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

Clean production process of 6-chloro-2,4-dinitroaniline

A dinitroaniline, clean production technology, applied in the preparation of amino compounds, the preparation of organic compounds, organic chemistry and other directions, can solve the problems of long chlorination time, troublesome post-processing, low equipment productivity, etc., and achieves fast reaction speed, Less side effects

Active Publication Date: 2014-01-29
浙江大井化工有限公司
View PDF0 Cites 23 Cited by
  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0016] The method uses sodium hypochlorite as the chlorination agent, and many by-products are produced in the reaction process, the product quality is poor, the color is deep, the chlorination time is long, the equipment productivity is low, and the aftertreatment is troublesome

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
  • Clean production process of 6-chloro-2,4-dinitroaniline
  • Clean production process of 6-chloro-2,4-dinitroaniline
  • Clean production process of 6-chloro-2,4-dinitroaniline

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0037] In a 500ml flask equipped with a stirrer and a thermometer, 350g of hydrochloric acid with a mass percentage concentration of 12% was added, and 54.9g of 2,4-dinitroaniline was added. After beating at 20°C for half an hour, slowly introduce 10.65g of chlorine gas, the time of chlorine flow is 2 hours, the temperature of chlorine flow is 20-40°C, after the completion of heat preservation for half an hour, the temperature is slowly raised to 40°C, and the concentration of 30% by mass percentage is added dropwise. 21.3 g of sodium chlorate solution, the dropwise addition time is 1 hour, and the reaction temperature is 40-55°C. After dripping, keep it warm for half an hour, filter, and wash with water to obtain 6-chloro-2,4-dinitroaniline with a purity of 98.4% and a yield of 96.5%. The mother liquor was collected and used in the next batch. The mother liquor was applied continuously for 10 batches, with an average purity of 97.2% and a yield of 96.9%.

Embodiment 2

[0039] In a 500ml flask equipped with a stirrer and a thermometer, 350g of hydrochloric acid with a mass percentage concentration of 18% was added, and 54.9g of 2,4-dinitroaniline was added. After beating at 30°C for half an hour, slowly introduce 6.39g of chlorine gas, the time for chlorine flow is 1 hour, the temperature of chlorine flow is 20-40°C, and after half an hour of heat preservation, the temperature is slowly raised to 40°C, and 30% sodium chlorate solution is added dropwise 29.8g, the dropping time is 1.5 hours, and the reaction temperature is 40-55°C. After dripping, keep it warm for half an hour, filter and wash with water to obtain 6-chloro-2,4-dinitroaniline with a purity of 97.8% and a yield of 96.2%. The mother liquor was collected and used in the next batch. The mother liquor was applied continuously for 10 batches, with an average purity of 96.8% and a yield of 96.5%.

Embodiment 3

[0041] In a 1000ml flask equipped with a stirrer and a thermometer, 490g of hydrochloric acid with a mass percentage concentration of 15% was added, and 54.9g of 2,4-dinitroaniline was added. After beating at 30°C for half an hour, slowly introduce 8.52g of chlorine gas for 2 hours and the temperature of 20-40°C. After half an hour of heat preservation, slowly raise the temperature to 40°C, and add 30% sodium chlorate solution dropwise 25.56g, the dropping time is 1.5 hours, and the reaction temperature is 40-55°C. After dripping, keep it warm for half an hour, filter, and wash with water to obtain 6-chloro-2,4-dinitroaniline with a purity of 98.5% and a yield of 96.1%. The mother liquor was collected and used in the next batch. The mother liquor was applied continuously for 10 batches, with an average purity of 97.1% and a yield of 95.8%.

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 clean production process of 6-chloro-2,4-dinitroaniline. The clean production process of 6-chloro-2,4-dinitroaniline comprises the following steps: 1, dispersing 2,4-dinitroaniline into hydrochloric acid solution for pulping, then introducing chlorine gas into the solution for reacting, and thus obtaining intermediate reaction solution; and 2, adding the intermediate reaction solution obtained in the step 1 into sodium chlorate solution for reacting, after the reaction is completed, processing the reaction solution to obtain the 6-chloro-2,4-dinitroaniline and mother solution, and returning the mother solution to the step 1 to serve as the hydrochloric acid solution. According to the production process, the chlorine gas and the sodium chlorate are sequentially employed as chloride agents for chlorinating in steps, so that the product purity and yield are improved and the cost of material is reduced; and the quantity of hydrochloric acid after the reaction is completed is kept stable basically, so that the mother solution is convenient to recycle for use and the pollution to environment is reduced.

Description

technical field [0001] The invention belongs to the field of synthesis of dye intermediates, in particular to a clean production process for 6-chloro-2,4-dinitroaniline. Background technique [0002] 6-Chloro-2,4-dinitroaniline, also known as 2-chloro-4,6-dinitroaniline, has the structure shown in formula (I), and its CAS number is 3531-19-9. It is an important Dye intermediates, as diazo components, are mainly used in the synthesis of disperse blue 270, 264, 259, 125 and 130, etc., and the disperse dyes made from it are widely used in the printing and dyeing industry of synthetic fibers. [0003] [0004] At present, there are four main synthetic methods of 6-chloro-2,4-dinitroaniline, which are introduced as follows: [0005] (1) 2,4-Dinitroaniline is beaten in hydrochloric acid, and the sodium chlorate prepared as a solution is slowly added to the beating material for chlorination reaction to obtain the product. The reaction formula is as follows: [0006] [000...

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): C07C211/52C07C209/74
Inventor 陈宝兴赵国生阮海兴高立江
Owner 浙江大井化工有限公司
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

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

© 2024 PatSnap. All rights reserved.Legal|Privacy policy|Modern Slavery Act Transparency Statement|Sitemap|About US| Contact US: help@patsnap.com