US2820769A - Process for preparing hydrogen-nitrogen mixtures from coke oven gas - Google Patents
Process for preparing hydrogen-nitrogen mixtures from coke oven gas Download PDFInfo
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- US2820769A US2820769A US576648A US57664856A US2820769A US 2820769 A US2820769 A US 2820769A US 576648 A US576648 A US 576648A US 57664856 A US57664856 A US 57664856A US 2820769 A US2820769 A US 2820769A
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- washing
- nitrogen
- residue
- zone
- condenser
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- IJGRMHOSHXDMSA-UHFFFAOYSA-N nitrogen Substances N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 title claims description 177
- 229910052757 nitrogen Inorganic materials 0.000 title claims description 95
- 239000007789 gas Substances 0.000 title claims description 52
- 239000000571 coke Substances 0.000 title claims description 23
- 239000000203 mixture Substances 0.000 title claims description 18
- 238000004519 manufacturing process Methods 0.000 title claims description 6
- 238000005406 washing Methods 0.000 claims description 121
- 239000007788 liquid Substances 0.000 claims description 48
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 claims description 20
- 238000001816 cooling Methods 0.000 claims description 13
- UGFAIRIUMAVXCW-UHFFFAOYSA-N Carbon monoxide Chemical compound [O+]#[C-] UGFAIRIUMAVXCW-UHFFFAOYSA-N 0.000 claims description 9
- 229910002091 carbon monoxide Inorganic materials 0.000 claims description 9
- 238000009835 boiling Methods 0.000 claims description 8
- 229960005419 nitrogen Drugs 0.000 description 84
- 238000000034 method Methods 0.000 description 17
- 239000001257 hydrogen Substances 0.000 description 12
- 229910052739 hydrogen Inorganic materials 0.000 description 12
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 9
- 238000000926 separation method Methods 0.000 description 8
- 238000001704 evaporation Methods 0.000 description 5
- 239000000470 constituent Substances 0.000 description 4
- 230000008020 evaporation Effects 0.000 description 4
- 239000002826 coolant Substances 0.000 description 3
- 150000002431 hydrogen Chemical class 0.000 description 3
- 238000010276 construction Methods 0.000 description 2
- 230000001419 dependent effect Effects 0.000 description 2
- 239000008246 gaseous mixture Substances 0.000 description 2
- 238000002360 preparation method Methods 0.000 description 2
- 230000000630 rising effect Effects 0.000 description 2
- 238000003786 synthesis reaction Methods 0.000 description 2
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 150000002829 nitrogen Chemical class 0.000 description 1
- 238000010992 reflux Methods 0.000 description 1
- 229920006395 saturated elastomer Polymers 0.000 description 1
Images
Classifications
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- F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
- F25—REFRIGERATION OR COOLING; COMBINED HEATING AND REFRIGERATION SYSTEMS; HEAT PUMP SYSTEMS; MANUFACTURE OR STORAGE OF ICE; LIQUEFACTION SOLIDIFICATION OF GASES
- F25J—LIQUEFACTION, SOLIDIFICATION OR SEPARATION OF GASES OR GASEOUS OR LIQUEFIED GASEOUS MIXTURES BY PRESSURE AND COLD TREATMENT OR BY BRINGING THEM INTO THE SUPERCRITICAL STATE
- F25J3/00—Processes or apparatus for separating the constituents of gaseous or liquefied gaseous mixtures involving the use of liquefaction or solidification
- F25J3/02—Processes or apparatus for separating the constituents of gaseous or liquefied gaseous mixtures involving the use of liquefaction or solidification by rectification, i.e. by continuous interchange of heat and material between a vapour stream and a liquid stream
- F25J3/0204—Processes or apparatus for separating the constituents of gaseous or liquefied gaseous mixtures involving the use of liquefaction or solidification by rectification, i.e. by continuous interchange of heat and material between a vapour stream and a liquid stream characterised by the feed stream
- F25J3/0219—Refinery gas, cracking gas, coke oven gas, gaseous mixtures containing aliphatic unsaturated CnHm or gaseous mixtures of undefined nature
