CN102281936A - Method and apparatus for separating nitrogen from a mixed stream comprising nitrogen and methane - Google Patents
Method and apparatus for separating nitrogen from a mixed stream comprising nitrogen and methane Download PDFInfo
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- CN102281936A CN102281936A CN2010800044866A CN201080004486A CN102281936A CN 102281936 A CN102281936 A CN 102281936A CN 2010800044866 A CN2010800044866 A CN 2010800044866A CN 201080004486 A CN201080004486 A CN 201080004486A CN 102281936 A CN102281936 A CN 102281936A
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D53/00—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols
- B01D53/02—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols by adsorption, e.g. preparative gas chromatography
- B01D53/04—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols by adsorption, e.g. preparative gas chromatography with stationary adsorbents
- B01D53/0462—Temperature swing adsorption
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D53/00—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols
- B01D53/02—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols by adsorption, e.g. preparative gas chromatography
- B01D53/04—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols by adsorption, e.g. preparative gas chromatography with stationary adsorbents
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D2253/00—Adsorbents used in seperation treatment of gases and vapours
- B01D2253/10—Inorganic adsorbents
- B01D2253/102—Carbon
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D2256/00—Main component in the product gas stream after treatment
- B01D2256/24—Hydrocarbons
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D2259/00—Type of treatment
- B01D2259/40—Further details for adsorption processes and devices
- B01D2259/416—Further details for adsorption processes and devices involving cryogenic temperature treatment
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Abstract
Methods and apparatus for separating nitrogen from a mixed stream (40) comprising nitrogen and methane employing a monolith sorption contactor (2) formed of a unitary construction of active carbon, said contactor (2) housing one or more separation flow channels (2a) intersecting the monolith sorption contactor (2), said one or more separation flow channels having at least one inlet (2b) to, and at least one outlet (2c) from, said contactor (2), said one or more separation flow channels (2a) defining one or more first internal surfaces (2d) of the monolith sorption contactor (2), said contactor (2) further comprising one or more first external surfaces (2e) provided with a barrier layer (2f), said first external surfaces (2e) being different from said first internal surfaces (2d). The mixed stream (40) is passed through at least one of the separation flow channels (2a), where methane is sorbed. The contactor (2) can be regenerated by contacting the contactor (2) with a heat exchange fluid (100) via the barrier layer (2f) at one or more of the external surfaces (2e).
Description
Technical field
The present invention relates to from the mixed flow that comprises nitrogen and methane, isolate the method and the equipment thereof of nitrogen.
Background technology
Some kinds of method and apparatus that are used for shifting out from the mixed flow that comprises nitrogen and methane nitrogen of cicada are such as the flash distillation liquefied natural gas stream.A reason that shifts out nitrogen from mixed flow may be the natural gas that obtains having the heat value (that is the content of energy when the gas combustion) of expectation for the requirement according to concrete gas classification or consumer.
Known a kind of method that is used for shifting out from the mixed flow that comprises nitrogen and methane nitrogen is open U.S. Patent Publication 2008/282885.This U.S. Patent Publication 2008/282885 has announced that a kind of being used for isolate the method for the gas component (such as nitrogen) of first weight from comprising the first heavy gas component (such as nitrogen) and second than the mist of lighter-than-air gas component (such as methane).This first gas component that weighs is absorbed by the micropore absorbent with the form of whole parallel passage contactors.
U.S. Patent Publication 2008/282885 has been announced absorber layer has been coated on the passage of the precast monolithic that is made of non-absorbing material, to be used for the heating absorption process.Also discussed being necessary also to apply pottery or metal glaze or solution-gel coat wall, thereby the gas of the passage that prevents to flow through enters in the main body of precast monolithic with seal channel.Whole contactor also can be provided with and can be used for heating/path or the split tunnel of cooling and absorbing agent.
Being provided with of this precast monolithic that comprises the passage that is coated with absorbent may have to be entered whole main body and keep the fluid of heating and cooling path or passage to separate to prevent gas by glazing, this is provided with needs complicated construction process, thereby cause the contactor price more expensive, if and the coating of separating the heating and cooling passage lost efficacy, and then increased the possibility of operating difficulties.
Summary of the invention
In first aspect, the invention provides a kind of method that is used for isolating nitrogen from the mixed flow that comprises nitrogen and methane, this method may further comprise the steps at least:
(a) the integral body absorption contactor that provides the single structure by active carbon to form, described contactor holds the one or more separated flow passage that runs through whole absorption contactor, described one or more separated flow passage has at least one inlet of feeding described contactor and from least one outlet of described contactor, described one or more separated flow passage defines one or more first inner surfaces of whole absorption contactor, described contactor also comprises one or more first outer surfaces that are provided with barrier layer, and described first outer surface is different with described first inner surface;
(b) mixed flow is fed at least one described one or more separated flow passage via described at least one inlet;
(c) be less than or equal under-60 ℃ the temperature and methane be adsorbed onto in the absorption contactor, so that provide nitrogen-enriched stream in described at least one exit via described one or more first inner surfaces at least one described one or more separated flow passage;
(d) interrupt the path of mixed flow by contactor;
(e) make contactor regeneration by following manner: contactor is contacted with heat-exchange fluid being provided with on described one or more first outer surfaces of barrier layer, contactor being heated to the temperature more than-60 ℃, thereby making the methane desorption and cold heat-exchange fluid stream is provided;
(f) from reclaim the methane of desorption from described at least one outlet of contactor, as methane-rich stream;
Wherein barrier layer is used to provide and prevents that heat-exchange fluid from feeding the fluid barriers in the whole absorption contactor.
