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A kind of device and method for continuous preparation of azo compounds

An azo compound and storage tank technology, applied in chemical instruments and methods, feeding devices, chemical/physical processes, etc., to achieve the effect of continuous synthesis, compact overall structure, and small footprint

Active Publication Date: 2022-04-15
SHENYANG RES INST OF CHEM IND
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0008] The purpose of the present invention is to provide a device and method for continuous preparation of azo compounds, which can realize the coupling of micro-collision flow and stirring system for the process of producing high-viscosity materials by rapid reaction of low-viscosity liquid-liquid system, and the collision and mixing will not Affected by the stirring system, it effectively prevents the clogging problem, strengthens the mass transfer, and improves the mixing efficiency

Method used

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  • A kind of device and method for continuous preparation of azo compounds
  • A kind of device and method for continuous preparation of azo compounds
  • A kind of device and method for continuous preparation of azo compounds

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0066] Apparatus for preparing an azo compound is employed, wherein the nozzle of the microstructure is 0.8 mm, the nozzle is a single hole structure, and the distance between the upper and lower nozzles is 15mm; the number of blade 16 N = 3, A = 15 mm, b = 20 mm, C = 4 mm; r = 100 mm, r = 360 / min.

[0067] Continuing preparation of dispersed red S-5BL compounds:

[0068]

[0069] The temperature of 10 ° C in the first storage tank 101, the concentration of 4.1% o-chlorine, the nitrophenantine nitrogen salt solution, by the first filling pump 103, which is fed into a collision stream and stirred by the first flow meter 112 and the first regulator 105. In the device 109, the temperature of 10 ° C in the second storage tank 102, N, N-diethyloxyethyl acetamide solution by the second feed pump 104, by the second feedmeter 114 and the second The adjustment valve 106 is sent into the collision flow agitating reactor 109, and the two phases volume flow rates are 300 l / h, and the two ...

Embodiment 1

[0070] Control Example 1: Intermittently dispersed red S-5BL compound

[0071] The temperature is 10 ° C, concentration of concentration of 4.1% o-chlorine is slowly added to a stirred tank containing a concentration of 7.6% N, N-diethyloxyethyl acetamide solution, control temperature reaction 10 ° C After the addition is completed, stirring was continued for 2 h, washed with water, and the chromatographic content of the dye red S-5BL was 88.5%, and the yield was 93.7%.

Embodiment 2

[0072] Example 2 Preparation of Dispersed Yellow 211 Compound

[0073]

[0074] With the microbilization of the microbilization of Example 1, the temperature of 12 ° C in the first storage tank 101, the concentration of 4.7%, the nitrogenic group, the chlorine-nitrogen salt solution, through the first flow meter 112 The first adjustment valve 105 is fed into the collision flow stirring reactor 109, the temperature of 18 ° C in the second storage tank 102, a concentration of 4.92% N-ethyl-3-cyano-4-methyl-6-hydroxyl group -2-pyridone solution is fed to the collision flow stirring reactor 109 by the second feed pump 104, and the two-phase volume flow rate is 200 l / h, and two materials. After the collision flow agitating reactor 109 collides with the mixed reaction, the generated material was sent to the slurry tank 111 by the discharge pump 110, washed with water filtration, and the dye yellow 211 compound was obtained, 99.3% of the test chromatography The yield was 99.1%.

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Abstract

The invention relates to the field of mixing devices in the chemical industry, in particular to a device and method for continuously preparing azo compounds. After the diazonium salt solution in the first storage tank 101 and the coupling component solution in the second storage tank 102 continuously collide and mix in the collision flow stirring reactor 109, the generated materials are sent to the In the slurry tank 111, an azo compound is obtained. The device of the invention has a compact overall structure and a small floor space, and can be used for chemical unit operations of extraction and rapid mixing reactions, especially suitable for the reaction of producing high-viscosity materials after mixing reactions, and is convenient for realizing continuous operation. The method of the invention combines the micro-collision flow technology with the stirring reactor, strengthens the mass transfer, effectively prevents the clogging problem, facilitates the realization of automatic control, improves the reaction efficiency and product yield, and realizes the continuous synthesis of azo compounds.

Description

Technical field [0001] The present invention relates to the field of mixing devices in the chemical industry, and in particular, apparatus and methods for continuously preparing an azo compounds. Background technique [0002] Impinging stream technology is a more novel engineering technology. It is first proposed by Belarusian scientist elPerin in 1961. The basic principle is: through the phase-to-high speed hit by fluid, the impact zone produces a height of turbulence, thereby greatly Improve mixing properties to achieve enhanced heat transfer, mass transfer and other purposes. At present, impact flow technologies have been widely used in various units of drying, absorption, extraction, mixing, heat transfer, crystallization, combustion. [0003] In recent years, the research on microchannel reactions at home and abroad has gradually been deeply in-depth, and various forms of impact flow reactors such as immersion and external circulation are developed. However, the Impinging St...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01J19/26B01J19/18B01J4/00
CPCB01J19/26B01J19/0093B01J19/0053B01J19/18B01J4/008B01J2204/002
Inventor 杨林涛鄢冬茂胥维昌刘东刘冰边策周川王珂贾志远刘嵩
Owner SHENYANG RES INST OF CHEM IND
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