CN111471482A - Method for dehydrating high-emulsification sump oil and device adopted by method - Google Patents
Method for dehydrating high-emulsification sump oil and device adopted by method Download PDFInfo
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- CN111471482A CN111471482A CN202010312190.6A CN202010312190A CN111471482A CN 111471482 A CN111471482 A CN 111471482A CN 202010312190 A CN202010312190 A CN 202010312190A CN 111471482 A CN111471482 A CN 111471482A
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- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10G—CRACKING HYDROCARBON OILS; PRODUCTION OF LIQUID HYDROCARBON MIXTURES, e.g. BY DESTRUCTIVE HYDROGENATION, OLIGOMERISATION, POLYMERISATION; RECOVERY OF HYDROCARBON OILS FROM OIL-SHALE, OIL-SAND, OR GASES; REFINING MIXTURES MAINLY CONSISTING OF HYDROCARBONS; REFORMING OF NAPHTHA; MINERAL WAXES
- C10G33/00—Dewatering or demulsification of hydrocarbon oils
- C10G33/04—Dewatering or demulsification of hydrocarbon oils with chemical means
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- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10G—CRACKING HYDROCARBON OILS; PRODUCTION OF LIQUID HYDROCARBON MIXTURES, e.g. BY DESTRUCTIVE HYDROGENATION, OLIGOMERISATION, POLYMERISATION; RECOVERY OF HYDROCARBON OILS FROM OIL-SHALE, OIL-SAND, OR GASES; REFINING MIXTURES MAINLY CONSISTING OF HYDROCARBONS; REFORMING OF NAPHTHA; MINERAL WAXES
- C10G2300/00—Aspects relating to hydrocarbon processing covered by groups C10G1/00 - C10G99/00
- C10G2300/10—Feedstock materials
- C10G2300/1003—Waste materials
- C10G2300/1007—Used oils
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Abstract
The invention discloses a method for dehydrating high-emulsification sump oil, which comprises the following steps: injecting the high-emulsified sump oil and a demulsifier into a jet-static mixer for full contact mixing to obtain an oil-water mixture after preliminary separation; and injecting the primarily separated oil-water mixture into a high-efficiency separator for gravity settling separation or coalescence separation to obtain the sump oil and the wastewater with the water content meeting the requirements. The invention also discloses a device adopted by the method for dehydrating the high-emulsification sump oil. Aiming at the problems of large production amount of refinery sump oil, high water content of the sump oil, huge sump oil storage pressure caused by the refinery, difficult sump oil recycling and the like, the invention develops a set of separation device integrated by a jet-static mixer and a high-efficiency separator based on the demulsification and coalescence settling principle, realizes the high-efficiency removal of water in the sump oil, simplifies the separation device while ensuring the qualification of final products, and realizes the resource utilization of the water-containing sump oil.
Description
Technical Field
The invention belongs to the technical field of chemical industry, and particularly relates to a method for dehydrating high-emulsification sump oil and a device adopted by the method.
Background
The refinery can produce dirty oil in normal production and abnormal production processes, such as device startup and shutdown, equipment maintenance, machine pump switching, coking coke cooling water tank cutting oil and the like. The components are also particularly complex due to the fact that the number of the parts generated by the dirty oil is large: has lighter gasoline component and heavier residual oil component. In addition, the dirty oil has the characteristics of high colloid content, high asphaltene content, strong emulsifying capacity, high impurity content, serious aging degree and the like. The impurities in the dirty oil come from drilling mud, fracturing fluid, sewage treatment agent, flocculant, coagulant, scale inhibitor, corrosion inhibitor, bactericide, caustic soda and the like, and the recovered oil contains more water and flocculent organic sludge and is not beneficial to re-refining. The dirty oil is usually conveyed to a normal-pressure storage tank for storage, and is recycled after water is cut, but the water content in the dirty oil is still not lower than 40% after standing and layering. At present, a refinery generally sends sump oil after water cutting to a delayed coking or atmospheric and vacuum device for recycling, but only a part of the sump oil can be recycled due to high water content of the sump oil, and the rest of the sump oil can still be stored in a storage tank, which causes huge sump oil storage pressure for the refinery. In addition, generally, the water content of the recycled dirty oil must be lower than 10%, and if the recycled dirty oil with the water content higher than 10%, a large amount of energy consumption is consumed, and the safe and stable production of various sets of devices upstream and downstream of the whole plant is affected. How to remove the water in the dirty oil and recycle the dirty oil is a difficult problem which always troubles refineries.
The existing oil-water separation technology mainly comprises a gravity settling method, a membrane separation method, a filtration method, a flotation method, an ultrasonic separation method, a cyclone separation method, a chemical demulsification method, an electric flocculation method and the like. The gravity settling method has large occupied area, long treatment time and poor separation effect on the water-containing dirty oil with serious emulsification; the membrane separation method has low energy consumption, convenient operation and compact structure, but has limited stability and heat resistance, high cost and is uneconomical; the filtration method has high power consumption, easy blockage and general separation effect; the flotation method has the advantages of large device treatment capacity, small sludge production amount, high separation efficiency and the like, but has the defects of long retention time, trouble in device manufacture and maintenance, high energy consumption and the like; the ultrasonic separation method has the defects of high energy consumption, limited actual operation effect and the like; the cyclone separation method has the advantages of simple structure, convenient operation, easy maintenance and the like, but because the water-containing dirty oil is seriously emulsified and the density difference between the oil and the water is not large, the actual cyclone separation effect is limited; the chemical demulsification method has the advantages of small one-time investment, simple process equipment, low power consumption and comprehensive treatment cost, poor adaptability to raw materials and limited effect. The electric flocculation method has the advantages of simple operation, high separation speed and the like, but has high energy consumption and high operation cost. In summary, the existing methods have some inevitable disadvantages.
Therefore, there is a strong need in the art to develop a method and apparatus for dewatering highly emulsified dirty oil.
