Crosslinkable diamine monomer, preparation method and application of crosslinkable diamine monomer in preparation of polyimide
A technology of diamine monomer and polyimide is applied in chemical instruments and methods, preparation of organic compounds, preparation of aminohydroxy compounds, etc. The effect of solvent resistance, low cost of raw materials, and simple and easy operation
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Embodiment 1
[0039] Example 1: Preparation of 4-(2,3,5,6-tetrafluoro-4-vinylphenoxy)benzene-1,3-diamine monomer
[0040] The first step reaction: add 5.93g (30mmol) of 2,4-diaminophenol dihydrochloride, 7g (36mmol) of 2,3,4,5,6- Pentafluorostyrene, 0.91g (6mmol) cesium fluoride, 65mL N,N-dimethylacetamide (DMAc); then divide into 6 times, slowly add 1.26g calcium hydride each time, add a total of 7.56g (180mmol) hydrogenation calcium. Stir and under nitrogen protection, heat to 80°C for 24h. After the reaction solution was cooled to room temperature, it was discharged into 600 mL of deionized water, and after standing for a period of time, it was filtered and the filter residue was collected. The filter residue was washed 4 times with deionized water until the filtrate in the lower layer was colorless, and dried in a vacuum oven at 100°C for 10 hours under vacuum. The crude product was purified by chromatographic column, the eluent ratio was 1:2 by volume of ethyl acetate and n-hexane, t...
Embodiment 2
[0042] Example 2: Preparation of 4,6-bis(2,3,5,6-tetrafluoro-4-vinylphenoxy)benzene-1,3-diamine monomer
[0043] The first step reaction: add 3.20g (15mmol) of 4,6-diaminoresorcinol dihydrochloride, 6.40g (33mmol) of 2,3,4, 5,6-Pentafluorostyrene, 6.84g (45mmol) cesium fluoride, 54mL N,N-dimethylacetamide (DMAc), and then divide into 6 times, slowly add 0.85g calcium hydride each time, add 5.1g in total (121mmol) calcium hydride, stirred and heated to 80°C for 24h under the protection of nitrogen. After the reaction solution was cooled to room temperature, it was discharged into 500 mL of deionized water, and after standing for a period of time, it was filtered and the filter residue was collected. The filter residue was washed 4 times with deionized water until the lower layer filtrate was colorless. Dry in a vacuum oven at 100°C for 10 hours under vacuum. The crude product was purified by chromatographic column, the eluent ratio was 1:60 by volume of ethyl acetate and dich...
Embodiment 3
[0045] Example 3: 4-(2,3,5,6-tetrafluoro-4-vinylphenoxy)benzene-1,3-diamine monomer, 4,4'-diaminostilbene-2, Preparation of Polyimide by Polymerization of 2'-Disulfonic Acid and 1,4,5,8-Naphthalene Tetracarboxylic Anhydride (TFVPDM-DSDSA-NTDA)
[0046] Add 1.332g (3.6mmol) 4,4'-diaminostilbene-2,2'-disulfonic acid and 0.802g (7.93mmol) of triethylamine, 10mL of m-cresol, heated to 80°C and stirred to dissolve, then added 0.119g (0.4mmol) of 4-(2,3,5,6-tetrafluoro-4- Vinylphenoxy) benzene-1,3-diamine monomer and 1.072g (4mmol) of 1,4,5,8-naphthalene tetracarboxylic anhydride, 0.672g (5.5mmol) of benzoic acid, and then add 10mL of m- Cresol, react at 80°C for 4 hours, heat up to 180°C for 24 hours to obtain a viscous polyimide, after the reaction is completed, add 20mL of m-cresol to dilute the reaction solution, cool to 100°C, and discharge the material into acetone to obtain a yellow silk The product was extracted and washed with acetone under reflux for 48 hours, dried in a...
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