CN114133969B - Desulfurization and decarburization method for high-sulfur high-carbon natural gas - Google Patents
Desulfurization and decarburization method for high-sulfur high-carbon natural gas Download PDFInfo
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- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10L—FUELS NOT OTHERWISE PROVIDED FOR; NATURAL GAS; SYNTHETIC NATURAL GAS OBTAINED BY PROCESSES NOT COVERED BY SUBCLASSES C10G, C10K; LIQUEFIED PETROLEUM GAS; ADDING MATERIALS TO FUELS OR FIRES TO REDUCE SMOKE OR UNDESIRABLE DEPOSITS OR TO FACILITATE SOOT REMOVAL; FIRELIGHTERS
- C10L3/00—Gaseous fuels; Natural gas; Synthetic natural gas obtained by processes not covered by subclass C10G, C10K; Liquefied petroleum gas
- C10L3/06—Natural gas; Synthetic natural gas obtained by processes not covered by C10G, C10K3/02 or C10K3/04
- C10L3/10—Working-up natural gas or synthetic natural gas
- C10L3/101—Removal of contaminants
- C10L3/102—Removal of contaminants of acid contaminants
- C10L3/103—Sulfur containing contaminants
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- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10L—FUELS NOT OTHERWISE PROVIDED FOR; NATURAL GAS; SYNTHETIC NATURAL GAS OBTAINED BY PROCESSES NOT COVERED BY SUBCLASSES C10G, C10K; LIQUEFIED PETROLEUM GAS; ADDING MATERIALS TO FUELS OR FIRES TO REDUCE SMOKE OR UNDESIRABLE DEPOSITS OR TO FACILITATE SOOT REMOVAL; FIRELIGHTERS
- C10L3/00—Gaseous fuels; Natural gas; Synthetic natural gas obtained by processes not covered by subclass C10G, C10K; Liquefied petroleum gas
- C10L3/06—Natural gas; Synthetic natural gas obtained by processes not covered by C10G, C10K3/02 or C10K3/04
- C10L3/10—Working-up natural gas or synthetic natural gas
- C10L3/101—Removal of contaminants
- C10L3/102—Removal of contaminants of acid contaminants
- C10L3/104—Carbon dioxide
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P20/00—Technologies relating to chemical industry
- Y02P20/151—Reduction of greenhouse gas [GHG] emissions, e.g. CO2
Abstract
The invention provides a desulfurization and decarburization method for high-sulfur high-carbon natural gas. The process enables the natural gas and the absorption liquid to be dispersed into a micron-scale infinitesimal dispersion system in the infinitesimal generating device, has huge phase interface area, remarkably improves the absorption rate, and further greatly reduces the size of the absorption equipment and can complete the desulfurization and decarburization tasks with only a small number of tower plates; meanwhile, the heights of the liquid layers of the infinitesimal dispersion systems in the infinitesimal dispersion bed and the infinitesimal dispersion section of the composite absorption tower are controllable, the gas-phase retention time can be adjusted by adjusting the heights of the liquid layers of the infinitesimal dispersion systems, so that the reaction degree is controlled, and the operation elasticity is increased; in addition, the composite absorption tower can be operated under the condition of lower barren liquor circulation amount, and compared with the conventional process, the regeneration energy consumption can be obviously reduced.
Description
Technical Field
The invention relates to a desulfurization and decarburization method for high-sulfur high-carbon natural gas, belonging to the technical field of natural gas purification.
Background
With the improvement of natural gas industrial infrastructure in China, the development speed is accelerated continuously, the natural gas industrial chain in China enters a rapid development stage, the demand of natural gas is increased sharply, and based on the industrial background that the domestic urbanization process is accelerated, the energy-saving and environment-friendly demand is increased, and the infrastructure and policy are improved continuously, the application range of the natural gas is expanded continuously after years of development, and the natural gas is gradually advanced to main energy. The natural gas quality of each producing area in China is uneven, the acid gas content in the natural gas of partial areas is higher, the requirement of China on the sulfur content in the natural gas is more strict, and the hydrogen sulfide content is required to be lower than 6mg/m according to a standard in GB17820-2018 3 Carbon dioxide content of less than 3 mol%, for some high CO 2 High content or high H 2 The treatment of natural gas with S content requires deep H removal 2 S, also requires a large removal of CO 2 Therefore, the requirements for the desulfurization and decarburization methods are high.
The natural gas desulfurization and decarburization method can be mainly divided into an absorption method, a direct conversion method, a desulfurizing agent method and the like aiming at H 2 S and CO 2 The natural gas with high content and the chemical solvent absorption method are most widely applied. In absorption processes, the process can be further divided intoThe chemical solvent, the physical solvent, the physicochemical solvent and the like can be selected according to the composition of the natural gas and the actual conditions. Specifically, the catalyst comprises single-component or multi-component organic amine solution of alcohol amines such as MDEA, TEA, MEA, DGA, DEA, DIPA, TBEE, TBIPE and the like, or organic amine solution added with an activating agent and an auxiliary agent, sulfone amine and the like.