Disclosure of Invention
It is a first object of the present invention to provide a method for dehydrating highly emulsified dirty oil. The invention aims to solve the technical problem that the production amount of the sump oil of a refinery is large, the water content of the sump oil is not lower than 40%, at present, the sump oil is usually sent to a delayed coking device or an atmospheric and vacuum device for recycling by the refinery, but only a part of the sump oil can be recycled due to high water content of the sump oil, and the rest of the sump oil can still be stored, so that huge sump oil storage pressure is caused for the refinery. Generally, the water content of the recycled dirty oil must be lower than 10%, and if the recycled dirty oil with the water content higher than 10%, a large amount of energy consumption is consumed, and the safe and stable production of various sets of devices upstream and downstream of the whole plant is affected. Therefore, dewatering of the dirty oil becomes necessary.
The second purpose of the invention is to provide a device used in the method for dehydrating the high-emulsification dirty oil.
In order to achieve the purpose, the technical scheme adopted by the invention is as follows:
in a first aspect of the present invention, there is provided a method for dewatering highly emulsified dirty oil, comprising the steps of:
injecting the high-emulsified sump oil and a demulsifier into a jet-static mixer for full contact mixing to obtain an oil-water mixture after preliminary separation; and injecting the primarily separated oil-water mixture into a high-efficiency separator for gravity settling separation or coalescence separation to obtain the sump oil and the wastewater with the water content meeting the requirements.
The water content of the high emulsified sump oil is not less than 40 percent, and the density is 900-990Kg/m3The oil is composed of crude oil, lubricating oil, engine oil, silt, organic sludge, surface active substances and water, and the dirty oil is seriously emulsified and generally exists in a W/O or O/W/O type emulsion at normal temperature.
The inlet flow of the high-emulsification sump oil is 0-2 m3/h。
The flow ratio of the high-emulsification sump oil to the demulsifier is 20: 1-100: 1.
The parameters of the jet-static mixer were set as: the pressure drop is 0.01-0.1 MPa, the temperature is 10-30 ℃, and the flow rate is 0.01-0.5 m/s.
The demulsifier is a high molecular weight polyether demulsifier obtained by multiple modifications. Firstly, ethylene oxide and propylene oxide block polyether demulsifier using tetraethylenepentamine as initiator is synthesized. Then, 2, 4-diisocyanatomethyl phenyl is used as a cross-linking agent to carry out cross-linking modification on the demulsifier, so that the molecular chain length is increased, and the high-efficiency demulsifier with high branching degree and higher molecular weight is generated. Finally, hydrogen-containing silicone oil is used as a molecular skeleton to graft and modify the demulsifier, so that the molecular weight of the demulsifier is improved, the original skeleton of the demulsifier is changed, and the novel high-efficiency demulsifier with high molecular weight is finally synthesized. The demulsifier has the characteristics of low demulsification temperature, high water yield speed and the like.
The molecular weight of the demulsifier is 3600-48000 g/mol.
The preparation method of the demulsifier comprises the following steps:
firstly, adding tetraethylenepentamine and an alkaline catalyst (sodium hydroxide) into a high-temperature reaction kettle, sealing the reaction kettle, purging and replacing the reaction kettle by nitrogen, vacuumizing the reaction kettle, repeating the operation at least twice, starting stirring, heating to 130-160 ℃, adding propylene oxide, controlling the reaction temperature and pressure (controlling the reaction temperature to be not more than 140 ℃ and the pressure to be not more than 0.5MPa), reacting until the pressure in the kettle is 0MPa, adding ethylene oxide, controlling the reaction temperature and pressure (controlling the reaction temperature to be not more than 150 ℃ and the pressure to be not more than 0.5MPa), reacting until the pressure in the kettle is 0MPa, heating to 140 ℃, adding propylene oxide, controlling the reaction temperature and pressure (controlling the reaction temperature to be not more than 150 ℃ and the pressure to be not more than 0.5MPa), reacting until the pressure in the kettle is 0MPa, continuing to react for 60-80min, cooling, opening the kettle, and discharging to obtain the ethylene oxide and propylene oxide block polyether demulsifier A;
based on the total weight of tetraethylenepentamine, propylene oxide and ethylene oxide, the tetraethylenepentamine accounts for 0.5-1% of the total weight, the first propylene oxide accounts for 24-29.5% of the total weight, the second propylene oxide accounts for 25-30% of the total weight, the ethylene oxide accounts for 40-50% of the total weight, and the alkaline catalyst accounts for 0.5-2% of the total weight;
secondly, under the action of a catalyst (dodecyl benzene sulfonic acid), performing self-crosslinking reaction on polycarboxylic acid (oxalic acid) and an ethylene oxide and propylene oxide block polyether demulsifier A to obtain a product B;
the ethylene oxide and propylene oxide block polyether demulsifier A accounts for 96.5 to 99 percent of the total weight, the polycarboxylic acid accounts for 1 to 3.5 percent of the total weight, and the catalyst accounts for 0.01 to 0.1 percent of the total weight; the reaction temperature is 60-80 ℃;
thirdly, performing a crosslinking reaction on the ethylene oxide and propylene oxide block polyether demulsifier A and the product B in a solvent (toluene) by using 2, 4-toluene diisocyanate as a crosslinking agent to obtain a product C;
the ethylene oxide and propylene oxide block polyether demulsifier A accounts for 25-45% of the total weight, the product B accounts for 55-75% of the total weight, the solvent dosage is 0.5-2.5 times of the total weight, and 2, 4-diisocyanate toluene is 0.5-5% of the total weight; the reaction temperature is 60-80 ℃;
fourthly, mixing the product C with hydrogen-containing silicone oil for reaction to obtain a demulsifier D;
the mass ratio of the hydrogen-containing silicone oil to the product C is (1-6): 100, and the reaction temperature is 60-80 ℃.
The parameters of the high-efficiency separator are set as follows: the pressure drop is 0.01-0.15 MPa, and the temperature is 10-30 ℃.
The dirty oil with the water content meeting the requirement is processed by demulsification and coalescence settling, and the water content of the separated product dirty oil is not higher than 0.3 percent.
