Preparation method of monomeric diamine compound of polyimide

A technology of diamine compound and polyimide, applied in the field of preparation of monomeric diamine compound, can solve the problems of low yield, complicated preparation process, etc., and achieves safe and simple reaction, high solubility, and avoids troublesome post-processing. Effect

Pending Publication Date: 2022-05-13
西安爱德克美新材料有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0009] The main purpose of the present invention is to provide a method for preparing a monomer diamine compound of polyimide, which solves the problems of complicated preparation process and low yield in the preparation method of the prior art

Method used

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  • Preparation method of monomeric diamine compound of polyimide
  • Preparation method of monomeric diamine compound of polyimide
  • Preparation method of monomeric diamine compound of polyimide

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preparation example Construction

[0030] More specifically, the preparation method of the monomeric diamine compound of the polyimide disclosed by the present invention comprises the steps of:

[0031] Step 1: Add o-chloro-p-nitrophenol and the first inorganic base into the mixed system of dioxane and water, then add a methylating reagent to react, extract and separate to obtain o-chloro-p-nitroanisole solution ;

[0032] Further, the molar ratio of o-chloro-p-nitrophenol and the first inorganic base is 1:1-1.5, preferably 1:1.2; the molar ratio of o-chloro-p-nitrophenol and methylating agent is 1:1-1.5 , preferably 1:1.3. Dioxane and water are used as solvents, which can be determined according to the dosage and solubility of o-chloro-p-nitrophenol and the first inorganic base, and can be set in excess.

[0033] Further, in step 1, add o-chloro-p-nitrophenol and the first inorganic base to the mixed system of dioxane and water and then raise the temperature to 40-50°C, then add a methylating reagent and hea...

Embodiment 1

[0050] This embodiment discloses a method for preparing a polyimide monomer diamine compound, which specifically includes the following steps:

[0051] Step 1: Add 174ml of water, 348ml of dioxane, 173.6g of o-chloro-p-nitrophenol, and 165.6g of potassium carbonate to the reaction device in sequence. Carry out heat preservation reaction at 90°C. After the reaction, cool down the system to 40°C. Add 348ml of water and 695ml of toluene to the system for extraction and washing. After liquid separation, the o-chloro-p-nitroanisole solution is obtained. , the yield is 100%;

[0052] Step 2: Take another reaction device and add the p-o-chloro-p-nitrotoluene ether solution prepared in step 1, potassium carbonate 165.5g, phenylboronic acid 134.2g, tetrabutylammonium bromide 96.7g, add tetrakis (triphenylphosphine ) Palladium (0) 1.16g, purified water 348ml, start stirring, heating, the temperature of the system is raised to 80°C for reaction, and the reaction is kept for 5 hours. Aft...

Embodiment 2

[0056] This embodiment discloses a method for preparing a monomeric diamine compound of polyimide, comprising steps:

[0057] Step 1: Add 174ml of water, 348ml of dioxane, 173.6g of o-chloro-p-nitrophenol, and 40.0g of sodium hydroxide to a reaction device in sequence, adjust the temperature of the system to 40°C, and then add 126.1g of dimethyl sulfate , the system was heated up to 80°C for heat preservation reaction. After the reaction, the system was cooled to 40°C, and 348ml of water and 695ml of toluene were added to the system for extraction and water washing. After liquid separation, o-chloro-p-nitroanisole solution was obtained, which was detected by HPLC The content is 97.8%, and the yield is 100%;

[0058] Step 2: get another reaction device to add successively the p-o-chloro-p-nitrotoluene ether solution that step 1 makes, potassium carbonate 165.5g, phenylboronic acid 134.2g, tetrabutylammonium bromide 96.7g, add palladium catalyst two ( Triphenylphosphine)palladi...

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Abstract

The preparation method comprises the following steps: adding o-chloro-p-nitrophenol and a first inorganic base into a mixed system of dioxane and water, then adding a methylation reagent, carrying out a reaction, and carrying out extraction and liquid separation so as to obtain an o-chloro-p-nitroanisole solution; adding potassium carbonate, phenylboronic acid and tetrabutylammonium bromide into the o-chloro-p-nitrotoluene ether solution to carry out Suzuki coupling reaction, then adding second inorganic alkali to carry out alkaline hydrolysis, and carrying out deprotection reaction to obtain 2-hydroxy-5-nitrobiphenyl; the preparation method comprises the following steps: carrying out esterification reaction on 2-hydroxyl 5-nitrobiphenyl, triethylamine, an esterification catalyst and p-nitrobenzoyl chloride to obtain 4-nitrobenzoic acid-5-nitrobiphenyl 2-phenolic ester; and carrying out hydrogenation reaction on the 4-nitrobenzoic acid-5-nitrobiphenyl 2-phenolic ester and a second reaction solvent. The preparation process adopts classical reaction and conventional operation, the reaction is safe and simple, and high-selectivity and high-quality synthesis of the product is also realized.

Description

technical field [0001] The invention relates to the technical field of chemical synthesis, in particular to a method for preparing a polyimide monomeric diamine compound. Background technique [0002] Generally speaking, in addition to high heat resistance, polyimide (PI) resin also has excellent mechanical strength, wear resistance, dimensional stability, corrosion resistance and other excellent properties, and is widely used in flexible printed circuit boards In the field of electronic materials such as electronic equipment, in addition to the field of electronic equipment, it has been widely used in cutting-edge technology fields such as aviation, aerospace, construction, automobiles, separation membranes, nanometers, and lasers, and has therefore attracted extensive attention from researchers. [0003] The most important raw materials for polyimide are aromatic diamines and aromatic dianhydrides, among which 4,4'-diaminodiphenyl ether (ODA) and 3,3',4,4'- Biphenyltetrac...

Claims

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Application Information

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IPC IPC(8): C07C229/60C07C227/04
CPCC07C227/04C07C201/12C07C229/60C07C205/57C07C205/22C07C205/37
Inventor 杨军义
Owner 西安爱德克美新材料有限公司
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