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Method for purifying industrial fluorine with drum

An industrial fluorene and drum technology, which is applied in crystallization purification/separation, organic chemistry, etc., can solve the problems of low industrial fluorene yield, high production cost, cumbersome process, etc., to reduce energy consumption, simplify production process, and reduce labor The effect of intensity

Active Publication Date: 2016-04-27
QUJING ZHONGYI FINE CHEMICAL INDUSTRY CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The above process makes the yield of industrial fluorene generally low, the production cost is high, and the process is relatively cumbersome. Therefore, it is very necessary to develop a method that can solve the above technical problems

Method used

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  • Method for purifying industrial fluorine with drum

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0032] In the processing of anthracene oil, the washing oil containing about 26% fluorene extracted from the top of the primary tower is used as a raw material, and is purified through a structured corrugated packing tower. The fluorene fraction containing 60-70% fluorene is extracted from the top of the tower, and the temperature is 170-190°C. First inject 20T of mixed solvent oil with a ratio of xylene and trimethylbenzene of 3:1 into the solid-liquid mixing agitator, and then start heating, and the temperature is controlled at 50-55°C. Then enter the flaky fluorene crystal 5T and then stir. The stirring speed is controlled at 60-80r / min, and the temperature is 55°C until the crystals are completely dissolved. Control the cooling rate according to 5°C / h, so that the fluorene starts to recrystallize, until the temperature of the slurry drops to 25°C, stop cooling and stop stirring. Begin to stand still to allow solid-liquid separation. The solid fluorene crystals are relea...

Embodiment 2

[0036] In the processing of anthracene oil, the washing oil containing about 26% fluorene extracted from the top of the primary tower is used as a raw material, and is purified through a structured corrugated packing tower. The fluorene fraction containing 50-60% fluorene is extracted from the top of the tower, and the temperature is 150-160°C. Inject the mixed solvent oil 20T with the ratio of xylene and trimethylbenzene at 2:1 into the solid-liquid mixing agitator first, then start heating, and control the temperature of the mixed solvent oil at 50-55°C. Then enter the flaky fluorene crystal 5T and then stir. The stirring speed is controlled at 60-180r / min, and the temperature is 55°C until the crystals are completely dissolved. Control the cooling rate according to 5°C / h, so that the fluorene starts to recrystallize, until the temperature of the slurry drops to 25°C, stop cooling and stop stirring. Begin to stand still to allow solid-liquid separation. The solid fluorene...

Embodiment 3

[0040] In the processing of anthracene oil, the washing oil containing about 26% fluorene extracted from the top of the primary tower is used as a raw material, and is purified through a structured corrugated packing tower. The fluorene fraction containing 60-70% fluorene is extracted from the top of the tower, and the temperature is 170-190°C. Inject the mixed solvent oil 20T with the ratio of xylene and trimethylbenzene in the ratio of 1:1 into the solid-liquid mixing agitator first, then start heating, and control the temperature of the mixed solvent oil at 50-55°C. Then enter the flaky fluorene crystal 5T and then stir. The stirring speed is controlled at 60-180r / min, and the temperature is 55°C until the crystals are completely dissolved. Control the cooling rate at 3°C / h to start recrystallization of fluorene until the temperature of the slurry drops to 25°C, stop cooling and stop stirring. Begin to stand still to allow solid-liquid separation. The solid fluorene crys...

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Abstract

The invention discloses a method for purifying industrial fluorine with a drum. Fluorine distillate with the fluorine content being 60-70% is used as a raw material, the distilled fluorine is cooled and crystallized into tabular crystals via the drum, then a solvent is added according to a certain proportion for stirring, crystallizing and washing. According to difference in solubility of various substances in the fluorine distillate in solvent oil, the other components are dissolved in the solvent to different degrees in the washing process. Fluorine is enabled to precipitate at the bottom of the solvent through stirring and standing, and the other substances are dissolved in the solvent and layered. The precipitated industrial fluorine is separated from mother liquor, and the industrial fluorine precipitated at the bottom is subjected to centrifugal separation to obtain an industrial fluorine product with the content more than or equal to 95%.

Description

technical field [0001] The invention belongs to the technical field of chemical industry, and in particular relates to a method for purifying industrial fluorene with a rotary drum. Background technique [0002] In recent years, the deep processing technology of coal tar resources in my country has been rapidly developed and applied. Among them, refined anthracene, carbazole, and fluorene with high added value in tar are important chemical raw materials. How to effectively purify these substances has always been the pursuit of the tar deep processing industry. one of the goals. However, due to the insufficient concentration of coal chemical industry, the production scale is not concentrated, and the system capacity of coal tar deep processing equipment is small, many independent coal tar deep processing enterprises have branched out. Such enterprises are steadily advancing towards modern chemical industry at a faster pace, and are gradually expanding towards fine chemical in...

Claims

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Application Information

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IPC IPC(8): C07C7/14C07C13/567
CPCC07C7/14C07C13/567
Inventor 魏福树罗国林
Owner QUJING ZHONGYI FINE CHEMICAL INDUSTRY CO LTD