CN113736504A - Oil rock oil sludge cracking separation process - Google Patents
Oil rock oil sludge cracking separation process Download PDFInfo
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- CN113736504A CN113736504A CN202111050670.0A CN202111050670A CN113736504A CN 113736504 A CN113736504 A CN 113736504A CN 202111050670 A CN202111050670 A CN 202111050670A CN 113736504 A CN113736504 A CN 113736504A
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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
- C10G1/00—Production of liquid hydrocarbon mixtures from oil-shale, oil-sand, or non-melting solid carbonaceous or similar materials, e.g. wood, coal
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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
- C10G1/00—Production of liquid hydrocarbon mixtures from oil-shale, oil-sand, or non-melting solid carbonaceous or similar materials, e.g. wood, coal
- C10G1/002—Production of liquid hydrocarbon mixtures from oil-shale, oil-sand, or non-melting solid carbonaceous or similar materials, e.g. wood, coal in combination with oil conversion- or refining processes
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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
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- Oil, Petroleum & Natural Gas (AREA)
- Life Sciences & Earth Sciences (AREA)
- Wood Science & Technology (AREA)
- Chemical Kinetics & Catalysis (AREA)
- General Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Treatment Of Sludge (AREA)
Abstract
The invention discloses an oil rock oil sludge cracking separation process, which comprises the following steps: step S1: mixing the oil rock with the wave-absorbing material; step S2: putting the mixed materials into a cracking kettle; step S3: pumping out air in the cracking kettle through a vacuumizing device; step S4: feeding microwave power into the waveguide pressure window to heat the oil rock; step S5: continuously pumping out reaction gas in the cracking kettle through a vacuumizing device; step S6: liquefying the reaction gas into a liquid state by a condenser; step S7: the liquid liquefied into liquid enters an oil-water separator for oil-water separation; step S8: and discharging residues in the cracking kettle to finish separation. In the invention, the microwave heating separation process is used, so that the material consumption is less, the steps are simple, the final separation effect is good, and the microwave heating separation process is an excellent and feasible separation process. The separated oil can be reused, and the residual residue meets the standard of pollutant control standard in agricultural sludge GB4284-1984, and the required oil content is less than 0.3 percent.
Description
Technical Field
The invention belongs to the technical field of crude oil leakage recovery processing in the oil extraction industry, and particularly relates to an oil-rock oil sludge cracking separation process.
Background
The oil sludge is a typical dangerous pollutant containing crude oil, silt and the like generated in industrial processes such as oil exploitation, storage and transportation, refining and processing and the like, has variable properties and complex phase state, has great harm to the environment and needs to be treated.
However, the existing oil sludge separation treatment agent mainly utilizes complex compounds such as conventional alkaline or acidic chemical auxiliary agents, highly toxic solvents, surfactants and the like, and has the disadvantages of large usage amount, high separation process cost, serious secondary pollution, poor crude oil stripping effect, incomplete separation and low oil content of the treated silt which does not reach the discharge standard.
Disclosure of Invention
The invention aims to provide an oil-rock oil sludge cracking and separating process, which aims to solve the problems of large using amount and high separation cost of oil sludge treated by using chemical agents in the prior art provided by the background technology.
In order to solve the technical problems, the technical scheme adopted by the invention is as follows:
a process for cracking and separating oil sludge from oil rock comprises the following steps:
step S1: mixing oil rock with wave-absorbing material
Step S2: putting the mixed materials into a cracking kettle;
step S3: pumping out air in the cracking kettle through a vacuumizing device;
step S4: feeding microwave power into the waveguide pressure window to heat the oil rock;
step S5: continuously pumping out reaction gas in the cracking kettle through a vacuumizing device;
step S6: liquefying the reaction gas into a liquid state by a condenser;
step S7: the liquid enters an oil-water separator for oil-water separation;
step S8: and discharging residues in the cracking kettle to finish separation.
According to the technical scheme, the ratio of the oil rocks to the wave-absorbing material in the step S1 is as follows: 0.3 to 10 percent.
According to the technical scheme, the air pressure in the cracking kettle in the step S3 is kept at-0.09-0.097 MPa.
According to the technical scheme, the temperature in the cracking kettle in the step S4 is increased to 450 ℃.
According to the technical scheme, in the step S7, the water at the lower layer enters the water receiving tank, and the oil at the upper layer enters the oil receiving tank.
According to the technical scheme, in the step S8, the residue in the cracking kettle is discharged through a temperature-reducing oxygen-isolating discharging machine.
