CN111996049A - Device and method for removing acid gas in natural gas by combining hydrate method and membrane separation method - Google Patents
Device and method for removing acid gas in natural gas by combining hydrate method and membrane separation method Download PDFInfo
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- 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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- C10L3/00—Gaseous fuels; Natural gas; Synthetic natural gas obtained by processes not covered by subclass C10G, C10K; Liquefied petroleum gas
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- 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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- 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
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- C10L3/108—Production of gas hydrates
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- C10L2290/00—Fuel preparation or upgrading, processes or apparatus therefore, comprising specific process steps or apparatus units
- C10L2290/54—Specific separation steps for separating fractions, components or impurities during preparation or upgrading of a fuel
- C10L2290/541—Absorption of impurities during preparation or upgrading of a fuel
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- C10L2290/00—Fuel preparation or upgrading, processes or apparatus therefore, comprising specific process steps or apparatus units
- C10L2290/54—Specific separation steps for separating fractions, components or impurities during preparation or upgrading of a fuel
- C10L2290/548—Membrane- or permeation-treatment for separating fractions, components or impurities during preparation or upgrading of a fuel
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- 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
- C10L2290/00—Fuel preparation or upgrading, processes or apparatus therefore, comprising specific process steps or apparatus units
- C10L2290/56—Specific details of the apparatus for preparation or upgrading of a fuel
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Abstract
The invention provides a device and a method for removing acid gas in natural gas by combining a hydrate method and a membrane separation method, which comprises a raw material gas separator, a buffer tank, a mixed gas separator, a decomposition tower, a dehydrator, a gas preheater, a compressor, and H2S/CO2Concentration detector, gas collection storage tank, etc. Removing solid impurities from natural gas by a raw material gas separator, feeding the natural gas into a mixing separator, and generating H under appropriate conditions2S/CO2Hydrate, setting H on natural gas pipeline2S/CO2And a concentration detector for performing multiple purifications according to concentration requirements. The device can quickly and effectively remove the acid gas in the natural gas by coupling the hydrate method and the membrane separation method, and the separated gas has high purity, low energy consumption, less investment and wide market prospect.
Description
Technical Field
The invention belongs to the field of natural gas desulfurization and decarburization, and particularly relates to a device and a method for removing acid gas in natural gas by combining a hydrate method and a membrane separation method.
Background
The natural gas produced in oil and gas fields is mainly composed of hydrocarbon and various impurity gases, and its main component is methane, besides, it also contains H2S、CO2The existence of the acidic substances can not only corrode pipelines and equipment, but also bring serious pollution to the environment, so that the nation has strict indexes on the content of the acidic gas in the natural gas for commodities, in recent years, with the proposal of an energy-saving and emission-reducing concept, the nation has stricter and stricter requirements on the aspect, and the efficient desulfurization and decarburization of the mined natural gas becomes the key for reasonably utilizing natural gas resources. Chemical absorption was earlier proposed for removing H from natural gas2S、CO2And the like, but the method has the problems of high energy consumption, low removal rate, environmental pollution and the like.
The temperature and pressure of the gas separated by the hydrate method are different according to the formation of the hydrate by different gases, the gas component which is not easy to hydrate is enriched in a gas phase, and the component which is easy to hydrate is enriched in a hydrate phase. At the same temperature, H2S、CO2、CH4The pressures at which hydrates are formed are different, so that H can be separated by the hydrate method2S/CO2/CH4And (4) mixing the gases. The membrane separation method is a process of separating different gas relative permeabilities of a polymer membrane under the action of partial pressure difference at two sides of the membrane by utilizing different dissolution and diffusion rates of different gas components in the polymer membrane. The membrane separation method has many unique advantages, such as small occupied area, energy conservation, environmental protection and the like, and is particularly suitable for treating CO because of the principle of membrane separation and simple element structure, low investment, low operation cost and flexibility of conveniently expanding treatment capacity2High-concentration raw gas, wide variation range of characteristics of produced gas, difficulty in meeting the purification rate of various working conditions by using a single-stage membrane system, and capability of obtaining high-purity CO2And high purity CH4A gas. Due to the fact thatTherefore, it is highly desirable to invent a method for removing H from natural gas by combining a hydrate method and a membrane separation method2S、CO2And sulfide thereof.
In patent document "201910274386.8" a method and apparatus for purifying gas based on gas separation principle of hydrate method "a method and apparatus for purifying gas by hydrate method is disclosed, but the method adopts multiple tower circulation operation and single hydrate method, so that the removal efficiency is low, the removal purity is not high, the occupied area of equipment is large, the investment cost is high and the equipment management is difficult.
Disclosure of Invention
In order to overcome the problems in the prior art, the invention provides a device and a method for removing acid gas in natural gas by combining a hydrate method and a membrane separation method, which have the advantages of good stability, high acid gas removal rate and good recovery effect in natural gas deacidification and are mainly used for onshore oil and gas fields with high CO content2And H2S purification treatment of natural gas, and can also be used in the field of gas separation of methane, factory flue gas and the like.
