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Continuous flow production process of Fast Red B

A production process, red-based technology, applied in the preparation of organic compounds, the preparation of aminohydroxy compounds, organic chemistry, etc., can solve the problems of poor safety, low production efficiency, and many by-products.

Active Publication Date: 2021-07-30
SHANDONG NORMAL UNIV EXPERIMENTAL PLANT CO LTD +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0008] Aiming at the problems of poor intrinsic safety, low production efficiency, high production cost and many by-products in the existing production process, the present invention makes creative improvements from two aspects of reaction route and production equipment
The nitration reaction uses concentrated nitric acid as a nitration reagent in an acetic acid solvent system, and uses a microchannel reactor to solve the problems of safety and conversion rate of the traditional process

Method used

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  • Continuous flow production process of Fast Red B
  • Continuous flow production process of Fast Red B

Examples

Experimental program
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Effect test

Embodiment 1

[0031] (1) Add 10mol o-methoxyacetanilide to 3850g acetic acid solution to prepare an acetic acid solution with a mass fraction of 30% o-methoxyacetanilide, 1204g concentrated nitric acid with a mass fraction of 68%, nitric acid / o-methoxy The molar ratio of acetanilide is 1.3:1. The two materials are pumped into the microchannel reactor at the same time. The total flow rate is 150g / min, the residence time is 60s, the reaction temperature is 80°C, and the pressure is 5.5bar. The nitration reaction is completed to obtain The reaction solution of oxy-4-nitro-acetanilide, detected and analyzed by liquid chromatography, the reaction conversion rate is 99.5%, and the selectivity is 85% (2-methoxy-4-nitro-acetanilide);

[0032] (2) The nitration reaction solution flows out of the microchannel reactor and enters the tubular heat exchanger, and the temperature of the reaction solution is lowered to 5°C;

[0033] (3) After cooling down, the slurry enters the pusher centrifuge to realize...

Embodiment 2

[0038] (1) Add 10mol of o-methoxyacetanilide to 6600g of acetic acid solution to form an acetic acid solution with a mass fraction of 20% o-methoxyacetanilide, 1155g of concentrated nitric acid with a mass fraction of 60%, nitric acid / o-methoxy The molar ratio of acetanilide is 1.1:1. The two materials are pumped into the microchannel reactor at the same time. The total flow rate is 40g / min, the residence time is 5s, the reaction temperature is 60°C, and the pressure is 3.5bar. The nitration reaction is completed to obtain The reaction solution of oxy-4-nitro-acetanilide was detected and analyzed by liquid chromatography, the reaction conversion rate was 93.5%, and the selectivity was 89.3% (2-methoxy-4-nitro-acetanilide);

[0039] (2) The nitration reaction solution flows out of the microchannel reactor and enters the tubular heat exchanger, and the temperature of the reaction solution is lowered to 5°C;

[0040] (3) After cooling down, the slurry enters the pusher centrifuge...

Embodiment 3

[0045] (1) Add 10mol o-methoxyacetanilide to 3064g acetic acid solution to prepare an acetic acid solution with a mass fraction of 35% o-methoxyacetanilide, 1260g concentrated nitric acid with a mass fraction of 80%, nitric acid / o-methoxy The molar ratio of acetanilide is 1.6:1. The two materials are pumped into the microchannel reactor at the same time. The total flow rate is 150g / min, the reaction temperature is 110°C, the residence time is 120s, and the pressure is 9.5bar. The reaction solution of oxy-4-nitro-acetanilide was detected and analyzed by liquid chromatography, the reaction conversion rate was 99.8%, and the selectivity was 78.0% (2-methoxy-4-nitro-acetanilide);

[0046] (2) The nitration reaction solution flows out of the microchannel reactor and enters the tubular heat exchanger, and the temperature of the reaction solution is lowered to 5°C;

[0047] (3) After cooling down, the slurry enters the pusher centrifuge to realize the continuous separation of solid a...

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Abstract

The invention discloses a continuous flow production process of Fast Red B, and belongs to the field of organic synthesis. According to the process, o-methoxyacetanilide is taken as an initial raw material, and continuous flow production of the Fast Red B is realized through two-step reaction of nitration and hydrolysis by using a micro-channel reactor / a tubular heat exchanger / a pusher centrifuge / a tubular reactor / continuous cooling and separation equipment. According to the process, common concentrated nitric acid is adopted as a nitration reagent, and continuous reaction and separation equipment is introduced, so that continuous production is realized, the production safety risk is reduced, the production period is shortened, and the blank in the technical field of continuous flow production of the product is filled.

Description

technical field [0001] The invention belongs to the field of organic synthesis, in particular to a continuous production process of red base B (2-methoxy-4-nitro-aniline). [0002] technical background [0003] O-methoxy-p-nitroaniline is an important organic dye, which is mainly used for dyeing and printing of cotton fiber fabrics, and is also used in the manufacture of fast pigments, bordeaux, golden yellow, black and other organic pigments, which are widely used in the printing and dyeing industry , the market demand is large. Its synthesis method can be obtained through two steps of nitration and hydrolysis of o-methoxyacetanilide. At present, the production process of this product is facing the problems of high risk factor, high production cost and many by-products. Nitrification is a dangerous process under national key supervision, and the traditional batch production process is extremely dangerous. The hydrolysis reaction needs to be carried out under strong alkali...

Claims

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Application Information

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IPC IPC(8): C07C217/84C07C213/02C07C233/25C07C231/12
CPCC07C213/02C07C231/12C07C217/84C07C233/25
Inventor 刘启奎杨松
Owner SHANDONG NORMAL UNIV EXPERIMENTAL PLANT CO LTD
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