An oil-water-solid-gas four-phase separation device and method

Abstract

The present invention provides an oil-water-solid-gas four-phase separation device, comprising: a separator; a gas-phase outlet is provided at the top of the separator, an oil-phase outlet is provided at the upper part, a water-phase outlet is provided at the lower part, and a solid-phase outlet is provided at the bottom; valves are respectively provided at the gas-phase outlet, the oil-phase outlet, the water-phase outlet and the solid-phase outlet; a plurality of salt slurry receiving tanks respectively connected to the solid-phase outlet; a feed cut-off valve is provided between each salt slurry receiving tank and the solid-phase outlet, a liquid supplement port, a stirring device and a density measuring device are provided at the top, and a discharge port is provided at the bottom; a salt slurry pump respectively connected to the discharge port of each salt slurry receiving tank; a discharge cut-off valve is provided between the salt slurry pump and the discharge port of each salt slurry receiving tank; the salt slurry pump is connected to a salt slurry separation device. The device adopts a specific structure and connection relationship to achieve good overall interaction, can realize the four-phase separation of oil, water, solid and gas without polluting the environment and without damaging the yield, and can also perform continuous separation.

Description

Technical Field

[0001] The present invention relates to the technical field of oil-water-solid-gas separation in a chemical reaction system, and more specifically, to an oil-water-solid-gas four-phase separation device and method that can achieve continuous separation without polluting the environment. Background Art

[0002] Currently, the domestic industrial method for synthesizing dicyclohexyl disulfide uses sodium sulfide, sulfur, and chlorocyclohexane as raw materials. In the first step, sodium disulfide is prepared by mixing sodium sulfide and sulfur in a certain ratio at a specific temperature. According to the conventional feeding method, the mass fraction of sodium disulfide in the sodium disulfide preparation system is 10-35 wt%. In the second step, chlorocyclohexane is added to react with sodium disulfide at a set temperature. After the reaction is completed, the system contains: organic phase: dicyclohexyl disulfide, chlorocyclohexane, cyclohexene, etc. (commonly known as the oil phase), unreacted sodium sulfide, sodium disulfide, water, and the generated sodium chloride form a water-soluble mother liquor. Since it is an oil-water two-phase system, the reaction solution is separated by static or dynamic stratification.

[0003] However, the preparation process of dicyclohexyl disulfide in the enterprise where the applicant is located is different from the above method. The main preparation process is as follows: In the first step, in the sodium disulfide solution system prepared by the high-concentration sodium disulfide preparation process, the mass fraction of sodium disulfide is more than 30 wt%. In the second step, chlorocyclohexane is added to react with sodium disulfide at a set temperature. The chlorocyclohexane is converted to release chloride ions, which react with sodium ions to form a saturated solution of sodium chloride and precipitate crystalline sodium chloride. After the reaction is completed, the system contains: (1) organic phase: dicyclohexyl disulfide, chlorocyclohexane, cyclohexene, etc. (commonly known as the oil phase), (2) water phase: unreacted sodium sulfide, sodium disulfide, water, and the generated sodium chloride form a water-soluble mother liquor, (3) solid phase: crystalline sodium chloride deposits at the lower layer of the mother liquor to form a salt slurry layer, (4) gas phase: volatile gases contained in the system.

[0004] There are various forms of oil-water two-phase separation devices in China, methane gas, sewage, and activated sludge three-phase separators in wastewater treatment systems, and oil-gas-water three-phase separators in oil production systems. It is reported that there is a three-phase separator, namely a centrifuge, which separates solids, and then the mother liquor and oil pass through an oil-water separator. The organic volatile oil phase in this separator is separated by centrifugation, and the volatile oil gas is discharged with the material and emitted into the space. However, due to the emission of the organic phase, this separation device not only pollutes the environment but also damages the yield, and cannot meet the needs of society and enterprises.

[0005] In addition, for the oil-water-gas-solid four-phase separator in the prior art, for example, CN2766932Y discloses an oil-gas-water-solid four-phase separation and filtration device. Its solid-phase separation directly sets a discharge port at the bottom, and the solid phase is directly discharged into the atmosphere. Due to the emission of the organic phase in this separation equipment, it not only pollutes the environment but also damages the yield, and cannot meet the needs of society and enterprises. If the solid phase is to be discharged into a relatively closed container, when the container is filled with the solid phase, the air in the container will enter the upper separator along the discharge pipeline, which will disrupt and destroy the relatively stable stratification state formed in the separator. At this time, a relatively stable stratification state cannot be formed in the separator, and continuous discharging of each phase cannot be achieved, which will make the separation process of the entire separation device discontinuous and seriously reduce the separation efficiency. Summary of the Invention

[0006] In view of this, the purpose of the present invention is to provide an oil-water-solid-gas four-phase separation device and method, which can achieve oil-water-solid-gas four-phase separation without polluting the environment, without damaging the yield, and can also continuously separate.

[0007] The present invention provides an oil-water-solid-gas four-phase separation device, including:

[0008] A separator; a gas-phase outlet is provided at the top of the separator, an oil-phase outlet is provided at the upper part, a water-phase outlet is provided at the lower part, and a solid-phase outlet is provided at the bottom; valves are respectively provided at the gas-phase outlet, oil-phase outlet, water-phase outlet and solid-phase outlet;

[0009] A plurality of salt slurry receiving tanks respectively connected to the solid-phase outlet; a feed cut-off valve is provided between each salt slurry receiving tank and the solid-phase outlet, a liquid supplement port, a stirring device and a density measuring device are provided at the top, and a discharge port is provided at the bottom;

[0010] A salt slurry pump respectively connected to the discharge port of each salt slurry receiving tank; a discharge cut-off valve is provided between the salt slurry pump and the discharge port of each salt slurry receiving tank; the salt slurry pump is connected to a salt slurry separation device.

