CN117326635B - Oil-water separation device based on hydrate technology and use method thereof - Google Patents

Abstract

The present invention discloses an oil-water separation device based on hydrate technology and a method for using the same, which separates oil and water. The device comprises a high-pressure reactor, a first cooling mechanism, a first water injection port, a first drainage port, a manual drain valve, a high-pressure filter reactor, and a filter screen; the high-pressure filter reactor is arranged below the high-pressure reactor; the high-pressure reactor is a sealed container, and the upper end of the high-pressure filter reactor is detachably and sealedly connected to the bottom of the high-pressure reactor; a first drainage port is arranged at the bottom of the high-pressure reactor, and a manual drain valve is also arranged at the bottom of the high-pressure reactor; a filter screen is arranged inside the high-pressure filter reactor; a first gas injection port and a first liquid injection port are arranged on the high-pressure reactor; and a first cooling mechanism is arranged on the inner side wall of the high-pressure reactor. By introducing methane and oil-water emulsion into the high-pressure reactor, water molecules in the oil-water emulsion continuously migrate to the gas phase under high pressure and low temperature conditions, and combine with _CH4 molecules to form hydrates.

Description

Oil-water separation device based on hydrate technology and use method thereof

Technical Field

The present invention relates to the application field of hydrate technology, and specifically to an oil-water separation device based on hydrate technology and a method of using the same, which is particularly suitable for solving the oil-water separation treatment of oil-water emulsions generated in the process of deep-sea oil and gas development.

Background technique

Oil-water mixture is a kind of industrial wastewater containing petroleum and organic solvents, which is an increasingly concerned issue in the process of seabed energy exploitation and utilization. In recent years, industrial oil-water mixture pollution and offshore oil spills have occurred frequently. The simple discharge of a large amount of oil-water mixture not only causes waste of resources and economic losses, but also damages the ecological environment and seriously endangers human health. Therefore, it is imperative to develop new technologies or new materials that can effectively solve the problems of oily wastewater. At the same time, more and more offshore oil fields have entered the medium and high water content period, and oil field water production has begun to face more and more problems. This is most prominent in the fact that the investment and operating costs of surface water treatment equipment continue to increase with the increase in oil field water production. The limited water treatment has led to the implementation of oil field liquid extraction and stable production measures being restricted. Due to the limited extraction of liquid, oil wells will gradually approach the limit of economic exploitation and cannot obtain the best final oil field recovery rate.

At present, the membrane separation method is mainly used for the treatment of oil-water mixture. Separation membrane materials can be divided into metal-based membrane materials, polymer-based membrane materials, biomass-based membrane materials and inorganic-based membrane materials. Although the technology of separating stable oil-water mixtures with separation membranes has made great progress, most membrane materials are still in the laboratory stage, and the membrane separation method still has the disadvantages of weak sustainability, low separation efficiency, and easy structural damage. There are defects in the existing technology that the oil-water separation efficiency is low and the research on separation membrane materials is not yet mature. Therefore, the field is urgently developing an effective and efficient oil-water separation technology.

Summary of the invention

In view of this, the present invention discloses an oil-water separation device using hydrate technology, and the specific scheme is as follows:

An oil-water separation device based on hydrate technology, comprising a high-pressure reactor, a first cooling mechanism, a manual drain valve, a high-pressure filtering reactor, and a filter screen;

The high-pressure reactor is a sealed container, and its internal chamber is a hydrate generation chamber. A first liquid discharge port is provided at the bottom of the high-pressure reactor, and a manual liquid discharge valve for opening or closing the first liquid discharge port is also provided at the bottom of the high-pressure reactor; a first gas injection port and a first liquid injection port are provided on the side wall of the high-pressure reactor; the first cooling mechanism is arranged on the inner side wall of the high-pressure reactor, and a flow channel for cooling water circulation is provided in the first cooling mechanism, and a first water injection port and a first drain port connected to the flow channel in the first cooling mechanism are provided on the outer side wall of the high-pressure reactor;

The high-pressure filtering reactor is arranged below the high-pressure reactor. It is a container with an opening on the top. The upper end of the high-pressure filtering reactor is detachably and sealedly connected to the bottom of the high-pressure filtering reactor. The chamber in the high-pressure filtering reactor is a hydrate filtering chamber. The hydrate generation chamber is connected to the hydrate filtering chamber through the first liquid discharge port of the high-pressure reactor. The filter screen is arranged in the high-pressure filtering reactor.

As a supplement to the technical solution of the present invention, it also includes a stirring device, a first temperature sensor and a first pressure sensor.

