Patent US1128859A successfully refreshed from Google Patents.
US4001111A
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Dual temperature gradient elution liquid chromatography
Assignee: ExxonMobil Technology and Engineering Co
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Filing: 1974-03-19
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Granted: 1977-01-04
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Expires: 1994-03-19
Abstract
Abstract In a liquid chromatography commercial process for the separation of two or more components contained in admixture in a feedstream including the steps of (a) contacting the feedstream mixture containing the components to be separated with a bed of crystalline aluminosilicate adsorbent at conditions to effect the selective retention of two or more of the components by said adsorbent, (b) passing through said bed an eluent selected from the group consisting of aromatics and substituted aromatics, (c) increasing the strength of the eluting agent in the liquid carrier during the operation of the steps (a) and (b) above, (d) recovering from said bed a stream or streams containing at least a portion of the less selectively adsorbed components, and (e) recovering a stream substantially enhanced in concentration of said selectively adsorbed components relative to other components of feedstream wherein the improvement comprises preheating the eluting agent of step (c) above prior to passing it through said bed at temperatures of at least 160° C., to thereby effect the desired separation under conditions that cause substantially lower elution volume to feed ratios. The improved liquid chromatography process is particularly applicable to the separation of paraxylene and ethylbenzene from a C8 aromatic isomer mixture containing ethylbenzene. The above process when operated with the eluting agent preheating step at temperatures of about 160° C or higher causes temperature waves to flow through the bed with the final peak of each feed slug being eluted with the hotter eluting agent-carrier mixture, thus providing lower elution volume to feed ratios and thereby producing paraxylene more economically.
Inventors
- 👤 Paul R. Geissler
- 👤 Robert P. Cahn
Bibliographic Details
Application Number
—
Jurisdiction
US
Data Source
google_patents
Last Synchronized
2026-11-03 12:00
CPC Classifications
B; B01; B01D; B01D15/00; B01D15/08; B01J; B01J20/00; B01J20/02; B01J20/10; B01J20/16; B01J20/18; B01J20/281; B01J20/282; C; C07; C07C; C07C7/00; C07C7/12; C07C7/13; C10; C10G; C10G25/00; C10G25/02; C10G25/03; G; G01; G01N; G01N30/00; G01N30/02; G01N30/26; G01N30/28; B01D15/10; B01D15/16; B01D15/166; B01J2220/00; B01J2220/50; B01J2220/54
Claims Analysis
Total Claims: 13
Claim 1
Independent Claim
211 words
In a liquid chromatographic separation process of up to two components contained in admixture in a feedstream including the steps of: a. contacting the feedstream mixture containing said components to be separated with a bed of crystalline aluminosilicate adsorbent at conditions to effect the selective retention of up to two of the components by said adsorbent; b. passing through said bed an eluent selected from the group consisting of aromatics and substituted aromatics; c. increasing the strength of the eluting agent during the operation of step (b) above to thereby effect desired separation under conditions that cause low elution volume to feed ratios; d. recovering from said bed a stream or streams containing a portion of the less preferentially adsorbed components; and e. recovering a stream or streams substantially enhanced in concentration of said selectively adsorbed components relative to other feedstream components wherein the improvement comprises preheating the eluting agent of step (c) above prior to passing it through said bed at temperatures of from about 160° to about 200° C to thereby effect the desired separation of one of said preferentially adsorbed components under conditions resulting in substantially lower elution volume to feed ratios without a corresponding substantial decrease in the separation of the other of said preferentially adsorbed components.
Claim 2
Dependent Claim
211 words
In a liquid chromatographic separation process of up to two components contained in admixture in a feedstream including the steps of: a. contacting the feedstream mixture containing said components to be separated with a bed of crystalline aluminosilicate adsorbent at conditions to effect the selective retention of up to two of the components by said adsorbent; b. passing through said bed an eluent selected from the group consisting of aromatics and substituted aromatics; c. increasing the strength of the eluting agent during the operation of step (b) above to thereby effect desired separation under conditions that cause low elution volume to feed ratios; d. recovering from said bed a stream or streams containing a portion of the less preferentially adsorbed components; and e. recovering a stream or streams substantially enhanced in concentration of said selectively adsorbed components relative to other feedstream components wherein the improvement comprises preheating the eluting agent of step (c) above prior to passing it through said bed at temperatures of from about 160° to about 200° C to thereby effect the desired separation of one of said preferentially adsorbed components under conditions resulting in substantially lower elution volume to feed ratios without a corresponding substantial decrease in the separation of the other of said preferentially adsorbed components.
Claim 3
Dependent Claim
28 words
The process of claim 1 wherein said feedstream mixture is a C 8 aromatic feedstream containing ethylbenzene and where said crystalline aluminosilicate adsorbent is a potassium Y aluminosilicate.
Claim 4
Dependent Claim
14 words
The process of claim 2 wherein said selectively adsorbed components are paraxylene and ethylbenzene.
Claim 5
Dependent Claim
40 words
The process of claim 3 wherein the initial concentration of said eluent is about 25% and is increased to a final concentration in the range of from about 50 to about 100% during the operation of steps (b) and (c).
