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Preparation method of perylene pigment

A pigment and perylene-based technology, applied in the field of preparation of perylene-based pigments, can solve the problems of high cost, must be recycled, environmental hazards, etc., and achieve the effect of simple method, strong hiding power, and uniform crystal grains

Active Publication Date: 2016-06-22
成都佳驰电子科技股份有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, these methods basically require four to five steps of reaction, and the cost is high.
At the same time, a large amount of organic solvent needs to be added as an auxiliary agent in the ball milling process. Due to the large amount of organic solvent used, it must be recycled, resulting in a large amount of waste water, which is harmful to the environment.

Method used

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  • Preparation method of perylene pigment
  • Preparation method of perylene pigment
  • Preparation method of perylene pigment

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0025] Step 1: Add 4ML benzylamine to 50ML glycerol solution, seal it, and sonicate for 30 minutes to obtain a mixed solution.

[0026] Step 2: Transfer the mixed solution obtained in Step 1 to a stainless steel reaction kettle at 50°C, add 5g of perylene-3,4,9,10-tetracarboximide, and heat for 30 minutes under stirring at 1000 rpm, the perylene -3,4,9,10-Tetracarboximide is fully dissolved and the solution is red.

[0027] Step 3: After raising the reaction temperature obtained in Step 2 to 140° C., seal and reflux successively, and keep the reaction for 4 hours under stirring at 2000 rpm.

[0028] Step 4: After step 3 is completed, adjust the reaction temperature to 50°C, cool naturally, add 25ML pure methanol to dilute, wash with water, filter, and dry at 60°C.

[0029] Step 5: Add the dry solid obtained in step 4 to 100ML mass fraction 10%Na 2 CO 3 , after ultrasonic dissolution, transferred to a 50°C reactor for reflux reaction for 1h, then cooled naturally, washed wit...

Embodiment 2

[0031] Step 1: Add 4ML phenethylamine to 50ML glycerol solution, seal it, and ultrasonicate for 30 minutes to obtain a mixed solution.

[0032] Step 2: Transfer the mixed solution obtained in Step 1 to a stainless steel reaction kettle at 40°C, add 5 g of perylene-3,4,9,10-tetracarboximide, and heat for 30 minutes under stirring at 1500 rpm. Ethylamine and perylene-3,4,9,10-tetracarboximide were fully dissolved, and the solution was red.

[0033] Step 3: After raising the reaction temperature obtained in Step 2 to 140° C., seal and reflux successively, and keep the reaction for 4 hours under stirring at 2000 rpm.

[0034] Step 4: After step 3 is completed, adjust the temperature to 50°C, add 25ML of pure methanol to dilute, wash with water, filter, and dry at 60°C.

[0035] Step 5: Add the dry solid obtained in step 4 to 100ML mass fraction 10%Na 2 CO 3 , after ultrasonic dissolution, transferred to a 50°C reactor for reflux reaction for 1h, then cooled naturally, washed wi...

Embodiment 3

[0037] Step 1: Add 5.2 g of 4-methoxybenzylamine to 50 mL of glycerol solution, seal it, and ultrasonicate for 30 minutes to obtain a mixed solution.

[0038] Step 2: Transfer the mixed solution obtained in Step 1 to a stainless steel reaction kettle at 50°C, add 5g of perylene-3,4,9,10-tetracarboximide, and heat for 30 minutes under stirring at 1000 rpm, the perylene -3,4,9,10-tetracarboximide and 4-methoxybenzylamine are fully dissolved, and the solution is red.

[0039] Step 3: After raising the reaction temperature obtained in Step 2 to 140° C., seal and reflux successively, and keep the reaction for 4 hours under stirring at 2500 rpm.

[0040] Step 4: After step 3 is completed, adjust the temperature to 50°C, add 25ML of pure methanol to dilute, wash with water, filter, and dry at 60°C.

[0041] Step 5: Add the dry solid obtained in step 4 to 100ML mass fraction 10%Na 2 CO 3 , after ultrasonic dissolution, transferred to a 50°C reactor for reflux reaction for 1 hour, t...

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Abstract

The invention relates to a preparation method of a perylene pigment. According to the method, the reaction temperature between the organic solvent and solute is firstly preheated at 40-60 DEG C, and the samples are thoroughly mixed and react completely, thereby lowering the temperature increase speed, reducing the aggregation, being beneficial to crystallization, facilitating cleaning and saving the cleaning cost. When the temperature is higher than 70 DEG C, the reaction quickly happens, thereby not being beneficial to the sufficient reaction of the reactants, causing many unreacted substances, not being beneficial to forming crystals with uniform size, and aggravating aggregation; and the prepared product has coarse and large particles, and the aggregation phenomenon is not beneficial to impurity cleaning. The preparation method provided by the invention omits the ball milling after-treatment, and thus, is environment-friendly and economical. The prepared perylene pigment has the advantages of uniform crystal grains, favorable dispersity and high covering power, and thus, can be directly used in paints conveniently.

Description

technical field [0001] The invention relates to a preparation method of perylene pigments, which belongs to the preparation technology of perylene pigments. Background technique [0002] As a component of pigments, organic pigments have the characteristics of bright colors, high tinting strength and low toxicity. As a part of organic pigments, perylene pigments, in addition to the characteristics of organic pigments, are widely used in coatings due to their wide color range, high thermal stability and resistance to organic solvents, weather resistance stability and chemical inertness , especially in plastic coloring and automotive finishes. [0003] Perylene pigments are basically N- and N’-substituted products of perylene-3,4,9,10-tetracarboximide, and its structure is as follows: [0004] [0005] Wherein R- includes aliphatic or aromatic groups. The perylene derivative wherein R = phenethyl is registered as C.I. Pigment Black 31 in the "Dye Index". The perylene der...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C09B67/20
CPCC09B67/0065C09B67/0069
Inventor 谢建良刘文乐刘云峰菅帅王慧邓龙江
Owner 成都佳驰电子科技股份有限公司
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