The stirring device comprises a stirring motor, a stirring head and a stirring rod, wherein the stirring motor is arranged outside the high-pressure reactor, the stirring head is arranged inside the high-pressure reactor, one end of the stirring rod is connected to the stirring motor, and the other end of the stirring rod passes through the side wall of the high-pressure reactor and is connected to the stirring head located inside the high-pressure reactor;

The first temperature sensor and the first pressure sensor are both arranged on the side wall of the high-pressure reactor, and are used to detect the temperature and pressure in the high-pressure reactor; an observation window is arranged on the side wall of the high-pressure filtering reactor.

As a supplement to the technical solution of the present invention, it also includes a second cooling mechanism, a second temperature sensor, and a second pressure sensor.

The high pressure filtering reactor is provided with a second gas injection port;

The high-pressure filtering reactor is provided with a second cooling mechanism, the second cooling mechanism is provided with a flow channel for cooling water circulation, and the outer wall of the high-pressure filtering reactor is provided with a second water injection port and a second drainage port connected with the cooling water flow channel in the second cooling mechanism;

The second temperature sensor and the second pressure sensor are both arranged on the high-pressure filtering reactor and are used to detect the temperature and pressure in the high-pressure filtering reactor.

As a supplement to the technical solution of the present invention, it also includes a third temperature sensor and a fourth temperature sensor;

The first cooling mechanism is a first water bath interlayer arranged on the inner side wall of the autoclave, and the third temperature sensor is arranged on the side wall of the autoclave to detect the temperature of cooling water in the first water bath interlayer;

The second cooling mechanism is a second water bath interlayer arranged on the inner side wall of the high-pressure filtering reactor; the fourth temperature sensor is arranged on the side wall of the high-pressure filtering reactor and is used to detect the temperature of cooling water in the second water bath interlayer.

As a supplement to the technical solution of the present invention, an exhaust port is further provided on the side wall of the high-pressure filtering reactor; and a second liquid discharge port is provided at the bottom of the high-pressure filtering reactor.

As a supplement to the technical solution of the present invention, it also includes a filter and a spray device.

The spray device is arranged inside the high-pressure reactor, and comprises a nozzle and a spray pipe. The spray pipe is connected with the first liquid injection port, and the nozzle is arranged on the spray pipe. The filter is arranged in the first liquid injection port.

As a supplement to the technical solution of the present invention, an upper annular protrusion is provided on the outer periphery of the lower end side wall of the high-pressure reactor, and a lower annular protrusion is provided on the outer periphery of the upper end side wall of the high-pressure filtering reactor. The upper annular protrusion fits the lower annular protrusion and the two are connected by bolts, and a sealing ring is provided between the upper annular protrusion and the lower annular protrusion.

As a supplement to the technical solution of the present invention, a guide portion is provided inside the high-pressure reactor, which is arranged at the lower part of the high-pressure reactor, the outer periphery of the guide portion is fixedly connected to the inner wall of the high-pressure reactor, the upper end face of the guide portion is a conical surface with a high outer side and a low middle side, the first liquid discharge port is a vertical through hole opened downward at the lowest point of the upper end face of the guide portion, and the manual liquid discharge valve is arranged below the guide portion.

As a supplement to the technical solution of the present invention, it also includes a scraper and an electric push rod. The scraper and the electric push rod are both arranged in the high-pressure reactor. The scraper is an annular tubular structure. The lower edge of the scraper is designed as a blade-like structure. The outer periphery of the scraper is in contact with the inner wall of the high-pressure reactor. The electric push rod is fixed on the inner wall of the high-pressure reactor. The lower end of the electric push rod is connected to the upper end of the scraper. The scraper is driven to perform lifting and lowering movements by the electric push rod.

The present invention also discloses a method for using the oil-water separation device, which specifically comprises the following steps:

S1. Use deionized water to thoroughly clean the inside of the high-pressure reactor and the high-pressure filter reactor, and then use a vacuum pump to extract the air inside the high-pressure reactor and the high-pressure filter reactor to eliminate the interference of impurities;

S2. Pure methane gas and oil-water emulsion are injected into the autoclave through the first gas injection port and the first liquid injection port, cooling water is injected into the first water bath interlayer, and when the injection amount of the oil-water emulsion in the autoclave reaches the set value, the injection of the oil-water emulsion is stopped;

S3. When the pressure and temperature in the autoclave reach the set values, the stirring device is started, the methane in the autoclave is fully contacted with the oil-water emulsion, the water molecules in the oil-water emulsion react with the methane molecules to form a solid hydrate, the water and oil in the oil-water emulsion are separated, the pressure and temperature in the autoclave are monitored in real time by the first temperature sensor and the first pressure sensor, and the stirring device is turned off when the pressure in the autoclave reaches stability;

S4. Inject methane into the high-pressure filter reactor through the second gas injection port, adjust the pressure in the high-pressure filter reactor, inject cooling water into the second water bath interlayer, adjust the temperature in the high-pressure filter reactor, and keep the pressure and temperature in the high-pressure filter reactor equal to the pressure and temperature in the high-pressure filter reactor;

S5. Open the drain valve to allow the hydrate in the high-pressure reactor to flow into the high-pressure filter reactor along with the oil. The filter in the high-pressure filter reactor will filter the hydrate.

