CN112983319A - Shale oil-based drilling cutting recycling device and method - Google Patents
Shale oil-based drilling cutting recycling device and method Download PDFInfo
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- CN112983319A CN112983319A CN202110297680.8A CN202110297680A CN112983319A CN 112983319 A CN112983319 A CN 112983319A CN 202110297680 A CN202110297680 A CN 202110297680A CN 112983319 A CN112983319 A CN 112983319A
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- 238000005520 cutting process Methods 0.000 title claims abstract description 36
- 238000000034 method Methods 0.000 title claims abstract description 34
- 239000003079 shale oil Substances 0.000 title claims abstract description 28
- 238000005553 drilling Methods 0.000 title claims abstract description 26
- 238000004064 recycling Methods 0.000 title claims abstract description 14
- 238000000197 pyrolysis Methods 0.000 claims abstract description 72
- 230000005674 electromagnetic induction Effects 0.000 claims abstract description 35
- 238000003795 desorption Methods 0.000 claims abstract description 13
- 238000004321 preservation Methods 0.000 claims abstract description 4
- 239000007789 gas Substances 0.000 claims description 30
- 239000002912 waste gas Substances 0.000 claims description 18
- 239000000243 solution Substances 0.000 claims description 8
- 238000009413 insulation Methods 0.000 claims description 7
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 6
- 239000003929 acidic solution Substances 0.000 claims description 5
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- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 4
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- 238000004140 cleaning Methods 0.000 description 2
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- 239000012530 fluid Substances 0.000 description 2
- 229910001385 heavy metal Inorganic materials 0.000 description 2
- 229910052760 oxygen Inorganic materials 0.000 description 2
- 239000001301 oxygen Substances 0.000 description 2
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- 238000000638 solvent extraction Methods 0.000 description 2
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Images
Classifications
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- E—FIXED CONSTRUCTIONS
- E21—EARTH DRILLING; MINING
- E21B—EARTH DRILLING, e.g. DEEP DRILLING; OBTAINING OIL, GAS, WATER, SOLUBLE OR MELTABLE MATERIALS OR A SLURRY OF MINERALS FROM WELLS
- E21B21/00—Methods or apparatus for flushing boreholes, e.g. by use of exhaust air from motor
- E21B21/06—Arrangements for treating drilling fluids outside the borehole
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F11/00—Treatment of sludge; Devices therefor
- C02F11/10—Treatment of sludge; Devices therefor by pyrolysis
-
- 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
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2101/00—Nature of the contaminant
- C02F2101/30—Organic compounds
-
- 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
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02W—CLIMATE CHANGE MITIGATION TECHNOLOGIES RELATED TO WASTEWATER TREATMENT OR WASTE MANAGEMENT
- Y02W10/00—Technologies for wastewater treatment
- Y02W10/40—Valorisation of by-products of wastewater, sewage or sludge processing
Abstract
The invention relates to a shale oil-based drill chip recycling treatment device which comprises an electromagnetic induction heater 1, a pyrolysis furnace 3, a temperature sensor 7, a pressure sensor 5, a vacuum pump 6, a condenser 8, a temperature controller 13 and an ECU control unit 14, wherein a three-channel one-way valve of an upper cover of the pyrolysis furnace is respectively connected with the vacuum pump 6, an exhaust gas circulation channel 34 and the condenser 8; an electromagnetic induction heater 1 is arranged in the pyrolysis furnace, and the heater is sequentially connected with an electromagnetic induction voltage regulator 2, a temperature controller 13 and an ECU control unit 14. The resource treatment method comprises the following steps: placing the shale oil-based drill cuttings into a pyrolysis furnace; inputting a set thermal desorption temperature and a heat preservation time after the pyrolysis furnace reaches a preset temperature through an ECU (electronic control Unit); vacuumizing the inside of the pyrolysis furnace by using a vacuum pump; and starting the electromagnetic induction heater to realize the resource treatment of the shale oil-based drilling cuttings. The invention can process the drill cuttings to reach the national hazardous waste discharge standard and simultaneously furthest recover the products with useful values, such as petroleum hydrocarbon and the like.
Description
Technical Field
The invention relates to the field of oil and gas well drilling cutting treatment, in particular to a shale oil-based drilling cutting resource treatment device and method.
