US4451273A
Expired / Lapsed
US
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Distillative freezing process for separating volatile mixtures and apparatuses for use therein
Assignee: SILK LP
•
Filing: 1983-03-31
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Granted: 1984-05-29
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Expires: 2003-03-31
Abstract
Abstract The distillative freezing process disclosed is useful in separating and purifying a mixture that contains a volatile and crystallizing component and one or more volatile and non-crystallizing components by vaporizing the volatile components from the mixture under a sufficiently reduced pressure to thereby simultaneously form a mass of solid enriched with the crystallizing component. Two components of a mixture processed are denoted as the key components: one is the crystallizing component and is denoted as B-component; the other is the non-crystallizing component present in the greatest amount and is denoted as A-component. For a mixture to be processable by the process, it is necessary that the vapor pressure ratio of the key components be within a certain range and a low pressure phase diagram of the binary system of the key components belongs to certain types of phase diagrams.
Inventors
- 👤 Chen-yen Cheng
- 👤 Sing-Wang Cheng
Bibliographic Details
Application Number
—
Jurisdiction
US
Data Source
google_patents
Last Synchronized
2026-10-27 09:04
CPC Classifications
B; B01; B01D; B01D7/00; B01D7/02; B01D9/00; B01D9/02; B01D9/04
Claims Analysis
Total Claims: 37
Claim 1
Independent Claim
284 words
A crystallization separation process for separating a multicomponent mixture that is at least partly in a liquid state and has two key volatile components, denoted as A-component, that volatile noncrystallizing component present in the greatest amount, and B-component, the volatile crystallizing component, into a B-enriched portion and a B-lean portion through formation of a B-enriched solid mass, comprising a determination that the two key volatile components form a binary system (a) whose characteristic vapor pressure ratio defined as the ratio of the vapor pressure of A-component to that of B-component both evaluated at the triple point temperature of B-component is in the range of 0.1 to 10 and is less than the ratio of the heat of sublimation to the heat of melting of B-component evaluated at the triple point temperature of B-component, and (b) whose constant pressure phase diagram that includes a three phase (B-enriched solid, liquid and vapor) state has a two phase (B-enriched solid and vapor) region covering a substantial concentration range above the temperature of the three phase state and a two phase (B-enriched solid and liquid) region below the temperature of the three phase state, and a first step of forming a first vapor mixture and a first condensed mass that comprises a mother liquor and a solid phase mass enriched in B-component by concurrently vaporizing the volatile components from the mixture in a first zone under a first temperature and a first pressure that are respectively lower than the triple point temperature and the triple point pressure of the pure B-component, and a second step of separating at least a major fraction of the A-component from the first condensed mass to thereby produce a B-enriched first condensed mass.
Claim 2
Dependent Claim
284 words
A crystallization separation process for separating a multicomponent mixture that is at least partly in a liquid state and has two key volatile components, denoted as A-component, that volatile noncrystallizing component present in the greatest amount, and B-component, the volatile crystallizing component, into a B-enriched portion and a B-lean portion through formation of a B-enriched solid mass, comprising a determination that the two key volatile components form a binary system (a) whose characteristic vapor pressure ratio defined as the ratio of the vapor pressure of A-component to that of B-component both evaluated at the triple point temperature of B-component is in the range of 0.1 to 10 and is less than the ratio of the heat of sublimation to the heat of melting of B-component evaluated at the triple point temperature of B-component, and (b) whose constant pressure phase diagram that includes a three phase (B-enriched solid, liquid and vapor) state has a two phase (B-enriched solid and vapor) region covering a substantial concentration range above the temperature of the three phase state and a two phase (B-enriched solid and liquid) region below the temperature of the three phase state, and a first step of forming a first vapor mixture and a first condensed mass that comprises a mother liquor and a solid phase mass enriched in B-component by concurrently vaporizing the volatile components from the mixture in a first zone under a first temperature and a first pressure that are respectively lower than the triple point temperature and the triple point pressure of the pure B-component, and a second step of separating at least a major fraction of the A-component from the first condensed mass to thereby produce a B-enriched first condensed mass.
