CN107213671B - Emulsion breaking device and treatment method thereof - Google Patents
Emulsion breaking device and treatment method thereof Download PDFInfo
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- CN107213671B CN107213671B CN201710363617.3A CN201710363617A CN107213671B CN 107213671 B CN107213671 B CN 107213671B CN 201710363617 A CN201710363617 A CN 201710363617A CN 107213671 B CN107213671 B CN 107213671B
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D17/00—Separation of liquids, not provided for elsewhere, e.g. by thermal diffusion
- B01D17/02—Separation of non-miscible liquids
- B01D17/0217—Separation of non-miscible liquids by centrifugal force
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D17/00—Separation of liquids, not provided for elsewhere, e.g. by thermal diffusion
- B01D17/02—Separation of non-miscible liquids
- B01D17/04—Breaking emulsions
- B01D17/047—Breaking emulsions with separation aids
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D17/00—Separation of liquids, not provided for elsewhere, e.g. by thermal diffusion
- B01D17/12—Auxiliary equipment particularly adapted for use with liquid-separating apparatus, e.g. control circuits
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Abstract
The invention provides an emulsion breaking device and a treatment method thereof, wherein the emulsion breaking device comprises a main reactor, and the main reactor sequentially comprises a centrifugal emulsion breaking device, a dewetting emulsion breaking device and a microorganism culture device from bottom to top; an oil phase outlet and a water phase outlet of the centrifugal demulsification device are respectively connected with the organic phase storage tank and the water phase storage tank; the residual emulsion outlet of the centrifugal demulsification device is connected with the emulsion inlet of the anti-wetting demulsification device through a pipeline; an oil phase outlet and a water phase outlet of the anti-wetting demulsification device are respectively connected with an organic phase storage tank and a water phase storage tank; and a cleaning liquid outlet of the microorganism culture device is connected with a cleaning liquid inlet of the anti-wetting demulsification device through a pipeline. The invention provides more efficient and energy-saving demulsification equipment.
Description
Technical Field
the invention belongs to the technical field of emulsion breaking, relates to an emulsion breaking device and a treatment method thereof, and particularly relates to an emulsion breaking device for an emulsion with high viscosity and a treatment method thereof.
background
The emulsion is a liquid-liquid dispersion system in which at least one liquid is dispersed in the form of liquid beads in another immiscible liquid, and belongs to a multiphase system. The volume of the dispersed phase can vary within wide limits and the system is not stable, but the stability of the system is greatly improved in the presence of emulsifiers. Common emulsions are oil-in-water, water-in-oil or multiple emulsions. In actual production, due to the wide variety and large amount of compounds in nature, many emulsions are multiple emulsions in production.
The emulsion has a large production amount in industrial production, and common emulsions comprise oil field wastewater, a third phase generated when solid waste is treated by an extraction method, a lubricant in the machining industry and the like. A large amount of emulsion is discharged into the environment, which not only damages the environment, but also wastes high-concentration compounds contained in the emulsion, so that the development of emulsion breaking equipment is carried forward. CN 201346412Y discloses a demulsification device, which can adopt acid and alkali to carry out demulsification, and the technical scheme is as follows: the equipment comprises a demulsification tank, a waste liquid tank, a gas storage tank, a water outlet, a sludge drying tank and the like; the pneumatic acid medicine box accurately controls medicine feeding. CN 2933521Y discloses an inorganic microfiltration membrane vacuum demulsification equipment, which comprises: the device comprises an emulsion tank, an infusion pump, an inorganic microfiltration membrane device, a liquid collecting tank and the like, and overcomes the defect that the traditional membrane demulsification needs a larger pressure difference.
however, the above devices all have the problems of large dosage of emulsion breaking agents or easy blockage. Therefore, how to develop an efficient and energy-saving demulsification device for multiple emulsions, particularly for emulsions with high viscosity, is a problem to be solved.
disclosure of Invention
Aiming at the problems in the existing emulsion breaking device, the invention provides an emulsion breaking device and a treatment method thereof. According to the invention, the centrifugal demulsification device and the anti-wetting device are integrated into one device, so that the efficient and automatic demulsification treatment of multiple emulsions, especially emulsions with high viscosity, can be realized, no additive is required to be added, the circulation of an organic phase is not influenced, and secondary pollution is avoided.
In order to achieve the purpose, the invention adopts the following technical scheme:
In a first aspect, the invention provides an emulsion breaking device, which comprises a main reactor, wherein the main reactor sequentially comprises a centrifugal emulsion breaking device, a dewetting emulsion breaking device and a microorganism culture device from bottom to top; the centrifugal demulsification device is provided with an emulsion inlet, an oil phase outlet, a water phase outlet and a residual emulsion outlet, and the oil phase outlet and the water phase outlet of the centrifugal demulsification device are respectively connected with the organic phase storage tank and the water phase storage tank; the anti-wetting demulsification device is provided with a cleaning liquid inlet, an emulsion inlet, an oil phase outlet, a water phase outlet and a cleaning liquid outlet, and a residual emulsion outlet of the centrifugal demulsification device is connected with an emulsion inlet of the anti-wetting demulsification device through a pipeline; an oil phase outlet and a water phase outlet of the anti-wetting demulsification device are respectively connected with an organic phase storage tank and a water phase storage tank; the microorganism culture device is provided with a microorganism feed inlet and a cleaning liquid outlet, and the cleaning liquid outlet of the microorganism culture device is connected with the cleaning liquid inlet of the anti-wetting demulsification device through a pipeline.
in the invention, the emulsion breaking device is special for emulsion breaking. After the emulsion enters an emulsion demulsification device, performing first-stage treatment on the emulsion through centrifugal demulsification, wherein the centrifugal demulsification rate can reach 80-90%; and (3) the rest 10-20% of the part difficult to centrifugally demulsify enters a de-wetting demulsifying device for secondary treatment.
the following technical solutions are preferred but not limited to the technical solutions provided by the present invention, and the technical objects and advantages of the present invention can be better achieved and realized by the following technical solutions.
