Method for preparing solvent blue 35

A solvent, dihydroxyanthraquinone technology, applied in the field of preparation of solvent blue 35, can solve the problems of low reaction yield, difficult to guarantee product quality, high by-products and tar, and achieves improving the reaction speed, reducing the generation of tar, Yield-enhancing effect

Active Publication Date: 2015-06-24
JIANGSU DAOBO CHEM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0005] The original production process is to use 1,4-dihydroxyanthraquinone as the raw material. In alkaline water, hydrosulfite is used as the reducing agent to react with n-butylamine. After the reaction, it is filtered, and the unreacted n-butylamine is washed away with hot water. Washing and drying to get the finished product, the reaction yield is low, the by-products and tar generated are relatively high, and the quality of the product is difficult to be guaranteed

Method used

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  • Method for preparing solvent blue 35
  • Method for preparing solvent blue 35

Examples

Experimental program
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Embodiment 1

[0020] In a 500ml four-necked bottle with mechanical stirring and a thermometer, add 150g of ethanol, 15g of anhydrous sodium sulfate, 20g of 1,4-dihydroxyanthraquinone, 4.5g of 1,4-dihydroxyanthraquinone leucosome, 5g of acetic acid, 30 g of butylamine was dropped into the reactor, the reactor was sealed, and the temperature was raised to reflux for reaction for 4 hours. After the reaction, part of 100g of ethanol and n-butylamine mixed solvent was evaporated, separated by adding 15wt% sodium hydroxide aqueous solution, filtered, washed, and dried to obtain 35.5g of solvent blue 35, with a content of 97.8% and a yield of 95.3%.

Embodiment 2

[0022] In a 500ml four-necked bottle with mechanical stirring and a thermometer, add 200g of ethanol, 20g of anhydrous sodium sulfate, 20g of 1,4-dihydroxyanthraquinone, 6g of 1,4-dihydroxyanthraquinone leuco, 8g of acetic acid, n-butyl 40 g of amine was put into the reactor, the reactor was sealed, and the temperature was raised to reflux for 2 hours. After the reaction, part of 160g of ethanol and n-butylamine mixed solvent was evaporated, separated by adding 15wt% sodium hydroxide aqueous solution, filtered, washed and dried to obtain 35.5g of solvent blue 35 with a content of 97.6% and a yield of 95.1%.

Embodiment 3

[0024] In a 500ml four-necked bottle with mechanical stirring and a thermometer, add 150g of ethanol, 20g of anhydrous sodium sulfate, 20g of 1,4-dihydroxyanthraquinone, 5g of 1,4-dihydroxyanthraquinone leuco, 5.8g of acetic acid, 50 g of butylamine was dropped into the reactor, the reactor was sealed, and the temperature was raised to reflux for 1 hour. After the reaction, part of 120g of ethanol and n-butylamine mixed solvent was evaporated, separated by adding 15wt% sodium hydroxide aqueous solution, filtered, washed, and dried to obtain 35.1g of solvent blue 35, with a content of 98.6% and a yield of 95.0%.

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Abstract

The invention discloses a method for preparing solvent blue 35. The method comprises the following steps: adding ethanol, anhydrous sodium sulfate, 1,4-dihydroxyanthraquinone, 1,4-dihydroxyanthraquinone leuco, acetic acid and n-butylamine into a reactor, closing the reactor, heating to a refluxing temperature, reacting under a pressure of 0.08Mpa or less for 1-4h, distilling off an ethanol and n-butylamine mixed solvent, adding alkaline water to realize separation, filtering, washing, drying, and discharging. In the invention, acetic acid is used as a catalyst, anhydrous sodium sulfate is used as a water absorbing agent, and 1,4-dihydroxyanthraquinone is mixed with the 1,4-dihydroxyanthraquinone leuco in reasonable proportion, so the reaction speed is improved, and the yield is improved; and ethanol is adopted as a solvent to reduce the generation of tar, and a recovered ethanol and n-butylamine mixed solution can be directly used after dehydration in order to reduce the generation of wastewater.

Description

technical field [0001] The invention relates to a preparation method of solvent blue 35, which belongs to the technical field of manufacturing chemical dyes and chemicals. Background technique [0002] Solvent blue 35, also known as solvent blue 2N, chemically named 1,4-di(1-butylamino)anthraquinone, is a solvent dye with excellent performance, mainly suitable for ABS, PC, HIPS, PMMS and other resins of coloring. [0003] Its molecular formula is C 22 h 26 N 2 o 2 , molecular weight 350.454. The structural formula of solvent blue 35 is: [0004] [0005] The original production process is to use 1,4-dihydroxyanthraquinone as the raw material. In alkaline water, hydrosulfite is used as the reducing agent to react with n-butylamine. After the reaction, it is filtered, and the unreacted n-butylamine is washed away with hot water. Washing and drying to obtain the finished product, the reaction yield is low, the by-products and tar generated are relatively high, and the...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C225/34C07C221/00C09B1/28
Inventor 徐松刘学峰郭维成
Owner JIANGSU DAOBO CHEM
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