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Industrial production method of pigment yellow 97

A production method and technology of pigment yellow, applied in chemical instruments and methods, azo dyes, organic dyes, etc., can solve the problem of poor heat resistance, light resistance, poor application performance, low yield of pigment yellow 97, narrow application range, etc. problem, to achieve the effect of improving the beating effect, speeding up the speed, and improving the dispersion effect.

Active Publication Date: 2015-03-11
CROWN CHEMICAL CORP
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Pigment Yellow 97 obtained by this method has low yield, poor dispersibility, dark shade, poor heat resistance, light resistance and other application properties, and narrow application range

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0033] 1) Add 134KgOBS into the ordinary reaction kettle, add 385Kg water for beating for 1h; then quickly add 201kg hydrochloric acid for beating for 1h; lower the temperature of the solution below 0°C, quickly add 150Kg of 40% sodium nitrite solution for diazotization, and then Stir for 1h, then carry out suction filtration to obtain clear diazonium liquid;

[0034] 2) Inject 132Kg of AS-IRG into an ordinary reaction kettle, add 622kg of water and 70Kg of liquid caustic soda, heat up to 35°C, stir and clear to obtain AS-IRG solution;

[0035] 3) Inject 50Kg of formic acid into the coupling reaction kettle, add 1000Kg of water, and stir evenly; then add Huaqing's additives Pingpingjia, OS-15 and SF-1; add ice cubes to lower the temperature to 5°C, and then gradually Add the AS-IRG solution obtained in step 2) for acid back analysis, and the addition time is 40 minutes to obtain a coupling solution, pH=4.8;

[0036] 4) Add the clear diazo solution to the coupling solution at ...

Embodiment 2

[0039] 1) Add 134KgOBS into the ordinary reaction kettle, add 385Kg water for beating for 2 hours; then quickly add 201kg hydrochloric acid for beating for 2 hours; lower the temperature of the solution to below 0°C, quickly add 160Kg of 40% sodium nitrite solution for diazotization and stirring reaction 1.5h, then carry out suction filtration to obtain clear diazo liquid;

[0040] 2) Inject 132Kg of AS-IRG into an ordinary reaction kettle, add 75Kg of liquid caustic soda, heat up to 35°C, and stir to dissolve to obtain AS-IRG solution;

[0041] 3) Pour 56Kg of glacial acetic acid into the coupling reaction kettle, add 1000Kg of water, and stir evenly; then add Huaqing's additives OS-15, SF-1 and MOA-4; add ice cubes to lower the temperature to 5°C, Then gradually add AS-IRG for acid reverse analysis, the addition time is 50 minutes, to obtain the coupling solution, pH=5.2;

[0042] 4) Add the clear diazo solution to the coupling solution at 15°C for coupling reaction, the ad...

Embodiment 3

[0044]1) Add 134KgOBS into the ordinary reaction kettle, add 385Kg water for beating for 1h; then quickly add 201kg hydrochloric acid for beating for 1h; lower the temperature of the solution to below 0°C, quickly add 170Kg of 40% sodium nitrite solution for diazotization and stirring reaction 2h, then carry out suction filtration to obtain clear diazo liquid;

[0045] 2) Inject 132Kg of AS-IRG into an ordinary reaction kettle, add 80Kg of liquid caustic soda, heat up to 35°C, stir and dissolve to obtain AS-IRG solution;

[0046] 3) Inject 25Kg of formic acid and 28Kg of glacial acetic acid into the coupling reaction kettle, add 1000Kg of water, and stir evenly; then add Huaqing additives Pingpingjia, OS-15, SF-2 and FM; add ice cubes to lower the temperature to 5°C, then gradually add AS-IRG for acid back analysis, the addition time is 1 hour, to obtain a coupling solution, pH=5.0;

[0047] 4) Add the clear diazo solution to the coupling solution at 15°C for coupling reactio...

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Abstract

The invention discloses an industrial production method of pigment yellow 97, and belongs to the technical field of fine chemical engineering synthesis. The industrial production method comprises the following steps: using 4-amino-2,5-dimethoxy sulfonamide as a raw material, performing acid treatment, then performing diazotization reaction under a low temperature condition, conducting a coupling reaction with 4-chloro-2,5-dimethoxy sulfonamide acidified with a mixing additive, and then using alkali to perform molecular recrystallization treatment to synthesize the high-performance pigment yellow 97. With application of the technology, reverse acidification, post-treatment and the addition of alkali are used to adjust the strong basicity to provide the strong base condition for the reaction, so as to break the bonds among the molecules which are partially and irregularly gathered during the coupling process, enable the pigment molecules to be recombined, enable the molecular crystal forms to be more regular and uniform. Therefore, the pigment properties can be improved, the acid resistance is up to level 6 above, the alkali resistance is up to level 7 above, the weather resistance is up to level 8 above, and the heat-resistance temperature is 230 DEG C.

Description

technical field [0001] The invention belongs to the technical field of fine chemical synthesis, and specifically relates to a kind of 4-amino-2,5-dimethoxybenzenesulfonic acid amide (OBS) as raw material, after acid treatment, diazotization reaction under low temperature conditions, and 4-Chloro-2,5-dimethoxyacetylacetanilide (AS-IRG) after acid precipitation was added to the mixing aid for coupling reaction, and then molecular recrystallization with alkali to synthesize high-performance Pigment Yellow 97 Industrial production methods. Background technique [0002] 4-Amino-2,5-dimethoxybenzenesulfonic acid amide (OBS) is an important organic pigment intermediate, which is used as a diazo component to synthesize C.I.P.Y.97 (Pigment Yellow 97) toner with a neutral yellow color, Similar to C.I.P.Y.1 (Pigment Yellow 1), it is a high-grade organic pigment with bright color and high hiding power. [0003] OBS and AS-IRG have multiple stabilizing groups methoxy and acetyl, and re...

Claims

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Application Information

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IPC IPC(8): C09B29/33
Inventor 杨宗泽贺小波毛波
Owner CROWN CHEMICAL CORP
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