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Anthrapyridone solvent dye and synthetic method thereof

A solvent dye and anthrapyridone technology, which is applied in the synthesis field of anthrapyridone solvent dyes, can solve the problems such as heat resistance and migration resistance to be improved, and achieves wide application range, improved heat resistance and migration resistance, The effect of high practical value

Active Publication Date: 2009-03-04
宁波龙欣精细化工有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Solvent Red 52 dye is generally not recommended for PET spinning, and its heat resistance and migration resistance still need to be improved

Method used

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  • Anthrapyridone solvent dye and synthetic method thereof
  • Anthrapyridone solvent dye and synthetic method thereof
  • Anthrapyridone solvent dye and synthetic method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0018] In a 250ml three-necked flask, add 160g of chlorosulfonic acid, start stirring, and slowly add 20g of solvent red 52, the temperature does not exceed 25°C. After the addition, the temperature was carefully raised to 35°C and kept at 35°C for 1 hour. Dilute the material into 1000 g of crushed ice, filter with suction, and wash the filter cake with ice water until slightly acidic. The chlorosulfonated filter cake is beaten with 500 grams of ice water, adjusted to pH 6.5-7.0 with 10% sodium carbonate solution, and 15 grams of cyclohexylamine is added dropwise to control the temperature below 10°C. After the dropwise addition, start to add 20 grams of 10% sodium carbonate solution dropwise, finish dropping in 1 hour, control the pH between 9.5 and 11.5, keep it below 10°C for 4 hours, then warm up to room temperature, and continue the reaction for 3 hours. Finally, raise the temperature to 60-70°C, keep it for 30 minutes, filter, and wash the filter cake with water at abou...

Embodiment 2

[0020] In a 250ml three-necked flask, add 120g of chlorosulfonic acid, start stirring, and slowly add 20g of solvent red 52, the temperature does not exceed 15°C. After the addition, the temperature was carefully raised to 35°C and kept at 35°C for 1 hour. Then 20 grams of thionyl chloride was added dropwise and stirred for 30 minutes. Dilute the material into 1000 g of crushed ice, filter with suction, and wash the filter cake with ice water until slightly acidic. Slurry the chlorosulfonated filter cake with 200 grams of ice and 300 grams of water, adjust the pH to 6.5-7.0 with 10% sodium carbonate solution, add a solution of 12.5 grams of aniline and 15 grams of methanol dropwise, keep the temperature at 10°C, and start to add 20 grams of 10% sodium carbonate solution, pH between 9.5 and 11.5, dripped in about 2 hours. Stirred at 10°C for 4 hours, then warmed to room temperature, and continued the reaction for 3 hours. Finally, raise the temperature to 60-70°C, keep it fo...

Embodiment 3

[0022] In a 250ml three-neck flask, add 150g of chlorosulfonic acid, start stirring, slowly add 20g of solvent red 52, the temperature does not exceed 25°C, after the addition, stir at room temperature for 2 hours. Dilute the material into 1000 grams of crushed ice, filter with suction, and wash the filter cake with ice water until it is nearly neutral. The filter cake is beaten with a solution of about 200 grams of ice and 200 grams of ethanol, the temperature is controlled at 3 ° C, and the pH is adjusted to 6.5 to 7 with 10% sodium carbonate solution, and a solution of 20.5 grams of p-toluidine dissolved in 35 grams of ethanol is started to be added dropwise. At the same time, 22 grams of 10% sodium carbonate solution was added dropwise, the temperature was controlled below 15° C., and the pH was between 9.5 and 11.5. After the dropwise addition, continue to stir for 5 hours, then raise the temperature in a water bath to 50°C, stir for 30 minutes, filter, wash the filter ca...

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Abstract

The invention relates to an anthr-pyridone solvent dye and a synthesizing method thereof. The synthesizing steps are as follows: a solvent red 52 is used as the material and is added into a chlorosulfonic acid for stirring reaction under the temperature of 0 to 50 DEG C for 0.5 to 2 hours, then is diluted in ice water, filtered and washed to obtain a filter mass; b, the filter mass is pulped and the pH is adjusted between 6.5 and 7; then an acid-binding agent is added simultaneously or after the organic amine is added; the pH is controlled between 9.5 and 11.5 for reacting for 5 to 8 hours under the temperature of 0 and 50 DEG C; c, the temperature of a reaction product is raised to the temperature between 50 and 70 DEG C and then the temperature is preserved for 30 minutes; then the reaction product is filtered, washed and dried, thus obtaining the dye. The heat resistance and the transference resistance of the dye are improved by different extents. The dye can be applied to thermoplastic resins like ABS, PA6 and PET; besides, the dye can also be applied to polyester and spinning.

Description

technical field [0001] The invention relates to an anthrapyridone solvent dye, and the invention also relates to a synthesis method of the anthrapyridone solvent dye. Background technique [0002] Solvent Red 52 is a blue light red solvent dye, the name on the dye index is Solvent Red 52, and the molecular formula is C 24 h 18 N 2 o 2 , molecular weight 366.4, melting point 276.68 ℃, mainly used in the coloring of PS, ABS, PMMA, PET, PA6 and other thermoplastic resins. Solvent red 52 maximum absorption wavelength λmax (DMF) 538nm, heat resistance: 0.05% dye plus 0.5% Bayer titanium ABS 240 ° C for 2 minutes; PA 280 ° C for 2 minutes, PET 330 ° C for 2 minutes; light resistance: transparent: (0.05 % dye, PS) 6 grades, opacity: (0.05% dye plus 0.5% Bayer titanium, PS) 5 grades; migration resistance: 4 grades. Solvent red 52 dye is generally not recommended for PET spinning, and its heat resistance and migration resistance still need to be improved. Contents of the inven...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C09B5/14
Inventor 刘晓梅
Owner 宁波龙欣精细化工有限公司
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