Preparation method for C8 side chain substituted fluorine-containing diamine monomer

A fluorine-containing diamine and monomer technology, which is applied in the preparation of carboxylic acid amides, the preparation of organic compounds, chemical instruments and methods, etc. Difficulties and other problems, to achieve the effect of improving light transmittance, high synthesis yield, and reducing order and symmetry

Pending Publication Date: 2020-05-01
YANCHENG TONGHAI BIOTECH CO LTD
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The reason is mainly because diamine monomers with innovative structures generally have a large molecular weight, the reduction of nitro groups is relatively difficult, and the production cost is relatively high, which limits the development of polyimides to a certain extent.

Method used

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  • Preparation method for C8 side chain substituted fluorine-containing diamine monomer
  • Preparation method for C8 side chain substituted fluorine-containing diamine monomer
  • Preparation method for C8 side chain substituted fluorine-containing diamine monomer

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0027] Step 1: Add 1.2L DMAC, 1000g 2,2-bis(3-amino-4-sodium phenolate) hexafluoropropane and 937g bromo-C8 alkane successively to a 10L four-necked reaction flask, start stirring and heating, and maintain React at 80°C for 2-3 hours. After the reaction of the raw materials is completed, turn off the heating, pour out the reaction liquid, and filter while it is hot. The upper layer of filter cake is the by-product sodium bromide, which is collected and stored. The filtrate is naturally cooled to room temperature, and then added to 2.4 Quenched in L water, a large amount of solids will appear at this time, filter with suction, wash the filter cake with 3.5L of water, and dry the filter cake in vacuum to obtain 1296g of pure C8-FN.

[0028] Step 2: Add 1296g C8-FN and 550mL NMP to a 10L four-necked reaction flask, start stirring, then slowly add a mixture of 812g m-nitrobenzoyl chloride and 550mL NMP dropwise, and control the volume of the reaction solution during the dropwise ad...

Embodiment 2

[0031] Step 1: Add 24.3L DMAC, 1000g 2,2-bis(3-amino-4-sodium phenolate) hexafluoropropane and 4684g bromo-C8 alkane to a 30L double-layer glass reactor, start stirring and heating, Maintain the reaction at 166°C for 2-3 hours. After the reaction of the raw materials is completed, turn off the heating, release the reaction liquid, and filter while it is hot. The upper layer of filter cake is the by-product sodium bromide, which is collected and stored. The filtrate is naturally cooled to room temperature, and then added to 48.6 Quenched in L water, a large amount of solids will appear at this time, filter with suction, wash the filter cake with 3.5L of water, and dry the filter cake in vacuum to obtain 1368g of pure C8-FN.

[0032] Step 2: Add 1368g C8-FN and 11.5L NMP to the 30L double-layer glass reactor, start stirring and jacket cooling, when the temperature of the reaction solution drops to 0°C, slowly add 4286g m-nitrobenzene dropwise For the mixed solution of formyl chl...

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Abstract

The invention designs a polyimide diamine monomer C8-FBDA with an innovative structure. According to the invention, C8 side chain alkyl, trifluoromethyl, an imide group and a plurality of benzene ringstructures are simultaneously introduced into the molecular structure of the polyimide diamine monomer, so the regularity and crystallinity of a polymer molecular chain are broken; the free volume ofa polymer is increased; the interaction between molecular chains is reduced; and the film-forming property and optical transparency of polyimide are greatly improved. In the aspect of synthesis of the C8-FBDA, an industrially applicable C8-FBDA production process is developed; and the production process is short in synthesis route, high in yield, cheap and easily available in used raw materials,low in production cost, simple and convenient to operate, friendly to the environment, capable of completely realizing large-scale mass production and extremely high in industrial application value.

Description

technical field [0001] The invention relates to the fields of fine chemical industry and polymer chemistry, in particular to the field of preparation of polyimide polymers. Background technique [0002] In recent years, with the development of optoelectronic devices, traditional transparent glass substrates have been unable to meet the requirements of flexible devices. Colorless and transparent polymers have the advantages of transparency, light weight, and impact resistance. Films, optical thin films, organic photovoltaic solar panels, flexible printed circuit boards and touch panels have received more and more attention. Polyimide has excellent high temperature resistance, dielectric properties and mechanical processing properties, and is the first choice to replace glass substrates. But for traditional polyimide, improving its light transmission performance is the key. [0003] Traditional polyimides are generally brown or brown-yellow transparent materials. This is due...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C237/40C07C231/12C08G73/14C08G73/10
CPCC07C213/06C07C231/02C07C231/12C08G73/1039C08G73/14C07C237/40C07C233/80C07C217/84
Inventor 王辉沈俭一王雪芹
Owner YANCHENG TONGHAI BIOTECH CO LTD
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