On the other hand, the invention provides a kind of equipment that is used for isolating from the mixed flow that comprises nitrogen and methane nitrogen, this equipment comprises at least:
-mixed flow source, this mixed flow source comprise in the mixed flow pipeline and are in the methane and the nitrogen of being less than or equal to-60 ℃ of temperature;
-warm heat-exchange fluid flows the warm heat-exchange fluid stream source in the pipeline;
-cold heat-exchange fluid flows the cold heat-exchange fluid stream source in the pipeline;
-integral body absorption the contactor that forms by the single structure of active carbon, described contactor holds the one or more separated flow passage that runs through whole absorption contactor, described one or more separated flow passage has at least one inlet that is communicated with the mixed flow line fluid and at least one outlet that is communicated with the nitrogen-enriched stream line fluid, described one or more separated flow passage defines one or more first inner surfaces of whole absorption contactor, described contactor also comprises one or more first outer surfaces, described first outer surface is different with described first inner surface, and carries out heat-exchange communication with described warm heat-exchange fluid stream pipeline and described cold heat-exchange fluid stream pipeline;
-barrier layer, described barrier layer are located on described one or more first outer surface, feed the whole fluid barriers that adsorbs in the contactor so that the heat-exchange fluid and the cold heat-exchange fluid that prevent heat to be provided.
Description of drawings
Now with reference to appended non-limitative drawings embodiments of the invention are only described by way of example, in the accompanying drawing:
Fig. 1 demonstrates the schematic diagram of whole absorption contactor;
Fig. 2 demonstrates an embodiment of the exemplary application of whole absorption contactor in method according to an embodiment of the invention;
Fig. 3 demonstrates an embodiment of a kind of exemplary process scheme according to an embodiment of the invention;
Fig. 4 demonstrates an embodiment of the exemplary process stream of the regeneration that is used for whole absorption contactor according to an embodiment of the invention.
Be purpose of description, reference number is assigned to a pipeline and is carried on stream in this pipeline.Identical reference number is represented similar parts, stream or pipeline.
The specific embodiment
At this a kind of method that is used for isolating nitrogen from the mixed flow that comprises nitrogen and methane has been proposed, this method uses the single structure by active carbon to form whole absorption contactor, it does not need the precast monolithic with the absorbent coating, does not perhaps need to handle with the seal channel wall.
Fig. 1 demonstrates a kind of typical whole absorption contactor 2.It is that single structure by absorbing material (for example, active carbon) forms, and it is provided with barrier layer 2f.Contactor holds the one or more separated flow passage 2a that runs through whole absorption contactor 2.As shown in Figure 1, the separated flow passage runs through the end face 2g of whole absorption contactor 2.In the separated flow passage one or more has at least one inlet (2b) and enters flow channel 2a to allow mixed flow.On opposite side, at least one outlet (not shown) is arranged.One or more separated flow passage 2a defines one or more first inner surface 2d of whole absorption contactor 2.Contactor 2 also comprises the one or more first outer surface 2es different with the first inner surface 2d.At least a portion of one or more first outer surface 2e is provided with barrier layer 2f.For clarity sake, the barrier layer 2f among Fig. 1 is shown as and is partly removed, partly to expose the outer surface 2e of whole absorption contactor 2.
The integral body absorption contactor 2 that is formed by the single structure of active carbon as used in this is favourable, and this is because the thermal coefficient of expansion of active carbon is little.This allows in very wide temperature range serviceability temperature change absorption that nitrogen is isolated from mixed flow, makes in the heating and cooling process by the thermal expansion of contactor simultaneously and shrink caused any problem to minimize.
And the amount that is used for the needed adsorbent of heating process methane and nitrogen separated from the mixed flow of methane with selected degree with specific flow rate significantly is lower than traditional heating absorption structure.
Contactor is operated so that nitrogen-enriched stream to be provided by at least a portion of the methane composition in the absorption mixed flow.Then, absorbed methane component is desorption from contactor subsequently, so that methane-rich stream to be provided.Be used in reference to absorption and one of absorb or both at this employed term " absorption ".In a preferred embodiment, for the active carbon absorbent, a kind of molecule or adsorbate (such as methane) have more excellent affinity than second kind of molecule or adsorbate (such as nitrogen).
Integral body is adsorbed contactor to be exposed in the heat-exchange fluid and can to promote desorption to improve its temperature.Before the permission mixed flow enters the separated flow passage (and/or simultaneously), heat-exchange fluid can be used for that also integral body is adsorbed contactor and takes low temperature to.
In context of the present disclosure, " warm heat-exchange fluid " can fingering go into whole absorption contactor with the heat-exchange fluid to its heating, perhaps it can instigate heat-exchange fluid that the cooling of whole absorption contactor produced (in this case, when it entered integral body absorption contactor, its temperature will be higher than initial heat-exchange fluid).Similarly, " cold heat-exchange fluid " can refer to be used for making the whole heat-exchange fluid that contactor warms and produced that adsorbs, and perhaps it can fingering go into whole absorption contactor with the heat-exchange fluid to its cooling.Therefore, the result of adsorbing the contactor heat exchange according to heat-exchange fluid and integral body is warmed or is cooled, and the heat-exchange fluid that whole absorption contactor can form heat respectively flows the part in source and the part that cold heat-exchange fluid flows the source.
Therefore, this method also can comprise an optional step before at step (c):
By in one or more first outer surfaces at least one made the contactor cooling via the contact of the cold heat-exchange fluid of barrier layer stream, thereby produce the heat-exchange fluid stream of heat.
When preparing to carry out adsorption step (c), the cold energy that shifts out from contactor in regeneration step (e) can turn back in the cold contactor.Like this, the cold energy recirculation that is discharged when adsorbent is reproduced is so that cool off contactor subsequently, and makes step (a) minimize to the energy requirement of the sorption cycle of (f), thereby more efficient separation method is provided.This can form contrast with the heating absorption method, and the heating absorption method is by the raise temperature of contactor of heating element heater, and this method may cause contactor to lose cold energy under adsorption temp.
The single structure of active carbon that is used for whole contactor described herein promotes more efficient power conversion so that heating or cooling contactor.Any energy that is used for heating or cools off contactor will change the temperature of acticarbon, and the energy that significantly reduces lost to change the temperature of associated part, and this associated part is such as being shell-type contactor or tubular type contactor or the precast monolithic of pottery or the precast monolithic of metal.
