CN109134186A - The raw materials for production and its continuous preparation method of liquid ventilation liquid and ophthalmologic operation material - Google Patents
The raw materials for production and its continuous preparation method of liquid ventilation liquid and ophthalmologic operation material Download PDFInfo
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- CN109134186A CN109134186A CN201810987241.8A CN201810987241A CN109134186A CN 109134186 A CN109134186 A CN 109134186A CN 201810987241 A CN201810987241 A CN 201810987241A CN 109134186 A CN109134186 A CN 109134186A
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C17/00—Preparation of halogenated hydrocarbons
- C07C17/093—Preparation of halogenated hydrocarbons by replacement by halogens
- C07C17/10—Preparation of halogenated hydrocarbons by replacement by halogens of hydrogen atoms
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Abstract
The present invention provides the raw materials for production and its continuous preparation method of liquid ventilation liquid and ophthalmologic operation material, including fluorine gas and octane organic matter, the fluorine gas and octane organic matter molar ratio are between 20:1~25:1, the fluorine gas is the gaseous mixture of pure fluorine or fluorine gas and inert gas, and the concentration of fluorine gas is not less than 10%；The octane organic matter is the mixture of octane, octane homologue or octane organic matter and inert gas.The present invention is suitable for scale continuous production, and reaction condition is easily controllable, and yield is high, and by-product is few, and reaction product can be easily separated purification, and production process three-waste free discharge.The perfluorooctane that purity >=99% can be prepared using the method for the invention can be used as the raw materials for production of liquid ventilation liquid and ophthalmologic operation preparation.
Description
Technical field
The present invention relates to perfluorooctane preparation method technical fields, in particular to liquid ventilation liquid and ophthalmologic operation material
Raw materials for production and its continuous preparation method.
Background technique
The preparation method of previous perfluorooctane has cobalt trifluoride fluoride process and electrofluorination method.Cobalt trifluoride method need by
Cohalt difluoride is first fluorinated and is converted into cobalt trifluoride, and cobalt trifluoride reacts to obtain containing perfluorooctane with octane in the reactor again
Mixture；Cobalt trifluoride need it is constantly regenerating, temperature of reactor be difficult to control uniformly, amplification is restricted, production cannot continuously into
Row, is unsuitable for producing in enormous quantities.In addition, the device is complicated for electrofluorination method synthesis perfluorooctane, condition controls difficulty height, by-product
More, yield is low, is usually no more than 15%.
Open (bulletin) number: the patent of CN104926597A discloses a kind of preparation method of perfluorooctane, including following
Step: (1) catalyst filling in reactor carries out fluorination treatment with fluorization agent at high temperature；(2) vaporizer is added in octane
To obtain octane steam, carburettor temperature is controlled between 100~150 DEG C；(3) inert gas is passed through vaporizer to described pungent
Alkane steam is diluted, and octane Steam dilution gaseous mixture is continuously passed through reactor and fluorization agent carries out fluorination substitution reaction；(4)
By reaction product by alkali cleaning, washing, rectification and purification, perfluorooctane is obtained；Perfluorooctane low yield, purity made from the patent
Also to be improved.
The invention proposes a kind of method for preparing perfluorooctane, the method is suitable for scale continuous production, reacts item
Part is easily controllable, and yield is high, and by-product is few, and reaction product can be easily separated purification.Production process three-waste free discharge.
Summary of the invention
In order to overcome the drawbacks of the prior art, the present invention provides the raw materials for production of liquid ventilation liquid and ophthalmologic operation material
And its continuous preparation method.
To achieve the goals above, the present invention the following technical schemes are provided:
Octane and its homologue are contacted with simple substance fluoride, and substitution reaction occurs for the hydrogen atom in fluorine atom and organic molecule, finally
Obtain perfluorinated or partially fluorinated product.Degree of fluorination depends on the control of reaction condition.The present invention is using simple substance fluoride or its is dilute
Outgassing body is accurate to control fluorization agent and the feed molar ratio of octane or partially fluorinated octane, reaction temperature and react as fluorization agent
Time is fluorinated organic reactant as far as possible completely, while reducing the fracture of intramolecular C-C key to greatest extent, improves target and produces
The yield of object perfluorooctane.