The second aspect of the invention provides a device adopted by the method for dehydrating the high emulsified sump oil, which consists of a jet flow-static mixer, a high-efficiency separator and a high-pressure jet flow system, wherein one end of the outside of the jet flow-static mixer is provided with a high emulsified sump oil inlet and a demulsifier inlet, and the other end of the outside of the jet flow-static mixer is provided with a mixture outlet; the jet flow-static mixer consists of a dumbbell-shaped shell, nozzles and corrugated plate fillers, wherein the number of the nozzles is 3, the nozzles are positioned in the dumbbell-shaped shell and are adjacent to a high-emulsification sump oil inlet, and the nozzles are distributed annularly at intervals of 120 degrees; the corrugated plate packing is provided with 3 sections in total, one section is close to the spray nozzle, the middle section is positioned at the middle section of the dumbbell-shaped shell, and the three sections are positioned inside the other end of the dumbbell-shaped shell; one end of the high-efficiency separator is provided with a mixture inlet, and the other end of the high-efficiency separator is provided with a sump oil outlet and a waste water outlet; the mixture inlet is connected with the mixture outlet of the jet-static mixer; the high-pressure jet system is formed by sequentially connecting a high-pressure pump, a pressure regulating valve, a pressure stabilizing tank, a stop valve and a pressure gauge; the pressure gauge is connected with a nozzle inside the jet flow-static mixer.
The distance between the nozzle and the corrugated plate filler is 3-5% of the total length of the jet-static mixer.
The distance between the adjacent corrugated plate fillers is 5 to 8 percent of the total length of the jet-static mixer.
The corrugated plate filler adopts a metal corrugated plate as the filler, and the length of each section of filler is 15-20% of the total length of the jet-static mixer.
The corrugated plate filler is a filler which takes stainless steel wires as a framework and is woven into an omega-shaped structure by combining polytetrafluoroethylene fibers, a filler which takes stainless steel wires as a framework and is woven into an X-shaped structure by combining the polytetrafluoroethylene fibers, and a filler which takes the stainless steel wires as a framework and is woven into a double X-shaped structure by combining the polytetrafluoroethylene fibers.
The corrugation angle of the adjacent corrugated plates and the axis of the longitudinal pipe are symmetrically distributed, and the corrugated plates of the connected mixing units rotate by 90 degrees. When fluid flows into the corrugated plate filling material, the fluid is firstly divided into a plurality of strands by the corrugated plates, then each strand of fluid is mixed and flows in two vertical directions in a channel formed by two adjacent corrugated plates or the corrugated plates and the wall surface, and the fluid rotates by 90 degrees and enters the second layer unit after flowing through the first layer mixing unit. In general, the fluid flows in three dimensions in the corrugated sheet packing. In the process, the fluid is divided, shifted and overlapped for multiple times, and finally the aim of uniform mixing is fulfilled.
The dumbbell-shaped shell is large at two ends and small in the middle and is similar to a dumbbell in shape. Based on the principle of reducing and increasing the speed, the flow velocity of the area with the suddenly reduced diameter of the mixer is suddenly increased, when the flow velocity is increased to be large, the flow line is not clearly distinguished any more, a plurality of small vortexes exist in the flow field, laminar flow is damaged, and adjacent flow layers not only slide but also are mixed. At the moment, the flowing state of the liquid is changed from laminar flow to turbulent flow, and the mixing effect of the water-containing sump oil and the novel demulsifier is greatly improved.
The nozzle is a Gaussian nozzle which has the characteristics of high jet velocity, low turbulent flow dissipation and low pressure, and the demulsifier can be sprayed out along a fixed direction in a high-speed jet shape. The jet flow has the important characteristic of entraining peripheral fluid, in the jet flow mixing process, the fast moving fluid (i.e. jet flow) is jetted into the slow flowing fluid (i.e. main flow), at the jet flow boundary, because the speed difference between the jet flow and the main flow forms discontinuous sections, once the discontinuous sections are disturbed, the discontinuous sections lose stability and generate vortex, the vortex entraining peripheral fluid enters the jet flow, and simultaneously, the continuous movement, deformation and division generate turbulent motion to form an inner and outer freely turbulent mixing layer. The mixing effect of the novel demulsifier and the water-containing sump oil is further enhanced in the entrainment and turbulence processes.
The flow velocity of jet flow in the nozzle is 0-100 m/s; the pressure is 0-140 MPa;
the high-pressure pump is used for generating high pressure required by jet flow, the pressure range is 0-140 MPa, and the jet flow has high speed and high energy at an outlet.
The pressure regulating valve may regulate a pressure of a fluid.
The pressure stabilizing tank is used for stabilizing the pressure of the pulsating fluid.
The jet flow-static mixer adopts a horizontal type or a vertical type according to actual requirements.
The efficient separator adopts a coalescence separator, and adopts single stage or multiple stages according to actual requirements.
Due to the adoption of the technical scheme, the invention has the following advantages and beneficial effects:
the method for dehydrating the high-emulsification sump oil adopts the novel demulsifier which has the characteristics of low demulsification temperature, high water yield, high water outlet speed and the like.
Aiming at the problems of large production amount of dirty oil of a refinery, high water content of the dirty oil, huge dirty oil storage pressure caused by the refinery, difficult recycling of the dirty oil and the like, the invention develops a set of separation device integrated by a jet-static mixer and a high-efficiency separator based on the principle of demulsification and coalescence sedimentation, realizes the high-efficiency removal of water in the dirty oil, simplifies the separation device while ensuring the qualification of final products, and realizes the resource utilization of the water-containing dirty oil.
Drawings
FIG. 1 is a schematic view of an apparatus used in the method for dehydrating highly emulsified contaminated oil according to the present invention.
Wherein, 1 is a jet flow-static mixer, 11 is a high emulsified sump oil inlet, 12 is a demulsifier inlet, 13 is a mixture outlet, 14 is a dumbbell-shaped shell, 15 is a nozzle, 16 is corrugated plate filler, 2 is a high-efficiency separator, 21 is a mixture inlet, 22 is a sump oil outlet, 23 is a wastewater outlet, 3 is a high-pressure jet system, 31 is a high-pressure pump, 32 is a pressure regulating valve, 33 is a pressure stabilizing tank, 34 is a stop valve, and 35 is a pressure gauge.