The integral body absorption contactor that uses in this method and equipment is compared with those method and apparatus of prior art has simple structure.It does not need fluid-encapsulated passage so that they are impermeable for mixed flow and/or heat-exchange fluid.It does not need to use precast monolithic in advance yet, and in precast monolithic, adsorbent must be applied in the separated flow passage.What substitute is that barrier layer is arranged on whole one or more second outer surfaces.It is a kind of simple technology that barrier layer is applied to that whole outer surface compares with the inner surface that barrier layer is applied to the separated flow passage, and has reduced the possibility that barrier layer lost efficacy in operating process.
It also is favourable that the single structure of contactor is compared with non-single structure or precast monolithic, because it reduces the energy requirement of separation method, non-single structure for example is micrometeor reactor (such as shell-type reactor or a tubular reactor), it holds specific adsorbent in pipe, precast monolithic has the adsorbent coating on the separated flow passage.These prior art constructions comprise non-adsorptivity parts (such as metal shell-type and tubular reactor, perhaps metal precast monolithic or ceramics preparative integral body), and these structures also must be heated or cooled in the alternating temperature absorption process, thereby need extra energy.
Adsorbent described herein is an active carbon.Activation charcoal or active carbon processedly think that it provides the charcoal of high surface area to form by a kind of, and it can be effective for the absorbing molecules individuality.Can surpass 500 meters squared per gram for the effective BET surface area of absorption, this is to determine by the known BET surface area measuring method of prior art, uses P/P such as the adsorptivity of nitrogen under liquid-nitrogen temperature
0(relative pressure/steam pressure) is that 0.08,0.14,0.20 multiple spot pressure is measured, and the absorption analysis instrument of use for example is the TriStar 3000 of Micromeritics Instrument Corp. U.S.A.BET surface area test method is at Brunauer, S.Emmett, P.H.﹠amp; Teller proposes among E.in " Adsorption of gases in multimolecular layers (gas absorption in the polymolecular layer) " J.Am.Chem.Soc.60, pp.309-319 (1938) and description.
The single configuration of whole absorption contactor preferred mainly by active carbon or optionally in other adsorbent and the production process accidental impurity form.More preferably, the single configuration of whole absorption contactor mainly is made up of impurity accidental in active carbon and the production process.Therefore, this whole contactor is structurally different with those contactors of prior art, and those contactors of prior art are formed by the prefabricated integral body of metal or ceramic material, have the passage that is coated with active carbon.
Whole absorption contactor can have any desired shape, and is triangular prism shaped such as clavate, quadrangular etc.The clavate contactor is preferred because these contactor is the easiest is attached in the separative element.
Contactor comprises one or more separated flow passage.Preferably, this separated flow passage extends through contactor along its longest dimension (vertically).The flow separation passage is a substantial linear.The flow separation passage can have various cross sections, such as annular, triangle, quadrangle, pentagon, hexagon, heptagon, octagon etc.The fluid passage defines first inner surface of contactor along one or more walls of its length.
Contactor also comprises one or more outer surfaces, vertically surperficial and two rounded end surfaces such as the tubulose of clavate contactor, perhaps three of triangular prism shaped contactor vertically surperficial and two triangle end surfaces of rectangle.One or more at least a portion in these outer surfaces is provided with (suitably being coated with) barrier layer (such as epoxy coating), so that one or more first outer surfaces with barrier layer are provided.As discussed below, barrier layer is used to provide fluid barriers, is sent in the main body of contactor to reduce (more preferably preventing) heat-exchange fluid.As a result, be apparent that heat-exchange fluid should only be provided for those outer surfaces with barrier layer of contactor.
The integral body absorption contactor that is formed by the single structure of active carbon for example can be by such as NOVACARB
TM(UK) phenolic resins is made for MAST Carbon Technology, Guildford.Integral body can provide by following manner: by squeeze, before pressure and/or molded method form the 3D shape of expectation, controlled curing, thereafter by grind with classification so that the macrostructure of expectation to be provided, follow by charing and activation step.A kind of appropriate preparation method is disclosed in following article: " Phenolic-resin-derived activated carbons (by the active carbon of phenolic resins generation) ", Applied Catalysts A:General 173 (1998), pages 289-311.
Have been found that using extremely simple method discussed above and/or equipment to provide isolates one or more hydrocarbon components (such as methane) expeditiously from mixed flow.It provides nitrogen-enriched stream, and this nitrogen-enriched stream is easier to be processed, as is discharged in the atmosphere, and need not any processing or any a large amount of further processing.
Method discussed above and/or equipment can provide methane-rich stream (or poor nitrogen stream) to be used for continuous the use by making the regeneration of whole absorption contactor after adsorbed methane and other heavier hydrocarbon component.The comparable original mixed flow of methane-rich stream uses more expeditiously.For example, the recompression of methane-rich stream (be poor nitrogen stream and can mainly comprise methane and one or more other hydrocarbon) since nitrogen content reduce and carry out more efficiently.The compressed hydrocarbon of any of these can for example be used as fuel or hydrocarbon product.Alternatively, methane-rich stream can be liquefied so that the hydrocarbon stream of liquefaction to be provided, such as liquefied natural gas (LNG).
Like this, can significantly reduce the Capital expenditure (CAPEX) and the operating cost of subsequent treatment methane-rich stream.
In addition, because the simplicity and the high efficiency of method disclosed herein and/or equipment, expect that it compares with known apparatus for production line (line-ups) very strong durability is arranged.
Fig. 2 demonstrates first embodiment of the whole absorption of the typical case contactor 2 as shown in Figure 1 that is used for method disclosed herein and/or equipment.Contactor shows with longitudinal cross-section.The mixed flow 40 that comprises nitrogen and methane arrives whole absorption contactor 2 through mixed flow decompressor 45 (all valve and/or hydraulic turbine units as shown).Nitrogen will can be stream any gaseous state, liquid or partial condensation or evaporation from isolated mixed flow 40 wherein, suitably is derived from naturally, more preferably is the stream that is derived from liquefied natural gas, suitably is the form of flash vapor stream.
