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Continuous preparation method of azo pigment in branch spiral tube

A technology of branched spiral tubes and azo pigments, which is applied in the direction of azo dyes, monoazo dyes, chemical instruments and methods, etc., can solve the problems of continuous reaction in reactors with no branched helical structure, and achieve broad industrialization prospects, The effect of high tinting strength and high quality stability

Active Publication Date: 2016-06-08
SUZHOU SUNMUN TECH CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

But at present, the branch mixer is mainly a planar branch structure, and there is no branch helical structure reactor and related reports on continuous reaction in this structure reactor.

Method used

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  • Continuous preparation method of azo pigment in branch spiral tube
  • Continuous preparation method of azo pigment in branch spiral tube
  • Continuous preparation method of azo pigment in branch spiral tube

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0032] Example 1 Preparation of Fast Yellow 5GX (C.I.PigmentYellow74)

[0033] (1) Continuous method for preparing diazonium salt

[0034] In a 500ml beaker, add 200ml of water, 16.8g of 2-methoxy-4-nitroaniline and 25ml of 37% concentrated hydrochloric acid successively, stir until completely dissolved, dilute with water until the total volume of the solution is 250ml, and obtain 2-methoxy-4-nitroaniline 4-nitroaniline solution, cooled to 0 ° C.

[0035] Add 200ml of water and 7.59g of sodium nitrite successively into a 500ml beaker, stir until the solution is complete, dilute with water until the total volume of the solution is 250ml to obtain a sodium nitrite solution, and cool to 0°C.

[0036] Transfer the above-mentioned 2-methoxyl-4-nitroaniline solution and sodium nitrite solution to two storage tanks respectively, and use a calibrated peristaltic pump to adjust the 2-methoxyl-4-nitroaniline solution and sodium nitrite solution. The flow rate of sodium nitrate solutio...

Embodiment 2

[0040] Embodiment 2 prepares permanent orange GR (C.I.PigmentOrange18)

[0041] (1) Continuous method for preparing diazonium salt

[0042] Add 150ml of ice water, 9.5ml of aniline and 25ml of 37% concentrated hydrochloric acid to a 500ml beaker in turn, stir until completely dissolved, add water to make up the total volume of the solution to 250ml to obtain aniline solution, and cool to 0°C.

[0043] Add 200ml of ice water and 7.5g of sodium nitrite successively into a 500ml beaker, stir until the solution is complete, add water to dilute until the total volume of the solution is 250ml, to obtain a sodium nitrite solution, and cool to 0°C.

[0044] Transfer the above-mentioned aniline solution and sodium nitrite solution to two storage tanks respectively, use a calibrated peristaltic pump to adjust the flow rate of the aniline solution and sodium nitrite solution to 20ml / min, and transport the two reactants to the branch Spiral tube reactor (the number of branch spiral tube ...

Embodiment 3

[0051] Embodiment 3 prepares toluidine red (C.I.PigmentRed3)

[0052] (1) Ordinary diazotization reaction

[0053] 200ml of water, 15g of 4-methyl-2-nitroaniline and 25ml of 37% hydrochloric acid were successively added into a 500ml beaker, and the mixture was cooled to 0-5° C. using an ice-water bath. Add 30ml of 25% sodium nitrite solution at this temperature, and continue to stir at 0°C for more than half an hour, add sulfamic acid to remove excess sodium nitrite. Dilute with water until the total volume of the solution is 500ml to obtain a diazonium salt solution.

[0054] (2) Continuous coupling reaction

[0055] 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, then add 10g of sodium carbonate, Dilute with water until the total volume of the solution is 500ml.

[0056] Transfer the 4-methyl-2-nitroaniline di...

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Abstract

The invention discloses a method for continuously preparing azo pigment in branch spiral tube, and belongs to the technical field of fine chemical industry. The preparation method comprises the following steps: (1) diazotization of aromatic amines or heterocyclic amines; (2) coupling reaction; (3) performing color lake which is selective, wherein at least the step (2) is performed in a branch spiral tube. According to the method, high-efficiency mixing of secondary flow of fluids generated in the spiral tube and the property that the branch structure changes the motion trajectory of fluids and increases the mixed surface area of the fluids to enhance the mixing effect allow full contact, mixing and reaction of two parts of materials, and therefore the method disclosed by the invention has the advantages of no need of mixing, narrow product size distribution, high quality stability and the like, not only is the continuous production of the pigment achieved, but also the prepared azo pigment has higher tinting strength and smaller size when used for preparing water base colorants, and wide industrial prospect is achieved.

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 an azo pigment in a branched spiral tube. Background technique [0002] Azo pigments have a wide chromatographic distribution and are the main category of organic pigments. The output accounts for about 40% of the total output of organic pigments. The production process of azo pigments involves a coupling reaction process, that is, the reaction of diazonium salts and coupling components such as aromatic amines or phenols to form azo compounds. In the coupling reaction, the diazonium salt is easy to decompose, especially when the coupling component is a phenolic compound, it often needs to be coupled under alkaline conditions. Molecules collide and react, quickly disintegrating. However, due to the large geometric size of the conventional reactor, it is impossible to achieve instant mixing, resulting in...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C09B29/33C09B29/16C09B29/15C09B67/20
Inventor 杜长森梁栋卢圣国梅成国周华
Owner SUZHOU SUNMUN TECH CO LTD
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