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B3/00—Hydrogen; Gaseous mixtures containing hydrogen; Separation of hydrogen from mixtures containing it; Purification of hydrogen
- C01B3/02—Production of hydrogen or of gaseous mixtures containing a substantial proportion of hydrogen
- C01B3/025—Preparation or purification of gas mixtures for ammonia synthesis
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B3/00—Hydrogen; Gaseous mixtures containing hydrogen; Separation of hydrogen from mixtures containing it; Purification of hydrogen
- C01B3/50—Separation of hydrogen or hydrogen containing gases from gaseous mixtures, e.g. purification
- C01B3/506—Separation of hydrogen or hydrogen containing gases from gaseous mixtures, e.g. purification at low temperatures
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- F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
- F25—REFRIGERATION OR COOLING; COMBINED HEATING AND REFRIGERATION SYSTEMS; HEAT PUMP SYSTEMS; MANUFACTURE OR STORAGE OF ICE; LIQUEFACTION SOLIDIFICATION OF GASES
- F25J—LIQUEFACTION, SOLIDIFICATION OR SEPARATION OF GASES OR GASEOUS OR LIQUEFIED GASEOUS MIXTURES BY PRESSURE AND COLD TREATMENT OR BY BRINGING THEM INTO THE SUPERCRITICAL STATE
- F25J3/00—Processes or apparatus for separating the constituents of gaseous or liquefied gaseous mixtures involving the use of liquefaction or solidification
- F25J3/02—Processes or apparatus for separating the constituents of gaseous or liquefied gaseous mixtures involving the use of liquefaction or solidification by rectification, i.e. by continuous interchange of heat and material between a vapour stream and a liquid stream
- F25J3/0228—Processes or apparatus for separating the constituents of gaseous or liquefied gaseous mixtures involving the use of liquefaction or solidification by rectification, i.e. by continuous interchange of heat and material between a vapour stream and a liquid stream characterised by the separated product stream
- F25J3/0276—Processes or apparatus for separating the constituents of gaseous or liquefied gaseous mixtures involving the use of liquefaction or solidification by rectification, i.e. by continuous interchange of heat and material between a vapour stream and a liquid stream characterised by the separated product stream separation of H2/N2 mixtures, i.e. of ammonia synthesis gas
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B2203/00—Integrated processes for the production of hydrogen or synthesis gas
- C01B2203/04—Integrated processes for the production of hydrogen or synthesis gas containing a purification step for the hydrogen or the synthesis gas
- C01B2203/0465—Composition of the impurity
- C01B2203/047—Composition of the impurity the impurity being carbon monoxide
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B2203/00—Integrated processes for the production of hydrogen or synthesis gas
- C01B2203/04—Integrated processes for the production of hydrogen or synthesis gas containing a purification step for the hydrogen or the synthesis gas
- C01B2203/0465—Composition of the impurity
- C01B2203/048—Composition of the impurity the impurity being an organic compound
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- F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
- F25—REFRIGERATION OR COOLING; COMBINED HEATING AND REFRIGERATION SYSTEMS; HEAT PUMP SYSTEMS; MANUFACTURE OR STORAGE OF ICE; LIQUEFACTION SOLIDIFICATION OF GASES
- F25J—LIQUEFACTION, SOLIDIFICATION OR SEPARATION OF GASES OR GASEOUS OR LIQUEFIED GASEOUS MIXTURES BY PRESSURE AND COLD TREATMENT OR BY BRINGING THEM INTO THE SUPERCRITICAL STATE
- F25J2200/00—Processes or apparatus using separation by rectification
- F25J2200/50—Processes or apparatus using separation by rectification using multiple (re-)boiler-condensers at different heights of the column
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- F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
- F25—REFRIGERATION OR COOLING; COMBINED HEATING AND REFRIGERATION SYSTEMS; HEAT PUMP SYSTEMS; MANUFACTURE OR STORAGE OF ICE; LIQUEFACTION SOLIDIFICATION OF GASES