Claim 3
Dependent Claim
52 words
The process of claim 1, wherein, in the first step, B-enriched solid is formed as the volatile components are vaporized and from a major fraction to substantially all of the heat released in the formation of the B-enriched solid is removed by the concurrent vaporizations of the volatile components from the mixture.
Claim 4
Dependent Claim
17 words
The process of claim 2, wherein the said first step is conducted under a substantially adiabatic condition.
Claim 5
Dependent Claim
79 words
The process of claim 3, which further comprises a third step of transforming the first vapor mixture into a second condensed mass, from a substantial fraction to all of which is a liquid phase mass, in a second zone by transferring heat therefrom while maintaining the vapor under a second pressure, said second pressure being also lower than the triple point pressure of the B-component, and said second pressure being established without any substantial pressurization of the first vapor.
Claim 6
Dependent Claim
31 words
The process of claim 4, wherein A-component has a greater volatility than the B-component, whereby the second condensed mass constitutes substantially a liquid output that is relatively enriched with the A-component.
Claim 7
Dependent Claim
30 words
The process of claim 4, wherein B-component has a greater volatility than A-component, whereby the second condensed mass includes a solid phase that is relatively enriched with respect to B-component.
Claim 8
Dependent Claim
59 words
The process of claim 4, wherein at least a portion of the second condensed mass is melted by transferring heat to the mass while maintaining the mass under an elevated pressure that is higher than the second pressure of the second step by vaporizing minor fraction of the second condensed mass and providing pressure isolation of the second zone.
Claim 9
Dependent Claim
63 words
The process of claim 4, wherein the said second step is a continuation of the said first step and the second step is continued until the mother liquor phase is reduced to a small amount, to thereby transfer from a large fraction to substantially all of the A-component in the original mixture to the first vapor mixture and thereby form a purified B-solid.
Claim 10
Dependent Claim
49 words
The process of claim 8, that further comprises a third step of melting the purified B-solid under a pressure that is slightly higher than the triple point pressure of the B-component by pressure isolating the B-solid and supplying heat thereto, the melt of the B-solid constituting a purified B-product.
Claim 11
Dependent Claim
63 words
The process of claim 3, wherein the said second step is a continuation of the said first step and the second step is continued until the mother liquor phase is reduced to a small amount, to thereby transfer from a large fraction to substantially all of the A-component in the original mixture to the first vapor mixture and thereby form a purified B-solid.
Claim 12
Dependent Claim
49 words
The process of claim 10, that further comprises a fourth step of melting the purified B-solid under a pressure that is slightly higher than the triple point pressure of the B-component by pressure isolating the B-solid and supplying heat thereto, the melt of the B-solid constituting a purified B-product.
Claim 13
Dependent Claim
79 words
The process of claim 2, which further comprises a third step of transforming the first vapor mixture into a second condensed mass, from a substantial fraction to all of which is a liquid phase mass, in a second zone by transferring heat therefrom while maintaining the vapor under a second pressure, said second pressure being also lower than the triple point pressure of the B-component, and said second pressure being established without any substantial pressurization of the first vapor.
Claim 14
Dependent Claim
31 words
The process of claim 12, wherein A-component has a greater volatility than the B-component, whereby the second condensed mass constitutes substantially a liquid output that is relatively enriched with the A-component.
Claim 15
Dependent Claim
30 words
The process of claim 12, wherein B-component has a greater volatility than A-component, whereby the second condensed mass includes a solid phase that is relatively enriched with respect to B-component.
Claim 16
Dependent Claim
60 words
The process of claim 12, wherein at least a portion of the second condensed mass is melted by transferring heat to the mass while maintaining the mass under an elevated pressure that is higher than the second pressure of the second step by vaporizing a minor fraction of the second condensed mass and providing pressure isolation of the second zone.
Claim 17
Dependent Claim
63 words
The process of claim 12, wherein the said second step is a continuation of the said first step and the second step is continued until the mother liquor phase is reduced to a small amount, to thereby transfer from a large fraction to substantially all of the A-component in the original mixture to the first vapor mixture and thereby form a purified B-solid.
