Check patentability & draft patents in minutes with Patsnap Eureka AI!

Method for producing M acid by catalytic hydrogenation method

A catalytic hydrogenation and catalyst technology, which is applied in chemical instruments and methods, physical/chemical process catalysts, metal/metal oxide/metal hydroxide catalysts, etc. Time and other issues, to achieve the effect of no three waste pollution, low cost and good product quality

Inactive Publication Date: 2017-08-01
济南和润化工科技有限公司
View PDF3 Cites 1 Cited by
  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Iron powder reduction method is used to produce M acid, the cost is low, and the production is relatively mature, but the working conditions are poor, and the environmental pollution caused by iron sludge is serious, so it is generally not used.
Indian scholar Gowda used hydrazine formate as a reducing agent and also achieved success with iron powder reduction, but so far it has only been tested in the laboratory, and it will take time to further apply it in large-scale industrial production

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 producing M acid by catalytic hydrogenation method
  • Method for producing M acid by catalytic hydrogenation method

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0017] Taking 400 kg of 3,5-dinitro-2,4,6-trimethylbenzenesulfonic acid as an example, the catalyst used is a self-made catalyst loaded with precious metals, and the total amount of catalyst used in the production process is 0.1-5% of the raw material ( 0.4-20 kg), the total amount of water is 3-10 times of the raw material (1200-4000 kg), before hydrogenation, 3,5-dinitro-2,4,6-trimethylbenzenesulfonic acid, water and The order in which the catalyst is put into the kettle is as follows:

[0018] 1. Put 400 kg of 3,5-dinitro-2,4,6-trimethylbenzenesulfonic acid and 1200-4000 kg of water into the reaction kettle, and add sodium hydroxide, potassium hydroxide, potassium carbonate or sodium carbonate etc., adjust the pH value of the reaction solution to 7-8, and replace the gas.

[0019] 2. Introduce hydrogen to start the hydrogenation reaction, control the reaction temperature to 50-100°C, and control the reaction pressure to 0.3-1.0Mpa.

[0020] 3, the reaction finishes filter...

Embodiment 2

[0023] Taking 400 kilograms of 3,5-dinitro-2,4,6-trimethylbenzenesulfonic acid to produce M acid as an example, the catalyst used in the production process is a self-made catalyst loaded with precious metals, and the dosage is 3,5-di Nitro-2,4,6-trimethylbenzenesulfonic acid 0.1-5% (0.4-20 kg), the total amount of water is 3-10 times of the raw material (1200-4000 kg), in continuous production, 3, 5-Dinitro-2,4,6-trimethylbenzenesulfonic acid, water and catalyst were added in the order of (1). In order to investigate the stability of the process, five consecutive experiments were carried out. The results are shown in Table 1 as follows :

[0024]

[0025] Reaction conditions: temperature 50-100°C, pressure 0.3-1.0Mpa, ph7-8.

[0026] As seen from the table, 3,5-dinitro-2,4,6-trimethylbenzenesulfonic acid conversion rate is 100%, the selectivity of M acid is more than 99.5%, and the finished product content is more than 99.7%, and the yield The rate is above 97%.

Embodiment 3

[0028] Taking 400 kg of 3,5-dinitro-2,4,6-trimethylbenzenesulfonic acid to produce M acid as an example, the catalyst used in the production process is a self-made catalyst loaded with precious metals, and the dosage is 3,5-dinitro- 0.1-5% (0.4-10 kg) of 2,4,6-trimethylbenzenesulfonic acid, the total amount of water is 3-10 times (1200-4000 kg) of the raw material, in continuous production, according to Example 1 The production process reacts, and the difference is that the catalyst is recycled. After the reaction in each kettle is completed, after the catalyst is filtered by pressure, the catalyst is blown back into the reaction kettle, and 0.1-1.0 kg of catalyst is added, and the catalyst is recycled. After the catalyst started to be used mechanically, the amount of new catalyst added was greatly reduced, only 5%-25% of the original, which greatly reduced the cost. After mass production experiments, this catalyst can be used continuously for more than ten times.

[0029] In...

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

This invention discloses a method for producing M acid by a catalytic hydrogenation method. The method comprises the following steps: adding an aqueous solution with 3,5-dinitro-2,4,6-trimethylbenzenesulfonicacid dissolved therein into a hydrogenation kettle, adding a catalyst, introducing hydrogen, carrying out a hydrogenation reaction, filtering, acidifying a filtrate, crystallizing and drying to obtain M acid. Conversion rate of the raw material is 100%. The product is white powder, chromatographic purity is 99% and above, and yield can reach 95% and above.

Description

technical field [0001] The invention relates to a method for producing organic acid, in particular to a method for producing M acid by catalytic hydrogenation. Background technique [0002] M acid is an important dye and pharmaceutical intermediate, mainly used in the synthesis of Ammonia Blue 3R and Reactive Brilliant Blue K-3R, etc., and has a large demand abroad. In the literature, there are three ways to prepare M acid by reduction of 3,5-dinitro-2,4,6-trimethylbenzenesulfonic acid: iron powder reduction, hydrazine reduction and hydrogenation reduction. The production of M acid by iron powder reduction method is relatively low in cost and mature in production, but the working conditions are poor and the environmental pollution caused by iron sludge is serious, so it is generally not used. Indian scholar Gowda used hydrazine formate as a reducing agent and also achieved success with iron powder reduction, but so far it has only been tested in the laboratory, and it will ...

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): C07C303/22C07C309/46B01J23/38
CPCC07C303/22B01J21/18B01J23/38C07C309/46
Inventor 王光侯卫波韩龙凯王超李娟唐国武
Owner 济南和润化工科技有限公司
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