CN112159678A - Hydrogenation reaction post-treatment process and device based on enhanced washing and separation - Google Patents
Hydrogenation reaction post-treatment process and device based on enhanced washing and separation Download PDFInfo
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- CN112159678A CN112159678A CN202011055019.8A CN202011055019A CN112159678A CN 112159678 A CN112159678 A CN 112159678A CN 202011055019 A CN202011055019 A CN 202011055019A CN 112159678 A CN112159678 A CN 112159678A
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- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10G—CRACKING HYDROCARBON OILS; PRODUCTION OF LIQUID HYDROCARBON MIXTURES, e.g. BY DESTRUCTIVE HYDROGENATION, OLIGOMERISATION, POLYMERISATION; RECOVERY OF HYDROCARBON OILS FROM OIL-SHALE, OIL-SAND, OR GASES; REFINING MIXTURES MAINLY CONSISTING OF HYDROCARBONS; REFORMING OF NAPHTHA; MINERAL WAXES
- C10G31/00—Refining of hydrocarbon oils, in the absence of hydrogen, by methods not otherwise provided for
- C10G31/06—Refining of hydrocarbon oils, in the absence of hydrogen, by methods not otherwise provided for by heating, cooling, or pressure treatment
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- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
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- B01D53/00—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols
- B01D53/007—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols by irradiation
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/02—Treatment of water, waste water, or sewage by heating
- C02F1/04—Treatment of water, waste water, or sewage by heating by distillation or evaporation
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Abstract
The invention provides a hydrogenation reaction post-treatment process and a device based on enhanced washing and separation, wherein a material subjected to hydrogenation reaction is subjected to gas-liquid separation through a hot high-pressure separator, and a gas-phase material subjected to separation through the hot high-pressure separator is subjected to oil-gas-water three-phase separation, H and H along a high-pressure low-temperature treatment route2Separating and collecting various components such as recovery and the like; the liquid phase material separated by the hot high-pressure separator is led to the hot low-pressure separator for gas-liquid two-phase separation, and the gas phase is injected with water and mixed and then enters the cold low-pressure separator for treatment. The invention strengthens the oil-water-gas three-phase separation performance of the hydrogenation device, reduces the operation energy consumption of the device, improves the hydrogen recovery rate, reduces the system corrosion and further improves the overall economic and technical level of the device.
Description
Technical Field
The invention belongs to the field of energy chemical industry, and particularly relates to a hydrogenation reaction post-treatment process and device based on enhanced washing and separation.
Background
Under the background of continuous and rapid development of social economy in China, the quality and level of daily life of people are continuously improved, and the overall demand of various energy sources and resources is higher and higher. Petroleum resources are one of the most important strategic resources in the world, and can be classified into two types, one is light petroleum and the other is heavy petroleum. Light petroleum is a petroleum resource widely applied to the market at the present stage, and the reduction of the proportion of hydrocarbon in petroleum is realized by adopting targeted measures, which has gradually become a key problem in research of various departments in recent years.
Among them, the hydrogenation technology is one of the very important technical means in the petroleum refining process. The hydrogenation technology is scientifically and reasonably utilized, the yield of light petroleum can be improved, and the whole content of petroleum hydrocarbon can be effectively controlled.
However, with global low-carbon economic revolution and the promulgation and implementation of national safety and environmental protection new rules, the quality standard of refining enterprises is continuously improved, the requirements on safety and environmental protection are increasingly strict, and the indexes of energy conservation and consumption reduction are increasingly prominent. It is difficult to find a clean production process which can meet all the existing requirements, even reduce the production cost on the basis of the clean production process, and improve the economic benefit.
In the processes of petrochemical industry, coal chemical industry and the like, the hydrogenation process is one of the steps of high safety risk and high energy consumption of refining enterprises, and a reaction system is in the presence of hydrogen, high temperature and high pressure. In the hydrogenation production process, along with the pressure reduction and temperature reduction treatment of the materials in the subsequent flow, a large amount of petroleum hydrocarbon and a small amount of NH can be separated out from the liquid phase3HCl and H2S, and the like, and therefore, relates to three-phase separation of oil, gas and water. The existing hydrogenation production technology is not enough to meet the requirement on the efficiency of three-phase separation under the conditions that the country advocates energy conservation and emission reduction vigorously and is safe and environment-friendly, and droplets which are not separated in a gas phase can cause the overall efficiency of a system to be reduced, so that the hydrogen recovery utilization rate is reduced; meanwhile, the low-efficiency oil-water separation can generate a large amount of domestic sewage, and the pressure of water treatment is greatly increased.
In order to reach the national production standard, the current method is to increase the size of equipment and improve the three-phase separation time, so that the efficiency is increased and the current situation is improved. But this will result in a less compact overall process system and a doubling of energy consumption and production costs. Although the method reaches the national standard, the economic benefit is greatly reduced, even the loss of enterprises is reduced.
Therefore, a novel production process technology is urgently needed to overcome the problems, so that three-phase separation of oil, gas and water is enhanced, the hydrogen recycling rate is increased, the production cost is reduced, and the economic benefit of the whole process flow is improved.
Disclosure of Invention
Aiming at the defects in the prior art, the invention provides a hydrogenation reaction post-treatment process and device based on enhanced washing and separation.
