Dichloro bisphthalimide intermediate as well as synthesis method and application thereof
A technology of dichlorobisphthalimide and synthesis method, applied in directions such as organic chemistry, can solve problems such as low yield, difficulty in separation and purification, etc.
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Embodiment 1
[0037] Add 10.00 g of 3-chlorophthalic anhydride (0.0548 mol), 2.963 g of p-phenylenediamine (0.0274 mol), 200 mL of DMAc (anhydrous), 0.049 g of 98% sulfuric acid, and 0.9864 g of acetic anhydride into a stirring paddle 500mL four-neck round bottom flask. Then the flask was installed with a condenser and a nitrogen adapter, and was purged with a large flow of nitrogen for several minutes to make the N 2 Fill the inside of the flask. Keep nitrogen purging, stir at 300 rpm, use an oil bath to increase the temperature of the liquid in the flask to 160° C., reflux for 10 hours, and then cool to room temperature. The reaction mixture was filtered under reduced pressure to obtain a crude product filter cake, and the filtrate was collected and used as the next batch of reaction solvent. The crude product was transferred to another 500mL four-necked round bottom flask equipped with a stirring paddle, nitrogen adapter and condenser tube, and 200mL of DMAc (anhydrous) was added, full...
Embodiment 2
[0040] 186.6 grams of 4-chlorophthalic anhydride (1.01mol), 27.02 grams of m-phenylenediamine (0.25mol), 102.1 grams of acetic anhydride (1.0mol), 1200mL of DMAc (anhydrous), 1000mL of the previous batch The reaction filtrate and 1.00 g of 98% sulfuric acid were added into a 3000 mL four-necked round bottom flask equipped with a stirring paddle. Another 27.02 g of m-phenylenediamine (0.25 mol) was dissolved in 300 mL of DMAc (anhydrous), and added to a 500 mL balance feeder. Then install the balance feeder on the flask, and install a condenser tube and a nitrogen connection on the flask, purging with a large flow of nitrogen for several minutes to make the N 2 Fill the inside of the flask. Keep nitrogen purging, stirring at 240rpm, using an oil bath to increase the temperature of the liquid in the flask to 166°C, then slowly add m-phenylenediamine solution dropwise, reflux for 10 hours, and then cool to room temperature. The reaction mixture was filtered under reduced pressu...
Embodiment 3
[0043] The m-phenylenediamine-type dichlorophthalimide intermediate produced in Example 2 was used in the synthesis of polyimide sulfide special engineering plastics. Get 14.01g of sodium hydrosulfide, 10.25g of sodium hydroxide, 7.5g of catalyst, 4.1g of auxiliary agent, and 550g of solvent, carry out pre-dehydration of raw materials in an autoclave under nitrogen protection atmosphere, add and implement after removing most of the water in the system 169 g of the m-phenylenediamine-type dichlorophthalimide intermediate synthesized in Example 2 was added with a certain amount of solvent and subjected to high-temperature polycondensation in an autoclave protected by a nitrogen atmosphere. After the polycondensation reaction is completed, the reaction slurry is subjected to high-temperature sedimentation, re-slurry, solvent washing, and water washing to obtain refined polyimide sulfide special functional plastics. A total of 94.1 g of the product was obtained, with a yield of 94...
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