Preparation method of 2,2-bis(3-amino-4-hydroxyphenyl)hexafluoropropane
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A technology of hydroxyphenyl and hexafluoropropane, which is applied in the field of preparation of monomer 2,2-dihexafluoropropane, can solve the problems of expensive palladium carbon, potential safety hazards, and high cost, and achieve low production equipment requirements and high repeatability Good, simple operation effect
Active Publication Date: 2017-07-11
河北君瑞沣新材料有限公司
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Problems solved by technology
The use of palladium carbon and nickel hydrogenation has great potential safety hazards, and the price of palladium carbon is expensive and the cost is high
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Embodiment 1
[0021] Add 3.36 kilograms of 2,2-bis(4-hydroxyphenyl) hexafluoropropane in the reactor, 4.04 kilograms of potassium nitrate, 12 kilograms of 80% phosphoric acid, and heat up to 85°C for reaction (molar ratio is: 2,2-bis( 4-Hydroxyphenyl)hexafluoropropane: potassium nitrate: 80% phosphoric acid = 1:4:10), after the reaction of the raw materials is complete, cool down to below 10°C, precipitate a solid, filter, wash and dry to obtain 2,2-bis( 4.22 kg of 3-nitro-4-hydroxyphenyl) hexafluoropropane, yellow solid, yield 98.9%.
Embodiment 2
[0023] Add 3.36 kilograms of 2,2-bis(4-hydroxyphenyl) hexafluoropropane in the reactor, 3.54 kilograms of potassium nitrate, 9.3 kilograms of 80% phosphoric acid, and heat up to 80°C for reaction (the molar ratio is: 2,2-bis( 4-Hydroxyphenyl)hexafluoropropane: potassium nitrate: 80% phosphoric acid = 1:3.5:8), after the reaction of raw materials is complete, cool down to below 10°C, precipitate solid, filter, wash and dry to obtain 2,2-bis( 4.1 kg of 3-nitro-4-hydroxyphenyl)hexafluoropropane, yellow solid, yield 96.3%.
Embodiment 3
[0025] Add 3.36 kilograms of 2,2-bis(4-hydroxyphenyl) hexafluoropropane, 4.55 kilograms of potassium nitrate, 13.8 kilograms of 80% phosphoric acid in the reactor, and heat up to 90°C for reaction (molar ratio is: 2,2-bis( 4-Hydroxyphenyl)hexafluoropropane: potassium nitrate: 80% phosphoric acid = 1:4.5:12), after the reaction of the raw materials is complete, cool down to below 10°C, precipitate a solid, filter, wash and dry to obtain 2,2-bis( 4.223 kg of 3-nitro-4-hydroxyphenyl)hexafluoropropane, yellow solid, yield 99.1%.
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Abstract
The invention relates to a method for preparing 2,2-Bis(3-amino-4-hydroxyphenyl)hexafluoropropane. The method includes the steps that 2,2-Bis(4-hydroxyphenyl)hexafluoropropane, potassium nitrate and 80% phosphoric acid are added into a reaction kettle, the temperature rises to 80-90 DEG C for reacting, the temperature drops to below 10 DEG C after reacting is completed, solids are precipitated for filtration, and 2,2-Bis(3-nitro-4-hydroxyphenyl)hexafluoropropane is obtained by means of washing and drying; zinc powder is added into ethyl alcohol, then ammonium chloride, acetic acid and water are added, stirring is conducted for one hour at the temperature of 60 DEG C, afterwards, the 2,2-Bis(3-nitro-4-hydroxyphenyl)hexafluoropropane is added for reacting under the reflux condition, the temperature drops to 30 DEG C for filtration after reacting is completed, a filter cake is washed through ethyl alcohol, filter liquor is merged, solvent is evaporated out through decompression, solids are precipitated, and the 2,2-Bis(3-amino-4-hydroxyphenyl)hexafluoropropane is obtained by means of filtering. The method is high in yield, easy to operate, good in repeatability and capable of being applied to heat-resistance polymer raw materials.
Description
technical field [0001] The invention relates to a preparation method of monomer 2,2-bis(3-amino-4-hydroxyphenyl)hexafluoropropane which can be used as polyimide special polymer functional material. Background technique [0002] 2,2-bis(3-amino-4-hydroxyphenyl)hexafluoropropane is a high-temperature polymer, which is mainly used as a raw material for heat-resistant polymers, such as aerospace, electronic microelectronics, electrical technology and other technical fields , high temperature resistant materials are getting more and more attention, in addition to synthetic wood flame retardants can also be used. [0003] The preparation methods of 2,2-bis(3-amino-4-hydroxyphenyl)hexafluoropropane are currently reported as follows: [0004] 1) Patent CN200910164249.5 uses 2,2-bis(4-hydroxyphenyl)hexafluoropropane as raw material, and first nitrates it with mixed acid to obtain 2,2-bis(3-nitro-4-hydroxyphenyl)hexafluoropropane , and then hydrazine hydrate / SeO 2 -SnO reduction to...
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