In order to solve the above technical problems, a first technical solution provided by the present invention is as follows: a hydrogenation reaction post-treatment process based on enhanced washing and separation comprises the following steps:
step 1: carrying out gas-liquid separation on the material subjected to the hydrogenation reaction by a hot high-pressure separator;
step 2: the gas-phase material separated in the step 1 is processed in a high-pressure low-temperature processing route, which comprises the following steps:
step 2.1: injecting water into the gas-phase material separated in the step 1 for mixing, cooling, and introducing into a cold high-pressure separator for oil-gas-water three-phase separation;
step 2.2: the gas phase separated by the cold high-pressure separator is led to a desulfurizing tower for desulfurization treatment, and the top of the desulfurizing tower is recovered with H2The sulfur-containing liquid at the bottom of the desulfurization tower is removed from a first rich liquid centrifugal flash evaporation dealkylation degreaser, the top of the first rich liquid centrifugal flash evaporation dealkylation degreaser obtains a gas phase containing sulfur-containing gas and gaseous light hydrocarbon, the middle part of the gas phase obtains oil, and the bottom of the gas phase obtains rich liquid;
further, in step 2.2, desulfurized H2Can be returned to a recycle hydrogen compressor to participate in hydrogenation reaction for reuse, the first pregnant solution centrifugal flash evaporation dealkylation degreaser obtains sulfur-containing gas and removes the gas desulfurization device, the oil is removed to an oil storage tank, and the pregnant solution is removed from the pregnant solution and regeneratedThe device is recycled and respectively collected and treated in a centralized way.
Step 2.3: injecting water into the oil phase separated by the cold high-pressure separator, mixing, and then feeding the oil phase into the cold low-pressure separator for three-phase separation of oil, gas and water to respectively obtain gaseous petroleum hydrocarbon, oil and sewage; and the separated sewage enters a second pregnant solution centrifugal flash evaporation dealkylation oil remover for treatment.
Step 2.4: collecting the water phase separated by the cold high-pressure separator and the sewage subjected to three-phase separation by the cold low-pressure separator in the step 2.3, feeding the collected water into a second pregnant solution centrifugal flash evaporation dealkylation degreaser, obtaining gas phase at the top of the second pregnant solution centrifugal flash evaporation dealkylation degreaser, wherein the gas phase comprises sulfur-containing gas, partial gaseous light hydrocarbon and other gaseous substances, obtaining oil at the middle part, and obtaining acidic sewage and wastewater at the bottom part;
further, in step 2.4, the gas phase obtained by the second rich solution centrifugal flash evaporation dealkylation degreaser is sent to a gas desulfurization device, oil is sent to an oil storage tank, acidic sewage and wastewater are subjected to acidic water stripping treatment, and the acidic sewage and wastewater are respectively collected and treated in a centralized manner.
And step 3: and (3) introducing the liquid-phase material separated in the step (1) to a hot low-pressure separator for gas-liquid two-phase separation, and introducing the gas phase after water injection and mixing into a cold low-pressure separator for treatment.
The invention is further set in that in the step 1, the initial pressure of the material is 11-13MPa, and the initial temperature is 250-260 ℃.
The invention is further configured that, in step 2.1, the specific process of the cooling treatment comprises: the temperature is reduced to 160-164 ℃ by the high-pressure heat exchanger, water is injected again by the water injection distributor, and then the temperature is reduced to 50 ℃ by the high-pressure air cooler and then the cooled high-pressure separator is introduced.
The invention is further arranged that in step 2.2, the gas phase separated by the cold high-pressure separator is firstly separated again into gas phase and liquid phase by the gas-liquid separation device in front of the desulfurizing tower, the liquid oil drops are sent to the oil storage tank and contain H2And leading the sulfur-containing gas of the S to a desulfurizing tower for desulfurization treatment.
The invention is further configured such that, in step 2.2, H is recovered2The pressure of (A) is 0.7-0.8 MPa.
The invention is further arranged that in step 2.3 the pressure of the obtained gaseous petroleum hydrocarbon is 2.8-3 MPa.
The second technical scheme provided by the invention is as follows: a device suitable for the hydrogenation reaction post-treatment process based on the enhanced washing and separation comprises a hot high-pressure separator, a water injection distributor, a high-pressure heat exchanger, a cold high-pressure separator, a hot low-pressure separator, a desulfurizing tower, a cold low-pressure separator, a first rich liquid centrifugal flash evaporation dealkylation degreaser and a second rich liquid centrifugal flash evaporation dealkylation degreaser;
the top of the hot high-pressure separator is provided with an air outlet connected with the high-pressure heat exchanger, a water injection distributor is arranged between the air outlet of the hot high-pressure separator and the high-pressure heat exchanger, and the high-pressure heat exchanger is connected with the cold high-pressure separator;
the top of the cold high-pressure separator is provided with an air outlet connected with the lower part of the desulfurizing tower, and the bottom of the desulfurizing tower is provided with a liquid outlet connected with the first pregnant solution centrifugal flash evaporation hydrocarbon-removing oil remover;
an oil phase outlet is arranged in the middle of the cold high-pressure separator and connected with an oil phase inlet arranged at the top of the cold low-pressure separator, and a water injection distributor is arranged between the oil phase inlet of the cold low-pressure separator and the cold high-pressure separator; the top of the cold low-pressure separator is provided with a gaseous petroleum hydrocarbon outlet, a partition plate is arranged in the cold low-pressure separator, and the bottoms of the cold low-pressure separators on the two sides of the partition plate are respectively provided with an oil outlet and a sewage outlet; the cold low-pressure separator is provided with a gas inlet, a fin separator and an oil-water rapid separation module are arranged inside the cold low-pressure separator, an oil phase inlet of the cold low-pressure separator is communicated with the fin separator and is positioned on one side of the oil-water rapid separation module, and the gas inlet of the cold low-pressure separator, the partition plate, an oil outlet of the cold low-pressure separator and a sewage outlet of the cold low-pressure separator are positioned on the other side of the oil-water rapid separation module;
the bottom water phase outlet of the cold high-pressure separator is connected with the second pregnant solution centrifugal flash evaporation hydrocarbon-removing oil remover;
the bottom of the hot high-pressure separator is provided with a liquid outlet which is connected with the hot low-pressure separator; the top of the hot low-pressure separator is provided with a gas outlet communicated with a gas inlet of the cold low-pressure separator, and a water injection distributor is arranged between the gas outlet of the hot low-pressure separator and the gas inlet of the cold low-pressure separator; an oil outlet is arranged at the bottom of the hot low-pressure separator.