The existing absorption equipment mainly comprises a plate tower and a packed tower, is limited by the lower mass transfer efficiency of the traditional tower equipment, has larger equipment volume and higher energy consumption of a device, and therefore, the aim of strengthening the mass transfer process of the absorption equipment to achieve the purposes of reducing the equipment size and realizing low consumption and high efficiency is always an important direction for developing the natural gas desulfurization technology. In particular, with the development of the natural gas industry, the throughput is rapidly increased, and the problem of the large-scale high-pressure absorption tower equipment is more and more prominent. Therefore, in addition to improving the process flow, the following two aspects are mainly developed: on one hand, the mass transfer efficiency can be improved on the basis of the conventional absorption tower, and on the other hand, novel mass transfer enhancement equipment such as a rotary packed bed and the like can be developed. Chinese patent CN202808741U proposes a deep purification system for natural gas desulfurization and decarburization, which can not only carry out conventional purification of natural gas containing sulfur raw material, satisfy the purification index requirements of common commodity natural gas, but also can deeply remove H in the natural gas raw material at one time 2 S、CO 2 And mercaptan, COS and other organic sulfur impurities, are common natural gas desulfurization processes at present, and the absorption equipment in the patent is a conventional absorption tower. Chinese patent CN109988659A proposes a natural gas desulfurization system and method, which adds a TSA desulfurization unit on the basis of an MDEA desulfurization unit to deeply remove hydrogen sulfide, but the system is more complex and uses more equipment. Chinese patent CN203096016U provides a composite plate-type absorption tower, which can effectively realize desulfurization and decarburization of natural gas by alcohol amine method, improve the operation stability of the absorption tower, and ensure the work efficiency of the absorption tower. Chinese patent CN103756743A proposes a method for removing hydrogen sulfide from low-content hydrogen sulfide raw material gas, which adopts an absorption oxidation method and utilizes a rotary packed bed to strengthen absorption reaction, thereby simplifying the process flow, reducing equipment, saving occupied area and being suitable for offshore platforms.
However, the conventional absorption tower is difficult to improve the desulfurization efficiency greatly and has very limited strengthening effect, and the rotating packed bed technology can greatly reduce the equipment volume and realize high selectivity, but can treat high CO 2 High content or high H 2 The natural gas of S requires significant attention to the removal rate. The natural gas desulfurization and decarbonization process by a chemical solvent absorption method is a typical gas-liquid reaction, and the removal efficiency and the macroscopic reaction rate of the process are mainly determined by acid gas (H) in natural gas 2 S and CO 2 Etc.) with the mass transfer efficiency of the absorption liquid. From the analysis of mass transfer, the mass transfer can be enhanced by improving the flow state to enable the gas and the liquid to generate a larger phase interface and improving the turbulence degree of the gas and the liquid, so that the absorption reaction is enhanced. The dispersion degree of gas-liquid two phases is not high in conventional tower equipment, and the gas-phase retention time is longer, so that the improvement of the selectivity of hydrogen sulfide is not facilitated; in the rotating packed bed, the liquid phase is dispersed into liquid films, liquid filaments and liquid droplets, the interfacial area is large, but there is still room for further reduction of the size of the dispersed phase.
Disclosure of Invention
The invention aims to overcome the defects of low gas-liquid two-phase dispersion degree, large equipment volume, difficult treatment of high-content carbon dioxide natural gas and high energy consumption in the conventional natural gas desulfurization and decarburization method, and provides a novel natural gas desulfurization and decarburization process based on a micro-element dispersion bed and a novel composite absorption tower and driven by a micro-element dispersion system with a micron scale, wherein the process enables the natural gas and absorption liquid to be dispersed into the micro-element dispersion system with the micron scale in a micro-element generation device, so that the micro-element dispersion system has huge phase interface area, the absorption rate is obviously improved, and the desulfurization and decarburization tasks can be completed only by a small number of tower plates by greatly reducing the size of the absorption equipment; meanwhile, the heights of the liquid layers of the infinitesimal dispersion systems in the infinitesimal dispersion bed and the infinitesimal dispersion section of the composite absorption tower are controllable, the gas-phase retention time can be adjusted by adjusting the heights of the liquid layers of the infinitesimal dispersion systems, so that the reaction degree is controlled, and the operation elasticity is increased; in addition, the composite absorption tower can be operated under the condition of lower barren liquor circulation amount, and compared with the conventional process, the regeneration energy consumption can be obviously reduced.
In order to achieve the aim, the invention provides a method for desulfurizing and decarbonizing high-sulfur high-carbon natural gas.