[0011] Preferably, the upper part of the separator is cylindrical and the lower part is conical; the water-phase outlet is arranged at the contact position between the upper and lower parts of the separator.

[0012] Preferably, the water-phase outlet is connected to a mother liquor receiving tank through a water-phase pipeline; the water-phase pipeline includes a water-phase outlet pipe communicated with the water-phase outlet and a water-phase overflow pipe communicated with the water-phase outlet pipe; the water-phase outlet pipe is arranged obliquely upward and forms a certain angle with the cylinder body of the separator, and the water-phase overflow pipe is arranged parallel to the cylinder body of the separator; an overflow port lower than the oil-phase outlet is provided on the water-phase overflow pipe; the overflow port is connected to the mother liquor receiving tank.

[0013] Preferably, the water phase outlet pipe forms an angle of ≤ 45° with the cylinder body of the separator.

[0014] Preferably, the gas phase outlet is connected to the condensate receiving tank through a gas phase balance pipe; the top of each salt slurry receiving tank and the top of the water phase overflow pipe are both connected to the gas phase balance pipe through pipelines.

[0015] Preferably, the gas phase outlet is connected to the inlet of an organic gas condenser through a gas phase balance pipe; the outlet of the organic gas condenser is connected to the condensate receiving tank;

[0016] The oil phase outlet is connected to the inlet of an oil phase outlet heat exchanger through a pipeline; the outlet of the oil phase outlet heat exchanger is connected to an oil phase receiving tank.

[0017] Preferably, the separator is provided with a distributor; the distributor penetrates through the top of the separator and is inserted into the separator, with a feed inlet at the upper part and discharge holes on the side of the lower part.

[0018] Preferably, the position where the distributor is inserted into the separator is at the 2 / 3 position from top to bottom of the separator; the height of the bottom of the distributor is lower than the height of the oil phase outlet and higher than the height of the water phase outlet.

[0019] Preferably, the solid phase outlet is connected to two salt slurry receiving tanks through pipelines respectively; the two salt slurry receiving tanks are the first salt slurry receiving tank and the second salt slurry receiving tank respectively;

[0020] The first salt slurry receiving tank is provided with a first liquid supplement port, a first stirrer and a first densitometer at the top, and a first discharge port at the bottom; the first salt slurry receiving tank is connected to the solid phase outlet through a first feed cut-off valve; the first discharge port is connected to a salt slurry pump through a first discharge cut-off valve;

[0021] The second salt slurry receiving tank is provided with a second liquid supplement port, a second stirrer and a second densitometer at the top, and a second discharge port at the bottom; the second salt slurry receiving tank is connected to the solid phase outlet through a second feed cut-off valve; the second discharge port is connected to a salt slurry pump through a second discharge cut-off valve;

[0022] The first densitometer is interlocked with the first feed cut-off valve, the second feed cut-off valve and the first discharge cut-off valve respectively; the second densitometer is interlocked with the second feed cut-off valve, the first feed cut-off valve and the second discharge cut-off valve respectively.

[0023] The present invention also provides an oil-water-solid-gas four-phase separation method, which includes the following steps:

[0024] Using the oil-water-solid-gas four-phase separation device described in the above technical solution, first fill each salt slurry receiving tank with the aqueous phase; then send the mixed liquid material containing oil, water, solid, and gas into the separator for stratification;

[0025] After stratification, while continuously sending the mixed liquid material containing oil, water, solid, and gas into the separator, discharge the volatile gas from the gas phase outlet, condense it and send it into the condensate receiving tank, discharge the oil phase from the oil phase outlet, condense it and send it into the oil phase receiving tank, discharge the saturated salt solution from the aqueous phase outlet and send it into the mother liquor receiving tank, alternately discharge the salt slurry from the solid phase outlet into each salt slurry receiving tank, and alternately send the salt slurry from each salt slurry receiving tank to the salt slurry separation equipment through the salt slurry pump to separate the salt slurry.

[0026] The present invention provides an oil-water-solid-gas four-phase separation device and method; the device includes: a separator; the separator is provided with a gas phase outlet at the top, an oil phase outlet at the upper part, an aqueous phase outlet at the lower part, and a solid phase outlet at the bottom; valves are respectively provided at the gas phase outlet, the oil phase outlet, the aqueous phase outlet, and the solid phase outlet; several salt slurry receiving tanks respectively connected to the solid phase outlet; a feed cut-off valve is provided between each salt slurry receiving tank and the solid phase outlet, a liquid supplement port, a stirring device, and a density measuring device are provided at the top, and a discharge port is provided at the bottom; a salt slurry pump respectively connected to the discharge port of each salt slurry receiving tank; a discharge cut-off valve is provided between the salt slurry pump and the discharge port of each salt slurry receiving tank; the salt slurry pump is connected to the salt slurry separation equipment. Compared with the prior art, the oil-water-solid-gas four-phase separation device provided by the present invention adopts a specific structure and connection relationship to achieve good overall interaction, can realize the four-phase separation of oil, water, solid, and gas without polluting the environment, without damaging the yield, and can also perform continuous separation. Description of the Drawings

[0027] Figure 1 It is a schematic structural diagram of the oil-water-solid-gas four-phase separation device provided by an embodiment of the present invention. Detailed Embodiments

[0028] Next, the technical solution of the present invention will be clearly and completely described in conjunction with the embodiments of the present invention. Obviously, the described embodiments are only a part of the embodiments of the present invention, rather than all the embodiments. Based on the embodiments of the present invention, all other embodiments obtained by those of ordinary skill in the art without making creative efforts shall fall within the protection scope of the present invention.