The raw materials for production of liquid ventilation liquid and ophthalmologic operation material, including fluorine gas and octane organic matter, the fluorine gas with
For octane organic matter molar ratio between 20:1~25:1, the fluorine gas is the gaseous mixture of pure fluorine or fluorine gas and inert gas, fluorine gas
Concentration be not less than 10%；The octane organic matter is the mixing of octane, octane homologue or octane organic matter and inert gas
Object.
Preferably, when the octane uses octane homologue, fluorine gas and octane molar ratio are between 10:1~20:1.
Preferably, the concentration of fluorine gas is between 10%~60%, 35% or so in the gaseous mixture of the fluorine gas and inert gas
It is optimal.
The continuous preparation method of the raw materials for production of liquid ventilation liquid and ophthalmologic operation material, comprising the following steps:
(1) filler will be filled in reactor, is first fluorinated with fluorine gas, maintain inside reactor temperature 120~280 DEG C it
Between；
(2) reaction raw materials are controlled into 1~10L/h of charging rate by feeder and vaporizer is added, control carburettor temperature 120
~140 DEG C, raw material is made to be unlikely to exist in liquid form in vaporizer；
(3) it is passed through vaporizer with nitrogen, makes reaction raw materials steam between the concentration 10%~40% in dilute gas mixture, by vapour
The reaction raw materials Steam dilution of change continuously brings fluorination reactor into, and maintaining inside reactor temperature is at 100-280 DEG C；
(4) it is continuously passed through fluorization agent into reactor, is reacted with the reaction raw materials steam for being continuously passed through reactor, reaction temperature
For degree between 200~260 DEG C, reaction pressure is negative pressure or normal pressure or positive pressure, is not particularly limited, preferably compares in atmospheric operation
Safety；Reaction time, the residence time in reactor characterized with reactant, and optional range is 5~15 seconds；
(5) reaction product is obtained into target product by alkali cleaning, washing, rectification and purification.
Preferably, the reactor is tubular reactor, and material is monel metal, nickel, stainless steel, red copper or carbon steel；
Pipe inner stuffing is the metals such as alkali metal, alkaline earth oxide or fluoride and nickel, cobalt, copper, aluminium, manganese and its fluoride
One of or it is a variety of, the filler with graininess be packed into reactor, granularity is more than 140 mesh.
Preferably, the starting filler not fluoride, need before being passed through reactant and being reacted with fluorine gas or
Fluorine-containing gaseous mixture is fluorinated, and filler is made to be fully converted to fluoride.
Preferably, step (1) the reactor interior reaction temperature is 180~250 DEG C.
Preferably, in the step (2) reaction raw materials by feeder be added the charging rate control of vaporizer 2~
8L/h。
Preferably, the step (2) and reaction raw materials in step (3) are one in C5-C16 alkane and its partially fluorinated object
Kind is a variety of；Concentration range of the reaction raw materials steam in nitrogen is 1~20%(V/V).
Preferably, fluorization agent can be pure fluorine gas in the step (4), can also be that fluorine and nitrogen, helium, argon gas etc. are lazy
Property gas gaseous mixture, fluorine gas in gaseous mixture concentration be not less than 5% (V/V), continuous feeding.
Beneficial effect of the invention is that being suitable for scale continuous production, reaction condition is easily controllable, yield
Height, by-product is few, and reaction product can be easily separated purification, and production process three-waste free discharge.It can be made using the method for the invention
The perfluorooctane of standby purity >=99%, can be used as the raw materials for production of liquid ventilation liquid and ophthalmologic operation preparation.
Specific embodiment
The preferred embodiments of the present invention will be described in detail below so that advantages and features of the invention can be easier to by
It will be appreciated by those skilled in the art that so as to make a clearer definition of the protection scope of the present invention.
