CN103288587A - Preparation method of perfluoroalkane - Google Patents
Preparation method of perfluoroalkane Download PDFInfo
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- CN103288587A CN103288587A CN2013101946976A CN201310194697A CN103288587A CN 103288587 A CN103288587 A CN 103288587A CN 2013101946976 A CN2013101946976 A CN 2013101946976A CN 201310194697 A CN201310194697 A CN 201310194697A CN 103288587 A CN103288587 A CN 103288587A
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Abstract
The invention provides a method for preparing perfluoroalkane. The method comprises the following steps of: filling a filler in a reactor, fluorating by using a fluorating agent, keeping the temperature inside the reactor between 100 to 300 DEG C, adding reaction materials in a vaporizer to vaporize, controlling the temperature inside the vaporizer between 130 to 150 DEG C, wherein the reaction materials comprise C5-C16 alkanes and one or more of partial fluorides of the C5-C16 alkanes, continuously bringing reaction material vapor in the reactor by using an inert gas, continuously feeding the fluorating agent in the reactor to react with the reaction material vapor continuously fed in the reactor, and separating and purifying to obtain the perfluoroalkane. The method provided by the invention is suitable for large-scale continuous productions; the reaction conditions are easily controlled; the yield is high; the by-products are less; the reaction production is easily separated and purified; no three wastes are discharged during the production process. With the adoption of the method, perfluorooctane with the purity being greater than or equal to 98% can be prepared and can act as a production material of lung cavity ventilation aerating liquid and a preparation for ophthalmologic operations.
Description
Technical field
The present invention relates to a kind of preparation method of perfluoro alkane, relate in particular to a kind of lung chamber aeration liquid and preparation method thereof.
Background technology
The preparation method of PFO had cobaltic fluoride fluorination method and electrofluorination method in the past.The cobaltic fluoride method need be fluoridized cohalt difluoride earlier and is converted into cobaltic fluoride, and cobaltic fluoride obtains containing the mixture of PFO again with the octane reaction in reactor; Cobaltic fluoride needs constantly regeneration, and temperature of reactor is difficult to control evenly, amplifies restrictedly, and production can not be carried out continuously, is unsuitable for production in enormous quantities.In addition, the electrofluorination method is synthesized PFO equipment complexity, condition control difficulty height, and by product is many, and yield is low, generally is no more than 15%.
Summary of the invention
The objective of the invention is to overcome above-mentioned deficiency, a kind of method of perfluoro alkane is provided, this method is suitable for the mass-producing serialization produces, and reaction conditions is easy to control, the productive rate height, and by product is few, and reaction product is separated purification easily, and the production process three-waste free discharge.
The invention provides a kind of method for preparing perfluoro alkane, it is characterized in that, may further comprise the steps:
Step 1 is filled to filler in the reactor, fluoridizes with fluorizating agent, and keeping the inside reactor temperature is at 100-300 ℃;
Step 2 joins reaction raw materials in the vaporizer with the feed rate of 1-10L/h and to vaporize, and temperature is 130-150 ℃ in the control vaporizer, and wherein, described reaction raw materials is the alkane of C5-C16 and in its partially fluorinated thing one or more;
Step 3 is brought into reactor with rare gas element continuously with the reaction raw materials steam that step 2 obtains;
Step 4 feeds fluorizating agent in the reactor continuously, reacts with the reaction raw materials steam of continuous feeding reactor, keeps the inside reactor temperature at 100-300 ℃;
Step 5 is separated and is purified, and obtains perfluoro alkane.
Wherein, described alkane can be preferably normal alkane for branched alkane or normal alkane.
Preferably, described reaction raw materials is one or more in C6-C12 alkane and its partially fluorinated thing, more preferably one or more in C8-C10 alkane and its partially fluorinated thing, more preferably one or more in octane and its partially fluorinated thing.
