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Method for preparing antimony pentafluoride

A technology of antimony pentafluoride and antimony trioxide, applied in chemical instruments and methods, inorganic chemistry, antimony compounds, etc., can solve the problems of high impurity content in finished products, high melting point, and difficult purification of products, and achieve reliable product quality, Easy to control, high yield effect

Active Publication Date: 2009-09-16
RES INST OF PHYSICAL & CHEM ENG OF NUCLEAR IND
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Problems solved by technology

[0007] However, in fact, the method for preparing antimony pentafluoride is not as simple as the above reaction formula. During the reaction, some intermediate fluorides are often generated, and there may also be adducts. These adducts are very stable and have relatively High melting point makes it difficult to purify the product, resulting in high impurity content in the finished product

Method used

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  • Method for preparing antimony pentafluoride
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  • Method for preparing antimony pentafluoride

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preparation example Construction

[0031] The preparation method of antimony pentafluoride of the present invention comprises the following steps:

[0032] (i) Fluorine gas purification

[0033] First, pass the fluorine gas in the fluorine gas storage tank 1 into the fluorine gas purifier 2 for freezing and liquefaction, and use the liquid nitrogen cold trap outside the fluorine gas purifier 2 to maintain the temperature of the fluorine gas purifier 2 at -140~- Between 195°C, the fluorine gas is liquefied at this time, and the impurity gases that cannot be condensed, such as hydrogen, oxygen and nitrogen, and other high-boiling substances are still in the gaseous state. Start the vacuum unit 7 to evacuate the impurity gas that cannot be condensed.

[0034] Then, by increasing the temperature of the fluorine gas purifier 2, the liquid fluorine is gasified to obtain a fluorine gas with a purity of more than 99%. Finally, the purified fluorine gas is input to the buffer tank 3 through pipelines, ready for compou...

Embodiment 1

[0044] First, purify the reactor 4, add 25 kg of antimony trioxide with a purity of 98.5% into the reactor 4; close the reactor, evacuate to -0.08MPa, and then preheat the reactor 4 to 100°C. Pass the purified fluorine gas in the buffer tank 3 into the reactor 4 .

[0045] During the reaction process, the temperature in the reactor was kept at 150°C. When the temperature of the reactor tended to drop significantly, the flow of fluorine gas was stopped to check that the reaction was terminated, and a liquid antimony pentafluoride crude product containing light impurities was obtained.

[0046] The liquid antimony pentafluoride crude product is pumped into the rectification tower for collection by means of negative pressure. First, the rectification tower is heated and the temperature is controlled at 100°C. As the temperature in the rectification tower rises, the liquid antimony pentafluoride begins to distill, vaporize and rise. The gas phase in the rectification tower rises ...

Embodiment 2

[0049] First, purify the reactor 4, add 25 kg of antimony trioxide with a purity of 98.5% into the reactor 4; close the reactor, evacuate to -0.08MPa, and then preheat the reactor 4 to 150°C. Pass the purified fluorine gas in the buffer tank 3 into the reactor 4 .

[0050] During the reaction process, the temperature in the reactor was kept at 200°C. When the temperature of the reactor tended to drop significantly, the flow of fluorine gas was stopped to check the termination of the reaction, and a liquid antimony pentafluoride crude product containing light impurities was obtained.

[0051] The liquid antimony pentafluoride crude product is pumped into the rectification tower for collection by means of negative pressure. First, the rectification tower is heated and the temperature is controlled at 125°C. As the temperature in the rectification tower rises, the liquid antimony pentafluoride begins to distill, vaporize and rise. The gas phase in the rectification tower rises t...

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Abstract

The invention discloses a method for preparing antimony pentafluoride, and the method comprises the following steps: firstly purifying raw material fluorine gas, removing high boiling point gas impurities which can not be condensed in the fluorine gas; carrying out the synthesis reaction on the fluorine gas and antimony trioxide for generating a liquid antimony pentafluoride crude product; further gasifying and condensing the liquid antimony pentafluoride crude product by the distillation process and removing the gas impurities in the crude product to obtain a high-purity liquid antimony pentafluoride product. The method has simple equipment, convenient operation, safe equipment operation, stable product quality and high purity of being greater than 98.5 percent.

Description

technical field [0001] The invention belongs to a method for preparing antimony pentafluoride, in particular to a method for preparing antimony pentafluoride by using fluorine gas and antimony as raw materials and carrying out a synthesis reaction in a negative pressure container. Background technique [0002] Antimony pentafluoride is a high-energy fluorinating agent widely used in anticancer drugs in the medical pharmaceutical industry. There are many methods for preparing antimony pentafluoride at present, and the commonly used preparation methods are as follows: [0003] One method is: fluorine gas (F 2 ) and antimony trifluoride (SbF 3 ) react to form antimony pentafluoride (SbF 5 ), the chemical reaction formula is: [0004] [0005] Another method is: the reaction of hydrogen fluoride and antimony pentachloride to prepare antimony pentafluoride. The method is to mix hydrogen fluoride gas (HF) and antimony pentachloride (SbCl 5 ) mixture was refluxed in a plati...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01G30/00
Inventor 崔学文贺邓仝庆汤进军崔建起董国芳
Owner RES INST OF PHYSICAL & CHEM ENG OF NUCLEAR IND
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