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Method for preparing high-purity dinuclear ferrocene by inert gas assisted steam distillation for low-boiling-point impurity removal

A steam distillation and inert gas technology, applied in chemical instruments and methods, metallocenes, organic chemistry, etc., can solve the problems of difficult separation of ferrocene and ferrocene, difficult to continue distillation, etc., to achieve large preparation volume and low production cost The effect of low cost and simple operation process

Active Publication Date: 2019-07-26
NORTHWESTERN POLYTECHNICAL UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] In the early stage, we separated the binuclear ferrocene raw materials by ordinary distillation and vacuum distillation. During the distillation process, we found that the boiling point of ferrocene derivatives is quite high, and it is difficult to separate them well by ordinary distillation or vacuum distillation. Low-boiling ferrocene, ethyl ferrocene, etc. At the same time, as the distillation proceeds, the +2 valence iron in ferrocene may be oxidized, or the ferrocene ring may be polymerized to form a viscous black paste , making it difficult for the distillation to continue

Method used

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  • Method for preparing high-purity dinuclear ferrocene by inert gas assisted steam distillation for low-boiling-point impurity removal
  • Method for preparing high-purity dinuclear ferrocene by inert gas assisted steam distillation for low-boiling-point impurity removal
  • Method for preparing high-purity dinuclear ferrocene by inert gas assisted steam distillation for low-boiling-point impurity removal

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Effect test

Embodiment 1

[0034] Assemble the steam distillation device, prepare ethanol: water = 1:9 mixed solution and add 500ml to the steam generator, set the temperature of the steam generator to 190°C, set the temperature of the distillation bottle to 130°C, wait until the water in the steam generator boils After that, open the valve of the gas cylinder and pass N into the distillation bottle 2 ; when the temperature at the upper end of the thorn-shaped fractionating tube reaches 85°C, and there are drops of water dripping from the sampling bottle, add five times the volume of petroleum ether to the binuclear ferrocene industrial product and ultrasonically disperse it for 10 minutes to prepare a solution, and pour it into the retort Add a petroleum ether solution containing 12g of sample to start the distillation; after 3.2 hours of distillation, when no brown droplets are observed in the condensation tube, turn off the heating and stop the distillation; when the temperature in the distillation bo...

Embodiment 2

[0036] Assemble the steam distillation device, prepare ethanol: water = 1:9 mixed solution and add 500ml to the steam generator, set the temperature of the steam generator to 190°C, set the temperature of the distillation bottle to 130°C, wait until the water in the steam generator boils After that, open the valve of the gas cylinder and pass N into the distillation bottle 2 ; when the temperature at the upper end of the thorn-shaped fractionating tube reaches 85°C, and there are drops of water dripping from the sampling bottle, add five times the volume of petroleum ether to the binuclear ferrocene industrial product and ultrasonically disperse it for 10 minutes to prepare a solution, and pour it into the retort Add a petroleum ether solution containing 12g of sample to start the distillation; after 3.2 hours of distillation, when no brown droplets are observed in the condensation tube, turn off the heating and stop the distillation; when the temperature in the distillation bo...

Embodiment 3

[0038] Assemble the steam distillation device, prepare ethanol: water = 1:9 mixed solution and add 500ml to the steam generator, set the temperature of the steam generator to 190°C, set the temperature of the distillation bottle to 130°C, wait until the water in the steam generator boils After that, open the valve of the gas cylinder and pass N into the distillation bottle 2 ; when the temperature at the upper end of the thorn-shaped fractionating tube reaches 85°C, and there are drops of water dripping from the sampling bottle, add five times the volume of petroleum ether to the binuclear ferrocene industrial product and ultrasonically disperse it for 10 minutes to prepare a solution, and pour it into the retort Add a petroleum ether solution containing 13g of the sample, and start distillation; after 3.2 hours of distillation, when no brown droplets are observed in the condensation tube, turn off the heating and stop the distillation; when the temperature in the distillation ...

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Abstract

The invention relates to a method for preparing high-purity dinuclear ferrocene by inert gas assisted steam distillation for low-boiling-point impurity removal. In an inert atmosphere, by regulation of steam composition, distillation temperature, steam device temperature and insert gas flow, impurities with low boiling points can be removed to obtain high-content high-boiling-point dinuclear ferrocene, and separation of the industrial dinuclear ferrocene is realized. The method is simple in operating process, and compared with a column chromatography method, the method has advantages of largepreparation capacity, avoidance of high solvent consumption and suitableness for large-scale industrial production. Compared with a common distillation method, a steam distillation method has advantages that great separation effects can be obtained at a temperature far below a boiling point of a to-be-separated substance, and energy saving, low production cost, low carbon and environmental friendliness are realized. By insert gas assistance, oxidation of dinuclear ferrocene derivatives at a high temperature is avoided, the problem of difficulty in high-temperature distillation of the dinuclearferrocene derivatives is solved, and distillation efficiency is improved.

Description

technical field [0001] The invention belongs to the field of separation and purification of binuclear ferrocene, and relates to a method for large-scale preparation of high-purity binuclear ferrocene by removing low-boiling point impurities through inert gas-assisted steam distillation. Background technique [0002] Ferrocene and its derivatives are a class of non-benzene aromatic ring metal organic compounds with a unique sandwich structure, which have been widely used in medicine, electrochemistry, liquid crystal materials, photosensitive materials, fuel oil smoke suppressants, gas combustion catalysts, etc. field. [0003] Ferrocene derivatives are also a kind of burning rate catalysts, and have been widely used in solid propellants, especially AP / AI / HTPB propellants. The difference in the number of ferrocene groups determines that ferrocene derivatives can be divided into mononuclear ferrocene derivatives and binuclear ferrocene derivatives. Binuclear ferrocene derivat...

Claims

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Application Information

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IPC IPC(8): C07F17/02
CPCC07F17/02
Inventor 马晓燕索奇张驰刘晓菊
Owner NORTHWESTERN POLYTECHNICAL UNIV