CN104528647A - Method and device for preparing hydrogen and high-purity carbon monoxide by separating synthetic gas - Google Patents
Method and device for preparing hydrogen and high-purity carbon monoxide by separating synthetic gas Download PDFInfo
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- CN104528647A CN104528647A CN201510014562.6A CN201510014562A CN104528647A CN 104528647 A CN104528647 A CN 104528647A CN 201510014562 A CN201510014562 A CN 201510014562A CN 104528647 A CN104528647 A CN 104528647A
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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
- F25J3/0223—H2/CO mixtures, i.e. synthesis gas; Water gas or shifted synthesis gas
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- 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
- F25J3/0233—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 CnHm with 1 carbon atom or more
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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
- F25J3/0252—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 hydrogen
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- 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
- F25J3/0257—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 nitrogen
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- 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
- F25J3/0261—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 carbon monoxide
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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
- F25J2200/72—Refluxing the column with at least a part of the totally 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
- F25J2235/00—Processes or apparatus involving steps for increasing the pressure or for conveying of liquid process streams
- F25J2235/02—Processes or apparatus involving steps for increasing the pressure or for conveying of liquid process streams using a pump in general or hydrostatic pressure increase
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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
- F25J2270/14—External refrigeration with work-producing gas expansion 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
Abstract
The invention provides a method for preparing hydrogen and high-purity carbon monoxide by separating synthetic gas. The synthetic gas is pretreated mixed gas. The method comprises the steps that H2 and low-boiling-point impurities are separated from a tower top through rectification to be obtained, CH4, O2 and high-boiling-point impurities are separated from a tower pot through second-time rectification to be obtained, N2 and remaining high-boiling-point impurities are separated from the tower top through third-time rectification to be obtained, and CO is separated from the tower pot through third-time rectification to be obtained, wherein the energy transfer process accompanying with the separation process is implemented through heat absorption and heat release of a circulation loop of the N2 obtained through separation. The invention further provides a device of the method. The device mainly comprises continuous rectification equipment composed of a dehydrogenation tower C1, a deoxygenation and demethanization tower C2 and a denitrification tower C3, and associated equipment used for achieving energy transfer. The method and device overcome the defects of a traditional method, reduce equipment input, lower energy consumption, increase the added value of the product and achieve the effect of circular economy.
Description
Technical field
The present invention relates to a kind of method of gas delivery, particularly relate to a kind of method of being carried out gas delivery by cryogenic liquefying effect, particularly, relate to the method and apparatus that a kind of synthetic gas is separated hydrogen making and high-purity CO.
Background technology
Along with the development of Chinese large-sized chemical field, with Sweet natural gas, coal and other hydrocarbon polymer for raw material carries out the total amount of the synthetic gas that steam reforming catalyzed conversion or partial oxidation produce also in sharp increase, except containing the carbon monoxide fully do not transformed in these synthetic gas, also usually containing hydrogen, nitrogen, methane, oxygen and carbonic acid gas etc.Due to impurity composition diversified in synthetic gas, often limit its further use, in large number situation, have every day a large amount of mixed gass can only to burn in vain emptying, cause the waste of resource and the aggravation of Greenhouse effect.
In fact, highly purified gas has become important basic chemical feedstock, and especially carbon monoxide and hydrogen, be widely used in the chemical processes such as oxo process, becomes the important source material of a series of basic organic chemical industry product and intermediate.Wherein, the source of carbon monoxide is by the gaseous mixture containing a certain amount of CO2, CO, H2, N2, CH4, O2, H2O etc. substantially, adopt deep cooling separating method, thus obtain highly purified CO, this method is applicable to large-scale industrial production, and can more effectively obtain highly purified CO.
At present, deep cooling separating method is generally by the synthetic gas of certain pressure is carried out throttling, expansion, to produce lower temperature thus to make all or part of liquefaction of synthetic gas, and then H2, CH4, CO is separated.Wherein, the core of separation by deep refrigeration is the difference utilizing boiling point between each component in synthetic gas, is realized the separation of gaseous mixture by rectifying tower.Solidify at low temperatures to prevent impurity contained in composite gas component thus block interchanger and pipeline, needing unstripped gas to carry out pre-treatment before entering ice chest, remove heavy hydrocarbon, CO2, H2O and H2S etc.
Chinese patent CN104011488A discloses a kind of method and apparatus by low-temperature distillation supply gaseous carbon monoxide, comprising, first material synthesis gas is cooled, then in methane wash column, most of hydrogen is removed, and enter remove hydrogen further in stripping tower after enter the middle part of demethanizing tower, then methane rich is obtained in tower reactor, methane rich pressurizes rear section as methane wash column phegma through liquor pump, part continues re-heat and goes out device as fuel gas, rich carbon monoxide is obtained at demethanizer overhead, rich carbon monoxide goes out device through re-heat and enters carbon monoxide cycle compressor boost, product carbon monoxide is extracted out from recycle compressor intermediate stage.The cold of the device carbon monoxide supplemented as recycle compressor outlet cools to extract out from middle part and enters expander to low pressure and return interchanger re-heat in interchanger.
