Method for preparing 1,4-di(4-amino-benzene oxygen) benzene

Abstract

The invention relates to a preparation method for 1, 4-double (4-amido phenoxyl) benzene. The method comprises the steps as follows: (1) hydrochinone and 4-halogenated nitrobenzene with a mole rate of 1.00: 1.80 to 2.80 are heated to carry a back flow water dividing reaction for 2 to 18 hours inside halogen agent, strong polarity non-proton or organic solvent system; the reaction is condensed and the reaction article system is cooled; water is filled in; a Kelly solid product is separated out and then is filtered and dried; (2) 1, 4-double (4-nitryl phenoxyl) benzene reacts for 2 to 20 hours by the common effect of ferric chloride / 20 to 95 percent hydrazine hydrate reduction system, alcohol alike solvent and active carbon under a temperature ranging from 50 DEG C to 90 DEG C, and then the 1, 4-double(4-nitryl phenoxyl) benzene is deoxidized to the 1, 4-double (4-amido phenoxyl) benzene crystal product. The invention has the advantages of easy operation, environment protection, being suitable to be used for industrial production, high product yield and more than 99 percent of purity. Besides, the solvent can be recycled and applied again and again.

Description

technical field [0001] The invention belongs to the field of preparation of aromatic dibasic primary amines, in particular to a preparation method of 1,4-bis(4-aminophenoxy)benzene. Background technique [0002] Aromatic polyimide has excellent thermal stability, nuclear radiation resistance, excellent mechanical properties, electrical properties and resistance to organic solvents, and has been widely used in aerospace, electronic microelectronics, electrical and other fields. [0003] With the development of high-performance, lightweight, thin, and refined information electronic products, higher requirements are put forward for the insulation materials of flexible copper clad laminates (FCCL), such as high heat resistance, low dielectric loss, and high strength. Wait. Therefore, polyimide materials have attracted much attention in the field of FCCL, especially thermoplastic polyimide materials used in two-layer FCCL. [0004] Aromatic primary diamines are one of the impor...

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Problems solved by technology

[0019] The disadvantages of this preparation method are: (1) the operation process is complicated, and there are many kinds of organic solvents used, which virtually increases the cost of purchase and storage and transportation; (2) in the synthesis of 1,4-bis(4-nitrophenoxy ) In the process of benzene, the reaction mixture is directly poured into the mixed solution of methanol and water to precipitate out the product, resulting in serious waste water, high treatment costs, and being unfavorable for environmental protection; (3) organic solvent recovery difficulty; (4) synthetically obtained 1 , 4-bis(4 nitrophenoxy)benzene also needs to be recrystallized through glacial acetic acid, which not only increases the cost, but also additionally produces three wastes; (5) 10% Pd / C is used in the reduction reaction, resulting in product cost (6) the 1,4-bis(4-aminophenoxy)benzene obtained by the reduction reaction also needs to be washed with methanol, which not only increases the cost, produces three wastes, but also increases the The burden of solvent recovery; (7) the yield of the first step and the second step is on the low side, resulting in a lower total yield, only 67%*65%=43.55%

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