Fig. 2 is a front view and a partial cross-sectional view of a nozzle in the apparatus of fig. 1.
Fig. 3 is a front and left side view of the corrugated board packing in the apparatus of fig. 1.
Detailed Description
In order to more clearly illustrate the invention, the invention is further described below in connection with preferred embodiments. It is to be understood by persons skilled in the art that the following detailed description is illustrative and not restrictive, and is not to be taken as limiting the scope of the invention.
FIG. 1 is a schematic view of an apparatus used in the method for dehydrating highly emulsified contaminated oil according to the present invention. As shown in figure 1, when the device works, the water-containing dirty oil is slowly injected into the jet flow-static mixer 1, the novel demulsifier is introduced into the high-pressure jet flow system 3 for pressurization and acceleration, and the high-speed high-pressure jet flow is formed through the nozzle 15 and is injected into the jet flow-static mixer 1. The water-containing sump oil is fully contacted and mixed with the novel demulsifier by utilizing the entrainment effect of jet flow. Because the novel demulsifier has large molecular weight, more branched chains and annular structures can adsorb and agglomerate liquid drops, the liquid drops are close to each other and agglomerate to realize demulsification, and an oil-water mixture after preliminary separation is obtained. The primarily separated oil-water mixture is injected into a high-efficiency separator 2 for gravity settling separation or coalescence separation, dispersed phase droplets in the fluid are subjected to coalescence process under the interception and inertial collision of fiber filler, the small droplets are gradually coalesced and grown into large droplets, and then the large droplets are subjected to enhanced settling separation. And the sump oil obtained after separation flows out from a light phase outlet of the high-efficiency separator 2 and enters a downstream for subsequent processes, and the wastewater is discharged from a heavy phase outlet of the high-efficiency separator 2.
The device adopted by the method for dehydrating the high-emulsification sump oil comprises a jet flow-static mixer 1, a high-efficiency separator 2 and a high-pressure jet flow system 3, wherein one end of the outside of the jet flow-static mixer 1 is provided with a high-emulsification sump oil inlet 11 and a demulsifier inlet 12, and the other end of the outside of the jet flow-static mixer 1 is provided with a mixture outlet 13; the jet flow-static mixer 1 consists of a dumbbell-shaped shell 14, nozzles 15 and corrugated plate fillers 16, wherein the number of the nozzles 15 is 3, the number of the nozzles 15 is positioned in the dumbbell-shaped shell 14 and is adjacent to a high-emulsification sump oil inlet 11, and the nozzles 15 are distributed annularly at intervals of 120 degrees; the corrugated plate packing 16 is provided with 3 sections in total, one section is close to the nozzle 15, the middle section is positioned at the middle section of the dumbbell-shaped shell 14, and the three sections are positioned inside the other end of the dumbbell-shaped shell 14; one end of the high-efficiency separator 2 is provided with a mixture inlet 21, and the other end is provided with a sump oil outlet 22 and a waste water outlet 23; the mixture inlet 21 is connected to the mixture outlet 13 of the jet-static mixer 1; the high-pressure jet system 3 is formed by sequentially connecting a high-pressure pump 31, a pressure regulating valve 32, a pressure stabilizing tank 33, a stop valve 34 and a pressure gauge 35; the pressure gauge 35 is connected to the nozzle 15 inside the jet-static mixer 1.
The flow velocity of jet flow in the nozzle 15 is 0-100 m/s; the pressure is 0-140 MPa; as shown in fig. 2, fig. 2 is a front view and a partial sectional view of the nozzle 15 in the apparatus shown in fig. 1.
The distance between the nozzle 15 and the corrugated plate packing 16 is 3% to 5% of the total length of the jet-static mixer 1.
The distance between the adjacent corrugated board packings 16 is 5% -8% of the total length of the jet-static mixer 1.
The corrugated plate filler 16 is a filler which is formed by weaving stainless steel wires serving as a framework and polytetrafluoroethylene fibers into an omega-shaped structure, a filler which is formed by weaving stainless steel wires serving as a framework and polytetrafluoroethylene fibers into an X-shaped structure, and a filler which is formed by weaving stainless steel wires serving as a framework and polytetrafluoroethylene fibers into a double X-shaped structure.
The corrugated plate packing 16 adopts a metal corrugated plate as packing, and the length of each section of packing is 15-20% of the total length of the jet-static mixer 1. As shown in fig. 3, fig. 3 is a front view and a left side view of the corrugated board packing in the apparatus shown in fig. 1.
The corrugation in the corrugated plate packing 16 forms 45 degrees with the axis of the longitudinal pipe, the inclination angle of the corrugation of the adjacent corrugated plates is symmetrically distributed with the axis of the longitudinal pipe, and the corrugated plates of the connected mixing units rotate 90 degrees. When the fluid flows into the corrugated plate packing 16, the fluid is firstly divided into a plurality of strands by the corrugated plates, then each strand of fluid is mixed and flows in two vertical directions in a channel formed by two adjacent corrugated plates or the corrugated plates and the wall surface, and the fluid rotates 90 degrees to enter a second layer unit after flowing through a layer of mixing unit. In general, the fluid flows in three dimensions in the corrugated sheet packing 16. In the process, the fluid is divided, shifted and overlapped for multiple times, and finally the aim of uniform mixing is fulfilled.
The dumbbell-shaped shell 14 is large at two ends and small in the middle and is shaped like a dumbbell. Based on the principle of reducing and increasing the speed, the flow velocity of the area with the suddenly reduced diameter of the mixer is suddenly increased, when the flow velocity is increased to be large, the flow line is not clearly distinguished any more, a plurality of small vortexes exist in the flow field, laminar flow is damaged, and adjacent flow layers not only slide but also are mixed. At the moment, the flowing state of the liquid is changed from laminar flow to turbulent flow, and the mixing effect of the water-containing sump oil and the novel demulsifier is greatly improved.