In method described above, because of lower boiling nitrogen along with carbon monoxide is enriched to demethanizer overhead together, therefore this device produce carbon monoxide in nitrogen cannot solve in this flow process, need to increase device to remove further, and rich carbon monoxide goes out that the pressure of device is lower need cooling box after in recycle compressor supercharging extract out from intermediate stage.The methane wash column of this invention, not containing reboiler, therefore once cannot remove in a tower, needs to increase stripping tower, and at stripper top discharge hydrogen-rich gas, this gas cannot use therefore device hydrogen extraction yield lower as gas product.
In addition, CN101568788B is disclosed a kind of separation by low-temperature distillation and at least comprises hydrogen, the method and apparatus of the mixture of nitrogen and carbon monoxide, although achieve certain separating effect, but the equipment adopted does not have further imperfection, especially starting to obtain containing methane for main separating hydrogen gas, in C1 and C2 of carbon monoxide and nitrogen mixture, need to arrange C2 tower to remove remaining hydrogen, and a part of raw hydrogen enters C1 tower bottom, thus in C2 tower raw material hydrogen content > 1.5% in C2 removed overhead, this part thick hydrogen can not use as hydrogen product, reduce hydrogen recovery rate.
Summary of the invention
In order to solve the method and apparatus that prior art proposes in separating-purifying synthetic gas, deficiency in actual applications, a kind of energy-efficient method and apparatus being separated hydrogen making and high-purity CO from synthetic gas is provided, the invention provides the method and apparatus that a kind of synthetic gas is separated hydrogen making and high-purity CO, first be with containing H2, CO, N2, CH4, the synthetic gas of the gaseous mixture of O2 etc. is raw material, and hydrogen and carbon monoxide can be produced simultaneously, the auxiliary method obtaining nitrogen and fuel gas, be exactly adopt dehydrogenation tower C1 in short, deoxidation-methane tower C2 and denitrification column C3 continuous rectification hydrogen making and high-purity CO, nitrogen and fuel gas are also separated from synthetic gas simultaneously, overcome the defect of traditional method, save facility investment, reduce energy consumption, improve added value of product, thus achieve recycling economy effect.
An object of the present invention is to provide a kind of method that synthetic gas high for foreign matter content carries out being separated.
Another object of the present invention obtains a kind of high purity H that can participate in synthesis or research as raw material or intermediate
2, on the other hand, described method is for separation H
2there is high-recovery.
Another object of the present invention obtains a kind of highly purified CO.
Object of the present invention also comprises the nitrogen and fuel gas of assisting and obtaining again utilizing.
The present invention also aims to state on the basis of object in realization, provide a kind of and reduce energy expenditure and reduce the method for cost of investment.
The present invention also aims to provide a kind of device to realize above-mentioned purpose.
The theme of a first aspect of the present invention is a kind of method that synthetic gas is separated hydrogen making and high-purity CO, it is characterized in that, described synthetic gas is main containing H after pre-treatment
2, CO, N
2, CH
4, O
2and the gas mixture of other gaseous impurities on a small quantity;
Described method comprises: H
2and lower-boiling impurity is obtained from tower top is separated by rectifying, CH
4, O
2and high-boiling-point impurity is obtained from tower reactor is separated by secondary rectifying, N
2and the high-boiling-point impurity be not removed is obtained from tower top is separated by three rectifying, CO is obtained from tower reactor is separated by three rectifying;
Wherein, the N that the energy transfer process that this process is adjoint is obtained by described separation
2the Process of absorption or liberation of heat of circulation loop realize.
A preferred embodiment according to a first aspect of the invention, wherein, about described synthetic gas, described pre-treatment comprises purifying, drying and other pretreatment operation well known by persons skilled in the art, is mainly used in removing heavy hydrocarbon, CO2, H2O and H2S etc.
A preferred embodiment according to a first aspect of the invention, wherein, the separated purity obtained of described CO is more than 98%, can reach more than 99.999%.
Described H
2the separated purity obtained is more than 93%, and after after main heat exchanger EH1 re-heat cooling box enter PSA hydrogen purification apparatus purification.
