Industrial production method for pigment yellow 81

A production method and technology for pigment yellow, applied in the direction of organic dyes, etc., can solve the problems of poor heat resistance, light resistance, poor application performance, low pigment yield, and narrow application range, and achieve low equipment requirements, short reaction time, enhanced The effect of application performance

Active Publication Date: 2013-05-15
CROWN CHEMICAL CORP
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The diazonium liquid obtained by this diazotization method is coupled with 2,4-dimethyl-N-acetylacetoanilide (AAMX for short), and the pigment yield is low, the color is dark, and the application of heat resistance and light resistance, etc. The performance is poor, the application range is narrow, and the synthesis cost is high

Method used

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  • Industrial production method for pigment yellow 81
  • Industrial production method for pigment yellow 81

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0028] 1) Put 175Kg of TCB into a common reaction kettle, add 2000Kg of water and 500Kg of ice cubes, beat 50Kg of zeolite at 0°C to form salt for 1 hour; quickly add 400Kg of 30% hydrochloric acid, and then slowly add 40% of nitrous acid at 0°C 200Kg of sodium solution was diazotized and stirred for 2 hours, and excess sodium nitrite was removed with sulfamic acid to obtain diazonium solution;

[0029] 2) Inject 233Kg AAMX into the coupling reaction kettle, add 200Kg dilute lye, stir until 2,4-dimethyl-N-acetoacetanilide is dissolved, add 24.5Kg surfactant SF-1 and 14KgSF to the coupling reaction kettle -2, hydrochloric acid acid precipitation at 0°C to a pH of 6.0;

[0030] 3) After filtering the diazo solution to remove the active adsorbent, add it to the coupling reaction kettle at 5°C for coupling reaction. After adding the diazo solution, stir for 30 minutes; post-treatment, heat up to 90°C, keep it warm for 30 minutes, cool down and filter, Drying at 90°C, the obtained...

Embodiment 2

[0033] 1) Pour 175Kg TCB into a common reactor, add 2000Kg water, 500Kg ice cubes and 50Kg kaolin, beat at -10°C for 3 hours; quickly add 400Kg of 30% hydrochloric acid, and then quickly add 40% nitrous acid at 10°C 200Kg of sodium solution was diazotized, reacted for 1 hour, and excess sodium nitrite was removed with sulfamic acid;

[0034] 2) Pour 233Kg AAMX into the coupling reaction kettle, add 200Kg dilute lye, stir to dissolve. Add 24.5Kg surfactants SF-1 and 14KgSF-2 to the coupling reaction kettle, hydrochloric acid acid analysis at 0°C until the pH is 5.0; filter the diazo solution to remove the adsorbent and add it to the coupling reaction kettle at 5°C for coupling reaction. Stir for 30 minutes after adding the diazonium solution; post-treatment, raise the temperature to 90°C, keep it warm for 30 minutes, cool down and filter, and dry at 90°C. The yield of the obtained pigment is 389.5Kg, the yield is 95.1%, and the appearance of the pigment is bright. Pigment ap...

Embodiment 3

[0036] Inject 175Kg of TCB into a high-speed stirring reactor, add appropriate amount of water and 87.5Kg of diatomaceous earth, beat for 2 hours at 0°C; quickly add 400Kg of 30% hydrochloric acid, and then quickly add 200Kg of 40% sodium nitrite solution at 0°C Nitriding, react for 1 hour, remove excess sodium nitrite with sulfamic acid; inject 250Kg AAMX into the coupling reaction kettle, add 200Kg dilute lye, stir to dissolve. Add 24.5Kg surfactants SF-1 and 14KgSF-2 to the coupling reaction kettle, hydrochloric acid acid analysis at 0°C until the pH is 5.5; filter the diazo solution to remove the adsorbent and add it to the coupling reaction kettle at 5°C for coupling reaction. Stir for 30 minutes after adding the diazonium solution; post-treatment, raise the temperature to 90°C, keep it warm for 30 minutes, cool down and filter, and dry at 90°C. The yield of the obtained pigment: 405.9 Kg, the yield rate is 99.0%, the appearance of the pigment is bright, the application ...

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Abstract

The invention discloses an industrial production method for pigment yellow 81 and belongs to the technical field of fine chemical synthesis. The industrial production method comprises the following steps of: pulping, diazotizing and coupling such materials as 2,2',5,5'-tetrachlorobiphenyl amine hydrochloride, 2,4-dimethyl-N-acetoacetanilide and the like; stirring the materials for 1 hour to 4 hours after the reaction is finished; heating up the reaction liquid to 80 DEG C to 100 DEG C, preserving the heat for reaction for 30 minutes; cooling the reaction liquid to the room temperature, filtering the reaction liquid; and drying the reaction liquid at 70 DEG C to 100 DEG C to obtain the pigment yellow 81. According to the industrial production method disclosed by the invention, the reaction conditions are gentle, the device requirements are low, the reaction time is short; moreover, the obtained product pigment yellow 81has a high yield of more than 90%, good performances, acid resistance of lever four or higher, alkali resistance of level four or high, weather resistance of level six or higher, and heat resistance to 200 DEG C or high, and so the pigment yellow 81 disclosed by the invention can be applied to rubber with high performance requirements and high-level paint.

Description

technical field [0001] The invention belongs to the technical field of fine chemical synthesis, and specifically relates to a kind of 2,2',5,5'-tetrachlorobenzidine hydrochloride as a raw material, which is synthesized by diazotization reaction and other reactions after adding an active adsorbent to disperse Industrial production method of Pigment Yellow 81. Background technique [0002] 2,2',5,5'-Tetrachlorobenzidine hydrochloride is an important organic pigment intermediate. The C.I.P.Y.81 (Pigment Yellow 81) toner synthesized as a diazo component is lemon yellow, bright in color and high in tinting strength. It is a high-grade organic pigment. [0003] 2,2',5,5'-Tetrachlorobenzidine hydrochloride has an electron-withdrawing group (chlorine group) at the ortho and para positions of the amino group, which helps to strengthen the formation of hydrogen bonds in C.I.P.Y.81, so the heat resistance of C.I.P.Y.81 It has excellent application properties such as durability and li...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C09B67/20
Inventor 杨宗泽陈奇文李红霞贺小波施国英
Owner CROWN CHEMICAL CORP
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