Preparation method of C16 side chain substituted fluorine-containing diamine monomer
A technology of fluorine-containing diamine and C16-FN, which is applied to the preparation of carboxylic acid amides, the preparation of organic compounds, chemical instruments and methods, etc., can solve the problems that limit the development of polyimide, the molecular weight of diamine monomers is large, and the nitro Problems such as difficulty in reduction can be achieved to improve light transmittance, high synthesis yield, and reduce order and symmetry
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Embodiment 1
[0027] Step 1: Add 1.2L DMAC, 1000g 2,2-bis(3-amino-4-sodium phenolate)hexafluoropropane and 1483.7g bromoC16alkane to a 10L four-necked reaction flask in sequence, start stirring and heating, Maintain the reaction 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 the Quenched in 2.4L of 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 1788g of pure C16-FN.
[0028] The second step: add 1788g C16-FN and 550mL NMP to the 10L four-necked reaction flask, start stirring, then slowly dropwise add the mixed solution of 812g m-nitrobenzoyl chloride and 550mL NMP to it, and control the concentration of ...
Embodiment 2
[0031] Step 1: Add 24.3L DMAC, 1000g 2,2-bis(3-amino-4-sodium phenolate) hexafluoropropane and 7418g bromo-C16alkane 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 1887g of pure C16-FN.
[0032] Step 2: Add 1887g C16-FN and 11.5L NMP to a 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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