[0029] The present invention provides an oil-water-solid-gas four-phase separation device, including:

[0030] A separator; the separator is provided with a gas phase outlet at the top, an oil phase outlet at the upper part, an aqueous phase outlet at the lower part, and a solid phase outlet at the bottom; valves are respectively provided at the gas phase outlet, the oil phase outlet, the aqueous phase outlet, and the solid phase outlet;

[0031] A plurality of salt slurry receiving tanks respectively connected to the solid phase outlet; a feed cut-off valve is provided between each of the salt slurry receiving tanks and the solid phase outlet, a liquid replenishment port, a stirring device and a density measuring device are provided at the top, and a discharge port is provided at the bottom;

[0032] A salt slurry pump respectively connected to the discharge port of each salt slurry receiving tank; a discharge cut-off valve is provided between the salt slurry pump and the discharge port of each salt slurry receiving tank; the salt slurry pump is connected to a salt slurry separation device.

[0033] In the present invention, the oil-water-solid-gas four-phase separation device includes a separator and a plurality of salt slurry receiving tanks; wherein, the separator is used for gravity stratification of the oil-water-solid-gas four-phase mixture, and the salt slurry receiving tank is used for receiving the solid phase in the separator through a water-phase filled accommodation space.

[0034] In the present invention, the separator is provided with a gas phase outlet, an oil phase outlet, a water phase outlet and a solid phase outlet in sequence from top to bottom in the height direction, and a valve is provided at each of the gas phase outlet, the oil phase outlet, the water phase outlet and the solid phase outlet.

[0035] In the present invention, the upper part of the separator is preferably cylindrical, and the lower part is preferably conical; the water phase outlet is preferably arranged at the contact position between the upper and lower parts of the separator.

[0036] In the present invention, the water phase outlet is connected to a mother liquor receiving tank through a water phase pipeline; the water phase pipeline includes a water phase outlet pipe communicated with the water phase outlet and a water phase overflow pipe communicated with the water phase outlet pipe; the water phase outlet pipe is arranged obliquely upward and forms a certain angle with the cylinder body of the separator, and the water phase overflow pipe is arranged parallel to the cylinder body of the separator; an overflow port with a height lower than the oil phase outlet is provided on the water phase overflow pipe; the overflow port is connected to the mother liquor receiving tank.

[0037] In the present invention, the water phase outlet pipe preferably forms an angle of ≤45° with the cylinder body of the separator.

[0038] In the present invention, the gas phase outlet is connected to a condensate receiving tank through a gas phase balance pipe; the top of each salt slurry receiving tank and the top of the water phase overflow pipe are both connected to the gas phase balance pipe through pipelines. If there is no gas phase balance pipe, the salt slurry receiving tank needs to be connected to the atmosphere, and the discharge port also needs to be higher than the oil-water separator, and there is a problem of unorganized emission of VOCs; it is not suitable to use a vacuum system here.

[0039] In the present invention, the gas phase outlet is connected to the inlet of an organic gas condenser through a gas phase balance pipe; the outlet of the organic gas condenser is connected to the condensate receiving tank.

[0040] In the present invention, the oil phase outlet is connected to the inlet of the oil phase outlet heat exchanger through a pipeline; the outlet of the oil phase outlet heat exchanger is connected to the oil phase receiving tank.

[0041] In the present invention, the separator is provided with a distributor; the distributor penetrates through the top of the separator and inserts into the interior of the separator, with a feed inlet at the upper part and discharge holes on the side of the lower part.

[0042] In the present invention, the position where the distributor inserts into the interior of the separator is preferably at the 2 / 3 position of the separator from top to bottom; the height of the bottom of the distributor is lower than the height of the oil phase outlet and higher than the height of the water phase outlet.

[0043] In a preferred embodiment of the present invention, the lower part of the salt slurry receiving tank is preferably conical, and a stirring device and a density measuring device extending into the interior of the salt slurry receiving tank are connected to the top; the stirring device is preferably a stirrer; the density measuring device is preferably a densitometer.

[0044] In the present invention, the stirring device is used to prevent the problem of blockage caused by the precipitation of solid salt; after the reaction of the materials in the reactor is completed, intermittent single-kettle feeding for oil-water separation can be carried out without a densitometer, and if multi-kettle continuous feeding is carried out for oil-water separation, a densitometer is required to judge whether the salt slurry receiving tank is full of salt slurry.

[0045] In a preferred embodiment of the present invention, the solid phase outlet is connected to two salt slurry receiving tanks through pipelines; the two salt slurry receiving tanks are respectively a first salt slurry receiving tank and a second salt slurry receiving tank;

[0046] The first salt slurry receiving tank is provided with a first liquid supplement port, a first stirrer and a first densitometer at the top, and a first discharge port at the bottom; the first salt slurry receiving tank is connected to the solid phase outlet through a first feed cut-off valve; the first discharge port is connected to a salt slurry pump through a first discharge cut-off valve;

[0047] The second salt slurry receiving tank is provided with a second liquid supplement port, a second stirrer and a second densitometer at the top, and a second discharge port at the bottom; the second salt slurry receiving tank is connected to the solid phase outlet through a second feed cut-off valve; the second discharge port is connected to a salt slurry pump through a second discharge cut-off valve;

[0048] The first densitometer is respectively interlocked with the first feed cut-off valve, the second feed cut-off valve and the first discharge cut-off valve; the second densitometer is respectively interlocked with the second feed cut-off valve, the first feed cut-off valve and the second discharge cut-off valve.

