Production raw material of liquid ventilation fluid and material for ophthalmic surgery and continuous preparation method of production raw material

An ophthalmic surgery and liquid technology, applied in the field of perfluorooctane preparation, can solve the problems of low perfluorooctane yield, low yield, many by-products, etc., and achieves easy control of reaction conditions, easy separation and purification, and no three wastes. The effect of emissions

Inactive Publication Date: 2019-01-04
苏州工业园区捷仕通医疗设备有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The cobalt trifluoride method needs to convert cobalt difluoride into cobalt trifluoride by fluorination first, and then cobalt trifluoride reacts with octane in the reactor to obtain a mixture containing perfluorooctane; cobalt trifluoride needs to be continuously regenerated , the reactor temperature is difficult to control uniformly, the scale-up is limited, the production cannot be carried out continuously, and it is not suitable for mass production
In addition, the electrolytic fluorination method to synthesize perfluorooctane has complex equipment, difficult condition control, many by-products, and low yield, which generally does not exceed 15%.
[0003] Publication (Announcement) No.: CN104926597A patent discloses a preparation method of perfluorooctane, which includes the following steps: (1) filling a catalyst in the reactor, and performing fluorination treatment at high temperature with a fluorinating agent; (2) Add octane to the vaporizer to obtain octane vapor, and control the temperature of the vaporizer between 100 and 150°C; (3) Pass inert gas into the vaporizer to dilute the octane vapor, and continuously pass the octane vapor diluted mixture into The reactor and the fluorinating agent undergo a fluorination substitution reaction; (4) The reaction product is purified by alkali washing, water washing, and rectification to obtain perfluorooctane; improve

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0026] A Monel alloy reactor with an inner diameter of 80 mm and a length of 1000 mm is filled with spherical alumina with a diameter of 3 mm. The reactor is heated to 250°C, and a mixed gas of 50% fluorine-50% nitrogen is introduced for fluorination, so that alumina is completely converted into aluminum fluoride. Then the temperature of the reactor is maintained at 200°C, 20% fluorine-nitrogen mixed gas and 10% octane-nitrogen mixed gas are continuously fed in at a molar ratio of fluorine gas to octane 20:1 for reaction, and the residence time is controlled for 5 seconds. After 10 hours, neutralize the collected reaction product with 20% potassium hydroxide aqueous solution to a neutral pH value, and let it stand. After layering, take the organic phase and wash it with deionized water three times. Separate the organic phase and dry it with anhydrous sodium sulfate After rectification and separation, take the fraction with a boiling point of 101-104°C to obtain 1000 g of perflu...

Embodiment 2

[0028] The same equipment as in Example 1 was used. The temperature of the reactor is maintained at 260°C, and 20% fluorine-nitrogen mixed gas and 20% octane-nitrogen mixed gas are continuously fed in at a molar ratio of fluorine gas to octane 20:1 for reaction, and the residence time is controlled for 10 seconds. After 10 hours, neutralize the collected reaction product with 20% potassium hydroxide aqueous solution to a neutral pH value, and let it stand. After layering, take the organic phase and wash it with deionized water three times. Separate the organic phase and dry it with anhydrous sodium sulfate After rectification and separation, take the fraction with a boiling point of 101-104°C to obtain 1500 grams of perfluorooctane with a purity of 99.5% and a yield of about 85%.

Embodiment 3

[0030] The same equipment as in Example 1 was used. The temperature of the reactor was maintained at 280°C, and 20% fluorine-nitrogen mixed gas and 15% octane-nitrogen mixed gas were continuously fed in at a ratio of 25:1 fluorine gas to octane molar ratio for reaction, and the residence time was controlled to be 10 seconds. After 10 hours, neutralize the collected reaction product with 20% potassium hydroxide aqueous solution to a neutral pH value, and let it stand. After layering, take the organic phase and wash it with deionized water three times. Separate the organic phase and dry it with anhydrous sodium sulfate After rectification and separation, take the fraction with a boiling point of 101-104°C to obtain 1600 g of perfluorooctane with a purity of 99% and a yield of about 80%.

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Abstract

The invention provides a production raw material of liquid ventilation fluid and a material for an ophthalmic surgery and a continuous preparation method of the production raw material. The productionraw material comprises fluorine and an octane organic matter, the molar ratio of the fluorine to the octane organic matter is 20: 1-25: 1, the fluorine is mixed gas of pure fluorine or fluorine and inert gas, and the concentration of the fluorine is not lower than 10%; and the octane organic matter is a mixture of octane, an octane homologue or a mixture of the octane organic matter and inert gas. The production raw material is suitable for being produced continuously on a large scale, reaction conditions are easy to control, the yield is high, by-products are less, reaction products are easyto separate and purify, and waste gas, waste water and solid wastes are not discharged in a production process. By the method of the invention, perfluorooctane of which the purify is greater than orequal to 99% can be prepared, and can serve as the production raw material of liquid ventilation fluid and a preparation for the ophthalmic surgery.

Description

Technical field [0001] The invention relates to the technical field of perfluorooctane preparation methods, in particular to the production raw materials of liquid ventilation fluids and materials for ophthalmic surgery and a continuous preparation method thereof. Background technique [0002] In the past, perfluorooctane preparation methods include cobalt trifluoride fluorination method and electrolytic fluorination method. The cobalt trifluoride method requires the first fluorination of the cobalt difluoride to convert it into cobalt trifluoride, and the cobalt trifluoride reacts with octane in the reactor to obtain a mixture containing perfluorooctane; the cobalt trifluoride needs to be continuously regenerated , The temperature of the reactor is difficult to control uniformly, the scale-up is limited, the production cannot be carried out continuously, and it is not suitable for mass production. In addition, the electrolytic fluorination method for synthesizing perfluorooctan...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C17/10C07C19/08
CPCC07C17/10C07C19/08
Inventor 鲁俞鲁俊
Owner 苏州工业园区捷仕通医疗设备有限公司
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