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Preparation method of pigment red 254

A technology of pigment red and p-chlorobenzonitrile, which is applied in the direction of chemical instruments and methods, organic dyes, azo dyes, etc., can solve the problems of less production equipment, less use of raw materials, and high production costs, and achieve less production equipment and environmental protection. The effect of less pollution and stable product quality

Inactive Publication Date: 2013-03-13
SHUANGLE CHEM PIGMENT YANGZHOU CITY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] The synthesis of this kind of pigment is a condensation ring-closing reaction. The intermediates generated in each stage of the reaction do not need to be separated, and can be completed in the same reactor at one time. It has less production equipment, simple process, and less raw material usage. Compared with other high-grade organic pigments, it is beneficial. For environmental protection and effective utilization of resources, there are relatively many manufacturers in recent years, and the product competition is fierce, and the yield of crude products in most production processes is relatively low, about 80%, which brings high production costs and makes products in the market. lack of competitiveness in the market

Method used

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  • Preparation method of pigment red 254
  • Preparation method of pigment red 254
  • Preparation method of pigment red 254

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Experimental program
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Effect test

Embodiment 1

[0032] This embodiment includes the following steps:

[0033] (1) Under the protection of nitrogen flow, add 21g of sodium metal, 180g of tert-amyl alcohol and 1g of ferric trichloride to the reaction kettle, heat to 100°C, stir and reflux for 7 hours to prepare sodium tert-amyloxide solution;

[0034] (2) Add 88g of p-chlorobenzonitrile to the sodium tert-amyl alcohol solution at 90°C and stir to dissolve it. At 90°C, add 74g of diisopropyl succinate and 50g of tert-amyl alcohol dropwise to the mixture. The mixed solution was condensed, and the dropping time was 3 hours. After the dropping, it was kept at 100°C for 3 hours. Adding 50g of tert-amyl alcohol was to dilute the concentration of diisopropyl succinate, increase the total amount, and facilitate long-term dropping;

[0035] (3) Add the condensed material to 1200ml of deionized water containing 3g of surfactant EL-40 (castor oil polyoxyethylene ether) for hydrolysis, and hydrolyze at 60°C for 6 hours;

[0036] (4) Eva...

Embodiment 2

[0039] (1) Under the protection of nitrogen flow, add 21g of sodium metal, 210g of tert-amyl alcohol and 0.5g of ferric trichloride to the reaction kettle, heat to 80°C, stir and reflux for 7 hours to prepare sodium tert-amyl alcohol solution;

[0040] (2) Add 80g of p-chlorobenzonitrile to the sodium tert-amyl alcohol solution at 70°C, and stir to dissolve it. At 70°C, add 88g of diisopropyl succinate and 50g of tert-amyl alcohol dropwise to the mixture. The mixed solution was condensed, the time of dropping was 2h, and after the dropping was completed, it was kept at 80°C for 2h;

[0041] (3) Add the condensed material to 1000ml of deionized water containing 3g of surfactant EL-40 (castor oil polyoxyethylene ether) for hydrolysis, and keep it at 40°C for 3 hours;

[0042] (4) Evaporate under reduced pressure to remove tert-amyl alcohol and the by-products generated by the reaction, filter, wash with water, and dry to obtain 100.44 g of crude Pigment Red 254, with a yield of ...

Embodiment 3

[0045] (1) Under the protection of nitrogen flow, add 21g of sodium metal, 290g of tert-amyl alcohol and 1g of ferric chloride into the reaction kettle, heat to 120°C, stir and reflux for 7h to prepare sodium tert-amyloxide solution;

[0046] (2) Add 80g of p-chlorobenzonitrile to the sodium tert-amyl alcohol solution at 100°C, stir to dissolve it, and then add 88g of diisopropyl succinate and 50g of tert-amyl alcohol dropwise to the mixture at 100°C The mixed solution of the mixture was condensed, and the dropwise addition time was 5h, and after the dropwise addition was completed, it was kept at 120°C for 5h;

[0047] (3) Add the condensed material to deionized water containing 3g of surfactant EL-40 (castor oil polyoxyethylene ether) for hydrolysis, and keep it at 80°C for 7 hours;

[0048] (4) Evaporate under reduced pressure to remove amyl alcohol and isopropanol produced by the reaction, filter, wash with water, and dry to obtain 98.2 g of crude Pigment Red 254, with a y...

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Abstract

The invention discloses a p reparation method of pigment red 254. The preparation method comprises the following steps: under protection of nitrogen flow, adding metallic sodium, tert-amyl alcohol and ferric trichloride into a reaction kettle, heating, stirring and refluxing to prepare a sodium tert-amyl alcohol solution; then adding 4-chlorobenzonitrile into the sodium tert-amyl alcohol solution, stirring to dissolve the 4-chlorobenzonitrile, dropwise adding diisopropyl succinate into the mixture for condensation, and then carrying heat insulation; hydrolyzing the condensed material with surfactant-containing deionized water; decompressing and evaporating to remove tert-amyl alcohol and isopropanol generated in reaction, filtering, rinsing and drying to obtain the crude product of pigment red 254. According to the preparation method, less production equipment is used, the process is simple, almost no environment pollution is caused, the quality of products is stable, the yield of products can be improved through effectively controlling the concentration of the sodium tert-amyl alcohol in a reaction system and on the premise of ensuring the quality of products, thereby providing guarantee for improving the product competence.

Description

technical field [0001] The present invention relates to a method for preparing high-yield high-grade organic pigment pyrrolopyrrole pigment red 254, in particular to a method for preparing pigment red 254. Background technique [0002] Pigment Red 254 is one of the DPP series pigments. DPP series pigments are referred to as diketopyrrolopyrrole for short. It is made of 1.4-diketopyrrolopyrrole as the pigment matrix. Its structural formula is as follows: [0003] [0004] DPP series pigments, especially Pigment Red 254, have various excellent properties and are representative of high-grade organic pigments. It has the characteristics of high tinting strength and bright color, and has good fluidity in the application medium and is fast to light. It can be compared with high-performance pigments such as perylene red pigments and quinacridone pigments. Because of its superior performance, it is widely used in the coloring of inks, coatings, and plastics. It is an important fa...

Claims

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Application Information

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IPC IPC(8): C09B57/00
Inventor 毛顺明朱骥陈军欣文卫
Owner SHUANGLE CHEM PIGMENT YANGZHOU CITY
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