In order to realize the technical purpose of the invention, the adopted technical scheme is as follows: a device for removing acid gas in natural gas by combining a hydrate method and a membrane separation method is characterized in that: comprises a raw material gas separator, a buffer tank, a gas preheater and an H gas separator which are sequentially connected and arranged along the gas flow direction of the raw material gas through a pipeline2S removal unit, compressor, CO2A removal unit, a dehydrator and a methane collection storage tank;
H2the S removing unit comprises: mixed gas separator II, booster pump and H2An S concentration detector; a separation membrane II is arranged in the mixed gas separator II and divides the interior of the mixed gas separator II into an upper layer and a lower layer, wherein the lower layer is used for containing H2S absorption liquid, H2S, the liquid level of the absorption liquid is separated from the separation membrane II by a distance to form a separation cavity; the gas inlet nozzle and the gas inlet nozzle are arranged on the lower layer of the mixed gas separator II in a staggered manner2An S hydrate slurry outlet and a liquid supplementing port, wherein the gas inlet nozzle is positioned at H2S is below the liquid level of the absorption liquid;the bottom of the mixed gas separator II positioned on the lower layer is provided with a stirring device, the top of the mixed gas separator II positioned on the upper layer is provided with a gas outlet, a gas inlet nozzle of the mixed gas separator II is connected with a gas preheater through a pipeline provided with a booster pump, and the gas outlet of the mixed gas separator II is connected with a compressor; h2The S concentration detector is arranged at the upper gas outlet of the mixed gas separator II3 and is used for detecting H in the gas discharged from the gas outlet2Whether the concentration of S reaches the standard or not; and also comprises H2S muffler, H2One end of the S air return pipe is connected with an air outlet of the mixed gas separator II, and the other end of the S air return pipe is connected with the mixed gas separator II positioned below the separation membrane II;
CO2the removing unit comprises a mixed gas separator I and CO2A concentration detector; a separation membrane I is arranged in the working cavity of the mixed gas separator I, and divides the separation cavity of the mixed gas separator I into an upper layer and a lower layer, wherein the lower layer is used for containing CO2Absorption liquid, CO2The liquid level of the absorption liquid is separated from the separation membrane I at a certain distance to form a separation cavity I, the gas is separated in the separation cavity I through the separation membrane I, and the side wall or the bottom wall of the lower mixed gas separator I is provided with a gas inlet nozzle and a CO staggered2The device comprises a hydrate slurry outlet and a liquid supplementing port, wherein a stirring device is arranged at the bottom of a mixed gas separator I, a gas outlet is arranged at the top of the mixed gas separator I positioned on the upper layer, and the gas outlet of the mixed gas separator I is connected with a dehydrator; and further comprises CO2Muffler, CO2One end of the air return pipe is connected with an air outlet of the mixed gas separator I, and the other end of the air return pipe is connected with the lower layer of the mixed gas separator I.
Further, CO2The removal unit also comprises a decomposition column I and CO2A collecting storage tank I, a microwave heating device is arranged in the decomposing tower I, the top of the decomposing tower I is provided with an air outlet, and the upper part of the decomposing tower I is provided with CO2Hydrate slurry inlet with water outlet at the bottom, gas outlet of decomposition tower I and CO2Collecting storage tank I connected, CO2Hydrate slurry inlet and CO2The hydrate slurry outlet is connected, and the water outlet of the decomposing tower I is connected with the liquid supplementing port of the mixed gas separator I.
Further, H2S removalThe unit also comprises a decomposing tower II provided with a microwave heating device, and a decomposing tower H2S, collecting a storage tank; the upper part of the decomposing tower II is provided with H2An S hydrate slurry inlet with an air outlet at the top and a water outlet at the lower part, wherein H2S hydrate slurry inlet and H2The S hydrate slurry outlet is connected, the water outlet of the decomposing tower II is connected with the liquid supplementing port of the mixed gas separator II, and the gas outlet of the decomposing tower II is connected with the gas inlet H2And S, collecting the storage tank.