The theme of a second aspect of the present invention is the device that a kind of synthetic gas is as described in relation to the first aspect separated the method for hydrogen making and high-purity CO, it is characterized in that, described device comprises the dehydrogenation tower C1, deoxidation-methane tower C2 and the denitrification column C3 continuous rectification equipment that are provided with overhead condensation vaporizer K1, K2, K3 and tower reactor reboiler B1, B2, B3;
Also comprise for realizing N
2circulation loop and energy transfer process and the recycle compressor CP1 established, main heat exchanger EH1, turbo-expander TP1, throttling valve V1, V2, V3, return tank SP1 and carbon monoxide screens pump BP1;
Wherein, particularly, low-pressure nitrogen 220 is through recycle compressor CP1 supercharging and after being cooled to normal temperature, nitrogen 201 enters in main heat exchanger EH1 and cools, wherein, enter at the middle part extraction section nitrogen 202 of main heat exchanger EH1 in the tower reactor reboiler B2 of deoxidation-methane tower C2 and cool, to make the liquid portion evaporation rectifying in C2 in the tower reactor of deoxidation-methane tower C2, and make that the methane concentration in tower reactor liquid promotes, carbon monoxide content minimizing; Cooled medium pressure nitrogen gas 204 again enters in the tower reactor reboiler B3 of denitrification column C3 and cools, to make the liquid portion evaporation rectifying in C3 in the tower reactor of deoxidation-methane tower C3, and to make in tower reactor liquid that carbon monoxide concentration promotes, a nitrogen content reduces and obtains qualified carbon monoxide liquid product; Cooled middle hydraulic fluid nitrogen 205 and cold junction in main heat exchanger EH1 are out liquefied and after excessively cold liquid nitrogen 203 converges, liquid nitrogen 207 enters the low-temperature receiver as overhead condensation vaporizer K2 in the overhead condensation vaporizer K2 of deoxidation-methane tower C2, rich liquid nitrogen 211 is divided into two strand 212 and 213 and enters in the overhead condensation vaporizer K1 of dehydrogenation tower C1 and the overhead condensation vaporizer K3 of denitrification column C3 after throttling valve throttling to normal pressure respectively, as the low-temperature receiver of overhead condensation vaporizer K1 and K3; The pressure nitrogen gas 208 evaporated in C2 tower condenser/evaporator enters in main heat exchanger EH1 and extracts nitrogen 209 out from the middle part of main heat exchanger EH1 after part re-heat, entering in nitrogen gas turbine decompressor TP1 expands produces the cold damage of cold supplementary device, the low-pressure nitrogen 218 and 217 mixed 219 evaporated in nitrogen after expansion 210 and overhead condensation vaporizer K1 and K3, after low-pressure nitrogen passage re-heat to the normal temperature entering main heat exchanger EH1 obtains nitrogen 220, enter in recycle compressor CP1 and recycle.
A preferred embodiment according to a second aspect of the invention, wherein, described carbon monoxide liquid refers to through carbon monoxide screens pump BP1 supercharging and is forced into higher than transfer pressure needed for gas product.
Medium pressure nitrogen gas in the described tower reactor reboiler B2 entering deoxidation-methane tower C2 and the medium pressure nitrogen gas in the tower reactor reboiler B3 entering denitrification column C3 are that sequential series is connected, and progressively converge through expenditure and pressure and liquid nitrogen 203 after cooling.
Described device also comprises dehydrogenation tower C1, deoxidation-methane tower C2, denitrification column C3, condenser/evaporator K1, K2, K3, tower reactor reboiler B1, B2, B3, the pipeline be connected between main heat exchanger EH1, turbo-expander TP1 and carbon monoxide screens pump BP1 and valve.
Pressure nitrogen gas 202 in the described tower reactor reboiler entering deoxidation-methane tower separates one nitrogen and mixes with the cooled nitrogen of tower reactor reboiler B3 of denitrification column before the tower reactor reboiler B3 entering denitrification column, and change separates the flow of one nitrogen to change the load of the tower reactor reboiler B3 of denitrification column.