[0049] On this basis, reference can be made to Figure 1 as shown Figure 1It is an oil-water-solid-gas four-phase separation device, including a separator 1 and two slurry receiving tanks (2, 3). The separator is used for gravity stratification of the oil-water-solid-gas four-phase mixed liquid, and the slurry receiving tank is used to receive the solid phase in the separator through an accommodation space filled with the water phase. The separator 1 is successively provided with a gas phase outlet 11, an oil phase outlet 12, a water phase outlet 13 and a solid phase outlet 14 from top to bottom along the height direction of the separator. Valves are provided at the gas phase outlet 11, the oil phase outlet 12, the water phase outlet 13 and the solid phase outlet 14;

[0050] The solid phase outlet 14 is connected to the two slurry receiving tanks (2, 3) through pipelines. A feed cut-off valve (21, 31) is provided between each slurry receiving tank (2, 3) and the solid phase outlet 14. A stirrer (22, 32) and a densitometer (23, 33) extending into the interior of the slurry receiving tank are connected to the top of each slurry receiving tank (2, 3). A liquid supplement port (24, 34) is provided at the top of each slurry receiving tank (2, 3), and a discharge port (25, 35) is provided at the bottom of each slurry receiving tank (2, 3). The discharge port (25, 35) is connected to a slurry pump 4 through a pipeline. A discharge cut-off valve (26, 36) is provided between the discharge port (25, 35) and the slurry pump 4. The slurry pump 4 is connected to a slurry separation device;

[0051] The liquid supplement port (24, 34) is a water phase liquid supplement port separated from the separator or a water liquid supplement port;

[0052] The solid phase outlet 14 is connected to the two slurry receiving tanks (2, 3) through pipelines. The two slurry receiving tanks (2, 3) are respectively a first slurry receiving tank 2 and a second slurry receiving tank 3;

[0053] A first densitometer 23 and a first stirrer 22 are connected to the top of the first slurry receiving tank 2. A first liquid supplement port 24 is provided at the top of the first slurry receiving tank 2, and a first discharge port 25 is provided at the bottom. The first slurry receiving tank 2 is connected to the solid phase outlet 14 through a first feed cut-off valve 21. The first discharge port 25 is connected to the slurry pump 4 through a first discharge cut-off valve 26;

[0054] A second densitometer 33 and a second stirrer 32 are connected to the top of the second slurry receiving tank 3. A second liquid supplement port 34 is provided at the top of the second slurry receiving tank 3, and a second discharge port 35 is provided at the bottom. The second slurry receiving tank 3 is connected to the solid phase outlet 14 through a second feed cut-off valve 31. The second discharge port 35 is connected to the slurry pump 4 through a second discharge cut-off valve 36;

[0055] The first densitometer 23 is respectively interlocked with the first feed cut-off valve 21, the second feed cut-off valve 31, and the first discharge cut-off valve 26. The second densitometer 33 is respectively interlocked with the second feed cut-off valve 31, the first feed cut-off valve 21, and the second discharge cut-off valve 36.

[0056] In the above embodiment, by interlocking the densitometer with the feed cut-off valve and the discharge cut-off valve, not only can the feeding and discharging processes be made more automated and precise, but also since the material continuously enters the separator, the solid phase outlet also needs to continuously discharge without interruption. The interlocking setting can accurately ensure that the solid phase outlet continuously discharges salt slurry without interruption, thereby ensuring the stable stratification inside the separator.

[0057] Based on the above embodiment, the lower parts of the separator 1 and the salt slurry receiving tanks (2, 3) are both set to be conical, which is convenient for discharging.

[0058] Based on the above embodiment, the aqueous phase outlet 13 is connected to the mother liquor receiving tank through the aqueous phase pipeline 5. The aqueous phase pipeline 5 includes an aqueous phase outlet pipe 51 communicating with the aqueous phase outlet 13 and an aqueous phase overflow pipe 52 communicating with the aqueous phase outlet pipe 51. The aqueous phase outlet pipe 51 is arranged obliquely upward and forms a certain angle with the cylinder of the separator 1; this can avoid the deposition of solid salt slurry in the aqueous phase outlet pipe and prevent the blockage of the aqueous phase outlet. The aqueous phase overflow pipe 52 is arranged parallel to the cylinder of the separator 1, and an overflow port 521 with a height lower than the oil phase outlet 12 is provided on the aqueous phase overflow pipe 52. The aqueous phase outlet 13 is set at a relatively low height, and the overflow port 521 is set at a relatively high height. By overflowing the aqueous phase through the overflow port 521, on the one hand, it can prevent the oil phase from entering the aqueous phase outlet 13, and on the other hand, it can prevent the solid phase from entering the subsequent aqueous phase receiving equipment through the aqueous phase overflow pipe 52. In the present invention, the aqueous phase receiving equipment is the mother liquor receiving tank.

[0059] Based on the above embodiment, the aqueous phase outlet pipe 51 forms an angle of ≤ 45° with the cylinder of the separator 1; this can better avoid the deposition of solid salt slurry in the aqueous phase outlet pipe and prevent the blockage of the aqueous phase outlet.

[0060] Based on the above embodiment, the gas phase outlet 11 is connected to the condensate receiving tank through the gas phase balance pipe 6; the salt slurry receiving tanks (2, 3) and the top of the aqueous phase overflow pipe 52 are both connected to the gas phase balance pipe 6 through pipelines; thus, on the one hand, it can balance the air pressure in each component of the separation device, and on the other hand, it can prevent organic volatile gases from being discharged into the air through the conventional exhaust pipe and polluting the environment.

