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Preparation method of pulmonic cavity ventilating liquid

A mixed gas and octane technology, which is applied in the preparation of halogenated hydrocarbons, chemical instruments and methods, respiratory diseases, etc., can solve the problems of low yield, difficult operation, and many by-products, and the reaction conditions are easy to control , easy to separate and purify, no waste discharge effect

Inactive Publication Date: 2015-09-23
SHANGHAI HUAJIE EYE MEDICAL EQUIP
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The cobalt trifluoride fluorination method needs to react cobalt difluoride or cobalt oxide with fluorine gas in advance to convert cobalt trifluoride, and then react cobalt trifluoride with octane in a reactor to obtain a mixture containing perfluorooctane; Cobalt trifluoride needs to be continuously regenerated, the temperature of the reactor is difficult to control uniformly, the amplification is limited, the production cannot be carried out continuously, and it is not suitable for mass production
The synthesis of perfluorooctane by electrolytic fluorination is complicated in equipment, difficult in condition control, with many by-products and low yield, generally no more than 20%.
The direct fluorination of elemental fluorine requires elemental fluorine, and the transportation of elemental fluorine is very difficult. The on-site fluorine production equipment is complex and difficult to operate. Regulatory control, not easy to obtain production license

Method used

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Examples

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preparation example Construction

[0021] The preparation principle of perfluorooctane is as follows: In the reactor, octane gas and fluorinating agent nitrogen trifluoride undergo a fluorinating substitution reaction under the action of a catalyst to obtain perfluorinated products or partially fluorinated by-products of octane. In order to increase its fluorination degree and improve the purity of perfluorooctane, it is necessary to control the reaction conditions. By controlling the feeding ratio of the fluorinating agent and octane gas, the reaction temperature and the residence time of the reaction mixture in the reactor, the octane gas can be fluorinated as completely as possible while minimizing the breakage of the C-C bond in the octane molecule, thereby Improve the yield of the target product perfluorooctane.

[0022] In this embodiment, the reactor may be a tubular reactor made of monel, nickel, stainless steel, red copper or carbon steel. The catalyst filled in the tube can be selected from alkali me...

specific Embodiment approach 1

[0032] A Monel alloy reactor with an inner diameter of 50 mm and a length of 1000 mm is filled with spherical aluminum fluoride with a diameter of 3 mm. The reactor is heated to 300°C, and pure nitrogen trifluoride gas is fed into it for fluorination treatment. Then the reactor temperature was maintained at 150°C, the temperature of the octane vaporizer was maintained at 100°C, and 20% nitrogen trifluoride-nitrogen mixed gas and 5% octane were continuously introduced at a molar ratio of nitrogen trifluoride to octane of 15:1. The alkane-nitrogen mixed gas is used for the reaction, and the residence time is controlled to 60 seconds. When the amount of metered pure octane passing through the reactor reaches 500 grams, the feeding is stopped. Neutralize the collected reaction product with 20% potassium hydroxide aqueous solution until the pH value is neutral, let it stand, after layering, take the organic phase and wash it with deionized water three times, separate the organic p...

specific Embodiment approach 2

[0034] Use the same equipment as in Example 1. The temperature of the reactor is maintained at 200°C, and 50% nitrogen trifluoride-nitrogen mixed gas and 20% octane-nitrogen mixed gas are continuously fed into the reaction according to the molar ratio of nitrogen trifluoride and octane of 30:1, and the residence time is controlled 10 seconds. When the amount of metered pure octane passing through the reactor reaches 500 grams, the feeding is stopped. Neutralize the collected reaction product with 20% potassium hydroxide aqueous solution until the pH value is neutral, 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. Separation by rectification, taking the fraction with a boiling point of 103-105°C, to obtain 1248 grams of perfluorooctane, with a purity of 99%, and a yield of about 65% based on the addition of octane.

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Abstract

The invention discloses a preparation method of perfluorinated octane. The method includes the following steps: (1) filling a reactor with a catalyst, and carrying out fluoridation treatment with a fluridizer at high temperature; (2) adding octane into a vaporizer to obtain an octane steam, and controlling the vaporizer temperature between 100-150 DEG C; (3) introducing inert gas into the vaporizer, diluting the octane steam, and continuously introducing the octane steam diluted mixed gas into the reactor to carry out a fluoridation substitution reaction with the fluridizer; and (4) carrying out alkali washing, water washing and rectifying purification on the reaction product, to obtain the perfluorinated octane. The perfluorinated octane obtained by the preparation method disclosed by the invention can be used as a pulmonic cavity ventilating liquid or used in manufacture of ophthalmic surgical instruments.

Description

technical field [0001] The invention relates to a preparation method of lung cavity ventilation liquid, in particular to a preparation method of perfluorooctane which can be used as lung cavity ventilation liquid and ophthalmic surgical instruments. [0002] Background technique [0003] Perfluorooctane is a key component of lung cavity ventilation fluid, and its purity directly affects the efficacy of lung cavity ventilation fluid in treating lung diseases. In the past, the preparation methods of perfluorooctane include cobalt trifluoride fluorination method, electrolytic fluorination method and direct fluorination method of elemental fluorine. The cobalt trifluoride fluorination method needs to react cobalt difluoride or cobalt oxide with fluorine gas in advance to convert cobalt trifluoride, and then react cobalt trifluoride with octane in a reactor to obtain a mixture containing perfluorooctane; Cobalt trifluoride needs to be continuously regenerated, it is difficult t...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C19/08C07C17/10A61K31/02A61P11/00
Inventor 鲁俞方治文
Owner SHANGHAI HUAJIE EYE MEDICAL EQUIP
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