Be separated a preferred embodiment of the method and apparatus of hydrogen making and high-purity CO according to a kind of synthetic gas of the present invention, wherein, particularly, described method comprises:
Step 1: described synthetic gas is cooled, then send into after again cooling in the tower reactor reboiler B1 of dehydrogenation tower C1, rectifying in dehydrogenation tower C1 is entered through throttling valve V1 decompression, wherein, the thick hydrogen obtained at tower top enters overhead condensation vaporizer K1 and liquid nitrogen heat exchange, make to be mixed in most of carbon monoxide wherein, nitrogen condensation become liquid and be back to lower top of tower, and uncooled hydrogen through main heat exchanger EH1 re-heat to normal temperature as output of products;
Step 2: be back in dehydrogenation tower C1 tower reactor reboiler B1 containing a small amount of hydrogen (hydrogeneous < 5 × 10
-6(V/V) synthetic gas liquid) imports in deoxidation-methane tower C2 after throttling valve V2 reduces pressure, wherein, tower top obtain containing micro amount of oxygen and substantially not containing the mixture of the carbon monoxide of methane, nitrogen, Microamounts of Hydrogen, enter in overhead condensation vaporizer K2 with liquid nitrogen heat exchange, part mixes is condensed into the phegma of liquid as C2, and portion gas mixture imports rectifying in denitrification column C3 through throttling valve V3; Extract in tower reactor that part is isolated is rich in methane (CH4 > 99.9 × 10
-2(V/V) liquid) uses as fuel gas after main heat exchanger EH1 re-heat;
Step 3: the gas mixture rectifying in denitrification column C3 after the throttling of V3 valve, wherein, the carbon monoxide liquid containing micro amount of oxygen and nitrogen in tower reactor reboiler B3 to import in main heat exchanger EH1 re-heat as output of products after carbon monoxide screens pump BP1 supercharging; The tower top nitrogen obtained containing micro CO enter in overhead condensation vaporizer K3 with liquid nitrogen heat exchange, part nitrogen mixture is condensed into the phegma of liquid as C3, and denitrogenation tower top obtains containing H
2< 5 × 10
-6(V/V), containing CO < 5 × 10
-6(V/V) high pure nitrogen, supplements as the nitrogen of nitrogen circulating system after entering main heat exchanger EH1 re-heat and system meter source of the gas uses.
Another preferred embodiment of the method and apparatus of hydrogen making and high-purity CO is separated according to a kind of synthetic gas of the present invention, wherein:
Adopt the dehydrogenation tower C1 of overhead condenser with pressure and tower bottom reboiler, deoxidation-methane tower C2 and denitrification column C3 continuous rectification hydrogen making and high-purity CO; Circulation medium pressure nitrogen gas is vaporized the synthetic gas in deoxidation-methane tower C2 and denitrification column C3, and cooled nitrogen enters the low-temperature receiver of condenser/evaporator as dehydrogenation tower, methane tower and denitrification column after throttling valve throttling after being liquefied; Highly purified aqueous carbon monoxide obtains from denitrogenation tower reactor B3, is vaporized with main heat exchanger EH1 as output of products after carbon monoxide screens pump BP1 is forced into required pressure; Hydrogen cooling box after main heat exchanger EH1 re-heat of the purity more than 93% obtained from described dehydrogenation top of tower enters the purification of PSA hydrogen purification apparatus; Entering medium pressure nitrogen gas in the tower reactor reboiler B2 of deoxidation-methane tower C2 and the medium pressure nitrogen gas in the tower reactor reboiler B3 entering denitrification column C3 is that sequential series is connected and progressively cools deutomerite and flow to into C1, C2, the condenser/evaporator K1 of C3 tower, K2, K2 is as rectifying tower C1, the low-temperature receiver of the phegma of C2, C3, enters the cold of turbo-expander expansion generator after the nitrogen under pressure re-heat that condenser/evaporator K2 evaporates.
A kind of synthetic gas of the present invention is separated the method and apparatus of hydrogen making and high-purity CO, owing to have employed technique scheme, has the following advantages and beneficial effect:
1, the present invention adopts overheated synthetic gas to enter in the middle part of rectifying tower after reboiler cools and maintains superheat state before entering dehydrogenation tower, lower boiling hydrogen major part in tower reactor is made to be obtained higher hydrogen extraction yield by evaporation, adopt three tower continuous prodution of band overhead condenser and tower reactor reboiler can produce hydrogen and carbon monoxide simultaneously, and obtaining nitrogen and fuel gas, throughput significantly improves;
2, the pressure nitrogen gas that the present invention adopts nitrogen supercharging, deoxidation-methane tower condenser/evaporator evaporates expands and produces the recycle system of cold; Liquid nitrogen is as rectifying tower condenser low-temperature receiver and carbon monoxide cycle ratio, higher heat transfer temperature difference can be obtained, condenser evaporating pressure can be improved, adopt the deoxidation-pressure nitrogen gas of methane tower condenser/evaporator evaporation to expand and produce cold holdout device cold balancing, therefore adopt nitrogen circulation amount of the present invention 10-20% lower than other process units;
3, in the present invention, dehydrogenation tower C1 is from lower-boiling impurities such as tower top separating hydrogen gas, and deoxidation-methane tower C2 is from separation of C H at the bottom of tower
4, O
2deng high-boiling-point impurity, and pass through the further separation of denitrification column C3, can process containing the many gas mixtures of impurity, lower relative to existing technologies to the requirement of gas mixture to be dealt with, applied range, is suitable for large-scale promotion and application;
4, the C1 tower arranging band tower reactor reboiler and overhead condenser disclosed by the invention, hydrogen substantially purifies in C1 tower, hydrogeneous < 5 × 10 in dehydrogenation tower bottom synthetic gas
-6(V/V), thus hydrogen of the present invention in C1 tower extraction yield more than 99.9%;
5, product carbon monoxide of the present invention be from C3 tower reactor by after pump pressurization direct among main heat exchanger EH1, evaporate re-heat after obtain band die pressing product carbon monoxide, adopt nitrogen circulation compressor to avoid the risk of carbon monoxide compressor operating safety.
