Preparation method of 4, 4-bi(4-aminophenoxy) biphenyl
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A technology of aminophenoxy and nitrophenoxy, which is applied in 4 fields, can solve the problems of complicated process and long time, and achieve the effect of simple operation, short reaction time and less waste
Inactive Publication Date: 2013-12-18
INST OF PETROCHEM HEILONGJIANG ACADEMY OF SCI
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[0005] The present invention aims to solve the problems of long time and complex process in the existing method for preparing 4,4-bis(4-aminophenoxy)biphenyl, and provides a 4,4-bis(4-aminophenoxy) base) preparation method of biphenyl
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specific Embodiment approach 1
[0008] Specific embodiment one: In this embodiment, a preparation method of 4,4-bis(4-aminophenoxy)biphenyl is carried out through the following steps: 4,4-bis(4-nitrophenoxy) ) Biphenyl and palladium / charcoal catalyst are added to alcohol solvent and placed in the reaction kettle, and then replaced with nitrogen gas, then filled with hydrogen, and then reacted at 60-70°C for 3-4 hours, and then used N 2 gas displacement, and then filter to collect the liquid phase, then cool to room temperature to precipitate a solid product, then filter to obtain the solid phase, then vacuum dry at room temperature to obtain 4,4-bis(4-aminophenoxy)biphenyl, namely Complete the preparation of 4,4-bis(4-aminophenoxy)biphenyl.
[0009] The method for preparing 4,4-bis(4-aminophenoxy)biphenyl in this embodiment has short reaction time, obvious energy saving and consumption reduction; simple operation, less chemical raw materials involved; solvent and catalyst can be recycled, and three wastes ar...
specific Embodiment approach 2
[0010] Embodiment 2: This embodiment differs from Embodiment 1 in that the mass fraction of the palladium / charcoal catalyst palladium is 1% to 10%. Others are the same as in the first embodiment.
specific Embodiment approach 3
[0011] Specific embodiment three: the difference between this embodiment and specific embodiment one or two is: the alcoholic solvent is methanol, ethanol, isopropanol, n-propanol, n-butanol, 1,2-propanediol and 1, 3-propanediol, a mixture of one or more of them in any ratio. Others are the same as in the first or second embodiment.
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Abstract
The invention provides a preparation method of 4, 4-bi(4-aminophenoxy) biphenyl, aiming at solving the problems that the existing method for preparing 4, 4-bi(4-aminophenoxy) biphenyl costs a long time and is complex in process. The method specifically comprises the following steps of: adding 4, 4-bi(4-nitrophenoxy) biphenyl and a palladium/carbon catalyst to an alcohols solvent; transferring into a reaction kettle; filling nitrogen to replace air; filling hydrogen; reacting for 3 to 4 hours at 60 to 70 DEG C; replacing with N2 gas; filtering again; collecting a liquid phase substance; cooling until reaching room temperature; filtering again to obtain a solid phase; and drying in a vacuum manner at room temperature, thus obtaining the 4, 4-bi(4-aminophenoxy) biphenyl. The method costs a little time for reaction, is obvious in energy conservationsaving and consumption reductionreducing, and simple in operation; a small amount of chemical raw materials related are used; the product yield is high and reaches 85%; and the purity reaches more than 99%.
Description
technical field [0001] The invention relates to a preparation method of 4,4-bis(4-aminophenoxy)biphenyl. Background technique [0002] Aromatic polyimide has excellent thermal stability, radiation resistance, flame retardancy, organic solvent resistance and excellent high and low temperature mechanical properties and electrical properties. It is used in aerospace, electronics, automobiles, ships, electrical and other high performance fields are widely used. [0003] With the development of information electronic products towards high performance, light weight, thinner and finer, higher requirements are put forward for insulating materials, such as high heat resistance, high strength, low dielectric constant and low dielectric loss, etc. Therefore, polyimide materials are favored in the field of insulation. [0004] 4,4-bis(4-aminophenoxy)biphenyl is one of the important raw materials for the synthesis of polyimide resin, and it can also be used for high temperature resista...
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Patent Type & Authority Applications(China)
IPC IPC(8): C07C217/90C07C213/02
Inventor 曹龙海胡永玲徐晓沐宁志强梁泰硕杨姝鲍春阳徐磊耿嘉阳张秀斌
Owner INST OF PETROCHEM HEILONGJIANG ACADEMY OF SCI
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