A method for removing acid gas in natural gas by combining a hydrate method and a membrane separation method into a whole is carried out based on a device for removing acid gas in natural gas by combining the hydrate method and the membrane separation method into a whole, and specifically comprises the following steps:
step 1: inputting H into the mixed gas separator II through a liquid supplementing port of the mixed gas separator II2The S absorption liquid inputs CO into the mixed gas separator I through a liquid supplementing port of the mixed gas separator I2An absorption liquid; CO 22The absorption liquid is a uniform mixed liquid of an accelerator, tetrabutylammonium bromide aqueous solution and diesel oil-cyclopentane mixed emulsion; the accelerant contains sodium dodecyl sulfate and sodium dodecyl benzene sulfonate;
step 2: starting a stirring device in a mixed gas separator II, removing solid impurities from natural gas by a raw material gas separator 1, then feeding the natural gas into a buffer tank, stabilizing the flow of the natural gas by the buffer tank, then feeding the natural gas into a gas preheater, raising the temperature of the gas to 38-40 ℃ by the gas preheater and removing water vapor, then uniformly and stably feeding H in a bubbling manner through a gas inlet nozzle of the mixed gas separator II after the natural gas is pressurized by a booster pump2S absorption liquid, wherein part of H2S gas is H2S absorption liquid absorbs and reacts to generate H2S hydrate, H not absorbed in time2S gas is intercepted in the separation cavity by the separation membrane II and is carried out by H2S, continuously absorbing by using absorption liquid;
and step 3: starting a stirring device in the mixed gas separator I, and enabling gas penetrating through the separation membrane II to pass through H arranged at an air outlet of the mixed gas separator II2S concentration detector detecting H2S concentration, if the concentration does not reach the standard, the concentration is determined by H2S return gas pipe returns mixed gas for separationThe device II is separated again to remove H2S, circulating until the concentration meets the requirement, entering a compressor after the concentration meets the standard, compressing by the compressor, and introducing CO in a bubbling manner through an air inlet nozzle of a mixed gas separator I2Absorption liquid in which part of CO2Gas CO2Absorbing by the absorption liquid and reacting to generate CO2Hydrates, CO not absorbed in time2The gas is intercepted in the separation cavity by the separation membrane I and is subjected to CO2Continuously absorbing by the absorption liquid; the gas permeating the separation membrane I passes through CO arranged at the gas outlet of the mixed gas separator I2Detecting by a concentration detector, and detecting by CO if the concentration does not reach the standard2The return air pipe is sent back to the mixed gas separator I for separating again to remove CO2Circularly reciprocating until the concentration reaches the requirement, dehydrating by a dehydrator, and feeding into CH after the concentration reaches the standard4And collecting and storing the water in the tank.
Furthermore, the rotating speed of the stirring device is 1000r/min, so that the CO is greatly improved2The dissolution rate is controlled so that the dissolution saturation can be achieved within 3min, and the dissolution rate is controlled in CO2The stirring effect is more remarkable in the dissolving and nucleating processes, the hydrate induction time is shortened, the energy consumption is reduced, and CO is2Induction time compared to CH4Much less when CO is present2After formation of hydrate, CH4Also in the gas phase, CH can be realized4With CO2Is rapidly separated, CH is reduced4Loss of (2).
Furthermore, the microwave heating device at the bottom of the separation tower I has the microwave power of 50KW, the decomposition of the hydrate by the microwave heating method is far faster than the water bath heating, the decomposition speed of the hydrate is increased, but the microwave energy consumption is far less than the water bath heating, so that the energy consumption of the whole device is reduced, and the hydrate decomposition by the microwave method is economic and effective.
Furthermore, after the pressure of the mixed gas is increased by the booster pump, the pressure of the mixed gas is 1.5MPa to 1.8MPa, and the concentration of the permeation gas of the polyimide separation membrane can be effectively increased by increasing the gas inlet pressure.
Furthermore, the film material is a polyimide film.
Further, the rated power of the compressor is 50KW, and the pressure of the gas pressurized by the compressor is 2-3 MPa.
Further, the gas preheater is a plate preheater.
Further, the decomposing tower I and/or the decomposing tower II are plate-type rectifying towers.
Further, to avoid H2S and sulfide corrode the pipeline, and the pipeline material should be aluminum alloy or stainless steel.
Furthermore, the temperature of the gas is increased to about 38-40 ℃ through the gas preheater, and the temperature of the residual gas and the temperature of the permeated gas are not lower than the dew point temperature, so that no liquid drop is generated when the gas enters the membrane component, and the phenomenon that the normal operation of the membrane separation system is influenced by the condensation of the liquid drop and the oil drop on the surface of the membrane is avoided.
Further, the method is used for H in natural gas2The S separation and removal device also comprises a compressor and an H2H between S concentration detectors2S cycle removal unit, said H2S concentration detector detecting H2Whether the concentration of S meets the requirement or not, if the concentration of S is removed to meet the requirement, the gas is compressed by a compressor and then enters a separation cavity of a mixed gas separator I through a nozzle; if H is2And if the concentration of S does not meet the requirement, the gas needs to be further purified, and the gas passing through the upper gas outlet of the mixed gas separator enters the mixed gas separator I again through a pipeline and is circularly purified until the concentration requirement is met.
Furthermore, the tetrabutylammonium bromide (TBAB) aqueous solution and the diesel-Cyclopentane (CP) mixed emulsion are used as separation media, under the synergistic effect, water can form microemulsion in oil-water emulsion, the gas-liquid contact area is increased, and CO in gas phase2The content is obviously reduced, the hydrate/diesel slurry is well dispersed after the separation and the balance, the aggregation and the blockage of the hydrate do not occur, and the whole slurry system shows good fluidity.
