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Method for scaling-up purification of ethyl dicyclopentadienyl iron

A technology of ethyl ferrocene and a new method, applied in chemical instruments and methods, metallocene, organic chemistry, etc., can solve the problems such as poor vacuum distillation effect, inability to remove impurities, and difficulty in removing impurity ferrocene

Active Publication Date: 2008-04-02
邱吉辉 +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Usually, the purification method of ethyl ferrocene is to use vacuum distillation (ethyl ferrocene: b.p.74~76℃ / 30Pa, 121~123℃ / 133Pa): For impurities such as ferrocene, in the process of vacuum distillation It will be distilled together with the ethyl ferrocene fraction. Even if multiple vacuum distillations are adopted, the impurity ferrocene is difficult to remove, and the effect of vacuum distillation is not good.
In the large-scale production of ethyl ferrocene, in order to shorten the production cycle and obtain a higher yield, often in the crude ethyl ferrocene, there are more impurities such as ferrocene, which are simply obtained by vacuum distillation It is impossible to remove these impurities

Method used

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Embodiment Construction

[0005] (1) Pour about 5 kg of ethylferrocene to be purified into a 5000 ml large-mouth temperature-resistant glass bottle, cover the bottle cap, and put it into a low-temperature constant temperature freezing tank at -25 ° C. The medium solution in the freezing tank is no Water ethanol, freezing treatment time is 3 hours, make it solidify, become brown paste.

[0006] (2) Take out the frozen glass bottle and gently place it on the rubber mat. Slowly melt the brown paste in the glass bottle at room temperature. During the melting process, brown insoluble matter will precipitate out. It takes 3 to 4 hours. In addition, during the melting process, do not accelerate the melting by stirring or shaking.

[0007] (3) When the paste in the glass bottle melts almost completely, immediately adopt fast filter paper to carry out suction filtration to remove brown insoluble matter, and the obtained filtrate is purified ethylferrocene.

[0008] (4) Use 10 low-temperature and constant-temp...

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Abstract

The ethyl ferrpcene is the intermediate to compose the efficient burning speed activator [2, 2-double (the ethyl ferrocene) the dimethylmethane] and has the important applied cost in aerospace industry and the national defence industry. So, the producing on a large scale and the purifying the ethyl ferrocene are very important. The impurity in the ethyl ferrocene is mainly the ferrocene and other ramification of the ferrocene. Generally, the vacuum distillation is adopted to purify the ethyl ferrocene; the impurity such as the ferrocene can be extracted with the ethyl ferrocene distillate during the reduced pressure distillation process, so the effect of the vacuum distillation is not good. The impurity can't be eliminated only by the vacuum distillation when producing the ethyl ferrocene on a large scale; So,the method is invented. The invention is easy and convenient.The invention wipe off the impurity by the ordinary case;so the ethyl ferrocene can be purified on a large scale. The invention has the important applied cost to the producing the ramification of the ferrocene on a large scale.

Description

technical field [0001] Organometallic Chemistry Metallocene Chemistry Ferrocene Derivatives Background technique [0002] Ethyl ferrocene is an intermediate for the synthesis of dinuclear ferrocene derivatives [2,2-bis(ethylferrocenyl)propane (commonly known as catocene, catocene)], dinuclear ferrocene derivatives [2, 2-bis(ethylferrocenyl)propane] is a high-efficiency burning rate catalyst for rocket composite solid propellants, and has important application value in aerospace industry and national defense industry. With the rapid development of aerospace industry and national defense industry, there is an urgent need for large-scale production of dinuclear ferrocene derivatives [2,2-bis(ethylferrocenyl)propane]. Therefore, large-scale production and purification of ethyl ferrocene has become very important. The impurities in ethyl ferrocene are mainly ferrocene, acetyl ferrocene and other ferrocene derivatives. Usually, the purification method of ethyl ferrocene is to u...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07F17/02
Inventor 邱吉辉邱吉昌
Owner 邱吉辉
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