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Preparation method for 9-fluorenone

The technology of fluorenone and quaternary ammonium salt is applied in the field of preparation of 9-fluorenone, which can solve the problems of human health damage, pyridine odor, environmental pollution and the like, and achieve the effect of low energy consumption

Active Publication Date: 2013-12-11
BAOSHUN TECH CO LTD +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Although this patent uses pyridine dissolved in water as a solvent, which simplifies the reaction process and is easy to operate, but pyridine has a foul smell, which pollutes the environment relatively large and is harmful to human health.

Method used

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  • Preparation method for 9-fluorenone

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0045] ① Take 5g of industrial fluorene, 0.1g of reagent grade tetra-n-butylammonium bromide and 20mL of quinoline, put them in a 50mL three-neck round bottom flask, and mechanically stir in a constant temperature water bath at 60°C until completely dissolved to obtain an oil phase;

[0046] ② Dissolve sodium hydroxide in 4mL water to prepare a 30wt% aqueous phase;

[0047] ③Mix the oil phase and the water phase, stir mechanically in a constant temperature water bath at 60°C at a stirring speed of 300r / min, feed air at a speed of 140mL / min, monitor the reaction process with thin-layer chromatography, after 2.5h, thin-layer The chromatogram showed that the fluorene spot of the raw material disappeared completely, and the reaction was stopped after continuing the reaction for 0.5h to obtain the reaction solution a;

[0048] ④ Cool and stratify the reaction liquid a, separate the water layer, recover the alkaline solution, take the oil layer, wash the oil layer with water until it ...

Embodiment 2

[0051] Except that in step 2, 4 mL of 40 wt % sodium hydroxide solution was used instead of 4 mL of 30 wt % sodium hydroxide solution, and steps 1 and 3 were changed to stirring, dissolving and reacting at 40 ° C, the others were the same as in Example 1. After 9.5 hours of reaction, thin-layer chromatography showed that the raw material fluorene spots completely disappeared, and the reaction was continued for 0.5 hours to stop the reaction. Obtain 5.0g product after step ④ a series of processing.

[0052] Samples were taken for GC analysis, and the spectrum showed that there was no fluorenone component. Except for the impurities brought in by 9-fluorenone and raw material industrial fluorene, no new components appeared, which also indicated that fluorene was 100% converted into 9-fluorenone.

Embodiment 3

[0054] Except that in step ②, 4mL of 40wt% sodium hydroxide solution was used instead of 4mL of 30wt% sodium hydroxide solution, and steps ① and ③ were changed to stirring, dissolving and reacting at 50°C, the others were the same as in Example 1. After 6.5 hours of reaction, thin-layer chromatography showed that the raw material fluorene spots completely disappeared, and the reaction was continued for 0.5 hours to stop the reaction.

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Abstract

The invention discloses a preparation method for 9-fluorenone. According to the method, industrial fluorene (the purity is more than 95 percent) is taken as a raw material, alkali is taken as a catalyst, a heterocyclic compound containing nitrogen and water are used as solvent and quaternary ammonium salt is taken as a phase transfer agent; under the lower temperature and stirring condition, fluorene and gas containing oxide react and the fluorene is converted into 9-fluorenone; by selecting proper reaction conditions, the conversion rate of the fluorene can reach 100 percent. The recovered alkali and solvent in the invention can be recycled without a special complex treatment process and benefit the industrialization. According to the preparation method disclosed by the invention, quinoline and isoquinoline as well as a mixer of the quinoline and the isoquinoline are taken as the solvent and the reaction condition that the fluorene is oxidized into the 9-fluorenone, the selection of the alkali as the catalyst and the phase transfer agent and the recycling of the solvent and the alkali are researched to obtain the conditions that the fluorene is converted into the 9-fluorenone at high conversion rate and high selectivity; and a complete synthetic process is provided.

Description

technical field [0001] The invention relates to a preparation method of 9-fluorenone, which belongs to the field of organic synthesis. Background technique [0002] Fluorene is a component of coal tar, which has not been developed and utilized, and its economic benefits are not high. Generally, the purity of industrial fluorene is greater than 95%, but the source of fluorene is different, and the components containing impurities are different, which will seriously affect the reaction rate and the purity of the product. The industrial fluorene used in the present invention has a purity greater than 95%, and contains impurities such as 9-fluorenol, oxyfluorene, and methylbiphenyl. Fluorenone, especially 9-fluorenone, is a very valuable raw material for the preparation of high polymer monomers, such as 9,9-bis(4-hydroxyphenyl)fluorene, which is widely used in the preparation of polycarbonate and epoxy resin. [0003] The following method has been disclosed in the prior art l...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C45/36C07C49/643
Inventor 高占先于丽梅高天翔李汇丰何永超
Owner BAOSHUN TECH CO LTD
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