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A kind of continuous nitration method and product of 1,2-diazooxynaphthalene-4-sulfonic acid

A technology of diazooxynaphthalene and sulfonic acid, which is applied in the field of chemical synthesis and reaction engineering, can solve the problems of limited application of solid or high-viscosity materials with high solid content, poor mass and heat transfer, waste of raw materials, etc., and achieves Improvement of concentrated acid demand, easy automatic control, and reduction of three wastes

Active Publication Date: 2022-08-09
杭州下沙恒升化工有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, this process usually has some disadvantages that cannot be ignored: the process produces a large amount of waste acid and waste water containing organic matter; the poor selectivity of the nitrification process leads to waste of raw materials along with the waste acid; strong acid causes equipment to rot; Poor quality and heat transfer often lead to side reactions such as multiple nitrification and oxidation, which may bring safety hazards, etc.
At present, the mainstream reactors on the market, such as Chemtrix, Corning and other microchannels, have such limitations, which limit the application of solid or high-viscosity materials with high solid content

Method used

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  • A kind of continuous nitration method and product of 1,2-diazooxynaphthalene-4-sulfonic acid
  • A kind of continuous nitration method and product of 1,2-diazooxynaphthalene-4-sulfonic acid
  • A kind of continuous nitration method and product of 1,2-diazooxynaphthalene-4-sulfonic acid

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preparation example Construction

[0050] In one embodiment, the preparation method of the material F includes: mixing 1,2-diazooxynaphthalene-4-sulfonic acid, sulfuric acid and a solvent, and fully stirring with a mechanical stirrer until the particles in the mixture are uniformly dispersed in the In the material system composed of sulfuric acid and solvent.

[0051] The preparation method of material F in the present invention ensures uniform feeding and facilitates maintenance of the pump.

[0052] In one embodiment, the material F is fed by a high-tolerance peristaltic pump or a gear pump, and the material N is fed by a PTFE plunger pump or a corrosion-resistant diaphragm pump such as PFA.

[0053] In one embodiment, n=2.

[0054] In the present invention, when n=2, the steps are simplified, the operation is convenient, and the work efficiency is improved.

[0055] In one embodiment, when n=2, as figure 1 , the continuous nitration method of the 1,2-diazooxynaphthalene-4-sulfonic acid comprises:

[0056...

Embodiment 1

[0073] Embodiment 1 of the present invention provides a continuous nitration method of 1,2-diazooxynaphthalene-4-sulfonic acid, such as figure 1 , the specific steps are as follows:

[0074] (1) mixing 1,2-diazooxynaphthalene-4-sulfonic acid and sulfuric acid, fully stirring with a mechanical stirrer until the particles in the mixture are uniformly dispersed in the material system formed by the sulfuric acid, to obtain material F1 and material F2 respectively; Nitric acid is used as material N1 and material N2;

[0075] (2) The material F1 and the material N1 continuously enter the reaction module 1 at a feed temperature of 40°C and react at 30°C; at the same time, the material F2 and the material N2 continuously enter the reaction module 2 at a feed temperature of 25°C for reaction at 35°C The reaction is obtained after gas-liquid separation.

[0076] The materials F1 and F2, in parts by weight, include 25 parts of 1,2-diazooxynaphthalene-4-sulfonic acid and 75 parts of sul...

Embodiment 2

[0082] Embodiment 2 of the present invention provides a continuous nitration method of 1,2-diazooxynaphthalene-4-sulfonic acid, specifically the following steps:

[0083] (1) mixing 1,2-diazooxynaphthalene-4-sulfonic acid and sulfuric acid, fully stirring with a mechanical stirrer until the particles in the mixture are uniformly dispersed in the material system formed by the sulfuric acid, to obtain material F1 and material F2 respectively; 80 parts of nitric acid and 20 parts of sulfuric acid are used as material N1 and material N2;

[0084] (2) The material F1 and the material N1 continuously enter the reaction module 1 at a feed temperature of 40°C and react at 30°C; at the same time, the material F2 and the material N2 continuously enter the reaction module 2 at a feed temperature of 25°C for reaction at 35°C The reaction is obtained after gas-liquid separation.

[0085] The materials F1 and F2, in parts by weight, include 25 parts of 1,2-diazooxynaphthalene-4-sulfonic ac...

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Abstract

The invention relates to the technical field of chemical synthesis and reaction engineering, and more particularly, to a continuous nitration method and product of 1,2-diazooxynaphthalene-4-sulfonic acid; A continuous nitration method for naphthalene-4-sulfonic acid, comprising: material F and material N are simultaneously fed at 0-90°C in n times, continuously reacting at 0-50°C in n reaction modules, and gas-liquid separation Get it later. Compared with the original traditional nitration process, the nitrification reaction process provided by the invention greatly shortens the time consumption, the nitrification product has high purity, less impurities, the reaction of the raw materials is more complete, the cost of the raw materials is reduced, the three wastes can be reduced by nearly 30%, the automatic control is easy to realize, and the operation is simple and convenient , more environmentally friendly.

Description

technical field [0001] The invention relates to the technical field of chemical synthesis and reaction engineering, and more particularly, to a continuous nitration method and product of 1,2-diazooxynaphthalene-4-sulfonic acid. Background technique [0002] Nitration reaction is an important unit reaction in organic synthesis chemistry and chemical production. The mixed acid nitration method (the mixed use of nitric acid and sulfuric acid in a certain proportion) is a traditional nitration method. Its outstanding advantages are simple reaction equipment and stable process, so it has always been the main method for industrial production of nitro compounds. However, this process usually has some shortcomings that cannot be ignored: the process produces a large amount of waste acid and wastewater containing organic matter; the poor selectivity of the nitrification process leads to waste of raw materials with the waste acid; the strong acid causes the equipment to rot; Poor qua...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07D271/12
CPCC07D271/12
Inventor 刘丰杰唐安定杨伟于东方
Owner 杭州下沙恒升化工有限公司