CN104926597A - Preparation method of pulmonic cavity ventilating liquid - Google Patents
Preparation method of pulmonic cavity ventilating liquid Download PDFInfo
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- CN104926597A CN104926597A CN201410099868.1A CN201410099868A CN104926597A CN 104926597 A CN104926597 A CN 104926597A CN 201410099868 A CN201410099868 A CN 201410099868A CN 104926597 A CN104926597 A CN 104926597A
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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
The present invention relates to the preparation method of a kind of lung chamber aeration liquid, be specifically related to a kind of preparation method that can be used as the PFO of lung chamber aeration liquid and manufacture ophthalmic instruments.
Background technology
PFO is as the key component of a kind of lung chamber aeration liquid, and its purity directly affects the effect of lung chamber aeration liquid treatment pulmonary disorder.The preparation method of PFO had cobaltic fluoride fluorination method, electrofluorination method and simple substance fluoride direct fluorination in the past.Cobaltic fluoride fluorination method needs cohalt difluoride or cobalt oxide to react with fluorine gas to be in advance 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.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 20%.Simple substance fluoride direct fluorination needs element fluorine, and element fluorine transport is very difficult, and fluorine equipment processed is complicated on the spot, and operation easier is large, and the easy chain rupture of reactant causes by product many, and yield is not high; And fluorine gas production is subject to strict regulation management and control, does not obtain production permit easily.Therefore, need a kind of safety of research, efficiently PFO preparation method, can scaleable, easily realize producing.
Summary of the invention
One aspect of the present invention provides a kind of preparation method of PFO, it is characterized in that comprising the following steps:
(1) catalyst filling in reactor, at high temperature carries out fluoridation with fluorizating agent;
(2) octane is added vaporizer to obtain octane steam, control carburettor temperature between 100 ~ 150 DEG C;
(3) rare gas element is passed into vaporizer to dilute described octane steam, octane Steam dilution gas mixture is passed into reactor continuously and fluorizating agent carries out fluoridizing substitution reaction;
(4) reaction product is passed through alkali cleaning, washing, rectification and purification, obtain PFO.
Preparation method as above, wherein, described fluoridation temperature is 300 DEG C.
Preparation method as above, wherein, described catalyzer is selected from basic metal, alkaline-earth metal fluoride or is made up of one or more of the metals such as nickel, cobalt, copper, aluminium, manganese or its oxide compound or fluorochemical.
Preparation method as above, wherein, described fluorizating agent is pure nitrogen trifluoride or nitrogen trifluoride gas mixture.
Preparation method as above, wherein, described nitrogen trifluoride and octane steam charged molar ratio scope are between 15:1 ~ 50:1.
Preparation method as above, wherein, described nitrogen trifluoride gas mixture is the gas mixture that trifluoro changes nitrogen and rare gas element entirely, and nitrogen trifluoride concentration range in gas mixture is 20% ~ 80%.
Preparation method as above, wherein, the concentration range of octane steam in described octane Steam dilution gas mixture is 5% ~ 50%.
Preparation method as above, wherein, described in fluoridize substitution reaction temperature and control between 150 ~ 350 DEG C.
Preparation method as above, wherein, described PFO purity is not less than 98%.
The present invention is that PFO preparation method as above prepared is as lung chamber aeration liquid or for the manufacture of ophthalmic instruments on the other hand.
Compared with the traditional method of preparation PFO, present invention employs the method that nitrogen trifluoride fluoridizes substitution reaction as fluorizating agent and octane under the effect of catalyzer and prepare PFO.The inventive method nitrogen trifluoride raw material used is easy to get, and facility investment is few, and reaction conditions is easy to control, and productive rate is high, and by product is few, the easy separating-purifying of reaction product, production process three-waste free discharge, operational safety, is suitable for all size scale interval or continuous prodution.
Embodiment
The preparation principle of PFO is as follows: in the reactor, and octane gas and fluorizating agent nitrogen trifluoride are fluoridized substitution reaction and obtained the Perfluorinate product of octane or partially fluorinated pair under the effect of catalyzer.For improving its degree of fluorination, improving the purity of PFO, need control reaction conditions.By controlling the feed molar ratio of fluorizating agent and octane gas, temperature of reaction and the residence time of reaction mixture in reactor, octane gas is made to fluoridize completely as far as possible, reduce the fracture of C-C key in octane molecular simultaneously to greatest extent, thus improve the productive rate of target product PFO.
In the present embodiment, described reactor can be tubular reactor, and material is Monel metal, nickel, stainless steel, red copper or carbon steel.The catalyzer of filling in pipe can be selected from basic metal, alkaline-earth metal fluoride or be made up of one or more of the metals such as nickel, cobalt, copper, aluminium, manganese or its oxide compound or fluorochemical.