The method for desulfurizing and decarbonizing the high-sulfur high-carbon natural gas comprises the following steps of:
1) the raw material gas 1 enters a gravity separator 2 to separate large-particle liquid drops and solid impurities, then enters a raw material gas filtering separator 3 to remove small solid particles and liquid drops which are possibly carried in the gas, then enters a first infinitesimal generating device 6 at the bottom of an infinitesimal dispersing bed 8 together with a circulating semi-rich liquid 5 to be dispersed into a first infinitesimal dispersing system 7 with micron scale, wherein highly dispersed micron scale natural gas bubbles are a dispersed phase, an absorption liquid is a continuous phase, and then the infinitesimal dispersing system 7 enters a bed layer of the infinitesimal dispersing bed 8 to perform desulfurization and decarburization reaction;
2) the first infinitesimal dispersion system 7 enters a first gas-liquid separator 9 to be separated into a gas-liquid two phase, the gas phase is a first crude degasification 10, the liquid phase is a rich liquid 11, the first crude degasification 10 and a lean liquid 12 from a regeneration unit or a semi-rich liquid from a second gas-liquid separator 19 are dispersed into a micron-scale second infinitesimal dispersion system 18 in a second infinitesimal generation device 17 in a infinitesimal generation section 16 at the bottom of a composite absorption tower 13, wherein highly dispersed micron-scale natural gas bubbles are dispersed phases, an absorption liquid is a continuous phase, then the second infinitesimal dispersion system 18 enters a infinitesimal dispersion section 15 in the composite absorption tower 13 to perform desulfurization and decarbonization reaction in the infinitesimal dispersion system, then the infinitesimal dispersion system performs gas-liquid separation in the second gas-liquid separator 19, the gas phase is a second crude degasification 20, enters a fine absorption section 14 of the composite absorption tower, and the fine absorption section contains a small amount of tower plates or fillers, the second coarse degassing 20 is in countercurrent contact with a barren solution 21 introduced from the top of the composite absorption tower 13, the desulfurization and decarburization reactions continue to occur, purified gas 22 is discharged from the top of the composite absorption tower, a semi-rich solution after gas phase separation from the second infinitesimal dispersion system is pressurized by a semi-rich solution circulating pump 4 and then enters a first infinitesimal generating device 6 (shown in fig. 1) or is divided into two parts, one part enters the first infinitesimal generating device 6, and the other part enters a second infinitesimal generating device 17 (shown in fig. 2);
3) the rich liquid 11 from the first gas-liquid separator 9 is depressurized by a turbine 23 and enters a flash tank 24 for flash evaporation, and flash evaporation gas 25 flows out from the top of the flash tank to remove fuel gasA system; the rich solution flowing out of the liquid phase outlet of the flash tank enters a lean and rich solution heat exchanger 26, exchanges heat with the regenerated lean solution, then is heated, and enters an inlet at the middle upper part of a regeneration tower 27; the outlet of the top of the regeneration tower is sequentially connected with a condenser 28 at the top of the regeneration tower and a reflux tank 29 of the regeneration tower, so that the absorption liquid absorbs CO in the natural gas 2 And H 2 S is enriched in acid gas, the acid gas 30 is discharged from a gas phase outlet at the top of a regeneration tower reflux tank 29, reflux liquid is discharged from a liquid phase outlet at the bottom of the regeneration tower reflux tank 29, and the reflux liquid is conveyed back to the top of the regeneration tower through a regeneration tower reflux pump 31; the liquid phase outlet at the bottom of the regeneration tower is connected with a reboiler 32 at the bottom of the regeneration tower, the liquid phase is heated in the reboiler and is partially gasified and returned to the bottom of the regeneration tower, the other part of the liquid is discharged from the outlet at the bottom of the reboiler to be used as regenerated absorption liquid barren solution, the barren solution is fed into a barren and rich solution heat exchanger 26 through a barren solution delivery pump 34 to be cooled, the barren solution is fed into a barren solution cooler 36 to be further cooled after being merged with supplementary absorption solution from an absorption solution storage and configuration unit 35, the outlet of the cooler is divided into two parts, one part of the two parts enters a filtering and purifying unit 37 to be removed of impurities and then is merged with the other part of the barren solution without being purified again, and the merged barren absorption solution is pressurized by a barren solution booster pump 38 and then is fed to the inlet at the top end of the composite absorption tower (shown in figure 2) or fed to the inlet at the top end of the composite absorption tower and a second infinitesimal generating device (shown in figure 1).
In the steps 1) and 2) of the method, the raw material gas and the barren solution or the semi-rich solution are dispersed into a micron-scale infinitesimal dispersion system in the first or second infinitesimal generating device, absorption reaction of the absorption liquid and acidic gases such as hydrogen sulfide and carbon dioxide in the natural gas is simultaneously carried out, and the infinitesimal dispersion system continuously reacts after entering the infinitesimal dispersion section of the infinitesimal dispersion bed or the composite absorption tower. Because the gas-liquid two-phase interfacial area in the infinitesimal dispersion system is huge, the turbulence degree is high, the absorption reaction is strengthened, the size of the absorption equipment is further greatly reduced, and the desulfurization and decarburization tasks can be completed only by coupling a small number of tower plates or fillers; meanwhile, the height of the liquid layer of the infinitesimal dispersion system in the infinitesimal dispersion bed or the infinitesimal dispersion section of the composite absorption tower is controllable, and the gas-phase retention time can be adjusted by adjusting the height of the liquid layer of the infinitesimal dispersion system so as to control H 2 S and CO 2 The reaction degree increases the operation flexibility; in addition, the composite absorption tower can be betterThe low barren solution circulation amount is used, and the regeneration energy consumption can be obviously reduced compared with the conventional process.
In the method, the infinitesimal dispersion bed is a hollow cylinder reactor, and the infinitesimal dispersion section is a hollow cylinder or a shell internally provided with a baffling baffle internal member. Inside it is the dispersion of said microelements produced by the said infinitesimal generating means and a series of outlets are provided at different heights in order to regulate the level of the liquid.
In the method, the phase interface area and the residence time are respectively one of the influencing factors influencing the absorption reaction efficiency, the phase interface area is controlled by the flow rate of the absorption liquid entering the infinitesimal generating device, and the residence time of the infinitesimal dispersion system is related to the height of the liquid layer of the infinitesimal dispersion system, so that the dispersion degree of the infinitesimal dispersion system and the residence time of two phases can be regulated and controlled by regulating the flow rate of the absorption liquid entering the infinitesimal generating device and the height of the liquid layer of the infinitesimal dispersion system, thereby achieving the purpose of regulating the reaction degree.
