Type I forked biphenyl diamine and preparation method and application thereof
A biphenylenediamine and fork-type technology is applied to fork-type biphenylenediamine and a preparation method thereof, and in the field of polyamide and polyimide materials to achieve good solubility and processability, expand application scope, The effect of improving organic solubility
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Embodiment 1
[0059] Embodiment 1: the synthesis of I-1 monomer (R 1 =R 2 = methyl)
[0060] Synthesis process parameters of intermediate I-1(2):
[0061] Based on raw material (1), NiCl 2 , Zn, triphenylphosphine and 2-bromo-p-xylene in a molar ratio of 0.01: 0.5: 0.01: 1 drop into N, N-dimethylformamide, and the amount of N, N-dimethylformamide makes the reactant The solid content of is 10% (w / v). The mixture is stirred at 100°C for 2h, filtered, and the solvent is evaporated to dryness. The remaining solid is distilled to obtain intermediate I-1(2).
[0062] Synthetic process parameters of intermediate I-1(3):
[0063] In terms of intermediate I-1 (2), the molar ratio of fuming nitric acid and intermediate I-1 (2) is 3.0: 1; drop in nitromethane, the consumption of nitromethane makes intermediate I-1 ( 2) with a solid content of 30% (w / v), and then stirred at 10°C for 12 hours. After the reaction, the reaction solution was poured into water to precipitate, filtered and dried to obta...
Embodiment 2
[0074] Embodiment 2: the synthesis of 1-2 monomer (R 1 =R 2 = methoxy)
[0075] Synthesis process parameters of intermediate I-2(2):
[0076] Based on raw material (1), NiBr 2 , Mn, tricresyl phosphorus and 2-chloro-p-dimethoxybenzene in a molar ratio of 0.1:1:0.1:1 into N,N-dimethylacetamide, the amount of N,N-dimethylacetamide The solid content of the reactant was 30% (w / v), the mixture was stirred at 80° C. for 6 h, filtered, and the solvent was evaporated to dryness. The remaining solid was distilled to obtain intermediate I-2(2).
[0077] Synthesis process parameters of intermediate I-2(3):
[0078] In terms of intermediate I-2 (2), the molar ratio of concentrated nitric acid and intermediate I-2 (2) is 2.0: 1; drop into the concentrated sulfuric acid, the consumption of nitric acid concentrated sulfuric acid makes intermediate I-2 (2) The solid content was 20% (w / v), and then stirred at 0° C. for 6 hours. After the reaction, the reaction solution was poured into wat...
Embodiment 3
[0089] Embodiment 3: the synthesis of 1-3 monomer (R 1 = methyl, R 2 = trifluoromethyl)
[0090] Synthesis process parameters of intermediate I-3(2):
[0091] Based on the raw material (1), Ni, Mg, triphenylphosphine and 3-bromo-4-methyltrifluorotoluene are dropped into the solvent hexamethylphosphoric triamide in a molar ratio of 0.05:0.75:0.05:1, and the solvent The amount of hexamethylphosphoric triamide is such that the solid content of the reactant is 30% (w / v). After the mixture is stirred at 120°C for 1h, it is filtered and the solvent is evaporated to dryness. The remaining solid is distilled to obtain intermediate I- 3(2).
[0092] Synthesis process parameters of intermediate I-3(3):
[0093] In terms of intermediate I-3 (2), the molar ratio of concentrated nitric acid and intermediate I-3 (2) is 2.1: 1; drop in methanol, the consumption of solvent methanol makes the solid of intermediate I-3 (2) The content was 10 (w / v), and then stirred at 30°C for 124 hours. A...
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