Unlock instant, AI-driven research and patent intelligence for your innovation.

A kind of nitration process for the industrial synthesis of H acid by diamine method

A technology of diamine method and process, which is applied in the new nitration process field of industrial synthesis of H acid by diamine method, which can solve the problems of ineffective treatment and application of waste acid, poor quality, low yield, etc., and improve the quality of H acid products , low cost, increase the effect of the curing step

Active Publication Date: 2017-12-12
CHUYUAN HIGH NEW TECH GRP
View PDF1 Cites 0 Cited by
  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] The purpose of the present invention is to provide a simple process, high product quality and yield, to solve the problems of low yield and poor quality in the existing nitration process, and the problem that waste acid cannot be effectively treated and applied mechanically. new nitrification process

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

[0022] Add 4032Kg of the tidal product 2.7-naphthalene disulfonic acid (the mass percentage of 2.7-naphthalene disulfonic acid is 50%, the mass percentage of sulfuric acid is 30%, and the rest is water) and 5765Kg of 98% sulfuric acid are added to the reactor to mix and dissolve, and stir ,clarify. Cool the dissolved material to below 10°C under the condition of stirring at 30 rpm, slowly add 990Kg of 98% fuming nitric acid dropwise, control the temperature of the material below 15°C during the dropping process, add one-third of the fuming nitric acid dropwise After the total amount of nitric acid, the viscosity of the material increases. At this time, the stirring speed is increased to 60 rpm, and under this stirring speed condition, the remaining 2 / 3 of the fuming nitric acid is added dropwise, and the time for adding the fuming nitric acid is 8 hours.

[0023] The material obtained above was heated to 100°C under the condition of stirring (60 rpm), and maintained for 2 hour...

Embodiment 2

[0026] With tidal product 2.7-naphthalene disulfonic acid 4032Kg (wherein the mass percentage of 2.7-naphthalene disulfonic acid is 50%, the mass percentage of sulfuric acid is 30%, all the other are water) and the 4294Kg 95% of embodiment 1 gained reclaim sulfuric acid and 1368Kg65 % oleum was added to the reactor for mixing and dissolving, stirred and clarified. Cool the dissolved material to below 10°C under the condition of stirring at 30 rpm, slowly add 990Kg of 98% fuming nitric acid dropwise, control the temperature of the material below 15°C during the dropping process, add one-third of the fuming nitric acid dropwise After the total amount of nitric acid, the viscosity of the material increases. At this time, the stirring speed is increased to 60 rpm, and under this stirring speed condition, the remaining 2 / 3 of the fuming nitric acid is added dropwise, and the time for adding the fuming nitric acid is 10 hours.

[0027]The material obtained above was heated to 100°C ...

Embodiment 3

[0030] With tidal product 2.7-naphthalene disulfonic acid 4032Kg (wherein the mass percentage of 2.7-naphthalene disulfonic acid is 50%, the mass percentage of sulfuric acid is 31.2%, all the other are water) and the 4271.5Kg 95.5% reclaiming sulfuric acid of embodiment 2 gained and 1328Kg65% oleum was added to the reactor for mixing and dissolving, stirred and clarified. Cool the dissolved material to below 10°C under the condition of stirring at 30 rpm, slowly add 990Kg of 98% fuming nitric acid dropwise, control the temperature of the material below 15°C during the dropping process, add one-third of the fuming nitric acid dropwise After the total amount of nitric acid, the viscosity of the material increases. At this time, the stirring speed is increased to 60 rpm, and under this stirring speed condition, the remaining 2 / 3 of the fuming nitric acid is added dropwise, and the time for adding the fuming nitric acid is 12 hours.

[0031] The material obtained above was heated ...

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 relates to a new nitration process for H acid, in particular to a new nitration process for industrially synthesizing H acid by a diamine method. The present invention uses 65% oleum and recovered sulfuric acid to replace concentrated sulfuric acid to dissolve 2.7-naphthalene disulfonic acid, and directly nitrates without dehydration and concentration. Salt out and crystallize, and filter to obtain 1.8-dinitro-3.6-naphthalene disulfonate. After the waste acid is oxidized and concentrated at high temperature, it is recycled to the nitration station. Compared with the original process, the present invention can reduce the generation of 2.7-naphthalene disulfonic acid nitration by-products, reduce the consumption of sulfuric acid, increase the aging steps and adopt the salting-out process to improve The yield of the nitration product 1.8-dinitro-3.6-sodium naphthalene disulfonate is 3%; at the same time, it has the characteristics of simple and convenient process for treating nitration waste acid and low cost.

Description

technical field [0001] The invention relates to a new nitration process for H acid, in particular to a new nitration process for industrially synthesizing H acid by a diamine method. Background technique [0002] H acid is an intermediate for the manufacture of dyes, and is widely used in printing and dyeing, textile, pharmaceutical and other industries. The traditional naphthalene trisulfonation-alkali fusion process for producing H acid has caused serious concerns from all walks of life due to the large amount of wastewater and high treatment costs. . In recent years, people have been constantly exploring new processes for the synthesis of H acid. Among them, the synthesis process of H acid by the diamine method has attracted widespread attention in the industry. It uses naphthalene as a raw material, and two sulfonic acid groups are introduced during sulfonation, and then nitrated and reduced. , hydrolysis, and refining processes to produce high-quality H acid. This proc...

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 Patents(China)
IPC IPC(8): C07C309/50C07C303/22C07C303/32
Inventor 廖杰安建平陈红兵曾炎花李敏胡齐彭建平
Owner CHUYUAN HIGH NEW TECH GRP