Embodiment one
Internal diameter 80mm, long 1000mm monel metal reactor in, filling diameter be Φ 3mm spherical alumina.Reaction
Device is heated to 250 DEG C, is passed through 50% fluoro- 50% nitrogen mixed gas and is fluorinated, aluminium oxide is made to be fully converted to aluminum fluoride.Then make anti-
It answers device temperature to maintain 200 DEG C, is continuously passed through 20% fluoro- nitrogen mixed gas and 10% pungent in fluorine gas and octane molar ratio 20:1 ratio
Alkane-nitrogen mixed gas is reacted, and is controlled the residence time 5 seconds.10 as a child by 20% potassium hydroxide water of the reaction product being collected into
Solution is neutralized to pH value as neutrality, stands, takes organic phase to be washed with deionized three times after layering, separate organic phase with anhydrous sulphur
Rectifying separation is carried out after sour sodium is dry, 101~104 DEG C of fractions of boiling point is taken, obtains 1000 grams of perfluorooctane, purity 99%, yield is about
85%。
Embodiment two
With equipment same as Example 1.Temperature of reactor maintains 260 DEG C, continuous in fluorine gas and octane molar ratio 20:1 ratio
It is passed through 20% fluoro- nitrogen mixed gas and 20% octane-nitrogen mixed gas is reacted, control the residence time 10 seconds.10 will as a child collect
To reaction product with 20% potassium hydroxide aqueous solution be neutralized to pH value be it is neutral, stand, organic phase deionized water taken after layering
Washing three times, carries out rectifying separation after separating organic phase anhydrous sodium sulfate drying, takes 101~104 DEG C of fractions of boiling point, obtain 1500
Gram perfluorooctane, purity 99.5%, yield about 85%.
Embodiment three
With equipment same as Example 1.Temperature of reactor maintains 280 DEG C, continuous in fluorine gas and octane molar ratio 25:1 ratio
It is passed through 20% fluoro- nitrogen mixed gas and 15% octane-nitrogen mixed gas is reacted, control the residence time 10 seconds.10 will as a child collect
To reaction product with 20% potassium hydroxide aqueous solution be neutralized to pH value be it is neutral, stand, organic phase deionized water taken after layering
Washing three times, carries out rectifying separation after separating organic phase anhydrous sodium sulfate drying, takes 101~104 DEG C of fractions of boiling point, obtain 1600
Gram perfluorooctane, purity 99%, yield about 80%.
Example IV
With equipment same as Example 1 and reaction condition, aluminium oxide is changed to cobalt oxide, fluorine gas is with octane charged molar ratio
22:1, fluorine gas are used with 20% fluoro- nitrogen mixed gas, and octane is with the use of 20% octane-nitrogen mixture.The control residence time 10 seconds.
10 as a child by the reaction product being collected into 20% potassium hydroxide aqueous solution be neutralized to pH value be it is neutral, stand, taken after layering
Machine is mutually washed with deionized three times, separate organic phase with anhydrous sodium sulfate it is dry after carry out rectifying separation, take boiling point 101~
104 DEG C of fractions obtain 1600 grams of perfluorooctane, purity 99%, yield about 85%.
The above description is merely a specific embodiment, but scope of protection of the present invention is not limited thereto, any
Those skilled in the art within the technical scope disclosed by the invention, can without the variation that creative work is expected or
Replacement, should be covered by the protection scope of the present invention.Therefore, protection scope of the present invention should be limited with claims
Subject to fixed protection scope.
Claims (10)
1. the raw materials for production of liquid ventilation liquid and ophthalmologic operation material, which is characterized in that including fluorine gas and octane organic matter, institute
Fluorine gas and octane organic matter molar ratio are stated between 20:1~25:1, the fluorine gas is the mixing of pure fluorine or fluorine gas and inert gas
The concentration of gas, fluorine gas is not less than 10%；The octane organic matter is octane, octane homologue or octane organic matter and inert gas
Mixture.
2. the raw materials for production of liquid ventilation liquid according to claim 1 and ophthalmologic operation material, which is characterized in that described
When octane uses octane homologue, fluorine gas and octane molar ratio are between 10:1~20:1.
