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Method for preparing refined fluorene

A technology of refined fluorene and filtrate, applied in the field of coal chemical industry, to achieve the effect of reducing the amount of recovery, low price and abundant resources

Active Publication Date: 2010-03-10
鞍钢化学科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0007] The above-mentioned methods have their own advantages and disadvantages, so the research on the preparation method of arginine is more urgent and necessary.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0021] The first crystallization: Put the raw material industrial fluorene and dichlorobenzene filtrate in a ratio of 1:3 into a three-necked flask. Then immerse the three-neck flask in a water bath; install a magnetic stirrer, and heat up while stirring. After the temperature reached 50°C and all the raw materials and solvents were dissolved, the temperature was maintained for 90 minutes. Then, the temperature program was started to cool down the mixed solution at a cooling rate of 4°C / min, and the mixed solution slowly crystallized. After continuing to cool down to 40°C, the three-neck flask was taken out of the water bath. Finally, pour the mixed solution in the three-neck flask into the pre-installed vacuum filtration device for vacuum filtration; the filter cake is a primary crystallization product after drying. The filtrate is recovered by distillation and reused.

[0022] The second crystallization: put the primary crystallization product and the tertiary chlorobenze...

Embodiment 2

[0026] The first crystallization: put the filtrate of raw material industrial fluorene and secondary chlorobenzene into a three-necked flask at a ratio of 1:0.5; immerse the three-necked flask in a water bath, and heat up while stirring; the temperature rises to 90°C, and the raw materials and solvent After all the dissolution, keep the constant temperature for 50 minutes; then the mixed solution starts to cool down at a rate of 0.5°C / min, and crystallization slowly appears; after the temperature drops to 15°C, take the three-necked flask out of the water bath: pour the mixed solution in the three-necked flask Put it into the pre-installed vacuum filtration device for vacuum filtration; after the filter cake is dried, it will be a primary crystallization product. The filtrate is recovered by distillation and reused.

[0027] The second crystallization: put the primary crystallization product and chlorobenzene into a three-necked flask at a ratio of 1:0.5; immerse the three-nec...

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Abstract

The invention provides a method for preparing refined fluorine. The method comprises the following steps of: dissolving industrial fluorene serving as a raw material in secondary chlorobenzene filtrate, third-time chlorobenzene filtrate, fourth-time chlorobenzene filtrate and chlorobenzene, which serve as solvents, at a dissolving time of between 40 and 90 DEG C for 40 and 90 minutes; performing programmed temperature-reduction crystallization of the mixed solution at a speed of 0.5 to 4 DEG C / min, wherein the final temperature of the crystallization is between 15 and 40 DEG C; and obtaining a refined fluorene product, of which the content is over 99 percent, by vacuum filtration and four-time crystallizations. The purity of the refined fluorene product prepared by the method is over 99 percent, the extraction efficiency of the refined fluorene is over 75 percent; the chlorobenzene filtrate can be recycled without distillation, so that a great deal of fluorene fractions in the filtrate can be recycled; except first-time filtrate, other filtrate can all be recycled, so that the recycling amount of the solvent is reduced; based on an annual industrial fluorene processing capacity of100 tons, the method can produce 75 tons of the refined fluorine each year and creates a economic benefit of 3 million yuan. In addition, the method has the advantages of rich and cheap industrial fluorene raw material resources, simple manufacturing process and convenient control and operation.

Description

technical field [0001] The invention belongs to the field of coal chemical industry, and in particular relates to a method for preparing refined fluorene with a content of more than 99% by using industrial fluorene, a by-product of tar. Background technique [0002] Industrial fluorene is one of the by-products of coal tar in coking plants, accounting for about 1% to 2% of coal tar. The output of industrial fluorene in my country is large, so the price of industrial fluorene is also very low. In recent years, the derivatives synthesized from fluorene have been widely used in the fields of chemical industry, bioengineering, polymer synthesis chemistry and functional polymer materials. The demand for fluorene in domestic and foreign markets has grown rapidly, especially in foreign markets. The demand for fine fluorene is increasing day by day, and the prospect is extremely broad. [0003] The boiling point of fluorene is 297°C, the melting point is 115°C, and its main impurit...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C13/567C07C7/14
Inventor 王萍李健王晓楠姚君刘冬杰宋亚楠田晓露
Owner 鞍钢化学科技有限公司