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Preparation method of 4,4'-bi(2-trifluoromethyl-4-aminophenoxyl)biphenyl

A technology of aminophenoxy and trifluoromethyl, applied in 4 fields, can solve the problems of high toxicity of hydrazine hydrate, increase of waste water treatment cost, low yield, etc., and achieve the effect of convenient source of raw materials, less types of use, and simple operation

Inactive Publication Date: 2009-10-21
DONGHUA UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

But the shortcoming of this method is: (1) use hydrazine hydrate, cause a large amount of ammonia gas to be produced in the production process, be unfavorable for environmental protection; (2) hydrazine hydrate toxicity is big, has increased the labor protection cost of operator and operating place; 3) After the reaction is finished, a large amount of waste water containing hydrazine hydrate and its by-products will be produced, which virtually increases the cost of waste water treatment; (4) the yield is low; (5) recrystallization and purification operations are required, and high-purity products cannot be obtained in one step

Method used

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  • Preparation method of 4,4'-bi(2-trifluoromethyl-4-aminophenoxyl)biphenyl

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Embodiment 1

[0033] 56.4 grams (0.10 moles) of 4,4'-bis(2-trifluoromethyl-4-nitrophenoxy)biphenyl, 700 milliliters of methanol solvent, 700 milliliters of N-methyl-2-pyrrolidone, 3.2 grams 10% (mass percentage content of metal palladium) palladium / carbon catalyst is added to the high-pressure reactor, hydrogen gas is passed, stirred, the residual air is replaced, hydrogen gas is continued, the temperature is raised to 40 ° C ~ 80 ° C, and the pressure in the reactor is maintained at 0.2 MPa~1.0MPa, keep the reaction for 4 hours, cool the reaction system to room temperature, slowly release the pressure, and pass nitrogen to replace all the residual hydrogen, ensure the inert atmosphere in the high-pressure reactor, filter, recover the filter residue (catalyst), and set aside Mother liquor, concentrate mother liquor, make its solid content control in the scope of 40%-80%, cool and stand, separate out white crystal product, filter, wash with deionized water 2~3 times, 25 ℃ of vacuum drying, ob...

Embodiment 2

[0037] 56.4 grams (0.10 moles) of 4,4'-bis(2-trifluoromethyl-4-nitrophenoxy)biphenyl, 452 milliliters of ethanol solvent, 678 milliliters of N,N-dimethylacetamide, 5.6 Add the palladium / charcoal catalyst of gram 1% (the mass percent of metal palladium) into the autoclave, feed hydrogen, stir, displace the residual air, continue to feed hydrogen, heat up to 40°C to 80°C, and maintain the pressure in the reactor 0.2MPa~1.0MPa, keep the reaction for 4 hours, cool the reaction system to room temperature, slowly release the pressure, and pass nitrogen to replace all the residual hydrogen, ensure the inert atmosphere in the high-pressure reactor, filter, recover the filter residue (catalyst), and leave Take the mother liquor, concentrate the mother liquor so that its solid content is controlled within the range of 40%-80%, cool and stand still, a white crystal product is precipitated, filter, wash with deionized water 2 to 3 times, and dry under vacuum at 25°C to obtain 45.3 g (prod...

Embodiment 3

[0039] 56.4 grams (0.10 moles) of 4,4'-bis(2-trifluoromethyl-4-nitrophenoxy)biphenyl, 1000 milliliters of ethanol solvent, 690 milliliters of ethylene glycol solvent, 0.6 gram of 15% (metal The palladium / carbon catalyst of the mass percentage of palladium) is added to the high-pressure reactor, hydrogen is passed, stirred, the residual air is replaced, the hydrogen is continued, the temperature is raised to 40°C-80°C, and the pressure in the reactor is maintained at 0.2MPa-1.0MPa , keep the reaction for 2 hours, cool the reaction system to room temperature, slowly release the pressure, and pass nitrogen to replace all residual hydrogen, ensure that the autoclave is an inert atmosphere, filter, reclaim the filter residue (catalyst), retain the mother liquor, concentrate the mother liquor , make its solid content control in the scope of 40%-80%, cool and stand still, separate out white crystal product, filter, wash 2~3 times with deionized water, 25 ℃ of vacuum dryings, obtain 46...

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Abstract

The invention relates to a preparation method of 4,4'-bi(2-trifluoromethyl-4-aminophenoxyl)biphenyl, comprising the steps of adding 4,4'-bi(2-trifluoromethyl-4-nitrophenoxyl)biphenyl, an organic mixed solvent containing alcohols, and a catalyst in a high pressure reaction kettle, infusing hydrogen, stirring, substituting residual air, continuously infusing hydrogen, heating and raising temperature, reacting for 2-4 hours, cooling the reaction system to room temperature, slowly discharging pressure, and infusing nitrogen to substitute all residual air so as to ensure that the high pressure reaction kettle is in inert atmosphere, filtering, recovering filter residue, maintaining the mother liquid, condensing the mother liquid such that the solid content of the mother liquid is in the range of 40-80%, cooling, putting the mother liquid aside, separating out white crystal product, filtering, washing and drying to obtain 4,4'-bi(2-trifluoromethyl-4-aminophenoxyl)biphenyl solid. The method has a simple technology, low cost, high purity and yield, and is environment-friendly and suitable for commercial production.

Description

technical field [0001] The invention belongs to the field of preparation of aromatic fluorine-containing organic compounds, in particular to a preparation method of 4,4'-bis(2-trifluoromethyl-4-aminophenoxy)biphenyl. Background technique [0002] Aromatic polyimide has excellent thermal stability, chemical stability, excellent mechanical properties, electrical properties and resistance to organic solvents, and has been widely used in aerospace, electronic microelectronics, electrical and other fields. Because of its high temperature resistance, high strength, corrosion resistance, good insulation, and simple film forming process, it is an excellent functional material that can meet the performance requirements of LCD (liquid crystal display). [0003] Fluorine-containing polyimide materials not only have the above-mentioned excellent properties, but also have very excellent optical transparency, flame retardancy and excellent molding processability. In addition, its dielect...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C217/90C07C213/02
Inventor 虞鑫海
Owner DONGHUA UNIV
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