As the preferable technical scheme of the invention, a connecting pipeline between the residual emulsion outlet of the centrifugal demulsification device and the emulsion inlet of the anti-wetting demulsification device is provided with a regulating valve.
Preferably, a regulating valve is arranged on a connecting pipeline between a cleaning liquid outlet of the microorganism culture device and a cleaning liquid inlet of the anti-wetting demulsification device.
In the invention, when the anti-wetting demulsification device is used for demulsifying, the regulating valve between the residual emulsion outlet of the centrifugal demulsification device and the emulsion inlet pipeline of the anti-wetting demulsification device is opened, and the regulating valve between the cleaning solution outlet of the microorganism culture device and the cleaning solution inlet pipeline of the anti-wetting demulsification device is closed.
When the anti-wetting demulsification device is idle, the regulating valve between the residual emulsion outlet of the centrifugal demulsification device and the emulsion inlet pipeline of the anti-wetting demulsification device is closed, and the regulating valve between the cleaning liquid outlet of the microorganism culture device and the cleaning liquid inlet pipeline of the anti-wetting demulsification device is opened, so that the cleaning liquid in the microorganism culture device enters the anti-wetting demulsification device for degradation and cleaning.
As a preferable technical scheme, the emulsion breaking device comprises an automatic control device, and the automatic control device is connected with all devices in the emulsion breaking device.
the automatic control device is used for realizing the automatic control of the emulsion demulsification device, adjusting the operation of each device in the emulsion demulsification device and the opening and closing of the adjusting valve through the automatic control device, and controlling the conditions of flow, reaction temperature, centrifugal speed, line switching and the like of fluid in the whole device.
In a preferred embodiment of the present invention, the de-wetting demulsifying device comprises at least 2 de-wetting apparatuses, such as 2, 3, 4 or 5, etc., and more, but not limited to the recited values, and other non-recited values in the range of values are also applicable, preferably 2.
Preferably, the anti-wetting demulsification device comprises a first anti-wetting device and a second anti-wetting device, the residual emulsion outlet of the centrifugal demulsification device is simultaneously connected with the emulsion inlet of the first anti-wetting device and the emulsion inlet of the second anti-wetting device, and the cleaning solution outlet of the microorganism culture device is simultaneously connected with the cleaning solution inlet of the first anti-wetting device and the cleaning solution inlet of the second anti-wetting device.
In the present invention, the first and second anti-wetting apparatuses are only named for anti-wetting apparatuses and are not limited to the order of use.
Preferably, a connecting pipeline between the residual emulsion outlet of the centrifugal demulsifying device and the emulsion inlet of the first anti-wetting device and a connecting pipeline between the residual emulsion outlet of the centrifugal demulsifying device and the emulsion inlet of the second anti-wetting device are both provided with regulating valves.
Preferably, a connecting pipeline between the cleaning liquid outlet of the microorganism culture device and the cleaning liquid inlet of the first anti-wetting device and a connecting pipeline between the cleaning liquid outlet of the microorganism culture device and the cleaning liquid inlet of the second anti-wetting device are both provided with regulating valves.
In the invention, the regulating valve between the residual emulsion outlet of the centrifugal demulsification device and the emulsion inlet pipeline of the first anti-wetting equipment and the regulating valve between the residual emulsion outlet of the centrifugal demulsification device and the emulsion inlet pipeline of the second anti-wetting equipment are controlled to be opened and closed by the automatic control device.
And the opening and closing of the adjusting valve between the cleaning liquid outlet of the microorganism culture device and the cleaning liquid inlet pipeline of the first anti-wetting device and the adjusting valve between the cleaning liquid outlet of the microorganism culture device and the cleaning liquid inlet pipeline of the second anti-wetting device are controlled by the automatic control device.
The first anti-wetting equipment and the second anti-wetting equipment are alternately used, and when the first anti-wetting equipment carries out demulsification operation, the second anti-wetting equipment carries out cleaning operation; when the first anti-wetting equipment is used for cleaning, the second anti-wetting equipment is switched to perform demulsification operation, so that the continuous operation of the whole device is ensured.
Preferably, the first and second anti-wetting apparatuses are identical in structure.
As a preferable technical scheme, the anti-wetting demulsification device comprises an anti-wetting solid phase pipe and a temperature controller, wherein the anti-wetting solid phase pipe and the temperature controller are arranged in anti-wetting equipment.
Wherein, the typical but non-limiting arrangement mode of the anti-wetting solid phase pipe in the anti-wetting demulsification device is as follows: arranged tangentially side by side.
The temperature controller is used for regulating and controlling the operating temperature of the anti-wetting demulsification device, namely, the device can be operated at higher temperature when the viscosity of the emulsion is higher.
Preferably, the number of said dewetting solid phase tubes is not less than 5000, such as 5000, 6000, 7000, 8000, 9000, 10000 or 11000, and more, but not limited to the recited values, and other non-recited values within the range of values are equally applicable, preferably 8000 to 10000.
Preferably, the anti-wetting solid phase tube is a hollow tube with holes on the surface.
preferably, the width of the pores on the surface of the anti-wetting solid phase tube is 0.2nm to 50nm, such as 0.2nm, 0.5nm, 1nm, 5nm, 10nm, 15nm, 20nm, 25nm, 30nm, 35nm, 40nm, 45nm, or 50nm, but is not limited to the recited values, and other values not recited in the numerical range are also applicable. In the invention, the liquid to be treated can enter the anti-wetting solid phase tube through the hollow tube with holes on the surface to react with the inorganic salt and the filler in the anti-wetting solid phase tube.
preferably, the surface of the anti-wetting solid phase tube has a porosity of 85% to 95%, such as 85%, 86%, 87%, 88%, 89%, 90%, 91%, 92%, 93%, 94%, or 95%, but is not limited to the recited values, and other values not recited within the range are equally applicable.