The nozzle 15 is a gaussian nozzle which has the characteristics of high jet velocity, low turbulent flow dissipation and low pressure, and the demulsifier can be sprayed out along a fixed direction in a high-speed high-pressure jet shape. The jet flow has the important characteristic of entraining peripheral fluid, in the jet flow mixing process, the fast moving fluid (i.e. jet flow) is jetted into the slow flowing fluid (i.e. main flow), at the jet flow boundary, because the speed difference between the jet flow and the main flow forms discontinuous sections, once the discontinuous sections are disturbed, the discontinuous sections lose stability and generate vortex, the vortex entraining peripheral fluid enters the jet flow, and simultaneously, the continuous movement, deformation and division generate turbulent motion to form an inner and outer freely turbulent mixing layer. The mixing effect of the novel demulsifier and the water-containing sump oil is further enhanced in the entrainment and turbulence processes.
The high-pressure pump 31 is used for generating high pressure required by jet flow, and the high pressure is 0-140 MPa, so that the jet flow has high speed and high energy at an outlet.
The pressure regulating valve 32 can regulate the pressure of the fluid.
The surge tank 33 is for stabilizing the pulsating fluid.
The jet flow-static mixer 1 adopts a horizontal type or a vertical type according to actual requirements.
The high-efficiency separator 2 adopts a coalescence separator, and the high-efficiency separator 2 adopts a single stage or multiple stages according to actual requirements.
The method for dehydrating the high-emulsification sump oil in the embodiment of the invention comprises the following steps: the high-emulsified sump oil enters the jet flow-static mixer 1 through the high-emulsified sump oil inlet 11, the demulsifier firstly boosts and accelerates through the high-pressure jet flow system 3, and then sequentially boosts and accelerates through the high-pressure pump 31, regulates the pressure through the pressure regulating valve 32, stabilizes the pressure through the pressure stabilizing tank 33, the stop valve 34 and the pressure gauge 35 enter the nozzle 15, a jet flow with extremely high energy is formed in the nozzle 15, the flow rate of the jet flow is 0-100 m/s, and the pressure is 0-140 MPa. The jet then enters the jet-static mixer 1 through the breaker inlet 12. The nozzle 15 can spray the emulsion breaker in a "high-speed high-pressure jet" shape along a fixed direction. The jet flow has the important characteristic of entraining peripheral fluid, in the jet flow mixing process, the fast moving fluid (i.e. jet flow) is jetted into the slow flowing fluid (i.e. main flow), at the jet flow boundary, because the speed difference between the jet flow and the main flow forms discontinuous sections, once the discontinuous sections are disturbed, the discontinuous sections lose stability and generate vortex, the vortex entraining peripheral fluid enters the jet flow, and simultaneously, the continuous movement, deformation and division generate turbulent motion to form an inner and outer freely turbulent mixing layer. The mixing effect of the novel demulsifier and the water-containing sump oil is further enhanced in the entrainment and turbulence processes. Then sequentially passes through 3 sections of corrugated plate packings 16, the corrugation in the corrugated plate packings 16 forms 45 degrees with the axial line of the longitudinal pipe, the inclination angles of the corrugations of adjacent corrugated plates are symmetrically distributed with the axial line of the longitudinal pipe, and the corrugated plates of the connected mixing units rotate 90 degrees. When the fluid flows into the corrugated plate packing 16, the fluid is firstly divided into a plurality of strands by the corrugated plates, then each strand of fluid is mixed and flows in two vertical directions in a channel formed by two adjacent corrugated plates or the corrugated plates and the wall surface, and the fluid rotates 90 degrees to enter a second layer unit after flowing through a layer of mixing unit. In general, the fluid flows in three dimensions in the corrugated sheet packing 16. In the process, the fluid is divided, shifted and overlapped for multiple times, and finally the aim of uniform mixing is fulfilled. And finally, the mixture leaves the jet-static mixer 1 through a mixture outlet 13 arranged at the other end outside the jet-static mixer 1 and enters the high-efficiency separator 2 through a mixture inlet 21, the high-efficiency separator 2 performs gravity settling separation or coalescence separation on the primarily separated oil-water mixture, dirty oil with the water content meeting the requirement is discharged through a dirty oil outlet 22, and wastewater is discharged through a wastewater outlet 23.
Example 1
The method and the device are adopted by a certain Wuhan refinery to dehydrate the sump oil after water is cut in the normal-pressure storage tank.
1. Conditions of the experiment
Materials: the water-containing dirty oil (the water content is about 42 percent) mainly comprises engine oil, lubricating oil and water, is seriously emulsified and generally exists in a W/O form at normal temperature. The density is 925Kg/m3The demulsifier adopts a novel demulsifier.
The preparation method of the demulsifier comprises the following steps:
firstly, adding 6g of tetraethylenepentamine and 10g of basic catalyst (sodium hydroxide) into a high-temperature reaction kettle, sealing the reaction kettle, purging and replacing the reaction kettle by nitrogen, vacuumizing the reaction kettle again, repeating the operation at least twice, starting stirring, stopping heating when the temperature is raised to 130 ℃, opening a feed valve, adding 255g of propylene oxide, controlling the reaction temperature to be not more than 140 ℃ and the pressure to be not more than 0.5MPa, and reacting until the pressure in the reaction kettle is 0 MPa. Then heating to 130 ℃, adding 470g of ethylene oxide, controlling the reaction temperature not to exceed 150 ℃ and the pressure not to exceed 0.5MPa, and reacting until the pressure in the kettle is 0 MPa. Finally, heating to 140 ℃, adding 269g of propylene oxide, controlling the reaction temperature to be not more than 150 ℃ and the pressure to be not more than 0.5MPa, reacting until the pressure in the kettle is 0MPa, and continuing to react for 60 min. After the reaction is finished, cooling, opening the kettle and discharging to obtain an ethylene oxide and propylene oxide block polyether demulsifier A taking tetraethylenepentamine as an initiator;
and secondly, adding 975g of ethylene oxide and propylene oxide block polyether demulsifier A into a high-temperature reaction kettle (HT-FJ series, Shanghai Huitong laboratory instruments Co., Ltd.), adding 25g of oxalic acid and 0.6g of dodecylbenzenesulfonic acid, heating, controlling the reaction temperature to be 60-80 ℃, reacting for 1.5 hours, vacuumizing for 1 hour, and filtering to obtain a product B for later use.