[0061] Based on the above embodiments, the gas phase outlet 11 is connected to the inlet of the organic gas condenser 7 through the gas phase balance pipe 6, and the outlet of the organic gas condenser 7 is connected to the condensate receiving tank; the oil phase outlet 12 is connected to the inlet of the oil phase outlet heat exchanger 8 through a pipeline, and the outlet of the oil phase outlet heat exchanger 8 is connected to the oil phase receiving tank; after cooling the gas phase and the oil phase, it is convenient to collect the low-boiling materials therein and reduce the collection loss of volatile materials.

[0062] Based on the above embodiments, a distributor 9 is connected to the top of the separator 1. The upper part of the distributor 9 is provided with a feed inlet 91. The lower part of the distributor 9 is inserted into the separator 1. The lower side of the distributor 9 is provided with a discharge hole 92; the material discharges horizontally through the discharge hole on the side of the distributor 9, and the flow direction of the material changes at the discharge hole, and the material flow is smoother, which can avoid the impact on the lower sedimentation layer when the material directly discharges downward and avoid affecting the stratification and sedimentation process in the separator.

[0063] Based on the above embodiments, the position where the bottom of the distributor 9 is inserted into the separator 1 is the 2 / 3 position of the separator 1 from top to bottom. The height of the bottom of the distributor 9 is lower than the height of the oil phase outlet 12 and higher than the height of the water phase outlet 13; setting the position of the discharge hole between the gas phase, the oil phase and the water phase and the solid phase can enable the material to stratify into the corresponding layer faster in the separator, making the sedimentation and stratification process in the separator 1 more efficient.

[0064] The present invention also provides an oil-water-solid-gas four-phase separation method, including the following steps:

[0065] Using the oil-water-solid-gas four-phase separation device described in the above technical solution, first fill each salt slurry receiving tank with the water phase; then send the mixed liquid material containing oil, water, solid and gas into the separator for stratification;

[0066] After stratification, while continuing to send the mixed liquid material containing oil, water, solid and gas into the separator, discharge the volatile gas from the gas phase outlet, condense it and send it into the condensate receiving tank, discharge the oil phase from the oil phase outlet, condense it and send it into the oil phase receiving tank, discharge the saturated salt solution from the water phase outlet and send it into the mother liquid receiving tank, alternately discharge the salt slurry from the solid phase outlet into each salt slurry receiving tank, and alternately send the salt slurry from each salt slurry receiving tank to the salt slurry separation equipment through the salt slurry pump to separate the salt slurry.

[0067] In the present invention, the stratification preferably relies on the different densities of the mixed liquid to achieve automatic gravity stratification.

[0068] In the present invention, when discharging the salt slurry from the solid phase outlet to each of the salt slurry receiving tanks and sending the salt slurry from each of the salt slurry receiving tanks to the salt slurry separation equipment for separating the salt slurry, first, open the feed cut-off valve between the first salt slurry receiving tank and the solid phase outlet. When the density meter detection port at the top of the first salt slurry receiving tank detects that the density is greater than the saturated brine density value by 0.05 g / ml, cut off the feed cut-off valve between the first salt slurry receiving tank and the solid phase outlet, and at the same time, open the feed cut-off valve between the next salt slurry receiving tank and the solid phase outlet to start feeding the salt slurry into the next salt slurry receiving tank. Also, open the discharge cut-off valve between the first salt slurry receiving tank and the salt slurry pump, start the stirrer in the first salt slurry receiving tank, and send the salt slurry into the salt slurry separation device through the salt slurry pump for centrifugally separating the salt slurry to separate out solid salt and salt-saturated mother liquor. After the salt slurry in the first salt slurry receiving tank is completely separated, fill the mother liquor into the first salt slurry receiving tank from which the solid salt has been separated, and wait for the next cycle; each salt slurry receiving tank repeats the above process of the first salt slurry receiving tank.

[0069] Combined with the oil-water-solid-gas four-phase separation device described in the above embodiments, the oil-water-solid-gas four-phase separation method provided by the present invention includes the following steps:

[0070] Fill each salt slurry receiving tank (2, 3) with the aqueous phase (mother liquor) or water;

[0071] Send the mixed liquid containing oil, water, solid, and gas (below 120 °C, above 25 °C, and a higher temperature is beneficial for rapid stratification) into the separator 1, and the mixed liquid automatically stratifies due to different densities;

[0072] After the mixed liquid is stratified, while continuing to send the mixed liquid containing oil, water, solid, and gas into the separator 1, discharge the volatile gas from the gas phase outlet 11, condense it and send it into the condensate receiving tank, discharge the oil phase from the oil phase outlet 12, condense it and send it into the oil phase receiving tank, discharge the saturated salt solution from the aqueous phase outlet 13, send it into the mother liquor receiving tank, alternately discharge the salt slurry from the solid phase outlet 14 into each of the salt slurry receiving tanks (2, 3), and alternately send the salt slurry from each of the salt slurry receiving tanks (2, 3) to the salt slurry separation equipment for separating the salt slurry.

[0073] Among them, when discharging the salt slurry from the solid phase outlet 14 to each salt slurry receiving tank (2, 3) and sending the salt slurry from each salt slurry receiving tank (2, 3) to the salt slurry separation equipment to separate the salt slurry, first open the feed cut-off valve 21 between the first salt slurry receiving tank 2 and the solid phase outlet 14. When the density meter 23 detection port at the top of the first salt slurry receiving tank 2 detects that the density is greater than the saturated brine density value of 0.05 g / ml, cut off the feed cut-off valve 21 between the first salt slurry receiving tank 2 and the solid phase outlet 14, and at the same time open the feed cut-off valve 31 between the next salt slurry receiving tank 3 and the solid phase outlet 14 to start feeding the salt slurry into the next salt slurry receiving tank 3. And open the discharge cut-off valve 26 between the first salt slurry receiving tank 2 and the salt slurry pump 4, turn on the stirrer 22 in the first salt slurry receiving tank 2, and send the salt slurry into the salt slurry separation device through the salt slurry pump 4 to centrifugally separate the salt slurry, separating out solid salt and salt-saturated mother liquor. After the salt slurry in the first salt slurry receiving tank 2 is separated, fill the mother liquor into the first salt slurry receiving tank 2 from which the solid salt has been separated, and wait for the next cycle; each salt slurry receiving tank (2, 3) repeats the foregoing process of the first salt slurry receiving tank 2.