CO in the gas mixture separator I2Gradually forming a set amount of CO at the temperature of between 0 and 7 ℃ and under the pressure of between 2 and 3MPa2Hydrate of CO generated in the gas separator I2Injecting hydrate slurry into a decomposition tower I, installing a microwave heating device at the bottom of the decomposition tower I to promote hydrate decomposition, and CO2The hydrate slurry flows from the uppermost layer to the lowermost layer of the top of the decomposing tower I step by step and is decomposed to generate water and CO2Gas, CO2The gas passes through a gas outlet at the upper part of the decomposition tower I and is made of CO2Collecting water and CO generated in the collecting storage tank2And the absorption liquid is injected into the mixed gas separator I again through a liquid supplementing port of the mixed gas separator I and circulates in sequence.
Furthermore, it should be noted that "connected" in the present invention may be directly connected or indirectly connected, and the final purpose is to achieve communication through the connection.
Compared with the existing natural gas purification method, the method has the advantages that:
(1) the device in the process flow comprises the buffer tank and the nozzle, wherein the buffer tank has a flow stabilizing effect, and the nozzle can enable the raw material gas to enter the mixed gas separator in a bubbling mode, so that the generation of the hydrate can be further promoted, the induction time can be shortened, and the whole process can be continuously and circularly carried out.
(2) The process flow of the invention is more flexible, the types of the specific mixed gas are more, the cost is low, and the effect is good. Such as CO in natural gas2High in content of H2When the S content is extremely low, CO can be directly carried out2Removal of (2), shutting off H2The S removal unit reduces the cost, increases a device capable of realizing multiple cycles, makes the separated gas purer, and judges whether the gas concentration reaches the standard according to the information fed back by the gas concentration detector on the pipeline.
(3) The invention replaces the previous multi-tower continuous separation device, has low installation cost, simple and easy operation, small occupied area, low energy consumption and improved removal efficiency, and finally obtains the methane gas with high purity which is more than 99 percent.
(4) Without the consumption of solvents and chemicals, space for processing and storage can be saved for the platform, while reducing the cost of logistics and transportation of these solvents and chemicals.
(5) The stirring device, the microwave heating device, the supercharging device, the hydrate accelerant, the oil-water system and the like arranged in the gas-liquid separator improve the decomposition efficiency to a certain extent, greatly shorten the separation time of the mixed gas and improve the efficiency of separating the mixed gas.
Compared with the common natural gas desulfurization and decarburization method, the method and the device provided by the invention are more economical and feasible, and can efficiently remove the acid gas in the natural gas to make the acid gas reach the pipeline transportation and use standards.
Drawings
FIG. 1 is a schematic flow chart of desulfurization and decarburization of natural gas by the method and apparatus of the present invention.
The reference numbers in the figures are as follows: 1-raw material gas separator; 2-a buffer tank; 3-mixed gas separator II; 4-decomposition column II; 5-a dehydrator; 6-decomposition tower I; 7-mixed gas separator I; 8-a booster pump; 9-H2S, collecting a storage tank; 10-microwave heating means; 11-H2An S concentration detector; 12-a compressor; 13-CO2A concentration detector; 14-a stirring device; 15-polyimide separation membrane I; 16-polyimide separation membrane II; 17-a gas preheater; 18-CO2A collection storage tank; 19-CH4And (5) collecting the storage tank.
Detailed Description
The invention is described in more detail below with reference to the following examples:
in practice, to accelerate CO2Hydrate formation, increase of hydration rate, CO2The absorption liquid is a uniform mixed liquid of an accelerant, tetrabutylammonium bromide aqueous solution and diesel oil-cyclopentane mixed emulsion, and the accelerant is composed of 0.05% of Sodium Dodecyl Sulfate (SDS) and 0.05% of Sodium Dodecyl Benzene Sulfonate (SDBS) which act together. TBAB aqueous solution/diesel oil-CP mixed emulsion (refer to patent publication: Huand Liu, Jin Wang, et al. high-efficiency separation of a CO)2/H2The mixed via hydrate formation in W/O emulsions in the presence of a cyclic and TBAB. international outlet of hydrogen energy 39(2014)7910-7918) are used as separation media, and under the synergistic action, water can form micro-emulsion in oil-water emulsion, so that the gas-liquid contact area is increased, and the gas phase is in gas phaseCO2The content is obviously reduced, the hydrate/diesel slurry is well dispersed after the separation and the balance, the aggregation and the blockage of the hydrate do not occur, and the whole slurry system shows good fluidity.
As shown in fig. 1, the device for removing acid gas from natural gas by integrating hydrate method and membrane separation method includes: a raw material gas separator 1, a buffer tank 2, a gas preheater 17 and a gas preheater H which are sequentially connected and arranged along the gas flow direction of the raw material gas through pipelines2S removal unit, compressor 12, CO2A removal unit, a dehydrator 5 and a methane collection tank 19.
