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Serial preparation method of cladding azo pigment in branch spiral pipe

A technology of branched spiral tubes and azo pigments, applied in the direction of azo dyes, monoazo dyes, chemical instruments and methods, etc., to achieve the effect of easy to become unstable, small particle size, and broad industrialization prospects

Active Publication Date: 2016-11-16
SUZHOU SUNMUN TECH CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Mercapto compounds can perform Michael addition reaction efficiently and quickly with compounds containing carbon-carbon double bonds. This reaction is widely used in the preparation of cross-linked network polymers and other functional polymers. The Michael addition reaction of active agents and mercapto compounds is rarely reported in the preparation of coated pigments, let alone the continuous preparation of coated azo pigments in small channels

Method used

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  • Serial preparation method of cladding azo pigment in branch spiral pipe
  • Serial preparation method of cladding azo pigment in branch spiral pipe
  • Serial preparation method of cladding azo pigment in branch spiral pipe

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0039] Example 1 Preparation of Coated Sunfast Yellow 5GX (C.I.Pigment Yellow 74)

[0040] Step 1: Preparation of Coupling Component Solution:

[0041]Add 20.7g o-methoxy acetoacetanilide and 400ml water in 800ml beaker, then add 2.07g cardanol base gemini surfactant as shown in formula (III), add 10.6g sodium carbonate again, stir, add water again dilute When the total volume of the solution is 500ml, a coupling component solution is obtained.

[0042] Step 2: Preparation of diazonium salt solution: prepare 2-methoxy-4-nitroaniline diazonium salt solution with the same molar concentration as the coupling component solution for later use.

[0043]

[0044] Step 3: Coupling reaction: transfer the 2-methoxy-4-nitroaniline diazonium salt solution and the o-methoxyacetoacetanilide solution to the storage tanks of the diazo component and the coupling component respectively, and use the calibrated peristaltic Pump, adjust the flow rate of the diazo component solution and the co...

Embodiment 2

[0047] Example 2 Preparation of coated toluidine red (C.I.Pigment Red 3)

[0048] Step 1: Preparation of Coupling Component Solution:

[0049] Add 300ml of water, 14.5g of 2-naphthol and 10g of sodium hydroxide successively in a 500ml beaker, stir until dissolved, then add 50mL of 37% hydrochloric acid solution, 2-naphthol is suspended in the solution, and then 2.9g of The cardanol-based gemini surfactant shown in formula IV, and add 10g sodium carbonate, add water and dilute to solution total volume and be 500ml.

[0050] Step 2: Preparation of diazonium salt solution: prepare 4-methyl-2-nitroaniline diazonium salt solution with the same molar concentration as the coupling component solution for later use.

[0051]

[0052] Step 3: Coupling reaction: transfer the 4-methyl-2-nitroaniline diazonium salt solution and the 2-naphthol suspension to the storage tanks of the diazo component and the coupling component respectively, and use a calibrated peristaltic pump to adjust ...

Embodiment 3

[0055] Example 3 Preparation of coated permanent yellow NCG (C.I.Pigment Yellow 16)

[0056] Step 1: Preparation of Coupling Component Solution:

[0057] In a 1L beaker, add 800ml of water, 38g 3,3'-dimethylbisacetoacetylbenzidine and 10g of sodium hydroxide successively, and stir. Then add 5.7g of cardanol-based gemini surfactant shown in formula III and 35ml of 30% sodium hydroxide solution, quickly add 50ml of glacial acetic acid, and 3,3'-dimethylbisacetoacetylbenzidine is suspended in Solution, add water to dilute to a total solution volume of 1000ml.

[0058] Step 2: Preparation of diazonium salt solution: prepare 2,5-dichloroaniline diazonium salt solution with the same molar concentration as the coupling component solution for later use.

[0059] Step 3: Coupling reaction: transfer the 2,5-dichloroaniline diazonium salt solution and the 3,3'-dimethylbisacetoacetylbenzidine suspension to the storage tanks of the diazo component and the coupling component respectively,...

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Abstract

The invention relates to a serial preparation method of cladding azo pigment in a branch spiral pipe. The preparation method comprises the following steps of step I, preparing a coupling component solution; step II, preparing a diazonium salt solution; step III, performing a coupling reaction in a branch spiral pipe reactor; step IV, preparing a thioglycolate solution; and step V, preparing cladding azo pigment fluid. According to the preparation method disclosed by the invention, on one hand, a high-efficiency mixed and branched structure enabling the fluid to produce a secondary flow in the spiral pipe is used for changing the movement track of the fluid and enlarging the mixed surface area of the fluid so as to strengthen mixing effects, diazo components and coupling components are in sufficient contact, mixing and reaction, and the azo pigment which is small in particle diameter of products and narrow in distribution is continuously prepared; and on the other hand, through a Michael addition reaction of carbon-carbon double bonds in gemini surfactants of a thioglycolate compound and gemini surfactants in a cardanol group, the cross-linking cladding of the newly-prepared azo pigment is realized, and cladding azo pigment dispersed bodies small in particle diameter, narrow in size distribution and high in dispersion stability are prepared.

Description

technical field [0001] The invention relates to the technical field of fine chemical industry, more specifically, the invention relates to a continuous preparation method of coated azo pigment in a branch spiral tube. Background technique [0002] Azo pigments are continuously synthesized in micro-reactors. Since the reaction is carried out continuously, the reaction solution is mixed evenly in a small space instantly, which prevents side reactions caused by local excess. The synthesized azo pigments have small particle size and narrow distribution. , high yield and high tinting strength. This process has a large number of literature reports at home and abroad, such as Chinese patents CN1398282 and CN1330115 respectively disclose a method of using a microchannel reactor to synthesize monoazo pigments and disazo pigments, and Chinese patent CN104479394A discloses a method using a small channel A method for synthesizing azo pigments in a branched helical tube reactor. Howeve...

Claims

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Application Information

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IPC IPC(8): C09B67/20C09B67/08C09B29/33C09B29/15
CPCC09B29/103C09B29/337C09B67/0013
Inventor 吕仕铭梁栋杜长森胡冲
Owner SUZHOU SUNMUN TECH CO LTD
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