CN103288587B - A kind of preparation method of perfluoro alkane - Google Patents
A kind of preparation method of perfluoro alkane Download PDFInfo
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- CN103288587B CN103288587B CN201310194697.6A CN201310194697A CN103288587B CN 103288587 B CN103288587 B CN 103288587B CN 201310194697 A CN201310194697 A CN 201310194697A CN 103288587 B CN103288587 B CN 103288587B
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Abstract
The invention provides a kind of method preparing perfluoro alkane: be filled to by filler in reactor, fluoridize with fluorizating agent, maintaining inside reactor temperature is in 100-~ 300 DEG C; Joined in vaporizer by reaction raw materials and vaporize, controlling temperature in vaporizer is 130-150 DEG C, and wherein, described reaction raw materials is one or more in C5-C16 alkane and its partially fluorinated thing; With rare gas element, reaction raw materials steam is brought into reactor continuously; In reactor, pass into fluorizating agent continuously, react with the reaction raw materials steam passing into reactor continuously; Separating-purifying, obtains perfluoro alkane.Method provided by the invention is suitable for mass-producing continuous prodution, and reaction conditions is easy to control, and productive rate is high, and by product is few, the easy separating-purifying of reaction product, and 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 of lung chamber aeration liquid and ophthalmologic operation preparation.
Description
Technical field
The present invention relates to a kind of preparation method of perfluoro alkane, particularly relate 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.Cobaltic fluoride method needs cohalt difluoride first to fluoridize to be converted into cobaltic fluoride, and cobaltic fluoride is obtained by reacting the mixture containing PFO more in the reactor with octane; Cobaltic fluoride needs constantly regeneration, and temperature of reactor is difficult to control evenly, and amplify restricted, production can not be carried out continuously, is unsuitable for producing in enormous quantities.In addition, electrofluorination method synthesis PFO equipment is complicated, and it is high that condition controls difficulty, and by product is many, and yield is low, is generally no more than 15%.
Summary of the invention
The object of the invention is to overcome above-mentioned deficiency, provide a kind of method of perfluoro alkane, this method is suitable for mass-producing continuous prodution, and reaction conditions is easy to control, and productive rate is high, and by product is few, the easy separating-purifying of reaction product, and production process three-waste free discharge.
The invention provides a kind of method preparing perfluoro alkane, it is characterized in that, comprise the following steps:
Step 1, is filled to filler in reactor, fluoridizes with fluorizating agent, and maintaining inside reactor temperature is at 100-300 DEG C;
Step 2, joins reaction raw materials in vaporizer with the feed rate of 1-10L/h and vaporizes, and controlling temperature in vaporizer is 130-150 DEG C, and wherein, described reaction raw materials is one or more in the alkane of C5-C16 and its partially fluorinated thing;
Step 3, reaction raw materials steam step 2 obtained with rare gas element is brought into reactor continuously;
Step 4, passes into fluorizating agent continuously in reactor, reacts with the reaction raw materials steam passing into reactor continuously, and maintaining inside reactor temperature is at 100-300 DEG C;
Step 5, separating-purifying, obtains perfluoro alkane.
Wherein, described alkane can be branched alkane or normal alkane, is preferably normal alkane.
Preferably, described reaction raw materials is one or more in C6-C12 alkane and its partially fluorinated thing, is more preferably one or more in C8-C10 alkane and its partially fluorinated thing, is 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, copper and fluorochemical thereof, aluminium and fluorochemical, manganese and fluorochemical thereof.
Preferably, described basic metal is one or more in lithium, sodium, potassium, caesium.
Preferably, granularity >=100 order of described filler.
Preferably, described fluorizating agent is the gas mixture of pure fluorine gas or fluorine and rare gas element, and wherein, in gas mixture, the concentration of fluorine gas is not less than 5%(V/V), the best is 10%-80%, particularly optimum between 20%-40%.
Preferably, in step 3, the concentration of reaction raw materials steam in rare gas element is 1-60%(V/V), be more preferably 1-40%, be more preferably 1-20%.
Preferably, in step 4, pass into the mol ratio of fluorizating agent in reactor and hydrogen atom in the reaction raw materials passed in reactor at (1-2): 1.
Preferably, in step 4, temperature of reaction is 100-300 DEG C, is more preferably 180-280 DEG C.
Wherein, in step 4, reaction pressure can be negative pressure, normal pressure or malleation, is not particularly limited, preferably safer at atmospheric operation.
Preferably, in step 4, the reaction times characterized with reactant residence time in reactor, and range of choices is 5-30 second, general optional 5-20 second, was 5-15 second between optimal zone.
Preferably, in 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.
Present invention also offers a kind of lung chamber aeration liquid, comprise PFO prepared by aforesaid method.Other known lung chamber aeration liquids can also be comprised, such as perfluorodecalin etc.
Preferably, described lung chamber aeration liquid is made up of PFO.
Present invention also offers 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, the feed molar ratio of accurate control fluorizating agent and octane or partially fluorinated octane, temperature of reaction and reaction times, organic reactant can be made to fluoridize completely as far as possible, reduce the fracture of C-C key in molecule to greatest extent, improve the productive rate of target product, by product is few, the easy separating-purifying of reaction product.