Claim 6
Dependent Claim
187 words
In a liquid chromatographic process for the separation of paraxylene from a feedstream containing a C 8 aromatic isomer mixture in ethylbenzene including the steps of: a. contacting said feedstream with a bed of crystalline aluminosilicate adsorbent at conditions to effect the selective retention of paraxylene by said adsorbent; b. passing through said bed an eluent selected from the group consisting of aromatics and substituted aromatics; c. increasing the strength of the eluent in a liquid carrier containing said eluent during operation of step (b) above; d. recovering from said bed a stream or streams containing a portion of the less preferentially adsorbed feedstream components; and e. recovering a stream or streams substantially enhanced in concentration of paraxylene wherein the improvement comprises preheating the eluting agent of step (c) above prior to passing it through said bed at temperatures of from about 160° to about 200° C to thereby effect the desired separation of one of said preferentially adsorbed components under conditions resulting in substantially lower elution volume to feed ratios without a corresponding substantial decrease in the separation of the other of said preferentially adsorbed components.
Claim 7
Dependent Claim
187 words
In a liquid chromatographic process for the separation of paraxylene from a feedstream containing a C 8 aromatic isomer mixture in ethylbenzene including the steps of: a. contacting said feedstream with a bed of crystalline aluminosilicate adsorbent at conditions to effect the selective retention of paraxylene by said adsorbent; b. passing through said bed an eluent selected from the group consisting of aromatics and substituted aromatics; c. increasing the strength of the eluent in a liquid carrier containing said eluent during operation of step (b) above; d. recovering from said bed a stream or streams containing a portion of the less preferentially adsorbed feedstream components; and e. recovering a stream or streams substantially enhanced in concentration of paraxylene wherein the improvement comprises preheating the eluting agent of step (c) above prior to passing it through said bed at temperatures of from about 160° to about 200° C to thereby effect the desired separation of one of said preferentially adsorbed components under conditions resulting in substantially lower elution volume to feed ratios without a corresponding substantial decrease in the separation of the other of said preferentially adsorbed components.
Claim 8
Dependent Claim
208 words
In a liquid chromatographic separation process for the separation of paraxylene contained in a C 8 aromatic isomer mixture containing ethylbenzene including the steps of: a. contacting a C 8 aromatic isomer mixture with a bed containing a type Y molecular sieve selected from the group consisting of potassium Y, ammonium/potassium Y and barium potassium Y at conditions to effect the selective retention of paraxylene by said sieve; b. passing through said sieve an eluent selected from the group consisting of metadiisopropylbenzene, paradiisopropylbenzene and toluene; c. increasing the strength of the eluent and the liquid carrier containing said eluent during the operation of step (b) above; d. recovering from said bed a stream or streams containing a portion of the feedstream components less preferentially adsorbed by said sieve; e. recovering a stream or streams substantially enhanced in concentration of paraxylene wherein the improvement comprises preheating the eluting agent of step (c) above prior to passing it through said bed at temperatures of from about 160° to about 200° to thereby effect the desired separation of one of said preferentially adsorbed components under conditions resulting in substantially lower elution volume to feed ratios without a corresponding substantial decrease in the separation of the other of said preferentially adsorbed components.
Claim 9
Dependent Claim
208 words
In a liquid chromatographic separation process for the separation of paraxylene contained in a C 8 aromatic isomer mixture containing ethylbenzene including the steps of: a. contacting a C 8 aromatic isomer mixture with a bed containing a type Y molecular sieve selected from the group consisting of potassium Y, ammonium/potassium Y and barium potassium Y at conditions to effect the selective retention of paraxylene by said sieve; b. passing through said sieve an eluent selected from the group consisting of metadiisopropylbenzene, paradiisopropylbenzene and toluene; c. increasing the strength of the eluent and the liquid carrier containing said eluent during the operation of step (b) above; d. recovering from said bed a stream or streams containing a portion of the feedstream components less preferentially adsorbed by said sieve; e. recovering a stream or streams substantially enhanced in concentration of paraxylene wherein the improvement comprises preheating the eluting agent of step (c) above prior to passing it through said bed at temperatures of from about 160° to about 200° to thereby effect the desired separation of one of said preferentially adsorbed components under conditions resulting in substantially lower elution volume to feed ratios without a corresponding substantial decrease in the separation of the other of said preferentially adsorbed components.
Claim 10
Dependent Claim
22 words
The process of claim 6 wherein said less preferentially adsorbed components are selected from the group consisting of metaxylene, orthoxylene and ethylbenzene.
Claim 11
Dependent Claim
31 words
The process of claim 6 wherein said eluent is metadiisopropylbenzene and is employed in admixture with an inert diluent selected from the group consisting of C 6 to C 20 paraffins.
Claim 12
Dependent Claim
18 words
The process of claim 8 wherein the composition of said eluent/diluent admixture is 25% metadiisopropylbenzene and 75% diluent.
Claim 13
Dependent Claim
10 words
The process of claim 9 wherein said diluent is n-dodecane.
References Cited (Backward Citations)
USPTO Annuity & Maintenance Windows
| Annuity Stage | Window Opens | Payment Deadline | Surcharge Period Until | Estimated Fee | Status |
|---|---|---|---|---|---|
| 3.5 Years (Year 4) | 1980-01-04 | 1980-07-05 | 1981-01-04 | $2000.00 | Window Closed / Lapsed |
| 7.5 Years (Year 8) | 1984-01-04 | 1984-07-05 | 1985-01-04 | $3760.00 | Window Closed / Lapsed |
| 11.5 Years (Year 12) | 1988-01-04 | 1988-07-05 | 1989-01-04 | $7700.00 | Window Closed / Lapsed |