According to the technical scheme, the wave-absorbing material in the step S1 is silicon carbide powder, carbon-based iron powder or graphite powder and a modified substance thereof.
According to the technical scheme, the vacuumizing device comprises a connecting pipeline, a buffer tank and a vacuum pump, the connecting pipeline is connected to a pipeline between the condenser and the oil-water separator, and the connecting pipeline is connected with the buffer tank and the vacuum pump.
According to the technical scheme, the condenser is connected with the vacuumizing device.
Compared with the prior art, the invention has the following beneficial effects:
in the present invention, a separation process for separating oil rocks using microwave heating is feasible. The microwave heating separation process is adopted, so that the material consumption is less, the steps are simple, the final separation effect is good, and the microwave heating separation process is an excellent and feasible separation process. The separated oil can be reused, and the residual residue meets the standard of pollutant control standard in agricultural sludge GB4284-1984, and the required oil content is less than 0.3 percent.
Drawings
FIG. 1 is a flow chart of a process for cracking and separating oil and oil sludge of oil rock;
FIG. 2 is a schematic view of the overall structure of the apparatus of the present invention;
FIG. 3 is a second schematic view of the overall structure of the device of the present invention;
FIG. 4 is a schematic view of the structure of a cracking kettle;
FIG. 5 is a schematic structural view of a temperature-reducing and oxygen-isolating discharging machine.
In the figure: 1-a cracking kettle, 2-an oil-water separator, 3-a water receiving tank, 4-an oil receiving tank, 5-a vacuum pump, 6-a microwave generator, 7-a straight waveguide, 8-a circulator, 9-a water load, 10-a coupler, 11-a waveguide window, 12-a waveguide connecting pipe, 13-a buffer tank, 14-a temperature-reducing and oxygen-isolating discharging machine, 15-a screw conveyor, 16-a motor, 17-a nitrogen inlet, 18-a solid residue inlet, 19-a solid residue outlet, 20-a water inlet, 21-a water outlet, 22-a stirring rod, 23-a helical blade, 24-a gas phase outlet and 25-a heat-insulating layer.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Example one
As shown in fig. 1, the oil-rock oil-sludge cracking separation process comprises the following steps:
step S1: mixing oil rock with wave-absorbing material
Step S2: putting the mixed materials into a cracking kettle 1;
step S3: pumping out air in the cracking kettle 1 through a vacuumizing device;
step S4: feeding microwave power into the waveguide pressure window to heat the oil rock;
step S5: continuously pumping out the reaction gas in the cracking kettle 1 through a vacuumizing device;
step S6: liquefying the reaction gas into a liquid state by a condenser;
step S7: the liquid enters an oil-water separator 2 for oil-water separation;
step S8: and discharging the residue in the cracking kettle 1 to finish the separation.
Further, the wave-absorbing material in the step 1 is silicon carbide powder, carbon-based iron powder or graphite powder.
Further, the power of the microwave is 5800MHz/2450MHz/915 MHz.
The use ratio of the wave-absorbing material in the step S1 is as follows: 0.3 to 10 percent.
In the step S3, the pressure in the cracking kettle 1 is kept at-0.09-0.097 MPa.
The temperature in the cracking vessel 1 in step S4 was raised to 450 ℃.
In step S7, the water in the lower layer enters the water receiving tank 3, and the oil in the upper layer enters the oil receiving tank 4.
In step S8, the residue in the cracking reactor 1 is discharged through the temperature-decreasing oxygen-insulating discharging device 14.
The wave-absorbing material in the step S1 is silicon carbide powder, carbon-based iron powder or graphite powder and a modified substance thereof.
The vacuumizing device comprises a connecting pipeline, a buffer tank 13 and a vacuum pump 5, the connecting pipeline is connected to a pipeline between the condenser and the oil-water separator 2, and the connecting pipeline is connected with the buffer tank 13 and the vacuum pump 5.
The condenser is connected with a vacuum-pumping device.
A stirring device is arranged on the cracking kettle 1, and comprises a stirring motor, a coupler, a stirring rod 22 and a helical blade 23; the stirring motor is arranged above the cracking kettle 1, and the stirring rod 22 is connected with the first motor 16 through a coupler; the helical blade 23 is arranged on the stirring rod 22;
the cracking kettle 1 is provided with a waveguide connecting pipe 12, microwaves enter the cracking kettle 1 from the waveguide connecting pipe 12, and the waveguide length of the waveguide connecting pipe 12 is 80-400 mm. The top of the cracking kettle 1 is provided with a gas phase outlet 24.
