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Continuous nitrification method of 1, 2-diazoxynaphthalene-4-sulfonic acid and product

A technology of diazooxynaphthalene and sulfonic acid, applied in the fields of chemical synthesis and reaction engineering, can solve the problems of restricting the application of solid or high-viscosity materials with high solid content, poor mass and heat transfer, waste of raw materials, etc. The effect of improving the demand for concentrated acid, easy automatic control, and improving economic benefits

Active Publication Date: 2020-11-27
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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  • Continuous nitrification method of 1, 2-diazoxynaphthalene-4-sulfonic acid and product
  • Continuous nitrification method of 1, 2-diazoxynaphthalene-4-sulfonic acid and product
  • Continuous nitrification method of 1, 2-diazoxynaphthalene-4-sulfonic acid and product

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preparation example Construction

[0050] In one embodiment, the preparation method of the material F includes: mixing 1,2-diazoxynaphthalene-4-sulfonic acid, sulfuric acid and a solvent, and fully stirring with a mechanical stirrer until the particles in the mixture are evenly 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 is convenient for pump maintenance.

[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 corrosion-resistant diaphragm pump such as a PTFE plunger pump or PFA.

[0053] In one embodiment, n=2.

[0054] When n=2 in the present invention, the steps are simplified, the operation is convenient, and the working efficiency is improved.

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

[00...

Embodiment 1

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

[0074] (1) Mix 1,2-diazoxynaphthalene-4-sulfonic acid and sulfuric acid, and fully stir with a mechanical stirrer until the particles in the mixture are uniformly dispersed in the material system composed of sulfuric acid to obtain material F1 and material F2 respectively; Nitric acid as material N1 and material N2;

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

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

[0077] The structure of the reacti...

Embodiment 2

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

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

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

[0085] The materials F1 and F2 include 25 parts of 1,2-diazooxynaphthalene-4-sulfonic acid and 75 parts of sulfuric acid in parts by weight.

[0086] T...

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Abstract

The invention belongs to the technical field of chemical synthesis and reaction engineering and relates to a continuous nitrification method of 1, 2-diazoxynaphthalene-4-sulfonic acid and a product. The continuous nitration method of the 1, 2-diazoxynaphthalene-4-sulfonic acid comprises the following steps of: feeding a material F and a material N for n times at 0-90 DEG C at the same time; continuously reacting in n reaction modules at 0-50 DEG C; and performing gas-liquid separation to obtain the 1, 2-diazoxynaphthalene-4-sulfonic acid. Compared with the traditional nitration process, the nitration reaction process provided by the invention has the advantages of greatly shortened time consumption, high nitration product purity, few impurities, more complete raw material reaction, reducedraw material cost, easy realization of automatic control, simple operation and environmental protection, and can reduce the three wastes by nearly 30%.

Description

technical field [0001] The invention relates to the technical field of chemical synthesis and reaction engineering, more specifically, the invention relates to a continuous nitration method and product of 1,2-diazooxynaphthalene-4-sulfonic acid. Background technique [0002] Nitrification is an important unit reaction in organic synthetic chemistry and chemical production. Mixed acid nitration method (mixing nitric acid and sulfuric acid in a certain proportion) is a traditional nitration method, and 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 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 ...

Claims

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Application Information

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Patent Type & Authority Applications(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