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Method for preparing black perylene derivatives pigment

A pigment and perylene-based technology, which is applied in the field of preparation of black perylene-based pigments, can solve the problems of high cost, high manufacturing cost, flammability and explosion, etc.

Inactive Publication Date: 2005-08-17
EAST CHINA UNIV OF SCI & TECH +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The disadvantage of this process is that the manufacturing cost is very high, not only expensive equipment is needed (to recover the solvent), but what is more fatal is that the acetone used is a low boiling point solvent, which is extremely volatile and inflammable and explosive in the air

Method used

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  • Method for preparing black perylene derivatives pigment
  • Method for preparing black perylene derivatives pigment
  • Method for preparing black perylene derivatives pigment

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0034] Preparation of N, N'-diphenylethylperylene tetraimide (C.I. Pigment Black 31)

[0035] 1) Synthesis of crude pigment:

[0036] Add 120g (0.3mol) 3,4,9,10-perylenetetraacid dianhydride in 1200g 10% KOH, heat to make it dissolve completely, cool to room temperature and add 89g (0.75mol) phenethylamine, after stirring evenly, Then add 160g of acetic acid, mix evenly, transfer the material to the autoclave, seal it, raise the temperature to 130-135°C (about 5 atmospheres), heat and stir for 5h, and take a sample for detection. If the perylene anhydride in the reactant is basically exhausted, then After the reaction was completed, it was cooled to room temperature, filtered, washed with water until neutral, and dried to obtain 180 g of a black solid, that is, N, N'-diphenylethylperylene tetraimide, and the yield was close to 100%.

[0037] 2) Pigmentation of crude pigments:

[0038] Put the dry 60g crude product pigment prepared by the above method into a ball mill, add 45...

Embodiment 2

[0040] Preparation of N, N'-diphenylethylperylene tetraimide (C.I. Pigment Black 31)

[0041] 1) Synthesis of crude pigment:

[0042] In a stainless steel reaction kettle, add 800g of glycerol, add 120g (0.3mol) of 3,4,9,10-perylenetetraic acid dianhydride and 89g (0.75mol) of phenylethylamine under stirring, and heat up to 170-175°C. Keep stirring for 1h. Sampling and detection, if the perylene anhydride in the reactant is basically exhausted, the reaction ends. Cool to 50°C, dilute with 300g of methanol, filter at 40°C, wash with methanol, then wash with water, and dry to obtain 160g of black crystals, that is, N,N'-diphenylethylperylene tetraimide, yield 90 %.

[0043] 2) Pigmentation of crude pigments:

[0044] Same example 1

Embodiment 3

[0046] Preparation of N,N'-bis(4'-methoxybenzyl)perylene tetraimide (C.I. Pigment Black 32)

[0047] 1) Synthesis of crude pigment:

[0048] In the stainless steel reactor, add 1500g glycerol, add 120g (0.3mol) 3,4,9,10-perylenetetraic acid dianhydride and 102g (0.75mol) 4-methoxybenzylamine under stirring, be warming up to 170 ~175°C, keep stirring for 1h. Sampling and detection, if the perylene anhydride in the reactant is basically exhausted, the reaction ends. Cool to 50°C, dilute with 800g of methanol, filter at 40°C, wash with methanol, then water, and dry to obtain 174g of black crystals, that is, N,N'-bis(4'-methoxybenzyl)perylenetetraacid di Imide, 97% yield.

[0049] 2) Pigmentation of crude pigments:

[0050] Put the dried 60g crude product pigment prepared by the above method into a ball mill, add 450g steel balls, a mixture of 240g sodium chloride and sodium sulfate (1:1), 2g calcium stearate and 1.2gN,N'-di Phenylethyl perylene tetraimide disulfonic acid, ba...

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Abstract

The present invention discloses black perylene pigment preparing process. During the preparation process, 3, 4, 9, 10-perylene tetracid dihydride is first reacted with aryl or substituent aryl aliphatic primary amine in the presence of potassium hydroxide and acetic acid to prepare coarse pigment product; the coarse pigment product is then ball milled in the presence of milling assistant, dispersant, and organic solvent, solid citric acid, maleic acid fumaric acid or calcium stearate; and the and the ball milled material is finally boiled in acid water medium containing surfactant and treated through filtering, water washing and drying to obtain the black perylene pigment. Thus prepared pigment has high black degree, high coloring capacity and easy dispersing.

Description

technical field [0001] The invention relates to a preparation method of a black perylene pigment. Background technique [0002] Perylene pigments are a class of high-performance pigments, and their chemical stability and application performance cannot be compared with ordinary pigments. The color spectrum of most perylene pigments is scarlet, bay red, purple and brown, so they are often called perylene red pigments. Perylene red pigment has extremely high resistance to organic solvents and heat stability, as well as high light and weather fastness. It has very high migration fastness in plastics and very good recoating resistance in paints. [0003] The perylene pigment involved in the present invention is different from others, and its chromatogram is black, and it is usually referred to as perylene black pigment, and its structure is as follows: [0004] [0005] In formula (1), n=1~3, R is H, CH 3 , OH or OCH 3 . [0006] Although the color spectrum of perylene b...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C09B3/18
Inventor 沈永嘉闫轲张忠胜张志刚白希栋张伟
Owner EAST CHINA UNIV OF SCI & TECH
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