Unlock instant, AI-driven research and patent intelligence for your innovation.

M-fluorophenol preparation method

A technology for m-fluorophenol and m-fluoroaniline, which is applied in the field of preparation of m-fluorophenol, can solve the problems of rare raw materials, difficult oxidation control, unsuitability for industrialization and the like, and achieves the effect of simple operation

Active Publication Date: 2015-05-27
郓城县世炬商贸有限公司
View PDF1 Cites 0 Cited by
  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0014] This process has rare raw materials, expensive raw materials, low yield, high cost, difficult to control oxidation, and is not suitable for industrialization

Method used

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
View more

Image

Smart Image Click on the blue labels to locate them in the text.
Viewing Examples
Smart Image
  • M-fluorophenol preparation method
  • M-fluorophenol preparation method
  • M-fluorophenol preparation method

Examples

Experimental program
Comparison scheme
Effect test

Embodiment １

[0028] Taking m-fluoroaniline as raw material, carry out the following steps successively:

[0029] (1) Add 768kg of 30%% sulfuric acid to a 1000L reactor, add 57kg of m-fluoroaniline dropwise at a temperature of 20°C, after dropping, keep warm at 20°C for 20-30min, cool down to -5°C, add dropwise 38kg of sodium nitrite Dissolve the solution in 122kg of water, after dripping, stir at <5°C for 30 minutes, then keep warm at <5°C for 30 minutes for later use.

[0030] (2) Add 70kg of water, 80kg of 98% sulfuric acid, and 90kg of copper sulfate to a 1000L hydrolysis kettle, then raise the temperature to 135°C, add the product of "step (1)" dropwise at 130-135°C, collect the distillate at the same time, distill out The lower oil layer was separated from the liquid, and the upper oil layer was rectified to collect the 95-96°C / 75mmHg fraction to obtain the m-fluorophenol product with a yield of 74.4% and a content of >99.5%.

Embodiment ２

[0032] Taking m-fluoroaniline as raw material, carry out the following steps successively:

[0033] (1) Add 768kg of 40% sulfuric acid to a 1000L reactor, add 57kg of m-fluoroaniline dropwise at a temperature of 25°C. The solution prepared in 110kg of water, after dripping, was stirred at <5°C for 30 minutes, and then kept at <5°C for later use.

[0034] (2) Add 80kg of water, 90kg of 98% sulfuric acid, and 100kg of copper sulfate to a 1000L hydrolysis kettle, then raise the temperature to 135°C, add the product of "step (1)" dropwise at 130-135°C, collect the distillate at the same time, distill The liquid was left to separate the lower oil layer, and the upper oil layer was rectified to collect the 95-96°C / 75mmHg fraction to obtain the m-fluorophenol product with a yield of 78.8% and a content of >99.5%.

Embodiment 3

[0036] Taking m-fluoroaniline as raw material, carry out the following steps successively:

[0037] (1) Add 768kg of 60% sulfuric acid to a 1000L reactor, add 57kg of m-fluoroaniline dropwise at a temperature of 30°C. The solution made of water, after dripping, was stirred at <5°C for 30 minutes, and then kept at <5°C for later use.

[0038] (2) Add 80kg of water, 90kg of 98% sulfuric acid, and 100kg of copper sulfate into a 1000L hydrolysis kettle, then raise the temperature to 135°C, add the product of "step (1)" dropwise at 130-135°C, collect the distillate at the same time, distill out The liquid was left to separate the lower oil layer, and the upper oil layer was rectified to collect the 95-96°C / 75mmHg fraction to obtain the m-fluorophenol product with a yield of 75.5% and a content of >99.5%.

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
Login to View More

PUM

No PUM Login to View More

Abstract

The invention relates to the field of chemical industry, and relates to an m-fluorophenol preparation method which comprises the following steps: (1) in a diazotization kettle, using m-fluoroaniline as a starting reactant for diazotization reaction with 30%-60% sulfuric acid; and (2) adding water, concentrated sulfuric acid and copper sulfate into a hydrolysis tank, dripping a product of the steps (1) for hydrolysis reaction at 90-160 DEG C, and collecting a distillate to obtain the product m-fluorophenol. The method has the advantages of easily-obtained raw material, simple operation, no need of special equipment, and the product yield can reach 74% to 79%, and is far higher than that of a previous process.

Description

(1) Technical field [0001] The invention relates to the field of chemical industry, and relates to a preparation method of m-fluorophenol. (2) Background technology [0002] Meta-fluorophenol is an important chemical intermediate, which is mainly used in the preparation of liquid crystals, pharmaceuticals, and pesticide intermediates. Its English name: 3-Fluorophenol, molecular formula: C 6 h 5 FO.CAS number is: 372-20-3 Structural formula: [0003] a [0004] At present, it has been reported in the literature that the process for preparing m-fluorophenol is: [0005] (1) Use m-aminophenol to prepare m-fluorophenol through the Schman reaction, and the reaction equation is: [0006] the [0007] the [0008] The pyrolysis process of this process is dangerous, the operating conditions are harsh, the industrialization is difficult, the total reaction yield is low, and the unit consumption is high. [0009] (2) Use m-difluorobenzene to prepare m-fluorophenol throug...

Claims

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
Login to View More

Application Information

Patent Timeline
no application Login to View More
Patent Type & Authority Patents(China)
IPC IPC(8): C07C39/27C07C37/045
CPCC07C37/045C07C245/20C07C39/27
Inventor 刘拥贤陈维德潘建龙
Owner 郓城县世炬商贸有限公司
Features
  • R&D
  • Intellectual Property
  • Life Sciences
  • Materials
  • Tech Scout
Why Patsnap Eureka
  • Unparalleled Data Quality
  • Higher Quality Content
  • 60% Fewer Hallucinations
Social media
Patsnap Eureka Blog
Learn More

Browse by: Latest US Patents, China's latest patents, Technical Efficacy Thesaurus, Application Domain, Technology Topic, Popular Technical Reports.

© 2025 PatSnap. All rights reserved.Legal|Privacy policy|Modern Slavery Act Transparency Statement|Sitemap|About US| Contact US: help@patsnap.com