A kind of preparation method of the azo lake type organic pigment that reduces aromatic amine residue

A technology of organic pigments and aromatic amines, applied in the field of organic pigments, can solve the problems of high cost and affecting the performance of pigments

Active Publication Date: 2022-05-10
LILY GRP CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

In this patent, 1-phenyl-3-methyl-5-pyrazolone and the second coupling component are added during the preparation of the coupling component liquid, which is costly and will affect the performance of the pigment to a certain extent

Method used

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  • A kind of preparation method of the azo lake type organic pigment that reduces aromatic amine residue
  • A kind of preparation method of the azo lake type organic pigment that reduces aromatic amine residue
  • A kind of preparation method of the azo lake type organic pigment that reduces aromatic amine residue

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0054] (1) Add 18.5 parts of p-toluidine o-sulfonic acid (4B acid) to 100 parts of water, stir and beat for 30 minutes, add 14 parts of 40% potassium hydroxide, heat up to 30°C, and dissolve transparently. Add ice to adjust the temperature to 10°C, add 8.6 parts of potassium nitrite, wait until it is completely dissolved, add ice and continue to adjust the temperature to 0°C, immediately add 30 parts of 30% hydrochloric acid, continue stirring for 1 hour until the diazotization is complete, and diazotization is obtained Liquid 1.

[0055] (2) 19 parts of 2-hydroxy-3 naphthoic acid, add 150 parts of water, stir for 30 minutes, add 15 parts of 40% potassium hydroxide and stir until completely dissolved, add ice to adjust the temperature to 10 ° C, adjust the system quality to 400 parts , prepared as coupling solution 2, to be coupled.

[0056] (3) Add diazonium salt 1 to coupling component 2 to carry out the coupling reaction. It takes 30 minutes to complete the addition. Durin...

Embodiment 2

[0060] (1) 22.1 parts of p-2-amino-4-chloro-5-methylbenzenesulfonic acid (2B acid), added to 150 parts of water, stirred and beaten for 30 minutes, added 8.8 parts of 20% ammonia water, heated to 35 ° C, Dissolves transparently. Add ice to adjust the temperature to 5°C, add 8.6 parts of potassium nitrite, until it is completely dissolved, add ice and continue to adjust the temperature to -2-0°C, immediately add 30 parts of 30% hydrochloric acid, and continue stirring for 1 hour until the diazotization is complete. Obtain diazo solution 1.

[0061] (2) 19 parts of 2-hydroxy-3 naphthoic acid, add 150 parts of water, stir for 30 minutes, add 9 parts of 20% ammonia water and stir until completely dissolved, add ice to adjust the temperature to 10°C, adjust the system quality to 400 parts, and prepare into coupling solution 2, to be coupled.

[0062] (3) Add the diazonium salt 1 to the coupling component 2 to carry out the coupling reaction. It takes 60 minutes to complete the ad...

Embodiment 3

[0066] Different from Example 1, in step (1), replace 8.6 parts of potassium nitrite with 6.9 parts of sodium nitrite, replace 14 parts of 40% potassium hydroxide with 13.4 parts of 30% sodium hydroxide, step (2) Replace 15 parts of 40% potassium hydroxide with 14.5 parts of 30% sodium hydroxide, all the other are the same. After the synthesis of step (3), use filter paper to detect, the inner circle of the permeation circle is red, and the outer circle is colorless, and the P.R.57 produced by the reaction partially dissociates molecular azo dyes, and most of the azo dyes are precipitates. In step (4), adjust the pH value with acid, and detect with filter paper until the percolation ring shows a change from red to colorless, at this time, pH=3-3.5, filter and rinse, and the mother liquor and rinse solution are colorless. In step (5), 25 parts of 40% potassium hydroxide are replaced by 24 parts of 30% sodium hydroxide, the system pH=11-11.5, and the azo dye crystal 5 is dissolv...

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Abstract

The invention discloses a method for preparing an azo lake-type organic pigment with reduced aromatic amine residue, and relates to the technical field of organic pigments. The method comprises the following steps: sequentially adding inorganic base, nitrite and strong inorganic acid to aromatic primary sulfonic acid or carboxylic acid derivatives to generate diazonium salt; adding inorganic base to naphthol compounds or their substituted derivatives to obtain Coupling component; mix reaction of diazonium salt and coupling component to generate soluble azo dye; adjust pH value of soluble azo dye, precipitate precipitated salt, filter and rinse to obtain azo dye crystal; disperse azo dye crystal in water , adding an inorganic base to dissolve, adding a precipitating agent for laking, and then undergoing pigmentation treatment to obtain the azo lake organic pigment. The method can reduce the residual aromatic amine of the azo lake organic pigment from 1000-5000ppm to below 500ppm, and has good application prospects.

Description

technical field [0001] The invention relates to the technical field of organic pigments, in particular to a method for preparing an azo lake-type organic pigment with reduced aromatic amine residues. Background technique [0002] Azo lake pigments are a class of diazo components that use aromatic primary sulfonic acid or carboxylic acid derivatives as diazo components, react with nitrous acid to form diazonium salts, and then react with naphthols and their substituted derivatives, such as: 2-naphthol, 2,3-acid, naphthol AS derivatives, naphthol sulfonic acid derivatives and other coupling components undergo coupling reactions to generate water-soluble azo dyes, which are then combined with precipitants (mainly metal ions) Such as: Ca 2+ , Ba 2+ , Mn 2+ ,Sr 2+ , Al 3+ and so on for precipitation reaction to generate azo lake pigments. If the diazo components such as aromatic primary amine sulfonic acid or carboxylic acid derivatives are not completely reacted during the...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C09B63/00C09B29/03C09B29/15
CPCC09B63/005C09B29/0007C09B29/106
Inventor 黄德平王丰莉熊永科陈立荣王迪明王桂峰高海华
Owner LILY GRP CO LTD
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