[0074] The present invention provides an oil-water-solid-gas four-phase separation device and method; the device includes: a separator; a gas phase outlet is provided at the top of the separator, an oil phase outlet is provided in the upper part, a water phase outlet is provided in the lower part, and a solid phase outlet is provided at the bottom; valves are respectively provided at the gas phase outlet, the oil phase outlet, the water phase outlet and the solid phase outlet; a plurality of salt slurry receiving tanks respectively connected to the solid phase outlet; a feed cut-off valve is provided between each salt slurry receiving tank and the solid phase outlet, a liquid supplement port, a stirring device and a density measuring device are provided at the top, and a discharge port is provided at the bottom; a salt slurry pump respectively connected to the discharge port of each salt slurry receiving tank; a discharge cut-off valve is provided between the salt slurry pump and the discharge port of each salt slurry receiving tank; the salt slurry pump is connected to the salt slurry separation equipment. Compared with the prior art, the oil-water-solid-gas four-phase separation device provided by the present invention adopts a specific structure and connection relationship to achieve better overall interaction, can achieve oil-water-solid-gas four-phase separation without polluting the environment, without damaging the yield, and can also continuously separate.

[0075] In order to further illustrate the present invention, the following detailed description is given through the following embodiments.

[0076] Embodiment

[0077] Please refer to Figure 1 , Figure 1This is a schematic structural diagram of the oil-water-solid-gas four-phase separation device provided by the embodiments of the present invention. Among them, each component and its number are as follows: 1. Separator; 11. Gas-phase outlet; 12. Oil-phase outlet; 13. Water-phase outlet; 14. Solid-phase outlet; 2. First salt slurry receiving tank; 21. First feed cut-off valve; 22. First stirrer; 23. First densitometer; 24. First liquid supplement port; 25. First discharge port; 26. First discharge cut-off valve; 3. Second salt slurry receiving tank; 31. Second feed cut-off valve; 32. Second stirrer; 33. Second densitometer; 34. Second liquid supplement port; 35. Second discharge port; 36. Second discharge cut-off valve; 4. Salt slurry pump; 5. Water-phase pipeline; 51. Water-phase outlet pipe; 52. Water-phase overflow pipe; 521. Overflow port; 6. Gas-phase balance pipe; 7. Organic gas condenser; 8. Oil-phase outlet heat exchanger; 9. Distributor; 91. Feed port; 92. Discharge hole.

[0078] The working process (oil-water-solid-gas four-phase separation method) of the oil-water-solid-gas four-phase separation device provided by the embodiments of the present invention is as follows:

[0079] Fill the first salt slurry receiving tank 2 and the second salt slurry receiving tank 3 with the water-phase mother liquor so that the solid phase can be mixed with the water-phase mother liquor in the salt slurry receiving tank to form a salt slurry that can be transported. In addition, before opening the feed cut-off valve of the first salt slurry receiving tank 2 or the second salt slurry receiving tank 3 for operation, the first salt slurry receiving tank 2 or the second salt slurry receiving tank 3 must be filled with the water-phase mother liquor. Otherwise, when the feed cut-off valve is opened, the water phase and the oil phase in the separator 1 will instantly rush into the first salt slurry receiving tank 2 or the second salt slurry receiving tank 3 from above, destroying the states of each layer in the separator, interrupting the separation operation, and moreover, since the oil phase rushes into the first salt slurry receiving tank 2 or the second salt slurry receiving tank 3, the oil phase will surely float upward into the water-phase outlet pipe, disrupting the separation order and destroying the separation effect.

[0080] Feed the mixed liquid (50 °C) material containing oil, water, solid and gas into the separator 1. The mixed liquid automatically stratifies according to different densities (the specific gravity of the oil phase ≤ 1, the specific gravity of the water-phase mother liquor ≥ 1.1, and the specific gravity of the solid phase (salt slurry) ≥ 1.4. Due to the large difference in specific gravity, for the device manufactured according to the design calculation, other layers of liquid will not be mixed during discharge).

[0081] After the mixture is completely stratified, while continuously feeding the mixture containing oil, water, solid and gas into the separator 1, the volatile gas is discharged from the gas phase outlet 11, condensed and then fed into the condensate receiving tank. The oil phase is discharged from the oil phase outlet 12, condensed and then fed into the oil phase receiving tank. The saturated salt solution is discharged from the water phase outlet 13 and fed into the mother liquor receiving tank. The salt slurry is alternately discharged from the solid phase outlet 14 to the first salt slurry receiving tank 2 and the second salt slurry receiving tank 3, and alternately sent to the salt slurry separation equipment through the salt slurry pump 4 to separate the salt slurry from the first salt slurry receiving tank 2 and the second salt slurry receiving tank 3 (since the separator operates continuously, in order to prevent the salt slurry in the receiving tank from reaching the index and disturbing the liquid layer separation state in the separator when it is pumped out for centrifugal separation due to the liquid level fluctuation in the salt slurry tank, therefore, the first salt slurry receiving tank 2 and the second salt slurry receiving tank 3 must be alternately opened as receiving tanks).