In the method, the size of the infinitesimal dispersion system can be regulated and controlled by adding an additional absorption liquid circulation between the first infinitesimal generating device and the first gas-liquid separator or between the second infinitesimal generating device and the second gas-liquid separator, wherein the absorption liquid circulation is driven by a circulating pump, and particularly, the additional absorption liquid circulation can be added between the first infinitesimal generating device and the first gas-liquid separator; an additional absorption liquid circulation can be added between the second infinitesimal generation device and the second gas-liquid separator; it is also possible to add additional absorption liquid circulation between the first infinitesimal generating device and the first gas-liquid separator as well as between the second infinitesimal generating device and the second gas-liquid separator. Correspondingly, in order to ensure the reasonability of the process, the connection mode between each absorption liquid stream and each device also needs to be adjusted correspondingly, and the specific setting method is explained by referring to the attached drawings.
In the method, the regenerated lean absorption liquid enters the absorption unit in various ways, and can directly enter an inlet above a fine absorption section of the composite absorption tower; or the two streams of the micro-element generating device can be divided into two streams, one stream enters an inlet above the fine suction section of the composite absorption tower, and the other stream enters the second micro-element generating device.
In the method, the infinitesimal dispersion system is separated into a gas phase and a liquid phase by a gas-liquid separator, the gas phase is coarse degasification, and the liquid phase is semi-rich liquid or rich liquid, wherein the gas-liquid separator is one or more of a centrifugal separator, a gravity separator, a baffling separator, a filler separator, a wire mesh separator and a microfiltration separator which can separate bubbles with the diameter of more than 30 micrometers from the liquid phase and is combined in series or in parallel.
In the method, the composite absorption tower comprises a fine absorption section of the composite absorption tower, a infinitesimal dispersion section of the composite absorption tower and a infinitesimal generation section of the composite absorption tower from the top to the bottom in sequence.
The infinitesimal generation section is composed of a second infinitesimal generation device and is connected with the infinitesimal dispersion section.
The fine suction section can be used for deep desulfurization and decarburization, and a small number of tower plates and a small number of fillers can be arranged in the fine suction section. The coarse degassing enters a tower plate or a filler from the lower part of a fine suction section of the composite absorption tower and flows from bottom to top; the regenerated barren solution enters a tower plate or a filler in the fine absorption section from the top of the composite absorption tower and flows from top to bottom. In the fine absorption section, the gas phase and the liquid phase are in countercurrent contact integrally, and the residual carbon dioxide and possible trace hydrogen sulfide in the gas phase are removed to below the national standard.
In the method, the infinitesimal dispersion bed is a hollow cylinder or a shell containing an internal member of a baffling baffle.
In the above method, the first and second infinitesimal generation devices are devices capable of dispersing the gas-liquid two phases into infinitesimal states (i.e., devices capable of dispersing the gas into the liquid phase as micron-sized bubbles, thereby changing the gas-liquid two phases into a state with a large specific surface area and uniform dispersion).
The first and second micro-element generating devices are one or more of a micro-porous membrane (with the aperture of 1-500,000 nanometers) capable of cutting a gas-liquid two-phase system into micro-elements with the size of 1-800 microns, a Venturi type micro-bubble generating device, an ultrasonic cavitation device, a hydrodynamic cavitation type micro-bubble generating device (such as a hydrodynamic cavitation piece of a CN201811308335.4 micro-bubble generator and a clothes processing device), a centrifugal type micro-bubble generating device (such as a centrifugal micro-bubble generating device of a CN 202020030699.7), a jet type micro-bubble generating device and a rotational type micro-bubble generating device which are connected in series or in parallel.
The operating pressure of the first and the second infinitesimal generating devices and the composite absorption tower is 3-15MPa, the operating temperature is 30-90 ℃, and the gas-liquid ratio of the raw material gas to the poor absorption liquid is 100-4000Nm 3 /m 3 Preferably, the gas-liquid ratio is 100-1000Nm 3 /m 3 。
In the above method, the absorption solution can be various chemical, physical or chemical-physical solvents, including single-component, multi-component or organic amine solution with activators and auxiliaries added thereto, such as alcohol amine, such as MDEA, TEA, MEA, DGA, DEA, DIPA, TBEE, TBIPE, and the like, and sulfone amine, and the like.
The method for desulfurizing and decarbonizing the high-carbon natural gas is suitable for treating the natural gas with the hydrogen sulfide content of less than 15 mol% and the carbon dioxide content of less than 35 mol%.
The method for desulfurizing and decarbonizing the high-sulfur high-carbon natural gas has the advantages that the natural gas and the absorption liquid are dispersed into a micron-scale infinitesimal dispersion system in the infinitesimal generation device, so that the method has huge phase interface area, remarkably improves the absorption rate, further greatly reduces the size of the absorption equipment, and can finish the task of desulfurizing and decarbonizing only by a small number of tower plates; meanwhile, the heights of the liquid layers of the infinitesimal dispersion system in the infinitesimal dispersion bed and the infinitesimal dispersion section of the composite absorption tower are controllable, the gas-phase retention time can be adjusted by adjusting the heights of the liquid layers of the infinitesimal dispersion system, so that the reaction depth is controlled, and the operation elasticity is increased; in addition, the composite absorption tower can be operated under the condition of lower barren liquor circulation amount, and compared with the conventional process, the regeneration energy consumption can be obviously reduced.
