CN1085536A - The separation method of pentafluoride ethane and five fluorine chloric ethane azeotropic mixtures and five fluorine chloric ethanes - Google Patents
The separation method of pentafluoride ethane and five fluorine chloric ethane azeotropic mixtures and five fluorine chloric ethanes Download PDFInfo
- Publication number
- CN1085536A CN1085536A CN 93107029 CN93107029A CN1085536A CN 1085536 A CN1085536 A CN 1085536A CN 93107029 CN93107029 CN 93107029 CN 93107029 A CN93107029 A CN 93107029A CN 1085536 A CN1085536 A CN 1085536A
- Authority
- CN
- China
- Prior art keywords
- mixture
- ethane
- fluorine
- ethanes
- fluorine chloric
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
Images
Classifications
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C19/00—Acyclic saturated compounds containing halogen atoms
- C07C19/08—Acyclic saturated compounds containing halogen atoms containing fluorine
- C07C19/10—Acyclic saturated compounds containing halogen atoms containing fluorine and chlorine
- C07C19/12—Acyclic saturated compounds containing halogen atoms containing fluorine and chlorine having two carbon atoms
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C17/00—Preparation of halogenated hydrocarbons
- C07C17/38—Separation; Purification; Stabilisation; Use of additives
- C07C17/383—Separation; Purification; Stabilisation; Use of additives by distillation
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C19/00—Acyclic saturated compounds containing halogen atoms
- C07C19/08—Acyclic saturated compounds containing halogen atoms containing fluorine
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
By distillation, heat up in a steamer the azeotropic mixture of pentafluoride ethane and five fluorine chloric ethanes, thereby from the mixture that contains pentafluoride ethane and five fluorine chloric ethanes, separate five fluorine chloric ethanes effectively the mixture of pentafluoride ethane and five fluorine chloric ethanes.
Description
The present invention relates to the azeotropic mixture of pentafluoride ethane (hereinafter referred to as R-125) and five fluorine chloric ethanes (hereinafter referred to as R-115), and by the method for separating R-115 in the generation mixture that contains R-125 and R-115.
R-125 mainly is used as the alternative refrigerant of chloro methylene fluoride.
Usually, be chlorination carbon and hydrogen fluoride (HF) reaction that utilizes zellon or the like, make R-125.But at this moment, often be difficult to remove and pay product R-115, and the latter is a kind of material that can destroy ozone.By the end of at present, do not find in the literature as yet to separate the record of the method for R-115 about from the generation mixture that contains R-125 and R-115.
The inventor is to having been carried out research repeatedly by the method for removing R-115 in the generation mixture that contains R-125 and R-115, it found that the minimum boiling point azcotrope that can form R-125 and R-115, thereby has finished the present invention.When in by the generation mixture that contains R-125 and R-115, removing R-115, if the technique of backflow in the use distillation procedure can therefrom be separated this azeotropic mixture effectively.
Therefore, first importance of the present invention has provided the azeotropic mixture of R-125 and R-115.The boiling point of R-125 under standard pressure is-48.5 ℃, and the boiling point of R-115 under standard pressure is-38.7 ℃.Because the boiling point of this azeotropic mixture under standard pressure is approximately-55 ℃, thereby can constitute minimum azeotrope.At this moment constituting of azeotrope, R-125 is about 85mol%, R-115 is about 15mol%.And under other pressure condition, such as at 10Kg/cm
2Under the absolute pressure, its boiling point is approximately 11.5 ℃, and the constituting of azeotrope, R-125 is about 93mol%, R-115 is about 7mol%.
Second importance of the present invention, provide the method for separating R-115 in a kind of mixture by R-125 and R-115, it is characterized in that by distillation R-125 and R-115 mixture, remove the azeotropic mixture of R-125 and R-125 before distillating, thereby obtain being substantially devoid of the R-125 of R-115.
Fig. 1 is the schema that can be used in the example of the present invention, that five fluorine chloric ethanes are removed device.
In Fig. 1, reference number 1 is for containing the input liquid that has generated of R-125 and R-115, and 2 is water distilling apparatus, and 3 is overhead product, and 4 for refluxing, and 5 is output.
