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Preparation method of fluorophenol

A technology of p-fluorophenol and synthesis method, which is applied in the field of synthesis of p-fluorophenol, can solve the problems of danger, large amount of waste water discharge and hidden dangers, and achieve the elimination of discharge of acid-containing waste water and by-products, reduction of reaction temperature, The effect of shortening the reaction time

Inactive Publication Date: 2018-10-16
CHANGZHOU UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The process adopts high-risk and high-pollution unit processes such as nitrification, hydrogenation, and diazotization reactions, and the production risk and waste water discharge are large.
[0008] There are many hidden dangers in the above synthetic techniques of p-fluorophenol in terms of safety and environmental protection.

Method used

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  • Preparation method of fluorophenol

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Experimental program
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Effect test

Embodiment 1

[0025] (1) in the 1000ml four-necked flask that thermometer and condenser tube are housed, add 126 gram p-fluorophenyl methyl ethers (1mol), 590 gram 48% hydrobromic acid and 1 gram phase-transfer catalyst tetrabutyl ammonium bromide, Stir vigorously under the protection of nitrogen, heat, react at 80°C for 3 hours, and cool to room temperature. The reaction solution was extracted with 300ml, 200ml, and 100ml of benzene respectively, left to stand for 1 hour, and the organic phases were combined. Benzene was recovered under normal pressure, and the 80-85°C / 20mmHg fraction was collected under reduced pressure to obtain 108 g of p-fluorophenol with a content of 99.2% and a yield of 96.4%.

[0026] (2) Add sodium bromide and concentrated phosphoric acid in proportion to a 500ml reaction flask, and heat and distill to obtain bromine-free hydrogen bromide. Hydrogen bromide gas is passed in the raffinate of step (1), temperature is controlled below 10 ℃, measures hydrobromic acid c...

Embodiment 2

[0029] (1) in the 1000ml four-necked flask that thermometer and condensing tube are housed, add 126 gram p-fluorophenyl methyl ethers (1mol), 650 gram 48% hydrobromic acid and 1.3 gram phase-transfer catalyst tetrabutyl ammonium bromide, Stir vigorously under the protection of nitrogen, heat, react at 80°C for 3 hours, and cool to room temperature. The reaction solution was extracted with 300ml, 200ml, and 100ml of benzene respectively, left to stand for 1 hour, and the organic phases were combined. Benzene was recovered under normal pressure, and the 80-85°C / 20mmHg fraction was collected under reduced pressure to obtain 107 g of p-fluorophenol with a content of 99.4% and a yield of 95.4%.

[0030] (2) Add sodium bromide and concentrated phosphoric acid in proportion to a 500ml reaction flask, and heat and distill to obtain bromine-free hydrogen bromide. Hydrogen bromide gas is passed in the raffinate of step (1), temperature is controlled below 10 ℃, measures hydrobromic aci...

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Abstract

The application relates to a preparation method of fluorophenol. The preparation method comprises the following steps: carrying out demethylation reaction on p-fluoroanisole and hydrobromic acid to generate fluorophenol and methyl bromide; separating the synthesized fluorophenol from a reaction system by using an extraction method; recycling raffinate through hydrogen bromide; directly introducingthe methyl bromide subjected to the demethylation reaction into an aqueous solution containing 15 percent p-methyl sodium benzenesulfinate to generate p-methyl phenylsulfone; concentrating mother liquor from which the p-methyl phenylsulfone is separated to obtain sodium bromide. The obtained sodium bromide can be applied to the step of generating hydrogen bromide. Therefore, the discharge of acid-containing wastewater and byproducts is fundamentally eliminated, and the requirements of clean production are met.

Description

technical field [0001] The invention belongs to the technical field of chemical industry and relates to a synthesis method for preparing p-fluorophenol. Background technique [0002] 4-Fluorophenol is a white crystal with a relative density of 1.1889, a melting point of 48.2°C and a boiling point of 185.6°C. poisonous. Corrosive. Soluble in water, easily soluble in organic solvents such as ethanol and ethyl acetate. [0003] P-fluorophenol is mainly used in antihypertensive drugs nebivolol, 5-HT 1A Synthesis of receptor antagonists and anti-inflammatory, anti-platelet aggregation, antibacterial and other drugs; also used in the synthesis of high-efficiency herbicide flucarbazone; it can also be used in the production of liquid crystal materials. [0004] According to literature reports, [0005] (1) Diazo-fluorination method: take p-aminoanisole as raw material, carry out diazotization reaction in fluoroboric acid medium, filter to obtain its fluoroboric acid diazonium ...

Claims

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Application Information

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IPC IPC(8): C07C37/055C07C39/27C07C315/00C07C317/14
CPCC07C17/093C07C37/055C07C315/00C07C39/27C07C317/14C07C19/075
Inventor 吴卫忠
Owner CHANGZHOU UNIV
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