Preferably, the diameter of the anti-wetting solid phase tube is 10um to 100um, such as 10um, 20um, 30um, 40um, 50um, 60um, 70um, 80um, 90um or 100um, but not limited to the recited values, and other non-recited values within the range of values are equally applicable.
preferably, the anti-wetting solid phase tube is filled with an inorganic salt and a filler.
Preferably, the inorganic salt is used in an amount of 0.5 wt% to 30 wt%, such as 0.5 wt%, 1 wt%, 3 wt%, 5 wt%, 7 wt%, 10 wt%, 13 wt%, 15 wt%, 17 wt%, 20 wt%, 23 wt%, 25 wt%, 27 wt%, or 30 wt%, based on the total mass of the inorganic salt and filler, but not limited to the recited values, and other non-recited values within this range are equally applicable, preferably 10 wt% to 25 wt%.
In the invention, the inorganic salt has the function of generating strong complexation with the emulsion, so that the emulsion is transferred from an oil-water interface to a solid phase interface and a hollow part, multiple emulsions are broken, and the aim of oil-water separation is fulfilled. The dosage of the emulsifier needs to be controlled within a certain range, and if the dosage of the emulsifier is small, the emulsifier can play a role in promoting emulsification. If it is too much, i.e., more than 30 wt% of the total mass of the inorganic salts and the fillers, the treatment cost is increased and secondary pollution to the waste water is caused.
Preferably, the cation in the inorganic salt is any one of ammonium ion, sodium ion, potassium ion, iron ion, manganese ion or titanium ion or a combination of at least two of them, and typical but non-linear examples of the combination are: a combination of ammonium ions and sodium ions, a combination of potassium ions and iron ions, a combination of manganese ions and titanium ions, a combination of ammonium ions, sodium ions and potassium ions, a combination of potassium ions, iron ions and manganese ions, a combination of potassium ions, iron ions, manganese ions and titanium ions, a combination of ammonium ions, sodium ions, potassium ions, iron ions, manganese ions and titanium ions, and the like. The cations may be mixed in any proportion.
Preferably, the anion in the inorganic salt is any one or a combination of at least two of sulfate ion, nitrate ion, hydroxide ion, fluoride ion, tungstate ion, molybdate ion, vanadate ion, chromate ion, or germanate ion, typical but non-limiting examples of which are: a combination of sulfate and nitrate ions, a combination of hydroxide and fluoride, a combination of tungstate and molybdate ions, a combination of vanadate and chromate, a combination of chromate and germanate, a combination of sulfate, nitrate and hydroxide, a combination of fluoride, tungstate, molybdate and vanadate, a combination of molybdate, vanadate, chromate, and germanate, a combination of sulfate, nitrate, hydroxide, molybdate, tungstate, chromate, vanadate, and germanate, a combination of sulfate, nitrate, vanadate, hydroxide, molybdate, tungstate, chromate, vanadate, chromate, and germanate, and the like. The anions can be mixed in any proportion.
Preferably, the inorganic salt is a metal inorganic salt.
Preferably, the metal inorganic salt contains at least 1 metal.
preferably, the filler is any one or a combination of at least two of coal slag, bentonite, glass fiber, polyurethane foam or quartz powder, and the combination is exemplified by the following typical but non-limiting examples: the combination of coal waste residue and bentonite, the combination of glass fiber and polyurethane foam, the combination of polyurethane foam and quartz powder, the combination of coal waste residue, bentonite and glass fiber, the combination of glass fiber, polyurethane foam and quartz powder, the combination of coal waste residue, bentonite, glass fiber and polyurethane foam, the combination of coal waste residue, bentonite, glass fiber, polyurethane foam and quartz powder and the like.
As a preferred technical scheme of the invention, the microorganism cultured in the microorganism culture device is any one or a combination of at least two of nitrite bacteria, pseudomonas or pseudomonas putida, and typical but non-linear examples of the combination are as follows: a combination of nitrite bacteria and pseudomonas, a combination of pseudomonas and pseudomonas putida, a combination of nitrite bacteria, pseudomonas and pseudomonas putida, and the like.
In a second aspect, the present invention provides a method for treating the above emulsion breaking device, the method comprising the steps of:
(1) After emulsion breaking, the emulsion enters a centrifugal emulsion breaking device in the emulsion breaking device for centrifugal emulsion breaking, and an oil phase and a water phase generated by centrifugal emulsion breaking respectively enter an organic phase storage tank and a water phase storage tank;
(2) The residual emulsion generated in the step (1) is sent into a de-wetting demulsification device for de-wetting demulsification, and an oil phase and a water phase generated in the de-wetting demulsification are respectively sent into an organic phase storage tank and a water phase storage tank;
(3) And (3) after the anti-wetting demulsification is finished, introducing a cleaning fluid into the anti-wetting demulsification device through a microorganism culture device to clean the anti-wetting demulsification device, and discharging the cleaned waste liquid into the environment.
As a preferred technical scheme of the invention, the emulsion to be broken in the step (1) is a multiple emulsion.
In the present invention, the multiple emulsion is a composite system of water-in-oil-in-water or oil-in-water-in-oil type, which is a general technical expression in the field and is a clear expression.
Preferably, the centrifugation rate of the centrifugation demulsification in the step (1) is 20000r/min to 30000r/min, such as 20000r/min, 21000r/min, 22000r/min, 23000r/min, 24000r/min, 25000r/min, 26000r/min, 27000r/min, 28000r/min, 29000r/min or 30000r/min, but not limited to the enumerated values, and other unrecited values in the numerical range are also applicable.
preferably, the temperature for the centrifugal demulsification in the step (1) is 40 ℃ to 60 ℃, such as 40 ℃, 43 ℃, 45 ℃, 47 ℃, 50 ℃, 53 ℃, 55 ℃, 57 ℃ or 60 ℃, but is not limited to the enumerated values, and other non-enumerated values in the numerical range are also applicable.
preferably, the demulsification rate of the centrifugal demulsification in the step (1) is 80-90%, such as 80%, 83%, 85%, 87% or 90%, but not limited to the enumerated values, and other unrecited values in the numerical range are also applicable.