Further, the outside of pyrolysis kettle 1 still is provided with heat preservation 25, and heat preservation 25 is used for keeping the inside temperature of pyrolysis kettle 1, prevents that the temperature dissipation is too fast, leads to the separation effect variation.
Further, the temperature-reducing and oxygen-isolating discharging machine 14 comprises a screw conveyer 15, a motor 16 and a nitrogen inlet 17, wherein a rotating shaft of the screw conveyer 15 is connected with the motor 16; the nitrogen inlet 17 is connected with a nitrogen supply device; the screw conveyer 15 is provided with a solid residue inlet 18, a solid residue outlet 19, a water inlet 20 and a water outlet 21. Wherein, solid residue entry 18 is connected with pyrolysis kettle 1, transports the residue in pyrolysis kettle 1 through screw conveyer 15 to carry nitrogen gas through supplying nitrogen device in to screw conveyer 15 and cool down, discharge through refrigerated residue at last.
Further, a buffer tank 13 is arranged between the condenser and the oil-water separator 2, and the buffer tank 13 is connected with a vacuum pumping device. The vacuumizing device is used for vacuumizing, and the buffer tank 13 prevents the vacuumizing device from being too high in vacuumizing speed and unstable in airflow to cause impact and damage to the device.
Further, the microwave generating device is connected with a waveguide which is connected with the cracking kettle 1; the cracking kettle 1 is provided with a waveguide connecting pipe 12, microwaves enter the cracking kettle 1 from the waveguide connecting pipe 12, and a waveguide window 11 is arranged on the waveguide connecting pipe 12.
Further, the microwave generating device is connected with the bent waveguide, the bent waveguide is connected with the circulator 8, the circulator 8 is connected with the coupler 10, the coupler 10 is connected with the rectangular waveguide (namely, the straight waveguide 7), and the rectangular waveguide is connected with the circular waveguide through the rectangular-circular transition waveguide;
further, the circulator 8 is also connected with a water load 9, and the water load 9 can absorb the reflected power from the cracking kettle 1 to play a role in protecting the microwave source (the microwave generator 6).
The circulator 8 is a one-way device for microwave transmission, and can be used together with the water load 9 to transmit the reflected power generated in the cracking kettle 1 to the water load 9, so that the water load 9 is converted into heat after absorption and dissipated, and the reflected power is prevented from being transmitted to the microwave source (the microwave generator 6) to influence the stable use of the microwave source.
The coupler 10 can couple out small power below 100mw in a high-power microwave environment for detecting the magnitude of microwave power and whether power transmission is normal. The coupler 10 is connected to a power meter through a cable (coaxial cable), and the power meter is used for displaying specific power values.
The rectangular waveguide and the bent waveguide are devices for conducting microwave power, which is conducted from a microwave source to the pyrolysis tank 1 and fed.
The reflected power generated in the cracking kettle 1 can reduce the efficiency of the cracking kettle 1, meanwhile, the reflected microwave power can also interfere with the stable work and the service life of the microwave source, and the three-pin regulator can regulate the magnitude of the reflected power within a certain range to keep the reflected power at the lowest possible level.
The waveguide pressure window is a sealed device made of microwave-transparent material, and can isolate air flow without influencing microwave power to pass through.
Example two
1. 100 kg of oil rock is taken and mixed with 0.5 percent (namely 0.5 kg) of wave-absorbing material. Then the mixed materials are put into a cracking kettle 1 through a feeder. The stirring rod 22 is used for stirring to make the wave-absorbing material uniformly distributed in the oil shale mixture. Then, the air in the cracking kettle 1 is pumped out by a vacuum pumping device, so that the air pressure in the cracking kettle 1 is kept at-0.09 MPa. The negative pressure pumping has three purposes: firstly, guiding the volatilized oil gas to enter a gas phase outlet 24; secondly, isolating oxygen; and thirdly, preventing the oil gas from burning in a high-temperature environment.
2. Microwave is fed into the cracking kettle 1 through a waveguide pressure window to heat the materials. Wherein, the power of microwave is 915MHz, heats the material through microwave, when the temperature reaches 80 ℃, the moisture is evaporated at first, when the temperature reaches 110 ℃, the oil gas in the oil sludge begins to volatilize, when the temperature reaches 450 ℃, the oil in the oil shale is exhausted.