H2The S removing unit comprises: a mixed gas separator II3, a booster pump 8, a decomposing tower II4 provided with a microwave heating device 10, and a decomposition tower H2S concentration detector 11, H2S collecting reservoir 9. A polyimide separation membrane II15 is arranged in the mixed gas separator II3, the polyimide separation membrane II15 divides the interior of the mixed gas separator II3 into an upper layer and a lower layer, wherein the lower layer is used for containing H2S absorption liquid, H2The distance between the liquid level of the S absorption liquid and the polyimide separation membrane II15 (H can be monitored by arranging a liquid level monitor)2S liquid level of the absorption liquid) for forming the separation chamber. The lower wall surface of the mixed gas separator II3, namely the air inlet nozzle and the H are arranged below the polyimide separation membrane II15 in a staggered manner2An S hydrate slurry outlet and a liquid supplementing port, wherein the gas inlet nozzle and the H2The S hydrate slurry outlets are all positioned at H2Preferably, H is present below the surface of the S-absorbent solution2And an S hydrate slurry outlet is arranged at the bottom of the mixed gas separator II 3. The bottom of the mixed gas separator II3 is provided with a stirring device 14, the top of the mixed gas separator II3 is provided with a gas outlet, a gas inlet nozzle of the mixed gas separator II3 is connected with a gas preheater 17 through a pipeline provided with a booster pump 8, and the gas outlet of the mixed gas separator II3 is connected with a compressor 12. The upper part of the decomposing tower II4 is provided with H2An S hydrate slurry inlet, an air outlet arranged at the top and a water outlet arranged at the lower part, wherein the H of the decomposing tower II42An S hydrate slurry inlet is communicated with H of a mixed gas separator II3 through a slurry pipeline2The S hydrate slurry outlet is connected, the water outlet of the decomposing tower II4 is connected with the liquid supplementing port of the mixed gas separator II3, and the decomposing towerII4 outlet connection H2S collecting reservoir 9. The upper gas outlet of the mixed gas separator II3 is connected with H2And an S concentration detector 11 for detecting whether the concentration of the treatment gas reaches the standard. And also comprises H2S muffler, H2One end of the S air return pipe is connected with the air outlet of the mixed gas separator II3, and the other end is connected with the mixed gas separator II3 positioned below the polyimide separating membrane II15, preferably positioned at H2Under the liquid level of the S absorption liquid, if the removal concentration meets the requirement, the gas is compressed by the compressor 12 and then enters CO2A removal unit; if H is2The concentration of S does not meet the requirement, the gas at the gas outlet is led to pass through H2The S return air pipe is sent back to the mixed gas separator II3 for separation again to remove H2And S, circularly purifying until the concentration requirement is met.
CO2The removing unit comprises a mixed gas separator I7, a decomposing tower I6 and CO2Collecting storage tank I18 and CO2And a concentration detector 13. A polyimide separation membrane I16 is arranged in a working cavity of the mixed gas separator I7, the polyimide separation membrane I16 divides the separation cavity of the mixed gas separator I7 into an upper layer and a lower layer, wherein the lower layer is used for containing CO2Absorption liquid, CO2The liquid level of the absorption liquid is separated from the polyimide separation membrane I16 at a certain distance to form a separation cavity, the gas is separated in the separation cavity by the polyimide separation membrane I16, and the side wall or the bottom wall of the lower layer of the mixed gas separator I7 is provided with a gas inlet nozzle and a CO staggered2A hydrate slurry outlet, a liquid supplementing port, a stirring device 14 arranged at the bottom of the mixed gas separator I7, and gas passing through CO in a bubbling manner2The absorption liquid enters the separation cavity.
The microwave heating device 10 is arranged in a decomposition tower I6, the top of the decomposition tower I6 is provided with an air outlet, and the upper part is provided with CO2Hydrate slurry inlet with water outlet at the bottom, wherein the gas outlet of the decomposition tower I6 and CO2The collecting storage tank I18 is connected with the CO of the decomposing tower I62CO of hydrate slurry inlet and mixed gas separator I72The hydrate slurry outlet is connected, and the water outlet of the decomposing tower I6 is connected with the liquid supplementing port of the mixed gas separator I7. CO is arranged at the gas outlet of the mixed gas separator I72A concentration detector 13 for detecting CO in the gas2Whether the concentration reaches the standard or not. And further comprises CO2Muffler, CO2One end of the air return pipe is connected with an air outlet of a mixed gas separator I7, and the other end is connected with a mixed gas separator I7 positioned below the polyimide separation membrane I16, preferably positioned at the position of CO2Under the surface of the absorption liquid, if CO2When the concentration reaches the requirement, the gas enters CH after being dehydrated by a dehydrator 54A collection tank 19; if CO is present2If the concentration does not meet the requirement, the gas needs to be further purified and treated by CO2The return air pipe is sent back to the mixed gas separator I7 for separating again to remove CO2And circularly purifying until the concentration requirement is met.
