Process for producing 2,2-di[4-(2-trifluoromethyl-4-nitrophenoxy)phenyl] hexafluoroacetore

A technology of nitrophenoxy and nitrotrifluoromethylbenzene, which is applied in the field of hexafluoropropane preparation, can solve the problems of unfavorable environmental protection, increase of three wastes, increase of chemical unit operations, etc., and achieve convenient source of raw materials and variety of uses The effect of less and simplified process

Inactive Publication Date: 2009-07-29
DONGHUA UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0008] But the shortcoming of this method is: (1) the yield of product is on the low side, and recrystallization yield only has 83%; (2) the organic solvent kind that involves is many, as DMAc, DMF, methyl alcohol etc.
This will inevitably lead to a large amount of waste water and consume a large amount of methanol, which also increases the cost of methanol recovery and the cost of waste water treatment, which is not conducive to environmental protection and reduces production costs; for further recrystallization to purify the product
This not only increases the chemical unit operation, increases the cost of chemical equipment and personnel, but also increases the cost of raw materials and production costs, and also increases the cost of the three wastes.

Method used

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  • Process for producing 2,2-di[4-(2-trifluoromethyl-4-nitrophenoxy)phenyl] hexafluoroacetore
  • Process for producing 2,2-di[4-(2-trifluoromethyl-4-nitrophenoxy)phenyl] hexafluoroacetore
  • Process for producing 2,2-di[4-(2-trifluoromethyl-4-nitrophenoxy)phenyl] hexafluoroacetore

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0025] 33.6 grams (0.10 moles) of 2,2-bis(4-hydroxyphenyl)hexafluoropropane (BHPFP), 47.4 grams (0.21 moles) of 2-chloro-5-nitrotrifluoromethylbenzene (CNB-TF) , 27.6 grams (0.20 moles) of potassium carbonate, 410 milliliters of anhydrous N, N-dimethylformamide were put into the reaction kettle, stirred, heated to 110°C for 5 hours, continued to heat up to 140°C for 5 hours , filtered while it was hot, removed the filter residue, concentrated the mother liquor, recovered the solvent for recycling, cooled and stood still, and precipitated a milky white solid product, filtered, washed 2 to 3 times with pure water, and dried to obtain 69.9 grams of 2,2-bis[4 -(2-Trifluoromethyl-4-nitrophenoxy)phenyl]hexafluoropropane (BNPFP-2TF) milky white solid product (theoretical yield is 71.4 g) with a purity of 99.5% and a melting point of 173.2°C-174.8 ℃ (WRR melting point apparatus, the initial setting temperature is 168 ℃, the heating rate is 1.0 ℃ / min), and its Fourier transform infrare...

Embodiment 2

[0028] 33.6 grams (0.10 moles) of 2,2-bis(4-hydroxyphenyl)hexafluoropropane (BHPFP), 56.4 grams (0.25 moles) of 2-chloro-5-nitrotrifluoromethylbenzene (CNB-TF) , 55.2 grams (0.40 moles) of potassium carbonate, 4490 milliliters of anhydrous N, N-dimethylacetamide were put into the reaction kettle, stirred, heated to 150° C. after reacting for 8 hours, filtered while hot, removed the filter residue, concentrated the mother liquor, The solvent was recovered for recycling, cooled and left to stand, and the milky white solid product was precipitated, filtered, washed 2 to 3 times with pure water, and dried to obtain 68.5 grams of 2,2-bis[4-(2-trifluoromethyl-4-nitrate phenyloxy)phenyl]hexafluoropropane (BNPFP-2TF) milky white solid product (theoretical yield: 71.4 g) with a purity of 99.0%.

[0029] According to the theoretical yield and the actual amount of 2,2-bis[4-(2-trifluoromethyl-4-nitrophenoxy)phenyl]hexafluoropropane (BNPFP-2TF), the calculated 2,2- The yield of bis[4-(2-...

Embodiment 3

[0031]33.6 grams (0.10 moles) of 2,2-bis(4-hydroxyphenyl)hexafluoropropane (BHPFP), 45.1 grams (0.20 moles) of 2-chloro-5-nitrotrifluoromethylbenzene (CNB-TF) , 10.6 grams (0.10 moles) of sodium carbonate, and 600 milliliters of anhydrous N-methyl-2-pyrrolidone were put into the reaction kettle, stirred, heated to 130° C. for 5 hours, continued to heat up to 200° C. for 0.5 hours after the reaction, Filtrate while hot, remove the filter residue, concentrate the mother liquor, recover the solvent for recycling, cool and stand still, and precipitate a milky white solid product, filter, wash 2 to 3 times with pure water, and dry to obtain 65.7 grams of 2,2-bis[4-( 2-trifluoromethyl-4-nitrophenoxy)phenyl]hexafluoropropane (BNPFP-2TF) milky white solid product with a purity of 99.2%.

[0032] Based on the amount of 2,2-bis[4-(2-trifluoromethyl-4-nitrophenoxy)phenyl]hexafluoropropane (BNPFP-2TF) actually obtained and the theoretical yield (71.4 g), calculate The yield of 2,2-bis[4-...

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Abstract

The invention relates to a preparation method of 2, 2-double [4-(2-trifluoromethane-4-nitrobenzene oxy) phenyl] hexafluoropropane. The invention comprises the following steps: (1) mixing 2, 2-double(4-hydroxyl phenyl) hexafluoropropane and 2-chlorine -5-nitryl trifluoromethyl benzene by the mol ratio of 1.0:2.0-2.5, then adding the mixtrue into a mixed solvent of a salifying agent and anhydrous organic solvent for reaction for 5 to 10 hours at 110 to 200 DEG C; (2) filtering when the solvent is hot, eliminating filter residue, condensing mother liquid, cooling and stewing to precipitate a milky solid product, and then filtering, washing and drying the product to obtain the milky solid powder of 2, 2-double [4-(2-trifluoromethyl-4-nitrobenzene oxy) phenyl] hexafluoropropane. The method with simple process, low cost, environment-friendliness and high purity and yield rate is applicable to the industrial production.

Description

technical field [0001] The invention belongs to the field of preparation of hexafluoropropane, in particular to a preparation method of 2,2-bis[4-(2-trifluoromethyl-4-nitrophenoxy)phenyl]hexafluoropropane. 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. [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 dielectric constant, dielectric loss and water absorption are relatively low. It is especial...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C205/38C07C201/12
Inventor 虞鑫海
Owner DONGHUA UNIV
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