S6. Open the exhaust port on the high-pressure filter reactor to keep the internal and external pressures of the entire device balanced, open the valve at the second drain port to discharge the oil in the high-pressure filter reactor, separate the high-pressure filter reactor from the high-pressure reactor, and take out the hydrate particles on the filter screen in the high-pressure filter reactor.

Beneficial effects: The present invention separates water molecules in the oil-water mixed emulsion by using the hydrate gas separation technology through the structural design of the oil-water separation device; compared with the traditional membrane separation method, it is more efficient and more sustainable; the device has the advantages of simple operation, convenient production, simple process flow, low energy consumption, and harmlessness to the environment.

BRIEF DESCRIPTION OF THE DRAWINGS

FIG1 is a schematic cross-sectional view of the structure of the present invention.

FIG. 2 is a schematic diagram of the structure of a high-pressure reactor according to the present invention.

FIG. 3 is a schematic diagram of the structure of the manual drain valve of the present invention.

FIG. 4 is a schematic structural diagram of a high-pressure filtering reactor according to the present invention.

FIG. 5 is a schematic diagram of the top view of the structure of the present invention.

In the figure: 1. high pressure reactor; 2. stirring head; 3. first water bath interlayer; 4. scraper; 5. first gas injection port; 6. first liquid injection port; 7. filter; 8. nozzle; 9. third temperature sensor; 10. first liquid discharge port; 11. first water injection port; 12. upper annular protrusion; 13. second pressure sensor; 14. exhaust port; 15. fourth temperature sensor; 16. second water injection port; 17. second liquid discharge port; 18. second water outlet; 19. second water bath interlayer; 20. filter screen; 21. high pressure filtration reactor; 22. second gas injection port; 23. second temperature sensor; 24. first water outlet; 25. first pressure sensor; 26. spray pipe; 27. first temperature sensor; 28. manual liquid discharge valve; 29. stirring motor; 30. stirring rod; 31. lower annular protrusion, 32. guide part.

Detailed ways

In the description of the present invention, it should be understood that the terms "first" and "second" are used for descriptive purposes only and should not be understood as indicating or implying relative importance or implicitly indicating the number of technical features indicated. Thus, a feature defined as "first" or "second" may explicitly or implicitly include at least one of the features. In the description of the present invention, the meaning of "plurality" is at least two, such as two, three, etc., unless otherwise clearly and specifically defined.

In the present invention, unless otherwise clearly specified and limited, the terms "installed", "connected", "connected", "fixed" and the like should be understood in a broad sense, for example, it can be a fixed connection, a detachable connection, or an integral one; it can be a mechanical connection, an electrical connection, or communication with each other; it can be a direct connection, or an indirect connection through an intermediate medium, it can be the internal connection of two elements or the interaction relationship between two elements, unless otherwise clearly defined. For ordinary technicians in this field, the specific meanings of the above terms in the present invention can be understood according to specific circumstances.

Hydrate gas separation is a new type _of gas separation technology. Gas hydrates are non-stoichiometric cage-type crystalline substances formed by water molecules (host) and small molecular gases such as _CH4 , _C2H6 , _CO2 (guest) under certain temperature and pressure conditions, and their appearance is similar to frost. The basic principle of gas separation by hydrate method is that different gas molecules have different degrees of difficulty in forming hydrates. Molecules that are easy to form hydrates will preferentially enter the hydrate phase, while molecules that are difficult to form hydrates will mainly remain in the gas phase, thereby achieving the separation effect. The conditions for the formation of hydrates in a pure water system are very harsh, and promoters are generally added in industry to reduce the conditions for the formation of hydrates. Hydrate gas separation technology has received widespread attention at home and abroad in recent years, and has gradually developed into a new type of gas separation method.

In order to solve the defects of low oil-water separation efficiency and immature research on separation membrane materials in the prior art, the present invention provides an oil-water separation device based on hydrate technology, which can separate water molecules in the oil-water mixed emulsion by real-time monitoring of working condition data and using hydrate gas separation technology. The specific technical scheme is as follows, as shown in Figures 1 to 5, an oil-water separation device based on hydrate technology includes a high-pressure reactor 1, a first cooling mechanism, a first water injection port 11, a first drain port 24, a stirring device, a manual drain valve 28, a high-pressure filtering reactor 21, and a filter 20.

