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Synthesis method of solvent green 3

A synthesis method and solvent technology, applied in the synthesis field of solvent green 3, can solve the problems of low yield and high reaction temperature, and achieve the effects of improved initiation and catalysis, mild reaction conditions, and improved filterability

Active Publication Date: 2017-05-17
JIANGSU DAOBO CHEM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The reaction temperature is high, resinification by-products are generated, the product has a certain solubility in the solvent, and the yield is not high

Method used

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  • Synthesis method of solvent green 3
  • Synthesis method of solvent green 3

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0026] In a 500mL four-necked flask with mechanical stirring and a thermometer, add 120g of ethanol, 60g of benzene, 2g of boric acid, 40g of 1,4-dihydroxyanthraquinone, 2g of sodium bisulfite, and 1,4-dihydroxyanthraquinone leuco After stirring evenly, 24 g of p-toluidine was added, and the temperature was raised to 64±2°C for dehydration reaction, and the reaction time was 12 hours. After the reaction, cool down to 20°C, filter, wash, and dry to obtain the target product 82.32g Solvent Green 3, with a purity of 98.5% and a yield of 97% (with 1,4-dihydroxyanthraquinone and 1,4-dihydroxyanthraquinone Anthraquinone leucosome total), shade (DC0.0, DH0.2, intensity 100.0), filter value 0.02.

Embodiment 2

[0028] In a 500mL four-neck flask equipped with mechanical stirring and a thermometer, add 160g of ethanol, 80g of benzene, 4g of boric acid, 40g of 1,4-dihydroxyanthraquinone, 4g of sodium bisulfite, and 1,4-dihydroxyanthraquinone leuco After stirring evenly, 23 g of p-toluidine was added, and the temperature was raised to 64±2°C for dehydration reaction, and the reaction time was 14 hours. After the reaction, cool down to 20°C, filter, wash, and dry to obtain 83.48g of the target product, Solvent Green 3, with a purity of 98.9% (based on the total of 1,4-dihydroxyanthraquinone and 1,4-dihydroxyanthraquinone leucosome ), the yield is 96.8%, shade (DC0.3, DH0.2, intensity 100.0), filter value 0.03.

Embodiment 3

[0030] In a 500mL four-necked flask with mechanical stirring and a thermometer, add 200g of ethanol, 100g of benzene, 6g of boric acid, 40g of 1,4-dihydroxyanthraquinone, 6g of sodium bisulfite, and 1,4-dihydroxyanthraquinone leuco After stirring evenly, 22 g of p-toluidine was added, and the temperature was raised to 64±2°C for dehydration reaction, and the reaction time was 16 hours. After the reaction, cool down to 20°C, filter, wash, and dry to obtain the target product 84.20g Solvent Green 3 with a purity of 99.5% (based on the total of 1,4-dihydroxyanthraquinone and 1,4-dihydroxyanthraquinone leucosome ), the yield is 96.3%, shade (DC0.6, DH0.4, intensity 100.0), filter value 0.01.

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Abstract

The invention discloses a synthesis method of a solvent green 3. According to the synthesis method, a target product is obtained by taking 1,4-dihydroxy anthraquinone and p-toluidine as raw materials, ethanol as a solvent, boric acid as a catalyst, a 1,4-dihydroxy anthraquinone leuco body as an initiator, sodium hydrogensulfite as an antioxidant and benzene as an azeotrope agent of a system through condensation reaction. According to the synthesis method, the ethanol with a low boiling point is used as the solvent and the solvent green 3 is hardly dissolved in the ethanol, so that the yield of a product is improved and the recycling energy consumption of the solvent is also reduced; the 1,4-dihydroxy anthraquinone leuco body is used as the initiator, has the effect of a reaction initiator and also has a catalytic action in a reaction process; the activity of the 1,4-dihydroxy anthraquinone leuco body can be guaranteed in the presence of the antioxidant, namely the sodium hydrogensulfite, and the initiation and catalysis effects are improved.

Description

technical field [0001] The invention relates to a synthesis method of solvent green 3, which belongs to the technical field of chemical dye synthesis. Background technique [0002] Solvent Green 3, also known as Transparent Green 5B, has a chemical name of 1,4-bis(4-methylphenyl)aminoanthraquinone, and is a blue-black powder. It is blue in concentrated sulfuric acid and produces a blue-green precipitate after dilution with water. Insoluble in water, soluble in chloroform, benzene, chlorobenzene, xylene, DMF and other organic solvents. Solvent Green 3 is mainly used in the coloring of plastic resin and polyester fiber pulp, and can also be used in the coloring of daily-use plastics, plexiglass, PVC packaging materials, industrial oils, inks, colored masterbatches, petroleum products, coatings, etc. [0003] Its molecular formula is C 28 h 22 N 2 o 2 , the molecular weight is 418.49, and the structural formula is: [0004] [0005] The main synthetic route of solvent...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C09B1/32
CPCC09B1/325
Inventor 刘学峰徐松郭维成汪港张龙龙陈路云朱止阳
Owner JIANGSU DAOBO CHEM
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