Looking for breakthrough ideas for innovation challenges? Try Patsnap Eureka!

Method for preparing o-trifluoromethyl benzaldehyde

A technology of trifluoromethylbenzaldehyde and trifluoromethyldichloromethylbenzene, which is applied in the field of preparation of o-trifluoromethylbenzaldehyde, can solve the problems of high production cost, high energy consumption, cumbersome operation, etc., and achieve The effects of less waste, low cost, and easy industrial production

Active Publication Date: 2014-09-03
LIAONING TIANYU CHEM +2
View PDF6 Cites 16 Cited by
  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0010] The technical problem to be solved by the present invention is in order to overcome in the existing preparation method of o-trifluoromethylbenzaldehyde, raw material price is expensive and difficult to obtain, production cost is high, waste water is many, energy consumption is high, operation is loaded down with trivial details and is unfavorable for industrialized production defect, and a kind of preparation method of o-trifluoromethylbenzaldehyde is provided

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
  • Method for preparing o-trifluoromethyl benzaldehyde
  • Method for preparing o-trifluoromethyl benzaldehyde
  • Method for preparing o-trifluoromethyl benzaldehyde

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0037] Chlorination reaction

[0038] In the photochlorination tower of 1500L, drop into 650kg o-xylene, 5kg azobisisobutyronitrile, open the tower jacket steam to raise the temperature, open the light source (4 ultraviolet lamps of 250w), open the tail gas system, slightly negative pressure (- 0.01Mpa) operation, when the temperature in the tower reaches 90-110°C, start to feed chlorine gas, the amount of chlorine flow is 40-60kg / h, fast first and then slow, keep the temperature in the tower at 110-130°C in the later stage, and pass through gas chromatography Analysis, ortho-dichloromethyldichlorotoluene (GC%)95% is the reaction end point, after passing through, stop logical chlorine, and chlorination The reaction solution was transferred to a transfer tank, purged with nitrogen for 0.5 h, and kept at 70°C for use (melting point about 53-54°C).

[0039] Fluorination reaction

[0040] 2300kg of chlorinated material (o-trichloromethyldichloromethylbenzene, preparation method ...

Embodiment 2

[0041] Embodiment 2 fluorination reaction

[0042] 2300kg of chlorinated material (o-trichloromethyldichloromethylbenzene, the preparation method is the same as the chlorination reaction in Example 1) and 1kg of antimony trifluoride are dropped into the fluorination kettle, and the still condenser refrigerant (cold brine temperature- 15~20℃), open the kettle jacket and cool the refrigerant down to 10℃, press 0.1kg nitrogen gas from the HF storage tank into 350kg HF to the HF transfer tank, then press 400kg recovered HF from the HF recovery tank to the transfer tank, and then release it by gravity into the fluorination kettle. Close the relevant valves, open the jacket steam of the fluorination kettle to slowly heat up, and control the reaction temperature at 70-90°C. When the pressure of the kettle reaches 2.5MPa, open the vent valve to slowly discharge the pressure. After decompression, the pressure does not rise any more, keep the temperature at 90-95°C, and after 4 hours o...

Embodiment 4

[0049] Hydrolysis reaction

[0050] Put 1500kg of the fluorinated crude product obtained in Example 1 into the hydrolysis kettle, add 7.5kg of ferric chloride, open the tail gas absorption system, open the jacket steam to raise the temperature, when the temperature reaches 100°C, start to add 105kg of water dropwise, and keep the reaction temperature at 100°C Between ~ 110°C, after the addition of water dropwise, keep warm for 2 ~ 3h, take a sample and analyze it with gas chromatography, the o-trifluoromethyl benzaldehyde content (GC) > 95%, then transfer the material to the rectification kettle, open the vacuum system (- 0.095Mpa), after vacuum stabilization, open the jacket steam, heat up rectification, collect the cut of 70~75 ℃ / -0.095MPa, obtain 965kg o-trifluoromethylbenzaldehyde, content (GC%)>99.0%. The fraction before rectification (containing a small amount of raw material) and the fraction after rectification (containing a small amount of raw material) are applied me...

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 discloses a method for preparing o-trifluoromethyl benzaldehyde. The method for preparing the o-trifluoromethyl benzaldehyde, disclosed by the invention, comprises the following steps: in the presence of a catalyst, carrying out hydrolysis reaction on a mixture of o-trifluoromethyl methylbenzene bichloride, o-trifluoromethyl chloro-fluoro-methylbenzene and o-trifluoromethyl methylbenzene difluoride and water at the temperature of 80-150 DEG C to obtain, wherein the mass of the catalyst accounts for 0.01-10% of the mass of the mixture. The method disclosed by the invention is cheap and easily available in raw materials, low in cost, little in wastewater, low in energy consumption and simple in operation and can be suitable for industrial production. The structural formula of the o-trifluoromethyl benzaldehyde is shown in the specification.

Description

technical field [0001] The invention relates to a preparation method of o-trifluoromethylbenzaldehyde. Background technique [0002] Due to the strong electronegativity and small atomic radius of fluorine atoms, fluorine-containing compounds have many unique properties, and have very important application values ​​in the fields of biochemistry, medicine, pesticides, functional materials and dyes. Currently, 30%-40% of agricultural chemicals and 20%-30% of pharmaceuticals contain at least one fluorine atom. Among these compounds, trifluoromethyl compounds occupy a considerable proportion. Due to the special structure of the trifluoromethyl group, the substrate can have strong polarity, stability and lipophilicity, so the medicines, pesticides and dyes synthesized from it have stronger activity than some traditional organic intermediates. Attracting attention at home and abroad, trifluoromethylbenzene products have become a group of important organic intermediates at present...

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
IPC IPC(8): C07C47/55C07C45/43
CPCC07C45/43C07C47/55
Inventor 樊小彬林行军刘家斌王国华
Owner LIAONING TIANYU CHEM
Who we serve
  • R&D Engineer
  • R&D Manager
  • IP Professional
Why Patsnap Eureka
  • Industry Leading Data Capabilities
  • Powerful AI technology
  • Patent DNA Extraction
Social media
Patsnap Eureka Blog
Learn More
PatSnap group products