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Triamine monomer containing pyridine structure and preparation method thereof

A technology of triamine monomer and pyridine, which is applied in the field of triamine monomer containing pyridine structure and its preparation, and achieves the effects of high permeability, low reaction temperature and reasonable selection

Inactive Publication Date: 2016-05-04
JILIN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

There are no reports of such structures containing pyridyl groups

Method used

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  • Triamine monomer containing pyridine structure and preparation method thereof
  • Triamine monomer containing pyridine structure and preparation method thereof
  • Triamine monomer containing pyridine structure and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0022] (1) Add 1,1,1-tris(4-hydroxyphenyl)ethane (10g, 32.64mmol) and 180mL N,N'-dimethylformamide into a three-necked flask, control the temperature at 10°C, and add potassium carbonate ( 18.04 g, 130.56 mmol), 2-chloro-5-nitropyridine (20.70 g, 130.56 mmol). The reaction was slowly heated to 60°C for 8 hours.

[0023] (2) After cooling down to room temperature, the reaction solution was poured into deionized water, a large amount of solids were precipitated, filtered, and washed with deionized water for 3 times, and the crude product was recrystallized with N,N'-dimethylformamide / water, 19 g of product after recrystallization.

[0024] (3) The recrystallized solid product was vacuum treated at 80° C. for 8 hours.

[0025] (4) Add 19 g of the intermediate product after recrystallization to a three-necked flask containing 200 mL of dioxane under nitrogen protection, add 3.8 g of palladium carbon, heat the reaction solution to 80 ° C and add 40 mL of hydrazine hydrate dropwis...

Embodiment 2

[0030] (1) Add 1,1,1-tris(4-hydroxyphenyl)ethane (5g, 16.48mmol) and 180mL N-methylpyrrolidone into a three-necked flask, control the temperature at 20°C, add sodium carbonate (8.73g, 82.40mmol ), 2-chloro-5-nitropyridine (13.06 g, 82.40 mmol). The reaction was slowly heated to 90°C for 5 hours.

[0031] (2) After cooling down to room temperature, the reaction solution was poured into deionized water, a large amount of solids were precipitated, filtered, and washed with deionized water three times. The crude product was recrystallized with N-methylpyrrolidone / water, and the product after recrystallization was 10 g.

[0032] (3) The recrystallized solid product was vacuum treated at 80° C. for 8 hours.

[0033] (4) Add 10 g of the intermediate product after recrystallization to a three-necked flask containing 200 mL of ethanol under nitrogen protection, add 3 g of platinum carbon, heat the reaction solution to 80 ° C and add 15 mL of hydrazine hydrate dropwise, and control th...

Embodiment 3

[0035] Add 1,1,1-tris(4-hydroxyphenyl)ethane (10g, 32.64mmol) and 150mL N,N'-dimethylformamide into the three-necked flask, control the temperature at 10°C, add sodium hydroxide (7.83g , 195.84mmol), 2-chloro-5-nitropyridine (15.52g, 97.92mmol). The reaction was slowly heated to 30°C for 5 hours. The reaction solution was poured into deionized water, a large amount of solid was precipitated, filtered, and washed with deionized water three times. The crude product was recrystallized from N,N'-dimethylformamide / water and vacuum treated at 60°C for 8 hours. Add 18g of the intermediate product after recrystallization to a three-necked flask containing 200mL of methanol under nitrogen protection, add 3g of platinum carbon, heat the reaction solution to 80°C, add 40mL of hydrazine hydrate dropwise, and control the reaction within 1 hour to complete the dropwise addition, at 80°C After reacting for 6 hours, it was filtered hot, and the filtrate was distilled under reduced pressure ...

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Abstract

The invention discloses a triamine monomer containing a pyridine structure and a preparation method thereof and belongs to the field of polymer synthesis. 1,1,1-tris(4-hydroxyphenyl)ethane serves as raw materials to react with a nitro compound containing pyridine groups with a polar solvent as a solvent and alkaline as a catalyst, an aromatic nitro compound is synthesized, and an intermediate product obtained after a reaction is catalyzed with a catalyst and subjected to hydrazine hydrate reduction so that finally the triamine monomer can be obtained. The nitro compound can be 2-chloro-5-nitropyridine, 2-chloro-5-nitro-3-picoline, 2-chloro-5-nitro-4-picoline and 6-chloro-3-nitro-2-picoline, alkali can be potassium hydroxide, sodium hydroxide, potassium carbonate, sodium carbonate, potassium acetate, sodium acetate and sodium bicarbonate. The monomer has high reaction activity; the preparation technology is simple, the yield is high, and purity is high; a better effect is achieved in the aspect of large-molecular-weight hyperbranched polymer preparation, and broad application prospects are achieved.

Description

technical field [0001] The invention belongs to the field of polymer synthesis, and in particular relates to a triamine monomer containing a pyridine structure and a preparation method thereof. Background technique [0002] As a special engineering plastic, polyimide is widely used in high-tech fields such as aerospace and microelectronics due to its excellent heat resistance, chemical corrosion resistance and good mechanical properties. Linear aromatic polyamide and polyimide are insoluble and infusible polymers that lack processability due to the rigidity of the chain. Once the multi-branched structure is introduced, the solubility in organic solvents can be significantly improved. Therefore, the synthesis and function of multibranched polymers are also attracting more and more attention. Because of its different three-dimensional shape, hyperbranched polyimide film has a lower dielectric constant, higher optical transmittance, and better solubility than the corresponding...

Claims

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Application Information

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IPC IPC(8): C07D213/73
CPCC07D213/73
Inventor 周宏伟姚佳楠陈春海赵晓刚党国栋王大明
Owner JILIN UNIV
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