Aniline black pigment producing method

A production method and nigrosine technology, applied in the direction of organic dyes, etc., can solve the problems of reddish color light and low yield of pigments, and achieve the effects of pure color light, high catalytic activity and mild reaction conditions.

Active Publication Date: 2013-04-17
LIAONING FIXED STAR FINE CHEM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] The purpose of this invention is to provide a new method for preparing nigrosine pigments, to overcome the use of hydrogen peroxide as an oxidant and the use of iron (II) and iron (III) salts as catalysts to produce nigrosine pigments. Low, reddish pigment color problem

Method used

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  • Aniline black pigment producing method

Examples

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Effect test

Embodiment 1

[0026] Add 200ml of water into a 500ml three-necked bottle, add 12g of hydrochloric acid with a weight percentage of 30%, add dropwise 9.9g of aniline under stirring, after fully dissolving, add 0.28g (2.8% of the weight of aniline) copper hydroxyphosphate catalyst, and heat up to 45 ℃, drop 40 grams of 30% hydrogen peroxide solution by weight, complete the dropwise addition in 35-40 minutes, incubate at 50 ℃ for 1 hour, filter, wash the filter cake with about 500ml water until colorless, in 140 ℃ After drying for 2 hours, 9.5 grams of nigrosine was obtained. The yield was 96% based on aniline, and the shade was blue light black.

Embodiment 2

[0028] Add 200ml of water to a 500ml three-necked bottle, add 12g of 30% hydrochloric acid by weight, add 9.9g of aniline dropwise under stirring, after fully dissolving, add 0.05g (0.5% of the weight of aniline) copper hydroxyphosphate catalyst, and heat up to 50 ℃, dropwise add 35 grams of 30% hydrogen peroxide solution by weight, complete the dropwise addition within 45-50 minutes, keep warm at 55℃ for 2 hours, filter, wash the filter cake with about 500ml water until colorless, and heat it at 140℃ Drying at high temperature for 2 hours gave 9.0 g of nigrosine, with a yield of 91%, and the shade was blue light black.

Embodiment 3

[0030] Add 200ml of water into a 500ml three-necked bottle, add 12g of hydrochloric acid with a weight percentage of 30%, add dropwise 9.9g of aniline under stirring, after it is completely dissolved, add 0.1g (1% of the weight of aniline) copper hydroxyphosphate catalyst, and heat up to 35 ℃, drop 35 grams of 30% hydrogen peroxide solution by weight, add dropwise within about 15-20 minutes, keep warm at 35 ℃ for 1.5 hours, filter, wash the filter cake with 500ml water until colorless, in 140 ℃ Drying at lower temperature for 2 hours gave 9.3 grams of nigrosine, with a yield of 94%, and the shade was blue light black.

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Abstract

The invention discloses an aniline black pigment producing method. The aniline black pigment producing method comprises the following steps of: taking aniline as a raw material, and adding hydrochloric acid to synthesize an aniline hydrochloride solution; adding a hydroxyl copper phosphate catalyst, and dripping hydrogen peroxide; and after reaction, filtering, cleaning, drying and grinding to obtain aniline black pigment. In the aniline black pigment producing method, dichromate is not taken as an oxidant, thus avoiding chromium pollution; the hydroxyl copper phosphate catalyst coordinates with the hydrogen peroxide oxidant, thus improving the yield of the aniline black pigment; the produced obtained aniline black pigment is pure in color and luster and is blue phase black; and the production is simple and convenient.

Description

technical field [0001] The present invention relates to a preparation method of aniline black pigment (Aniline Black) Background technique [0002] Aniline Black (Aniline Black), the dye index number is Pigment Black 1, it is medium black, with wide spectral absorption and small dispersion. , which makes it very easy to disperse in various media. The essential difference between aniline black and carbon black is that it is not conductive, and its tinting strength is worse than that of carbon black. It is currently used in coatings, paints and printing inks, especially where black velvet-like color effects are required and where carbon black is not competent. In addition, nigrosine pigments are also used in the toner of laser printers as positive charge regulators. [0003] During 1860-1863, the technology of synthesizing nigrosine on fibers was successfully developed. The way people synthesize nigrosine pigments is similar to this now, that is, aniline is dissolved in co...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C09B67/20
Inventor 宋明志荣星唐丽李刚董明东
Owner LIAONING FIXED STAR FINE CHEM
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