As previously mentioned, have (minimum) azeotropic mixture that constitutes by R-125 and two kinds of compositions of R-115.This azeotropic mixture is that the inventor finds first.
Have now found that if distill the mixture of R-125 and R-115 under standard pressure, then the mol ratio of R-125/R-115 is being approximately at 85/15 o'clock, just be difficult to further concentrate its R-125.In other words, the liquid phase body of this proportion of composing is identical with the proportion of composing of its gas phase in equilibrium state.
Owing to have now found that the azeotropic mixture that can form R-125 and R-115, thereby when in the mixture of R-125 and R-115, the component proportions of its R-125 is during less than the component proportions in the azeotrope, the distillation procedure that can utilize R-125 and R-115 azeotropic mixture to reflux, when distillating the azeotropic constituent, obtain to be substantially free of the R-125 of R-115 effectively by the tower bottom by the cat head place.
Otherwise, when in the mixture of R-125 and R-115, the composition ratio of its R-115 is during greater than the component proportions in the azeotrope, the distillation procedure that can utilize R-125 and R-115 azeotropic mixture to reflux, when distillating the azeotropic constituent, obtain to be substantially free of the R-115 of R-125 effectively by the tower bottom by the cat head place.
Adopt the present invention,, also can pass through distillation procedure, the azeotropic constituent of formation R-125 and R-115 even when in containing the generation mixture of R-125 and R115, also containing other composition simultaneously.That is to say,, adopt the present invention also R-125 and R-115 can be separated even when except that R-115 and R-125, also having other composition.At this moment, can be according to the relation of the relative height between the boiling point of the azeotropic temperature of Azeotrope compositions and other composition of coexistence, make and preferentially contain other coexistence composition distillating side or outgoing side.
The water distilling apparatus that can be used for this distillation procedure can adopt the conventional various water distilling apparatus with necessary distillation function.If adopt the rectifier unit of sieve-tray tower, packing tower or the like, can obtain better result, and, also can carry out batch distillation or continuous still battery.
The distillatory operational condition is a kind of problem of practical application, can suitably determine according to the requirement of required separation degree or the like.If consider that the tower top temperature that should not make distillation tower is low excessively, its working pressure is got about 1～30Kg/cm
2Absolute pressure is more quite a lot of, and gets about 5～15Kg/cm
2Absolute pressure is then better.At this moment tower temperature is respectively approximately-55～60 ℃ and approximately-10～30 ℃.
The present invention when being used to have catalyzer, to tetrachloroethane with gasiform hydrogen fluoride (HF) carry out fluoridation resulting, contain R-125 and pay the mixture of product R-115 and remove R-115, be effective especially.
The following describes preferred forms of the present invention.
Fig. 1 represents to can be used for the schema of an example of the tripping device of method of the present invention.In general, the resultant of previous reaction is gaseous state output.Contain R-125 in the mixture that is obtained, 1,1,1, the 2-tetrafluoro is for monochloroethane (R-124), and 1,1,1-three fluoro monochloroethane (R-123), hydrogen fluoride (HF), and organism such as hydrogenchloride and a spot of R-115.By conventional methods, such as washing and separatory, modes such as component distillation will contain organic mixtures 1 such as R-125, R-124, R-123 and a small amount of R-115 remove de-chlorine hydride and HF from the mixture of this resultant of reaction after, be directed into water distilling apparatus 2.In this situation, as the proportion of composing of the R-115 that pays resultant, with the relative proportion relation of R-125, less than the component ratio of its azeotrope.
By water distilling apparatus 2, can discharge as overhead product 3 with R-125 with the part of its azeotropic R-115 at the cat head place, and make another part be back to the cat head place of water distilling apparatus as reflux 4.By the tower bottom of water distilling apparatus 1 discharge as output 5 be substantially devoid of R-115, by R-125, R-124, R-123 with and boiling point be higher than the mixture that a small amount of organism of R-125 constitutes.Can from aforementioned mixture, R-115 be removed effectively in this way.
This operation can be step, but continous way preferably.
Explain the present invention below by embodiment.