- F25J—LIQUEFACTION, SOLIDIFICATION OR SEPARATION OF GASES OR GASEOUS OR LIQUEFIED GASEOUS MIXTURES BY PRESSURE AND COLD TREATMENT OR BY BRINGING THEM INTO THE SUPERCRITICAL STATE
- F25J2200/00—Processes or apparatus using separation by rectification
- F25J2200/74—Refluxing the column with at least a part of the partially condensed overhead gas
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- F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
- F25—REFRIGERATION OR COOLING; COMBINED HEATING AND REFRIGERATION SYSTEMS; HEAT PUMP SYSTEMS; MANUFACTURE OR STORAGE OF ICE; LIQUEFACTION SOLIDIFICATION OF GASES
- F25J—LIQUEFACTION, SOLIDIFICATION OR SEPARATION OF GASES OR GASEOUS OR LIQUEFIED GASEOUS MIXTURES BY PRESSURE AND COLD TREATMENT OR BY BRINGING THEM INTO THE SUPERCRITICAL STATE
- F25J2200/00—Processes or apparatus using separation by rectification
- F25J2200/80—Processes or apparatus using separation by rectification using integrated mass and heat exchange, i.e. non-adiabatic rectification in a reflux exchanger or dephlegmator
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- F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
- F25—REFRIGERATION OR COOLING; COMBINED HEATING AND REFRIGERATION SYSTEMS; HEAT PUMP SYSTEMS; MANUFACTURE OR STORAGE OF ICE; LIQUEFACTION SOLIDIFICATION OF GASES
- F25J—LIQUEFACTION, SOLIDIFICATION OR SEPARATION OF GASES OR GASEOUS OR LIQUEFIED GASEOUS MIXTURES BY PRESSURE AND COLD TREATMENT OR BY BRINGING THEM INTO THE SUPERCRITICAL STATE
- F25J2205/00—Processes or apparatus using other separation and/or other processing means
- F25J2205/02—Processes or apparatus using other separation and/or other processing means using simple phase separation in a vessel or drum
- F25J2205/04—Processes or apparatus using other separation and/or other processing means using simple phase separation in a vessel or drum in the feed line, i.e. upstream of the fractionation step
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- F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
- F25—REFRIGERATION OR COOLING; COMBINED HEATING AND REFRIGERATION SYSTEMS; HEAT PUMP SYSTEMS; MANUFACTURE OR STORAGE OF ICE; LIQUEFACTION SOLIDIFICATION OF GASES
- F25J—LIQUEFACTION, SOLIDIFICATION OR SEPARATION OF GASES OR GASEOUS OR LIQUEFIED GASEOUS MIXTURES BY PRESSURE AND COLD TREATMENT OR BY BRINGING THEM INTO THE SUPERCRITICAL STATE
- F25J2205/00—Processes or apparatus using other separation and/or other processing means
- F25J2205/30—Processes or apparatus using other separation and/or other processing means using a washing, e.g. "scrubbing" or bubble column for purification purposes
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- F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
- F25—REFRIGERATION OR COOLING; COMBINED HEATING AND REFRIGERATION SYSTEMS; HEAT PUMP SYSTEMS; MANUFACTURE OR STORAGE OF ICE; LIQUEFACTION SOLIDIFICATION OF GASES
- F25J—LIQUEFACTION, SOLIDIFICATION OR SEPARATION OF GASES OR GASEOUS OR LIQUEFIED GASEOUS MIXTURES BY PRESSURE AND COLD TREATMENT OR BY BRINGING THEM INTO THE SUPERCRITICAL STATE
- F25J2210/00—Processes characterised by the type or other details of the feed stream
- F25J2210/14—Coke-ovens gas
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- F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
- F25—REFRIGERATION OR COOLING; COMBINED HEATING AND REFRIGERATION SYSTEMS; HEAT PUMP SYSTEMS; MANUFACTURE OR STORAGE OF ICE; LIQUEFACTION SOLIDIFICATION OF GASES
- F25J—LIQUEFACTION, SOLIDIFICATION OR SEPARATION OF GASES OR GASEOUS OR LIQUEFIED GASEOUS MIXTURES BY PRESSURE AND COLD TREATMENT OR BY BRINGING THEM INTO THE SUPERCRITICAL STATE
- F25J2210/00—Processes characterised by the type or other details of the feed stream
- F25J2210/42—Nitrogen
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- F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
- F25—REFRIGERATION OR COOLING; COMBINED HEATING AND REFRIGERATION SYSTEMS; HEAT PUMP SYSTEMS; MANUFACTURE OR STORAGE OF ICE; LIQUEFACTION SOLIDIFICATION OF GASES
