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

Preparation process of 2-naphthylamine-3,6,8-trisulfonic acid

A preparation process, amino technology, applied in the direction of sulfonic acid preparation, organic chemistry, etc., can solve the problems of reducing yield, increasing operation steps, etc., and achieve the effects of reducing pressure, high safety factor, and reducing loss

Active Publication Date: 2014-01-29
ZHEJIANG RUNTU INST
View PDF6 Cites 13 Cited by
  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

This preparation process needs to separate the G salt for subsequent reactions, which increases the operating steps and reduces the yield

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
  • Preparation process of 2-naphthylamine-3,6,8-trisulfonic acid
  • Preparation process of 2-naphthylamine-3,6,8-trisulfonic acid
  • Preparation process of 2-naphthylamine-3,6,8-trisulfonic acid

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0036] In a four-necked flask with stirring, add 200 grams of 100% sulfuric acid, add 150 grams of 2-naphthol in batches under stirring and cooling, control the feeding temperature at 40-60 ° C, then add 175 grams of 105% sulfuric acid, after the addition is complete Stir the reaction for 5 to 8 hours, and keep warm at 80°C for 7 hours to obtain the sulfonated compound; add the sulfonated compound to a solution of 221 grams of 20% ammonia water and 49 grams of sodium chloride, and keep warm at 85°C for 2 hours after the addition is completed. Hour, cooling, filters, obtains G salt and R salt mixture 320 grams, wherein G salt content 66.1%, R salt content 15.3%.

[0037] Dissolve 320 grams of the above G salt and R salt mixture in 165 grams of 20% ammonia water and 25 grams of catalyst (the molar ratio of ammonium bisulfate and sulfurous acid is 1:1), add it to the autoclave, raise the temperature to 130-140 ° C, and the pressure is 0.8-0.9MPa, maintain for 9-10 hours, after th...

Embodiment 2

[0042] In a 5000L glass-lined reactor, add 2000KG100% sulfuric acid, add 1500KG2-naphthol in batches under stirring and cooling, control the feeding temperature at 40-50°C, then add 1750KG105% sulfuric acid, stir and react for 5-8 hours after the addition is complete, After the reaction at 80°C for 7 hours, the sulfonate was added to a solution of 2200KG 20% ammonia water and 490KG sodium chloride, and after the addition was completed, it was kept at 85°C for 2 hours, cooled to 30°C, and filtered to obtain a mixture of G salt and R salt 3310KG, of which the G salt content is 65.3%, and the R salt content is 15.2%.

[0043] Dissolve 3310KG of the above G salt and R salt mixture in 1690KG of 20% ammonia water and 31KG of catalyst (the molar ratio of ammonium bisulfate and sulfurous acid is 1:1), put it into the autoclave, raise the temperature to 130-140°C, and the pressure is 0.8-0.9MPa , maintained for 8 to 12 hours, cooled down and diluted into water after the reaction, added...

Embodiment 3

[0047] In a four-necked flask with stirring, add 200 grams of 100% sulfuric acid, add 150 grams of 2-naphthol in batches under stirring and cooling, control the feeding temperature at 40-60 ° C, then add 175 grams of 105% sulfuric acid, after the addition is complete Stir the reaction for 5 hours, and then keep it warm at 80°C for 7 hours. After the reaction, the sulfonated compound is obtained; the sulfonated compound is added to the solution of 200 grams of 20% ammonia water and 55 grams of sodium chloride, and after the addition is completed, it is kept at 85° C. for 2 hours. Hour, cooled to 30 ℃ and left standstill for 2 hours, filtered to obtain 312 grams of G salt and R salt mixture, wherein the G salt content was 65.9%, and the R salt content was 15.7%.

[0048] Dissolve 312 grams of the above G salt and R salt mixture in 165 grams of 20% ammonia water and 25 grams of catalyst (the molar ratio of ammonium bisulfate and sulfurous acid is 1:1.2), add it to the autoclave, rai...

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 preparation process of 2-naphthylamine-3,6,8-trisulfonic acid. The preparation process of 2-naphthylamine-3,6,8-trisulfonic acid comprises the following steps: 1, adding 2-isonaphthol into sulfuric acid for carrying out sulfonation reaction, and thus obtaining a sulfonated product after the reaction is completed; 2, adding the sulfonated product into the mixed solution of ammonium hydroxide and sodium chloride for salting out, and thus obtaining salt mixture and mother solution; 3, under the existence of ammonolysis catalyst, carrying out the ammonolysis reaction between the salt mixture and the ammonium hydroxide, and after the reaction is completed, acidizing, dehydrating and drying to obtain amide; and 4, adding the amide into fuming sulphuric acid for carrying out sulfonation reaction, and after the reaction is completed, obtaining the 2-naphthylamine-3,6,8-trisulfonic acid by aftertreatment. According to the preparation process, a one-step method is employed for salting-out and one-time ammoniating, so that the operating steps are simple, the problem of wastewater treatment in traditional technology is solved, meanwhile the unit consumption of 2-isonaphthol, as the material, is reduced, and the production cost is also reduced.

Description

technical field [0001] The invention belongs to the field of preparation of dye intermediates, in particular to a preparation process of amino K acid. Background technique [0002] Amino K acid, chemical name: 2-naphthylamine-3,6,8-trisulfonic acid, structure as shown in formula (I), is an important dye intermediate, mainly used in azo dyes, reactive dyes And in the field of organic pigments, it can be used in the production of cationic dyes, reactive brilliant red K-2G, etc. [0003] [0004] At present, amino K acid is generally prepared industrially by further sulfonation reaction of amino G acid (2-naphthylamine-6,8-disulfonic acid). It can be obtained through reaction steps such as chemical reaction, salting-out, ammoniation and acid-out. During the sulfonation reaction, 2-naphthol first generates 2-naphthol-6,8-disulfonic acid (G acid) and other sulfonated by-products, and the most important by-product is R acid (2-naphthol -3,6-disulfonic acid), in order to carr...

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): C07C309/47C07C303/06
Inventor 唐勇郑鑫梁赵国生阮海兴高立江
Owner ZHEJIANG RUNTU INST
Features
  • Generate Ideas
  • 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