Claim 18
Dependent Claim
49 words
The process of claim 16, that further comprises a fourth step of melting the purified B-solid under a pressure that is slightly higher than the triple point pressure of the B-component by pressure isolating the B-solid and supplying heat thereto, the melt of the B-solid constituting a purified B-product.
Claim 19
Dependent Claim
63 words
The process of claim 2, wherein the said second step is a continuation of the said first step and the second step is continued until the mother liquor phase is reduced to a small amount, to thereby transfer from a large fraction to substantially all of the A-component in the original mixture to the first vapor mixture and thereby form a purified B-solid.
Claim 20
Dependent Claim
49 words
The process of claim 18, that further comprises a fourth step of melting the purified B-solid under a pressure that is slightly higher than the triple point pressure of the B-component by pressure isolating the B-solid and supplying heat thereto, the melt of the B-solid constituting a purified B-product.
Claim 21
Dependent Claim
79 words
The process of claim 1 which further comprises a third step of transforming the first vapor mixture into a second condensed mass, from a substantial fraction to all of which is a liquid phase mass, in a second zone by transferring heat therefrom while maintaining the vapor under a second pressure, said second pressure being also lower than the triple point pressure of the B-component, and said second pressure being established without any substantial pressurization of the first vapor.
Claim 22
Dependent Claim
31 words
The process of claim 20, wherein A-component has a greater volatility than the B-component, whereby the second condensed mass constitutes substantially a liquid output that is relatively enriched with the A-component.
Claim 23
Dependent Claim
30 words
The process of claim 20, wherein B-component has a greater volatility than A-component, whereby the second condensed mass includes a solid phase that is relatively enriched with respect to B-component.
Claim 24
Dependent Claim
60 words
The process of claim 20, wherein at least a portion of the second condensed mass is melted by transferring heat to the mass while maintaining the mass under an elevated pressure that is higher than the second pressure of the second step by vaporizing a minor fraction of the second condensed mass and providing pressure isolation of the second zone.
Claim 25
Dependent Claim
136 words
The process of claim 20, wherein the B-component is selected from the group consisting of: Aluminum Chloride, Terephthalic Acid, Acetylene, Para-formaldehyde, Carbon Dioxide, Ferric Chloride, Hydrogen Cyanide, Hydrogen Chloride, 2,2-Dimethyl Propane, Hexachlorobenzene, 1,3-Butadiyne, Anthraquinone, Ammonia, t-Butyl Alcohol, Hydrogen, Methane, Carbon Tetrabromide, Anthracene, Carbazole, Cyclobutane, Benzene, 1,2,4,5 Tetrachlorobenzene, t-Butyl Chloride, 1,4 Dioxane, Tetrachloroethylene, Chlorine, Chlorine Dioxide, Dimethyl Terephthalate, Salicylic Acid, Pyrocatechol, Formic Acid, Hydroquinone, 1,2,4,5-Tetramethylbenzene, 4-tert-Butylphenol, Camphene, Benzonic Acid, 2-Naphthol, Pyrogallol, Acetic Acid, 1,4 Dichlorobenzene, Phthalic Anhydride, Naphthalene, Formaldehyde, Water, 1,2 Ethanediamine, p-xylene, Iodosilane, Maleic Anhydride, Chloroacetic Acid, Acetamide, Succinimide, Acrylic Acid, Dichloroethane, Diacetamide, Oxygen, Phenol, t-Amyl Alcohol, 1-Naphthol, 4-Bromotoluene, 4-Chlorotoluene, 4-Chloroaniline, Cyclohexanol, Piperidine, Acenaphthene, Tetrachloroethylene, Tiglic Acid, p-Nitrotoluene, Biphenyl, Acetanilide, Ethylene, Silicon Tetrachloride, 2,4 Dichlorophenol, 1,3 Butadiene, Epichlohydrin, Menthol, Silane (SiH 4 ), Titanium Tetrachloride, Hydrogen Peroxide, o-Xylene, Styrene, Acrylnitrile, 1-Butene, m-Xylene, Ethane, Trichlorosilane, Ethyl benzene.