- F25J—LIQUEFACTION, SOLIDIFICATION OR SEPARATION OF GASES OR GASEOUS OR LIQUEFIED GASEOUS MIXTURES BY PRESSURE AND COLD TREATMENT OR BY BRINGING THEM INTO THE SUPERCRITICAL STATE
- F25J2270/00—Refrigeration techniques used
- F25J2270/12—External refrigeration with liquid vaporising loop
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- F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
- F25—REFRIGERATION OR COOLING; COMBINED HEATING AND REFRIGERATION SYSTEMS; HEAT PUMP SYSTEMS; MANUFACTURE OR STORAGE OF ICE; LIQUEFACTION SOLIDIFICATION OF GASES
- F25J—LIQUEFACTION, SOLIDIFICATION OR SEPARATION OF GASES OR GASEOUS OR LIQUEFIED GASEOUS MIXTURES BY PRESSURE AND COLD TREATMENT OR BY BRINGING THEM INTO THE SUPERCRITICAL STATE
- F25J2270/00—Refrigeration techniques used
- F25J2270/42—Quasi-closed internal or closed external nitrogen refrigeration cycle
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- F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
- F25—REFRIGERATION OR COOLING; COMBINED HEATING AND REFRIGERATION SYSTEMS; HEAT PUMP SYSTEMS; MANUFACTURE OR STORAGE OF ICE; LIQUEFACTION SOLIDIFICATION OF GASES
- F25J—LIQUEFACTION, SOLIDIFICATION OR SEPARATION OF GASES OR GASEOUS OR LIQUEFIED GASEOUS MIXTURES BY PRESSURE AND COLD TREATMENT OR BY BRINGING THEM INTO THE SUPERCRITICAL STATE
- F25J2290/00—Other details not covered by groups F25J2200/00 - F25J2280/00
- F25J2290/40—Vertical layout or arrangement of cold equipments within in the cold box, e.g. columns, condensers, heat exchangers etc.
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y10—TECHNICAL SUBJECTS COVERED BY FORMER USPC
- Y10S—TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y10S62/00—Refrigeration
- Y10S62/92—Carbon monoxide
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y10—TECHNICAL SUBJECTS COVERED BY FORMER USPC
- Y10S—TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y10S62/00—Refrigeration
- Y10S62/931—Recovery of hydrogen
- Y10S62/934—From nitrogen
Definitions
- the present invention relates to the preparation of a mixture of hydrogen and nitrogen suitable for the synesis of NH using coke oven gas as the source of hydrogen.
- a gaseous residue consisting essentially of hydrogen can be obtained from coke oven gas by cooling the gas under pressure, e. g. 10 to 30 atmospheres and 165 to -190 C., to condense therefrom less volatile components.
- the resulting gaseous residue contains, in ad dition to hydrogen, about 4% by volume of nitrogen, about 4% by volume of CO and, dependent upon the cooling, from 2 to 8% by volume of CH
- the present invention is particularly concerned with novel improvements for washing this impure gaseous residue with liquid nitrogen so as to remove CH and CO substantially quantitatively.
- washing of the gaseous residue it is customary for the washing of the gaseous residue to be carried out by flowing the residue through a washing column, while the residue is maintained under the pressure utilized in separating the less volatile components therefrom, in counter-current relationship to liquid washing nitrogen.
- the temperature in the washing column must be very low although it may be varied within relatively wide limits depending upon the pressure utilized.
- a column temperature of about l90 C. can be utilized when the separating pressure is 13 atmospheres.
- the condenser In order that the low temperature necessary for efiecting a substantially complete removal of the C may be maintained, it is customary to install a condenser, either in front, or on top, of the washing column, through which the gaseous residue is passed and cooled by the evaporation therein of liquid nitrogen under a constant pressure.
- the nitrogen in the condenser is evaporated at a pressure slightly higher than 1 atmosphere, namely, 1.3 atmosphe es.
- the nitrogen in the condenser has a temperature of -l93 C., and the gas mixture flowing through the condenser is cooled to a temperature which is slightly higher, namely, --190 C.
- the washing process is preferably carried out in such a way that L is equal to V or even slightly smaller (e. g. 5-10 cu. in.) than V.
