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A kind of micro-mixer for continuous synthesis of azo pigments and its continuous preparation method

A technology of azo pigments and micro-mixing, applied in chemical instruments and methods, azo dyes, chemical/physical/physicochemical processes, etc., can solve problems such as difficult disassembly and cleaning, improve reaction yield and product performance, overcome Easy to clog and reduce energy consumption

Active Publication Date: 2022-02-01
天津隐一科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the narrower channel increases the probability of clogging, and it is difficult to disassemble and clean once a clog occurs

Method used

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  • A kind of micro-mixer for continuous synthesis of azo pigments and its continuous preparation method
  • A kind of micro-mixer for continuous synthesis of azo pigments and its continuous preparation method
  • A kind of micro-mixer for continuous synthesis of azo pigments and its continuous preparation method

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0045]A continuous micro-mixing device, the continuous mixing device is a "T"-shaped structure, including an upper transverse part and an outlet channel connected to the middle of the upper transverse part and vertically connected with the upper transverse part; The first part is a tubular structure with a length of 60mm and an inner diameter of 4mm, and its two ends are feed ports. The outlet channel is also a tubular structure and is divided into upper and lower sections. The upper outlet channel has a length of 40mm and an inner diameter of 15mm and the lower outlet The length of the channel is 30mm, and the inner diameter is 15mm. The upper outlet channel and the lower outlet channel are connected by a flange. The center of the gasket of the flange is provided with a spoiler rod with a length of 25mm and a diameter of 6mm. The spoiler rod Extending to the upper horizontal part, the spoiler bar is also provided with two spherical spoiler particles, the diameter of which is 1...

Embodiment 2

[0047] Preparation of Pigment Yellow 12 Compound (Benzidine Yellow G, C.I.Pigment Yellow 12)

[0048] Both the continuous diazotization reaction and the coupling reaction use the continuous micro-mixing device in Example 1

[0049] 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 1.5 L, beat for 60 minutes to prepare 3,3'-dichlorobenzidine slurry, and cool to 0°C.

[0050] 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.

[0051] Transfer the above-mentioned 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 ni...

Embodiment 3

[0058] Preparation of Pigment Yellow 14 Compound (Eternal Yellow G, C.I.Pigment Yellow 14)

[0059] Both the continuous method diazotization reaction and the coupling reaction use the micro-mixer in Example 1

[0060] 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 1.5 L, beat for 60 minutes to prepare 3,3'-dichlorobenzidine slurry, and cool to 0°C.

[0061] 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.

[0062] Transfer the above-mentioned 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 flo...

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Abstract

The invention discloses a continuous micro-mixing device, which is characterized in that the continuous micro-mixing device is a "T"-shaped structure, including an upper transverse part connected to the middle part of the upper transverse part and vertically connected to the upper transverse part The outlet channel; the outlet channel is divided into an upper outlet channel and a lower outlet channel, and the upper outlet channel and the lower outlet channel are connected by a flange and sealed by a flange gasket, and the center of the flange gasket is provided with a A spoiler bar, the spoiler bar extends toward the upper transverse part, the spoiler bar is also provided with spoiler particles, and the flange gasket is also provided with flow holes for material circulation. Also disclosed is a continuous preparation method for azo pigments, which adopts the above continuous micro-mixing device; has a higher reaction temperature, reduces the demand for cold media, and greatly reduces energy consumption; greatly shortens the The time for pigment preparation improves the production efficiency, meanwhile, the yield of the product is high (>98%) 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 continuous synthesis device of an azo pigment and a continuous preparation method thereof. Background technique [0002] Dyes and pigments are traditional fine chemical products. Up to now, many varieties of dyes and pigments with good cost performance have been widely used, and the production of corresponding varieties and intermediates has reached a scale of tens of thousands of tons. Among organic pigments, azo pigments are a typical type of pigment with a complete color spectrum, accounting for more than 75% of the total production of organic pigments, and are widely used in various fields such as inks, plastics, coatings, and textiles, and have become indispensable in national life. The product. At present, my country's dyeing and pigment industry generally uses batch reactors to produce azo pigments, which have problems such as long reaction time, p...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01J19/00C09B35/035C09B67/20
CPCB01J19/0093C09B35/035C09B67/0065B01J2219/00889B01J2219/00894
Inventor 周雪琴李巍刘东志石至平杜允
Owner 天津隐一科技有限公司
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