As known in the art, liquefied natural gas stream can have various compositions.Usually, be evaporated or the liquefied natural gas stream of flash distillation mainly comprises methane, for example comprise 60-65mol% (mole percent) methane at least.Flash vapors is rich in the component with some low boiling temperatures usually, and methane content can be between 40mol% to 70mol%, and more typically, methane content is between the 40mol% to 60mol%, and this depends on the concentration such as the low boiling component of nitrogen.
Liquefied natural gas stream can comprise the hydrocarbon that overweights methane of different content, and comprises other non-hydrocarbon compound, such as nitrogen, helium and hydrogen.Any hydrocarbon that overweights methane can be adsorbed by acticarbon with methane.
According to the difference in source, mixed flow 40 also can comprise the compound of different amounts, such as water, carbon dioxide, hydrogen sulfide and other sulfide etc.But, if mixed flow is by the mixed flow of (in advance) liquefaction, such as liquefied natural gas, then these compositions of back have been removed usually basically, because otherwise they are frozen, thereby cause obstruction and relevant issues in the liquefaction device in liquefaction process.Because do not expect that for liquefaction step and for removing the step of component (such as water, carbon dioxide and hydrogen sulfide) is known to those skilled in the art, so be not further discussed at this.
The active carbon that forms whole absorption contactor 2 is as methane adsorbate and any than the heavy hydrocarbon adsorbent of (if present).Preferably active carbon is an active carbon at least 5 times of the affinity of nitrogen adsorbate to the affinity of methane adsorbate.
Adsorption step is being less than or equal under-60 ℃ the temperature and is being carried out.Do not wish bound by theory, think that active carbon is best to methane and any other absorption affinity than the heavy hydrocarbon component in the about 100 ℃ of scopes of the dew point of methane component, for example in-165 ℃ to-60 ℃ scopes, preferably in-160 ℃ to-60 ℃ scopes.
Under the situation that at least a portion that is cooled to the adsorption temp scope at contactor 2 provides by mixed flow 40, mixed flow for example can be the liquefied natural gas stream from the partial condensation of liquefaction unit, and can have the temperature between-165 ℃ to-140 ℃.If mixed flow is used for cooling contactor 2 before absorption, then Liu this part can be recycled to liquefaction unit and liquefied before returning the contactor that is cooled now 2 that is used to separate being used for again.
Fig. 2 also demonstrates one or more separated flow passage 2a, and they are through the main body of contactor 2.The wall 2d of separated flow passage thereby form by acticarbon.
In case contactor is cooled to adsorption temp, mixed flow 40 flows to one or more inlet 2b of one or more separated flow passage 2a, is fit to flow into via optional inlet house steward 12.At least a portion of methane in the mixed flow will absorb via inner surface 2d contactor 2 through separated flow passage 2a the time, and this inner surface is formed by active carbon.
In a preferred embodiment, near or equal to provide mixed flow 40 under the adsorption temp of contactor 2, that is, be less than or equal under-60 ℃ the temperature mixed flow 40 be provided.If provide mixed flow 40 under the temperature of adsorption temp being higher than, its adsorption temp of will having to be pre-cooling to then, perhaps contactor 2 will be frozen to keep temperature to be in the adsorption range.Can carry out the freezing of contactor 2 by the heat-exchange fluid that is used to that contactor 2 is warmed and cools off contactor 2, hereinafter will go through.
When contactor 2 during near the absorbent full load (such as there being methane or any than heavy hydrocarbon), mixed flow decompressor 45 can be closed, and continues to flow into contactor 2 thereby interrupt mixed flow 40.So contactor 2 can be reproduced to discharge adsorbed methane or any than the heavy hydrocarbon component, as methane-rich stream 80.
After the mixed flow 40 that flows to contactor 2 is interrupted and before regeneration, preferably make bodies for purifying fluids stream through one or more separated flow passage 2a.For example, bodies for purifying fluids stream can enter one or more inlet 2b of fluid passage 2a along first auxiliary line 75.Bodies for purifying fluids can and anyly remove any residual component (such as nitrogen and unabsorbed methane) the mixed flow from separated flow passage 2a before than the heavy hydrocarbon component at desorption methane.Can leave fluid passage 2a via outlet 2c with the bodies for purifying fluids stream of crossing, and from contactor 2, shift out by the second auxiliary line (not shown).Also can expect the bodies for purifying fluids of adverse current, wherein bodies for purifying fluids stream flows to fluid passage inlet 2b from fluid passage outlet 2c via second and first auxiliary line.
After optional purifying step, contactor 2 can absorb by alternating temperature/adsorb and regenerate.The temperature of contactor 2 is lifted to be less than or equal to more than-60 ℃ the methane adsorption temperature range, with desorption methane and any than heavy hydrocarbon.The component of desorption can be left one or more separated flow passage 2a at outlet 2c place, and shifts out from separator 2 as being rich in methane fluid 80.The methane-rich stream optional outlet header 13 that also can flow through.
In a preferred embodiment, methane-rich stream 80 shifts out from contactor 2 under the pressure that reduces, to promote methane and any desorption than the heavy hydrocarbon adsorbate.Alternatively, flush fluid stream (such as methane-rich stream itself) can be fed into separated flow passage 2a via the auxiliary intake pipeline 75 of contactor 2 after optionally compressing, to shift out the hydrocarbon of any residual desorption.If flush fluid stream is not made of methane-rich stream, then it can withdraw from the pipeline (not shown) and shift out via auxiliary from the outlet 2c of separated flow passage 2a, pollutes methane-rich stream 80 so that prevent with flush fluid.