Thirdly, 1500g of toluene is added into a high-temperature reaction kettle (HT-FJ series, Shanghai Huitong laboratory instruments Co., Ltd.), 300g of the prepared ethylene oxide and propylene oxide block polyether demulsifier A and 700g of the product B are added, the temperature is raised by heating, the reaction temperature is controlled to be 60-80 ℃, 10g of 2, 4 toluene diisocyanate is slowly dripped, after the dripping is finished, the product C is prepared by filtering after the reaction is carried out for 1 hour, and the product C is reserved.
And fourthly, adding the product C100g and 3g of hydrogen-containing silicone oil into a high-temperature reaction kettle (HT-FJ series, Shanghai Huitong laboratory instruments Co., Ltd.), heating and raising the temperature, controlling the reaction temperature to be 60-80 ℃, and maintaining for 1.5 hours to enable the mixture to fully react, thereby finally obtaining the target product, namely the novel demulsifier D.
Equipment parameters: in the device, a jet flow-static mixer 1 uses a nozzle 15 (shown in figure 2) to inject demulsifier, an internal part uses metal corrugated plate filler (shown in figure 3), and a high-efficiency separator 2 adopts a coalescence separator (the filler uses stainless steel wires as a framework and is combined with polytetrafluoroethylene fibers to be woven into an omega-shaped structure).
The operating parameters are as follows: the inlet flow of the water-containing dirty oil is 1.5m3Per h, flow of demulsifier injected is 0.03m3The pressure drop of the jet flow-static mixer 1 is controlled to be about 0.07MPa, the temperature is 15 ℃, and the flow speed is 0.25 m/s; the pressure drop of the high-efficiency separator 2 is about 0.12MPa, and the temperature is 15 ℃.
Content determination: the water content was determined using a karl fischer moisture meter.
2. Process flow
Injecting the high-emulsified sump oil and a demulsifier into a jet-static mixer for full contact mixing to obtain an oil-water mixture after preliminary separation; and injecting the primarily separated oil-water mixture into a high-efficiency separator for gravity settling separation or coalescence separation to obtain the sump oil and the wastewater with the water content meeting the requirements.
3. Application results
After the treatment by the method and the device, the water content of the product sump oil is lower than 0.25 percent, and the requirement of a downstream production process is met.
Example 2
The method and the device are adopted by a certain Hainan chemical plant to dehydrate a large amount of water-containing dirty oil generated in the processes of offshore oil and gas field exploitation and chemical production.
1. Conditions of the experiment
Materials: the water-containing dirty oil (the water content is about 46 percent) mainly comprises crude oil, lubricating oil, silt and water, is seriously emulsified and generally exists in the form of O/W/O type emulsion at normal temperature. The density is 946Kg/m3The demulsifier adopts a novel demulsifier.
The preparation method of the demulsifier comprises the following steps:
firstly, adding 8g of tetraethylenepentamine and 15g of basic catalyst (sodium hydroxide) into a high-temperature reaction kettle, sealing the reaction kettle, purging and replacing the reaction kettle by nitrogen, vacuumizing the reaction kettle again, repeating the operation at least twice, starting stirring, stopping heating when the temperature is raised to 130 ℃, opening a feed valve, adding 272g of propylene oxide, controlling the reaction temperature to be not more than 140 ℃ and the pressure to be not more than 0.5MPa, and reacting until the pressure in the reaction kettle is 0 MPa. Then heating to 130 ℃, adding 450g of ethylene oxide, controlling the reaction temperature not to exceed 150 ℃ and the pressure not to exceed 0.5MPa, and reacting until the pressure in the kettle is 0 MPa. And finally, heating to 140 ℃, adding 270g of propylene oxide, controlling the reaction temperature to be not more than 150 ℃ and the pressure to be not more than 0.5MPa, reacting until the pressure in the kettle is 0MPa, and continuing to react for 1 hour. After the reaction is finished, cooling, opening the kettle and discharging to obtain an ethylene oxide and propylene oxide block polyether demulsifier A taking tetraethylenepentamine as an initiator;
and secondly, adding 985g of ethylene oxide and propylene oxide block polyether demulsifier A into a high-temperature reaction kettle, adding 15g of oxalic acid and 0.8g of dodecylbenzenesulfonic acid, heating, controlling the reaction temperature to be 60-80 ℃, reacting for 1.5 hours, vacuumizing for 1 hour, and filtering to obtain a product B for later use.
And thirdly, adding 2000g of toluene into a high-temperature reaction kettle, adding 400g of the prepared ethylene oxide and propylene oxide block polyether demulsifier A and 600g of the product B, heating to raise the temperature, controlling the reaction temperature to be 60-80 ℃, slowly dropwise adding 25g of 2, 4 toluene diisocyanate, finishing dropwise adding, reacting for 1 hour, and filtering to prepare a product C for later use.
And fourthly, adding the product C100g and 4g of hydrogen-containing silicone oil into a high-temperature reaction kettle, heating to raise the temperature, controlling the reaction temperature to be 60-80 ℃, and maintaining for 1.5 hours to enable the mixture to fully react, thereby finally obtaining the target product, namely the novel demulsifier D.
Equipment parameters: in the device, a jet flow-static mixer 1 uses a nozzle to inject demulsifier, internal parts use metal corrugated plate filler, and a high-efficiency separator 2 adopts a coalescence separator (the filler takes stainless steel wires as a framework and is woven into an X-shaped structure by combining polytetrafluoroethylene fibers);
the operating parameters are as follows: the inlet flow of the water-containing dirty oil is 1.2m3Per h, the flow of demulsifier injected is 0.045m3The pressure drop of the jet flow-static mixer 1 is controlled to be about 0.085MPa, the temperature is 20 ℃, and the flow speed is 0.35 m/s; the pressure drop of the high-efficiency separator 2 is about 0.14MPa, and the temperature is 20 ℃.
Content determination: the water content was determined using a karl fischer moisture meter.
