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Preparation method of pigment yellow 81

A pigment yellow and slurry technology, applied in the field of pigment yellow 81 preparation, can solve the problems of unable to meet the performance requirements of pigment yellow 81, large gap between standard samples, large production particle size, etc., to reduce color difference, reduce impurities, reduce The effect of particle size

Active Publication Date: 2019-12-31
龙口佳源颜料有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, at present, the production particle size of Pigment Yellow 81 is relatively large. For example, the Chinese patent with the authorized announcement number CN108752974B discloses a preparation method of benzidine organic pigments, and the minimum particle size of the prepared pigments is also as high as 15.401 μm , the hiding power is weak, and the gap with the standard sample is large, which cannot meet the current performance requirements for Pigment Yellow 81

Method used

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  • Preparation method of pigment yellow 81
  • Preparation method of pigment yellow 81

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Experimental program
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Embodiment 1

[0035] A preparation method of Pigment Yellow 81, comprising the following steps:

[0036] a, synthesis of diazo solution:

[0037] In parts by weight, beat 1200 parts of water, 150 parts of tetrachlorobenzidine, and 7.5 parts of adsorbent clay for 1 hour and 10 minutes, add 435 parts of hydrochloric acid with a mass concentration of 30%, add ice and stir for 6 hours and cool down to 0°C to obtain a slurry;

[0038] After dissolving 63 parts of sodium nitrite, add it to the slurry in 1 minute, the starch potassium iodide test paper shows a slight blue color, stir at 3°C ​​for 120 minutes, add sulfamic acid to remove excess nitrite ions, add diatomaceous earth and filter to obtain diazonium solution for later use ;

[0039] b. Preparation of coupling solution:

[0040] Stir and dissolve 2000 parts of water, 268 parts of liquid caustic soda with a mass concentration of 30%, and 180 parts of acetylacetyl-2,4-dimethylaniline, and adjust the temperature to 5°C to obtain a couplin...

Embodiment 2

[0047] A preparation method of Pigment Yellow 81, comprising the following steps:

[0048] a, synthesis of diazo solution:

[0049] In parts by weight, 1200 parts of water, 150 parts of tetrachlorobenzidine, and 10 parts of adsorbent clay were beaten for 1 hour and 10 minutes, and 455 parts of hydrochloric acid with a mass concentration of 30% were added, and stirred with ice for 6 hours and cooled to 1 ° C to obtain a slurry;

[0050] After dissolving 69 parts of sodium nitrite, add it to the slurry in 2 minutes, the starch potassium iodide test paper shows a slight blue color, stir at 4°C for 120 minutes, add sulfamic acid to remove excess nitrite ions, add diatomaceous earth and filter to obtain diazonium solution for later use ;

[0051] b. Preparation of coupling solution:

[0052] Stir and dissolve 2000 parts of water, 268 parts of liquid caustic soda with a mass concentration of 30%, and 199 parts of acetylacetyl-2,4-dimethylaniline, and adjust the temperature to 8°C ...

Embodiment 3

[0059] A preparation method of Pigment Yellow 81, comprising the following steps:

[0060] a, synthesis of diazo solution:

[0061] In parts by weight, beat 1200 parts of water, 150 parts of tetrachlorobenzidine, and 15 parts of adsorbent clay for 1 hour and 10 minutes, add 480 parts of hydrochloric acid with a mass concentration of 30%, add ice and stir for 6 hours and cool down to 2°C to obtain a slurry;

[0062] After dissolving 75 parts of sodium nitrite, add it to the slurry in 2 minutes, the starch potassium iodide test paper shows a slight blue color, stir at 5°C for 120 minutes, add sulfamic acid to remove excess nitrite ions, add diatomaceous earth and filter to obtain diazonium solution for later use ;

[0063] b. Preparation of coupling solution:

[0064] Stir and dissolve 2000 parts of water, 268 parts of liquid caustic soda with a mass concentration of 30%, and 225 parts of acetylacetyl-2,4-dimethylaniline, and adjust the temperature to 10°C to obtain a coupling...

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Abstract

The invention discloses a preparation method of pigment yellow 81. The method comprises the following steps: a, synthesis of diazonium liquid: adding tetrachlorobenzidine and an adsorbent into water,carrying out smashing, carrying out cooling to 2 DEG C or below, carrying out stirring to obtain slurry, and under an acidic condition, adding sodium nitrite into the slurry for a diazotization reaction to obtain diazonium liquid for later use; b, preparation of a coupling liquid: dissolving sodium hydroxide and 2',4'-dimethylacetoacetanilide in water, adjusting a temperature to 5-10 DEG C to obtain a coupling component liquid, adding an emulsifier into the coupling component liquid, and performing acid precipitation for 40-50 minutes until a pH value is equal to 5-6 after acid precipitation is finished so as to obtain the coupling liquid, wherein the emulsifier is prepared from tallow-based propylene diamine and dimethyldodecylamine oxide in a mass ratio of 1: (0.37-0.75); c, a coupling reaction: dropwise adding the diazonium liquid into the coupling liquid, and carrying out the coupling reaction to obtain feed liquid; and d, heating and heat preservation: heating the feed liquid to 85-95 DEG C, keeping the feed liquid at the temperature for 15-25 minutes, and successively carrying out cooling, filtering, washing with water, drying and crushing to obtain the pigment yellow 81 withsmall particle size, high covering power and small difference between color measurement data and a standard sample.

Description

technical field [0001] The invention relates to the technical field of pigment preparation, in particular to a preparation method of Pigment Yellow 81. Background technique [0002] Pigment Yellow 81 is an important organic pigment in powder form. As a synthetic product of the diazo component, the adjacent and para-positions of the amino group of the diazo component of Pigment Yellow 81 have charge-absorbing groups, which help to strengthen the formation of hydrogen bonds in Pigment Yellow 81. Therefore, the resistance of Pigment Yellow 81 It has good properties such as heat resistance and light resistance, and has a wide range of applications in the coloring of plastics, paints, inks, rubber and other materials, with broad prospects. [0003] In the production process, the particle size of Pigment Yellow 81 is an important factor to determine its performance. The smaller the particle size, the higher the hiding power and the better the vividness of Pigment Yellow 81 under ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C09B29/33C09B67/20
CPCC09B29/33C09B67/0065
Inventor 王伟
Owner 龙口佳源颜料有限公司