3. The gas pumped by the vacuum pumping device is liquefied into liquid state by a condenser, enters the oil-water separator 2 and is separated by the oil-water separator 2, the water at the lower layer enters the water receiving tank 3, and the oil at the upper layer enters the oil receiving tank 4. The residue in the cracking kettle 1 is discharged through a temperature-reducing oxygen-isolating discharging machine 14. The content of the residual oil is 0.28 percent through detection, meets the national environmental protection standard and can return to the land. (please confirm the correctness of experimental data)
The oil gas and the water vapor of the oil rock are volatilized and the residue is settled by heating through the microwave, so that the effect of separating the oil rock into the oil, the water and the residue is achieved. However, water is the most capable of absorbing microwaves in the oil rocks, the water is evaporated most quickly along with the rise of the temperature, and the residual mixture is not sensitive to the microwaves and cannot be heated continuously. 0.3 to 10 percent of wave-absorbing material is mixed in the oil rock, the wave-absorbing material absorbs microwave to generate heat, and the temperature is continuously increased to heat the oil rock, thereby achieving the purpose of separation.
EXAMPLE III
This embodiment is a further refinement of embodiment two. 1. 100 kg of oil rock is taken and mixed with 2 percent (namely 2 kg) of wave-absorbing material. Then the mixed materials are put into a cracking kettle 1 through a feeder. The stirring rod 22 is used for stirring to make the wave-absorbing material uniformly distributed in the oil shale mixture. Then, the air in the cracking vessel 1 was evacuated by a vacuum evacuation device to maintain the pressure in the cracking vessel 1 at-0.097 MPa.
2. Microwave is fed into the cracking kettle 1 through a waveguide pressure window to heat the materials. Wherein the microwave power is 2450MHz, the microwave is used for heating the material, when the temperature reaches 80 ℃, the water is firstly evaporated, when the temperature reaches 110 ℃, the oil gas in the oil sludge begins to volatilize, and when the temperature reaches 450 ℃, the oil in the oil shale is completely discharged.
3. The gas pumped by the vacuum pumping device is liquefied into liquid state by a condenser, enters the oil-water separator 2 and is separated by the oil-water separator 2, the water at the lower layer enters the water receiving tank 3, and the oil at the upper layer enters the oil receiving tank 4. The residue in the cracking kettle 1 is discharged through a temperature-reducing oxygen-isolating discharging machine 14. The content of the residual oil is 0.26 percent through detection, meets the national environmental protection standard and can return to the land.
Example four
This embodiment is a further refinement of embodiment two. 1. 100 kg of oil rock is taken and mixed with 5 percent (namely 5 kg) of wave-absorbing material. Then the mixed materials are put into a cracking kettle 1 through a feeder. The stirring rod 22 is used for stirring to make the wave-absorbing material uniformly distributed in the oil shale mixture. Then, the air in the cracking kettle 1 is pumped out by a vacuum pumping device, so that the air pressure in the cracking kettle 1 is kept at-0.09 MPa.
2. Microwave is fed into the cracking kettle 1 through a waveguide pressure window to heat the materials. Wherein, the power of the microwave is 915MHz, the material is heated by the microwave, the moisture at 80 ℃ is firstly evaporated, when the temperature reaches 110 ℃, the oil gas in the oil sludge begins to volatilize, and when the temperature reaches 450 ℃, the oil in the oil shale is completely discharged.
3. The gas pumped by the vacuum pumping device is liquefied into liquid state by a condenser, enters the oil-water separator 2 and is separated by the oil-water separator 2, the water at the lower layer enters the water receiving tank 3, and the oil at the upper layer enters the oil receiving tank 4. The residue in the cracking kettle 1 is discharged through a temperature-reducing oxygen-isolating discharging machine 14. The content of the residual oil is 0.25 percent through detection, meets the national environmental protection standard and can return to the land.
EXAMPLE five
This embodiment is a further refinement of embodiment two. 1. 100 kg of oil rock is taken and mixed with 8 percent (namely 8 kg) of wave-absorbing material. Then the mixed materials are put into a cracking kettle 1 through a feeder. The stirring rod 22 is used for stirring to make the wave-absorbing material uniformly distributed in the oil shale mixture. Then, the air in the cracking vessel 1 was evacuated by a vacuum evacuation device to maintain the pressure in the cracking vessel 1 at-0.095 MPa.
2. Microwave is fed into the cracking kettle 1 through a waveguide pressure window to heat the materials. Wherein the microwave power is 2450MHz, the material is heated by microwave, the water at 80 ℃ is evaporated firstly, when the temperature reaches 110 ℃, the oil gas in the oil sludge is volatilized, and when the temperature reaches 450 ℃, the oil in the oil shale is substantially exhausted.