The high-pressure filtering reactor 21 is arranged below the high-pressure reactor 1; the high-pressure reactor 1 is a sealed container, and its internal chamber is a hydrate generation chamber; the high-pressure filtering reactor 21 is a container with an opening on the top, and the upper end of the high-pressure filtering reactor 21 is detachably and sealedly connected to the bottom of the high-pressure reactor 1, and the chamber inside the high-pressure filtering reactor 21 is a hydrate filtration chamber; a first drain port 10 is provided at the bottom of the high-pressure reactor 1, and the hydrate generation chamber is connected to the hydrate filtration chamber through the first drain port 10 of the high-pressure reactor 1, and a manual drain valve 28 for opening or closing the first drain port 10 is also provided at the bottom of the high-pressure reactor 1.

The high-pressure reactor 1 is provided with a first gas injection port 5 and a first liquid injection port 6, and the high-pressure reactor 1 is provided with a valve for opening or closing the first gas injection port 5 and the first liquid injection port 6. The high-pressure reactor 1 is connected to the first gas injection port 5 through a pipeline, and methane gas is injected into the hydrate formation chamber in the high-pressure reactor 1. The pipeline connected to the first gas injection port 5 is provided with a gas flowmeter to monitor the gas injection amount in the high-pressure reactor 1. The high-pressure reactor 1 is connected to the first liquid injection port 6 through a pipeline, and the oil-water emulsion is injected into the hydrate formation chamber in the reactor. The specific gas injection amount in the high-pressure reactor 1 is determined according to the injection amount of the oil-water emulsion.

The inner wall of the autoclave 1 is provided with a first cooling mechanism, in which a flow channel for cooling water is provided, and the outer wall of the autoclave 1 is provided with a first water injection port 11 and a first drain port 24 connected with the flow channel in the first cooling mechanism, and cooling water is injected into the first cooling mechanism through the first water injection port 11, and the cooling water flows out from the first drain port 24. The temperature of the hydrate generation chamber in the autoclave 1 is controlled by heat exchange between the first cooling mechanism and the hydrate generation chamber in the autoclave 1.

After the hydrate generation in the high-pressure reactor 1 is completed, the manual drain valve 28 is opened to discharge the hydrate slurry into the high-pressure filtering reactor 21, wherein the hydrate slurry is composed of liquid oil and solid granular hydrate. The filter screen 20 in the high-pressure filtering reactor 21 is used to filter the solid granular hydrate, separate the oil and the hydrate, and achieve the purpose of oil-water separation. Preferably, the outer periphery of the filter screen 20 is connected to the inner side wall of the high-pressure filtering reactor 21, and a protrusion may be provided on the inner side wall of the high-pressure filtering reactor 21, and the outer edge of the filter screen 20 is placed on the protrusion.

As a supplement to the above technical solution, a first temperature sensor 27 and a first pressure sensor 25 are also included. The first temperature sensor 27 and the first pressure sensor 25 are both arranged on the side wall of the high-pressure reactor 1. The measuring ends of the first temperature sensor 27 and the first pressure sensor 25 are located inside the high-pressure reactor 1, and are used to detect the temperature and pressure inside the high-pressure reactor 1.

As a preferred technical solution of the present invention, a stirring device is also included, which includes a stirring motor 29, a stirring head 2, and a stirring rod 30. The stirring motor 29 is arranged outside the high-pressure reactor 1, and the stirring head 2 is arranged inside the high-pressure reactor 1. One end of the stirring rod 30 is connected to the stirring motor 29, and the other end of the stirring rod 30 passes through the side wall of the high-pressure reactor 1 and is connected to the stirring head 2 located in the high-pressure reactor 1. The stirring head 2 is driven to rotate by the motor to fully stir the oil-water emulsion in the hydrate formation chamber, so that the methane gas is fully dissolved in the oil-water emulsion. During the stirring process, the water molecules in the oil-water emulsion continuously migrate to the gas phase under the conditions of high pressure and low temperature, and combine with the guest _CH4 molecules to form hydrates.

As a supplement to the above technical solution, in order to avoid the destruction of the formed hydrates due to the sudden change of working conditions during the filtration process when the hydrate slurry is discharged from the high-pressure reactor 1 to the high-pressure filtration reactor 21. The present invention controls the temperature and pressure in the high-pressure filtration reactor 21, and the pressure and temperature in the high-pressure filtration reactor 21 are synchronized with the pressure and temperature in the high-pressure reactor 1. Specifically, the oil-water separation device also includes a second cooling mechanism, a second water injection port 16, a second drain port 18, a second temperature sensor 23, and a second pressure sensor 13,

The side wall of the high-pressure filtering reactor 21 is provided with a second gas injection port 22, and the high-pressure filtering reactor 21 is provided with a valve for opening or closing the second gas injection port 22, which is connected to the second gas injection port 22 through a gas booster pump, and methane is injected into the high-pressure filtering reactor 21 to increase the pressure in the high-pressure filtering reactor 21. The second pressure sensor 13 is arranged on the high-pressure filtering reactor 21, and its measuring end for detecting pressure is located inside the high-pressure filtering reactor 21, and is used to detect the pressure in the high-pressure filtering reactor 21.