Preferably, described filler is selected from one or more in basic metal, alkaline earth metal oxide, alkaline-earth metal fluoride, nickel and fluorochemical thereof, cobalt and fluorochemical thereof, copper and fluorochemical thereof, aluminium and fluorochemical thereof, manganese and the fluorochemical thereof.
Preferably, described basic metal is one or more in lithium, sodium, potassium, the caesium.
Preferably, the granularity of described filler 〉=100 orders.
Preferably, described fluorizating agent is the gas mixture of pure fluorine gas or fluorine and rare gas element, and wherein, the concentration of fluorine gas is not less than 5%(V/V in the gas mixture), the best is 10%-80%, and is particularly optimum between 20%-40%.
Preferably, in the step 3, the concentration of reaction raw materials steam in rare gas element is 1-60%(V/V), more preferably 1-40%, more preferably 1-20%.
Preferably, in the step 4, the mol ratio that feeds hydrogen atom in fluorizating agent and the reaction raw materials that feeds in the reactor in the reactor is at (1-2): 1.
Preferably, in the step 4, temperature of reaction is 100-300 ℃, more preferably 180-280 ℃.
Wherein, reaction pressure can be not particularly limited for negative pressure, normal pressure or malleation in the step 4, and it is safer to be preferably in atmospheric operation.
Preferably, in the step 4, the reaction times characterized with reactant residence time in reactor, and optional scope is 5-30 second, general optional 5-20 second was 5-15 second between optimal zone.
Preferably, in the step 5, by alkali cleaning, washing, rectification and purification, obtain perfluoro alkane.
Preferably, described reactor is tubular reactor, and material is Monel metal, nickel, stainless steel, red copper or carbon steel.
The present invention also provides a kind of lung chamber aeration liquid, comprises the PFO of method for preparing.Can also comprise other known lung chamber aeration liquids, for example perfluorodecalin etc.
Preferably, described lung chamber aeration liquid is made up of PFO.
The present invention also provides the application of a kind of above-mentioned lung chamber aeration liquid in the medicine of preparation treatment respiratory distress syndrome.
Method provided by the invention can adopt simple substance fluoride or its diluent gas as fluorizating agent, accurately feed molar ratio, temperature of reaction and the reaction times of control fluorizating agent and octane or partially fluorinated octane, organic reactant is fluoridized fully as far as possible, reduce the fracture of intramolecularly C-C key to greatest extent, improve the productive rate of target product, by product is few, and reaction product is separated purification easily.
Method provided by the invention is suitable for the mass-producing serialization produces, and reaction conditions is easy to control, the productive rate height, and by product is few, and reaction product is separated purification easily, and the production process three-waste free discharge.Adopt the method for the invention can prepare the PFO of purity 〉=98%, can be used as the raw materials for production that lung chamber aeration liquid and ophthalmologic operation are used preparation.
Embodiment
Below with reference to specific embodiment the present invention is further described, to understand the present invention better.
Reactor of the present invention can be selected tubular reactor for use, and material can be Monel metal, nickel, stainless steel, red copper or carbon steel etc.Fill basic metal, alkaline earth metal oxide, alkaline-earth metal fluoride, nickel and fluorochemical, cobalt and fluorochemical thereof, copper and fluorochemical thereof, aluminium and fluorochemical thereof, manganese and fluorochemical thereof in the pipe, if initial weighting material is not fluorochemical entirely, need before the feeding reactant reacts, fluoridize with the gas mixture of fluorine gas or fluorine, make weighting material be converted into fluorochemical fully.Weighting material is with the particulate state reactor of packing into, and granularity is more than 100 orders.
Embodiment 1
In the Monel metal reactor of internal diameter 80mm, long 1000mm, filling diameter is the spherical alumina of Φ 3mm.Reactor is heated to 300 ℃, feeds 50% fluoro-, 50% nitrogen mixed gas and fluoridizes, and makes aluminum oxide be converted into aluminum fluoride fully.Make temperature of reactor maintain 200 ℃ then, feed 20% fluoro-nitrogen mixed gas and 10% octane-nitrogen mixed gas continuously in fluorine gas and octane mol ratio 20:1 ratio and react 5 seconds residence time of control.10 as a child the reaction product collected to be neutralized to pH value with 20% potassium hydroxide aqueous solution be neutral, leave standstill, get organic phase deionized water wash three times after the layering, tell organic phase and carry out rectifying separation after with anhydrous sodium sulfate drying, get boiling point 100-105 ℃ cut, get 1000 gram PFO, purity 98%, productive rate about 70%.