3. the raw materials for production of liquid ventilation liquid according to claim 1 and ophthalmologic operation material, which is characterized in that described
In the gaseous mixture of fluorine gas and inert gas the concentration of fluorine gas be 10%~60% between, it is optimal 35% or so.
4. the continuous preparation method of the raw materials for production of liquid ventilation liquid and ophthalmologic operation material, which is characterized in that including following
Step:
(1) filler will be filled in reactor, is first fluorinated with fluorine gas, maintain inside reactor temperature 120~280 DEG C it
Between；
(2) reaction raw materials are controlled into 1~10L/h of charging rate by feeder and vaporizer is added, control carburettor temperature 120
~140 DEG C, raw material is made to be unlikely to exist in liquid form in vaporizer；
(3) it is passed through vaporizer with nitrogen, makes reaction raw materials steam between the concentration 10%~40% in dilute gas mixture, it will
The reaction raw materials Steam dilution of vaporization continuously brings fluorination reactor into, and maintaining inside reactor temperature is at 100-280 DEG C；
(4) it is continuously passed through fluorization agent into reactor, is reacted with the reaction raw materials steam for being continuously passed through reactor, reaction temperature
For degree between 200~260 DEG C, the reaction time is 5~15 seconds；
(5) reaction product is obtained into target product by alkali cleaning, washing, rectification and purification.
5. the continuous preparation method of the raw materials for production of liquid ventilation liquid according to claim 4 and ophthalmologic operation material,
It is characterized in that, the reactor is tubular reactor, material is monel metal, nickel, stainless steel, red copper or carbon steel；In pipe
Filler is in the metals such as alkali metal, alkaline earth oxide or fluoride and nickel, cobalt, copper, aluminium, manganese and its fluoride
One or more, the filler is packed into reactor with graininess, and granularity is more than 140 mesh.
6. the continuous preparation method of the raw materials for production of liquid ventilation liquid according to claim 5 and ophthalmologic operation material,
It is characterized in that, the starting filler not fluoride, needs before being passed through reactant and being reacted with fluorine gas or fluorine-containing
Gaseous mixture be fluorinated, so that filler is fully converted to fluoride.
7. the continuous preparation method of the raw materials for production of liquid ventilation liquid according to claim 4 and ophthalmologic operation material,
It is characterized in that, step (1) the reactor interior reaction temperature is 180~250 DEG C.
8. the continuous preparation method of the raw materials for production of liquid ventilation liquid according to claim 4 and ophthalmologic operation material,
It is characterized in that, reaction raw materials are controlled by the charging rate that vaporizer is added in feeder in 2~8L/h in the step (2).
9. the continuous preparation method of the raw materials for production of liquid ventilation liquid according to claim 4 and ophthalmologic operation material,
It is characterized in that, in the step (2) and step (3) reaction raw materials be one of C5-C16 alkane and its partially fluorinated object or
It is a variety of；Concentration range of the reaction raw materials steam in nitrogen is 1~20% (V/V).
10. the continuous preparation method of the raw materials for production of liquid ventilation liquid according to claim 4 and ophthalmologic operation material,
It is characterized in that, fluorization agent can be pure fluorine gas in the step (4), it can also be the indifferent gas such as fluorine and nitrogen, helium, argon gas
The gaseous mixture of body, fluorine gas concentration in gaseous mixture are not less than 5% (V/V), continuous feeding.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201810987241.8A CN109134186A (en) | 2018-08-28 | 2018-08-28 | The raw materials for production and its continuous preparation method of liquid ventilation liquid and ophthalmologic operation material |
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| CN201810987241.8A CN109134186A (en) | 2018-08-28 | 2018-08-28 | The raw materials for production and its continuous preparation method of liquid ventilation liquid and ophthalmologic operation material |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103288587A (en) * | 2013-05-23 | 2013-09-11 | 上海华捷视医疗设备有限公司 | Preparation method of perfluoroalkane |
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- 2018-08-28 CN CN201810987241.8A patent/CN109134186A/en active Pending
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103288587A (en) * | 2013-05-23 | 2013-09-11 | 上海华捷视医疗设备有限公司 | Preparation method of perfluoroalkane |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
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