The inner wall of the high-pressure filtering reactor 21 is provided with a second cooling mechanism, and a flow channel for cooling water circulation is provided in the second cooling mechanism. The outer wall of the high-pressure filtering reactor 21 is provided with a second water injection port 16 and a second drain port 18 connected to the flow channel in the second cooling mechanism. Cooling water is injected into the second cooling mechanism through the second water injection port 16, and the cooling water flows out from the second drain port 18. The temperature in the high-pressure filtering reactor 21 is controlled by the second cooling mechanism. The second temperature sensor 23 is provided on the high-pressure filtering reactor 21, and its measuring end for detecting temperature is located inside the high-pressure filtering reactor 21, and is used to detect the temperature in the high-pressure filtering reactor 21.

As a preferred technical solution of the present invention, a third temperature sensor 9 and a fourth temperature sensor 15 are also included.

The first cooling mechanism is a first water bath interlayer 3 arranged on the inner side wall of the autoclave 1. The autoclave 1 adopts a double-layer side wall structure, and the double-layer side wall structure forms the first water bath interlayer 3. The space in the first water bath interlayer 3 is a flow channel for cooling water circulation. The third temperature sensor 9 is arranged on the side wall of the autoclave 1, and is used to detect the temperature of the cooling water in the first water bath interlayer 3. The measuring end of the third temperature sensor 9 for detecting the temperature is located inside the first water bath interlayer 3 and contacts the cooling water in the water bath interlayer. The temperature in the first water bath interlayer 3 is detected by the third temperature sensor 9 to control the water bath temperature.

The second cooling mechanism is a second water bath interlayer 19 disposed on the inner side wall of the high-pressure filtration reactor 21. The high-pressure filtration reactor 21 adopts a double-layer side wall structure, which forms a first water bath interlayer 3. The space in the second water bath interlayer 19 is a flow channel for cooling water circulation. The fourth temperature sensor 15 is disposed on the side wall of the high-pressure filtration reactor 21 and is used to detect the temperature of the cooling water in the second water bath interlayer 19. The temperature in the second water bath interlayer 19 is detected by the fourth temperature sensor 15 to control the water bath temperature.

As a preferred technical solution of the present invention, it also includes a filter 7 and a spray device.

The spray device is arranged inside the high-pressure reactor 1, and includes a nozzle 8 and a spray pipe 26. The spray pipe 26 is connected to the first liquid injection port 6, and the nozzle 8 is arranged on the spray pipe 26. The oil-water emulsion flows into the spray pipe 26 through the first liquid injection port 6, and the oil-water emulsion is sprayed into the high-pressure reactor 1 at the nozzle 8. The spray device is arranged to increase the gas-liquid contact area, achieve full contact between the oil-water emulsion and the methane gas, dissolve more methane gas in the oil, and improve the reaction efficiency of the oil-water separation process.

The filter 7 is disposed in the first liquid injection port 6 to perform preliminary filtration on the oil-water emulsion to prevent the residue in the oil-water emulsion from clogging the nozzle 8 of the spraying device. Preferably, the filter 7 can be an industrial filter.

As a preferred technical solution of the present invention, an upper annular protrusion 12 is provided on the outer periphery of the lower end side wall of the high-pressure reactor 1, and a lower annular protrusion 31 is provided on the outer periphery of the upper end side wall of the high-pressure filtering reactor 21. When the high-pressure reactor 1 is connected to the high-pressure filtering reactor 21, the upper annular protrusion 12 on the high-pressure reactor 1 is fitted with the lower annular protrusion 31 on the high-pressure sealing reactor, and the upper annular protrusion 12 is connected to the lower annular protrusion 31 by a bolt structure. A sealing ring is provided between the upper annular protrusion 12 and the lower annular protrusion 31 to achieve a sealed connection between the high-pressure reactor 1 and the high-pressure filtering reactor 21.

As a preferred technical solution of the present invention, a flow guide 32 is provided inside the high-pressure reactor 1, which is arranged at the lower part of the high-pressure reactor 1, and the outer periphery of the flow guide 32 is fixedly connected to the inner wall of the high-pressure reactor 1, and the upper end surface of the flow guide 32 is a conical surface with a high outer side and a low middle side, so that the hydrate slurry in the high-pressure reactor 1 can flow smoothly along the upper end surface of the flow guide 32 to the position of the first drain port 10. The first drain port 10 is a vertical through hole opened downward at the lowest point of the upper end surface of the flow guide 32, and the manual drain valve 28 is arranged below the flow guide 32.