As a preferred technical scheme of the invention, the anti-wetting demulsification process in the anti-wetting demulsification device in the step (2) comprises the following steps:
(a) the residual emulsion generated by the centrifugal demulsification device enters first anti-wetting equipment for anti-wetting demulsification treatment; meanwhile, the connection between the centrifugal demulsification device and the second anti-wetting equipment is disconnected, the connection between the microorganism culture device and the first anti-wetting equipment is disconnected, the microorganism culture device and the second anti-wetting equipment are communicated, cleaning liquid is injected into the second anti-wetting equipment through the microorganism culture device to clean the second anti-wetting equipment, and the cleaning waste liquid is directly discharged into the environment;
(b) after the anti-wetting demulsification treatment of the first anti-wetting equipment is finished, disconnecting the centrifugal demulsification device from the first anti-wetting equipment, communicating the centrifugal demulsification device with the second anti-wetting equipment, and performing anti-wetting demulsification operation through the second anti-wetting equipment; meanwhile, the microorganism culture device is communicated with second anti-wetting equipment, the connection between the microorganism culture device and the first anti-wetting equipment is opened, cleaning liquid is injected into the first anti-wetting equipment through the microorganism culture device to clean the first anti-wetting equipment, and cleaning waste liquid is directly discharged into the environment;
(c) And (c) repeating the steps (a) to (b).
As a preferred embodiment of the present invention, after the first anti-wetting apparatus in step (b) performs anti-wetting treatment for 48h to 72h, the centrifugal demulsifying device is disconnected from the first anti-wetting apparatus, wherein the treatment time may be 48h, 50h, 53h, 55h, 57h, 60h, 63h, 65h, 67h, 70h or 72h, but is not limited to the recited values, and other values not recited in the range of the values are also applicable.
In the invention, the rest 10-20% of emulsions difficult to be centrifugally demulsified are multiple emulsions with stable interfaces, such as W/O/W and O/W/O, and are difficult to be demulsified. When the emulsion passes through a reverse-wetting solid phase pipe in a reverse-wetting demulsification device, the inorganic metal salt in the solid phase pipe has strong complexation effect on the emulsion with a certain interfacial tension value, so that the emulsion is transferred to a solid phase interface and a hollow part from an oil-water interface, multiple emulsion demulsification is caused, and the aim of oil-water separation is fulfilled. In addition, heavy metal ions can form a strong electron layer on the surface of the solid phase tube, an electric double layer of the emulsion is compressed, emulsion breaking of the emulsion is accelerated, and the emulsion breaking rate of the device reaches 99-100%.
In the invention, the long-term accumulation of the adsorption emulsifier on the surface and inside of the anti-wetting solid phase pipe can cause the demulsification capability of the solid phase pipe to be reduced, even the blockage to be ineffective. Therefore, after the anti-wetting solid phase tube is recycled for a period of time, the anti-wetting solid phase tube is cleaned by a biodegradation method, and the regeneration purpose is achieved.
Compared with the prior art, the invention has the following beneficial effects:
(1) According to the invention, the centrifugal demulsification device and the anti-wetting device are integrated into one device, multiple demulsification technologies are combined, so that the energy is saved, the efficiency is high, the demulsification efficiency is improved, and the final demulsification rate can reach 99-100%;
(2) the device and the treatment method do not need to add any additive, do not influence the recycling of the organic phase and do not cause secondary pollution;
(3) The device and the treatment method can realize full-automatic control and continuous operation, and the demulsification and cleaning of the reactor can be carried out simultaneously, so that the device and the treatment method are accurate, rapid and labor cost is saved;
(4) The device and the treatment method have wide application range, can be used for demulsification of an emulsification intermediate layer generated by an extraction method and a back extraction method device, and can also be used for an oil field wastewater oil removal system with high viscosity.
Drawings
FIG. 1 is a schematic diagram of the structure of an emulsion breaking apparatus according to example 1 of the present invention;
The method comprises the following steps of 1-a main reactor, 2-a centrifugal demulsification device, 3-a dewetting demulsification device, 4-a microorganism culture device, 5-an organic phase storage tank, 6-a water phase storage tank, 7-an automatic control device, 31-first dewetting equipment and 32-second dewetting equipment.
Detailed Description
In order to better illustrate the present invention and facilitate the understanding of the technical solutions of the present invention, the present invention is further described in detail below. The following examples are merely illustrative of the present invention and do not represent or limit the scope of the claims, which are defined by the claims.
The specific embodiment of the invention provides an emulsion demulsification device and a treatment method thereof, wherein the emulsion demulsification device comprises a main reactor 1, and the main reactor 1 sequentially comprises a centrifugal demulsification device 2, a dewetting demulsification device 3 and a microorganism culture device 4 from bottom to top; the centrifugal demulsification device 2 is provided with an emulsion inlet, an oil phase outlet, a water phase outlet and a residual emulsion outlet, and the oil phase outlet and the water phase outlet of the centrifugal demulsification device 2 are respectively connected with an organic phase storage tank 5 and a water phase storage tank 6; the anti-wetting demulsification device 3 is provided with a cleaning liquid inlet, an emulsion inlet, an oil phase outlet, a water phase outlet and a cleaning liquid outlet, and the residual emulsion outlet of the centrifugal demulsification device 2 is connected with the emulsion inlet of the anti-wetting demulsification device 3 through a pipeline; an oil phase outlet and a water phase outlet of the anti-wetting demulsification device 3 are respectively connected with an organic phase storage tank 5 and a water phase storage tank 6; the microorganism culture device 4 is provided with a microorganism feed inlet and a cleaning liquid outlet, and the cleaning liquid outlet of the microorganism culture device 4 is connected with the cleaning liquid inlet of the anti-wetting demulsification device 3 through a pipeline.