3. The gas pumped by the vacuum pumping device is liquefied into liquid state by a condenser, enters the oil-water separator 2 and is separated by the oil-water separator 2, the water at the lower layer enters the water receiving tank 3, and the oil at the upper layer enters the oil receiving tank 4. The residue in the cracking kettle 1 is discharged through a temperature-reducing oxygen-isolating discharging machine 14. The content of the residual oil is 0.21 percent through detection, meets the national environmental protection standard and can return to the land.
It is noted that, herein, relational terms such as first and second, and the like may be used solely to distinguish one entity or action from another entity or action without necessarily requiring or implying any actual such relationship or order between such entities or actions. Also, the terms "comprises," "comprising," or any other variation thereof, are intended to cover a non-exclusive inclusion, such that a process, method, article, or apparatus that comprises a list of elements does not include only those elements but may include other elements not expressly listed or inherent to such process, method, article, or apparatus.
Finally, it should be noted that: although the present invention has been described in detail with reference to the foregoing embodiments, it will be apparent to those skilled in the art that changes may be made in the embodiments and/or equivalents thereof without departing from the spirit and scope of the invention. Any modification, equivalent replacement, or improvement made within the spirit and principle of the present invention should be included in the protection scope of the present invention.
Claims (9)
1. A process for cracking and separating oil sludge from oil rock is characterized by comprising the following steps: the method comprises the following steps:
step S1: mixing the oil rock with a wave-absorbing material;
step S2: putting the mixed materials into a cracking kettle;
step S3: pumping out air in the cracking kettle through a vacuumizing device;
step S4: the microwave generating device feeds microwave power into the waveguide pressure window to heat the oil rock;
step S5: continuously pumping out reaction gas in the cracking kettle through a vacuumizing device;
step S6: liquefying the reaction gas into a liquid state by a condenser;
step S7: the liquid enters an oil-water separator for oil-water separation;
step S8: and discharging residues in the cracking kettle to finish separation.
2. The oil rock and oil sludge cracking separation process according to claim 1, characterized in that: the ratio of the oil rock to the wave-absorbing material in the step S1 is as follows: 0.3 to 10 percent.
3. The oil rock and oil sludge cracking separation process according to claim 1, characterized in that: in step S3, the pressure in the cracking kettle is kept between-0.09 MPa and-0.097 MPa.
4. The oil rock and oil sludge cracking separation process according to claim 1, characterized in that: the temperature in the pyrolysis reactor in step S4 was raised to 450 ℃.
5. The oil rock and oil sludge cracking separation process according to claim 1, characterized in that: in step S7, the water in the lower layer enters the water receiving tank, and the oil in the upper layer enters the oil receiving tank.
6. The oil rock and oil sludge cracking separation process according to claim 1, characterized in that: in step S8, the residue in the cracking kettle is discharged through a temperature-reducing and oxygen-isolating discharging machine.
7. The oil rock and oil sludge cracking separation process according to claim 1, characterized in that: the wave-absorbing material in the step S1 is silicon carbide powder, carbon-based iron powder or graphite powder and a modified substance thereof.
8. The oil rock and oil sludge cracking separation process according to claim 1, characterized in that: the vacuumizing device comprises a connecting pipeline, a buffer tank and a vacuum pump, the connecting pipeline is connected to a pipeline between the condenser and the oil-water separator, and the connecting pipeline is connected with the buffer tank and the vacuum pump.
9. The oil rock and oil sludge cracking separation process according to claim 1, characterized in that: the condenser is connected with a vacuum-pumping device.
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| US20110114470A1 (en) * | 2009-11-19 | 2011-05-19 | Chang Yul Cha | Process and system for recovering oil from tar sands using microwave energy |
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| CN208373058U (en) * | 2018-06-07 | 2019-01-15 | 张家港保税区宝成环保科技有限公司 | For greasy filth, waste oil, Regenevating Waste Activated Carbon microwave cracking machine |
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2021
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| US20110114470A1 (en) * | 2009-11-19 | 2011-05-19 | Chang Yul Cha | Process and system for recovering oil from tar sands using microwave energy |
| CN108465449A (en) * | 2018-06-07 | 2018-08-31 | 张家港保税区宝成环保科技有限公司 | For greasy filth, the microwave cracking machine and cleavage method of waste oil, Regenevating Waste Activated Carbon |
| CN208373058U (en) * | 2018-06-07 | 2019-01-15 | 张家港保税区宝成环保科技有限公司 | For greasy filth, waste oil, Regenevating Waste Activated Carbon microwave cracking machine |
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