The invention is further arranged that at least one high-pressure air cooler is arranged between the high-pressure heat exchanger and the cold high-pressure separator, and if a plurality of high-pressure air coolers are used at the same time, all the high-pressure air coolers are arranged in parallel in a pipeline; and a water injection distributor is arranged between the high-pressure heat exchanger and the high-pressure air cooler.
The invention is further provided that a venturi scrubber is connected to the oil phase inlet of the cold low pressure separator, and the venturi scrubber is communicated with the fin separator.
The invention is further provided that the top of the desulfurizing tower is provided with an MDEA inlet and a gas outlet.
The invention is further provided that the top of the first rich liquid centrifugal flash evaporation dealkylation degreaser is provided with a gas outlet for discharging gas phase, the middle part is provided with an oil phase outlet, and the bottom is provided with a rich liquid outlet; the top of the second rich liquid centrifugal flash evaporation dealkylation degreaser is provided with a gas outlet, the middle part is provided with an oil phase outlet, and the bottom is provided with an acidic sewage and wastewater outlet. As further treatment, the sulfur-containing gas can be sent to a gas desulfurization device for centralized collection and treatment, the oil is sent to an oil storage tank, the rich solution is sent to a rich solution regeneration device for reuse, and the acidic wastewater is stripped by removing acidic water.
The invention is further arranged in such a way that a gas-liquid separation device in front of the desulfurizing tower is connected between the gas outlet of the cold high-pressure separator and the desulfurizing tower, the top of the gas-liquid separation device in front of the desulfurizing tower is provided with a gas outlet connected with the lower part of the desulfurizing tower, the bottom of the gas-liquid separation device in front of the desulfurizing tower is provided with an oil phase outlet, and oil can be collected in an oil storage tank.
The invention is further configured such that the hot high pressure separator comprises a tank body, a gas-liquid inertial separation module fixed in the tank body, and a plurality of centrifugal flash modules fixed on the bottom surface of the gas-liquid inertial separation module.
The cold high-pressure separator comprises a tank body, a gas-liquid condensation separation module fixed in the upper tank body, a gas-liquid inertia separation module fixed in the middle tank body, a plurality of centrifugal flash modules fixed on the bottom surface of the gas-liquid inertia separation module, and an oil-water condensation separation module fixed in the lower tank body;
the hot low-pressure separator is the same as the hot high-pressure separator in structure;
the front gas-liquid separation device of the desulfurizing tower comprises a tank body and a gas-liquid condensation separation module fixed on the tank body;
the first rich liquid centrifugal flash evaporation dealkylation oil remover and the second rich liquid centrifugal flash evaporation dealkylation oil remover are identical in structure and respectively comprise a tank body, a distributor fixed in the tank body, a liquid collecting disc positioned below the distributor, a centrifugal flash evaporation module positioned below the liquid collecting disc and an inclined plate positioned below the centrifugal flash evaporation module, wherein a through hole is formed in the middle of the inclined plate, and an oil-water rapid separation module is fixed in the through hole.
Further, the gas-liquid condensation separation module is a fiber module which is coated and fixed by a wire mesh, the gas-liquid condensation separation module comprises a disc-shaped top structure and a bottom structure connected below the top structure, the top structure is circular or rectangular, and the bottom structure is a conical cylinder or symmetrical petal body.
The invention further provides that the gaseous petroleum hydrocarbon outlet is connected with a supersonic speed temperature-changing type based gas purifier, and the supersonic speed temperature-changing type based gas purifier comprises a supersonic speed separator and a condensate separator;
the supersonic speed separator comprises a gradually-reduced acceleration cavity, a vortex-making cavity, a supersonic speed separation cavity and a gradually-expanded boosting cavity which are sequentially connected according to a treatment sequence, wherein the vortex-making cavity comprises a cavity body and a plurality of spiral blades which are uniformly fixed on the cavity body, the inner diameters of the vortex-making cavity and the supersonic speed separation cavity are the same, a gas phase inlet is formed in the gradually-reduced acceleration cavity, a high-temperature purified gas outlet is formed in the gradually-expanded boosting cavity, and a condensate outlet is formed in the bottom of the supersonic speed separation cavity;
the condensate separator includes a jar body and fixes the internal gas-liquid condensation separation module of jar, gas-liquid condensation separation module below open the condensate import on the jar body, condensate import intercommunication the condensate export, the top of the jar body is equipped with low temperature and purifies the gas outlet, the bottom of the jar body is equipped with purifies the condensate export.
Further, the spiral angle of the spiral blade is 10-35 degrees; the reducing angle of the reducing accelerating cavity is 20-30 degrees; the divergent angle of the divergent pressure rising cavity is 5-25 degrees.
Further, the tapered acceleration chamber: the vortex-making cavity comprises: the supersonic separation chamber: the length ratio of the gradually-expanding boosting cavity is 1.5-2.5: 1: 1.5-2.5: 4-6.
In conclusion, the invention has the following beneficial effects:
(1) the process and the device can strengthen the oil-gas-water three-phase separation performance of hydrogenation reaction, improve the separation efficiency by 95-99 percent compared with the traditional process by 20-40 percent, reduce the operation energy consumption of the device and improve the recovery rate of hydrogen. The separation efficiency calculation method comprises the following steps: the isolated pure (weight) is divided by the total amount (weight) before isolation times 100%.