- the process is carried out under such conditions that the amount of washing nitrogen introduced into the washing column evaporates completely in the column and is removed at the top thereof together with the hydrogen freed of methane and CO, while the amount of liquid nitrogen collected at the bottom of the, column, which is mixed with a large amount of CO, is equal to or slightly smaller than the amount of nitrogen continuously introduced into the washing columnas part of the gaseous residue from the coke oven gas separation (about 4% by volume N If the condenser is placed in front of the column, the temperature in the column is very low. As a result, V has a relatively low value and L may also be small.
- the degree to which the CO is removed is highly dependent on flue-- tuations in the amount L and, moreover, the CO percentage of the washed hydrogen'immediately rises to an undesired level when the amount of L becomes too small.
- the amount of liquid nitrogen L flowing down in the wash ing column which in this case is equal to the sum of the liquid nitrogen supplied at the top of the washing column and the condensate formed in the condenser, is chosen to be equal to V, or preferably to be evenslightly smaller than V. Consequently, the value of L is much greater thanin the casewhere'. the condenser is arranged in front of the column.
- the processof the present invention employs boiling liquid nitrogen as cool ant in the condenser, the nitrogen being kept under a constant pressure preferably slightly higher than atmospheric, e. g. 1.05 to 1.60 atmospheres. In this way, a constant and very low temperature is maintained in the condenser.
- the cold gaseous residue of the coke oven gas separation is conducted to condenser 2 by means of conduit 4.
- the residue is cooled indirectly in the condenser by the evaporation of nitrogen supplied by the apparatus 3 wherein nitrogen is compressed to about 200 atmospheres and strongly cooled.
- the high-pressure rntrogen flows from apparatus 3 through conduit 7 and into the condenser after expansion thereof in valve 7a.
- the evaporated nitrogen is returned through conduit 8 into apparatus 3. 1 V
- the cold residue of the coke oven gas separation flows directly through conduit 4 into the bottom section of washing column 1, in which it is washed by means of liquid nitrogen supplied through conduit 6.
- the washed gas flows through condenser 2, in which indirect cooling takes place by nitrogen evaporating in the condenser.
- FIG. 3 exemplifies. the process and apparatus of the present invention.
- the cold gaseous residue of the coke oven gas separation first, flows into the bottom section of a washing compartment 1a and subsequently through condenser 2 into washing compartment 1b.
- Liquid nitrogen supplied through conduit 6 is fed into the top section of washing compartment 1b.
- the washing column may also comprise two separate parts, as'is shown in Figure 4, which communicate by means of a U-shaped conduit 12, through which the wash ing liquid flows from one washing compartment into the other and by means of a conduit 13, which conducts gas.
- This latter embodiment offers the advantage that damming of the liquid in the condenser by arriving gas is impossible.
- the combined height of the two washing compartments is not greater than the height of the washing column commonly used in the conventional construction with only one washing compartment. Furthermore, it has been found that the first washing compartment, located under. the condenser, may be smaller than the second washing compartment. Thus, if the number of theoretical plates in the first washing compartment is about A; to Mt of the totalnumber of theoretical plates needed, the CO removal reaches its optimum value, under otherwise equal conditions.
- the CO content relatesto the eventual NH -synthesis mixture (3 parts by volume of H and 1 part by volume of N obtained by making up the shortage of nitrogen after the washing treatment.
- the data given is based on passing at a pressure of 13 .atm. the gaseous residue of 1000 cu. m. N. P. T..of coke oven gas, i. e. 620 cu. m. H 39.7 cu. m. N 41.8 cu. m. CO and 59.5 cu. m. CH, per. hour through the apparatus.
- the temperature of the boiling nitrogen in the condenser was 193 C., so that the cooled gas mixture leavingthe condenser had a temperature of C.
- the temperature in the bottom section of the washing column according to Figure l was 195 C.
- the temperature of'the' gas prevailing throughout the column of Figure 2 and in the lower washing compartment of Figure 3 was --'182 113.
- the temperature in the second or upper washing steam-res compartmentof Figure 3' was --1'90 C;
- the totali number of theoretical plates was-equal in: all threecases and amounted to 22.