As a preferred technical solution of the present invention, an exhaust port 14 is also provided on the side wall of the high-pressure filtering reactor 21. A valve for opening or closing the exhaust port 14 is provided on the side wall of the high-pressure filtering reactor 21, which is connected to the exhaust port 14 through a pipeline. After the filter screen 20 completes the filtration of the hydrate, the valve at the exhaust port 14 is opened to balance the air pressure inside and outside the high-pressure reactor 1, and the waste gas in the high-pressure reactor 1 is recovered into the gas storage tank. A second drain port 17 is provided at the bottom of the high-pressure filtering reactor 21. A valve for opening or closing the drain port 17 is provided on the high-pressure filtering reactor 21, which is connected to the second drain port 17 through a pipeline. After the valve is opened, the oil in the high-pressure reactor 1 is discharged through the second drain port 17.

As a preferred technical solution of the present invention, during the hydrate generation process in the autoclave 1, part of the hydrate will be generated on the inner wall of the autoclave 1 and adhere to the inner wall of the autoclave 1, resulting in that when the drain valve is opened, this part of the hydrate is not discharged. In order to solve the above technical problems, the oil-water separation device also includes a scraper 4 and an electric push rod (not shown in the figure), and the scraper 4 and the electric push rod are both arranged in the autoclave 1. The scraper 4 is an annular tubular structure, and the lower edge of the scraper 4 is designed as a blade-like structure. The outer periphery of the scraper 4 is in contact with the inner wall of the autoclave 1, and the hydrate on the inner wall of the autoclave 1 is scraped off by the downward movement of the scraper 4, so that it falls into the hydrate slurry.

The electric push rod is fixed on the inner wall of the autoclave 1, and the lower end of the electric push rod is connected to the upper end of the scraper 4, and the scraper 4 is driven by the electric push rod to move up and down. Preferably, in order to prevent the oil-water emulsion in the autoclave 1 from entering the electric push rod and causing a short circuit, the electric push rod should be covered with a waterproof structure,

As a preferred technical solution of the present invention, an observation window is provided on the side wall of the high-pressure filtering reactor 21 for observing the filtering condition of hydrates by the filter screen 20 in the high-pressure reactor 1 .

The present invention also discloses a method for using the above device, which specifically comprises the following steps:

S1. Use deionized water to thoroughly clean the inside of the high-pressure reactor 1 and the high-pressure filtering reactor 21, and then use a vacuum pump to extract the air inside the high-pressure reactor 1 and the high-pressure filtering reactor 21 to eliminate the interference of impurities.

S2. Open the valves on the first gas injection port 5 and the first liquid injection port 6, and inject pure methane gas and oil-water emulsion into the high-pressure reactor 1 at a liquid content ratio of 1:6. When the injected volume of the oil-water emulsion reaches 2/3 of the volume of the high-pressure reactor 1, stop injecting the oil-water emulsion into the high-pressure reactor 1, and inject cooling water with a temperature of 5°C into the first water bath interlayer 3.

S3. Inject methane gas into the high-pressure reactor 1 through the first gas injection port 5 to stabilize the pressure in the device to 6MPa, start the stirring device, and measure the pressure and temperature in the high-pressure reactor 1 through the first temperature sensor 27 and the first pressure sensor 25. Due to the stirring of the stirring device, the pressure value in the high-pressure reactor 1 increases. When the pressure in the high-pressure reactor 1 drops and reaches stability, turn off the stirring device and record the temperature and pressure at this time.

S4. Start the electric push rod to drive the scraper 4 to scrape off the hydrates adhered to the wall of the hydrate generation chamber, so that the hydrates adhered to the wall of the hydrate generation chamber fall into the oil. At the same time, methane is injected into the high-pressure filter reactor 21 through the second gas injection port 22, and cooling water is injected into the second water bath interlayer 19, so that the pressure in the high-pressure filter reactor 21 is almost the same as the pressure in the high-pressure reactor 1.

S5. Open the drain valve at the bottom of the high-pressure reactor 1 to discharge the hydrate slurry into the high-pressure filtering reactor 21. The filter screen 20 filters the hydrate particles and then the mixture is allowed to stand.

S6. After the standing is completed, the exhaust port 14 on the high-pressure filter reactor 21 is opened to balance the pressure inside and outside the whole device, the valve on the second drain port 17 is opened to discharge the oil in the high-pressure filter reactor 21, the high-pressure filter reactor 21 is separated from the high-pressure reactor 1, and the hydrate particles on the filter screen 20 in the high-pressure filter reactor 21 are taken out. The filter screen 20 can separate the hydrate particles with a particle size of more than 15 um.

