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US4110374A Expired / Lapsed US ⏱️ 0.0 years remaining

Process for separating and recovering unreacted materials in urea synthesis

Assignee: Mitsui Toatsu Chemicals Inc
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Filing: 1977-04-18
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Granted: 1978-08-29
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Expires: 1997-04-18
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Abstract

Abstract A urea synthesis effluent is subjected to at least one high pressure decomposition stage and then a low pressure decomposition stage to decompose and recover unreacted materials contained in said effluent for recycle to the urea synthesis. The urea synthesis effluent discharged from a high pressure decomposition stage is cooled to 105° - 170° C. by indirect heat exchange with the urea synthesis effluent in the rectification zone of the low pressure decomposition stage and then is flashed into the top of said rectification zone, whereby the bottom of said rectification zone is heated to 100° - 140° C. and the temperature at the top of said rectification zone is maintained at 60° - 120° C. to minimize the water content in the distillate from the rectification zone.

Inventors

  • 👤 Shigeru Inoue

Bibliographic Details

Application Number —
Jurisdiction US
Data Source google_patents
Last Synchronized 2026-10-29 22:21
CPC Classifications
C; C07; C07C; C07C273/00; C07C273/02; C07C273/04

Claims Analysis

Total Claims: 18
Claim 1
Independent Claim 350 words
In a process for recovering unreacted materials and heat from a urea synthesis effluent including the steps of reacting in a urea synthesis zone carbon dioxide with ammonia under urea synthesis temperature and pressure conditions to obtain said urea synthesis effluent containing urea, an excess of ammonia, unreacted ammonium carbamate and water, subjecting said urea synthesis effluent to at least two ammonium carbamate decomposition stages including at least one high pressure steps at a gauge pressure above 10 kg/cm 2 and a low pressure stage at a gauge pressure below 5 kg/cm 2 to separate from said urea synthesis effluent gaseous mixtures each composed of ammonia, carbon dioxide and water vapor in the respective separation zones of said high pressure and low pressure decomposition stages, at least a portion of the separation zone of the low pressure stage being a rectification zone having a top zone and a bottom zone, contacting each of said gaseous mixtures with an absorbent in absorption zones each of which has substantially the same pressure as that of each of the corresponding separation zones to absorb said gaseous mixtures in said absorbent successively, and recycling the thus-obtained absorbate to the urea synthesis zone, the improvement which comprises cooling the urea synthesis effluent from the separation zone of said high pressure stage to a temperature of 105° - 170° C. by indirect heat exchange in a heat exchange zone with the urea synthesis effluent present in said bottom zone of the rectification zone of said low pressure stage, reducing the pressure of said cooled urea synthesis effluent to that of the low pressure stage, introducing the thus pressure reduced effluent into the top zone of the rectification zone and at the same time heating said urea synthesis effluent present in the bottom zone of said rectification zone by said indirect heat exchange in said heat exchange zone and in an additional heating zone to maintain the temperature of the top zone of the rectification zone at 60° - 120° C. and the temperature of the bottom zone of the rectification zone at 100° - 140° C.
Claim 2
Dependent Claim 350 words
In a process for recovering unreacted materials and heat from a urea synthesis effluent including the steps of reacting in a urea synthesis zone carbon dioxide with ammonia under urea synthesis temperature and pressure conditions to obtain said urea synthesis effluent containing urea, an excess of ammonia, unreacted ammonium carbamate and water, subjecting said urea synthesis effluent to at least two ammonium carbamate decomposition stages including at least one high pressure steps at a gauge pressure above 10 kg/cm 2 and a low pressure stage at a gauge pressure below 5 kg/cm 2 to separate from said urea synthesis effluent gaseous mixtures each composed of ammonia, carbon dioxide and water vapor in the respective separation zones of said high pressure and low pressure decomposition stages, at least a portion of the separation zone of the low pressure stage being a rectification zone having a top zone and a bottom zone, contacting each of said gaseous mixtures with an absorbent in absorption zones each of which has substantially the same pressure as that of each of the corresponding separation zones to absorb said gaseous mixtures in said absorbent successively, and recycling the thus-obtained absorbate to the urea synthesis zone, the improvement which comprises cooling the urea synthesis effluent from the separation zone of said high pressure stage to a temperature of 105° - 170° C. by indirect heat exchange in a heat exchange zone with the urea synthesis effluent present in said bottom zone of the rectification zone of said low pressure stage, reducing the pressure of said cooled urea synthesis effluent to that of the low pressure stage, introducing the thus pressure reduced effluent into the top zone of the rectification zone and at the same time heating said urea synthesis effluent present in the bottom zone of said rectification zone by said indirect heat exchange in said heat exchange zone and in an additional heating zone to maintain the temperature of the top zone of the rectification zone at 60° - 120° C. and the temperature of the bottom zone of the rectification zone at 100° - 140° C.
