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Large-scale preparation method for covalence copolymer with triazine frame

A technology for large-scale preparation of triazine compounds, which is applied in the field of large-scale preparation of covalent polymers with triazine skeletons, can solve the problems of harsh reaction vessel requirements, difficulty in large-scale preparation, and carbonization of products, and achieves low production cost, Easy to industrialize and scale up production, easy to achieve effect

Active Publication Date: 2018-08-14
SHANGHAI ADVANCED RES INST CHINESE ACADEMY OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

It mainly solves the technical problems that the preparation methods in the prior art are difficult to prepare in large quantities, waste energy, product carbonization, and have strict requirements on the reaction vessel

Method used

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  • Large-scale preparation method for covalence copolymer with triazine frame
  • Large-scale preparation method for covalence copolymer with triazine frame
  • Large-scale preparation method for covalence copolymer with triazine frame

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0066] Accurately weigh 1,4-dibromobenzene (30mmol, 3 equivalents, 7070mg, purity: 98%) and dissolve it in toluene in a 20mL three-necked flask. The solution (61mmol, 6.1 equivalents, 24.4mL, 2.5mol / L) was added dropwise into a three-necked flask, and at the same time, toluene was added, stirred for 30min, and heated to reflux to prepare 1,4-dilithiumbenzene (nucleophile).

[0067] 2,4,6-Trichloro-1,3,5-triazine (20mmol, 2eq, 3763mg, purity: 98%) was dissolved in 10mL of dry 1,4-dioxane, and then the dissolved 2 , 4,6-trichloro-1,3,5-triazine was slowly dropped into the three-necked flask, and refluxed for 22 hours.

[0068] After reflux, cool to room temperature naturally, add saturated ammonium chloride solution to quench the reaction, filter the filter residue, wash the filter residue with water to remove lithium salt, then wash with ethyl acetate, methanol and other organic solvents to remove small molecule products in the filter residue, and finally The filter residue wa...

Embodiment 2

[0071] Accurately weigh 4,4'-dibromobiphenyl (15mmol, 3 equivalents, 4775mg, purity: 98%) and dissolve it in toluene in a 20mL three-necked flask, and replace the air with nitrogen as a protective gas. The n-hexane solution (30.5mmol, 6.1 equivalents, 12.2mL, 2.5mol / L) was added dropwise into a three-necked flask, and at the same time, toluene was added, stirred for 30min, and heated to reflux to prepare 4,4'-dilithium biphenyl (nucleophilic Reagent).

[0072] 2,4,6-Trichloro-1,3,5-triazine (10 mmol, 2 equivalents, 1882 mg, purity: 98%) was dissolved in 5 mL of dry 1,4-dioxane, and the dissolved 2 , 4,6-trichloro-1,3,5-triazine was slowly added dropwise into the three-necked flask, and refluxed for 22 hours.

[0073] After reflux, cool to room temperature naturally, add saturated ammonium chloride solution to quench the reaction, filter the filter residue, wash the filter residue with water to remove lithium salt, then wash with ethyl acetate, methanol and other organic solve...

Embodiment 3

[0076] Accurately weigh 1,4-dibromonaphthalene (15mmol, 3 equivalents, 4377mg, purity: 98%) and dissolve it in toluene in a 20mL three-necked flask, and replace the air with nitrogen as a protective gas. Add alkane solution (30.5mmol, 6.1 equivalents, 12.2mL, 2.5mol / L) dropwise into a three-necked flask, add toluene at the same time, stir for 30min, and heat to reflux to prepare 1,4-dilithium naphthalene (nucleophile).

[0077] 2,4,6-Trichloro-1,3,5-triazine (10 mmol, 2 equivalents, 1882 mg, purity: 98%) was dissolved in 5 mL of dry 1,4-dioxane, and the dissolved 2 , 4,6-trichloro-1,3,5-triazine was slowly added dropwise into the three-necked flask, and refluxed for 22 hours.

[0078] After reflux, cool to room temperature naturally, add saturated ammonium chloride solution to quench the reaction, filter the filter residue, wash the filter residue with water to remove lithium salt, then wash with ethyl acetate, methanol and other organic solvents to remove small molecule produ...

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Abstract

The invention discloses a large-scale preparation method for a covalence copolymer with a triazine frame. The method comprises the steps of 1, preparing a nucleophilic reagent; 2, performing a polymerization reaction, wherein the prepared nucleophilic reagent and a triazine compound are mixed in a reaction solvent under the protective atmosphere, a reaction is performed under the temperature of 80-120 DEG C, and cooling is performed to reach the room temperature to obtain a reaction mixture; 3, performing postprocessing, wherein a quenching agent is added into the reaction mixture, and filtering, cleaning and drying are performed to obtain the covalent triazine polymer. A wet method is adopted for preparing the covalent triazine polymer, reaction conditions are simple, the production costis low, and the good industrial application prospect is achieved. The preparation method has no special requirement for operation equipment, the reaction temperature is not high, and therefore industrialized enlarged production is easily performed.

Description

technical field [0001] The invention belongs to the technical field of organic chemical synthesis, and relates to a preparation method of a covalent triazine polymer, in particular to a large-scale preparation method of a covalent polymer with a triazine skeleton. Background technique [0002] Covalent organic frameworks (COFs) have attracted extensive attention from scientific research and industry due to their potential applications in gas separation, catalysis, optoelectronics, energy storage and sensors. Covalent triazine frameworks (CTFs) are covalent organic frameworks with triazine rings as repeating units. At present, the methods for synthesizing covalent triazine framework materials are generally ionothermal method and superacid catalysis method. Among them, the ionothermal method is to mix the dicyanide monomer and zinc chloride in an ampoule, fill it with a protective atmosphere, and react at 400°C for 40 hours. Due to the limited volume of the ampoule, this meth...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G83/00
CPCC08G83/008
Inventor 文珂陈涛胡维波胡文敬李文茜王焯李昆昂姜标
Owner SHANGHAI ADVANCED RES INST CHINESE ACADEMY OF SCI
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