Unlock instant, AI-driven research and patent intelligence for your innovation.

Method for preparing coarse fluorene and fluorenone by taking wash oil as raw material

A technology for washing oil and crude fluorene, which is applied in chemical instruments and methods, preparation of carbon-based compounds, preparation of organic compounds, etc. It can solve the problems of high energy, difficulty in industrial fluorene, waste of materials, etc., and achieve the effect of reducing energy consumption

Inactive Publication Date: 2015-02-18
LANZHOU UNIVERSITY
View PDF2 Cites 0 Cited by
  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the components in the wash oil are complex, and it is difficult to obtain industrial fluorene through separation. During the separation process, a lot of materials will be wasted and a lot of energy will be consumed, which is very economically uneconomical.

Method used

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
View more

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0020] (1) Use an equal volume of 10% sulfuric acid solution (weight ratio) and 10% sodium hydroxide solution (weight ratio) to wash the washing oil with acid and alkali at room temperature in sequence, and wash with distilled water to remove residual alkali or salt and magnesium sulfate , drying to remove residual moisture, the obtained neutral washing oil rectification cut 275 ° C fraction, and then secondary rectification respectively cut 265 ° C, 270 ° C fractions, and then these fractions were put into the refrigerator to cool and crystallize to obtain crude fluorene.

[0021] (2) Weigh 2g of crude fluorene, 14g of N,N-dimethylformamide, and 0.050g of potassium hydroxide into a round low flask equipped with a magnetic stirrer, reflux condenser, and air blowing device, and turn on the magnetic stirring The fluorenone mixture was stirred by using a mixer, and air was blown to the reaction device at a blowing rate of 450ml / min. The reaction was carried out at room temperature...

Embodiment 2

[0025] (1) Use an equal volume of 10% sulfuric acid solution (weight ratio) and 10% sodium hydroxide solution (weight ratio) to wash the washing oil with acid and alkali at room temperature in sequence, and wash with distilled water to remove residual alkali or salt and magnesium sulfate , drying to remove residual moisture, the obtained neutral washing oil rectification cut 260 ° C fraction, and then secondary rectification respectively cut 260 ° C, 265 ° C fractions, and then these fractions were put into the refrigerator to cool and crystallize to obtain crude fluorene.

[0026] (2) Weigh 2g of crude fluorene, 14g of N,N-dimethylformamide, and 0.050g of potassium hydroxide into a round low flask equipped with a magnetic stirrer, reflux condenser, and air blowing device, and turn on the magnetic stirrer Stir, and blow air to the reaction device, the air blow rate is 450ml / min, the reaction is carried out at room temperature, and the whole reaction process is detected by TLC u...

Embodiment 3

[0030] (1) Use an equal volume of 10% sulfuric acid solution (weight ratio) and 10% sodium hydroxide solution (weight ratio) to wash the washing oil with acid and alkali at room temperature in sequence, and wash with distilled water to remove residual alkali or salt and magnesium sulfate , drying to remove residual moisture, the obtained neutral washing oil rectification cut 270 ° C fractions, and then secondary rectification were cut 260 ° C, 270 ° C fractions, and then these fractions were placed in the refrigerator to cool and crystallize to obtain crude fluorene.

[0031] (2) Weigh 2g of crude fluorene, 16g of N,N-dimethylformamide, and 0.056g of potassium hydroxide into a round low flask equipped with a magnetic stirrer, reflux condenser, and air blowing device, and turn on the magnetic stirring Stir with a mixer, and blow air to the reaction device, the air blow rate is 450ml / min, the reaction is carried out at room temperature, the whole reaction process is detected by T...

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
Login to View More

PUM

No PUM Login to View More

Abstract

The invention discloses a method for preparing coarse fluorene and fluorenone by taking wash oil as a raw material. The method comprises the following steps of: firstly, carrying out acid and alkali treatment on wash oil fraction obtained by fractionating coal tar, and enriching in a rectifying way to obtain coarse fluorene; secondly, converting fluorene in the coarse fluorene into fluorenone by an air liquid phase catalytic oxidation method; and based on ethylene glycol as entrainer, carrying out azeotropic distillation on reaction mixture to separate the fluorenone in the reaction mixture. The method has the advantages that a process route of first reaction and second separation is adopted, so that the fluorenone can be directly prepared by taking the coarse fluorene as the raw material, therefore, the fluorenone can be more easily separated from the reaction mixture; and the conventional preparation method of the fluorenone by firstly separating the fluorene from the coarse fluorene can be replaced, as the conventional method has the problems such as large material loss, high energy consumption, high cost, environment pollution and the like since the fluorene is very hard to separate.

Description

technical field [0001] The invention relates to a method for preparing crude fluorene and fluorenone, in particular to a method for preparing crude fluorene and fluorenone by using the washing oil fraction obtained by fractional distillation of coal tar as a raw material. Background technique [0002] Fluorenone is a raw material for the synthesis of fine chemicals, which are widely used in medicine, pesticides, dyes, functional polymer materials and other fields. At present, the preparation methods of fluorenone include vacuum decomposition of alkylbenzene derivatives and air liquid-phase oxidation method and air gas-phase oxidation method using fluorene as raw material; among them, because the liquid phase oxidation method has low reaction temperature and high yield of fluorenone, The reaction process is easy to control and is widely used; however, the raw material used in the liquid phase oxidation method is industrial fluorene, and its source is greatly limited. [0003...

Claims

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
Login to View More

Application Information

Patent Timeline
no application Login to View More
Patent Type & Authority Patents(China)
IPC IPC(8): C07C49/675C07C45/36C07C45/84C07C13/567C07C7/14C07C7/04
Inventor 石辉文白仲兰石贇张振华
Owner LANZHOU UNIVERSITY