The processing method comprises the following steps:
(1) After emulsion breaking emulsion enters a centrifugal emulsion breaking device 2 in the emulsion breaking device for centrifugal emulsion breaking, and oil phase and water phase generated by centrifugal emulsion breaking respectively enter an organic phase storage tank 5 and a water phase storage tank 6;
(2) The residual emulsion generated in the step (1) enters a de-wetting demulsification device 3 for de-wetting demulsification, and an oil phase and a water phase generated in the de-wetting demulsification enter an organic phase storage tank 5 and a water phase storage tank 6 respectively;
(3) And (3) after the anti-wetting demulsification is finished in the step (2), introducing a cleaning solution into the anti-wetting demulsification device 3 through a microorganism culture device 4 to clean the anti-wetting demulsification device 3, and discharging the cleaned waste liquid into the environment.
The following are typical but non-limiting examples of the invention:
Example 1:
The embodiment provides an emulsion demulsification device and a treatment method thereof, as shown in fig. 1, the emulsion demulsification device comprises a main reactor 1, and the main reactor 1 sequentially comprises a centrifugal demulsification device 2, a dewetting demulsification device 3 and a microorganism culture device 4 from bottom to top; the centrifugal demulsification device 2 is provided with an emulsion inlet, an oil phase outlet, a water phase outlet and a residual emulsion outlet, and the oil phase outlet and the water phase outlet of the centrifugal demulsification device 2 are respectively connected with an organic phase storage tank 5 and a water phase storage tank 6; the anti-wetting demulsification device 3 is provided with a cleaning liquid inlet, an emulsion inlet, an oil phase outlet, a water phase outlet and a cleaning liquid outlet, and the residual emulsion outlet of the centrifugal demulsification device 2 is connected with the emulsion inlet of the anti-wetting demulsification device 3 through a pipeline; an oil phase outlet and a water phase outlet of the anti-wetting demulsification device 3 are respectively connected with an organic phase storage tank 5 and a water phase storage tank 6; the microorganism culture device 4 is provided with a microorganism feed inlet and a cleaning liquid outlet, and the cleaning liquid outlet of the microorganism culture device 4 is connected with the cleaning liquid inlet of the anti-wetting demulsification device 3 through a pipeline.
The emulsion breaking device comprises an automatic control device 7, and the automatic control device 7 is connected with all devices in the emulsion breaking device.
wherein, the anti-wetting demulsification device comprises a first anti-wetting device 31 and a second anti-wetting device 32, the residual emulsion outlet of the centrifugal demulsification device 2 is simultaneously connected with the emulsion inlet of the first anti-wetting device 31 and the emulsion inlet of the second anti-wetting device 32, and the cleaning solution outlet of the microorganism culture device 4 is simultaneously connected with the cleaning solution inlet of the first anti-wetting device 31 and the cleaning solution inlet of the second anti-wetting device 32;
A connecting pipeline between the residual emulsion outlet of the centrifugal demulsifying device 2 and the emulsion inlet of the first anti-wetting device 31 and a connecting pipeline between the residual emulsion outlet of the centrifugal demulsifying device 2 and the emulsion inlet of the second anti-wetting device 32 are both provided with regulating valves; a connecting pipeline between the cleaning liquid outlet of the microorganism culture device 4 and the cleaning liquid inlet of the first anti-wetting device 31 and a connecting pipeline between the cleaning liquid outlet of the microorganism culture device 4 and the cleaning liquid inlet of the second anti-wetting device 32 are both provided with regulating valves; the first and second dewetting devices 31, 32 are identical in construction.
the anti-wetting demulsification device 3 comprises an anti-wetting solid phase pipe and a temperature controller; the anti-wetting solid phase tube is a hollow tube with holes on the surface, the number of the anti-wetting solid phase tubes is about 9000, the width of the holes on the surface of the anti-wetting solid phase tube is 0.3nm, the diameter of the anti-wetting solid phase tube is 20 mu m, and the porosity of the surface of the anti-wetting solid phase tube is about 90%; inorganic salt and filler are filled in the anti-wetting solid phase tube, the using amount of the inorganic salt accounts for 10 wt% of the total mass of the inorganic salt and the filler, cations of the inorganic salt are the combination of ammonium ions, sodium ions and potassium ions, anions are the combination of nitrate radicals, chromate radicals and vanadate radicals, and the filler is the mixture of coal waste residues and glass fibers.
the microorganism in the microorganism culture device 4 is a mixture of nitrite bacteria ATCC19718 and pseudomonas Pxy-40.
Treating an emulsion by using the emulsion demulsification device, wherein the emulsion is an emulsification intermediate layer generated when the coking wastewater is treated by an extraction method, and the main components of an organic phase comprise methyl isobutyl ketone (MIBK) and toluene; the water phase mainly comprises water, phenol, cresol and dihydric phenol, and the emulsifier mainly comprises oil and solid powder, and is multiple emulsion.
