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Modification method of heat-resistant toughened methyl tetrahydrophthalic anhydride

A technology of toughness methyltetrahydrophthalic anhydride and methyltetrahydrophthalic anhydride, which is applied in the field of organic chemistry, can solve the problems of low heat resistance and toughness of methyltetrahydrophthalic anhydride, and achieves outstanding cost performance, improved heat resistance and toughness, The effect of reducing product cost

Inactive Publication Date: 2012-09-05
朱瑞澄 +2
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0013] The purpose of the present invention is to provide a modification method of heat-resistant and toughened methyltetrahydrophthalic anhydride. The technical problem of low heat resistance and toughness of phthalic anhydride

Method used

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  • Modification method of heat-resistant toughened methyl tetrahydrophthalic anhydride
  • Modification method of heat-resistant toughened methyl tetrahydrophthalic anhydride
  • Modification method of heat-resistant toughened methyl tetrahydrophthalic anhydride

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Effect test

Embodiment 1

[0038]In the above device, add 200g of methyltetrahydrophthalic anhydride, 1.5g of sulfuric acid, 0.5g of tetramethylphosphonium hydroxide, 40g of polypropylene glycol diglycidyl ether, and 50g of nadic acid anhydride, heat to 165°C under stirring, and react for 1 hour. Then it was flash evaporated under vacuum at -0.09Mpa to obtain a yellow transparent liquid with a yield of 92.3.

[0039] Curing test E51: Modified methyltetrahydrophthalic anhydride: 2-ethyl-4-methylimidazole = 100: 105: 1

[0040] Curing temperature 80°C degassing for half an hour 100°C / 2h+130°C / 3h+150°C / 2h

[0041] Glass transition temperature: 155℃ Impact strength: 25KJ / m 2

Embodiment 2

[0043] In the above device, add 200g of methyltetrahydrophthalic anhydride, 1.0g of polyphosphoric acid, 1.0g of phenylphosphonic acid, 30g of hydroxy-terminated nitrile rubber, 25g of pyromellitic anhydride, and 25g of nadic anhydride, and heat to 170°C under stirring , reacted for 1.5 hours, and then flashed under vacuum at -0.09Mpa to obtain a reddish-brown liquid with a yield of 92.5%.

[0044] Curing test E51: Modified methyl tetrahydrophthalic anhydride: 2-ethyl-4-methylimidazole=100:102:1

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

[0046] Glass transition temperature: 142℃ Impact strength: 24KJ / m 2

Embodiment 3

[0048] Add 200g of methyltetrahydrophthalic anhydride, 1.0g of sulfuric acid, 1.0g of phenylphosphonic acid, 50g of pyromellitic anhydride, and 40g of diethylene glycol glycidyl ether into 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 91%.

[0049] Curing test E51: Modified methyl tetrahydrophthalic anhydride: 2-ethyl-4-methylimidazole = 100:100:1

[0050] Curing temperature 80°C degassing for half an hour 100°C / 2h+130°C / 3h+150°C / 2h (curing temperature can refer to "Epoxy Resin and Epoxy Coatings" 2003 edition, Chemical Industry Press, pages P 216-P218)

[0051] Glass transition temperature: 140℃ Impact strength: 20KJ / m 2

[0052] 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 v...

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Abstract

The invention provides a modification method of heat-resistant toughened methyl tetrahydrophthalic anhydride. The modification method is characterized in that methyl tetrahydrophthalic anhydride, heat-resistant acid anhydrides and flexibilizers undergo a heating reaction in the presence of acidic catalysts to produce methyl tetrahydrophthalic anhydride liquid crude products, wherein a weight ratio of the methyl tetrahydrophthalic anhydride to the heat-resistant acid anhydrides to the flexibilizers to the acidic catalysts is 1: (0.06 to 0.5): (0.10 to 0.40): (0.008 to 0.05) and a reaction temperature is in a range of 80 to 200 DEG C, and the methyl tetrahydrophthalic anhydride liquid crude products are putted into a flash evaporation kettle and carrying out a flash evaporation process under conditions of kettle temperature of 170 to 240 DEG C and vacuum degree of -0.070 to -0.095 Mpa to obtain modified heat-resistant toughened methyl tetrahydrophthalic anhydride. Cured products of epoxy resin and modified methyl tetrahydrophthalic anhydride have a glass transition temperature of 135 to 150 DEG C and an impact-resistant strength of 16 to 25 KJ / m <2>.

Description

Technical field: [0001] The invention relates to the field of organic chemistry, in particular to an acid anhydride curing agent used for curing epoxy resins, in particular to methyltetrahydrophthalic anhydride, and in particular to a modification method for heat-resistant and toughened methyltetrahydrophthalic anhydride. Background technique: [0002] In the prior art, methyltetrahydrophthalic anhydride is often used as a curing agent for epoxy resins. Methyltetrahydrophthalic anhydride is obtained by reacting piperylene with isoprene and maleic anhydride. After the reaction, solid methyltetrahydrophthalic anhydride is obtained. Solid methyltetrahydrophthalic anhydride is isomerized at high temperature in the presence of a catalyst Reaction, after isomerization, an isomerized mixture that remains liquid at a low temperature below -15°C can be obtained. The more isomers in the mixture, the lower the freezing point and the more stable the product. [0003] Methyltetrahydroph...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08G59/42
Inventor 朱瑞澄朱新凯朱新乾庄玉林
Owner 朱瑞澄