Drawings
FIG. 1 is a schematic view 1 of an embodiment of the present invention. Wherein, 1-raw gas, 2-gravity separator, 3-raw gas filtering separator, 4-semi-rich liquid circulating pump, 5-semi-rich liquid, 6-first infinitesimal generator, 7-first infinitesimal dispersion system, 8-infinitesimal dispersion bed, 9-first gas-liquid separator, 10-first crude degassing, 11-rich liquid, 12, 21-poor absorption liquid, 13-composite absorption tower, 14-composite absorption tower fine suction section, 15-composite absorption tower infinitesimal dispersion section, 16-composite absorption tower infinitesimal generation section, 17-second infinitesimal generator, 18-second infinitesimal dispersion system, 19-second gas-liquid separator, 20-second crude degassing, 22-purified gas, 23-turbine, 24-flash tank, 25-flash gas, 26-lean rich liquid heat exchanger, 27-regeneration tower, 28-regeneration tower top condenser, 29-regeneration tower reflux tank, 30-acid gas, 31-regeneration tower reflux pump, 32-reboiler, 33-saturated steam, 34-lean liquid delivery pump, 35-absorption liquid storage and configuration unit, 36-lean liquid cooler, 37-filtering unit and 38-absorption liquid booster pump.
FIG. 2 is a schematic diagram of an embodiment of the present invention 2. Wherein, 1-raw gas, 2-gravity separator, 3-raw gas filtering separator, 4-semi-rich liquid circulating pump, 5, 12-semi-rich liquid, 6-first infinitesimal generator, 7-first infinitesimal dispersion system, 8-infinitesimal dispersion bed, 9-first gas-liquid separator, 10-first crude degassing, 11-rich liquid, 13-composite absorption tower, 14-composite absorption tower fine suction section, 15-composite absorption tower infinitesimal dispersion section, 16-composite absorption tower infinitesimal generation section, 17-second infinitesimal generator, 18-second infinitesimal dispersion system, 19-second gas-liquid separator, 20-second crude degassing, 21-lean absorption liquid, 22-purified gas, 23-turbine, 24-flash tank, 25-flash gas, 26-lean rich liquid heat exchanger, 27-regeneration tower, 28-regeneration tower top condenser, 29-regeneration tower reflux tank, 30-acid gas, 31-regeneration tower reflux pump, 32-reboiler, 33-saturated steam, 34-lean liquid delivery pump, 35-absorption liquid storage and configuration unit, 36-lean liquid cooler, 37-filtering unit and 38-absorption liquid booster pump.
Detailed Description
Materials, reagents and the like used in the following examples are commercially available unless otherwise specified.
FIG. 1 is a schematic diagram of an embodiment of the present invention.
As shown in fig. 1. Raw material gas 1 enters a gravity separator 2 to separate large-particle liquid drops and solid impurities, then enters a raw material gas filtering separator 3 to remove small solid particles and liquid drops which are possibly carried in the gas, then enters a first infinitesimal generating device 6 together with semi-rich liquid 5 from a semi-rich liquid circulating pump 4 to be dispersed into a first infinitesimal dispersion system 7 (the size is 1-800 mu m, the optimal value is 50-350 mu m) with micron scale, highly dispersed micron scale natural gas bubbles are dispersed phase, absorption liquid is continuous phase, and then the infinitesimal dispersion system enters a infinitesimal dispersion bed 8 (an empty barrel reactor) to carry out desulfurization and decarburization reaction. Then, the first infinitesimal dispersion system enters a first gas-liquid separator to be separated into a gas phase and a liquid phase in a separation 9, wherein the gas phase is a first crude degasification 10, and the liquid phase is a rich solution 11. The first crude degassing and the lean solution 12 from the regeneration unit are dispersed into a micron-scale second infinitesimal dispersion system 18 (the size is 1-800 μm, the optimal value is 50-350 μm) in a infinitesimal generation section 16 at the bottom of a composite absorption tower 13, highly dispersed micron-scale natural gas bubbles are dispersed phases, the absorption liquid is a continuous phase, then the second infinitesimal dispersion system enters a infinitesimal dispersion section 15 in the composite absorption tower, desulfurization and decarburization reactions occur in the infinitesimal dispersion system, then the infinitesimal dispersion system separates gas and liquid in a second gas-liquid separator 19, the liquid phase is a semi-rich solution, the semi-rich solution is circulated to the first infinitesimal generation device 6 through a semi-rich solution circulating pump 4, the gas phase is a second crude degassing 20, the gas enters a fine absorption section 14 of the composite absorption tower, the fine absorption section contains a small amount of trays or fillers, the second crude degassing is in countercurrent contact with the lean solution 21 introduced from the top of the composite absorption tower, the desulfurization and decarburization reactions continue to occur, and the purified gas 22 is discharged from the top of the composite absorption tower and enters the subsequent purification process. The rich liquid 11 from the first gas-liquid separator 9 is depressurized by a turbine 23 and enters a flash evaporation tank 24 for flash evaporation, and flash evaporation gas 25 flows out of the top of the flash evaporation tank to a fuel gas system. The rich solution flowing out of the liquid phase outlet of the flash tank enters a lean rich solution heat exchanger 26, exchanges heat with the regenerated lean solution, then is heated, and enters the inlet at the middle upper part of the regeneration tower 27. An outlet at the top of the regeneration tower is sequentially connected with a condenser 28 at the top of the regeneration tower and a reflux tank 29 of the regeneration tower, acid gas 30 is discharged from a gas phase outlet at the top of the reflux tank of the regeneration tower, reflux liquid is discharged from a liquid phase outlet at the bottom of the reflux tank of the regeneration tower, and the reflux liquid is conveyed back to the top of the regeneration tower through a reflux pump 31 of the regeneration tower; the liquid phase outlet at the bottom of the regeneration tower is connected with a reboiler 32 at the bottom of the regeneration tower, the liquid phase is heated in the reboiler and partially gasified, the liquid phase returns to the bottom of the regeneration tower, the other part of the liquid is discharged from the outlet at the bottom of the reboiler to be used as regenerated absorption liquid barren solution, the barren solution is conveyed to enter a barren and rich solution heat exchanger 26 through a barren solution conveying pump 34 to be cooled, the other part of the liquid is converged with supplementary absorption liquid from an absorption liquid storage and configuration unit 35 and then enters a barren solution cooler 36 to be further cooled, the outlet of the cooler is divided into two parts, one part of the liquid enters a filtering and purifying unit 37 to be recombined with the other part of the liquid, and the converged barren absorption liquid is pressurized through a barren absorption liquid booster pump 38 and then is conveyed to the inlet at the top end of the composite absorption tower and a second microelement generating device, so that the cyclic utilization of the absorption liquid is realized.