In the above step S3, the purpose of recording the temperature and pressure in the high-pressure filtering reactor 21 after the pressure in the high-pressure reactor 1 drops and reaches stability is to determine whether the temperature and pressure in the reactor meet the conditions for hydrate formation. If the conditions for hydrate formation are not met, the oil-water separation work fails, and the device is checked for problems such as air leakage.

In summary, the oil-water separation device disclosed in the present invention has the advantages of simple operation, convenient manufacture, simple process flow, low energy consumption, no pollutants and impurities generated during the reaction process, and is harmless to the environment.

The above description is only a preferred specific implementation manner of the present invention, but the protection scope of the present invention is not limited thereto. Any technician familiar with the technical field can make equivalent replacements or changes according to the technical solutions and inventive concepts of the present invention within the technical scope disclosed by the present invention, which should be covered by the protection scope of the present invention.

Claims (10)

1. An oil-water separation device based on hydrate technology, characterized in that it comprises a high-pressure reactor (1), a first cooling mechanism, a manual drain valve (28), a high-pressure filtering reactor (21), and a filter screen (20); The high-pressure reactor (1) is a sealed container, the internal chamber of which is a hydrate formation chamber. The bottom of the high-pressure reactor (1) is provided with a first liquid discharge port (10), and the bottom of the high-pressure reactor (1) is also provided with a manual liquid discharge valve (28) for opening or closing the first liquid discharge port (10); the side wall of the high-pressure reactor (1) is provided with a first gas injection port (5) and a first liquid injection port (6); the first cooling mechanism is arranged on the inner side wall of the high-pressure reactor (1), and a flow channel for cooling water circulation is provided in the first cooling mechanism; the outer side wall of the high-pressure reactor (1) is provided with a first water injection port (11) and a first drain port (24) which are connected to the flow channel in the first cooling mechanism; The high-pressure filtering reactor (21) is arranged below the high-pressure reactor (1), and is a container with an opening at the top. The upper end of the high-pressure filtering reactor (21) is detachably and hermetically connected to the bottom of the high-pressure reactor (1). The chamber in the high-pressure filtering reactor (21) is a hydrate filtering chamber. The hydrate generation chamber is connected to the hydrate filtering chamber through the first liquid discharge port (10) of the high-pressure reactor (1); and the filter screen (20) is arranged in the high-pressure filtering reactor (21). 2. The oil-water separation device based on hydrate technology according to claim 1, characterized in that it also includes a stirring device, a first temperature sensor (27) and a first pressure sensor (25), The stirring device comprises a stirring motor (29), a stirring head (2), and a stirring rod (30); the stirring motor (29) is arranged outside the high-pressure reactor (1); the stirring head (2) is arranged inside the high-pressure reactor (1); one end of the stirring rod (30) is connected to the stirring motor (29); and the other end of the stirring rod (30) passes through the side wall of the high-pressure reactor (1) and is connected to the stirring head (2) located inside the high-pressure reactor (1); The first temperature sensor (27) and the first pressure sensor (25) are both arranged on the side wall of the high-pressure reactor (1) and are used to detect the temperature and pressure in the high-pressure reactor (1); an observation window is arranged on the side wall of the high-pressure filtering reactor (21). 3. The oil-water separation device based on hydrate technology according to claim 2, characterized in that it also includes a second cooling mechanism, a second temperature sensor (23), and a second pressure sensor (13), The high-pressure filtering reaction kettle (21) is provided with a second gas injection port (22); The high-pressure filtering reaction kettle (21) is provided with a second cooling mechanism, the second cooling mechanism is provided with a flow channel for cooling water circulation, and the outer wall of the high-pressure filtering reaction kettle (21) is provided with a second water injection port (16) and a second water discharge port (18) which are connected to the cooling water flow channel in the second cooling mechanism; The second temperature sensor (23) and the second pressure sensor (13) are both arranged on the high-pressure filtering reactor (21) and are used to detect the temperature and pressure in the high-pressure filtering reactor (21). 4. The oil-water separation device based on hydrate technology according to claim 3, characterized in that it also includes a third temperature sensor (9) and a fourth temperature sensor (15); The first cooling mechanism is a first water bath interlayer (3) arranged on the inner side wall of the high-pressure reactor (1), and the third temperature sensor (9) is arranged on the side wall of the high-pressure reactor (1) and is used to detect the temperature of cooling water in the first water bath interlayer (3); The second cooling mechanism is a second water bath interlayer (19) arranged on the inner wall of the high-pressure filtering reactor (21); the fourth temperature sensor (15) is arranged on the side wall of the high-pressure filtering reactor (21) and is used to detect the temperature of cooling water in the second water bath interlayer (19). 