A method for removing acid gas in natural gas by combining a hydrate method and a membrane separation method into a whole is carried out based on a device for removing acid gas in natural gas by combining the hydrate method and the membrane separation method into a whole, and specifically comprises the following steps:
step 1: inputting H into a mixed gas separator II3 through a liquid supplementing port2The S absorption liquid is used for inputting CO into the mixed gas separator I7 through a liquid supplementing port2An absorption liquid; CO 22The absorption liquid comprises an accelerator and tetrabutylammonium bromide (TBAB) aqueous solution/diesel oil-CP mixed emulsion. The accelerant contains Sodium Dodecyl Sulfate (SDS) with the mass fraction of 0.05 percent and Sodium Dodecyl Benzene Sulfonate (SDBS) with the mass fraction of 0.05 percent;
step 2: the natural gas enters the buffer tank 2 after solid impurities are removed through the raw material gas separator 1, after water vapor is removed through the steady flow effect of the buffer tank 2 and the heating of the gas preheater 17, the temperature of the gas is increased to about 38-40 ℃ through the gas preheater 17, the temperature of residual gas intercepted by the polyimide separation membrane I16 or the polyimide separation membrane II15 and the temperature of permeation gas passing through the polyimide separation membrane I16 or the polyimide separation membrane II15 are not lower than the dew point temperature, and therefore the gas is ensured not to have liquid drops when entering the polyimide separation membrane I16 or the polyimide separation membrane II15, and the phenomenon that the liquid drops and the oil drops are condensed on the surface of the membrane to influence the normal operation of a membrane separation system is avoided. The natural gas heated by the preheater 17 is pressurized by a booster pump 8 and then uniformly and stably introduced into H in a bubbling mode through an air inlet nozzle of a mixed gas separator II32S absorption liquidWherein part H2S gas is H2S absorption liquid absorbs and reacts to generate H2S hydrate, H not absorbed in time2S gas is intercepted in the separation cavity by a polyimide separation membrane II15 and is subjected to H2And continuously absorbing the S absorption liquid. The stirring device 14 is used for shortening H2Induction time for S hydrate formation;
and step 3: the gas passing through the polyimide separation membrane II15 passes through H arranged at the gas outlet of the mixed gas separator II32The S concentration detector 11 enters the compressor 12 after the detected concentration reaches the standard, and after the gas is compressed by the compressor 12 (the gas pressure is increased, the gas permeation efficiency can be effectively improved, and the gas can reach the pressure for forming hydrate), the gas is introduced into the CO in the mixed gas separator I7 in a bubbling mode through the gas inlet nozzle of the mixed gas separator I72Absorption liquid in which part of CO2Gas CO2Absorbing by the absorption liquid and reacting to generate CO2Hydrates, CO not absorbed in time2The gas is intercepted in the separation cavity by a polyimide separation membrane I16 and is subjected to CO2The absorption liquid continues to absorb, and the stirring device 14 is used for shortening CO2Induction time for hydrate formation. The gas passing through the polyimide separation membrane I16 was passed through CO at the gas outlet provided above the mixed gas separator I72The concentration detector 13 detects that if the concentration does not reach the standard, further purification is needed, and CO is used2The return air pipe is sent back to the mixed gas separator I7 for separating again to remove CO2Circulating until the concentration reaches the requirement, dehydrating by a dehydrator and feeding CH if the concentration reaches the requirement4And collecting and storing the water in the tank.
H in mixed gas separator II32S is at 0-7 ℃ and 2-3MPa (the mixed gas separator II3 is provided with a jacket, a circulating cooling medium is introduced into the jacket for adjusting the internal gas temperature to reach the temperature for forming the hydrate), and H with a set amount is generated in the mixed gas separator II32After S hydrate slurry is obtained, H generated by a mixed gas separator II32Injecting S hydrate slurry into decomposing tower II4 and H inside decomposing tower II42The S hydrate slurry flows from the uppermost layer to the lowermost layer of the tower top step by stepAfter decomposition H is obtained2The microwave heating device 10 is arranged at the bottom of the S gas mixing and decomposing tower II4 to accelerate the decomposition rate of hydrate slurry, H2The S gas flows out of a gas outlet of the decomposing tower II4 and enters H2S collecting tank 9, H2And the S absorption liquid and the make-up water are injected into the mixed gas separator II3 again through a water outlet of the decomposing tower II4, and are circulated in sequence to complete the absorption treatment of sulfide in the natural gas.
H2The S absorption liquid is a uniform mixed liquid of N-Methyldiethanolamine (MEDA) solution and an accelerant, and the accelerant contains Sodium Dodecyl Sulfate (SDS) with the mass fraction of 0.05% and Sodium Dodecyl Benzene Sulfonate (SDBS) with the mass fraction of 0.05% to play a role together.
CO in the mixture gas separator I72Gradually forming a set amount of CO under the conditions that the temperature is between 0 and 7 ℃ and the pressure is between 2 and 3MPa (a mixed gas separator I7 is provided with a jacket, and a circulating cooling medium is introduced into the jacket and is used for adjusting the internal gas temperature to reach the temperature for forming the hydrate)2Hydrate, CO generated in the mixed gas separator I72Injecting hydrate slurry into a decomposition tower I6, and installing a microwave heating device 10 at the bottom of the decomposition tower I6 to promote CO2Decomposition of hydrate, CO2The hydrate slurry flows from the uppermost layer of the top of the decomposing tower I6 to the lowermost layer gradually and generates CO after decomposition2Absorption liquid and CO2Gas, CO2The gas passes through a gas outlet at the upper part of a decomposition tower I6 and is led by CO2Collecting water and CO generated in the collecting tank 182And the absorption liquid is injected into the mixed gas separator I7 again through a liquid supplementing port of the mixed gas separator I7 and circulates sequentially.