2. Process flow
Injecting the high-emulsified sump oil and a demulsifier into a jet-static mixer for full contact mixing to obtain an oil-water mixture after preliminary separation; and injecting the primarily separated oil-water mixture into a high-efficiency separator for gravity settling separation or coalescence separation to obtain the sump oil and the wastewater with the water content meeting the requirements.
3. Application results
After the treatment by the method and the device, the water content is lower than 0.16 percent, and the requirement of a downstream production process is met.
Example 3
The method and the device are adopted by a certain Daqing oil refinery to dehydrate a large amount of seriously emulsified water-containing dirty oil generated in the oil field development process.
1. Conditions of the experiment
Materials: the water-containing dirty oil (the water content is about 48 percent) mainly comprises crude oil, organic sludge, surface active substances and water, is seriously emulsified and generally exists in a W/O mode at normal temperature. The density is 967Kg/m3The demulsifier adopts a novel demulsifier.
The preparation method of the demulsifier comprises the following steps:
firstly, adding 10g of tetraethylenepentamine and 20g of basic catalyst (sodium hydroxide) into a high-temperature reaction kettle, sealing the reaction kettle, purging and replacing the reaction kettle by nitrogen, vacuumizing the reaction kettle again, repeating the operation at least twice, starting stirring, stopping heating when the temperature is raised to 130 ℃, opening a feed valve, adding 250g of propylene oxide, controlling the reaction temperature to be not more than 140 ℃ and the pressure to be not more than 0.5MPa, and reacting until the pressure in the reaction kettle is 0 MPa. Then heating to 130 ℃, adding 450g of ethylene oxide, controlling the reaction temperature not to exceed 150 ℃ and the pressure not to exceed 0.5MPa, and reacting until the pressure in the kettle is 0 MPa. Finally, heating to 140 ℃, adding 290g of propylene oxide, controlling the reaction temperature not to exceed 150 ℃ and the pressure not to exceed 0.5MPa, reacting until the pressure in the kettle is 0MPa, and continuing to react for 1 hour. After the reaction is finished, cooling, opening the kettle and discharging to obtain an ethylene oxide and propylene oxide block polyether demulsifier A taking tetraethylenepentamine as an initiator;
secondly, 990g of ethylene oxide and propylene oxide block polyether demulsifier A is added into a high-temperature reaction kettle, 10g of oxalic acid and 0.9g of dodecylbenzene sulfonic acid are added, the temperature is raised by heating, the reaction temperature is controlled to be 60-80 ℃, the reaction is carried out for 1.5 hours, the reaction is carried out for 1 hour, and the product B is prepared for standby after filtration.
And thirdly, adding 2500g of toluene into a high-temperature reaction kettle, adding 450g of the prepared ethylene oxide and propylene oxide block polyether demulsifier A and 550g of the product B, heating to raise the temperature, controlling the reaction temperature to be 60-80 ℃, slowly adding 40g of toluene 2, 4 diisocyanate dropwise, finishing the dropwise adding, reacting for 1 hour, and filtering to obtain a product C for later use.
Fourthly, adding the product C100g and 6g of hydrogen-containing silicone oil into a high-temperature reaction kettle, heating, controlling the reaction temperature to be 60-80 ℃, and maintaining for 1.5 hours to enable the mixture to react fully, thereby finally obtaining the target product, namely the novel demulsifier D.
Equipment parameters: in the device, a jet flow-static mixer 1 uses a nozzle to inject demulsifier, internal parts use metal corrugated plate packing (as shown in figure 2), and a high-efficiency separator 2 adopts a coalescence separator (the packing uses stainless steel wires as a framework and is woven into a double-X-shaped structure by combining polytetrafluoroethylene fibers).
The operating parameters are as follows: the inlet flow of the water-containing dirty oil is 2.0m3Flow rate of demulsifier injected is 0.1m3The pressure drop of the jet flow-static mixer 1 is controlled to be about 0.095MPa, the temperature is 25 ℃, and the flow speed is 0.45 m/s; the pressure drop of the high-efficiency separator 2 is about 0.15MPa, and the temperature is 25 ℃.
Content determination: the water content was determined using a karl fischer moisture meter.
2. Process flow
Injecting the high-emulsified sump oil and a demulsifier into a jet-static mixer for full contact mixing to obtain an oil-water mixture after preliminary separation; and injecting the primarily separated oil-water mixture into a high-efficiency separator for gravity settling separation or coalescence separation to obtain the sump oil and the wastewater with the water content meeting the requirements.
3. Application results
After the treatment by the method and the device, the water content is lower than 0.21 percent, and the requirement of a downstream production process is met.
Comparative example 1
The novel demulsifier prepared was not added, and the rest was the same as in example 1. The water content of the finally treated dirty oil was 16%.
Comparative example 2
The apparatus of the present application was not used, and a general gravity settling apparatus was used, and the rest was the same as in example 1. The water content of the finally treated dirty oil was 21%.
According to the method and the device for treating the sump oil, disclosed by the embodiment 1 of the application, the water content of the finally treated sump oil is lower than 0.25%, and the water content of the finally treated sump oil in the comparative examples 1 and 2 is respectively 16% and 21%, so that the requirements of downstream production processes are not met.
Although the present invention has been described with reference to a preferred embodiment, it should be understood that various changes, substitutions and alterations can be made herein without departing from the spirit and scope of the invention as defined by the appended claims.
Claims (10)
1. The method for dehydrating the high-emulsification sump oil is characterized by comprising the following steps of:
injecting the high-emulsified sump oil and a demulsifier into a jet-static mixer for full contact mixing to obtain an oil-water mixture after preliminary separation; and injecting the primarily separated oil-water mixture into a high-efficiency separator for gravity settling separation or coalescence separation to obtain the sump oil and the wastewater with the water content meeting the requirements.
2. The method for dehydrating highly emulsified dirty oil as claimed in claim 1, wherein the water content of the highly emulsified dirty oil is not less than 40%, and the density is 900-3；
The inlet flow of the high-emulsification sump oil is 0-2 m3/h；
The flow ratio of the high-emulsification sump oil to the demulsifier is 20: 1-100: 1.