Claim 26
Dependent Claim
50 words
The process of claim 24, wherein, in the first step, B-enriched solid is formed as the volatile components are vaporized and from a major fraction to all of the heat released in the formation of B-enriched solid is removed by the concurrent vaporizations of the volatile components from the mixture.
Claim 27
Dependent Claim
17 words
The process of claim 25, wherein the said first step is conducted under a substantially adiabatic condition.
Claim 28
Dependent Claim
62 words
The process of claim 26, wherein the said second step is a continuation of the said first step and the second step is continued until the mother liquor phase is reduced to a small amount, to thereby transfer from a large fraction to substantially all of the A-component in the original mixture to the first vapor and thereby form a purified B-solid.
Claim 29
Dependent Claim
49 words
The process of claim 27, that further comprises a third step of melting the purified B-solid under a pressure that is slightly higher than the triple point pressure of the B-component by pressure isolating the B-solid and supplying heat thereto, the melt of the B-solid constituting a purified B-product.
Claim 30
Dependent Claim
62 words
The process of claim 25, wherein the said second step is a continuation of the said first step and the second step is continued until the mother liquor phase is reduced to a small amount, to thereby transfer from a large fraction to substantially all of the A-component in the original mixture to the first vapor and thereby form a purified B-solid.
Claim 31
Dependent Claim
49 words
The process of claim 29, that further comprises a third step of melting the purified B-solid under a pressure that is slightly higher than the triple point pressure of the B-component by pressure isolating the B-solid and supplying heat thereto, the melt of the B-solid constituting a purified B-product.
Claim 32
Dependent Claim
62 words
The process of claim 24, wherein the said second step is a continuation of the said first step and the second step is continued until the mother liquor phase is reduced to a small amount, to thereby transfer from a large fraction to substantially all of the A-component in the original mixture to the first vapor and thereby form a purified B-solid.
Claim 33
Dependent Claim
49 words
The process of claim 31, that further comprises a third step of melting the purified B-solid under a pressure that is slightly higher than the triple point pressure of the B-component by pressure isolating the B-solid and supplying heat thereto, the melt of the B-solid constituting a purified B-product.
Claim 34
Dependent Claim
63 words
The process of claim 20, wherein the said second step is a continuation of the said first step and the second step is continued until the mother liquor phase is reduced to a small amount, to thereby transfer from a large fraction to substantially all of the A-component in the original mixture to the first vapor mixture and thereby form a purified B-solid.
Claim 35
Dependent Claim
49 words
The process of claim 33, that further comprises a fourth step of melting the purified B-solid under a pressure that is slightly higher than the triple point pressure of the B-component by pressure isolating the B-solid and supplying heat thereto, the melt of the B-solid constituting a purified B-product.
Claim 36
Dependent Claim
63 words
The process of claim 1, wherein the said second step is a continuation of the said first step and the second step is continued until the mother liquor phase is reduced to a small amount, to thereby transfer from a large fraction to substantially all of the A-component in the original mixture to the first vapor mixture and thereby form a purified B-solid.
Claim 37
Dependent Claim
49 words
The process of claim 35, that further comprises a fourth step of melting the purified B-solid under a pressure that is slightly higher than the triple point pressure of the B-component by pressure isolating the B-solid and supplying heat thereto, the melt of the B-solid constituting a purified B-product.
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USPTO Annuity & Maintenance Windows
| Annuity Stage | Window Opens | Payment Deadline | Surcharge Period Until | Estimated Fee | Status |
|---|---|---|---|---|---|
| 3.5 Years (Year 4) | 1987-05-29 | 1987-11-28 | 1988-05-29 | $2000.00 | Window Closed / Lapsed |
| 7.5 Years (Year 8) | 1991-05-29 | 1991-11-28 | 1992-05-29 | $3760.00 | Window Closed / Lapsed |
| 11.5 Years (Year 12) | 1995-05-29 | 1995-11-28 | 1996-05-29 | $7700.00 | Window Closed / Lapsed |