Tubular continuous o-fluorophenol production method

A technology of o-fluorophenol and o-fluoroaniline, which is applied in the field of tubular continuous production of o-fluorophenol, can solve the problems of reverse mixing of materials and uneven temperature distribution of materials, and improve the yield of diazonium reaction, increase yield, The effect of increasing product yield

Inactive Publication Date: 2016-04-13
ZHEJIANG LINJIANG CHEM
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0013] The invention provides a method for continuous tubular production of o-fluorophenol. The method adopts a continuous tubular production method, which solves the problems of back-mixing of materials and uneven temperature distribution of materials in kettle reactions.

Method used

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  • Tubular continuous o-fluorophenol production method
  • Tubular continuous o-fluorophenol production method

Examples

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Embodiment 1

[0044] Step (1): Tubular diazonium reaction: pump 220Kg o-fluoroaniline and 600Kg dichloromethane into the stirred tank, stir well and pump into the o-fluoroaniline high tank; then pump into the stirred tank

[0045] 660Kg of nitrosylsulfuric acid solution (the concentration of nitrosylsulfuric acid is 45.8wt%) and 355Kg of concentrated sulfuric acid are pumped into the nitrosylsulfuric acid header tank after stirring evenly. Open the bottom valves of the two high-level tanks, control the flow ratio to 1:1.24, mix evenly through the static mixer and enter the tubular diazonium reactor, the molar ratio of o-fluoroaniline and nitrosyl sulfuric acid is 1:1.2; temperature control At 20°C, the generated diazo solution enters the liquid storage tank.

[0046] Step (2): Tubular hydrolysis reaction: 550Kg copper sulfate pentahydrate and 1210Kg water are put into the reactor, stirred and clarified, then pumped into the copper sulfate solution high level tank; the diazo solution in the ...

Embodiment 2

[0049] Step (1): nitric acid was added to the remaining acid solution recovered in Example 1, and the mass fraction of nitric acid in the mixed solution obtained by stirring and mixing was 25.5wt%. Sulfur dioxide is absorbed in the falling film absorption tower connected in two series, and when the concentration of nitrosyl sulfuric acid in the obtained nitrosyl sulfuric acid solution A is 30wt%, the nitrosyl sulfuric acid solution A is produced.

[0050] Step (2): Tubular diazonium reaction: add a dichloromethane solution of o-fluoroaniline (220Kg) into the stirred tank, stir evenly and pump it into the o-fluoroaniline-dichloromethane high level tank; then pump it into the stirred tank The nitrosylsulfuric acid solution A1000kg that step (1) makes is pumped into the nitrosylsulfuric acid head tank after stirring evenly. Open the bottom valves of the two high level tanks, and control the molar ratio of o-fluoroaniline and nitrosyl sulfuric acid to be 1:1.2. After the static m...

Embodiment 3

[0055] Step (1): Tubular diazonium reaction: 44.4g o-fluoroaniline and 240g dichloromethane are mixed and stirred (o-fluoroaniline solution); 132g nitrosylsulfuric acid (46.16wt%) is mixed and stirred with 66g vitriol oil ( nitrosylsulfuric acid solution). The o-fluoroaniline solution and the nitrosyl sulfuric acid solution were pumped into the silica gel tube by a peristaltic pump to carry out the diazotization reaction. The silica gel tube was placed in a water bath at 20° C., and the residence time in the tube was 15 s.

[0056] Step (2): Tubular hydrolysis reaction: Mix 100g of copper sulfate pentahydrate and 200g of water to form a clarified liquid and a diazo liquid (maintain the liquid temperature at 20°C). The peristaltic pump is pumped into the silicone tube for tubular hydrolysis reaction. The tube length is 20 m. The silicone tube is placed in an oil bath at 135° C., and the residence time in the tube is 20 min to obtain a hydrolyzate.

[0057] Step (3): Extraction...

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Abstract

The present invention discloses a tubular continuous o-fluorophenol production method comprising tubular diazo reaction of a nitrosyl sulfuric acid solution and an o-fluoroaniline solution in a tubular reactor to obtain a diazo solution; tubular hydrolysis reaction of the diazo solution and a copper sulphate water solution in the tubular reactor to obtain a hydrolysis solution; and after-treatment of the hydrolysis solution to obtain o-fluorophenol. The method uses the tubular reactor for the tubular diazo reaction and the tubular hydrolysis reaction to solve the phenomenon of material backmixing and uneven temperature distribution of kettle-type reaction, reduces the incidence of side effects, and improves the yield of the product.

Description

technical field [0001] The invention belongs to the field of synthesis of organic intermediates, in particular to a method for tubular continuous production of o-fluorophenol. Background technique [0002] O-fluorophenol is mainly used in the synthesis of new fluorine-containing antibacterial and anti-inflammatory drugs, insecticides, paraffinicides, herbicides and intermediates of liquid crystal materials. [0003] There are many synthetic methods for the preparation of o-fluorophenol. According to the raw material route, there are mainly low-temperature fluorination of phenol, hydrolysis of o-fluorobromobenzene, and diazotization hydrolysis of o-fluoroaniline. [0004] 1. Dissolve phenol in an appropriate amount of solvent, lower the temperature to -10~-3°C, and then pass in fluorine gas diluted with nitrogen to react to obtain o-fluorophenol and p-fluorophenol, the ratio of which is 57 :14, the synthesis equation is shown in Equation 1: [0005] [0006] Formula 1 ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C37/045C07C39/27
CPCC07C37/045C07C245/20
Inventor 易苗吴然吴冬沈焕军
Owner ZHEJIANG LINJIANG CHEM
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