Heat exchange flow body cavity 11 can be configured to the vertical outer surface 2e around contactor 2, and it can be filled with heat-exchange fluid.Warm heat-exchange fluid 100 can enter the heat exchange flow body cavity or leave the heat exchange flow body cavity via warm heat exchange flow fluid line 100, and cold heat-exchange fluid 110 can leave the heat exchange flow body cavity via cold heat exchange flow fluid line 110 respectively and enter the heat exchange flow body cavity.Preferably, there is barrier layer 2f in any position on the outer surface 2e of heat exchange flow body cavity 11 inside.At contactor 2 is among the embodiment of clavate, and heat exchange flow body cavity 11 can be an annular chamber.
As an example, the outer surface 2e of contactor 2 can limit pipe, and this pipe is coated with barrier layer 2f.By this way, contactor 2 can be maximized by the outer surface 2e area of warm heat-exchange fluid 100 heating, keep the heat-exchange fluid and the annular end 2g of contactor 2 to separate simultaneously, one or more inlet 2b of annular end 2g and separated flow passage 2a are adjacent with one or more outlet 2c.
The temperature of contactor 2 can be during desorption contacts with heat-exchange fluid 100 at the one or more first outer surface 2e places with barrier layer 2f by contactor 2 and is raised.Allow heat-exchange fluid to contact in the surface that it deviates from the outer surface 2e that is provided with barrier layer 2f with barrier layer 2f.
Heat-exchange fluid stream is preferably warmer, as preferably having the temperature higher than the temperature of contactor 2.Barrier layer 2f is provided for preventing that heat-exchange fluid from arriving the main body of contactor 2 and preventing to pollute separated flow passage 2a.Preferred barrier layer is an epoxy resin.The outer surface 2e (being provided with barrier layer 2f) that warm heat-exchange fluid 100 is supplied to contactor 2 is favourable, and this is because it has simplified the structure of contactor 2.
The outer surface 2e that barrier layer 2f is applied to contactor 2 is direct process forward.Will not be applied to all outer surfaces of contactor 2 by barrier layer, be applied to those surfaces that can contact with heat-exchange fluid as long as can satisfy.Therefore, in the embodiment shown in Figure 2, will barrier layer be applied to inlet 2b and the adjacent end outer surface 2g of outlet 2c with separated flow passage 2a, this is to separate because of these positions and heat-exchange fluid.In an illustrated embodiment, barrier layer 2f only needs to be applied to vertical outer surface 2e.
If inner hot switching path will be set in the main body of contactor, then these hot switching paths are had to processedly to seal their wall, prevent that heat-exchange fluid from seeing through to pollute contiguous separated flow passage 2a.This is the process of a complexity, need seal the wall of these hot switching paths with pottery or metal glaze.Alternatively, have to be provided with the precast monolithic with separated flow passage and hot switching path, wherein the separated flow passage has to be coated with one deck adsorbent layer, has increased the cost of the integral body absorption contactor of finishing and the complexity of manufacturing operation again.Therefore provide lot of advantages in simple structure and use aspect easy at this employed contactor.
Warm heat-exchange fluid 100 is provided under the temperature more than the adsorption temp of contactor 2, as more than-60 ℃, preferably is being equal to or higher than under-50 ℃ the temperature, even more preferably be equal to or higher than under-40 ℃ the temperature.For example, the temperature of Nuan heat-exchange fluid 100 can be at ambient temperature or approximately-10 ℃ to 0 ℃.In some cases, temperature also can be in-40 ℃ to-30 ℃ scope, for example, and in using the liquefied natural gas (LNG) production process also under the situation as the stream of cold-producing medium stream.The temperature of warm heat-exchange fluid stream 100 is lowered after the barrier layer with contactor 2 contacts, to provide (being cooled) heat-exchange fluid that is colder to flow the cold heat-exchange fluid stream of 110 forms, meanwhile the temperature of contactor 2 is raised to promote desorption.
Be apparent that cold heat-exchange fluid stream 110 has the required cold energy of adsorption step of contactor 2.Therefore, after heated contactor 2 regeneration, cold heat-exchange fluid 110 be that a part (preferably all parts) can be used to temperature with contactor 2 and is reduced to and meets the desired temperature of adsorption operations at least, this is by (perhaps cold heat-exchange fluid being returned processing procedure via pipeline 100 circulations in the contactor 2 that cold heat-exchange fluid stream 110 is backflowed, thereby the maintenance flow direction, but use warm heat exchange flow fluid line to supply cold heat-exchange fluid and use cold heat exchange flow fluid line to shift out the heat-exchange fluid that warms) realize.By this way, contactor 2 can be placed the required cold energy of absorption mode be recycled to contactor after each regenerative operation, thereby improve the efficient of this method and apparatus.
Therefore, can provide absorption and regeneration cycle by following manner: utilize heat-exchange fluid cold energy to be shifted out and turns back to contactor.Therefore, be fed into contactor 2 with before being used for adsorption step at mixed flow 40, contactor 2 can be cooled by among the one or more first outer surface 2e with barrier layer 2f at least one contact with cold heat-exchange fluid stream 110, thereby provides warm heat-exchange fluid to flow 100.
In a preferred embodiment, two or more contactors 2 can be arranged in parallel, so that when contactor 2 during near full load, mixed flow 40 can flow to second contactor (not shown) that does not add load, so that can realize the continuous processing of mixed flow 40.
Therefore, whole absorption contactor 2 can be used as the part of contact unit, this contact unit forms any suitable equipment, system or the device that comprise one or more whole absorption contactors, can optionally absorb methane and any than heavy hydrocarbon from mixed flow.It will be understood by those of skill in the art that contact unit can have a lot of forms, comprise one or more series connection, in parallel or not only connected but also one or more whole absorption contactors in parallel.
For example, have at least one whole absorption contactor and be in absorption mode, and have at least one whole absorption contactor to be in regeneration or desorption pattern.According to actual needs, may be two, three, four or more a plurality of whole combination of adsorbing contactors, one of them is in absorption mode, other the different phase that is in regeneration or desorption pattern.