Method provided by the invention is suitable for mass-producing continuous prodution, and reaction conditions is easy to control, and productive rate is high, and by product is few, the easy separating-purifying of reaction product, and 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 of lung chamber aeration liquid and ophthalmologic operation preparation.
Embodiment
Referring to specific embodiment, the present invention is further described, to understand the present invention better.
Reactor of the present invention can select tubular reactor, and material can be Monel metal, nickel, stainless steel, red copper or carbon steel etc.Basic metal, alkaline earth metal oxide, alkaline-earth metal fluoride, nickel and fluorochemical thereof, cobalt and fluorochemical, copper and fluorochemical thereof, aluminium and fluorochemical, manganese and fluorochemical thereof is filled in pipe, if initial weighting material is not fluorochemical entirely, need to fluoridize with the gas mixture of fluorine gas or fluorine passing into before reactant reacts, make weighting material be converted into fluorochemical completely.Weighting material loads reactor with particulate state, and granularity is more than 100 orders.
embodiment 1
In the Monel metal reactor of internal diameter 80mm, long 1000mm, fill the spherical alumina that diameter is Φ 3mm.Reactor is heated to 300 DEG C, passes into 50% fluoro-50% nitrogen mixed gas and fluoridizes, make aluminum oxide be converted into aluminum fluoride completely.Then make temperature of reactor maintain 200 DEG C, pass into 20% fluoro-nitrogen mixed gas continuously in fluorine gas and octane mol ratio 20:1 ratio and 10% octane-nitrogen mixed gas reacts, control 5 seconds residence time.10 as a child the reaction product collected to be neutralized to pH value with 20% potassium hydroxide aqueous solution be neutral, leave standstill, organic phase deionized water wash is got three times after layering, rectifying separation is carried out after separating organic phase anhydrous sodium sulfate drying, get boiling point 100-105 DEG C cut, obtain 1000 grams of PFO, purity 98%, productive rate about 70%.
embodiment 2
With with embodiment 1 identical device.Temperature of reactor maintains 260 DEG C, passes into 20% fluoro-nitrogen mixed gas continuously and 20% octane-nitrogen mixed gas reacts in fluorine gas and octane mol ratio 20:1 ratio, controls 10 seconds residence time.10 as a child the reaction product collected to be neutralized to pH value with 20% potassium hydroxide aqueous solution be neutral, leave standstill, organic phase deionized water wash is got three times after layering, rectifying separation is carried out after separating organic phase anhydrous sodium sulfate drying, get boiling point 100-105 DEG C cut, obtain 1500 grams of PFO, purity 98.5%, productive rate about 75%.
embodiment 3
With with embodiment 1 identical device.Temperature of reactor maintains 280 DEG C, passes into 20% fluoro-nitrogen mixed gas continuously and 15% octane-nitrogen mixed gas reacts in fluorine gas and octane mol ratio 25:1 ratio, controls 10 seconds residence time.10 as a child the reaction product collected to be neutralized to pH value with 20% potassium hydroxide aqueous solution be neutral, leave standstill, organic phase deionized water wash is got three times after layering, rectifying separation is carried out after separating organic phase anhydrous sodium sulfate drying, get boiling point 100-105 DEG C cut, obtain 1600 grams of 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, and fluorine gas and octane charged molar ratio are 22:1, and fluorine gas uses with 20% fluoro-nitrogen mixed gas, and octane uses with 20% octane-nitrogen mixture.Control 10 seconds residence time.10 as a child the reaction product collected to be neutralized to pH value with 20% potassium hydroxide aqueous solution be neutral, leave standstill, organic phase deionized water wash is got three times after layering, rectifying separation is carried out after separating organic phase anhydrous sodium sulfate drying, get boiling point 100-105 DEG C cut, obtain 1600 grams of PFO, purity 98%, productive rate about 75%.
Be described in detail specific embodiments of the invention above, 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, equalization conversion done without departing from the spirit and scope of the invention and amendment, all should contain within the scope of the invention.
Claims (1)
1. prepare the method for perfluoro alkane for one kind, it is characterized in that, comprise the following steps: at internal diameter 80mm, in the Monel metal reactor of long 1000mm, fill the spherical alumina that diameter is Φ 3mm, reactor is heated to 300 DEG C, pass into 50% fluoro-50% nitrogen mixed gas to fluoridize, aluminum oxide is made to be converted into aluminum fluoride completely, then temperature of reactor is made to maintain 200 DEG C, 20% fluoro-nitrogen mixed gas is passed into continuously and 10% octane-nitrogen mixed gas reacts in fluorine gas and octane mol ratio 20:1 ratio, control 5 seconds residence time, it is neutral for after 10 hours, the reaction product collected being neutralized to pH value with 20% potassium hydroxide aqueous solution, leave standstill, organic phase deionized water wash is got three times after layering, rectifying separation is carried out after separating organic phase anhydrous sodium sulfate drying, get boiling point 100-105 DEG C cut, obtain 1000 grams of PFO, purity 98%, productive rate 70%.
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| 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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| Publication number | Priority date | Publication date | Assignee | Title |
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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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