(2) The invention adopts the technologies of centrifugal flash evaporation gas-liquid separation, self-adaptive degassing and dealkylation separation and the like, has high treatment efficiency and short material retention time, so the size of an internal part is small, the whole size of the equipment is small, the volume of the whole equipment can be reduced by 30-50 percent by taking conventional or traditional equipment as reference, the whole process system is more compact, the occupation of space resources is reduced, and meanwhile, the energy consumption is reduced by 25-45 percent, thereby reducing the production cost and improving the economic benefit;
(3) the invention can effectively treat NH carried in the gas by arranging a plurality of water injection distributors to inject water into the separated gas phase3HCl and H2S, etc., to prevent NH from being precipitated due to instantaneous temperature decrease during heat exchange3 +And Cl-Iso-corrosion heat exchangers; simultaneously, a water injection distributor injects oil to the outlet of the cold high-pressure separatorThe water is treated by a Venturi scrubber, and most of salt in the oil can be effectively removed. Through the desalination treatment to ammonia and chlorine etc., can wholly reduce the corruption of system, promote life, specifically, can increase high-pressure heat exchanger and high-pressure air cooler 35% -50%'s life, and then promote whole economic technology level of whole process system.
(4) The hydrogen recovery efficiency of the invention can reach more than 99 percent, the hydrogen recovery rate is high, the resource utilization is realized, and the economic benefit is improved.
(5) The invention is provided with the cold low-pressure separator, the cold high-pressure separator, the first pregnant solution centrifugal flash evaporation dealkylation degreaser and the second pregnant solution centrifugal flash evaporation dealkylation degreaser, the oil recovery rate can reach 97-99%, and the oil recovery rate can be increased by 30-40% compared with the traditional or conventional process;
(6) the invention is provided with the gas purifier based on the supersonic speed temperature change, and the gas purifier based on the supersonic speed temperature change comprises a supersonic speed separator and a condensate separator, so that the separation of light hydrocarbon and heavy hydrocarbon is realized, and the thorough separation of materials is realized.
Drawings
FIG. 1 is a schematic diagram of the structure of a hydrogenation reaction post-treatment device based on enhanced washing and separation according to the present invention;
FIG. 2 is a schematic structural diagram of a gas-liquid condensation separation module (the top structure is circular, the bottom structure is a conical cylinder, and contour lines on two sides of the conical cylinder are straight lines);
FIG. 3 is a schematic structural diagram of a gas-liquid condensation separation module (the top structure is circular, the bottom structure is a conical cylinder, and the contour lines on two sides of the conical cylinder are arc-shaped);
fig. 4 is a schematic structural diagram of the gas-liquid condensation separation module (the top structure is rectangular, the bottom structure is a symmetrical petal body, and contour lines on two sides of the petal body are straight lines);
fig. 5 is a schematic structural diagram of the gas-liquid condensation separation module (the top structure is rectangular, the bottom structure is a symmetrical petal body, and the contour lines on the two sides of the petal body are arc-shaped);
FIG. 6 is a schematic view showing a connection structure of a distributor and a drip pan;
fig. 7 is a schematic structural diagram of a gas purifier based on supersonic variable temperature.
Wherein, 1: a hot high pressure separator; 2. 9, 28: a gas-liquid inertia separation module; 3. 10, 29, 33: a centrifugal flash module; 4. 6, 20, 31: a water injection distributor; 5: a high pressure heat exchanger; 7: a high-pressure air cooler; 8: a cold high pressure separator; 11: an oil-water condensation separation module; 12. 14, 35: a gas-liquid condensation separation module; 13: a gas-liquid separation device in front of the desulfurizing tower; 15: a desulfurizing tower; 16: a first rich liquid centrifugal flash evaporation dealkylation degreaser; 25: a second rich liquid centrifugal flash evaporation hydrocarbon-removing oil remover; 18. 24, 27: an oil-water rapid separation module; 21: a cold low pressure separator; 22: a venturi scrubber; 23: a fin separator; 30: a hot low pressure separator; 31: a distributor; 32: a liquid collecting tray; 33. a top structure; 34. a bottom structure; 36. a gas phase inlet; 37. a tapered acceleration chamber; 38. a vortex making cavity; 39. a supersonic separation chamber; 40. gradually expanding the pressure rising cavity; 41. a high temperature purified gas outlet; 42. a condensate outlet; 43. a condensate separator; 44. a helical blade;
100: returning to the recycle hydrogen compressor; 200: a de-gas desulfurization unit; 300: removing the oil storage tank; 400: a de-pregnant solution regeneration device; 500: gaseous petroleum hydrocarbons; 600: a dephlegmation system; 700: acid water removal and steam stripping; f1, mixed gas; f2, condensation; f3, high-temperature purified gas; f4, low-temperature purified gas; f5, purified gas; f6, purifying the condensate.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Example 1
A hydrogenation reaction post-treatment process based on enhanced washing and separation comprises the following steps:
step 1: the material after hydrogenation reaction is subjected to gas-liquid separation by a hot high-pressure separator 1, preferably, the initial pressure of the material is 11-13MPa, and the initial temperature is 250-260 ℃.
Step 2: the separated product in the step 1 mainly comprises HCl and NH3Comprising H2The high-pressure low-temperature treatment route of the gas-phase materials of S containing gases such as sulfur gas and the like comprises the following steps:
step 2.1: and (3) injecting water into the gas-phase material separated in the step (1) for mixing, cooling, and introducing into a cold high-pressure separator (8) for oil-gas-water three-phase separation.
Step 2.2: the gas phase separated by the cold high-pressure separator 8 is led to a desulfurizing tower 15 for desulfurization treatment, and H contained in the gas phase is removed under the action of MDEA2S and other sulfur-containing gases are removed, and H is recovered from the top of the desulfurizing tower 152Recovery of H2The pressure of the desulfurization tower is about 0.7-0.8Mpa, and the recovered H is desulfurized2The sulfur-containing liquid at the bottom of the desulfurizing tower 15 is sent to a first pregnant solution centrifugal flash evaporation dealkylation degreaser 16, the top of the first pregnant solution centrifugal flash evaporation dealkylation degreaser 16 obtains a gas phase, the gas phase comprises sulfur-containing gas, gaseous light hydrocarbon and the like, wherein the sulfur-containing gas can be sent to a gas desulfurizing device 200, the oil obtained at the middle part can be sent to an oil storage tank 300, the pregnant solution obtained at the bottom can be sent to a pregnant solution regenerating device 400 for recycling, and the process flow is returned to again after the treatment.