[0082] Among them, when discharging the salt slurry from the solid-phase outlet 14 to the first salt slurry receiving tank 2 and the second salt slurry receiving tank 3, and when sending the salt slurry from the first salt slurry receiving tank 2 and the second salt slurry receiving tank 3 to the salt slurry separation equipment to separate the salt slurry, first open the feed cut-off valve 21 between the first salt slurry receiving tank 2 and the solid-phase outlet 14 (at this time, since the specific gravity of the salt slurry at the solid-phase outlet is greater than that of the saturated salt mother liquor in the first salt slurry receiving tank 2, and the saturated salt solution contains salt crystals, when the flow velocity is less than 0.1 m / s, natural stratification will form by gravity, the heavy phase will sink, and the light phase will be pushed out and float; but at this time, only the salt slurry flows out from the solid-phase outlet in the separator 1, and its stratification will not move downward). When the density meter 23 detection port at the top of the first salt slurry receiving tank 2 detects that the density is greater than the saturated brine density value of 0.05 g / ml, cut off the feed cut-off valve 21 between the first salt slurry receiving tank 2 and the solid-phase outlet 14, and at the same time open the feed cut-off valve 31 between the second salt slurry receiving tank 3 and the solid-phase outlet 14, start feeding the salt slurry into the second salt slurry receiving tank 3, and open the discharge cut-off valve 26 between the first salt slurry receiving tank 2 and the salt slurry pump 4, turn on the stirrer 22 in the first salt slurry receiving tank 2, and send the salt slurry into the salt slurry separation centrifugal separation of the salt slurry through the salt slurry pump 4, separate the solid salt and the salt-saturated mother liquor. After separating the salt slurry in the first salt slurry receiving tank 2, fill the mother liquor into the first salt slurry receiving tank 2 that has been separated from the solid salt, and wait for the next cycle; when the density meter 33 detection port at the top of the second salt slurry receiving tank 3 detects that the density is greater than the saturated brine density value of 0.05 g / ml, cut off the feed cut-off valve 31 between the second salt slurry receiving tank 3 and the solid-phase outlet 14, and at the same time open the feed cut-off valve 21 between the first salt slurry receiving tank 2 and the solid-phase outlet 14, start feeding the salt slurry into the first salt slurry receiving tank 2, and open the discharge cut-off valve 36 between the second salt slurry receiving tank 3 and the salt slurry pump 4, turn on the stirrer 32 in the second salt slurry receiving tank 3, and send the salt slurry into the salt slurry separation centrifugal separation of the salt slurry through the salt slurry pump 4, separate the solid salt and the salt-saturated mother liquor. After separating the salt slurry in the second salt slurry receiving tank 3, fill the mother liquor into the second salt slurry receiving tank 3 that has been separated from the solid salt, and wait for the next cycle.

[0083] The specific experimental data are as follows:

[0084] Single kettle reaction material components:

[0085]

[0086] Single kettle reaction material volume ratio:

[0087] oil phase aqueous phase mother liquor solid phase salt slurry 27.21％ 53.41％ 19.38％

[0088] Oil-water separation experiment 1 (original feed):

[0089] 1. Each kettle produces 18.9 m of material 3 ;

[0090] 2. Send out the mother liquor in the mother liquor receiving tank to fill the oil-water separator and the salt slurry receiving tank;

[0091] 3. After the reaction is completed, the reaction materials are pumped into the system with a delivery time of 45 minutes.

[0092]

[0093] Oil-water separation experiment 2 (normal feeding):

[0094] 1. Each kettle produces 18.9m3 of material 3 ;

[0095] 2. After the reaction is completed, the reaction materials are pumped into the system with a delivery time of 45 minutes.

[0096]

[0097] Oil-water separation experiment three (normal feeding):

[0098] 1. Each kettle produces 18.9m3 of material 3 ;

[0099] 2. After the reaction is completed, the reaction materials are pumped into the system with a delivery time of 45 minutes.

[0100]

[0101] Oil-water separation experiment 4 (normal feeding):

[0102] 1. Each kettle produces 18.9m3 of material 3 ;

[0103] 2. After the reaction is completed, the reaction materials are pumped into the system with a delivery time of 45 minutes.

[0104]

[0105] Oil-water separation experiment 5 (normal feeding):

[0106] 1. Each kettle produces 18.9m3 of material 3 ;

[0107] 2. After the reaction is completed, the reaction materials are pumped into the system with a delivery time of 45 minutes.

[0108]

[0109] In summary, the beneficial effects of the present invention are as follows: The present invention conducts a gravity separation experiment on the oil-water-solid-gas four-phase reaction liquid, and the above system will clearly separate into three layers in a short time; according to the above experimental principle, the oil-water-solid-gas four-phase separation device designed in the present application can automatically separate the oil-water-solid-gas four-phase mixed liquid during continuous feeding, and at least two salt slurry receiving tanks filled with the aqueous phase are arranged to alternately receive the salt slurry coming out from the solid phase outlet. Since the salt slurry receiving tank is not in communication with the atmosphere, the environment is not polluted. Since the salt slurry receiving tank is filled with the aqueous phase before use, the aqueous phase will not be squeezed upward by the entering solid phase into the separator, and the relatively stable stratification in the separator will not be damaged. Therefore, each phase in the separator can be continuously discharged; in addition, through the setting of the density meter, the feeding can be stopped after the salt slurry receiving tank receives a certain amount of solid phase salt slurry; by quantitatively setting the volume of the separator and the aperture of the solid phase outlet, while the separator is continuously feeding, the solid phase outlet at the lower part of the separator can continuously and alternately discharge salt slurry into each salt slurry receiving tank, so that continuous salt slurry discharge can be realized and the salt slurry can be transported to the salt slurry separation equipment, and further, continuous automatic separation of the oil-water-solid-gas four phases can be realized.