To the flask shape position of tower bottom input 240 gram (2mol) R-125 and 30.9 gram (0.2mol) R-115, under standard pressure, begin distillation in the total reflux mode with telescopic Ao Erde angle distillation tower (25 millimeters of diameters, 15 sections).When tower top temperature reaches about 55 ℃, distillate is taken a sample.Analyze this sample as can be known, the mol ratio of R-125/R-115 is about 85/15.
By this analytical results as can be known, its boiling point is higher than the atmospheric boiling point-38.7 ℃ of high pressure boiling point-48.5 ℃＜R-115 of the R-115(R-125 of R-125) be concentrated in the top of tower place, thus can confirm to have formed the minimum boiling point azcotrope of R-125 and R-115.
Embodiment 2
Adopt device similarly to Example 1, same mode, input 360 gram (3mol) R-125 and 15.5 gram (0.1mol) R-115 make distillation tower reach stable in the total reflux mode under standard pressure.After stable, when discharging distillate slowly by the cat head place, tower top temperature goes up long the liter slowly, when tower top temperature arrives distillation temperature (48.5 ℃), stops heating.Amount of liquid by cat head output is approximately 210 grams, and by about 150 grams of R-125 of the R-115 that can obtain containing about 30ppm in the distiller.
This result shows that R-125 in the time of can utilizing distillation R-125 and R-115 mixture and the azeotropism of R-115 are by in R-125 and the R-115 mixture R-115 being separated.
Claims (3)
1, the azeotropic mixture of pentafluoride ethane and five fluorine chloric ethanes.
2, the method for from the mixture that contains pentafluoride ethane and five fluorine chloric ethanes at least, separating five fluorine chloric ethanes, it is characterized in that heating up in a steamer the azeotropic mixture of pentafluoride ethane and five fluorine chloric ethanes by distillation to the generation mixture that contains pentafluoride ethane and five fluorine chloric ethanes at least.
3, method as claimed in claim 2 is characterized in that the distillatory working pressure is 1～30Kg/cm
2Absolute pressure.
Applications Claiming Priority (2)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP12460892A JP3182869B2 (en) | 1992-05-18 | 1992-05-18 | Azeotropic mixture of pentafluoroethane and pentafluorochloroethane and method for separating pentafluorochloroethane |
| JP124608/92 | 1992-05-18 |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN1085536A true CN1085536A (en) | 1994-04-20 |
Family
ID=14889646
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN 93107029 Pending CN1085536A (en) | 1992-05-18 | 1993-05-18 | The separation method of pentafluoride ethane and five fluorine chloric ethane azeotropic mixtures and five fluorine chloric ethanes |
Country Status (4)
| Country | Link |
|---|---|
| JP (1) | JP3182869B2 (en) |
| CN (1) | CN1085536A (en) |
| AU (1) | AU4088093A (en) |
| WO (1) | WO1993023355A1 (en) |
Families Citing this family (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5346595A (en) * | 1993-02-23 | 1994-09-13 | Alliedsignal Inc. | Process for the purification of a pentafluoroethane azeotrope |
| US5421964A (en) * | 1993-04-30 | 1995-06-06 | E. I. Du Pont De Nemours And Company | Process for separating HCl and halocarbons |
| WO1994025419A1 (en) * | 1993-04-30 | 1994-11-10 | E.I. Du Pont De Nemours And Company | AZEOTROPIC AND AZEOTROPE-LIKE COMPOSITIONS AND A PROCESS FOR SEPARATING HCl AND HALOCARBONS |
| BR9402038A (en) * | 1993-05-25 | 1995-03-07 | Showa Denko Kk | Pentafluor ethane purification process |
| ES2140682T3 (en) * | 1994-02-07 | 2000-03-01 | Du Pont | PROCEDURE FOR SEPARATING PENTAFLUOROETHANE FROM A MIXTURE THAT INCLUDES HALOGENATED HYDROCARBONS AND CHLOROPENTAFLUOROETHANE. |
| US5718807A (en) * | 1994-09-20 | 1998-02-17 | E. I. Du Pont De Nemours And Company | Purification process for hexafluoroethane products |