Embodiment 2
With with embodiment 1 identical device.Temperature of reactor maintains 260 ℃, feeds 20% fluoro-nitrogen mixed gas and 20% octane-nitrogen mixed gas continuously in fluorine gas and octane mol ratio 20:1 ratio and reacts 10 seconds residence time of control.10 as a child the reaction product collected to be neutralized to pH value with 20% potassium hydroxide aqueous solution be neutral, leave standstill, get organic phase deionized water wash three times after the layering, tell organic phase and carry out rectifying separation after with anhydrous sodium sulfate drying, get boiling point 100-105 ℃ cut, get 1500 gram PFO, purity 98.5%, productive rate about 75%.
Embodiment 3
With with embodiment 1 identical device.Temperature of reactor maintains 280 ℃, feeds 20% fluoro-nitrogen mixed gas and 15% octane-nitrogen mixed gas continuously in fluorine gas and octane mol ratio 25:1 ratio and reacts 10 seconds residence time of control.10 as a child the reaction product collected to be neutralized to pH value with 20% potassium hydroxide aqueous solution be neutral, leave standstill, get organic phase deionized water wash three times after the layering, tell organic phase and carry out rectifying separation after with anhydrous sodium sulfate drying, get boiling point 100-105 ℃ cut, get 1600 gram PFO, purity 98%, productive rate about 65%.
Embodiment 4
With with embodiment 1 identical device and reaction conditions, aluminum oxide is changed to cobalt oxide, the reinforced mol ratio of fluorine gas and octane is 22:1, fluorine gas uses with 20% fluoro-nitrogen mixed gas, octane is with 20% octane-nitrogen mixture use.10 seconds residence time of control.10 as a child the reaction product collected to be neutralized to pH value with 20% potassium hydroxide aqueous solution be neutral, leave standstill, get organic phase deionized water wash three times after the layering, tell organic phase and carry out rectifying separation after with anhydrous sodium sulfate drying, get boiling point 100-105 ℃ cut, get 1600 gram PFO, purity 98%, productive rate about 75%.
More than specific embodiments of the invention are described in detail, but it is just as example, the present invention is not restricted to specific embodiment described above.To those skilled in the art, any equivalent modifications that the present invention is carried out and substituting also all among category of the present invention.Therefore, not breaking away from impartial conversion and the modification of doing under the spirit and scope of the present invention, all should contain within the scope of the invention.
Claims (10)
1. a method for preparing perfluoro alkane is characterized in that, may further comprise the steps:
Step 1 is filled to filler in the reactor, fluoridizes with fluorizating agent, and keeping the inside reactor temperature is at 100-300 ℃;
Step 2 joins reaction raw materials in the vaporizer with the feed rate of 1-10L/h and to vaporize, and temperature is 130-150 ℃ in the control vaporizer, and wherein, described reaction raw materials is the alkane of C5-C16 and in its partially fluorinated thing one or more;
Step 3 is brought into reactor with rare gas element continuously with the reaction raw materials steam that step 2 obtains, and keeping the inside reactor temperature is at 100-300 ℃;
Step 4 feeds fluorizating agent in the reactor continuously, reacts with the reaction raw materials steam of continuous feeding reactor;
Step 5 is separated and is purified, and obtains perfluoro alkane.
2. method according to claim 1 is characterized in that, described reaction raw materials is one or more in octane and its partially fluorinated thing.
3. method according to claim 1, it is characterized in that described filler is selected from one or more in basic metal, alkaline earth metal oxide, alkaline-earth metal fluoride, nickel and fluorochemical thereof, cobalt and fluorochemical thereof, copper and fluorochemical thereof, aluminium and fluorochemical thereof, manganese and the fluorochemical thereof.
