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Method for preparing pigment red 177 in ionic liquid

An ionic liquid, pigment red technology, applied in chemical instruments and methods, anthracene dyes, organic dyes, etc., can solve problems such as intractability and recycling, restricting the production of pigment red 177, environmental protection issues, etc.

Active Publication Date: 2014-05-07
宇虹颜料股份有限公司 +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Due to the dilution with water, a large amount of sulfuric acid-containing wastewater will be produced, with a concentration of about 20%, which is difficult to handle and recycle. This is the biggest shortcoming of the current desulfonation reaction.
Due to the discharge of a large amount of waste acid, serious environmental problems have been caused, and the production of Pigment Red 177 has also been limited.

Method used

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  • Method for preparing pigment red 177 in ionic liquid
  • Method for preparing pigment red 177 in ionic liquid

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0016] The weight ratio of BSMTF to DAS is 6:1;

[0017] The weight ratio of methanol solvent to DAS is 40:1;

[0018] Weigh 5 g of DAS and 30 g of BSMTF ionic liquid, and add them into a 300 mL four-neck flask. The flask was placed in an oil bath, stirred and heated to 140°C, and kept for reaction for 11 hours. Then the reaction mixture was cooled to below 50°C (methanol does not boil), and 200g of methanol solvent was added, stirred, and Pigment Red 177 was precipitated. The diluted mixture was filtered with suction, and the filter cake was dried at 80°C for 12 hours to obtain Pigment Red 177 in a yield of 97.9%. The methanol in the filtrate is recovered by distillation, and the ionic liquid obtained after the methanol is distilled is also recovered.

Embodiment 2

[0020] The weight ratio of BSMTF to DAS is 4:1;

[0021] The weight ratio of methanol solvent to DAS is 35:1;

[0022] Weigh 5 g of DAS and 20 g of BSMTF ionic liquid, and add them into a 300 mL four-neck flask. The flask was placed in an oil bath, stirred and heated to 150° C., and kept for 9 hours for reaction. Then the reaction mixture was cooled to below 50° C., diluted with 175 g of methanol solvent, stirred, and Pigment Red 177 was precipitated. After suction filtration, the filter cake was dried at 80°C for 12 hours to obtain Pigment Red 177 in a yield of 96.8%. The methanol in the filtrate is recovered by distillation, and the ionic liquid obtained after the methanol is distilled off is recovered.

Embodiment 3

[0024] The weight ratio of BSMTF to DAS is 8:1;

[0025] The weight ratio of methanol solvent to DAS is 45:1;

[0026] Weigh 5 g of DAS and 40 g of BSMTF ionic liquid, and add them into a 300 mL four-neck flask. The flask was placed in an oil bath, stirred and heated to 135° C., and kept for 6 hours for reaction. Then the reaction mixture was cooled to below 50° C., 225 g of methanol solvent was added to dilute the reaction mixture, stirred, and Pigment Red 177 was precipitated. After suction filtration, the filter cake was dried at 80°C for 12 hours to obtain Pigment Red 177 in a yield of 96.2%. The methanol in the filtrate is recovered by distillation, and the ionic liquid obtained after the methanol is distilled off is recovered.

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Abstract

The invention belongs to a method for preparing pigment red 177 in an ionic liquid. The method comprises the steps: mixing 4, 4'-diamino-1, 1'-dianthraquinone-3, 3'-disulfonic acid (DAS) in the ionic liquid, heating at high temperature, and carrying out desulfonation reaction; and after the reaction is ended, adding a methyl alcohol solvent into the reaction mixture to separate out the pigment red 177, filtering and drying to obtain the pigment red 177. The problem that a great deal of waste acid is discharged in the existing preparation technology of the pigment red 177 is solved; the process for preparing the pigment red 177 through carrying out desulfonation reaction on the DAS in about 70-80% of slfuric acid medium is not needed, no waste dilute sulphuric acid is discharged, and the yield of the pigment red 177 is over 95%. According to the invention, the pigment red 177 is prepared by using a technology for carrying out desulfonation reaction in the ionic liquid, so that the process is simple, the discharged waste acid is greatly reduced, and the yield is relatively high.

Description

technical field [0001] The invention belongs to the field of synthesis of fine chemicals, and particularly proposes a method for preparing an organic pigment C.I. Pigment Red 177 in an ionic liquid. Background technique [0002] C.I. Pigment Red 177 (hereinafter referred to as Pigment Red 177) is a high-grade red organic pigment with excellent weather resistance, heat resistance, solvent resistance and chemical resistance. It has high tinting strength, good migration resistance, and plastic molding temperature resistance. It is the main red organic pigment for synthetic resin and plastic coloring. It is also widely used in paints, inks, coatings, synthetic fibers, and liquid crystals. With the rise of market demand, its production is increasing. [0003] The current production technology of Pigment Red 177 is basically to react 4,4′-diamino-1,1′-dianthraquinone-3,3′-disulfonic acid (hereinafter referred to as DAS) in sulfuric acid medium to remove di A sulfonic acid group,...

Claims

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Application Information

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IPC IPC(8): C09B67/20C09B1/22
Inventor 张天永李威李彬吕东军费学宁陈都方
Owner 宇虹颜料股份有限公司
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