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Synthesis method of solvent blue 102

A synthesis method and solvent technology, applied in the field of synthesis of solvent blue 102, can solve the problems of lowering product quality, affecting product hue, and high production cost, and achieve the effects of low production cost, good color and uniform distribution

Inactive Publication Date: 2017-06-06
JIANGSU DAOBO CHEM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] The original production process is to condense 1-methylamino-4-bromoanthraquinone with isopropylamine. Since 1-methylamino-4-bromoanthraquinone is unstable under alkaline conditions, it is prone to hydrolysis and debromination to form by-products Purple by-product, by-product 1-methylaminoanthraquinone, by-product purple by-product and 1-methylamino-anthraquinone affect the hue of the product, reduce the quality of the product, and the reaction production cost is high, the yield is low, and the process still has Room for improvement

Method used

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  • Synthesis method of solvent blue 102
  • Synthesis method of solvent blue 102
  • Synthesis method of solvent blue 102

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preparation example Construction

[0023] A kind of synthetic method of solvent blue 102, concrete steps are as follows,

[0024] Put isopropanol, polyethylene glycol, and 1,4-dihydroxyanthraquinone leuco into the container in sequence, stir evenly, add monomethylamine and isopropylamine mixed aqueous solution, heat up to 70-75°C and react for more than 5 hours, After the reaction, desolventize to 80-85°C under normal pressure, cool down to 40-45°C (steam out monomethylamine and isopropylamine), add water, sodium hydroxide, copper sulfate, open the reaction vessel, Stir at ℃ for more than 10 hours, filter, wash, dry and discharge.

[0025] Among them, the mass ratio of 1,4-dihydroxyanthraquinone leucosome to isopropanol is 1: (5-7.5), and the mass ratio of 1,4-dihydroxyanthraquinone leucosome to polyethylene glycol is 1 : (0.05-0.25), the mass ratio of 1,4-dihydroxyanthraquinone leucosome and 70wt% monomethylamine is 1: (0.357-0.5), 1,4-dihydroxyanthraquinone leucosome and isopropylamine The mass ratio of 1: ...

Embodiment 1

[0028] In a 500mL four-neck flask equipped with a mechanical stirrer and a thermometer, add 100g of isopropanol, 1g of polyethylene glycol, 20g of 1,4-dihydroxyanthraquinone leuco, and after stirring evenly, add 70wt% monomethylamine A mixed solution of 7.14 g, 7 g of isopropylamine, and 9.5 g of water was heated up to 70° C., and the reaction was carried out for 5 hours. After the reaction, the solution was precipitated to 85°C under normal pressure, cooled to 40°C, 200g of pure water, 4g of sodium hydroxide, and 0.5g of copper sulfate were added in sequence, and stirred at 45°C for 10 hours. After stirring, filter, wash, and dry to obtain 24.5 g of the target product (including: 21.41 g of 1-methylamino-4-isopropylaminoanthraquinone, 1.77 g of 1,4-bis(methylamino)anthraquinone, 1,4 - Di(isopropyl)aminoanthraquinone 1.07g), yield 1.22, shade (DC0.6, DH0.2, intensity 101.0).

Embodiment 2

[0030] In a 500mL four-necked flask equipped with a mechanical stirrer and a thermometer, add 120g of isopropanol, 2g of polyethylene glycol, and 20g of 1,4-dihydroxyanthraquinone leuco. After stirring evenly, add 70wt% monomethylamine 9. A mixed solution of 9.28 g, 10 g of isopropylamine, and 55 g of water was heated up to 73° C., and the heat preservation reaction was carried out for 6 hours. After the reaction is over, desolvate to 85°C under normal pressure, cool down to 40°C, add 250g of pure water, 5g of sodium hydroxide, and 1g of copper sulfate in sequence, and stir at 45°C for 14 hours. After stirring, filter, wash, and dry to obtain 24.35 g of the target product (including: 20.68 g of 1-methylamino-4-isopropylaminoanthraquinone, 2.21 g of 1,4-bis(methylamino)anthraquinone, 1,4 -Di(isopropyl)aminoanthraquinone 1.34), output rate 1.21, shade (DC0.8, DH0.5, intensity 102.3).

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Abstract

The invention discloses a synthesis method of solvent blue 102. The method comprises the following steps of sequentially adding isopropyl alcohol, polyethylene glycol and a 1,4-dihydroxy anthraquinone leuco body into a container, stirring evenly, and adding a mixed water solution of monomethylamine and isopropylamine; heating the container to 70-75 DEG C, carrying out condensation reaction, carrying out atmospheric desolvation to 80-85 DEG C and cooling to 40-45 DEG C; and adding pure water, sodium hydroxide and copper sulfate to the container, opening the reaction container, stirring at 40-45 DEG C, carrying out oxidizing reaction, filtering, washing, drying and discharging. 1-methylthio-4-bromoanthraquinone is replaced with the 1,4-dihydroxy anthraquinone leuco body, so that the solvent blue 102 is high in yield, available in raw material and low in price, the production cost is much lower than that of an old technology, bromine-containing wastewater is not generated and the wastewater treatment difficulty is also relieved.

Description

technical field [0001] The invention relates to a synthesis method of solvent blue 102, which belongs to the technical field of chemical dye synthesis. Background technique [0002] Solvent blue 102, the chemical name is 1-methylamino-4-isopropylaminoanthraquinone, is a dark blue powder, is a solvent dye with excellent performance, mainly suitable for packaging, decoration, paint, ink, polyester, nylon, etc. of coloring. [0003] Its molecular formula is C 18 h 18 N 2 o 2 , molecular weight 294.35. The structural formula of solvent blue 102 is: [0004] [0005] The original production process is to condense 1-methylamino-4-bromoanthraquinone with isopropylamine. Since 1-methylamino-4-bromoanthraquinone is unstable under alkaline conditions, it is prone to hydrolysis and debromination to form by-products Purple by-product, by-product 1-methylaminoanthraquinone, by-product purple by-product and 1-methylamino-anthraquinone affect the hue of the product, reduce the qu...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C09B1/28
CPCC09B1/285
Inventor 刘学峰徐松郭维成汪港陈路云朱止阳
Owner JIANGSU DAOBO CHEM
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