A plurality of whole absorption contactors are produced by transmitting the possibility that heat-exchange fluid recovers energy from a contactor to another contactor in the different phase operation of circulation.Like this, the cold energy that belongs to one of contactor of entering in the regeneration mode can be saved by using it to cool off other whole contactor.
Fig. 3 schematically demonstrates and is used for thus, obtaining having the methane-rich stream 80 of higher heat value from isolate the processing scheme of nitrogen from the mixed flow that comprises nitrogen and methane 40 of liquefied natural gas.
The processing scheme of Fig. 3 comprises that whole absorption contactor 2 (can also be a contact unit that comprises one or more whole absorption contactors), gas/liquid separation 3, expansion gear 4 (such as turbo-expander), second decompressor 5 (such as Joule-Thomson valve), liquefaction unit 6 (comprise one or more heat exchanger (not shown) that are associated with kind of refrigeration cycle, pump 7 and fluid reservoir 8 (such as natural gas storage tank).Those skilled in the art will appreciate that if necessary and can have other element.
In operation, liquefaction unit 6 produces the hydrocarbon stream 10 of partial liquefaction (preferably liquefaction fully) at least, such as liquefied natural gas stream.The hydrocarbon stream 10 of this partial liquefaction at least is inflated in expansion gear 4 with the hydrocarbon stream 20 that expansion is provided, and process decompressor 5 is to provide controlled expansion hydrocarbon stream 30 subsequently, and it may be the liquefied natural gas stream of partial condensation.So controlled expansion hydrocarbon stream 30 flows to first inlet 31 of gas/liquid separation 3, gas-liquid separator 3 can be the terminal flash vessel.Typically, controlled expansion hydrocarbon stream 30 can cling to between 10 crust 0.5 at the pressure at inlet 31 places, more preferably between 1 crust clings to 5, even more preferably between 1 crust clings to 2.The inlet temperature of gas/liquid separation 3 can be between-165 ℃ to-140 ℃.When stream 30 when being the liquefied natural gas stream of partial condensation, it can comprise approximately greater than the methane peace treaty of the 80mol% nitrogen greater than 1mol%.
In gas/liquid separation 3, controlled expansion hydrocarbon stream 30 is separated into the overhead stream (shifting out from exporting 32) of gaseous state and liquid bottom stream 50 (shifting out from exporting 33), and the overhead stream of this gaseous state is the mixed flow 40 that comprises nitrogen and methane.
Liquid bottom stream 50 is rich in methane than stream 30, and comprises the major part of controlled expansion hydrocarbon stream 30 usually.Use pump 7 bottom of liquid state can be flowed 50 as flowing 60 pumps in fluid reservoir 8 (such as LNG tank).Liquid bottom stream temporarily is stored in the fluid reservoir 8.
Processing scheme at Fig. 3 is positioned under the situation of liquefied natural gas outlet terminal, and the liquefied natural gas that is stored in the jar can be loaded onto (not shown) in the cask subsequently, transports to external then.Form in the processing scheme of Fig. 3 under the situation of a part of regasification terminal (at the liquefied natural gas input position, usually supply with by cask at this place's liquefied natural gas, rather than by gasification unit 6 supplies), the liquefied natural gas in the jar 8 flows to the vaporizer (not shown) subsequently.
Because the effect of gas/liquid separation 3, the nitrogen in the stream 30 help upwards flowing out by exporting 32.Therefore, be provided at the gaseous state overhead stream that outlet 32 places of separator 3 shifts out as the mixed flow 40 that comprises nitrogen and methane.This stream 40 flows to the inlet 21 of whole absorption contactor 2.Usually, stream 40 comprises greater than 15mol% or greater than the nitrogen of 25mol%, such as between the 30mol% to 60mol%.
By during the contactor 2, be present in the acticarbon absorption at least a portion (especially methane) contactor 2 in one or more hydrocarbon in the mixed flow 40 at mixed flow 40; And nitrogen phase most of at least continue by and shift out from contactor 2 at outlet 22 places.This nitrogen-enriched stream is collected with as nitrogen-enriched stream 70.
Be collected with after as stream 70 at nitrogen-enriched stream as mentioned above, the hydrocarbon of the charcoal absorption in the contactor 2 can carry out desorption, thereby makes contactor 2 regeneration.This uses the heating adsorption/absorption to carry out, and introduces flushing flow usually, purifies stream and heat exchange flow etc., so that remove the hydrocarbon of desorption from acticarbon.The desorption hydrocarbon shifts out at outlet 23 places, perhaps directly collected, perhaps be collected after Purge gas is separated with as methane-rich stream (poor nitrogen) 80.Stream 80 can be used as fuel.Alternatively, stream 80 can reconfigure with liquefied natural gas stream 50, is compressing for the first time and is reconfiguring after the fluidized flow 80 more alternatively.
One skilled in the art should appreciate that outlet 22 and 23 can be outlet or the same outlet that separates.And what one skilled in the art should appreciate that a contactor 2 of replacement is to use several contactors in parallel.Moreover several contactors (comprise different sorbing materials, wherein at least one is the integral body absorption contactor that the single structure by active carbon described herein forms) also can in series be laid so that can separate one or more and plant other stream (nitrogenous).
Can be subjected to the manner known in the art influence from the cold energy recovery in nitrogen-enriched stream 70 and/or the poor nitrogen stream 80.For example, nitrogen-enriched stream 70 can flow into first cold energy recovery unit (not shown) in further processing or row before atmosphere.Simultaneously, methane-rich stream 80 can reclaim the unit (not shown) so that the stream that warms to be provided through second cold energy, this stream that warms then through compressor so that the hydrocarbon stream of compression to be provided, the hydrocarbon stream of this compression can be used as fuel, perhaps even be recycled to (not shown) in the hydrocarbon liquefaction device.
