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A kind of preparation method of dye

A dye and dihydro technology, applied in the preparation of organic compounds, anthracene dyes, organic dyes, etc.

Active Publication Date: 2017-02-08
JIANGSU DAOBO CHEM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

We have not found any information about 3,3'-[(9,10-dihydro-9,10-dioxo-1,4-anthracendiyl)diimino]bis[N-cyclohexyl- A report on the synthetic route of 2,4,6-trimethyl]benzenesulfonamide

Method used

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  • A kind of preparation method of dye
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Examples

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Effect test

Embodiment 1

[0022] Step 13, 3'-[(9,10-dihydro-9,10-dioxo-1,4-anthracendiyl)diimino]bis(2,4,6-trimethylbenzene)sulfonyl chloride Synthesis

[0023] In a 150ml four-necked bottle with mechanical stirring and a thermometer, add 7g of solvent blue 104 and 49g of chlorosulfonic acid, stir and heat to 30°C, and keep warm for 15 minutes. After completion, the temperature was lowered to 15° C., and the reaction was kept for 7 hours. After the reaction, the reaction solution was slowly added to the ice-water mixture, the temperature was controlled at -5°C, and the addition was completed, stirred at -5°C for 30 minutes, filtered, and the filter cake was washed with cold water to obtain 22 g of the wet product of the sulfonyl chloride compound. Content 50.5%, purity 80.2%;

Embodiment 2

[0025] Step 13, 3'-[(9,10-dihydro-9,10-dioxo-1,4-anthracendiyl)diimino]bis(2,4,6-trimethylbenzene)sulfonyl chloride Synthesis

[0026] Add 7g of solvent blue 104 and 84g of chlorosulfonic acid into a 150ml four-necked bottle with mechanical stirring and a thermometer, stir and heat to 40°C, keep warm for 15 minutes, start adding 6g of thionyl chloride dropwise after the warming is over, and the dropwise addition is complete Afterwards, the temperature was lowered to 23° C., and the reaction was maintained for 6 hours. After the reaction, the reaction solution was slowly added to the ice-water mixture, and the temperature was controlled at about 0°C. After the addition was completed, it was stirred at 0°C for 30 minutes, filtered, and the filter cake was washed with cold water to obtain 23.5 g of the wet product of the sulfonyl chloride compound. Content 51.5%, purity 83.1%;

Embodiment 3

[0028] Step 13, 3'-[(9,10-dihydro-9,10-dioxo-1,4-anthracendiyl)diimino]bis(2,4,6-trimethylbenzene)sulfonyl chloride Synthesis

[0029] Add 7g of solvent blue 104 and 84g of chlorosulfonic acid to a 150ml four-necked bottle with mechanical stirring and a thermometer, stir and heat to 35°C, keep warm for 15 minutes, start adding 4g of thionyl chloride dropwise after the warming is over, and the dropwise addition is complete Afterwards, the temperature was lowered to 15° C., and the reaction was maintained for 8 hours. After the reaction, the reaction solution was slowly added to the ice-water mixture, the temperature was not higher than 15°C, after the addition was completed, it was stirred at 15°C for 30 minutes, filtered, and the filter cake was washed with cold water to obtain 21.5g of the wet product of the sulfonyl chloride compound. Content 52.1%, purity 80.1%;

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Abstract

The invention discloses a preparation method of a dye. The dye is 3,3'-[(9,10-dihydro-9,10-dioxo-1,4-anthryl-di-yl)diimino]bis[N-cyclohexyl-2,4,6-trimethyl]benzenesulfonamide. The target product is prepared through a reaction of solvent blue 104 and chlorosulfonic acid as initial raw materials. Thionyl chloride adopted in the invention has little influence on the reaction and has large influence on the quality of the product; and the reaction temperature and the water washing temperature are controlled in the reaction in order to realize no stickiness or caking of the target product.

Description

technical field [0001] The present invention relates to a preparation method of a dye, especially a 3,3'-[(9,10-dihydro-9,10-dioxo-1,4-anthracenediyl)diimino]bis[ The preparation method of N-cyclohexyl-2,4,6-trimethyl]benzenesulfonamide belongs to the technical leader of chemical dyes and chemicals. Background technique [0002] 3,3'-[(9,10-Dihydro-9,10-dioxo-1,4-anthracendiyl)diimino]bis[N-cyclohexyl-2,4,6-trimethyl ] Benzenesulfonamide is a relatively new variety of solvent dyes. This pigment has good application fastness, excellent heat resistance, and meets the requirements of environmental protection quality. Its application performance in PET bottles, environmental protection wood paints, toy paints, etc. Relatively excellent. Its molecular formula is C44H52N4O6S2, its relative molecular weight is 797.04, and its structural formula is: [0003] [0004] 3,3'-[(9,10-Dihydro-9,10-dioxo-1,4-anthracendiyl)diimino]bis[N-cyclohexyl-2,4,6-trimethyl ] Benzenesulfonamide...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C225/34C07C221/00C09B1/32
CPCC09B1/346
Inventor 徐松刘学峰郭维成
Owner JIANGSU DAOBO CHEM
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