| US5918481A (en) * | 1997-11-20 | 1999-07-06 | Alliedsignal Inc. | Process for separating hydrogen fluoride from fluorocarbons |
| JP2003055277A (en) * | 2001-08-16 | 2003-02-26 | Showa Denko Kk | Method for producing hexafluoroethane and use thereof |
Family Cites Families (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US3505233A (en) * | 1968-11-12 | 1970-04-07 | Union Carbide Corp | Chloropentafluoroethane-pentafluoroethane azeotropic compositions |
| JPH02197634A (en) * | 1989-01-25 | 1990-08-06 | Toto Ltd | Privates cleaner |
| US5087329A (en) * | 1991-05-16 | 1992-02-11 | E. I. Du Pont De Nemours And Company | Process for separating pentafluoroethane from a mixture of halogenated hydrocarbons containing chloropentafluoroethane |
-
1992
- 1992-05-18 JP JP12460892A patent/JP3182869B2/en not_active Expired - Fee Related
-
1993
- 1993-05-14 WO PCT/JP1993/000637 patent/WO1993023355A1/en active Application Filing
- 1993-05-14 AU AU40880/93A patent/AU4088093A/en not_active Withdrawn
- 1993-05-18 CN CN 93107029 patent/CN1085536A/en active Pending
Also Published As
| Publication number | Publication date |
|---|---|
| AU4088093A (en) | 1993-12-13 |
| JPH05320077A (en) | 1993-12-03 |
| JP3182869B2 (en) | 2001-07-03 |
| WO1993023355A1 (en) | 1993-11-25 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| AU618617B2 (en) | Process for the separation of hf via azeotropic distillation | |
| EP0503771B1 (en) | Process for the separation of a product stream comprising fluorocarbons by distillation | |
| US5898088A (en) | Production of pentafluoroethane | |
| EP0522639A1 (en) | Process for the preparation of 1-chloro-1,1,3,3,3-pentafluoropropane and of 1,1,1,3,3,3-hexafluoropropane | |
| EP0467531A1 (en) | Process for the separation of 1,1,1,2-tetrafluoroethane from mixtures thereof with hydrogen fluoride and/or 1-chloro-2,2-difluoroethylene | |
| EP0395793A1 (en) | Process for the separation of 1,1-dichloro-1-fluoroethane and 1,1,1,3,3-pentafluorobutane | |
| AU663586B2 (en) | Method of removing hydrogen fluoride | |
| CN1085536A (en) | The separation method of pentafluoride ethane and five fluorine chloric ethane azeotropic mixtures and five fluorine chloric ethanes | |
| FR2724167A1 (en) | PROCESS FOR THE HYDROFLUORATION OF CHLORO (FLUORO) BUTANE | |
| JP2947158B2 (en) | Production of hexafluoroethane | |
| CN1027061C (en) | Extractive distillation | |
| JP3535563B2 (en) | Azeotropic composition containing water and fluorohydrocarbon, method for removing water from solution by azeotropic distillation, and method for producing hydrofluoroalkane | |
| US5714652A (en) | Process for the preparation of 1,1-difluoroethane | |
| JP3856820B2 (en) | Method for purifying pentafluoroethane | |
| US5772852A (en) | Separating HCI and halocarbons | |
| RU2024474C1 (en) | Method of synthesis of 1,1-dichloro-1-fluoroethane and a method of 1,1-dichloroethylene content decrease | |
| US6111151A (en) | Removal of water from process streams | |
| US5849160A (en) | Process of separating pentafluoroethane and process of producing pentafluoroethane using the same | |
| US6540882B1 (en) | Processes for the synthesis of pentafluorobutane and the separation of hydrogen fluoride and pentafluorobutane mixtures | |
| MXPA02004431A (en) | Process for the preparation of halogenated ethanes. | |
| Nagata et al. | Thermodynamics of associated solutions involving aniline and ethanol | |
| US20050096247A1 (en) | Azeotrope-like compositions of iodine heptafluoride and hydrogen fluoride | |
| JPH0912487A (en) | Separation of pentafluoroethane from 1,1,1-trifluoroethane | |
| JPH08301800A (en) | Production of pentafluoroethane and composition suitable to be converted into pentafluoroethane | |
| CN1207723A (en) | Production of chloro-2,2,2-trifluoroethane |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C01 | Deemed withdrawal of patent application (patent law 1993) | ||
| WD01 | Invention patent application deemed withdrawn after publication |