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Preparation process of solvent dye

A preparation process and a technology of solvent dyes, which are applied in the preparation process of 2-indan-1,3-dione and the field of solvent dyes, and can solve the problem of difficult control of the amount of bromine used, high energy consumption and high consumption of recycled solvents. It can improve the uniformity of dyeing, reduce the difficulty of processing and use economically.

Inactive Publication Date: 2018-06-01
JIANGSU DAOBO CHEM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

This method will produce bromine vapor in the process of adding bromine, because the volatilization of bromine makes it difficult to control the amount of bromine used, and some unreacted bromine remains in the solution. The subsequent steps require a bromine extraction device, which not only increases the cost, but also Harmful to the environment
Although bromine has high reactivity, it has poor selectivity and easily produces dibromine by-products
In this method, organic solvents with high boiling points are used, and the subsequent recovery of solvents consumes a lot of energy, and NNO is used as a dispersant, and the dosage is too large, which brings pressure on environmental protection.

Method used

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  • Preparation process of solvent dye
  • Preparation process of solvent dye
  • Preparation process of solvent dye

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0017] In a 500mL four-neck flask equipped with an electric stirrer, add 3.18g Pingpingo, 79.5g 2-(3-hydroxy-2-quinolyl)-1H-indene-1,3(2H)-dione and 126mL of dichloromethane, stirred and raised to 40°C, 159g of 1,3-dibromo-5,5-dimethylhydantoin was added in 3 batches, and the temperature was raised to reflux for 5h. After the reaction, filter, wash, and dry to obtain 96.57 g of the target product. The yield is 95.4%, the purity is 98.0%, and the tinting strength is 100.15%.

Embodiment 2

[0019] In a 500mL four-neck flask equipped with an electric stirrer, add 79.5g 2-(3-hydroxy-2-quinolyl)-1H-indene-1,3(2H)-dione, 4g Pingjiao and 150mL Dichloromethane, stirred and raised to 40°C, 170.93g of 1,3-dibromo-5,5-dimethylhydantoin was added in 4 batches, and the temperature was raised to reflux for 6 hours. After the reaction was finished, filter, wash, and dry to obtain 97.48 g of the target product. The yield is 96.3%, the purity is 98.24%, and the tinting strength is 100.73%.

Embodiment 3

[0021] In a 500mL four-neck flask equipped with an electric stirrer, add 7.95g Pingpingo O, 180mL dichloromethane, 79.5g 2-(3-hydroxy-2-quinolinyl)-1H-indene-1,3(2H )-diketone, stirred, heated to reflux, added 178.88g of 1,3-dibromo-5,5-dimethylhydantoin in 5 batches, stirred and heated to 40°C, then heated to reflux for 8 hours. After the reaction, filter, wash, and dry to obtain 98.7 g of the target product. The yield is 97.5%, the purity is 98.70%, and the tinting strength is 100.89%.

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Abstract

The invention discloses a preparation process of solvent dye. The preparation process of the solvent dye comprises the following steps: sequentially putting 2-(3-hydroxy-2-quinolyl)-1H-indene-1,3(2H)-dione, dichloromethane, peregal O and dibromohydantoin into a reaction device, and performing heating and stirring until refluxing to perform substitution reaction; and after the reaction, performingfiltering, washing the materials with water and performing drying to obtain 2-(4-bromo-3-hydroxy-2-quinolyl)indan-1,3-dione dye. Bromine is replaced by the dibromohydantoin, so that the operation stepis simplified; the dibromohydantoin serves as a brominating agent, so that the inconvenience caused by adding bromine is avoided, pollution to the environment is avoided and the yield of products isincreased, and the solvent dye is high in bromine content, high in storage stability, economical to use and suitable for industrialization; meanwhile, the low-boiling-point dichloromethane serves as asolvent and the surfactant peregal O serves as an auxiliary material, so energy consumption is reduced, the waste water treatment difficulty is reduced, and the dyeing uniformity of the products is improved.

Description

technical field [0001] The invention relates to a preparation process of a solvent dye, in particular to a preparation process of 2-(4-bromo-3-hydroxy-2-quinolyl)indan-1,3-dione, which belongs to the field of dye preparation . Background technique [0002] 2-(4-Bromo-3-hydroxy-2-quinolyl)indan-1,3-dione, mainly used for polyester dyeing, can get bright pure yellow, good light fastness, good hiding Well, it is the main dye for dyeing medium and light colors. It is also used in the dyeing of nylon, acetate fiber, polyester wool blended products and the direct printing of polyester silk. As one of the three primary colors, it can form three primary colors with Disperse Red 3B (or Disperse Red FB) and Disperse Blue 2BLN (or Disperse Blue FBL). It has good level dyeing property, good compatibility and stable shade. Its molecular formula is C 18 h 10 BrNO 3 , the relative molecular mass is 368.18, and the structural formula is: [0003] [0004] 2-(4-bromo-3-hydroxy-2-qu...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C09B57/00
CPCC09B57/00
Inventor 徐松刘学峰陈路云朱止阳
Owner JIANGSU DAOBO CHEM
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