Step 2.3: the oil phase separated by the cold high-pressure separator 8 is injected with water and mixed, and then enters the cold low-pressure separator 21 to carry out three-phase separation of oil, gas and water, so as to respectively obtain gaseous petroleum hydrocarbon 500, oil and sewage, wherein the pressure of the obtained gaseous petroleum hydrocarbon is about 2.8-3 MPa. Wherein, the separated sewage enters a second pregnant solution centrifugal flash evaporation dealkylation degreaser 25 for treatment, and the separated oil enters a fractionation system 600.
Step 2.4: and (3) collecting the water phase separated by the cold high-pressure separator 8 and the sewage subjected to three-phase separation by the cold low-pressure separator 21 in the step 2.3, feeding the collected water phase into a second rich solution centrifugal flash evaporation dealkylation degreaser 25, wherein the gas phase obtained at the top of the second rich solution centrifugal flash evaporation dealkylation degreaser 25 can be removed to the gas desulfurization device 200, the oil obtained at the middle part can be removed to the oil storage tank 300, and the acidic sewage and wastewater obtained at the bottom part can be stripped by removing acidic water 700.
And step 3: the liquid phase material separated in the step 1 is led to a hot low pressure separator 30, the pressure is reduced, and a large amount of gas including petroleum hydrocarbon gas and NH can be emitted from the original liquid material3HCl and H2S and the like. The gas phase is treated in a cold low pressure separator 21 after being mixed by water injection. The bottom of the hot low pressure separator 30 is provided with an oil outlet and the oil goes to a fractionation system 600.
Further, in step 2.2, the gas phase separated by the cold high-pressure separator 8 passes through the pre-desulfurizing-tower gas-liquid separator 13 to be separated again into gas and liquid oil droplets containing H and flowing into the oil storage tank 3002The sulfur-containing gas of S is passed to a desulfurizing tower 15 to be subjected to desulfurization treatment.
Further, in step 2.1, the specific process of the cooling treatment includes: after the temperature is reduced to 160-164 ℃ by the high-pressure heat exchanger 5, water is injected again by the water injection distributor 6, and then the temperature is reduced to 50 ℃ by the high-pressure air cooler 7 and is introduced into the cold high-pressure separator 8.
Example 2
An apparatus suitable for the hydrogenation reaction post-treatment process based on the enhanced washing and separation is shown in fig. 1 and comprises a hot high-pressure separator 1, a water injection distributor, a high-pressure heat exchanger 5, a cold high-pressure separator 8, a hot low-pressure separator 30, a desulfurizing tower 15, a cold low-pressure separator 21, a first rich liquid centrifugal flash evaporation dealkylation degreaser 16 and a second rich liquid centrifugal flash evaporation dealkylation degreaser 25.
The top of the hot high-pressure separator 1 is provided with an air outlet connected with a high-pressure heat exchanger 5, a water injection distributor 4 is arranged between the air outlet of the hot high-pressure separator 1 and the high-pressure heat exchanger 5, and the high-pressure heat exchanger 5 is connected with a cold high-pressure separator 8.
The top of the cold high-pressure separator 8 is provided with an air outlet connected with the lower part of the desulfurizing tower 15, and the bottom of the desulfurizing tower 15 is provided with a liquid outlet connected with a first rich liquid centrifugal flash evaporation hydrocarbon-removing oil remover 16. The top of the desulfurizing tower 15 is provided with an MDEA inlet and a gas outlet, and the gas outlet is mainly used for H2And (4) discharging and recovering.
An oil phase outlet is arranged in the middle of the cold high-pressure separator 8 and is connected with an oil phase inlet arranged at the top of the cold low-pressure separator 21, and a water injection distributor 20 is arranged between the oil phase inlet of the cold low-pressure separator 21 and the cold high-pressure separator 8. The top of the cold low-pressure separator 21 is provided with a gaseous petroleum hydrocarbon 500 outlet, a partition plate is arranged in the cold low-pressure separator 21, and the bottoms of the cold low-pressure separators 21 on the two sides of the partition plate are respectively provided with an oil outlet and a sewage outlet. It has gas inlet to open on cold low pressure separator 21, and cold low pressure separator 21's inside is equipped with fin separator 23 and profit quick separation module 24, and cold low pressure separator 21's oil phase import intercommunication fin separator 23 just is located one side of profit quick separation module 24, and cold low pressure separator 21's gas inlet, baffle, cold low pressure separator 21's oil export and cold low pressure separator 21's sewage export are located the opposite side of profit quick separation module 24.
The bottom water phase outlet of the cold high-pressure separator 8 is connected with a second pregnant solution centrifugal flash evaporation hydrocarbon-removing oil remover 25.
The bottom of the hot high-pressure separator 1 is provided with a liquid outlet connected with a hot low-pressure separator 30. The top of the hot low-pressure separator 30 is provided with a gas outlet communicated with the gas inlet of the cold low-pressure separator 21, and a water injection distributor 31 is arranged between the gas outlet of the hot low-pressure separator 30 and the gas inlet of the cold low-pressure separator 21. The bottom of the hot low pressure separator 30 is provided with an oil outlet.
At least one high-pressure air cooler 7 is arranged between the high-pressure heat exchanger 5 and the cold high-pressure separator 8, and if a plurality of high-pressure air coolers 7 are used at the same time, all the high-pressure air coolers 7 are installed in parallel in the pipeline. A water injection distributor 6 is arranged between the high-pressure heat exchanger 5 and the high-pressure air cooler 7.
The oil phase inlet of the cold low pressure separator 21 is connected with a venturi scrubber 22, and the venturi scrubber 22 is communicated with a fin separator 23. The oil phase separated by the cold high-pressure separator 8 is injected with water and mixed with the water injection distributor 20, then flows through the venturi scrubber 22, and is cavitated by the venturi scrubber 22, so that the salt contained in the oil can be effectively removed, and the quality of the oil is improved. And then the oil, gas and water are separated in a cold low pressure separator 21.