Accompanying drawing explanation
Fig. 1 is method and the device schematic diagram of the embodiment of the present invention 1 correspondence.
Wherein: C1 dehydrogenation tower; C2 deoxidation-methane tower; C3 denitrification column; K1, K2, K3 overhead condensation vaporizer; B1, B2, B3 tower reactor reboiler; EH1 main heat exchanger; TP1 turbo-expander; BP1 carbon monoxide screens pump; SP1 return tank; CP1 recycle compressor; V1, V2, V3 throttling valve; 101,102,103,104 synthetic gas; 105,106 hydrogen; 107, the synthetic gas after 108 dehydrogenations; 109,110 for N2/CO be main gas mixture; 111,112 methane rich (fuel gas); 113,114,115 carbon monoxide; 201, hydraulic fluid nitrogen in 202,204 medium pressure nitrogen gas, 203,205,206,207,211,212,213 pressure liquid nitrogen; 208,209 pressure nitrogen gas; 214,215 low pressure liquid nitrogen; 216,217,218,210,219,220 low-pressure nitrogens.
Wherein: middle end finger pressure >=1.6MPa, low pressure finger pressure is lower than 0.1MPa, and pressure nitrogen, nitrogen under pressure finger pressure are between 0.1MPa-1.6MPa.
Embodiment
The invention provides a kind of method that synthetic gas is separated hydrogen making and high-purity CO, it is characterized in that, described synthetic gas is main containing H after pre-treatment
2, CO, N
2, CH
4, O
2and the gas mixture of other gaseous impurities on a small quantity;
Described method comprises: H
2and lower-boiling impurity is obtained from tower top is separated by rectifying, CH
4, O
2and high-boiling-point impurity is obtained from tower reactor is separated by secondary rectifying, N
2and the high-boiling-point impurity be not removed is obtained from tower top is separated by three rectifying, CO is obtained from tower reactor is separated by three rectifying;
Wherein, the N that the energy transfer process that this process is adjoint is obtained by described separation
2the Process of absorption or liberation of heat of circulation loop realize.
According to a preferred embodiment of the present invention, wherein, about described synthetic gas, described pre-treatment comprises purifying, drying and other pretreatment operation well known by persons skilled in the art, is mainly used in removing heavy hydrocarbon, CO2, H2O and H2S etc.
Present invention also offers the device that a kind of synthetic gas is as described in relation to the first aspect separated the method for hydrogen making and high-purity CO, it is characterized in that, described device comprises the dehydrogenation tower C1, deoxidation-methane tower C2 and the denitrification column C3 continuous rectification equipment that are provided with overhead condensation vaporizer K1, K2, K3 and tower reactor reboiler B1, B2, B3;
Also comprise for realizing N
2circulation loop and energy transfer process and the recycle compressor CP1 established, main heat exchanger EH1, turbo-expander TP1, throttling valve V1, V2, V3, return tank SP1 and carbon monoxide screens pump BP1;
Wherein, particularly, low-pressure nitrogen 220 is through recycle compressor CP1 supercharging and after being cooled to normal temperature, nitrogen 201 enters in main heat exchanger EH1 and cools, wherein, enter at the middle part extraction section nitrogen 202 of main heat exchanger EH1 in the tower reactor reboiler B2 of deoxidation-methane tower C2 and cool, to make the liquid portion evaporation rectifying in C2 in the tower reactor of deoxidation-methane tower C2, and make that the methane concentration in tower reactor liquid promotes, carbon monoxide content minimizing; Cooled medium pressure nitrogen gas 204 again enters in the tower reactor reboiler B3 of denitrification column C3 and cools, to make the liquid portion evaporation rectifying in C3 in the tower reactor of deoxidation-methane tower C3, and to make in tower reactor liquid that carbon monoxide concentration promotes, a nitrogen content reduces and obtains qualified carbon monoxide liquid product; Cooled middle hydraulic fluid nitrogen 205 and cold junction in main heat exchanger EH1 are out liquefied and after excessively cold liquid nitrogen 203 converges, liquid nitrogen 207 enters the low-temperature receiver as overhead condensation vaporizer K2 in the overhead condensation vaporizer K2 of deoxidation-methane tower C2, rich liquid nitrogen 211 is divided into two strand 212 and 213 and enters in the overhead condensation vaporizer K1 of dehydrogenation tower C1 and the overhead condensation vaporizer K3 of denitrification column C3 after throttling valve throttling to normal pressure respectively, as the low-temperature receiver of overhead condensation vaporizer K1 and K3; The pressure nitrogen gas 208 evaporated in C2 tower condenser/evaporator enters in main heat exchanger EH1 and extracts nitrogen 209 out from the middle part of main heat exchanger EH1 after part re-heat, entering in nitrogen gas turbine decompressor TP1 expands produces the cold damage of cold supplementary device, the low-pressure nitrogen 218 and 217 mixed 219 evaporated in nitrogen after expansion 210 and overhead condensation vaporizer K1 and K3, after low-pressure nitrogen passage re-heat to the normal temperature entering main heat exchanger EH1 obtains nitrogen 220, enter in recycle compressor CP1 and recycle.