Directly place at contactor 2 under the situation of gas/liquid separation 3 back, the condition (clinging to and-160 ℃ as 1) that flows to the mixed flow of one or more separated flow passage in the contactor 2 is optimised for the alternating temperature adsorption/absorption technology that is used for desorption.The cold energy of nitrogen-enriched stream 70 can be used to technology, and nitrogen-enriched stream can be arranged to atmosphere afterwards.Simultaneously, methane is absorbed on the active carbon.
Owing to the arts demand energy still less that liquefies again than prior art of one or more desorption hydrocarbon (such as methane) further advantage is arranged at this disclosed method and apparatus, this is because the nitrogen cryogenic separation process that no longer needs to carry out simultaneously thereupon.
In first alternate embodiments of layout shown in Figure 3, contactor 2 can place before the gas/liquid separation 3, so that isolate nitrogen from the controlled expansion hydrocarbon stream as mixed flow, this mixed flow is directly to be expanded by the one or many of the hydrocarbon stream of partial liquefaction (such as liquefied natural gas) at least to obtain usually.
Fig. 4 schematically shows a processing scheme isolating nitrogen from the mixed flow 40 that comprises nitrogen and methane according to another embodiment described herein.In the mode similar to the mode of having discussed, gas/liquid separation 3 (such as the end flash separator) can provide the top mixed flow 40 that comprises methane and nitrogen from suitable supply flow (such as the liquefied natural gas 30 of partial condensation).
As see figures.1.and.2 discuss, mixed flow 40 can be through whole absorption contactor 2 to be used for nitrogen and methane and anyly to be separated into nitrogen-enriched stream 70 and methane-rich stream 80 than the heavy hydrocarbon component.
In the embodiment shown in fig. 4, the heat-exchange fluid that is used for changing contactor 2 temperature can be a cold-producing medium, this cold-producing medium can provide from refrigerant loop, the refrigerant loop of the cooling stage of the liquefaction unit that refrigerant loop preferably is associated, for example, under the situation of natural gas processing, be liquefaction unit 6 according to Fig. 3.
For example, heat-exchange fluid can be the propane of liquid state or gaseous state, for example from the pre-cooled circulation of liquefaction unit, perhaps comes the hot mix refrigerant of the low temperature heat exchanger that is used for natural gas liquefaction under comfortable-40 ℃ to-30 ℃ temperature.
Fig. 4 demonstrates refrigerant loop, and this refrigerant loop comprises: the refrigeration compressor 9 that has the driver D1 that is associated; With cooler 10 (such as aerial cooler or water cooler), this cooler has been incorporated into heat-exchange fluid has been sent in the loop of contactor 2.
The warm heat-exchange fluid 100 that is produced by cooling contactor 2 can flow to coolant compressor 9, perhaps is used for subsequently heating contactor 2 so that the methane of contactor 2 absorption and anyly regenerate than the heavy hydrocarbon component.
If warm heat-exchange fluid 100 flows to coolant compressor 9, then heat-exchange fluid 100 is compressed the heat-exchange fluid 95 so that compression to be provided.The heat-exchange fluid 95 of this compression is cooled in cooler 10 then, and so that cold heat-exchange fluid stream 110 to be provided, this cold heat-exchange fluid stream can be used to cooling or preferably makes natural gas flow liquefaction; Perhaps flow to contactor 2 and be reduced to adsorption range, thereby warm heat-exchange fluid 100 is provided with temperature with contactor 2.
If mixed flow is in higher temperature, then such flow process also can be used to make contactor 2 to remain on the adsorption temp scope, although this embodiment is not preferred, so task refrigerant loop because the required cooling task of contactor is divided.
Alternately, can be used for natural gases cooling in the liquefaction process, perhaps be stored so that after finishing regenerative operation, contactor 2 is cooled to adsorption temp by contactor 2 being heated to cold heat-exchange fluid stream 110 that desorption temperature produces.
Preferably, the methane-rich stream of desorption is cooled and is liquefied.There are multiple choices to be used for realizing such liquefaction again: for example by initial supply flow being recycled to liquefaction system (as the liquefaction unit 6 of Fig. 3).Preferably, in regeneration mode, use the cold heat-exchange fluid stream of the integral body absorption contactor that is derived from the same whole absorption contactor that is heated by heat-exchange fluid and/or is arranged in parallel to liquefy from the methane-rich stream of integral body absorption contactor.This cold refrigerant fluid can at first be inflated, and exchanges in lower pressure levels to be the cooling of methane rich fluid with the methane-rich stream body heat again.
In another the alternative embodiment that arranges shown in the accompanying drawing, contactor 2 can be arranged in the gaseous state mixed flow stream of the nitrogen that comprises hydrocarbon (comprising methane) and high concentration, thereby is included in the stream under the high pressure (for example less than 70 crust).
Those skilled in the art will appreciate that under the situation of the scope that does not depart from appended claims and can implement the present invention in many ways.
Claims (16)
1. method that is used for isolating nitrogen from the mixed flow that comprises nitrogen and methane, this method may further comprise the steps at least:
(a) the integral body absorption contactor that provides the single structure by active carbon to form, described contactor holds the one or more separated flow passage that runs through whole absorption contactor, described one or more separated flow passage has at least one inlet of feeding described contactor and from least one outlet of described contactor, described one or more separated flow passage defines one or more first inner surfaces of whole absorption contactor, described contactor also comprises one or more first outer surfaces that are provided with barrier layer, and described first outer surface is different with described first inner surface;
(b) mixed flow is fed at least one described one or more separated flow passage via described at least one inlet;
(c) be less than or equal under-60 ℃ the temperature and methane be adsorbed onto in the absorption contactor, so that provide nitrogen-enriched stream in described at least one exit via described one or more first inner surfaces at least one described one or more separated flow passage;
(d) interrupt the path of mixed flow by contactor;
(e) make contactor regeneration by following manner: contactor is contacted with heat-exchange fluid being provided with on described one or more first outer surfaces of barrier layer, contactor being heated to the temperature more than-60 ℃, thereby making the methane desorption and cold heat-exchange fluid stream is provided;
(f) from reclaim the methane of desorption from described at least one outlet of contactor, as methane-rich stream;
Wherein barrier layer is used to provide and prevents that heat-exchange fluid from feeding the fluid barriers in the whole absorption contactor.
