Supercharge Your Innovation With Domain-Expert AI Agents!

Method and device for preparing 2-chloro-5-nitrobenzonitrile in pipeline

A technology of nitrobenzonitrile and chlorobenzonitrile, which is applied in the field of tubular nitrification, can solve the problems of poor selectivity, oxidation side reactions, less corrosiveness and three waste discharges, etc., and achieves simple operation and high safety. , post-processing simple effects

Active Publication Date: 2019-02-22
ZHEJIANG UNIV OF TECH
View PDF15 Cites 1 Cited by
  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] Although the green nitrification technology of nitrogen dioxide nitrification system using ozone medium has less corrosiveness and three-waste discharge than the traditional mixed acid nitrification technology, but because ozone itself is a strong oxidant, so in the tank reaction process In the process, it will be accompanied by a considerable proportion of oxidation side reactions, and the selectivity is poor

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 and device for preparing 2-chloro-5-nitrobenzonitrile in pipeline
  • Method and device for preparing 2-chloro-5-nitrobenzonitrile in pipeline

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0046] The structure of the reaction device is as figure 1 , the reaction pipeline 6 length that is filled with catalyzer is 20m, and internal diameter is 6mm, and external diameter is 8mm, and pipeline material is corrosion-resistant high-pressure metal material, is Hastelloy C-276 (Hastelloy C-276); Filled with catalyzer The catalyst in the reaction pipeline 6 is a spherical molecular sieve with a particle size of 3-5mm.

[0047] The operation steps are as follows:

[0048] First the catalyst is loaded into the reaction pipeline 6, the amount of the catalyst is based on filling the pipeline, and the two ends of the pipeline are sealed with a screen to prevent the catalyst from flowing out with the reaction solution, connect the device, and check the tightness; the raw material 2-chlorobenzyl Nitrile is dissolved in the methylene chloride organic solvent, and its volumetric dosage is 5mL / g based on the mass of the raw material 2-chlorobenzonitrile, and is added to the storag...

Embodiment 2

[0050] The structure of the reaction device is as figure 1 , the reaction pipeline 6 length that is filled with catalyzer is 25m, and inner diameter is 6mm, and outer diameter is 8mm, and pipeline material is corrosion-resistant high-pressure metal material, is Hastelloy C-276; The catalyzer in the reaction pipeline 6 that is filled with catalyzer Silica gel particles with a particle size of 3-5mm.

[0051] The volume consumption of the organic solvent is 6mL / g based on the mass of the raw material 2-chlorobenzonitrile, and the reaction pipeline 6 filled with the catalyst is preheated until the reaction temperature is 40°C; the pressure in the reaction pipeline 6 is maintained at 0.6MPa; The molar ratio of 2-chlorobenzonitrile to nitrogen dioxide was 1:1.5; the residence time of the nitration reaction was 40 min; the others were the same as in Example 1, and the product was obtained after post-treatment with a yield of 87% and an HPLC purity of 99.0%.

Embodiment 3

[0053] The structure of the reaction device is as figure 1 , the reaction pipeline 6 length that is filled with catalyzer is 30m, and inner diameter is 6mm, and outer diameter is 8mm, and pipeline material is corrosion-resistant high-pressure metal material, is Hastelloy C-276; The catalyzer in the reaction pipeline 6 that is filled with catalyzer It is a spherical molecular sieve with a particle size of 3-5mm.

[0054] The volume consumption of the organic solvent is 8mL / g based on the mass of the raw material 2-chlorobenzonitrile, and the reaction pipeline 6 filled with the catalyst is preheated to a reaction temperature of 30°C; the pressure in the reaction pipeline 6 is maintained at 0.8MPa; The molar ratio of 2-chlorobenzonitrile to nitrogen dioxide was 1:1.8; the residence time of the nitration reaction was 35 min; the others were the same as in Example 1, and the product was obtained after post-treatment with a yield of 85% and an HPLC purity of 99.2%.

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

PropertyMeasurementUnit
Lengthaaaaaaaaaa
The inside diameter ofaaaaaaaaaa
Outer diameteraaaaaaaaaa
Login to View More

Abstract

The invention discloses a method and a device for preparing 2-chloro-5-nitrobenzonitrile in a pipeline. The device comprises a storage tank, a nitrogen oxide steel cylinder, an ozone generator, a flowpump, a gas flowmeter, a reaction pipeline filled with a catalyst, a mixer, a cooling system, a heating system, a backpressure valve and a receiving tank. The method comprises the following steps: dissolving a raw material 2-chlorobenzonitrile in an organic solvent and adding the mixture into the storage tank; opening the cooling system and the heating system; opening the ozone generator and adjusting the backpressure value; mixing the raw material 2-chlorobenzonitrile and nitrogen dioxide through the mixer and feeding the mixture into the reaction pipeline for a nitrification reaction; and carrying out post-treatment to obtain 2-chloro-5-nitrobenzonitrile. The method is simple to operate, mild in reaction condition, quick to transfer mass and heat, simple in post-treatment, high in safety and good in economical benefit, the catalyst can be repeatedly used, and the method is a green and environment-friendly process suitable for industrial production.

Description

technical field [0001] The invention relates to the technical field of tubular nitration, in particular to a method and device for preparing 2-chloro-5-nitrobenzonitrile through pipeline. Background technique [0002] 2-Chloro-5-nitrobenzonitrile is an intermediate of the dye disperse red S-FL, which is prepared from o-chlorobenzonitrile through nitration. The traditional nitration process uses 98% concentrated sulfuric acid and 98% concentrated nitric acid to prepare a mixed acid as a nitration reagent, and it is made by nitration at a low temperature of 0-10°C. The process has strict requirements on the concentration of sulfuric acid and nitric acid. If the concentration is lower, side reactions will occur, which will affect the quality of the product. At the same time, nitrification requires low temperature, and the cooling of frozen brine consumes a lot of electric energy. [0003] The Chinese invention patent application with publication number CN105859581A (applicatio...

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): C07C253/30C07C255/50
CPCC07C253/30C07C255/50Y02P20/584
Inventor 贾建洪叶孙斌冯东张久明李益珠
Owner ZHEJIANG UNIV OF TECH
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