3. The method for dewatering highly emulsified dirty oil as claimed in claim 1, wherein the parameters of the jet-static mixer are set as: the pressure drop is 0.01-0.1 MPa, the temperature is 10-30 ℃, and the flow rate is 0.01-0.5 m/s;
the molecular weight of the demulsifier is 3600-48000 g/mol.
4. The method for dewatering highly emulsified dirty oil as claimed in claim 1, wherein the demulsifier is prepared by the following steps: firstly, adding tetraethylenepentamine and an alkaline catalyst into a high-temperature reaction kettle, sealing the reaction kettle, purging and replacing by using nitrogen, vacuumizing, repeating the operation at least twice, starting stirring, heating to 130-160 ℃, adding propylene oxide, controlling the reaction temperature and pressure until the pressure in the kettle is 0MPa, adding ethylene oxide, controlling the reaction temperature and pressure until the pressure in the kettle is 0MPa, heating to 140 ℃, adding propylene oxide, controlling the reaction temperature and pressure until the pressure in the kettle is 0MPa, continuing to react for 60-80min, cooling to open the kettle and discharging to obtain an ethylene oxide and propylene oxide block demulsifier A after the reaction is finished;
based on the total weight of tetraethylenepentamine, propylene oxide and ethylene oxide, the tetraethylenepentamine accounts for 0.5-1% of the total weight, the first propylene oxide accounts for 24-29.5% of the total weight, the second propylene oxide accounts for 25-30% of the total weight, the ethylene oxide accounts for 40-50% of the total weight, and the alkaline catalyst accounts for 0.5-2% of the total weight;
secondly, carrying out self-crosslinking reaction on polycarboxylic acid and ethylene oxide and propylene oxide block polyether demulsifier A under the action of a catalyst to obtain a product B;
the ethylene oxide and propylene oxide block polyether demulsifier A accounts for 96.5 to 99 percent of the total weight, the polycarboxylic acid accounts for 1 to 3.5 percent of the total weight, and the catalyst accounts for 0.01 to 0.1 percent of the total weight; the reaction temperature is 60-80 ℃;
thirdly, performing a crosslinking reaction on the ethylene oxide and propylene oxide block polyether demulsifier A and the product B in a solvent by using 2, 4 toluene diisocyanate as a crosslinking agent to obtain a product C;
the ethylene oxide and propylene oxide block polyether demulsifier A accounts for 25-45% of the total weight, the product B accounts for 55-75% of the total weight, the solvent dosage is 0.5-2.5 times of the total weight, and 2, 4-diisocyanate toluene is 0.5-5% of the total weight; the reaction temperature is 60-80 ℃;
fourthly, mixing the product C with hydrogen-containing silicone oil for reaction to obtain a demulsifier D;
the mass ratio of the hydrogen-containing silicone oil to the product C is (1-6): 100, and the reaction temperature is 60-80 ℃.
5. The method for dewatering highly emulsified dirty oil as claimed in claim 1, wherein the parameters of the high efficiency separator are set as: the pressure drop is 0.01-0.15 MPa, and the temperature is 10-30 ℃;
the water content of the sump oil with the water content meeting the requirement is not higher than 0.3 percent.
6. The device for dehydrating the high emulsified sump oil according to any one of claims 1 to 5, which comprises a jet-static mixer, a high-efficiency separator and a high-pressure jet system, wherein the external end of the jet-static mixer is provided with a high emulsified sump oil inlet and a demulsifier inlet, and the other external end of the jet-static mixer is provided with a mixture outlet; the jet flow-static mixer consists of a dumbbell-shaped shell, nozzles and corrugated plate fillers, wherein the number of the nozzles is 3, the nozzles are positioned in the dumbbell-shaped shell and are adjacent to a high-emulsification sump oil inlet, and the nozzles are distributed annularly at intervals of 120 degrees; the corrugated plate packing is provided with 3 sections in total, one section is close to the spray nozzle, the middle section is positioned at the middle section of the dumbbell-shaped shell, and the three sections are positioned inside the other end of the dumbbell-shaped shell; one end of the high-efficiency separator is provided with a mixture inlet, and the other end of the high-efficiency separator is provided with a sump oil outlet and a waste water outlet; the mixture inlet is connected with the mixture outlet of the jet-static mixer; the high-pressure jet system is formed by sequentially connecting a high-pressure pump, a pressure regulating valve, a pressure stabilizing tank, a stop valve and a pressure gauge; the pressure gauge is connected with a nozzle inside the jet flow-static mixer.
7. The device used in the method for dehydrating highly emulsified dirty oil according to claim 6, wherein the flow velocity of the jet flow in the nozzle is 0 to 100m/s, and the pressure is 0 to 140 MPa;
the nozzle is a gaussian nozzle;
the distance between the nozzle and the corrugated plate filler is 3-5% of the total length of the jet-static mixer.
8. The apparatus for dewatering highly emulsified dirty oil as claimed in claim 6, wherein the distance between the adjacent corrugated plate packing is 5% -8% of the total length of the jet-static mixer;
the corrugated plate filler adopts a metal corrugated plate as the filler, and the length of each section of the filler is 15-20% of the total length of the jet-static mixer;
the corrugated plate filler is a filler which takes stainless steel wires as a framework and is woven into an omega-shaped structure by combining polytetrafluoroethylene fibers, a filler which takes stainless steel wires as a framework and is woven into an X-shaped structure by combining the polytetrafluoroethylene fibers, and a filler which takes the stainless steel wires as a framework and is woven into a double X-shaped structure by combining the polytetrafluoroethylene fibers.
9. The apparatus for dewatering highly emulsified dirty oil as claimed in claim 6, wherein the corrugation angle of the corrugated plate packing is 45 ° to the longitudinal pipe axis, the inclination angle of the corrugation of the adjacent corrugated plates is symmetrically distributed to the longitudinal pipe axis, and the corrugated plate of the connected mixing unit is rotated 90 °;
the dumbbell-shaped shell is large at two ends and small in the middle and is similar to a dumbbell in shape.
10. The device for dehydrating highly emulsified dirty oil as claimed in claim 6, wherein the jet-static mixer is horizontal or vertical;
the high-efficiency separator adopts a coalescence separator and adopts a single stage or multiple stages.
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