According to the method for Fig. 1 embodiment of the present invention 1 correspondence and device schematic diagram, method and apparatus synthetic gas of the present invention being separated to hydrogen making and high-purity CO is further explained and illustrates.
Embodiment 1
Middle pressure (general pressure is between 2.5-5MPa) is containing H
2, CO, N
2, CH
4, O
2and the material synthesis gas 101 of other gaseous impurities is on a small quantity cooled to-100 to-140 DEG C in main heat exchanger EH1, then the gas 103 sent into after being cooled to a little higher than reboiler still liquid temperature of saturation in the tower reactor reboiler B1 of dehydrogenation tower C1 enters rectifying in dehydrogenation tower C1 after throttling valve V1 reduces pressure, the thick hydrogen obtaining ((~ 92%H2)) at tower top enters overhead condensation vaporizer K1 and liquid nitrogen 214 heat exchange, then by most carbon monoxide, nitrogen becomes liquid through overhead condensation vaporizer K1 condensation, then lower top of tower is back to, in overhead condensation vaporizer K1, uncooled hydrogen 105 (~ 93%H2) exports as product 106 to normal temperature through main heat exchanger EH1 re-heat,
Be back to bottom dehydrogenation tower C1 in tower reactor B1 containing a small amount of hydrogen (hydrogeneous < 5 × 10
-6(V/V) synthetic gas liquid 107 (main component is carbon monoxide, methane, nitrogen)) is decompressed to through throttling valve V2 and obtains gas-liquid state flow 108 after 0.15-0.5MPa and import rectifying in deoxidation-methane tower C2; Tower top obtain containing micro amount of oxygen and substantially not containing the mixture of the carbon monoxide of methane, nitrogen, Microamounts of Hydrogen enter in overhead condensation vaporizer K2 with liquid nitrogen heat exchange, part mixes is condensed into the phegma of liquid as C2, and portion gas mixture 109 imports rectifying in denitrification column C3 through throttling valve V3; Extract in C2 tower reactor that part is isolated is rich in methane (CH4 > 99.9 × 10
-2(V/V) liquid 111) uses as fuel gas 112 after main heat exchanger EH1 re-heat;
The rectifying in denitrification column C3 (pressure is between 0.06-0.3MPa) of gas mixture 110 after the throttling of V3 valve, importing re-heat in main heat exchanger EH1 export as product 115 containing carbon monoxide liquid 113 (purity ~ 98%CO, reaches as high as more than 99.999%CO) liquid 114 after carbon monoxide screens pump BP1 is pressurized to 0.2-5MPa in the tower reactor B3 of bottom; The tower top nitrogen obtained containing micro CO enter in condenser/evaporator K3 with liquid nitrogen heat exchange, part nitrogen mixture is condensed into the phegma of liquid as C3, and denitrogenation tower top obtains containing H
2< 5 × 10
-6(V/V), containing CO < 5 × 10
-6(V/V) high pure nitrogen, supplements as the nitrogen of nitrogen circulating system after entering main heat exchanger EH1 re-heat and system meter source of the gas uses;
Low-pressure nitrogen 220 (pressure ~ 0.01MPa) (201) after circulating nitrogen gas compressor CP1 is pressurized to 2.5-5MPa and is cooled to normal temperature enters in main heat exchanger EH1 and to cool in the middle part of main heat exchanger after extraction section medium pressure nitrogen gas 202 (temperature ~-100 DEG C to-130 DEG C) enters and be cooled to the temperature of a little higher than C2 tower bottoms in deoxidation-methane tower reboiler B2, make the liquid portion evaporation rectifying in C2 in the tower reactor of deoxidation-methane tower C2, methane concentration lifting, carbon monoxide content in tower reactor liquid are reduced; Cooled medium pressure nitrogen gas (or liquid) 204 again enters in denitrification column reboiler B3 and cools further, make the liquid portion evaporation rectifying in C3 in the tower reactor of deoxidation-methane tower C3, to make in tower reactor liquid that carbon monoxide concentration promotes, a nitrogen content reduces and obtain qualified carbon monoxide liquid product 113; Cooled middle hydraulic fluid nitrogen 205 and cold junction in main heat exchanger EH1 are out liquefied and excessively cold liquid nitrogen 203 207 enters low-temperature receiver as C2 tower condenser/evaporator in deoxidation-methane tower condenser/evaporator K2 after converging, rich liquid nitrogen 211 is divided into two strand 212 and 213 after throttling valve throttling to normal pressure, pours C1 tower condenser/evaporator K1 and C2 tower condenser/evaporator K3 respectively into, as the low-temperature receiver of C1 and C3 tower condenser/evaporator;
The pressure nitrogen gas 208 (pressure 0.08MPa-0.5MPa) evaporated in C2 tower condenser/evaporator enters part re-heat in main heat exchanger and in the middle part of interchanger, extracts 209 to-140 DEG C to-165 DEG C out, enter in nitrogen gas turbine decompressor TP1 and be expanded to the cold damage that 0.015MPa to 0.05MPa produces cold supplementary device, the low-pressure nitrogen 218,217 evaporated in nitrogen after expansion 210 and condenser/evaporator K1 and K3 mix afterwards 219 enter the re-heat to normal temperature 220 of main heat exchanger low-pressure nitrogen passage again after enter in circulating nitrogen gas compressor CP1 and recycle.