FIG. 2 is a schematic diagram of an embodiment of the present invention. As shown in fig. 2, a raw material gas 1 enters a gravity separator 2 to separate large-particle liquid drops and solid impurities, then enters a raw material gas filtering separator 3 to remove small solid particles and liquid drops possibly carried in the gas, then enters a first infinitesimal generator 6 together with a semi-rich liquid 5 from a semi-rich liquid circulating pump 4 to be dispersed into a first infinitesimal dispersion system 7 (the size is 10-500 μm, the optimal value is 50-350 μm) with micron-scale natural gas bubbles as a dispersed phase and an absorption liquid as a continuous phase, and then enters a infinitesimal dispersion bed 8 to perform desulfurization and decarburization reactions. Then, the first infinitesimal dispersion system enters a first gas-liquid separator to be separated into a gas phase and a liquid phase in a separation 9, wherein the gas phase is a first crude degasification 10, and the liquid phase is a rich solution 11. The first coarse degassing and the semi-rich liquid 12 from the semi-rich liquid circulating pump 4 are dispersed into a micron-scale second infinitesimal dispersion system 18 (the size is 10-500 mu m, the optimal value is 50-350 mu m) in a infinitesimal generation section 16 at the bottom of a composite absorption tower 13, highly dispersed micron-scale natural gas bubbles are in a dispersed phase, the absorption liquid is a continuous phase, then the second infinitesimal dispersion system enters a infinitesimal dispersion section 15 in the composite absorption tower, desulfurization and decarburization reaction occurs in the infinitesimal dispersion system, then the infinitesimal dispersion system separates gas and liquid in a second gas-liquid separator 19, the liquid phase is the semi-rich liquid and enters the semi-rich liquid circulating pump 4, the gas phase is the second coarse degassing 20 and enters a fine suction section 14 of the composite absorption tower, the fine suction section contains a small amount of tower plates or fillers, the second coarse degassing is in countercurrent contact with a lean liquid 21 introduced from the top of the composite absorption tower, deep desulfurization and decarburization reaction continues to occur, and the purified gas 22 is discharged from the top of the composite absorption tower and enters a subsequent purification process. The rich liquid 11 from the first gas-liquid separator 9 is depressurized by a turbine 23 and enters a flash drum 24 for flash evaporation, and flash vapor 25 flows out of the top of the flash drum to a fuel gas system. The rich solution flowing out of the liquid phase outlet of the flash tank enters a lean rich solution heat exchanger 26, exchanges heat with the regenerated lean solution, then is heated, and enters the inlet at the middle upper part of the regeneration tower 27. An outlet at the top of the regeneration tower is sequentially connected with a condenser 28 at the top of the regeneration tower and a reflux tank 29 of the regeneration tower, acid gas 30 is discharged from a gas phase outlet at the top of the reflux tank of the regeneration tower, reflux liquid is discharged from a liquid phase outlet at the bottom of the reflux tank of the regeneration tower, and the reflux liquid is conveyed back to the top of the regeneration tower through a reflux pump 31 of the regeneration tower; the liquid phase outlet at the bottom of the regeneration tower is connected with a reboiler 32 at the bottom of the regeneration tower, the liquid phase is heated in the reboiler and partially gasified, the liquid phase returns to the bottom of the regeneration tower, the other part of the liquid is discharged from the outlet at the bottom of the reboiler to be used as regenerated absorption liquid barren solution, the absorption liquid barren solution is conveyed to enter a barren and rich solution heat exchanger 26 through a barren solution conveying pump 34 to be cooled, the barren solution is merged with supplementary absorption liquid from an absorption liquid storage and configuration unit 35 and then enters a barren solution cooler 36 to be further cooled, the outlet of the cooler is divided into two parts, one part of the liquid enters a filtering and purifying unit 37 to be re-merged with the other part of the liquid without being purified, the merged barren absorption liquid is pressurized through a barren absorption liquid booster pump 38 and then is conveyed to the inlet at the top end of the composite absorption tower, and the cyclic utilization of the absorption liquid is realized.