Background
With the large-scale development of shale gas wells, oil-based drilling fluids with the advantages of strong inhibition, temperature resistance, pollution resistance, lubricity and the like are generally used, and a large amount of shale oil-based drilling fluid solid waste is generated in the drilling process and mainly consists of shale oil-based drilling cuttings. The organic substance is made of organic substances with biodegradability, biotoxicity and slow release property, heavy metals with nondegradable property and biotoxicity, alkaline salts can cause salinization of soil, the substances are difficult to naturally degrade through microorganisms, long-term accumulation can affect the plant growth on the earth surface, water sources, atmosphere and soil pollution can be caused seriously, and the life safety of people is endangered.
The requirements for environmental protection are becoming stricter at home and abroad, and the discharge requirements for the oil-based drilling cuttings are clearly regulated by related laws, regulations and standards. Since 1993, europe requires that the content of oil in solid waste should be less than 1%, and zero emission is achieved after 11 months in 2000. In recent years, oil-based drilling cuttings and related waste treatment are paid great attention to in various drilling enterprises in China, and the oil-containing sludge must be subjected to harmless treatment according to clear requirements of national clean production promotion laws and solid waste environmental pollution prevention laws.
The current oil-bearing rock debris treatment technology at home and abroad comprises the following steps: landfill method, reinjection method, incineration method, chemical cleaning method, solvent extraction method, etc. The landfill method is mainly suitable for water-based drilling cuttings, and has the hidden danger of environmental pollution. The reinjection method cannot utilize resources, has high cost and has hidden danger of environmental pollution. The incineration method is used for completely treating organic matters, but crude oil cannot be recovered, and smoke discharged by combustion contains sulfides, dioxin, heavy metals and the like, so that secondary pollution is serious, and a large amount of carbon dioxide is discharged into the atmosphere. The oil content of the drill cuttings treated by the chemical cleaning method is more than 2 percent, the standard requirement is difficult to meet, the drill cuttings cannot be recycled, the residual sewage and sludge amount is large, secondary pollution is formed, and the chemical treatment agent has single property. The solvent extraction method has high requirement on the tightness of equipment, complex process and high price, is only suitable for drilling cuttings with low oil content, has large amount of residual sewage and sludge and needs secondary treatment.
The electromagnetic induction heating treatment method can lead the oily drilling cuttings to be completely inorganic, the hydrocarbon can be recycled, the treatment speed is high, the drilling cuttings are thoroughly treated, the secondary pollution is less, and the method is not limited by scale. On the one hand, in a heat treatment device, a plurality of pyrolysis furnaces contain a large amount of oxygen, and the inside of the pyrolysis furnaces cannot be in an anaerobic state; on the other hand, the pyrolysis furnace has high heat exchange with the outside, so that the heat utilization rate of the pyrolysis furnace is low. Based on the technical problems, the invention provides the method for recycling the shale oil-based drilling cuttings, the vacuumizing system is utilized to reduce oxygen in the pyrolysis furnace, the anaerobic state in the pyrolysis furnace is ensured, the waste gas circulating system is utilized to improve the energy utilization rate of the pyrolysis furnace, so that resources can be recycled, and good social and economic benefits are obtained while the environment is protected.
Disclosure of Invention
The invention aims to provide a shale oil-based drilling cutting resource treatment device, which adopts an electromagnetic induction heater which is heated uniformly to ensure that a pyrolysis furnace is heated uniformly, adopts a waste gas recycling system, increases the energy utilization rate of the pyrolysis furnace by recycling waste gas and solves the defect of high energy consumption of the pyrolysis furnace; and a waste liquid classification treatment system is adopted to treat the waste liquid in a targeted manner, so that the later working cost is reduced, and the economic benefit is increased.
The invention also aims to provide a method for carrying out resource treatment on shale oil-based drill cuttings by using the device, which solves the technical problems of high energy consumption, low heat utilization rate, complex petroleum hydrocarbon recovery and the like of the conventional thermal desorption method, furthest recovers the valuable products such as the petroleum hydrocarbon and the like when the drill cuttings are treated to reach the national hazardous waste discharge standard, and realizes green recycling of resources.
In order to achieve the technical purpose, the invention adopts the following technical scheme.
