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Preparation method of 3-fluorophenol

A technology of fluorophenol and aminophenol, which is applied in the field of preparation of 3-fluorophenol, can solve the problems of unsuitability for industrial production, high technical difficulty, and rare raw materials, and achieve the effects of low environmental protection pressure, simple process equipment, and low raw material cost

Inactive Publication Date: 2015-01-14
FUXIN SIWEI HALIDE
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0027] This is the laboratory preparation method with the highest cost, the most technical difficulty and rare raw materials among the known preparation methods, which is not suitable for industrial production

Method used

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  • Preparation method of 3-fluorophenol
  • Preparation method of 3-fluorophenol
  • Preparation method of 3-fluorophenol

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0043] (1) 1000L equipped with frequency conversion stirring, solvent metering tank, alkali solution dripping tank, reflux condenser, temperature display gauge, screw conveyor, add 600L of toluene into the lead-lined reaction kettle, start stirring, and add it evenly by the screw conveyor at room temperature The raw material m-aminophenol is 200kg, and the speed of the reactor is gradually increased to 100red / min. After all the raw materials are dissolved, the reactor is sealed, and the jacketed brine cooling valve of the reflux condenser is opened, and the anhydrous hydrofluoric acid metering tank is dripped into the reactor. Add 110kg of anhydrous hydrofluoric acid, and control the reaction temperature to be 20-25°C. After the anhydrous hydrofluoric acid was added dropwise, the reaction was incubated for 60 minutes.

[0044] (2) Open the cooling brine valve of the jacket of the reaction kettle, and after the temperature in the reaction kettle reaches -10°C, add KNO evenly fr...

Embodiment 2

[0050] (1) 1000L is equipped with frequency conversion stirring, solvent metering tank, alkali solution dripping tank, reflux condenser, temperature indicator, lead-lined reaction kettle of screw conveyor, add 600L of fluorobenzene into the reaction kettle, start stirring, and the screw conveyor is evenly distributed at room temperature Add 200kg of raw material m-aminophenol, and gradually increase the speed of the reactor to 100red / min. After all the raw materials are dissolved, close the reactor, open the jacketed brine cooling valve of the reflux condenser, and flow from the anhydrous hydrofluoric acid metering tank to the reactor. 120kg of anhydrous hydrofluoric acid was added dropwise to the mixture, and the reaction temperature was controlled to be 20-25°C. After the anhydrous hydrofluoric acid was added dropwise, the reaction was incubated for 60 minutes.

[0051] (2) Open the cooling brine valve of the jacket of the reaction kettle, and after the temperature in the re...

Embodiment 3

[0057] (1) 1000L is equipped with frequency conversion stirring, solvent metering tank, alkali solution dripping tank, reflux condenser, temperature display gauge, lead-lined reaction kettle with screw conveyor, add m-fluorotoluene 600L, start stirring, and the screw conveyor Evenly add 200kg of raw material m-aminophenol, and gradually increase the speed of the reactor to 100red / min. After all the raw materials are dissolved, seal the reactor, open the jacketed brine cooling valve of the reflux condenser, and flow from the anhydrous hydrofluoric acid metering tank to the reactor. 115kg of anhydrous hydrofluoric acid was added dropwise to the mixture, and the reaction temperature was controlled to be 20-25°C. After the anhydrous hydrofluoric acid was added dropwise, the reaction was incubated for 60 minutes.

[0058] (2) Open the cooling brine valve of the jacket of the reaction kettle, and after the temperature in the reaction kettle reaches -10°C, add KNO evenly from the scr...

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Abstract

The invention relates to a preparation method of 3-fluorophenol. According to the preparation method, m-aminophenol is used as a raw material, fluoro-substitution reaction is performed in an organic solvent by quantitatively using anhydrous hydrofluoric acid and KNO2 is used as a diazotization reagent, so that the environmental pressure brought by recovering hydrofluoric acid is alleviated; the organic solvent is recovered and reused, so that the environmental treatment pressure is alleviated to the maximum extent. The preparation method provided by the invention is low in cost of raw materials, mild in reaction condition and simple in equipment and provides a feasible process line for industrial production of 3-fluorophenol.

Description

technical field [0001] The invention is a preparation method of fluorine-containing phenol chemicals, and particularly proposes a preparation method of 3-fluorophenol. Background technique [0002] 3-Fluorophenol is a colorless transparent liquid, and is a commonly used chemical intermediate used in the synthesis of liquid crystal materials, pharmaceuticals, antibacterial agents, insecticides and other chemical intermediates. [0003] The known preparation method of 3-fluorophenol is as follows: [0004] 1. Preparation method of m-fluoroaniline by diazotization and hydrolysis [0005] [0006] The market price of the raw material m-fluoroaniline is relatively high, and the phenol-containing wastewater produced by the diazotization reaction is difficult to pass under the current environmental protection situation. [0007] 2. Pyrolysis preparation method of m-aminophenol fluoroborate [0008] [0009] Fluoroborate pyrolytic fluorination generally has a recognized flu...

Claims

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Application Information

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IPC IPC(8): C07C39/27C07C37/62
CPCC07C37/62C07C37/685C07C37/72C07C37/74C07C37/86
Inventor 吕尚刘冶高金胜吕铁环
Owner FUXIN SIWEI HALIDE
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