The specific treatment process comprises the following steps:
(1) The emulsion to be demulsified enters a centrifugal demulsification device 2 in the emulsion demulsification device under the control of an automatic control device 7 to carry out centrifugal demulsification, wherein the centrifugal speed is 25000r/min, the centrifugal temperature is 50 ℃, the centrifugal demulsification rate is 89%, and an oil phase and a water phase generated by the centrifugal demulsification respectively enter an organic phase storage tank 5 and a water phase storage tank 6;
(2) the residual emulsion generated by the centrifugal demulsification device 2 enters a first anti-wetting device 31 for anti-wetting demulsification treatment; meanwhile, the connection between the centrifugal demulsification device 2 and the second anti-wetting device 32 is disconnected, the connection between the microorganism culture device 4 and the first anti-wetting device 31 is disconnected, the microorganism culture device 4 and the second anti-wetting device 32 are communicated, cleaning liquid is injected into the second anti-wetting device 32 of the microorganism culture device 4 to clean the second anti-wetting device 32, and cleaning waste liquid is directly discharged into the environment;
(3) After the first anti-wetting equipment 31 is subjected to anti-wetting treatment for 48 hours, the connection between the centrifugal demulsifying device 2 and the first anti-wetting equipment 31 is disconnected, the centrifugal demulsifying device 2 and the second anti-wetting equipment 32 are communicated, and anti-wetting operation is performed through the second anti-wetting equipment 32; meanwhile, the connection between the microorganism culture device 4 and the second anti-wetting device 32 is disconnected, the microorganism culture device 4 and the first anti-wetting device 31 are communicated, cleaning liquid is injected into the first anti-wetting device 31 through the microorganism culture device 4 to clean the first anti-wetting device 31, and the cleaning waste liquid is directly discharged into the environment;
(4) And (4) repeating the step (2) to the step (3).
Finally, the emulsion breaking efficiency of the emulsion is 99.8% by the emulsion breaking device.
Example 2:
The present embodiment provides an emulsion breaking apparatus and a processing method thereof, where the structure of the emulsion breaking apparatus is different from that of the emulsion breaking apparatus in embodiment 1 in that: the number of the anti-wetting solid phase tubes in the anti-wetting solid phase tube is about 8000, the width of the surface hole is 0.4nm, the diameter of the tube is 50um, the porosity of the surface of the anti-wetting solid phase tube is 86%, the use amount of inorganic salt accounts for 0.5 wt% of the total mass of the inorganic salt and the filler, and the cation of the inorganic salt is the combination of sodium ions, potassium ions, manganese ions and titanium ions; the anion is the combination of nitrate ions, fluoacid ions, tungstate ions and germanate ions; the filler is a mixture of polyurethane foam and quartz powder; the microorganism in the microorganism culture apparatus is a mixture of nitrite bacteria ATCC19718, Pseudomonas Pxy-40 and Pseudomonas putida ML 2.
treating an emulsion by using the emulsion demulsification device, wherein the emulsion is an emulsified intermediate layer generated when vanadium-chromium waste residues are treated by an extraction method, and the main components of an organic phase comprise tributyl phosphate, toluene and kerosene; the main components of the water phase are water, vanadate radical, chromate radical and the like, and the emulsifier mainly comprises oil and solid powder and is a multiple emulsion.
The specific processing flow refers to the processing flow in example 1, with the difference that: the centrifugation speed in the step (1) is 21000r/min, the centrifugation temperature is 40 ℃, and the switching time in the step (3) is 60 h.
in this embodiment, the demulsification rate of the centrifugal demulsification is 86%, and the final demulsification rate of the emulsion demulsification device is 99.7%.
Example 3:
The present embodiment provides an emulsion breaking apparatus and a processing method thereof, where the structure of the emulsion breaking apparatus is different from that of the emulsion breaking apparatus in embodiment 1 in that: the number of the anti-wetting solid phase tubes in the anti-wetting solid phase tube is 10000, the width of the surface hole is 20nm, the diameter of the tube is 60um, the porosity of the surface of the anti-wetting solid phase tube is 95%, and the amount of the inorganic salt accounts for 15 wt% of the total mass of the inorganic salt and the filler; the inorganic salt cation is the combination of ammonium ions, sodium ions, potassium ions, iron ions, manganese ions and titanium ions; the anion is a combination of nitrate ion, molybdate ion, vanadate ion and chromate ion; the filler is a mixture of bentonite, glass fiber, polyurethane foam and quartz powder. The microorganism in the microorganism culture device is a mixture of nitrite bacteria ATCC19718, pseudomonas Pxy-40, pseudomonas Pxy-82 and pseudomonas putida ML 2.
The emulsion demulsification device is used for treating the emulsion, the emulsion is Daqing oilfield wastewater, and the main components of the organic phase of the emulsion are alkane, aromatic hydrocarbon, polycyclic aromatic hydrocarbon and the like; the water phase mainly comprises water, inorganic salt, high molecular polymer, etc., and the emulsifier mainly comprises oil and solid powder, and is multiple emulsion.
the specific processing flow refers to the processing flow in example 1, with the difference that: the centrifugation speed in the step (1) is 30000r/min, the centrifugation temperature is 60 ℃, and the switching time in the step (3) is 72 h.
In this embodiment, the demulsification rate of the centrifugal demulsification is 81%, and the final demulsification rate of the emulsion demulsification device is 99.8%.
Example 4:
The present embodiment provides an emulsion breaking apparatus and a processing method thereof, where the structure of the emulsion breaking apparatus is different from that of the emulsion breaking apparatus in embodiment 1 in that: the number of the wet reverse-wetting solid phase tubes of the hollow tubes in the reverse-wetting solid phase tube is 5000, the width of the surface hole is 50nm, the diameter of the tube is 100um, and the using amount of the inorganic salt accounts for 30 wt% of the total mass of the inorganic salt and the filler.
The emulsion breaking device is used for treating the emulsion, and the emulsion is the same as the emulsion treated in the example 1.
The specific processing flow refers to the processing flow in example 1.
In this embodiment, the demulsification rate of the centrifugal demulsification is 82%, and the final demulsification rate of the emulsion demulsification device is 99.5%.
example 5:
the present embodiment provides an emulsion breaking apparatus and a processing method thereof, where the structure of the emulsion breaking apparatus is different from that of the emulsion breaking apparatus in embodiment 1 in that: the hollow tube in the anti-wetting solid phase tube has a tube diameter of 10um, and the amount of the inorganic salt accounts for 25 wt% of the total mass of the inorganic salt and the filler.
the emulsion breaking device is used for treating the emulsion, and the emulsion is the same as the emulsion treated in the example 1.
The specific processing flow refers to the processing flow in example 1.