To verify the effectiveness of the present invention, the process flow shown in fig. 2 was used, and the feed gas properties are shown in table 1. The raw material gas with the flow of 3792kmol/h and the pressure of 7.0MPa sequentially enters a gravity separator and a raw material gas filtering separator to remove solid particles and liquid drops carried in the gas, then enters a first infinitesimal generating device (a microporous membrane with the average pore diameter of 50 nanometers) together with semi-rich liquid from a semi-rich liquid circulating pump to be dispersed into a first infinitesimal dispersion system 7 (the average size is 200 micrometers) with the micrometer scale, highly dispersed micrometer scale natural gas bubbles are used as a dispersed phase, an absorption liquid is used as a continuous phase, and then the infinitesimal dispersion system enters a infinitesimal dispersion bed to perform desulfurization and decarburization reaction. Then, the first infinitesimal dispersion system enters a first gas-liquid separator (centrifugal gas-liquid separator) for separation and is separated into a gas phase and a liquid phase, wherein the gas phase is first crude degasification, and the liquid phase is rich liquid. The first coarse degasification and the second infinitesimal generating device (microporous membrane with the average pore diameter of 50 nanometers) of the semi-rich liquid from the semi-rich liquid circulating pump in the infinitesimal generating section at the bottom of the composite absorption tower are dispersed into a second infinitesimal dispersion system (with the average size of 150 micrometers) with highly dispersed micrometer natural gas bubbles as a dispersed phase and the absorption liquid as a continuous phase, then the second infinitesimal dispersion system enters the infinitesimal dispersion section in the composite absorption tower, desulfurization and decarburization reaction occurs in the infinitesimal dispersion system, then the infinitesimal dispersion system separates gas and liquid in a second gas-liquid separator (centrifugal gas-liquid separator), the liquid phase is semi-rich liquid, the liquid phase enters the semi-rich liquid circulating pump, the gas phase is the second coarse degasification and enters the fine absorption section of the composite absorption tower, the fine absorption section contains 4 tower plates, the second coarse degasification and the lean liquid (with the flow rate of 11700kmol/h, MDEA solution with MDEA concentration of 50 wt% and temperature of 40 ℃) to continuously perform deep desulfurization and decarburization reaction, and the purified gas is discharged from the top of the composite absorption tower to enter a subsequent purification process, wherein the operation conditions are shown in table 2. And the rich liquid from the first gas-liquid separator is decompressed by a turbine and then enters a flash tank for flash evaporation, and the flash evaporation gas flows out of the top of the flash tank to enter a fuel gas system. And the rich solution flowing out of the liquid phase outlet of the flash tank enters a lean-rich solution heat exchanger, exchanges heat with the regenerated lean solution, then is heated, and enters an inlet at the middle upper part of the regeneration tower. An outlet at the top of the regeneration tower is sequentially connected with a condenser at the top of the regeneration tower and a reflux tank of the regeneration tower, acid gas is discharged from a gas phase outlet at the top of the reflux tank of the regeneration tower, reflux liquid is discharged from a liquid phase outlet at the bottom of the reflux tank of the regeneration tower, and the reflux liquid is conveyed back to the top of the regeneration tower through a reflux pump of the regeneration tower; the liquid phase outlet at the bottom of the regeneration tower is connected with a reboiler at the bottom of the regeneration tower, the liquid phase is heated in the reboiler and partially gasified and returns to the bottom of the regeneration tower, the other part of liquid is discharged from the outlet at the bottom of the reboiler and is used as regenerated absorption liquid barren solution, the barren solution is conveyed to enter a barren and rich solution heat exchanger through a barren solution conveying pump to be cooled, the barren solution is merged with supplementary absorption liquid from an absorption liquid storage and configuration unit and then enters a barren solution cooler to be further cooled, the outlet of the cooler is divided into two streams, one stream enters a filtering and purifying unit to be re-merged with the other stream after impurities are removed, the merged barren amine solution is pressurized through a barren absorption liquid booster pump and then is conveyed to the inlet at the top end of the composite absorption tower, and the cyclic utilization of the absorption liquid is realized.
In contrast, a conventional alcohol amine process is adopted, which differs from the present process in the process flow in that all equipment within the dashed box of fig. 2 is replaced by a conventional plate absorption tower with a plate number of 25. The properties and flow rates of the treated feed gases are shown in Table 1, and the main process conditions are shown in Table 2.
The desulfurization and decarburization effects, equipment size and energy consumption are shown in Table 3. As can be seen from Table 3, under the same operating conditions, the absorption unit volume of the process can be reduced by about 57%, and the lean recycle is reduced to show a higher CO than the conventional alcoholamine process 2 The removal rate is reduced, and the regeneration energy consumption is obviously reduced due to the reduction of the circulation quantity of the barren solution, so that the desulfurization effect is obviously superior to that of the conventional alcohol amine absorption method process.