Claim 3
Dependent Claim 24 words
The process as claimed in claim 1 wherein said rectification zone is operated under a gauge of from 1.5 to 3.0 kg/cm 2 .
Claim 4
Dependent Claim 54 words
The process as claimed in claim 1 wherein said rectification zone and one or both of said heat exchange zone and said additional heating zone are integrated, whereby the heat exchanger of one or both of said heat exchange zone and additional heating zone is built into said bottom zone of the rectification zone.
Claim 5
Dependent Claim 34 words
The process as claimed in claim 1 wherein said rectification zone is a rectification column selected from the group consisting of a bubble cap plate column, a sieve plate column and a packed column.
Claim 6
Dependent Claim 38 words
The process as claimed in claim 1 wherein said additional heating zone is a heater indirectly heated with steam and selected from the group consisting of a one pass type, reboiler type and falling film type heat exchanger.
Claim 7
Dependent Claim 91 words
The process as claimed in claim 1 wherein said heat exchange zone and said additional heating zone are constituted separately from said rectification zone, and at least a portion of said urea synthesis effluent present in said bottom zone of rectification zone is discharged from said bottom zone, is circulated through said heat exchange zone and additional heating zone to be heated by indirect heat exchange with said urea synthesis effluent from the separation zone of said high pressure stage and is returned to said bottom zone of said rectification zone.
Claim 8
Dependent Claim 36 words
The process as claimed in claim 6 wherein said urea synthesis effluent discharged from the bottom of the rectification zone is circulated through said heat exchange zone and said additional heating zone provided in parallel arrangement.
Claim 9
Dependent Claim 36 words
The process as claimed in claim 6 wherein said urea synthesis effluent discharged from the bottom of the rectification zone is circulated through said heat exchange zone and said additional heating zone provided in series arrangement.
Claim 10
Dependent Claim 35 words
The process as claimed in claim 1 wherein the urea synthesis effluent discharged from said rectification zone is fed to a stripping zone and stripped with a stripping gas to strip off remaining unreacted materials.
Claim 11
Dependent Claim 15 words
The process as claimed in claim 9 wherein said stripping zone is a packed column.
Claim 12
Dependent Claim 14 words
The process as claimed in claim 9 wherein said stripping gas is carbon dioxide.
Claim 13
Dependent Claim 40 words
The process as claimed in claim 11 wherein the amount of said carbon dioxide fed to said stripping zone is from 0.01 to 0.2 mol per mol of urea contained in said urea synthesis effluent treated in the stripping zone.
Claim 14
Dependent Claim 41 words
The process as claimed in claim 9 wherein said rectification zone and said stripping zone are integrated whereby said rectification zone is the upper portion of said separation zone and said stripping zone is the lower portion of said separation zone.
Claim 15
Dependent Claim 44 words
The process as claimed in claim 13 wherein said rectification zone, said stripping zone and said additional heating zone are integrated, whereby the heat exchanger of said additional heating zone is built into said separation zone between said rectification zone and said stripping zone.
Claim 16
Dependent Claim 95 words
The process as claimed in claim 9 wherein said heat exchange zone and said additional heating zone are constituted separately from said rectification zone and said stripping zone, and at least a portion of said urea synthesis effluent present in said bottom zone of rectification zone is discharged from said bottom zone, is circulated through said heat exchange zone and additional heating zone to be heated by indirect heat exchange with said urea synthesis effluent from the separation zone of said high pressure stage and is returned to said bottom zone of said rectification zone.
Claim 17
Dependent Claim 36 words
The process as claimed in claim 15 wherein said urea synthesis effluent discharged from the bottom of the rectification zone is circulated through said heat exchange zone and said additional heating zone provided in parallel arrangement.
Claim 18
Dependent Claim 36 words
The process as claimed in claim 15 wherein said urea synthesis effluent discharged from the bottom of the rectification zone is circulated through said heat exchange zone and said additional heating zone provided in series arrangement.

References Cited (Backward Citations)

US3725210A Cited
US3824283A Cited

USPTO Annuity & Maintenance Windows

Annuity Stage Window Opens Payment Deadline Surcharge Period Until Estimated Fee Status
3.5 Years (Year 4) 1981-08-28 1982-02-27 1982-08-29 $2000.00 Window Closed / Lapsed
7.5 Years (Year 8) 1985-08-28 1986-02-27 1986-08-29 $3760.00 Window Closed / Lapsed
11.5 Years (Year 12) 1989-08-28 1990-02-27 1990-08-29 $7700.00 Window Closed / Lapsed

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