n,n' alkylated diaminodicyclohexylmethane curing agent and preparation method
A technology of alkylating diaminodicyclohexylmethane and curing agent, which is applied in the preparation of amino-substituted functional groups, organic chemistry, etc., and can solve problems such as easy twists and turns, failure to meet extreme environmental requirements, and insufficient toughness of epoxy resins. To achieve the effect of enhancing toughness
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Embodiment 1
[0047] Example 1: Preparation of N,N'-dimethyl-4,4-diaminodicyclohexylmethane
[0048] In a 1L autoclave, add 105g (0.5 mol) of 4,4-diaminodicyclohexylmethane, add 142g (1 mol) of iodomethane, heat and stir to dissolve, add 400g of dioxane, and add macroporous strong basic anion Exchange resin (D201) 6g, close the autoclave, pass N 2 Replaced 3-5 times, started to raise the temperature to 50°C, controlled the pressure of the reaction system to about 1 MPa, stirred and reacted for 2 hours, fractionated, and the yield of the product N,N'-dimethyl-4,4-diaminodicyclohexylmethane was 99%.
Embodiment 2
[0049] Example 2: Preparation of N,N'-diethyl-4,4-diaminodicyclohexylmethane
[0050] In a 1L autoclave, add 105g (0.5 mole) of 4,4-diaminodicyclohexylmethane, add 156g (1 mole) of iodoethane, heat and stir to dissolve, add 400g of dioxane, and add macroporous strong alkali Anion exchange resin (D201) 6g, close the autoclave, pass N 2 Replaced 3-5 times, started to raise the temperature to 70°C, controlled the pressure of the reaction system to about 1.5 MPa, stirred and reacted for 2 hours, and fractionated, the yield of the product N,N'-diethyl-4,4-diaminodicyclohexylmethane was 97%.
Embodiment 3
[0051] Example 3: Preparation of N,N'-dibutyl-4,4-diaminodicyclohexylmethane
[0052] In a 1L autoclave, add 105g (0.5 moles) of 4,4-diaminodicyclohexylmethane, add 202.4g (1.1 moles) of iodobutane, add 300g of dioxane, heat and stir to dissolve, add macroporous strong base Anion exchange resin (D201) 12g, close the autoclave, pass N 2 Replaced 3-5 times, started to raise the temperature to 100°C, controlled the pressure of the reaction system to about 3 MPa, stirred and reacted for 3 hours, fractionated, and the yield of the product N,N'-dibutyl-4,4-diaminodicyclohexylmethane was 95%.
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