Following table is the concrete data of embodiment 1:
The present invention can realize less energy-consumption ground hydrogen making, carbon monoxide; The carbon monoxide product of more than 98% and 99.999% can be produced; Producing carbon monoxide pressure higher than needing during 0.2MPa to arrange carbon monoxide compressor thus reaching energy-conservation and investment reduction, strengthen the object of safety in operation.
Be described in detail specific embodiments of the invention above, but it is just as example, the present invention is not restricted to specific embodiment described above.To those skilled in the art, any equivalent modifications that the present invention is carried out and substituting also all among category of the present invention.Therefore, equalization conversion done without departing from the spirit and scope of the invention and amendment, all should contain within the scope of the invention.
Claims (10)
1. synthetic gas is separated a method for hydrogen making and high-purity CO, it is characterized in that, described synthetic gas is main containing H after pre-treatment
2, CO, N
2, CH
4, O
2and the gas mixture of other gaseous impurities on a small quantity;
Described method comprises: H
2and lower-boiling impurity is obtained from tower top is separated by rectifying, CH
4, O
2and high-boiling-point impurity is obtained from tower reactor is separated by secondary rectifying, N
2and the high-boiling-point impurity be not removed is obtained from tower top is separated by three rectifying, CO is obtained from tower reactor is separated by three rectifying;
Wherein, the N that the energy transfer process that this process is adjoint is obtained by described separation
2the Process of absorption or liberation of heat of circulation loop realize.
2. method according to claim 1, it is characterized in that, the pre-treatment of described synthetic gas comprises purifying, drying and other pretreatment operation well known by persons skilled in the art, is mainly used in removing heavy hydrocarbon, CO2, H2O and H2S etc.
3. method according to claim 1, is characterized in that, described H
2the separated purity obtained is more than 93%, and after after main heat exchanger EH1 re-heat cooling box enter PSA hydrogen purification apparatus purification.
4. method according to claim 1, it is characterized in that, the separated purity obtained of described CO is more than 98%, can reach more than 99.999%.