The top of the first rich liquid centrifugal flash evaporation dealkylation degreaser 16 is provided with a gas outlet for discharging sulfur-containing gas and can be used for discharging the sulfur-containing gas to the gas desulfurization device 200, the middle part is provided with an oil phase outlet for discharging the oil storage tank 300, and the bottom is provided with a rich liquid outlet for discharging rich liquid and can be used for discharging the rich liquid to the rich liquid regeneration device 400 for recycling. The top of the second rich liquid centrifugal flash evaporation dealkylation degreaser 25 is provided with a gas outlet for discharging sulfur-containing gas and removing the sulfur-containing gas to the gas desulfurization device 200, the middle part is provided with an oil phase outlet for removing the oil storage tank 300, the bottom is provided with a rich liquid outlet for discharging rich liquid and removing the rich liquid regeneration device 400 for recycling, and the bottom is stripped 700 by removing acid water from the acid sewage and wastewater.
Further, a gas-liquid separation device 13 in front of the desulfurizing tower is connected between a gas outlet of the cold high-pressure separator 8 and the desulfurizing tower 15, the top of the gas-liquid separation device 13 in front of the desulfurizing tower is provided with a gas outlet connected with the lower part of the desulfurizing tower 15, and the bottom of the gas-liquid separation device 13 in front of the desulfurizing tower is provided with an oil phase outlet which can be used for removing the oil storage tank 300.
Specifically, the hot high-pressure separator 1 comprises a tank body, a gas-liquid inertia separation module 2 fixed in the tank body, and a plurality of centrifugal flash modules 3 fixed on the bottom surface of the gas-liquid inertia separation module 2.
The cold high-pressure separator 8 comprises a tank body, a gas-liquid condensation separation module 12 fixed in the upper tank body, a gas-liquid inertia separation module 9 fixed in the middle tank body, a plurality of centrifugal flash modules 10 fixed on the bottom surface of the gas-liquid inertia separation module 9, and an oil-water condensation separation module 11 fixed in the lower tank body.
The hot low pressure separator 30 is of the same construction as the hot high pressure separator 1.
The gas-liquid separation device 13 in front of the desulfurizing tower comprises a tank body and a gas-liquid condensation separation module 14 fixed on the tank body.
Referring to fig. 6, the first rich liquid centrifugal flash dealkylation degreaser 16 and the second rich liquid centrifugal flash dealkylation degreaser 25 have the same structure, and both include a tank body, a distributor 31 fixed in the tank body, a liquid collecting tray 32 located below the distributor 31, a centrifugal flash module 33 located below the liquid collecting tray 32, and an inclined plate located below the centrifugal flash module, wherein a through hole is formed in the middle of the inclined plate, and oil-water rapid separation modules (18, 27) are fixed in the through hole.
Example 3
On the basis of the embodiment 2, the invention is further provided that the gaseous petroleum hydrocarbon outlet is connected with a supersonic variable temperature based gas purifier, and the supersonic variable temperature based gas purifier comprises a supersonic separator and a condensate separator, which can be seen in fig. 7.
The supersonic separator comprises a gradually-reduced acceleration cavity, a vortex-making cavity, a supersonic separation cavity and a gradually-expanded boosting cavity which are sequentially connected according to a treatment sequence, wherein the vortex-making cavity comprises a cavity body and a plurality of spiral blades which are uniformly fixed on the cavity body, the inner diameters of the vortex-making cavity and the supersonic separation cavity are the same, a gas phase inlet is formed in the gradually-reduced acceleration cavity, a high-temperature purified gas outlet (light hydrocarbon) is formed in the gradually-expanded boosting cavity, and a condensate outlet is formed in the bottom of the supersonic separation cavity;
the condensate separator includes the jar body and fixes the gas-liquid condensation separation module in the jar body, it has the condensate import to open on the jar body of gas-liquid condensation separation module below, condensate import intercommunication condensate export, the top of the jar body is equipped with low temperature and purifies gas outlet (light hydrocarbon), high temperature purifies gas outlet and low temperature and purifies the gas outlet and is communicateing the purification gas outlet jointly through the pipeline, realize that the light hydrocarbon collects, the bottom of the jar body is equipped with and purifies condensate outlet (heavy hydrocarbon), and then realize the separation of light hydrocarbon and heavy hydrocarbon.
Example 4
More specifically, the gas-liquid inertial separation module (2, 9, 28) used in the present invention may be a wire mesh mist catcher, also called a wire mesh mist eliminator, a wire mesh demister, for gas-liquid separation, and for reducing the humidity of various kinds of steam in the gas. Various steam mist in the silk screen defroster separation gas, the effect principle is based on inertial collision, the random motion of steam molecule, and the mist that shows to the silk screen through a large amount of random motion adhesion constantly assembles, just forms big liquid drop to silk screen structure bottom to the cutout drips when can't overcome the action of gravity, realizes gas-liquid separation. The gas-liquid inertial separation module (2, 9, 28) may be the inertial gas-liquid separator disclosed in application No. 201380042315.6, and the gas-liquid inertial separation module (2, 9, 28) may be another existing type of gas-liquid separation module.