4. method according to claim 3 is characterized in that, described basic metal is one or more in lithium, sodium, potassium, the caesium.
5. method according to claim 1 is characterized in that, described fluorizating agent is the gas mixture of pure fluorine gas or fluorine and rare gas element, and wherein, the concentration of fluorine gas is not less than 5%(V/V in the gas mixture).
6. method according to claim 1 is characterized in that, the concentration of reaction raw materials steam in rare gas element is 1-20%(V/V in the step 3).
7. method according to claim 1 is characterized in that, in the step 4, the mol ratio that feeds hydrogen atom in fluorizating agent and the reaction raw materials that feeds in the reactor in the reactor is at (1-2): 1.
8. method according to claim 1 is characterized in that, in the step 4, the reaction times is 5-30 second.
9. a lung chamber aeration liquid is characterized in that, comprises the PFO according to claim 1 or 2 described method preparations.
10. the application of the described lung of claim 7 chamber aeration liquid in the medicine of preparation treatment respiratory distress syndrome.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105693463A (en) * | 2014-11-28 | 2016-06-22 | 浙江省化工研究院有限公司 | Method for preparing C2-C6 perfluoroalkane |
| CN109134186A (en) * | 2018-08-28 | 2019-01-04 | 苏州工业园区捷仕通医疗设备有限公司 | The raw materials for production and its continuous preparation method of liquid ventilation liquid and ophthalmologic operation material |
| CN110511111A (en) * | 2019-04-29 | 2019-11-29 | 苏州工业园区捷仕通医疗设备有限公司 | Gas exchanges dielectric fluid |
| CN112778077A (en) * | 2021-01-18 | 2021-05-11 | 福建德尔科技有限公司 | Micro-reactor based electronic stage C2F6Preparation method |
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| CN1161953A (en) * | 1996-03-08 | 1997-10-15 | 昭和电工株式会社 | Method for production of tetrafluoro-methane |
| CN101671217A (en) * | 2009-09-28 | 2010-03-17 | 南京第一农药集团有限公司 | Method for preparing organic chlorofluoro compounds from organic polychlorinated compounds |
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2013
- 2013-05-23 CN CN201310194697.6A patent/CN103288587B/en active Active
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1161953A (en) * | 1996-03-08 | 1997-10-15 | 昭和电工株式会社 | Method for production of tetrafluoro-methane |
| CN101671217A (en) * | 2009-09-28 | 2010-03-17 | 南京第一农药集团有限公司 | Method for preparing organic chlorofluoro compounds from organic polychlorinated compounds |
Non-Patent Citations (2)
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| 方克明: "制备全氟有机化合物的工艺", 《有机氟工业》 * |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105693463A (en) * | 2014-11-28 | 2016-06-22 | 浙江省化工研究院有限公司 | Method for preparing C2-C6 perfluoroalkane |
| CN109134186A (en) * | 2018-08-28 | 2019-01-04 | 苏州工业园区捷仕通医疗设备有限公司 | The raw materials for production and its continuous preparation method of liquid ventilation liquid and ophthalmologic operation material |
| CN110511111A (en) * | 2019-04-29 | 2019-11-29 | 苏州工业园区捷仕通医疗设备有限公司 | Gas exchanges dielectric fluid |
| CN112778077A (en) * | 2021-01-18 | 2021-05-11 | 福建德尔科技有限公司 | Micro-reactor based electronic stage C2F6Preparation method |
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Effective date of registration: 20190418 Address after: No. 55 Jinyan Road, Suzhou Industrial Park, Jiangsu Province Patentee after: Suzhou Industrial Park Jieshitong Medical Equipment Co., Ltd. Address before: 200040 5th Floor, 717 Huaian Road, Jing'an District, Shanghai Patentee before: Shanghai Huajie Eye Medical Equipment Co., Ltd. |
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