- the improved process of the invention comprises initially washing the cold gaseous residue by passing same upwardly through a first washing zone wherein the residue is washed by counter-current contact with liquid nitrogen, then passing the thus treated gaseous residue upwardly through an intermediate condensing zone wherein the residue is indirectly cooled with boiling nitrogen under a constant pressure preferably slightly higher than atmospheric and a condensate of nitrogen is obtained from the residue, thereafter further washing the gaseous residue by passing same upwardly through a second washing zone in counter-current contact with liquid nitrogen, collecting liquid washing nitrogen contaminated with carbon monoxide from said second washing zone and utilizing the collected nitrogen and the condensate from the condensing zone as the liquid nitrogen for washing the gaseous residue in the first washing zone.
- the nitrogen utilized for washing in the second washing zone is substantially pure nitrogen.
- the temperature of the gas being washed in the first and second washing zones is about l82 C. and 190 C., respectively, although other temperatures include 175 to -l88 C. in the first zone and 185 to 195 C. in the second zone.
- the temperature of the gas is, therefore, reduced by about 3 to C. in the condensing zone.
- the pressure of the gas during the treatment is preferably the same as that used in initially condensing low volatile constituents from the coke oven gas, e. g. 10 to 30 atmospheres with 13 atmospheres particularly advantageous.
- the apparatus of the invention broadly described, comprises an upper gas washing compartment, means for supplying liquid washing nitrogen downwardly through the compartment in countor-current relationship to gas flowing upwardly therethrough, means for collecting liquid washing nitrogen from the upper washing compartment, a lower washing compartment, means for passing gas to be washed upwardly and successively through the first and second washing compartments, condensing means for indirectly cooling said gas between the first and second washing compartments, the cooling means comprising boiling nitrogen under a constant pressurepreferably slightly above atmospheric, means for collecting condensate ob-.- tained from the gas in said condensing meansand means for supplying liquid nitrogen collected from the upper compartment and the condensate from the condensing means to the lower compartment as the wash liquidinthe lastrrnentioned compartment.
- gaseous residue passed into said first washing zone consists essentially of, by volume, about 4% nitrogen, about 4% carbon monoxide, from 2 to 8% methane and the remainder hydrogen.
- 10.-Apparatus for preparing gaseous hydrogen-nitrogen mixtures from coke oven gas comprising an upper gas washing compartment, means for supplying liquid l washing zone in counter-current contact with liquidnitro- I gen thegheight-of; said first washing zone being substan:
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- Mechanical Engineering (AREA)
- Thermal Sciences (AREA)
- General Engineering & Computer Science (AREA)
- Combustion & Propulsion (AREA)
- Inorganic Chemistry (AREA)
- Separation By Low-Temperature Treatments (AREA)
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Applications Claiming Priority (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
NL793605X | 1955-04-07 |
Publications (1)
Publication Number | Publication Date |
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US2820769A true US2820769A (en) | 1958-01-21 |
Family
ID=19834485
Family Applications (1)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
US576648A Expired - Lifetime US2820769A (en) | 1955-04-07 | 1956-04-06 | Process for preparing hydrogen-nitrogen mixtures from coke oven gas |
Country Status (6)
Country | Link |
---|---|
US (1) | US2820769A (is") |
BE (1) | BE546755A (is") |
DE (1) | DE1014136B (is") |