A resource treatment device for shale oil-based drilling cuttings comprises an electromagnetic induction heater, an electromagnetic induction voltage regulator, a pyrolysis furnace, a temperature sensor, a pressure sensor, a vacuum pump, a condenser, a PH sensor, a temperature controller, an ECU (electronic control Unit), a liquid collector and a tail gas processor. The pyrolysis furnace consists of an upper cover, a base, a heat insulation layer and an exhaust gas circulation channel, wherein the upper cover is provided with a temperature sensor and a three-channel one-way valve. The three-channel one-way valve is characterized in that a first channel is connected with the pressure sensor and the vacuum pump, a second channel is connected with the waste gas circulation channel, and a third channel is connected with the condenser; one end of the condenser is connected with the waste gas circulation channel and the three-channel one-way valve, and the other end of the condenser is connected with the two-channel one-way valve; a PH sensor is arranged between the condenser and the double-channel one-way valve; one end of the liquid collector is connected with the double-channel one-way valve, and the other end of the liquid collector is connected with the tail gas processor; the electromagnetic induction heater is arranged in the pyrolysis furnace and is connected with an electromagnetic induction voltage regulator and a temperature controller; the temperature sensor, the three-channel one-way valve, the two-channel one-way valve, the PH sensor and the electromagnetic induction voltage regulator are all connected with the ECU control unit.
The pyrolysis furnace is covered with a heat insulation handle, so that the upper cover can be conveniently opened, and a sealing steel ring is arranged between the upper cover and the base, so that the upper cover and the base can be conveniently sealed.
The heating temperature range of the electromagnetic induction heater to the pyrolysis furnace is 100-1000 ℃. The electromagnetic induction heater is regulated by a temperature controller, and the temperature in the pyrolysis furnace is controlled by the voltage of the electromagnetic induction voltage regulator.
The temperature sensor, the electromagnetic induction heater and the temperature controller form a closed-loop control system.
The electromagnetic induction heaters are uniformly distributed on the base of the pyrolysis furnace.
And the vacuum pump is used for vacuumizing the pyrolysis furnace before the pyrolysis furnace starts thermal desorption. When the vacuum pump and the pyrolysis furnace do not work, the three-channel one-way valve is in a closed state; when the vacuum pump works, the pyrolysis furnace does not work, and the three-channel one-way valve only opens the channel connected with one side of the vacuum pump.
The waste gas circulation channel is arranged at the periphery of the pyrolysis furnace, and waste gas in the pyrolysis furnace is secondarily utilized, so that the heat efficiency of the pyrolysis furnace is improved.
The ECU control unit detects the temperature sensor, if the temperature sensor reaches a preset temperature for recycling the waste gas, the three-channel one-way valve is only in an open state with the channel connected with the waste gas circulation channel, and if the temperature does not reach the preset temperature, the three-channel one-way valve is only in an open state with the channel connected with the condenser.
And the PH sensor enables tail gas to be classified through a two-channel one-way valve.
The method for carrying out resource treatment on the shale oil-based drilling cuttings by utilizing the device sequentially comprises the following steps:
(1) opening the pyrolysis furnace, putting the shale oil-based drilling cuttings into the pyrolysis furnace, enabling the pyrolysis furnace to be well sealed, and switching on a power supply;
(2) inputting a set thermal desorption temperature and a heat preservation time after the pyrolysis furnace reaches a preset temperature through an ECU control unit, and setting an opening temperature and a closing temperature of an exhaust gas circulation channel through the ECU control unit;
(3) the vacuum pump is used for vacuumizing the interior of the pyrolysis furnace, so that the interior of the pyrolysis furnace is in an oxygen-free state, and thermal analysis can be carried out harmlessly;
(4) the electromagnetic induction heater is started, the temperature of the electromagnetic induction heater is gradually increased to a preset thermal desorption temperature, the processes of temperature rise, water vapor evaporation, oil gas desorption, condensation, classification treatment and tail gas treatment are sequentially completed in the anaerobic state of the pyrolysis furnace, and the shale oil-based drilling cuttings are recycled.
Preferably, the temperature of thermal analysis in the step (2) is set to be 600-850 ℃ through an ECU (electronic control Unit), and the heat preservation time after the set temperature is reached is 50-90 min.
Preferably, the opening temperature of the waste gas circulation channel in the step (2) is 500 ℃, when the temperature sensor detects that the temperature reaches the preset temperature, the three-channel check valve and the valve on one side of the waste gas circulation channel are in an open state, so that the pyrolysis furnace is in a low-temperature state, the system is in a full heating working condition of the pyrolysis furnace, and after the pyrolysis furnace reaches a certain preset temperature, the waste gas circulation channel is started to improve the efficiency of the pyrolysis furnace, so that the purpose of energy conservation is achieved.
Preferably, when the vacuum pump is used for vacuumizing in the step (3), the vacuum pump stops working when a pressure gauge of the vacuum pump reaches-0.1 Mpa, and a channel of the three-channel check valve, which is connected with the vacuum pump, is in a closed state.