2. method according to claim 1 is wherein carried out under the temperature of adsorption step (c) in the scope from-160 ℃ to-60 ℃.
3. according to each the described method in the aforementioned claim, the regeneration in the step (e) is elevated to the temperature in the scope from-40 ℃ to-30 ℃ by the temperature with contactor.
4. according to each the described method in the aforementioned claim, described method also comprises by making nitrogen-enriched stream cool off contactor through one or more in the described one or more separated flow passage.
5. according to each the described method in the aforementioned claim, described method also is included in step (c) optional step before:
Contact with cold heat-exchange fluid stream by in described one or more first outer surfaces that will have barrier layer at least one and to cool off contactor, thereby provide warm heat-exchange fluid to flow.
6. according to claim 4 and/or 5 described methods, wherein cool off contactor and the temperature of contactor is reduced to is less than or equal to-60 ℃.
7. according to each the described method in the aforementioned claim, wherein barrier layer comprises epoxy resin.
8. according to each the described method in the aforementioned claim, wherein mixed flow is derived from liquefaction unit, and heat-exchange fluid is the cold-producing medium from described liquefaction unit.
9. according to each the described method in the aforementioned claim, wherein step (e) also comprises and makes flush fluid stream through described one or more separated flow passage.
10. according to each the described method in the aforementioned claim, described method also is included between step (d) and the step (e) and makes the step of bodies for purifying fluids by described one or more separated flow passage.
11. according to each the described method in the aforementioned claim, wherein mixed flow obtains from gas/liquid separation, described gas/liquid separation provides the hydrocarbon stream and the liquid hydrocarbon stream of gaseous state, and this liquid hydrocarbon stream is liquefied natural gas preferably.
12. method according to claim 10, wherein at least a portion in the hydrocarbon stream of gaseous state contacts with active carbon as mixed flow.
13. according to one in the aforementioned claim or multinomial described method, wherein mixed flow is under the temperature below 0 ℃, preferably is in-30 ℃ ,-100 ℃, the temperature below-140 ℃ or-150 ℃.
14. according to one in the aforementioned claim or multinomial described method, wherein mixed flow is under the pressure of being less than or equal to 10 crust, preferably is under the pressure of 1 crust to the 2 crust scopes.
15. according to one in the aforementioned claim 11 to 14 or multinomial described method, wherein at least a portion in the mixed flow is liquefied in gas/liquid blender upstream.
16. an equipment that is used for isolating from the mixed flow that comprises nitrogen and methane nitrogen, described equipment comprises at least:
-mixed flow source, this mixed flow source comprise in the mixed flow pipeline and are in the methane and the nitrogen of being less than or equal to-60 ℃ of temperature;
-warm heat-exchange fluid flows the warm heat-exchange fluid stream source in the pipeline;
-cold heat-exchange fluid flows the cold heat-exchange fluid stream source in the pipeline;
-integral body absorption the contactor that forms by the single structure of active carbon, described contactor holds the one or more separated flow passage that runs through whole absorption contactor, described one or more separated flow passage has at least one inlet that is communicated with the mixed flow line fluid and at least one outlet that is communicated with the nitrogen-enriched stream line fluid, described one or more separated flow passage defines one or more first inner surfaces of whole absorption contactor, described contactor also comprises one or more first outer surfaces, described first outer surface is different with described first inner surface, and carries out heat-exchange communication with described warm heat-exchange fluid stream pipeline and described cold heat-exchange fluid stream pipeline;
-barrier layer, described barrier layer are located on described one or more first outer surface, lead to the whole fluid barriers that adsorbs in the contactor so that the heat-exchange fluid and the cold heat-exchange fluid that prevent heat to be provided.
Applications Claiming Priority (3)
| Application Number | Priority Date | Filing Date | Title |
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| EP09150637 | 2009-01-15 | ||
| EP09150637.8 | 2009-01-15 | ||
| PCT/EP2010/050320 WO2010081809A1 (en) | 2009-01-15 | 2010-01-13 | Method and apparatus for separating nitrogen from a mixed stream comprising nitrogen and methane |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN102281936A true CN102281936A (en) | 2011-12-14 |
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| CN2010800044866A Pending CN102281936A (en) | 2009-01-15 | 2010-01-13 | Method and apparatus for separating nitrogen from a mixed stream comprising nitrogen and methane |
Country Status (5)
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| US (1) | US20110296871A1 (en) |
| CN (1) | CN102281936A (en) |
| AU (1) | AU2010205669B2 (en) |
| GB (1) | GB2478488B (en) |
| WO (1) | WO2010081809A1 (en) |
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| CN105363316A (en) * | 2015-11-24 | 2016-03-02 | 工业和信息化部电子第五研究所 | Adsorption device and drying device for automobile VOC detection |
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- 2010-01-13 CN CN2010800044866A patent/CN102281936A/en active Pending
- 2010-01-13 US US13/144,322 patent/US20110296871A1/en not_active Abandoned
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| CN105363316A (en) * | 2015-11-24 | 2016-03-02 | 工业和信息化部电子第五研究所 | Adsorption device and drying device for automobile VOC detection |
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Also Published As
| Publication number | Publication date |
|---|---|
| WO2010081809A1 (en) | 2010-07-22 |
| US20110296871A1 (en) | 2011-12-08 |
| GB2478488A (en) | 2011-09-07 |
| AU2010205669A1 (en) | 2011-07-28 |
| AU2010205669B2 (en) | 2013-03-28 |
| GB2478488B (en) | 2013-10-30 |
| GB201111264D0 (en) | 2011-08-17 |
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