5. An oil-water separation device based on hydrate technology according to claim 4, characterized in that an exhaust port (14) is also provided on the side wall of the high-pressure filtering reactor (21); and a second liquid discharge port (17) is provided at the bottom of the high-pressure filtering reactor (21). 6. The oil-water separation device based on hydrate technology according to claim 1, characterized in that it also includes a filter (7), a spray device, The spray device is arranged inside the high-pressure reactor (1), and comprises a nozzle (8) and a spray pipe (26); the spray pipe (26) is connected to the first liquid injection port (6); the nozzle (8) is arranged on the spray pipe (26); and the filter (7) is arranged inside the first liquid injection port (6). 7. An oil-water separation device based on hydrate technology according to claim 1, characterized in that an upper annular protrusion (12) is provided on the outer periphery of the lower end side wall of the high-pressure reactor (1), and a lower annular protrusion (31) is provided on the outer periphery of the upper end side wall of the high-pressure filtering reactor (21), the upper annular protrusion (12) and the lower annular protrusion (31) are in contact with each other and the two are connected by bolts, and a sealing ring is provided between the upper annular protrusion (12) and the lower annular protrusion (31). 8. An oil-water separation device based on hydrate technology according to claim 1, characterized in that a guide portion (32) is provided inside the high-pressure reactor (1), which is arranged at the lower part of the high-pressure reactor (1), the outer periphery of the guide portion (32) is fixedly connected to the inner wall of the high-pressure reactor (1), the upper end surface of the guide portion (32) is a conical surface with a high outer side and a low middle side, the first drain port (10) is a vertical through hole opened downward at the lowest point of the upper end surface of the guide portion (32), and the manual drain valve (28) is arranged below the guide portion (32). 9. An oil-water separation device based on hydrate technology according to claim 1, characterized in that it also includes a scraper (4) and an electric push rod, the scraper (4) and the electric push rod are both arranged in the high-pressure reactor (1), the scraper (4) is an annular tubular structure, the lower edge of the scraper (4) is designed as a blade-like structure, the outer periphery of the scraper (4) is in contact with the inner wall of the high-pressure reactor (1), the electric push rod is fixed on the inner wall of the high-pressure reactor (1), the lower end of the electric push rod is connected to the upper end of the scraper (4), and the scraper (4) is driven by the electric push rod to perform lifting movement. 10. The method for using the oil-water separation device according to claim 5, characterized in that it specifically comprises the following steps: S1. The high pressure reactor (1) and the high pressure filter reactor (21) are thoroughly cleaned with deionized water, and then the air inside the high pressure reactor (1) and the high pressure filter reactor (21) is extracted using a vacuum pump to eliminate the interference of impurities; S2. Pure methane gas and oil-water emulsion are injected into the autoclave (1) through the first gas injection port (5) and the first liquid injection port (6), and cooling water is injected into the first water bath interlayer (3). When the injection amount of the oil-water emulsion in the autoclave (1) reaches the set value, the injection of the oil-water emulsion is stopped; S3. When the pressure and temperature in the high-pressure reactor (1) reach the set values, the stirring device is started, and the methane in the high-pressure reactor (1) is fully in contact with the oil-water emulsion, so that the water molecules in the oil-water emulsion react with the methane molecules to form a solid hydrate, and the water and oil in the oil-water emulsion are separated. The pressure and temperature in the high-pressure reactor (1) are monitored in real time by the first temperature sensor (27) and the first pressure sensor (25). When the pressure in the high-pressure reactor (1) reaches stability, the stirring device is turned off; S4. Inject methane into the high-pressure filter reactor (21) through the second gas injection port (22) of the high-pressure filter reactor (21), adjust the pressure in the high-pressure filter reactor (21), inject cooling water into the second water bath interlayer (19), and adjust the temperature in the high-pressure filter reactor (21) so that the pressure and temperature in the high-pressure filter reactor (21) are kept equal to the pressure and temperature in the high-pressure reactor (1); S5. Open the drain valve to allow the hydrate in the high-pressure reactor (1) to flow into the high-pressure filter reactor (21) along with the oil, and the filter screen (20) in the high-pressure filter reactor (21) filters the hydrate. S6. Open the exhaust port (14) on the high-pressure filtering reactor (21) to keep the pressure inside and outside the whole device balanced, open the valve at the second drain port (17) to discharge the oil in the high-pressure filtering reactor (21), separate the high-pressure filtering reactor (21) from the high-pressure reactor (1), and remove the hydrate particles on the filter screen (20) in the high-pressure filtering reactor (21).