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Method for preparing azo compounds with narrow particle size distribution

A technology for azo compounds, which is applied in the field of preparing azo compounds with narrow particle size distribution, and can solve the problems of cumbersome and lengthy steps

Inactive Publication Date: 2018-03-13
NANTONG HENGSHENG FINE CHEM +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] In summary, the existing preparation particle size distribution D 90 The steps of the method for azo compounds of 0.10μ~0.15μ are quite cumbersome and lengthy, and require high-precision sanding machinery

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0019] Example 1 (Preparation of Ultrafine C.I. Pigment Yellow 1)

[0020] (1) diazotization reaction

[0021] In a 250mL three-necked flask, add red base GL (15.5g, 0.1mol) and 10% hydrochloric acid (105mL, 0.3mol), heat up to 75℃~80℃ with stirring, make the red base GL completely dissolve, and cool the material to 0℃~ At 5°C, the red base GL is precipitated at this time, keeping the temperature at 0°C to 5°C, adding 30% sodium nitrite solution uniformly within 45 minutes, adding activated carbon and Taikoo oil after the reaction for decolorization and filtering, and the filtrate is kept warm for later use.

[0022] (2) Preparation of coupling solution

[0023] In a 1000mL three-necked flask, add o-nitro-p-methylacetanilide (24.1g, 0.102mol), 5% NaOH (300mL, 0.15mol), stir until all dissolved, then add ultra-fine titanium dioxide (7.7g), add Taikoo oil (1 mL), stir for 1 hour, adjust pH=6-7 with 50% acetic acid, adjust the temperature to 15°C to 20°C, and wait for coupling....

Embodiment 2

[0028] Example 2 (Preparation of Ultrafine C.I. Pigment Red 4)

[0029] (1) diazotization reaction

[0030] In a 250mL three-necked flask, add o-chloro-p-nitroaniline (173.5g, 0.1mol), 10% hydrochloric acid (105mL, 0.3mol), and stir at room temperature for 1 hour to completely dissolve the o-chloro-p-nitroaniline, and then cool the material To 3 ℃~6 ℃, keep the temperature, add 30% sodium nitrite solution evenly within 90 minutes, add activated carbon and Taikoo oil after the reaction for decolorization and filtration, and keep the filtrate for use.

[0031] (2) Preparation of coupling solution

[0032] 2-naphthol (14.9g, 0.102mol), 5% NaOH (300mL, 0.15mol) were added to a 1000mL three-necked flask, the mixture was heated to 70°C under stirring to completely dissolve 2-naphthol, and then ultrafine titanium dioxide (6.7 g), add Taikoo oil (1 mL), stir for 1 hour, adjust pH=8-9 with 10% hydrochloric acid, adjust the temperature to 15-20°C, and wait for coupling.

[0033] (3) ...

Embodiment 3

[0037] Example 3 (Preparation of Ultrafine C.I. Pigment Red 8)

[0038] (1) diazotization reaction

[0039] In a 250mL three-necked flask, add red base G (150g, 0.1mol), 10% hydrochloric acid (105mL, 0.3mol), heat up to 70°C with stirring, so that the red base G is completely dissolved, and then cool the material to 5~10°C , keep the temperature, add 30% sodium nitrite solution evenly within 90 minutes, add activated carbon and Taikoo oil after the reaction for decolorization and filtration, and keep the filtrate for use.

[0040] (2) Preparation of coupling solution

[0041] In a 1000mL three-necked flask, add chromophane AS-E (30.3g, 0.102mol), 5% NaOH (300mL, 0.15mol), heat the mixture to 70°C with stirring to completely dissolve the chromophane AS-E, and then add ultrafine titanium dioxide (9g), add Taikoo oil (1mL), stir for 1 hour, adjust pH=3-4 with 10% hydrochloric acid, adjust the temperature to 15-20°C, and wait for coupling.

[0042] (3) Coupling reaction

[004...

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PUM

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Abstract

The invention relates to a method for preparing azo compounds with narrow particle size distribution. The method mainly comprises the following steps: coating the surfaces of titanium dioxide particles with narrow particle size distribution, with a coupling component to obtain titanium dioxide particles with surfaces coated with the coupling component; performing a coupling reaction between the obtained titanium dioxide particles with surfaces coated with the coupling component and a diazonium salt component to obtain target objects. According to the method provided by the invention, azo compounds with narrow particle size distribution (especially azo compounds with D90 between 0.10mum and 0.15mum) can be prepared by a relatively simple method, and the problems (including complex and lengthy steps, expensive high-precision sanding machinery and the like) of the prior art are overcome.

Description

technical field [0001] The present invention relates to a preparation method of azo compounds, in particular to a preparation method of azo compounds with narrow particle size distribution (such as particle size distribution D 90 0.10μ~0.15μ azo compound etc.) method. Background technique [0002] Most organic pigments are water-insoluble azo compounds in chemical structure, which are composed of water-soluble diazonium salt components (usually aromatic primary amine diazonium salts) and water-soluble coupling components (usually aromatic amines or Aromatic phenol and its derivatives) obtained by coupling reaction. Because the resulting azo compounds are water-insoluble, it is very important for pigment manufacturers to control their particle size and distribution. Society, 2007.7, Beijing). However, no matter how it is controlled, the particle size distribution of the azo compounds generated after the coupling reaction is still very broad. 50 between 0.5-100.0μ. [000...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C09B67/02C09B67/08C09B67/36
CPCC09B67/0095C09B67/0013C09B67/0079C09B67/0097
Inventor 沈永嘉周长凯蔡鹏飞陶雪松
Owner NANTONG HENGSHENG FINE CHEM