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Tubular micro mixer and continuous preparation method for azo pigment by using same

A micro-mixer and azo pigment technology, applied in the direction of azo dyes, monoazo dyes, chemical instruments and methods, etc., can solve the problems of large-scale and long-term pigment production, narrow microreactor mixing channels, It is difficult to clean the reactor and other problems, and achieve the effect of suppressing local overheating, improving reaction yield and product performance, and shortening the time

Active Publication Date: 2020-02-14
TIANJIN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the mixing channel of the microreactor is narrow, solid particles can easily block the channel, and the reactor is difficult to disassemble, it is difficult to clean the inside of the reactor, and it is difficult to apply to large-scale and long-term pigment production

Method used

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  • Tubular micro mixer and continuous preparation method for azo pigment by using same
  • Tubular micro mixer and continuous preparation method for azo pigment by using same
  • Tubular micro mixer and continuous preparation method for azo pigment by using same

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0039] A tubular micro-mixer, comprising a top cover 2, a cylinder body 3, and an outlet channel 7; the top cover 2 is tightly connected to the top of the cylinder body 3 in the form of a flange, and the length of the cylinder body 3 is 120mm, and the inner diameter The outlet channel 7 is coaxially connected to the bottom of the cylinder 3, and the inner diameter and outer diameter of the outlet channel 7 gradually decrease from top to bottom; the side wall of the cylinder 3 is provided with a second A feed port 1-1 and a second feed port 1-2, the first feed port 1-1 and the second feed port 1-2 are arranged oppositely, the length between the ports of the two feed ports The inner diameter of the two feeding ports is 90mm, and the inner diameter of the two feed ports is 4mm. The top cover 2 and the top of the cylinder body 3 are sealed by a flange gasket 4; a spoiler bar 5 is arranged at the center of the flange gasket 4, and the The spoiler rod 5 extends toward the outlet pas...

Embodiment 2

[0041] Preparation of Pigment Red 146 Compound by Continuous Process

[0042] Both the continuous diazotization reaction and the coupling reaction use the tubular micro-mixer in Example 1

[0043] Add 800mL of ice water, 30ml of 37% concentrated hydrochloric acid and 25.47g of 3-amino-4-methoxy-N-phenylbenzamide (red base KD) into a 2L beaker successively. Add water to make up the total volume of the suspension to 1 L, beat for 60 minutes to prepare 3-amino-4-methoxy-N-phenylbenzamide slurry, and cool to 0°C.

[0044] Add 800mL of ice water and 12.35g of sodium nitrite into a 2L beaker, stir until completely dissolved, dilute with water until the total volume of the solution is 1L to prepare a sodium nitrite solution, and cool to 0°C.

[0045] Transfer the above-mentioned 3-amino-4-methoxy-N-phenylbenzamide slurry and sodium nitrite solution to two storage tanks respectively, and use a calibrated metering pump to adjust the The flow rates of the oxy-N-phenylbenzamide slurry ...

Embodiment 3

[0056] Preparation of Pigment Yellow 12 Compound (Benzidine Yellow G, C.I.Pigment Yellow 12)

[0057] Both the continuous diazotization reaction and the coupling reaction use the tubular micro-mixer in Example 1

[0058] In a 2L beaker, add 1L of ice water, 140ml of 37% concentrated hydrochloric acid and 105g of 3,3'-dichlorobenzidine hydrochloride (DCB hydrochloride) successively. Add water to make up the total volume of the suspension to 1.5L, beat for 60 minutes to prepare 3,3'-dichlorobenzidine slurry, and cool to 0°C.

[0059] Add 1L of ice water and 55g of sodium nitrite into a 2L beaker, stir until completely dissolved, dilute with water until the total volume of the solution is 1.5L to prepare a sodium nitrite solution, and cool to 0°C.

[0060] Transfer the above 3,3'-dichlorobenzidine slurry and sodium nitrite solution to two storage tanks respectively, and use a calibrated metering pump to adjust the 3,3'-dichlorobenzidine slurry and sodium nitrite The flow rates ...

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Abstract

The invention discloses a tubular micro mixer which comprises a top cover, a cylinder body and an outlet channel. The top cover is tightly connected with the top of the cylinder body in a flange mode,and the outlet channel is coaxially connected with the bottom of the cylinder body. The inner diameter and the outer diameter of the outlet channel gradually decrease from top to bottom. A first feeding hole and a second feeding hole are oppositely formed in the side wall of the cylinder body. The top cover and the cylinder body are sealed through a flange gasket. A spoiler bar is arranged in thecenter of the flange gasket, an electrode bar is inserted into the spoiler bar in a hollow structure, and spoiler particles are further arranged on the spoiler bar. The invention also discloses a continuous preparation method of azo pigment, which adopts the tubular micro mixer and comprises the following steps: 1) diazonium salt solution preparation, 2) coupling reaction, 3, depigmentation and 4) separation and drying. The reaction process of the method does not need to be carried out at a low temperature, the demand on a cold medium is reduced, and the energy consumption is greatly reduced;the preparation time of the pigment is greatly shortened, the production efficiency is improved, the product yield is high, and the average particle size is small.

Description

technical field [0001] The invention belongs to the technical field of organic chemistry, and in particular relates to a tubular micro-mixer and its continuous preparation method for azo pigments. Background technique [0002] In fine chemical industry, polymer chemical industry, and pharmaceutical engineering, it is often necessary to uniformly disperse the components to ensure that the mixing is fully completed and some complex chemical processes are completed. Therefore, it is necessary to adopt more efficient and economical production technology. Continuous production technology is a new and efficient process intensification technology, which has the advantages of efficient mass and heat transfer, easy scale-up, and safety (Chem.Soc.Rev.2010, 39(3):1153-1182). Some of them are widely used, but they are rarely used in the continuous reaction of solid-liquid system. [0003] Azo pigments are widely used in printing, ink, paint and textile industries, accounting for more ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J19/00C09B29/20C09B29/33C09B67/36
CPCB01J19/0093B01J2219/00797B01J2219/00853B01J2219/00873B01J2219/00889B01J2219/00894B01J2219/00961B01J2219/00966C09B29/20C09B29/33C09B67/0079
Inventor 周雪琴刘东志李巍石至平
Owner TIANJIN UNIV
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