In some embodiments, the preparation process of PFO is as follows:
Step one: catalyzer loads reactor with particulate state, the granularity of this granules of catalyst can more than 100 orders.Before passing into reactant to reactor, first between high temperature is as 150 ~ 300 DEG C, fluoridation is carried out to catalyzer as the gas mixture of nitrogen, helium or argon gas with fluorizating agent nitrogen trifluoride or nitrogen trifluoride and rare gas element, make catalytic conversion be fluorochemical.
Step 2: add in vaporizer by octane liquid, controls carburettor temperature to generate octane steam between 100 ~ 150 DEG C, by rare gas element as nitrogen, helium, argon gas and octane steam pass into mixing tank dilution mixture in proportion.The concentration of octane steam in dilute gas mixture is between 5% ~ 50%, and the best is between 10% ~ 30%.
Step 3: pass into the pure nitrogen trifluoride of fluorizating agent or nitrogen trifluoride gas mixture in reactor continuously, nitrogen trifluoride gas mixture can be the gas mixture of the rare gas element such as nitrogen trifluoride and nitrogen, helium, argon gas, in mixed gas, the concentration of nitrogen trifluoride is not less than 20%, and the best is between 50% ~ 80%.
Step 4: octane Steam dilution gas mixture is passed in reactor continuously and carries out catalytic fluorination reaction with fluorizating agent nitrogen trifluoride, pass into speed to control nitrogen trifluoride and octane mol ratio between 15:1 ~ 50:1 by what control fluorizating agent and/or octane dilute gas mixture, the best is between 20:1 ~ 40:1.Reaction times characterized with reactant residence time in reactor, and the scope of this reaction time can be 3 ~ 60 seconds, and most optimal retention time is 5 ~ 10 seconds.
Fluoridizing substitution reaction temperature controls between 150 ~ 350 DEG C, and optimal reaction temperature is between 200 ~ 300 DEG C.Reaction pressure is negative pressure or normal pressure or malleation, is not particularly limited, preferably at atmospheric operation.
Step 5: by reaction product by alkali cleaning, washing, rectification and purification, obtain PFO.
Above step is not limited to present embodiment, in other embodiments, the enforcement of reactions steps adjusts according to practical situation, such as, above step can be carried out according to different order, step and another step can synchronously be carried out, and can add the step that some are conducive to improving speed of reaction or improving product purity according to actual needs.According to the adjustment of step, reaction vessel can carry out corresponding increase or reduce accordingly.
embodiment one:
In the Monel metal reactor that internal diameter is 50mm, long 1000mm, fill the spherical aluminum fluoride that diameter is 3mm.Reactor is heated to 300 DEG C, passes into pure gas of nitrogen trifluoride and carries out fluoridation.Then make temperature of reactor maintain 150 DEG C, octane carburettor temperature maintains 100 DEG C, in nitrogen trifluoride and octane mol ratio 15:1 ratio passes into 20% nitrogen trifluoride-nitrogen mixed gas continuously and 5% octane-nitrogen mixed gas reacts, controls 60 seconds residence time.Measure when pure octane reaches 500 grams by the amount of reactor and stop feeding in raw material.It is neutral that the reaction product collected is 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 103 ~ 105 DEG C of cuts, obtain 1152 grams of PFO, purity 98%, collects rate about 60% by adding octane.
embodiment two:
With with embodiment 1 identical device.Temperature of reactor maintains 200 DEG C, in nitrogen trifluoride and octane mol ratio 30:1 ratio passes into 50% nitrogen trifluoride-nitrogen mixed gas continuously and 20% octane-nitrogen mixed gas reacts, controls 10 seconds residence time.Measure when pure octane reaches 500 grams by the amount of reactor and stop feeding in raw material.It is neutral that the reaction product collected is 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 103 ~ 105 DEG C of cuts, obtain 1248 grams of PFO, purity 99%, collects rate about 65% by adding octane.
embodiment three:
With with embodiment 1 identical device.Temperature of reactor maintains 300 DEG C, in nitrogen trifluoride and octane mol ratio 50:1 ratio passes into 80% nitrogen trifluoride-nitrogen mixed gas continuously and 50% octane-nitrogen mixed gas reacts, controls 3 seconds residence time.Measure when pure octane reaches 500 grams by the amount of reactor and stop feeding in raw material.It is neutral that the reaction product collected is 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 103 ~ 105 DEG C of cuts, obtain 1440 grams of PFO, purity 99%, collects rate about 75% by adding octane.
embodiment four:
In embodiment 1 same reactor, fill the spherical cobalt oxide that diameter is 3mm.Reactor is heated to 300 DEG C, passes into 50% nitrogen trifluoride-50% nitrogen mixed gas and activates.Then make temperature of reactor maintain 350 DEG C, octane carburettor temperature maintains 150 DEG C, in nitrogen trifluoride and octane mol ratio 30:1 ratio passes into pure nitrogen trifluoride continuously and 20% octane-nitrogen mixed gas reacts, controls 5 seconds residence time.Measure when pure octane reaches 500 grams by the amount of reactor and stop feeding in raw material.It is neutral that the reaction product collected is 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 103 ~ 105 DEG C of cuts, obtain 1537 grams of PFO, purity 99%, collects rate about 80% by adding octane.
