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A kind of solid phase continuous reaction prepares the method for 1-amino-4 naphthalene sulfonate sodium

A technology of sodium naphthalenesulfonate and amino, which is applied in the field of solid-phase continuous reaction to prepare sodium 1-amino-4naphthalenesulfonate, can solve the problems of low batch reaction production capacity, low local overheating yield, production site pollution, etc., and achieve Realize the effect of DCS automatic control, easy enlargement of production scale and improvement of production environment

Active Publication Date: 2017-02-01
常州华达纳米材料科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0007] Aiming at the problems in the prior art that direct fire heating is used in industrial production to cause large pollution, low local overheating yield, low production capacity of intermittent reaction, serious pollution on the production site, etc., the invention provides a solid-phase continuous sulfonation transposition of menaphthylamine and sulfuric acid The method for producing sodium 1.4 acid significantly improves the product yield, realizes continuous, efficient, and uniform heating in the reaction process, and the operation can realize automatic control, which meets the needs of large-scale and modern production

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0035] A method for preparing 1-amino-4 naphthalenesulfonate sodium by solid phase continuous reaction, the steps are:

[0036] (A) Salt sulfonation: Add the reaction raw materials menaphthylamine, sulfuric acid and water to the salt forming kettle respectively, the quality of menaphthylamine, sulfuric acid and water is 2000KG\:1600KG\:600KG\, stir evenly, and react to get carbinol Amine sulfate;

[0037] (B) sulfonation: the menaphthylamine sulfate obtained in the step (A) is continuously introduced into the vertical sulfonation reactor of 10M3 at a speed of 1050KG / hr, and the reactor outside has a jacket, and heat transfer oil is used as heat The sulfonation reaction kettle was heated by medium indirect circulation heating method for sulfonation reaction, the stirring speed was 20 rpm, the stirring method was frame stirring, the sulfonation reaction temperature was 220°C, and the residence time was 4 hours. Water is removed, and the remaining reaction product is a solid mix...

Embodiment 2

[0042] With embodiment 1, difference is: the mass ratio of the menaphthylamine in the step (A), sulfuric acid and water is 2000KG\1300KG\:0.0KG; The sulfonation reactor of step (B) is a horizontal reactor, There is a heating coil outside the reaction kettle, the stirring method is rake stirring, the stirring speed is 40 rpm, the sulfonation reaction temperature is 180°C, the reaction time is 12 hours, and the reaction product is containing 1,4 acid (>94% ) and unreacted raw material (2.5%) solid mixture; the alkali that adds in the step (C) is potassium hydroxide, according to solid mixture: 30% sodium hydroxide: the mass ratio of water is 1:0.6:10 ratio to add , the extraction solvent is benzene; the sodium 1,4-acid content in the product obtained after concentration and crystallization is 99.2%, and the product yield after the crystallization mother liquor is 91.5%.

Embodiment 3

[0044] With embodiment 1, difference is: the mass ratio of menaphthylamine, sulfuric acid and water in step (A) is 2000KG\: 1800KG\: 3000KG; The sulfonation reaction temperature in step (B) is 230 ℃, reaction There is a heating coil inside the kettle, the stirring method is paddle stirring, the stirring speed is 60 rpm, the reaction time is 2 hours, and the reaction product is containing 1,4 acid (>93%) and unreacted raw materials (6.5%) ) solid mixture; the alkali added in the step (C) is sodium carbonate, according to the solid mixture: 30% sodium carbonate: the mass ratio of water is added in the ratio of 1:1.3:4, and the extraction solvent is toluene; after concentrated crystallization, obtain The sodium 1,4-acid content in the product is 99.3%, and the product yield is 89% after the crystallization mother liquor is applied mechanically.

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Abstract

The invention discloses a method for preparing sodium 1-amino-4-naphthalenesulfonate by solid-phase continuous reaction, belonging to a production method of a chemical dye intermediate. The method mainly comprises the following steps: A) adding methyl naphthylamine, sulfuric acid and water into a salifying kettle, and stirring to react to obtain methylnaphthylamine sulfate; B) continuously introducing the methylnaphthylamine sulfate obtained in the step A) into a sulfonation reaction kettle; C) heating the sulfonation reaction kettle to carry out sulfonation reaction, thereby obtaining a reaction product solid mixture; D) dissolving the solid mixture obtained in the step C) in water, and neutralizing by adding an alkali solution; E) adding a solvent into the mixed solution in the step D) to carry out extraction; F) concentrating the water phase obtained in the step E); and G) cooling the concentrated solution in the step F) to crystallize, and carrying out centrifugal separation on the crystalline solution to obtain the product 1-amino-4-naphthalenesulfonate and a crystallizing mother solution. The method has the advantages of high product yield, low production cost and simple technical process, can implement DCS automatic control, and is easy to operate.

Description

technical field [0001] The present invention belongs to a kind of chemical industry, the production method of dye intermediate, specifically, relate to a kind of preparation method of dye intermediate 1-amino-4 naphthalene sulfonate sodium, more specifically, relate to a kind of solid phase continuous reaction preparation Sodium 1-amino-4naphthalenesulfonate method. Background technique [0002] Sodium 1-amino-4-naphthalenesulfonate (also known as sodium 4-amino-1-naphthalenesulfonate, referred to as sodium 1,4-acid), is an important pharmaceutical, chemical, and dye intermediate, which can be used to prepare acidic, direct Dye and food coloring, the product form is white crystal or powder. It can lose crystal water at 100°C, and its anhydrate will be carbonized without melting at 280-300°C. 1,4 acid will turn rose color when placed in the air, and its sodium salt contains two crystal waters or four crystal waters. The sodium salt containing four crystal waters is white o...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C309/47C07C303/32C07C303/44
Inventor 徐光辉欧阳祥周豪黄平刘军
Owner 常州华达纳米材料科技有限公司