The gas-liquid condensation separation modules (12, 14) are fiber modules which are coated and fixed by silk screens, the weaving mode of the fiber modules can be X-type or omega-type, and the hydrophilic and hydrophobic fiber modules are formed by weaving materials such as Teflon, PTFE, PP, or 316L metal wires with increased strength singly or in a mixed way. The gas-liquid condensation separation modules (12, 14) comprise a disc-shaped top structure and a bottom structure connected below the top structure, wherein the top structure is circular or rectangular, and the bottom structure is in a conical barrel shape or a symmetrical petal shape. The longitudinal section of the gas-liquid condensation separation module (12, 14) is preferably pi-shaped, and according to the shape of the fixed tank body and the amount of materials to be treated, the top structure can be round or rectangular, the bottom structure can be horn-shaped (see fig. 2 and 3) expanding downwards and outwards, and the gas-liquid condensation separation module can also be a discontinuous structure, such as a left lobe and a right lobe which are separately arranged (see fig. 4 and 5). The inclination angles (included angles with the vertical direction) of the gas-liquid condensation separation modules (12 and 14) can be adjusted within the range of 15-60 degrees according to working conditions, so that the filtering area is increased by 15-25%, the installation space is saved, secondary gas-liquid entrainment caused by overlarge gas velocity can be avoided, and the gas-liquid two-phase separation efficiency is improved by 45-75% (relative to the vertical gas-liquid condensation separation module).
The oil-water condensation separation module 11 is a fiber module which is coated and fixed by a silk screen, and the fiber module can be made of different materials according to actual conditions, such as hydrophilic and hydrophobic fiber modules which are formed by weaving teflon, PTFE, PP, 316L and other materials singly or in a mixed manner; the shape structure can be round, square, braided structure, metal corrugated structure, etc. according to actual needs. As shown in fig. 1, a fixing plate may be fixed in the lower portion of the cold high-pressure separator 8, and two oil-water condensation separation modules may be fixed on the fixing plate for oil-water separation.
The centrifugal flash module (3, 10, 29, 33) may be a jet flash separator in 201310239487.4. The centrifugal effect is realized by arranging a rotational flow structure at the inlet section of the jet flash separator, and the rotational flow structure can be a guide groove or a helical blade and the like.
Similarly, the oil-water rapid separation modules (18, 24, 27) are fiber modules fixed by wire mesh coating, and the fiber modules can be made of different materials according to actual conditions, such as hydrophilic-hydrophobic fiber modules formed by weaving teflon, PTFE, PP, 316L and other materials singly or in a mixed manner; the shape can be changed according to actual requirements.
The above description is only for the purpose of illustrating the preferred embodiments of the present invention and is not to be construed as limiting the invention, and any modifications, equivalents, improvements and the like that fall within the spirit and principle of the present invention are intended to be included therein.
Claims (12)
1. A hydrogenation reaction post-treatment process based on enhanced washing and separation is characterized by comprising the following steps:
step 1: carrying out gas-liquid separation on the material subjected to the hydrogenation reaction by a hot high-pressure separator;
step 2: the gas-phase material separated in the step 1 is processed in a high-pressure low-temperature processing route, which comprises the following steps:
step 2.1: injecting water into the gas-phase material separated in the step 1 for mixing, cooling, and introducing into a cold high-pressure separator for oil-gas-water three-phase separation;
step 2.2: the gas phase separated by the cold high-pressure separator is led to a desulfurizing tower for desulfurization treatment, and the top of the desulfurizing tower is recovered with H2Removing the sulfur-containing liquid at the bottom of the desulfurization tower from a first pregnant solution centrifugal flash evaporation dealkylation degreaser, obtaining a gas phase at the top of the first pregnant solution centrifugal flash evaporation dealkylation degreaser, obtaining oil in the middle of the first pregnant solution centrifugal flash evaporation dealkylation degreaser, and obtaining a pregnant solution at the bottom of the first pregnant solution centrifugal flash evaporation dealkylation degreaser;
step 2.3: injecting water into the oil phase separated by the cold high-pressure separator, mixing, and then feeding the oil phase into the cold low-pressure separator for three-phase separation of oil, gas and water to respectively obtain gaseous petroleum hydrocarbon, oil and sewage; and the separated sewage enters a second pregnant solution centrifugal flash evaporation dealkylation oil remover for treatment.
Step 2.4: collecting the water phase separated by the cold high-pressure separator and the sewage subjected to three-phase separation by the cold low-pressure separator in the step 2.3, feeding the collected water into a second pregnant solution centrifugal flash evaporation dealkylation degreaser, obtaining gas phase at the top of the second pregnant solution centrifugal flash evaporation dealkylation degreaser, obtaining oil at the middle part and obtaining acidic sewage and wastewater at the bottom;
and step 3: and (3) introducing the liquid-phase material separated in the step (1) to a hot low-pressure separator for gas-liquid two-phase separation, and introducing the gas phase after water injection and mixing into a cold low-pressure separator for treatment.
2. The hydrogenation reaction post-treatment process based on enhanced washing and separation as claimed in claim 1, wherein the initial pressure of the material in step 1 is 11-13MPa, and the initial temperature is 250-260 ℃.
3. The hydrogenation reaction post-treatment process based on enhanced washing and separation as claimed in claim 1, wherein in step 2.1, the specific process of temperature reduction treatment comprises: the temperature is reduced to 160-164 ℃ by the high-pressure heat exchanger, water is injected again by the water injection distributor, and then the temperature is reduced to 50 ℃ by the high-pressure air cooler and then the cooled high-pressure separator is introduced.
4. The hydrogenation reaction post-treatment process based on enhanced washing and separation as claimed in claim 1, wherein in step 2.2, the gas phase separated by the cold high-pressure separator is passed through a gas-liquid separation device in front of the desulfurizing tower for gas-liquid two-phase separation again, and the liquid oil drops are sent to the oil storage tank and contain H2And leading the sulfur-containing gas of the S to a desulfurizing tower for desulfurization treatment.