By PFO prepared by above embodiment, its purity is not less than 98%.In some embodiments, can be used as lung chamber aeration liquid by the PFO that as above preparation method obtains or for the manufacture of ophthalmic instruments.
Although describe the present invention in conjunction with specific embodiment, those skilled in the art will appreciate that and can make many amendments and modification to the present invention.Therefore, recognize, the intention of claims is to be encompassed in all such modifications in true spirit of the present invention and scope and modification.
Claims (10)
1. a preparation method for PFO, is characterized in that comprising the following steps:
(1) catalyst filling in reactor, at high temperature carries out fluoridation with fluorizating agent;
(2) octane is added vaporizer to obtain octane steam, control carburettor temperature between 100 ~ 150 DEG C;
(3) rare gas element is passed into vaporizer to dilute described octane steam, octane Steam dilution gas mixture is passed into reactor continuously and fluorizating agent carries out fluoridizing substitution reaction;
(4) reaction product is passed through alkali cleaning, washing, rectification and purification, obtain PFO.
2. preparation method as claimed in claim 1, wherein, described fluoridation temperature is 300 DEG C.
3. preparation method as claimed in claim 1, wherein, described catalyzer is selected from basic metal, alkaline-earth metal fluoride or is made up of one or more of the metals such as nickel, cobalt, copper, aluminium, manganese or its oxide compound or fluorochemical.
4. preparation method as claimed in claim 1, wherein, described fluorizating agent is pure nitrogen trifluoride or nitrogen trifluoride gas mixture.
5. preparation method as claimed in claim 4, wherein, described nitrogen trifluoride and octane steam charged molar ratio scope are between 15:1 ~ 50:1.
6. preparation method as claimed in claim 4, wherein, described nitrogen trifluoride gas mixture is the gas mixture that trifluoro changes nitrogen and rare gas element entirely, and nitrogen trifluoride concentration range in gas mixture is 20% ~ 80%.
7. preparation method as claimed in claim 1, wherein, the concentration range of octane steam in described octane Steam dilution gas mixture is 5% ~ 50%.
8. preparation method as claimed in claim 1, wherein, described in fluoridize substitution reaction temperature and control between 150 ~ 350 DEG C.
9. preparation method as claimed in claim 1, wherein, described PFO purity is not less than 98%.
10. PFO preparation method as claimed in claim 1 prepared is as lung chamber aeration liquid or for the manufacture of ophthalmic instruments.
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| CN201410099868.1A CN104926597A (en) | 2014-03-18 | 2014-03-18 | Preparation method of pulmonic cavity ventilating liquid |
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105461507A (en) * | 2015-11-19 | 2016-04-06 | 中国船舶重工集团公司第七一八研究所 | A method of preparing hexafluoroethane at high temperature |
| CN107098790A (en) * | 2017-06-05 | 2017-08-29 | 广东华特气体股份有限公司 | A kind of method for preparing high-purity octafluoropropane |
| 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 |
| CN110550996A (en) * | 2019-04-29 | 2019-12-10 | 苏州工业园区捷仕通医疗设备有限公司 | Preparation method of novel lung cavity ventilation liquid |
| CN112079757A (en) * | 2020-10-20 | 2020-12-15 | 山东重山光电材料股份有限公司 | Preparation and purification method of trifluoromethyl sulfur pentafluoride |
| CN113200868A (en) * | 2021-05-21 | 2021-08-03 | 江西国化实业有限公司 | Process for producing and preparing perfluorotributylamine |
-
2014
- 2014-03-18 CN CN201410099868.1A patent/CN104926597A/en active Pending
Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105461507A (en) * | 2015-11-19 | 2016-04-06 | 中国船舶重工集团公司第七一八研究所 | A method of preparing hexafluoroethane at high temperature |
| CN105461507B (en) * | 2015-11-19 | 2018-03-23 | 中国船舶重工集团公司第七一八研究所 | A kind of method that perfluoroethane is prepared under high temperature |
| CN107098790A (en) * | 2017-06-05 | 2017-08-29 | 广东华特气体股份有限公司 | A kind of method for preparing high-purity octafluoropropane |
| 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 |
| CN110550996A (en) * | 2019-04-29 | 2019-12-10 | 苏州工业园区捷仕通医疗设备有限公司 | Preparation method of novel lung cavity ventilation liquid |
| CN110550996B (en) * | 2019-04-29 | 2022-04-05 | 苏州工业园区捷仕通医疗设备有限公司 | Preparation method of novel lung cavity ventilation liquid |
| CN112079757A (en) * | 2020-10-20 | 2020-12-15 | 山东重山光电材料股份有限公司 | Preparation and purification method of trifluoromethyl sulfur pentafluoride |
| CN113200868A (en) * | 2021-05-21 | 2021-08-03 | 江西国化实业有限公司 | Process for producing and preparing perfluorotributylamine |
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Application publication date: 20150923 |