The above description is only for the preferred embodiment of the present invention, but the scope of the present invention is not limited thereto, and any person skilled in the art should be considered to be within the technical scope of the present invention, and the technical solutions and their concepts should be equivalent or changed within the technical scope of the present invention.
The present invention is not limited to the following embodiments, and those skilled in the art can implement the present invention in other embodiments according to the disclosure of the present invention, or make simple changes or modifications on the design structure and idea of the present invention, and fall into the protection scope of the present invention. It should be noted that the embodiments and features of the embodiments may be combined with each other without conflict.
In the description of the present invention, it is to be understood that the terms "center", "longitudinal", "lateral", "up", "down", "front", "back", "left", "right", "vertical", "horizontal", "top", "bottom", "inner", "outer", and the like, indicate orientations or positional relationships based on those shown in the drawings, and are used only for convenience in describing the present invention and for simplicity in description, and do not indicate or imply that the referenced devices or elements must have a particular orientation, be constructed and operated in a particular orientation, and thus, are not to be construed as limiting the present invention. Furthermore, the terms "first", "second", etc. are used for descriptive purposes only and are not to be construed as indicating or implying relative importance or implicitly indicating the number of technical features indicated. Thus, a feature defined as "first," "second," etc. may explicitly or implicitly include one or more of that feature. In the description of the present invention, "a plurality" means two or more unless otherwise specified.
In the description of the present invention, it should be noted that, unless otherwise explicitly specified or limited, the terms "mounted," "connected," and "connected" are to be construed broadly, e.g., as meaning either a fixed connection, a removable connection, or an integral connection; can be mechanically or electrically connected; they may be connected directly or indirectly through intervening media, or they may be interconnected between two elements. The specific meaning of the above terms in the present invention can be understood by those of ordinary skill in the art through specific situations.
Claims (8)
1. A device for removing acid gas in natural gas by combining a hydrate method and a membrane separation method is characterized in that: comprises the raw material gas is sequentially connected through a pipeline along the gas flow direction of the raw material gasThe raw material gas separator, the buffer tank, the gas preheater and the gas preheater are arranged2S removal unit, compressor, CO2A removal unit, a dehydrator and a methane collection storage tank;
H2the S removing unit comprises: mixed gas separator II, booster pump and H2An S concentration detector; a separation membrane II is arranged in the mixed gas separator II and divides the interior of the mixed gas separator II into an upper layer and a lower layer, wherein the lower layer is used for containing H2S absorption liquid, H2S, the liquid level of the absorption liquid is separated from the separation membrane II by a distance to form a separation cavity; the gas inlet nozzle and the gas inlet nozzle are arranged on the lower layer of the mixed gas separator II in a staggered manner2An S hydrate slurry outlet and a liquid supplementing port, wherein the gas inlet nozzle is positioned at H2S is below the liquid level of the absorption liquid; the bottom of the mixed gas separator II positioned on the lower layer is provided with a stirring device, the top of the mixed gas separator II positioned on the upper layer is provided with a gas outlet, a gas inlet nozzle of the mixed gas separator II is connected with a gas preheater through a pipeline provided with a booster pump, and the gas outlet of the mixed gas separator II is connected with a compressor; h2The S concentration detector is arranged at the upper gas outlet of the mixed gas separator II3 and is used for detecting H in the gas discharged from the gas outlet2Whether the concentration of S reaches the standard or not; and also comprises H2S muffler, H2One end of the S air return pipe is connected with an air outlet of the mixed gas separator II, and the other end of the S air return pipe is connected with the mixed gas separator II positioned below the separation membrane II;
CO2the removing unit comprises a mixed gas separator I and CO2A concentration detector; a separation membrane I is arranged in the working cavity of the mixed gas separator I, and divides the separation cavity of the mixed gas separator I into an upper layer and a lower layer, wherein the lower layer is used for containing CO2Absorption liquid, CO2The liquid level of the absorption liquid is separated from the separation membrane I at a certain distance to form a separation cavity I, the gas is separated in the separation cavity I through the separation membrane I, and the side wall or the bottom wall of the lower mixed gas separator I is provided with a gas inlet nozzle and a CO staggered2The device comprises a hydrate slurry outlet and a liquid supplementing port, wherein a stirring device is arranged at the bottom of a mixed gas separator I, a gas outlet is arranged at the top of the mixed gas separator I positioned on the upper layer, and the gas outlet of the mixed gas separator I is connected with a dehydrator;and further comprises CO2Muffler, CO2One end of the air return pipe is connected with an air outlet of the mixed gas separator I, and the other end of the air return pipe is connected with the lower layer of the mixed gas separator I.
