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

O-chlorobenzoic acid synthesis process

A technology of o-chlorobenzoic acid and synthesis process, applied in the field of synthesis technology of o-chlorobenzoic acid, can solve the problems of high production cost, short technological process, low conversion rate and the like, and achieves low cost, high yield and short process flow. Effect

Inactive Publication Date: 2014-02-26
NANTONG BOTAO CHEM
View PDF2 Cites 5 Cited by
  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] The photochlorination method has the advantages of short process flow, easy control of the reaction, easy-to-obtain raw materials, and high reaction yield, but its production cost is high, the equipment is seriously corroded, and a large amount of waste liquid and gas are generated, causing environmental pollution; the reaction conditions of the chemical chlorination method Relatively mild, easy to operate, and mature methods, but the price of chemical oxidants is relatively high. Although the reduction products of some oxidants can be recycled, there are still problems in the treatment of waste water and waste residues; Generally, acetic acid is used as a solvent, and the amount of solvent used is large, so the utilization rate of equipment is low, a large amount of acetic acid needs to be recycled, and acetic acid is highly corrosive, which puts forward high requirements for anticorrosion of reaction equipment and acetic acid recovery equipment. To ensure that acetic acid exists in liquid phase at a higher reaction temperature, pressurized operation is required; the air oxidation method has cheap oxidant, low cost, and good reaction selectivity, but the reaction is carried out at a lower temperature, with weak oxidation ability and low conversion rate. The post-processing operation is complicated, the reaction solution is corrosive, and the equipment needs to use excellent corrosion-resistant materials. Generally, pressurized operation is required to increase the solubility of oxygen, thereby increasing the reaction speed.

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

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0015] Put 280g of o-chlorotoluene and 150g of acetic acid into a 500ml autoclave, then add 0.5g of cobalt acetate, 0.2g of manganese acetate, and 1.0g of sodium bromide as composite catalysts, cover the autoclave, and heat it. When the temperature rises to 135°C, fill Enter oxygen, speed 10L / min, control between 135~145°C, react under 1.0Mpa pressure for 6 hours, cool down, discharge, cool down, filter, wash with water, and get 340g of o-chlorobenzoic acid with a content of 99.5% (HPLC ), melting point: 139.5~141.2℃, yield 98.2%.

Embodiment 2

[0017] Put 280g of o-chlorotoluene and 120g of acetic acid into a 500ml autoclave, then add 0.8g of cobalt acetate, 0.3g of manganese acetate, and 1.2g of sodium bromide as composite catalysts, cover the autoclave, and heat it. When the temperature rises to 135°C, fill Enter oxygen, speed 15L / min, control between 135~145°C, react under 1.0Mpa pressure for 6 hours, cool down, discharge, cool down, filter, wash with water to get 338g of o-chlorobenzoic acid with a content of 99.4% (HPLC ), melting point: 139.5~141.2℃, yield 98.1%.

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 an o-chlorobenzoic acid synthesis process. The innovation point is that the process adopts o-chlorotoluene as a raw material and acetic acid as a solvent and comprises the following steps: heating to 134-136 DEG C under the effect of the composite catalysts cobalt acetate, manganese acetate and sodium bromide; filling oxygen for reaction, wherein the reaction temperature is 135-145 DEG C, the reaction pressure is 1.0MPa, and the reaction time is 5.5-6.5 hours; and after the reaction, cooling, discharging, cooling, filtering and washing to obtain the target product o-chlorobenzoic acid. The synthesis process disclosed by the invention gives overall consideration to the factors such as raw material cost, production flow, production cost and environmental pollution, and has the advantages of high yield, low cost, short flow, no water pollution and the like.

Description

technical field [0001] The invention relates to a synthesis process of o-chlorobenzoic acid, in particular to a synthesis process of o-chlorobenzoic acid with high yield, low cost, short flow and no water pollution, and belongs to the technical field of compound synthesis. Background technique [0002] The molecular weight of o-chlorobenzoic acid is 156.57, colorless acicular or monoclinic crystal, melting point 142°C, easy to sublimate when heated, relative density 1.544, soluble in alcohol and ether, soluble in 900 parts of cold water, more soluble in hot water, insoluble in toluene. O-chlorobenzoic acid is an important fine organic chemical product, an important organic synthesis intermediate and analytical reagent in the fields of dyes, pesticides, medicines, etc. Drugs such as azoles are standard reagents for alkali and iodometric methods, and are used as adhesives, paint preservatives, synthetic dyes, and color films. [0003] According to reports, o-chlorobenzoic ac...

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 Applications(China)
IPC IPC(8): C07C63/70C07C51/265
CPCC07C51/265C07C63/70
Inventor 黄海波黄海涛黄奎生王宏李桂萍黄雪平
Owner NANTONG BOTAO 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