FR (1) | FR1150767A (is") |
GB (1) | GB793605A (is") |
NL (1) | NL99841C (is") |
Cited By (7)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
US2895304A (en) * | 1955-06-02 | 1959-07-21 | Linde Eismasch Ag | Process and apparatus for gas purification |
US3187485A (en) * | 1961-12-13 | 1965-06-08 | Foster Wheeler Corp | Purification of hydrogen by scrubbing with nitrogen at high pressures |
US3269130A (en) * | 1957-01-04 | 1966-08-30 | Air Prod & Chem | Separation of gaseous mixtures containing hydrogen and nitrogen |
US3407146A (en) * | 1964-01-22 | 1968-10-22 | Linde Ag | Process for the recovery of hydrogennitrogen mixtures with reduced carbon-monoxide content |
CN104495749A (zh) * | 2014-12-23 | 2015-04-08 | 东北大学 | 一种利用焦炉荒煤气制取氢气的装置及方法 |
CN109399564A (zh) * | 2018-11-07 | 2019-03-01 | 中国矿业大学 | 一种直接利用高温焦炉荒煤气制取高纯氢的装置及方法 |
CN111676069A (zh) * | 2020-06-18 | 2020-09-18 | 中冶西北工程技术有限公司 | 焦炉煤气净化系统 |
Families Citing this family (1)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
DE1279699B (de) * | 1963-05-29 | 1968-10-10 | Zd Y Vitezneho Unora Narodni P | Verfahren und Vorrichtung zur Gewinnung eines Gasgemisches |
Citations (4)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
US2293601A (en) * | 1939-07-19 | 1942-08-18 | Air Liquide | Process of production of mixtures of gases hard to liquefy |
US2692484A (en) * | 1950-04-24 | 1954-10-26 | Air Liquide | Separation of gaseous mixtures |
US2729954A (en) * | 1951-08-01 | 1956-01-10 | Air Liquide | Separation of gaseous mixtures |
US2743590A (en) * | 1952-11-29 | 1956-05-01 | Air Liquide | Method for the fractionation of gas mixtures |
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0
- BE BE546755D patent/BE546755A/xx unknown
- NL NL99841D patent/NL99841C/xx active
-
1956
- 1956-04-05 DE DEST11035A patent/DE1014136B/de active Pending
- 1956-04-05 GB GB10477A patent/GB793605A/en not_active Expired
- 1956-04-06 US US576648A patent/US2820769A/en not_active Expired - Lifetime
- 1956-04-06 FR FR1150767D patent/FR1150767A/fr not_active Expired
Patent Citations (4)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
US2293601A (en) * | 1939-07-19 | 1942-08-18 | Air Liquide | Process of production of mixtures of gases hard to liquefy |
US2692484A (en) * | 1950-04-24 | 1954-10-26 | Air Liquide | Separation of gaseous mixtures |
US2729954A (en) * | 1951-08-01 | 1956-01-10 | Air Liquide | Separation of gaseous mixtures |
US2743590A (en) * | 1952-11-29 | 1956-05-01 | Air Liquide | Method for the fractionation of gas mixtures |
Cited By (10)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
US2895304A (en) * | 1955-06-02 | 1959-07-21 | Linde Eismasch Ag | Process and apparatus for gas purification |
US3269130A (en) * | 1957-01-04 | 1966-08-30 | Air Prod & Chem | Separation of gaseous mixtures containing hydrogen and nitrogen |
US3187485A (en) * | 1961-12-13 | 1965-06-08 | Foster Wheeler Corp | Purification of hydrogen by scrubbing with nitrogen at high pressures |
US3407146A (en) * | 1964-01-22 | 1968-10-22 | Linde Ag | Process for the recovery of hydrogennitrogen mixtures with reduced carbon-monoxide content |
DE1626323B1 (de) * | 1964-01-22 | 1970-09-24 | Linde Ag | Verfahren und Vorrichtung zum Gewinnen von kohlenoxidarmem stickstoffhaltigem Wasserstoff |
CN104495749A (zh) * | 2014-12-23 | 2015-04-08 | 东北大学 | 一种利用焦炉荒煤气制取氢气的装置及方法 |
CN104495749B (zh) * | 2014-12-23 | 2016-05-11 | 东北大学 | 一种利用焦炉荒煤气制取氢气的装置及方法 |
CN109399564A (zh) * | 2018-11-07 | 2019-03-01 | 中国矿业大学 | 一种直接利用高温焦炉荒煤气制取高纯氢的装置及方法 |
CN111676069A (zh) * | 2020-06-18 | 2020-09-18 | 中冶西北工程技术有限公司 | 焦炉煤气净化系统 |
CN111676069B (zh) * | 2020-06-18 | 2021-05-04 | 中冶西北工程技术有限公司 | 焦炉煤气净化系统 |
Also Published As
Publication number | Publication date |
---|---|
FR1150767A (fr) | 1958-01-17 |
NL99841C (is") | 1961-07-17 |
GB793605A (en) | 1958-04-16 |
BE546755A (is") | 1956-04-30 |
DE1014136B (de) | 1957-08-22 |
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