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A New Purification and Refining Process of Crude Fluorene

A crude fluorene and process technology, which is applied in the field of crude fluorene purification and refining new process, can solve the problems of high solvent toxicity, high cost, and low product purity, and achieve simple equipment and process, less production, and low operation and running costs Effect

Active Publication Date: 2016-02-03
江西科美香料有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The disadvantages of domestic fluorene separation technology are high cost, high solvent toxicity and low product purity

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0018] Take 1000.00g of crude fluorene containing 69.91% by mass of fluorene, add 1000.00g of n-butanol to the reactor, stir at room temperature for 40min at a stirring speed of 30r / min, then filter and dry to obtain industrial Fluorene 673.80g, wherein the yield of fluorene is 85.22%;

[0019] Then, according to the mass ratio of toluene, water and industrial fluorene at 0.5:0.5:1, add 673.80g of industrial fluorene obtained above into the reactor—"a new type of equipment for purifying refined fluorene from industrial fluorene" (patent number 2012205596915), Then add 336.89g of toluene and 336.89g of water, turn on the program heating and cooling control device to heat, turn on the mixer, the stirring speed is 30r / min, stir for 40min, and heat to 90°C until the above industrial fluorene is completely dissolved; turn off the mixer, pass the program The temperature rise and fall control device adjusts the temperature of the reactor to keep the temperature at a cooling rate of 5...

Embodiment 2

[0021] Take 1000.00g of crude fluorene containing 60.55% by mass of fluorene, add 1000.00g of ethyl acetate to the reaction kettle, stir at room temperature for 50min at a stirring speed of 60r / min, then filter and dry to obtain 588.68g of mass content with a purity of 85.70% The fluorene, wherein the yield of fluorene is 83.32%.

[0022] According to the mass ratio of cyclohexane, water and industrial fluorene of 0.5:0.5:1, 588.68g of industrial fluorene, 294.34g of cyclohexane and 294.34g of water obtained above are added to the reaction kettle——"a kind of purification from industrial fluorene In "New Equipment for Fluorene" (Patent No. 2012205596915), turn on the program heating and cooling control device to heat, turn on the mixer, stir at a speed of 60r / min, stir for 50 minutes, and heat to 90°C until the above-mentioned industrial fluorene is completely dissolved; turn off the mixer, The temperature of the reactor is adjusted by the programmed temperature rise and fall c...

Embodiment 3

[0024] Take 1000.00g of crude fluorene containing 65.82% by mass of fluorene, add 1000.00g of solvent dimethylformamide to the reaction kettle, stir at room temperature for 60min at a stirring speed of 90r / min, then filter and dry to obtain 649.95g of mass content Fluorene with a purity of 86.23%, wherein the yield of fluorene is 85.11%.

[0025] According to the mass ratio of cyclopentadiene, water and industrial fluorene of 0.5:0.5:1, 649.95g of industrial fluorene, 324.98g of cyclopentadiene and 324.98g of water obtained above are added to the reactor—"a kind of industrial fluorene In the new equipment for purifying refined fluorene" (Patent No. 2012205596915), turn on the program heating and cooling control device to heat, turn on the mixer, stir at a speed of 90r / min, stir for 60 minutes, and heat to 90°C until the above industrial fluorene is completely dissolved; close Stirrer, adjust the temperature of the reactor through the programmed temperature rise and fall contro...

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Abstract

The invention relates to a new process for purifying and refining coarse fluorene. The new process comprises the following steps: first, adding fluorene with the mass content of 60 to 70 percent and an organic solvent in a mass ratio of 1:1 into a reaction kettle, stirring for 40 to 60 minutes at normal temperature at the stirring speed of 30 to 90r / min, and performing suction filtration and drying to obtain industrial fluorene with the mass content being over 80 percent; then, adding the industrial fluorene into the reaction kettle according to the proportion that the ratio of organic solvent to water to the industrial fluorene is 0.5:0.5:1, then adding the organic solvent and the water, turning on a program heating and cooling control device for heating the mixture, starting a stirring machine for stirring 40 to 60 minutes at the stirring speed of 30 to 90 r / min, heating to 90+ / -2 DEG C until the industrial fluorene is dissolved completely; turning off the stirring machine, adjusting the temperature of the reaction kettle and keeping the temperature of the reaction kettle at the cooling speed of 1 to 5 DEG C / min for performing program cooling crystallization by using the program heating and cooling control device, wherein the final crystallization temperature is controlled to be 30+ / -2 DEG C; and finally, filtering crystals to obtain fine fluorene with the mass content purity being higher than 98 percent.

Description

technical field [0001] The invention relates to a purification technology of industrial fluorene, in particular to a new purification process of crude fluorene. Background technique [0002] The chemical structure of fluorene is a special biphenyl structure, that is, a methylene group fixes two benzene rings on a plane. Compared with general biphenyl, it has stronger rigidity in structure. This also brings about many other differences in properties, such as better thermal stability, larger conjugate absorption wavelength, more obvious photoluminescence (fluorescence and phosphorescence), and electroluminescence. Due to the special structure of fluorene, it is widely used in the organic synthesis industry, especially in the synthetic resin industry, and can also be used to prepare fluorene-based metal compounds, organic photoconductors, resins, and dyes. [0003] The fluorenone produced by oxidation of fluorene is reduced and esterified to produce bisphenol fluorene. Due to ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C13/567C07C7/14C07C7/10
Inventor 熊道陵陈玉娟邱萍王庚亮杨金鑫许光辉
Owner 江西科美香料有限公司