 165°C under stirring, react for 1 hour, and then Flash evaporation under vacuum at -0.09Mpa gave milky yellow opaque liquid with a yield of 92.3%.

[0049] Curing test E51: modified methyl nadic anhydride: 2-ethyl-4-methylimidazole = 100:77:1

[0050] Curing temperature 80°C Degassing for half an hour 100°C / 2h+130°C / 3h+150°C / 3h+180°C / 3h

[0051] Glass transition temperature: 172℃ Impact strength: 26KJ / m 2

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Abstract

The process of preparing modified heat resistant toughened methyl nadic anhydride includes heated reaction of methyl nadic anhydride, heat resistant anhydride, toughening agent and catalyst of inorganic acid and / or phosphorus-containing compound in certain weight proportion inside a reactor to obtain liquid coarse product, and flash evaporation of the coarse product in a flash evaporation kettle to obtain heat resistant toughened methyl nadic anhydride product. The process has yield up to 90 %, normal pressure operation and low cost; and modified nadic anhydride has raised heat resistance and toughness.

Description

Technical field: [0001] The invention relates to the field of chemistry, in particular to an acid anhydride curing agent used for curing epoxy resins, in particular to methyl nadic anhydride, and in particular to a method for modifying heat-resistant and toughened methyl nadic anhydride. Background technique: [0002] Methylnadic anhydride is obtained by the reaction of methylcyclopentadiene and maleic anhydride, and its scientific name is 4,7-methylene cumylfuran-1,3 dione-3aα, 4a, 7a, 7aα- Tetrahydromethyl, molecular formula: C 10 h 10 o 3 , molecular weight: 178.2, the structural formula is as follows: [0003] [0004] Because it has better heat resistance after curing with epoxy resin than the cured product after curing with methyl tetrahydrophthalic anhydride and epoxy resin, and methyl nadic anhydride is a liquid anhydride with low viscosity, which can be mixed with epoxy resin The post-pot life is long, so it is widely used, but for high-performance electronic...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D307/89C08G59/42
Inventor 朱新乾杭颂高允中朱瑞澄朱新凯
Owner 朱新干