2. The device for removing acid gas in natural gas by combining the hydrate method and the membrane separation method as claimed in claim 1, wherein: CO 22The removal unit also comprises a decomposition column I and CO2A collecting storage tank I, a microwave heating device is arranged in the decomposing tower I, the top of the decomposing tower I is provided with an air outlet, and the upper part of the decomposing tower I is provided with CO2Hydrate slurry inlet with water outlet at the bottom, gas outlet of decomposition tower I and CO2Collecting storage tank I connected, CO2Hydrate slurry inlet and CO2The hydrate slurry outlet is connected, and the water outlet of the decomposing tower I is connected with the liquid supplementing port of the mixed gas separator I.
3. The device for removing acid gas in natural gas by combining the hydrate method and the membrane separation method as claimed in claim 1, wherein: said H2The S removing unit also comprises a decomposing tower II and a decomposing tower H which are provided with microwave heating devices2S, collecting a storage tank; the upper part of the decomposing tower II is provided with H2An S hydrate slurry inlet with an air outlet at the top and a water outlet at the lower part, wherein H2S hydrate slurry inlet and H2The S hydrate slurry outlet is connected, the water outlet of the decomposing tower II is connected with the liquid supplementing port of the mixed gas separator II, and the gas outlet of the decomposing tower II is connected with the gas inlet H2And S, collecting the storage tank.
4. The device for removing acid gas in natural gas by combining the hydrate method and the membrane separation method as claimed in claim 1, wherein: the gas preheater is a plate preheater.
5. The device for removing acid gas in natural gas by combining the hydrate method and the membrane separation method as claimed in claim 2, wherein: the decomposing tower I is a plate rectifying tower.
6. The device for removing acid gas in natural gas by combining the hydrate method and the membrane separation method as claimed in claim 3, wherein: the decomposing tower II is a plate-type rectifying tower.
7. A method for removing acid gas in natural gas by combining a hydrate method and a membrane separation method is characterized in that: the device for removing acid gas in natural gas based on the integration of the hydrate method and the membrane separation method according to any one of claims 1 to 6 comprises the following steps:
step 1: inputting H into the mixed gas separator II through a liquid supplementing port of the mixed gas separator II2The S absorption liquid inputs CO into the mixed gas separator I through a liquid supplementing port of the mixed gas separator I2An absorption liquid; CO 22The absorption liquid is a uniform mixed liquid of an accelerator, tetrabutylammonium bromide aqueous solution and diesel oil-cyclopentane mixed emulsion; the accelerant contains sodium dodecyl sulfate and sodium dodecyl benzene sulfonate; h2The S absorption liquid is a uniform mixed liquid of N-methyldiethanolamine solution and an accelerant, and the accelerant contains 0.05 mass percent of sodium dodecyl sulfate and 0.05 mass percent of sodium dodecyl benzene sulfonate.
Step 2: starting a stirring device in a mixed gas separator II, removing solid impurities from natural gas by a raw material gas separator 1, then feeding the natural gas into a buffer tank, stabilizing the flow of the natural gas by the buffer tank, then feeding the natural gas into a gas preheater, raising the temperature of the gas to 38-40 ℃ by the gas preheater and removing water vapor, then uniformly and stably feeding H in a bubbling manner through a gas inlet nozzle of the mixed gas separator II after the natural gas is pressurized by a booster pump2S absorption liquid, wherein part of H2S gas is H2S absorption liquid absorbs and reacts to generate H2S hydrate, H not absorbed in time2S gas is intercepted in the separation cavity by the separation membrane II and is carried out by H2S, continuously absorbing by using absorption liquid;
and step 3: starting a stirring device in the mixed gas separator I, and enabling gas penetrating through the separation membrane II to pass through H arranged at an air outlet of the mixed gas separator II2S concentration detector detecting H2S concentration if notWhen the standard is reached, the process is carried out by H2The S return air pipe is sent back to the mixed gas separator II for separation again to remove H2S, circulating until the concentration meets the requirement, entering a compressor after the concentration meets the standard, compressing by the compressor, and introducing CO in a bubbling manner through an air inlet nozzle of a mixed gas separator I2Absorption liquid in which part of CO2Gas CO2Absorbing by the absorption liquid and reacting to generate CO2Hydrates, CO not absorbed in time2The gas is intercepted in the separation cavity by the separation membrane I and is subjected to CO2Continuously absorbing by the absorption liquid; the gas permeating the separation membrane I passes through CO arranged at the gas outlet of the mixed gas separator I2Detecting by a concentration detector, and detecting by CO if the concentration does not reach the standard2The return air pipe is sent back to the mixed gas separator I for separating again to remove CO2Circularly reciprocating until the concentration reaches the requirement, dehydrating by a dehydrator, and feeding into CH after the concentration reaches the standard4And collecting and storing the water in the tank.
8. The method for removing acid gas in natural gas by integrating the hydrate method and the membrane separation method according to claim 7, wherein the method comprises the following steps: in the accelerant, the mass fraction of the sodium dodecyl sulfate is 0.05 percent, and the mass fraction of the sodium dodecyl benzene sulfonate is 0.05 percent.
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