5. An apparatus suitable for the hydrogenation reaction post-treatment process based on enhanced washing and separation as claimed in any one of claims 1 to 4, which comprises a hot high-pressure separator, a water injection distributor, a high-pressure heat exchanger, a high-pressure air cooler, a cold high-pressure separator, a hot low-pressure separator, a desulfurizing tower, a cold low-pressure separator, a first rich liquid centrifugal flash dealkylation degreaser and a second rich liquid centrifugal flash dealkylation degreaser;
the top of the hot high-pressure separator is provided with an air outlet connected with the high-pressure heat exchanger, a water injection distributor is arranged between the air outlet of the hot high-pressure separator and the high-pressure heat exchanger, and the high-pressure heat exchanger is connected with the cold high-pressure separator;
the top of the cold high-pressure separator is provided with an air outlet connected with the lower part of the desulfurizing tower, and the bottom of the desulfurizing tower is provided with a liquid outlet connected with the first pregnant solution centrifugal flash evaporation hydrocarbon-removing oil remover;
an oil phase outlet is arranged in the middle of the cold high-pressure separator and connected with an oil phase inlet arranged at the top of the cold low-pressure separator, and a water injection distributor is arranged between the oil phase inlet of the cold low-pressure separator and the cold high-pressure separator; the top of the cold low-pressure separator is provided with a gaseous petroleum hydrocarbon outlet, a partition plate is arranged in the cold low-pressure separator, and the bottoms of the cold low-pressure separators on the two sides of the partition plate are respectively provided with an oil outlet and a sewage outlet; the cold low-pressure separator is provided with a gas inlet, a fin separator and an oil-water rapid separation module are arranged inside the cold low-pressure separator, an oil phase inlet of the cold low-pressure separator is communicated with the fin separator and is positioned on one side of the oil-water rapid separation module, and the gas inlet of the cold low-pressure separator, the partition plate, an oil outlet of the cold low-pressure separator and a sewage outlet of the cold low-pressure separator are positioned on the other side of the oil-water rapid separation module;
the bottom water phase outlet of the cold high-pressure separator is connected with the second pregnant solution centrifugal flash evaporation hydrocarbon-removing oil remover;
the bottom of the hot high-pressure separator is provided with a liquid outlet which is connected with the hot low-pressure separator; the top of the hot low-pressure separator is provided with a gas outlet communicated with a gas inlet of the cold low-pressure separator, and a water injection distributor is arranged between the gas outlet of the hot low-pressure separator and the gas inlet of the cold low-pressure separator; an oil outlet is arranged at the bottom of the hot low-pressure separator.
6. The apparatus of claim 5, wherein at least one high pressure air cooler is provided between the high pressure heat exchanger and the cold high pressure separator, all of which are installed in parallel in a pipeline if a plurality of high pressure air coolers are used simultaneously; and a water injection distributor is arranged between the high-pressure heat exchanger and the high-pressure air cooler.
7. The device of claim 5, wherein a venturi scrubber is connected to the oil phase inlet of the cold low pressure separator, and the venturi scrubber is communicated with the fin separator.
8. The apparatus of claim 5, wherein the top of the desulfurization tower is provided with an MDEA inlet and a gas outlet.
9. The device of claim 5, wherein the top of the first rich liquid centrifugal flash evaporation hydrocarbon-removing oil remover is provided with a gas outlet, the middle part is provided with an oil phase outlet, and the bottom is provided with a rich liquid outlet; the top of the second rich liquid centrifugal flash evaporation dealkylation degreaser is provided with a gas outlet, the middle part is provided with an oil phase outlet, and the bottom is provided with an acidic sewage and wastewater outlet.
10. The device of claim 5, wherein a pre-desulfurization tower gas-liquid separation device is connected between the gas outlet of the cold high-pressure separator and the desulfurization tower, the top of the pre-desulfurization tower gas-liquid separation device is provided with a gas outlet connected with the lower part of the desulfurization tower, and the bottom of the pre-desulfurization tower gas-liquid separation device is provided with an oil phase outlet.
11. The apparatus of claim 5, wherein the hot high pressure separator comprises a tank, a gas-liquid inertial separation module secured within the tank, and a plurality of centrifugal flash modules secured to a bottom surface of the gas-liquid inertial separation module.
The cold high-pressure separator comprises a tank body, a gas-liquid condensation separation module fixed in the upper tank body, a gas-liquid inertia separation module fixed in the middle tank body, a plurality of centrifugal flash modules fixed on the bottom surface of the gas-liquid inertia separation module, and an oil-water condensation separation module fixed in the lower tank body;
the hot low-pressure separator is the same as the hot high-pressure separator in structure;
the front gas-liquid separation device of the desulfurizing tower comprises a tank body and a gas-liquid condensation separation module fixed on the tank body;
the first rich liquid centrifugal flash evaporation dealkylation oil remover and the second rich liquid centrifugal flash evaporation dealkylation oil remover are identical in structure and respectively comprise a tank body, a distributor fixed in the tank body, a liquid collecting disc positioned below the distributor, a centrifugal flash evaporation module positioned below the liquid collecting disc and an inclined plate positioned below the centrifugal flash evaporation module, wherein a through hole is formed in the middle of the inclined plate, and an oil-water rapid separation module is fixed in the through hole.
12. The apparatus of claim 5, wherein the gaseous petroleum hydrocarbon outlet is coupled to a supersonic temperature-change based gas purifier comprising a supersonic separator and a condensate separator;
the supersonic speed separator comprises a gradually-reduced acceleration cavity, a vortex-making cavity, a supersonic speed separation cavity and a gradually-expanded boosting cavity which are sequentially connected according to a treatment sequence, wherein the vortex-making cavity comprises a cavity body and a plurality of spiral blades which are uniformly fixed on the cavity body, the inner diameters of the vortex-making cavity and the supersonic speed separation cavity are the same, a gas phase inlet is formed in the gradually-reduced acceleration cavity, a high-temperature purified gas outlet is formed in the gradually-expanded boosting cavity, and a condensate outlet is formed in the bottom of the supersonic speed separation cavity;
the condensate separator includes a jar body and fixes the internal gas-liquid condensation separation module of jar, gas-liquid condensation separation module below open the condensate import on the jar body, condensate import intercommunication the condensate export, the top of the jar body is equipped with low temperature and purifies the gas outlet, the bottom of the jar body is equipped with purifies the condensate export.
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