TABLE 1 Properties of the feed gases
TABLE 2 Main Process conditions
| Item | Scheme of the invention | Conventional alcohol amine method process |
| Size of the infinitesimal dispersion system, mum | 150-200 | - |
| Concentration of the absorption solution in wt% | 50 | 50 |
| Lean amine solution circulation volume, kmol/h | 1.170×10 4 | 1.462×10 4 |
| Temperature of lean amine solution, deg.C | 40 | 40 |
TABLE 3 desulfurization Effect, Equipment size and energy consumption
Claims (7)
1. A desulfurization and decarburization method for high-sulfur high-carbon natural gas comprises the following steps:
1) the method comprises the following steps that raw material gas (1) enters a gravity separator (2) to separate large-particle liquid drops and solid impurities, then enters a raw material gas filtering separator (3) to remove small solid particles and liquid drops carried in the gas, then enters a first infinitesimal generating device (6) at the bottom of a infinitesimal dispersing bed (8) together with circulating semi-rich liquid (5) to be dispersed into a first infinitesimal dispersing system (7) with a micron scale, wherein highly dispersed micron-scale natural gas bubbles are a dispersed phase, an absorption liquid is a continuous phase, and then the first infinitesimal dispersing system (7) enters a bed layer of the infinitesimal dispersing bed (8) to perform desulfurization and decarburization reactions;
2) the first micro-element dispersion system (7) enters a first gas-liquid separator (9) to be separated into a gas phase and a liquid phase, the gas phase is a first crude degassing gas (10), the liquid phase is a rich liquid (11), the first crude degassing gas (10) and a lean liquid (12) from a regeneration unit or a semi-rich liquid from a second gas-liquid separator (19) are dispersed into a second micro-element dispersion system (18) with a micron scale in a second micro-element generation device (17) in a micro-element generation section (16) at the bottom of a composite absorption tower (13), wherein highly dispersed micron scale natural gas bubbles are in a dispersed phase, an absorption liquid is a continuous phase, then the second micro-element dispersion system (18) enters a micro-element dispersion section (15) in the composite absorption tower (13), a desulfurization reaction is carried out in the micro-element dispersion system, then the micro-element dispersion system carries out gas-liquid degassing separation in the second gas-liquid separator (19), and the gas phase is a second crude gas phase (20), entering a fine absorption section (14) of a composite absorption tower, wherein a small amount of tower plates or fillers are contained in the fine absorption section, a second coarse degassing (20) is in countercurrent contact with a barren solution (21) introduced from the top of the composite absorption tower (13) to continuously perform desulfurization and decarburization reactions, purified gas (22) is discharged from the top of the composite absorption tower, a semi-rich solution after gas phase separation from a second infinitesimal dispersion system is pressurized by a semi-rich solution circulating pump (4) and then enters a first infinitesimal generation device (6) or is divided into two strands, one strand enters the first infinitesimal generation device (6), and the other strand enters a second infinitesimal generation device (17);
3) the rich liquid (11) from the first gas-liquid separator (9) is depressurized by a turbine (23) and enters a flash tank (24) for flash evaporation, and flash evaporation gas (25) flows out of the top of the flash tank to a fuel gas system; the rich solution flowing out of the liquid phase outlet of the flash tank enters a lean and rich solution heat exchanger (26), is heated after exchanging heat with the regenerated lean solution, and enters an inlet at the middle upper part of a regeneration tower (27); the outlet of the top of the regeneration tower is sequentially connected with a condenser (28) at the top of the regeneration tower and a reflux tank (29) of the regeneration tower, so that the absorption liquid absorbs CO in the natural gas 2 And H 2 S is enriched in acid gas, the acid gas (30) is discharged from a gas phase outlet at the top of a regeneration tower reflux tank (29), reflux liquid is discharged from a liquid phase outlet at the bottom of the regeneration tower reflux tank (29), and the reflux liquid is conveyed back to the top of the regeneration tower through a regeneration tower reflux pump (31); the outlet of the liquid phase at the bottom of the regeneration tower is connected with a reboiler (32) at the bottom of the regeneration tower, the liquid phase is heated in the reboiler and is partially gasified and returns to the bottom of the regeneration tower, the other part of liquid is discharged from the outlet at the bottom of the reboiler and is used as regenerated absorption liquid barren solution, the barren solution is conveyed by a barren solution conveying pump (34) to enter a barren and rich solution heat exchanger (26) for cooling, the barren solution is merged with supplementary absorption liquid from an absorption liquid storage and configuration unit (35) and then enters a barren solution cooler (36) for further cooling, the outlet of the cooler is divided into two parts, and one part of the two parts enters a barren solution cooler (36)The mixed lean absorption liquid is pressurized by a lean absorption liquid booster pump (38) and then is sent to the inlet at the top end of the composite absorption tower or is sent to the inlet at the top end of the composite absorption tower and a second infinitesimal generating device.
2. The method of claim 1, wherein: in the method, the infinitesimal dispersion system is separated into a gas phase and a liquid phase by a gas-liquid separator, the gas phase is coarse degasification, and the liquid phase is semi-rich liquid or rich liquid, wherein the gas-liquid separator is one or a combination of a centrifugal separator, a gravity separator, a baffling separator, a filler separator, a wire mesh separator and a microfiltration separator which can separate bubbles with the diameter of more than 30 micrometers from the liquid phase in series or in parallel.
3. The method according to claim 1 or 2, characterized in that: in the method, the first infinitesimal generating device and the second infinitesimal generating device are devices which can disperse gas-liquid two phases into infinitesimal states; the device is formed by one or more of a microporous membrane, a Venturi type micro bubble generating device, an ultrasonic cavitation device, a hydrodynamic cavitation type micro bubble generating device, a centrifugal type micro bubble generating device, a jet type micro bubble generating device and a rotational flow type micro bubble generating device which can cut a gas-liquid two-phase system into micro elements with the size of 1-800 mu m in series and parallel connection.
4. The method according to claim 1 or 2, characterized in that: in the method, the infinitesimal dispersion bed is a hollow cylinder reactor or a shell containing a baffle internal component, the infinitesimal dispersion system generated by the infinitesimal generation device is arranged in the shell, and a series of outlets are arranged at different heights so as to adjust the liquid level.
5. The method according to claim 1 or 2, characterized in that: the composite absorption tower comprises a composite absorption tower fine absorption section, a composite absorption tower infinitesimal dispersion section and a composite absorption tower infinitesimal generation section from the top to the bottom in sequence.
6. The method according to claim 1 or 2, characterized in that: the operating pressure of the first and second micro-element generating devices and the composite absorption tower is 3-15MPa, the operating temperature is 30-90 ℃, and the gas-liquid ratio of the raw material gas to the poor absorption liquid is 100-4000Nm 3 /m 3 。
7. The method according to claim 1 or 2, characterized in that: the method is suitable for treating natural gas with hydrogen sulfide content of less than 15 mol% and carbon dioxide content of less than 35 mol%.
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