[0110] The foregoing description of the disclosed embodiments enables those skilled in the art to make or use the present invention. Various modifications to these embodiments will be readily apparent to those skilled in the art, and the general principles defined herein may be implemented in other embodiments without departing from the spirit or scope of the present invention. Thus, the present invention is not intended to be limited to the embodiments shown herein but is to be accorded the widest scope consistent with the principles and novel features disclosed herein.

Claims

1. An oil-water-solid-gas four-phase separation device, characterized in that, Comprising: Separator; The top of the separator is provided with a gas phase outlet, the upper part is provided with an oil phase outlet, the lower part is provided with a water phase outlet, and the bottom is provided with a solid phase outlet; valves are respectively provided at the gas phase outlet, the oil phase outlet, the water phase outlet and the solid phase outlet; A plurality of salt slurry receiving tanks respectively connected to the solid phase outlet; a feed cut-off valve is provided between each salt slurry receiving tank and the solid phase outlet, a liquid supplement port, a stirring device and a density measuring device are provided at the top, and a discharge port is provided at the bottom; A salt slurry pump respectively connected to the discharge port of each salt slurry receiving tank; a discharge cut-off valve is provided between the salt slurry pump and the discharge port of each salt slurry receiving tank; the salt slurry pump is connected to a salt slurry separation device.

2. The oil-water-solid-gas four-phase separation device according to claim 1, wherein The upper part of the separator is cylindrical and the lower part is conical; the water phase outlet is arranged at the contact position between the upper and lower parts of the separator.

3. The oil-water-solid-gas four-phase separation device according to claim 1, characterized in that, The water phase outlet is connected to a mother liquor receiving tank through a water phase pipeline; the water phase pipeline includes a water phase outlet pipe communicated with the water phase outlet and a water phase overflow pipe communicated with the water phase outlet pipe; the water phase outlet pipe is arranged obliquely upward and forms a certain angle with the cylinder body of the separator, and the water phase overflow pipe is arranged parallel to the cylinder body of the separator; an overflow port with a height lower than that of the oil phase outlet is provided on the water phase overflow pipe; the overflow port is connected to the mother liquor receiving tank.

4. The oil-water-solid-gas four-phase separation device according to claim 3, characterized in that, The water phase outlet pipe forms an angle of ≤45° with the cylinder body of the separator.

5. The oil-water-solid-gas four-phase separation device according to claim 3, wherein The gas phase outlet is connected to a condensate receiving tank through a gas phase balance pipe; the top of each salt slurry receiving tank and the top of the water phase overflow pipe are respectively connected to the gas phase balance pipe through pipelines.

6. The oil-water-solid-gas four-phase separation device according to claim 5, wherein The gas phase outlet is connected to the inlet of an organic gas condenser through a gas phase balance pipe; the outlet of the organic gas condenser is connected to the condensate receiving tank; The oil phase outlet is connected to the inlet of an oil phase outlet heat exchanger through a pipeline; the outlet of the oil phase outlet heat exchanger is connected to an oil phase receiving tank.

7. The oil-water-solid-gas four-phase separation device according to claim 1, wherein The separator is provided with a distributor; the distributor penetrates through the top of the separator and inserts into the separator, a feed inlet is provided at the upper part, and a discharge hole is provided at the lower side.

8. The oil-water-solid-gas four-phase separation device according to claim 7, wherein, The position where the distributor inserts into the separator is the 2 / 3 position of the separator from top to bottom; the height of the bottom of the distributor is lower than the height of the oil phase outlet and higher than the height of the water phase outlet.

9. The oil-water-solid-gas four-phase separation device according to claim 1, wherein, The solid phase outlet is respectively connected to two salt slurry receiving tanks through pipelines; the two salt slurry receiving tanks are respectively a first salt slurry receiving tank and a second salt slurry receiving tank; The first salt slurry receiving tank is provided with a first liquid supplement port, a first stirrer and a first density meter at the top, and a first discharge port at the bottom; the first salt slurry receiving tank is connected to the solid phase outlet through a first feed cut-off valve; the first discharge port is connected to the salt slurry pump through a first discharge cut-off valve; The second salt slurry receiving tank is provided with a second liquid supplement port, a second stirrer and a second density meter at the top, and a second discharge port at the bottom; the second salt slurry receiving tank is connected to the solid phase outlet through a second feed cut-off valve; the second discharge port is connected to the salt slurry pump through a second discharge cut-off valve; The first densitometer is interlocked with the first feed cut-off valve, the second feed cut-off valve, and the first discharge cut-off valve respectively; the second densitometer is interlocked with the second feed cut-off valve, the first feed cut-off valve, and the second discharge cut-off valve respectively.

10. A method for separating oil, water, solid and gas, characterized in that, It includes the following steps: Using the oil-water-solid-gas four-phase separation device according to any one of claims 1 to 9, first fill each salt slurry receiving tank with the aqueous phase; then send the mixed liquid material containing oil, water, solid, and gas into the separator for stratification. After stratification, while continuously sending the mixed liquid material containing oil, water, solid, and gas into the separator, discharge the volatile gas from the gas phase outlet, send it to the condensate receiving tank after condensation, discharge the oil phase from the oil phase outlet, send it to the oil phase receiving tank after condensation, discharge the saturated salt solution from the aqueous phase outlet, send it to the mother liquor receiving tank, alternately discharge the salt slurry from the solid phase outlet into each salt slurry receiving tank, and alternately send the salt slurry from each salt slurry receiving tank to the salt slurry separation equipment through the salt slurry pump to separate the salt slurry.

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