In this embodiment, the demulsification rate of the centrifugal demulsification is 82%, and the final demulsification rate of the emulsion demulsification device is 99.8%.
Comparative example 1:
The present comparative example provides an emulsion breaking apparatus and a treatment method thereof, the structure of which is different from that of the emulsion breaking apparatus of example 1 in that: the emulsion breaking device does not comprise a centrifugal breaking device 2.
The emulsion breaking device is used for treating the emulsion, and the emulsion is the same as the emulsion treated in the example 1.
The specific processing flow refers to the processing flow in example 1, and the difference is that the processing is not carried out with centrifugal demulsification, and is directly carried out with a dewetting demulsification device 3 and a microorganism culture device 4.
In the comparison example, the emulsion breaking rate of the emulsion breaking device is 95%, and it can be seen that the emulsion breaking rate of the wastewater is reduced if the emulsion breaking device is not subjected to centrifugal emulsion breaking treatment, and the anti-wetting emulsion breaking device is easy to block or even fail.
The invention integrates the centrifugal demulsification device and the anti-wetting device into one device, combines multiple demulsification technologies, saves energy, has high efficiency, improves the demulsification efficiency, and ensures that the final demulsification rate can reach 99-100%; the device and the treatment method do not need to add any additive, do not influence the recycling of the organic phase and do not cause secondary pollution; the device and the treatment method can realize full-automatic control and continuous operation, and the demulsification and cleaning of the reactor can be carried out simultaneously, so that the device and the treatment method are accurate, rapid and labor cost is saved; the device and the treatment method have wide application range, can be used for demulsification of an emulsification intermediate layer generated by an extraction method and a back extraction method device, and can also be used for an oil field wastewater oil removal system with high viscosity.
The applicant states that the present invention is illustrated in detail by the above examples, but the present invention is not limited to the above detailed methods, i.e. it is not meant that the present invention must rely on the above detailed methods for its implementation. It should be understood by those skilled in the art that any modification of the present invention, equivalent substitutions of the raw materials of the product of the present invention, addition of auxiliary components, selection of specific modes, etc., are within the scope and disclosure of the present invention.
Claims (24)
1. The emulsion breaking device is characterized by comprising a main reactor (1), wherein the main reactor (1) sequentially comprises a centrifugal emulsion breaking device (2), a dewetting emulsion breaking device (3) and a microorganism culture device (4) from bottom to top; the centrifugal demulsification device (2) is provided with an emulsion inlet, an oil phase outlet, a water phase outlet and a residual emulsion outlet, and the oil phase outlet and the water phase outlet of the centrifugal demulsification device (2) are respectively connected with the organic phase storage tank (5) and the water phase storage tank (6); the anti-wetting demulsification device (3) is provided with a cleaning liquid inlet, an emulsion inlet, an oil phase outlet, a water phase outlet and a cleaning liquid outlet, and the residual emulsion outlet of the centrifugal demulsification device (2) is connected with the emulsion inlet of the anti-wetting demulsification device (3) through a pipeline; an oil phase outlet and a water phase outlet of the anti-wetting demulsification device (3) are respectively connected with an organic phase storage tank (5) and a water phase storage tank (6); the microorganism culture device (4) is provided with a microorganism feeding port and a cleaning liquid outlet, and the cleaning liquid outlet of the microorganism culture device (4) is connected with the cleaning liquid inlet of the anti-wetting demulsification device (3) through a pipeline;
The anti-wetting demulsification device (3) comprises anti-wetting solid phase tubes and a temperature controller, wherein the number of the anti-wetting solid phase tubes is more than or equal to 5000, the anti-wetting solid phase tubes are hollow tubes with holes on the surfaces, the width of the holes on the surfaces of the anti-wetting solid phase tubes is 0.2-50 nm, the porosity of the surfaces of the anti-wetting solid phase tubes is 85-95%, the diameters of the anti-wetting solid phase tubes are 10-100 um, and inorganic salt and filler are filled in the anti-wetting solid phase tubes;
The anti-wetting demulsification device comprises a first anti-wetting device (31) and a second anti-wetting device (32), a residual emulsion outlet of the centrifugal demulsification device (2) is simultaneously connected with an emulsion inlet of the first anti-wetting device (31) and an emulsion inlet of the second anti-wetting device (32), and a cleaning liquid outlet of the microorganism culture device (4) is simultaneously connected with a cleaning liquid inlet of the first anti-wetting device (31) and a cleaning liquid inlet of the second anti-wetting device (32).
2. The emulsion breaking device according to claim 1, wherein a regulating valve is arranged on a connecting pipeline between the residual emulsion outlet of the centrifugal breaking device (2) and the emulsion inlet of the anti-wetting breaking device (3).
3. the emulsion breaking device according to claim 1, wherein a connection pipeline between the cleaning solution outlet of the microorganism culture device (4) and the cleaning solution inlet of the de-wetting emulsion breaking device (3) is provided with a regulating valve.
4. The emulsion breaking device according to claim 1, wherein the emulsion breaking device comprises an automatic control device (7), and the automatic control device (7) is connected with all equipment in the emulsion breaking device.
5. The emulsion breaking device of claim 1, wherein the de-wetting breaking device comprises at least 2 de-wetting apparatuses.
6. the emulsion breaking device according to claim 1, wherein a connection line between the residual emulsion outlet of the centrifugal breaking device (2) and the emulsion inlet of the first anti-wetting apparatus (31) and a connection line between the residual emulsion outlet of the centrifugal breaking device (2) and the emulsion inlet of the second anti-wetting apparatus (32) are provided with regulating valves.
7. The emulsion breaking device according to claim 1, wherein a connection pipeline between the cleaning liquid outlet of the microorganism cultivation device (4) and the cleaning liquid inlet of the first anti-wetting apparatus (31) and a connection pipeline between the cleaning liquid outlet of the microorganism cultivation device (4) and the cleaning liquid inlet of the second anti-wetting apparatus (32) are provided with regulating valves.