5. one kind as claimed in claim 1 synthetic gas be separated the device of the method for hydrogen making and high-purity CO, it is characterized in that, described device comprises the dehydrogenation tower C1, deoxidation-methane tower C2 and the denitrification column C3 continuous rectification equipment that are provided with overhead condensation vaporizer K1, K2, K3 and tower reactor reboiler B1, B2, B3;
Also comprise for realizing N
2circulation loop and energy transfer process and the recycle compressor CP1 established, main heat exchanger EH1, turbo-expander TP1, throttling valve V1, V2, V3, return tank SP1 and carbon monoxide screens pump BP1;
Wherein, low-pressure nitrogen 220 is through recycle compressor CP1 supercharging and after being cooled to normal temperature, nitrogen 201 enters in main heat exchanger EH1 and cools, wherein, enter at the middle part extraction section nitrogen 202 of main heat exchanger EH1 in the tower reactor reboiler B2 of deoxidation-methane tower C2 and cool, to make the liquid portion evaporation rectifying in C2 in the tower reactor of deoxidation-methane tower C2, and make that the methane concentration in tower reactor liquid promotes, carbon monoxide content minimizing; Cooled medium pressure nitrogen gas 204 again enters in the tower reactor reboiler B3 of denitrification column C3 and cools, to make the liquid portion evaporation rectifying in C3 in the tower reactor of deoxidation-methane tower C3, and to make in tower reactor liquid that carbon monoxide concentration promotes, a nitrogen content reduces and obtains qualified carbon monoxide liquid product; Cooled middle hydraulic fluid nitrogen 205 and cold junction in main heat exchanger EH1 are out liquefied and after excessively cold liquid nitrogen 203 converges, liquid nitrogen 207 enters the low-temperature receiver as overhead condensation vaporizer K2 in the overhead condensation vaporizer K2 of deoxidation-methane tower C2, rich liquid nitrogen 211 is divided into two strand 212 and 213 and enters in the overhead condensation vaporizer K1 of dehydrogenation tower C1 and the overhead condensation vaporizer K3 of denitrification column C3 after throttling valve throttling to normal pressure respectively, as the low-temperature receiver of overhead condensation vaporizer K1 and K3; The pressure nitrogen gas 208 evaporated in C2 tower condenser/evaporator enters in main heat exchanger EH1 and extracts nitrogen 209 out from the middle part of main heat exchanger EH1 after part re-heat, entering in nitrogen gas turbine decompressor TP1 expands produces the cold damage of cold supplementary device, the low-pressure nitrogen 218 and 217 mixed 219 evaporated in nitrogen after expansion 210 and overhead condensation vaporizer K1 and K3, after low-pressure nitrogen passage re-heat to the normal temperature entering main heat exchanger EH1 obtains nitrogen 220, enter in recycle compressor CP1 and recycle.
6. device according to claim 5, it is characterized in that, described method comprises in said device:
Step 1: described synthetic gas is cooled, then send into after again cooling in the tower reactor reboiler B1 of dehydrogenation tower C1, rectifying in dehydrogenation tower C1 is entered through throttling valve V1 decompression, wherein, the thick hydrogen obtained at tower top enters overhead condensation vaporizer K1 and liquid nitrogen heat exchange, make to be mixed in most of carbon monoxide wherein, nitrogen condensation become liquid and be back to lower top of tower, and uncooled hydrogen through main heat exchanger EH1 re-heat to normal temperature as output of products;
Step 2: the synthetic gas liquid containing a small amount of hydrogen be back in dehydrogenation tower C1 tower reactor reboiler B1 imports in deoxidation-methane tower C2 after throttling valve V2 reduces pressure, wherein, tower top obtain containing micro amount of oxygen and substantially not containing the mixture of the carbon monoxide of methane, nitrogen, Microamounts of Hydrogen, enter in overhead condensation vaporizer K2 with liquid nitrogen heat exchange, part mixes is condensed into the phegma of liquid as C2, and portion gas mixture imports rectifying in denitrification column C3 through throttling valve V3; Extract the isolated liquid being rich in methane of part in tower reactor to use as fuel gas after main heat exchanger EH1 re-heat;
Step 3: the gas mixture rectifying in denitrification column C3 after the throttling of V3 valve, wherein, the carbon monoxide liquid containing micro amount of oxygen and nitrogen in tower reactor reboiler B3 to import in main heat exchanger EH1 re-heat as output of products after carbon monoxide screens pump BP1 supercharging; The tower top nitrogen obtained containing micro CO enter in overhead condensation vaporizer K3 with liquid nitrogen heat exchange, part nitrogen mixture is condensed into the phegma of liquid as C3, and the regeneration source of the gas as purified synthesis gas device after all the other nitrogen enter main heat exchanger EH1 re-heat uses.
7. device according to claim 6, is characterized in that, in described step 3, described carbon monoxide liquid refers to through carbon monoxide screens pump BP1 supercharging and is forced into higher than transfer pressure needed for gas product.
8. device according to claim 5, it is characterized in that, medium pressure nitrogen gas in the described tower reactor reboiler B2 entering deoxidation-methane tower C2 and the medium pressure nitrogen gas in the tower reactor reboiler B3 entering denitrification column C3 are that sequential series is connected, and progressively converge through expenditure and pressure and liquid nitrogen 203 after cooling.
9. device according to claim 5, it is characterized in that, described device also comprises dehydrogenation tower C1, deoxidation-methane tower C2, denitrification column C3, condenser/evaporator K1, K2, K3, tower reactor reboiler B1, B2, B3, the pipeline be connected between main heat exchanger EH1, turbo-expander TP1 and carbon monoxide screens pump BP1 and valve.
10. device according to claim 5, it is characterized in that, pressure nitrogen gas 202 in the described tower reactor reboiler entering deoxidation-methane tower separates one nitrogen and mixes with the cooled nitrogen of tower reactor reboiler B3 of denitrification column before the tower reactor reboiler B3 entering denitrification column, and change separates the flow of one nitrogen to change the load of the tower reactor reboiler B3 of denitrification column.
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