8. The emulsion breaking device according to claim 1, wherein the first and second de-wetting apparatuses (31, 32) are identical in structure.
9. The apparatus for demulsifying an emulsion as claimed in claim 1, wherein the number of the anti-wetting solid phase pipes is 8000-10000.
10. the emulsion breaking device according to claim 1, wherein the inorganic salt is used in an amount of 0.5 wt% to 30 wt% based on the total mass of the inorganic salt and the filler.
11. the emulsion breaking device according to claim 10, wherein the inorganic salt is used in an amount of 10 wt% to 25 wt% based on the total mass of the inorganic salt and the filler.
12. The apparatus for demulsifying an emulsion as claimed in claim 1, wherein the cation of the inorganic salt is any one or a combination of at least two of ammonium ion, sodium ion, potassium ion, iron ion, manganese ion or titanium ion.
13. the apparatus for demulsifying an emulsion as claimed in claim 1, wherein the anion of the inorganic salt is any one or a combination of at least two of sulfate ion, nitrate ion, hydroxide ion, fluoride ion, tungstate ion, molybdate ion, vanadate ion, chromate ion, or germanate ion.
14. The emulsion breaking device of claim 1, wherein the inorganic salt is a metallic inorganic salt.
15. The emulsion breaking apparatus of claim 14, wherein the inorganic salt of a metal comprises at least 1 metal element.
16. The emulsion breaking device according to claim 1, wherein the filler is one or a combination of at least two of coal waste residue, bentonite, glass fiber, polyurethane foam, or quartz powder.
17. The emulsion breaking device according to claim 1, wherein the microorganism cultured in the microorganism culturing device (4) is any one or a combination of at least two of nitrite bacteria, pseudomonas or pseudomonas putida.
18. The method of treating an emulsion breaking device according to any one of claims 1 to 17, comprising the steps of:
(1) After emulsion breaking, the emulsion enters a centrifugal emulsion breaking device (2) in the emulsion breaking device for centrifugal emulsion breaking, and an oil phase and a water phase generated by centrifugal emulsion breaking respectively enter an organic phase storage tank (5) and a water phase storage tank (6);
(2) Residual emulsion generated by the centrifugal demulsification in the step (1) enters a de-wetting demulsification device (3) for de-wetting demulsification, and an oil phase and a water phase generated by the de-wetting demulsification respectively enter an organic phase storage tank (5) and a water phase storage tank (6);
(3) And (3) after the anti-wetting demulsification is finished in the step (2), introducing a cleaning solution into the anti-wetting demulsification device (3) through a microorganism culture device (4) to clean the anti-wetting demulsification device (3), and discharging the cleaned waste liquid into the environment.
19. The process of claim 18, wherein the emulsion to be broken in step (1) is a multiple emulsion.
20. The treatment method as claimed in claim 18, wherein the centrifugation rate of the centrifugal demulsification in the step (1) is 20000r/min to 30000 r/min.
21. The process of claim 18, wherein the temperature of the centrifugal demulsification in the step (1) is 40-60 ℃.
22. The treatment method as claimed in claim 18, wherein the demulsification rate of the centrifugal demulsification in the step (1) is 80-90%.
23. The treatment method as claimed in claim 18, wherein the de-wetting demulsification process in the de-wetting demulsification device (3) in the step (2) is as follows:
(a) Residual emulsion generated by the centrifugal demulsification device (2) enters a first anti-wetting device (31) for anti-wetting demulsification treatment; meanwhile, the connection between the centrifugal demulsification device (2) and the second anti-wetting equipment (32) is disconnected, the connection between the microorganism culture device (4) and the first anti-wetting equipment (31) is disconnected, the microorganism culture device (4) and the second anti-wetting equipment (32) are communicated, a cleaning solution is injected into the second anti-wetting equipment (32) through the microorganism culture device (4) to clean the second anti-wetting equipment (32), and the cleaning waste liquid is directly discharged into the environment;
(b) after the first anti-wetting equipment (31) finishes anti-wetting demulsification treatment, disconnecting the centrifugal demulsification device (2) from the first anti-wetting equipment (31), communicating the centrifugal demulsification device (2) with the second anti-wetting equipment (32), and performing anti-wetting operation through the second anti-wetting equipment (32); meanwhile, the connection between the microorganism culture device (4) and the second anti-wetting device (32) is disconnected, the microorganism culture device (4) and the first anti-wetting device (31) are communicated, cleaning liquid is injected into the first anti-wetting device (31) through the microorganism culture device (4) to clean the first anti-wetting device (31), and cleaning waste liquid is directly discharged into the environment;
(c) And (c) repeating the steps (a) to (b).
24. The process according to claim 23, wherein the centrifugal demulsifying means (2) is disconnected from the first anti-wetting apparatus (31) after the first anti-wetting apparatus (31) is subjected to the anti-wetting treatment for 48 to 72 hours in step (b).
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| WO2003000377A1 (en) * | 2001-03-21 | 2003-01-03 | Mantis Oil Separation Limited | Separation of oil and water |
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| CN104419519A (en) * | 2013-08-30 | 2015-03-18 | 中国石油化工股份有限公司 | Method for demulsifying emulsified biodiesel |
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| US20060237372A1 (en) * | 2005-04-22 | 2006-10-26 | Ge Betz, Inc. | Separation of drilling mud emulsions |
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| WO2003000377A1 (en) * | 2001-03-21 | 2003-01-03 | Mantis Oil Separation Limited | Separation of oil and water |
| CN103813842A (en) * | 2011-07-26 | 2014-05-21 | 沙特阿拉伯石油公司 | Dynamic demulsification system for use in a gas-oil separation plant |
| CN103215068A (en) * | 2013-05-07 | 2013-07-24 | 武汉凯迪工程技术研究总院有限公司 | Modification method of biomass pyrolysis oil |
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