Preferably, the acidic solution used in the classification treatment in step (4) is 10% HNO3Solution and 10% H2O2The mixed solution of the solution and the alkaline solution is 10 percent of NaOH solution and 5 percent of Na2CO3And (3) a mixed solution of the solution.
Compared with the prior art, the invention has the beneficial effects that:
(1) the invention utilizes the electromagnetic induction heater as a heat source for thermal desorption, has the advantage of high thermal desorption efficiency, and can not generate gas polluting the environment while generating heat.
(2) The invention utilizes the circulation of waste gas to preserve the temperature of the pyrolysis furnace, thereby saving energy and protecting environment and improving the working efficiency of the pyrolysis furnace.
(3) The invention ensures that the internal environment of the pyrolysis furnace is in an oxygen-free environment before pyrolysis work by arranging the vacuum pumping pump, thereby fundamentally ensuring that no secondary pollution is generated in the process of thermal desorption.
(4) The method classifies the analyzed organic matters through liquid classification treatment, on one hand, the maximum recovery of petroleum hydrocarbon is ensured, on the other hand, the workload at the later stage is reduced, and the working efficiency is improved.
(5) The method treats the oil content of the shale oil-based drilling cuttings, and meanwhile, valuable recovery is carried out on organic matters (petroleum hydrocarbon) in the shale oil-based drilling cuttings, so that the secondary utilization of wastes is realized to the maximum extent, and the method is environment-friendly and can generate better economic benefit.
Drawings
FIG. 1 is a schematic structural diagram of a shale oil-based drill cuttings recycling device.
FIG. 2 is a schematic view of a pyrolysis furnace.
In the figure: 1-an electromagnetic induction heater, 2-an electromagnetic induction voltage regulator, 3-a pyrolysis furnace, 4-a three-channel one-way valve, 5-a pressure sensor, 6-a vacuum pump, 7-a temperature sensor, 8-a condenser, 9-a PH sensor, 10-a two-channel one-way valve, 11-1-an alkaline solution, 11-2-an acidic solution, 12-1-a tail gas processor, 12-2-a tail gas processor, 13-a temperature controller, 14-an ECU (electronic control Unit), 31-an upper cover, 32-a base, 33-a heat insulation layer, 34-a waste gas circulation channel, 35-a heat insulation handle and 36-a sealing steel ring.
Detailed Description
The present invention will be described in further detail with reference to the accompanying drawings. It should be understood that the specific embodiments described herein are merely illustrative of the invention and are not intended to limit the invention.
See fig. 1. A resource treatment device for shale oil-based drill cuttings comprises an electromagnetic induction heater 1, an electromagnetic induction voltage regulator 2, a pyrolysis furnace 3, a temperature sensor 7, a pressure sensor 5, a vacuum pump 6, a condenser 8, a PH sensor 9, a temperature controller 13 and an ECU (electronic control Unit) 14.
The pyrolysis furnace 3 comprises an upper cover 31, a base 32, a heat insulating layer 33 and an exhaust gas circulating channel 34, wherein the upper cover 31 is provided with a temperature sensor 7 and a three-channel one-way valve 4, the first channel of the three-channel one-way valve is connected with a pressure sensor 5 and a vacuum pump 6, the second channel of the three-channel one-way valve is connected with the exhaust gas circulating channel 34, and the third channel of the three-channel one-way valve is connected with a condenser 8; one end of the condenser is connected with the waste gas circulation channel and the three-channel one-way valve, the other end of the condenser is connected with the two-channel one-way valve 10 through the PH sensor 9, and the two-channel one-way valve is respectively connected with the tail gas processor 12-1 and the tail gas processor 12-2 through the alkaline solution 11-1 and the acidic solution 11-2.
An electromagnetic induction heater 1 is arranged in the pyrolysis furnace, the electromagnetic induction heater is sequentially connected with an electromagnetic induction voltage regulator 2, a temperature controller 13 and an ECU control unit 14, and the temperature sensor, the three-channel check valve, the two-channel check valve and the PH sensor are also connected with the ECU control unit.
A heat insulation handle 35 is arranged above the upper cover 31 of the pyrolysis furnace, and a sealing steel ring 36 is arranged between the upper cover and the base 32.
As shown in fig. 2, one end of the exhaust gas circulation passage 34 is connected to the three-way check valve 4, and the other end is connected to the condenser 8. The waste gas circulation channel is arranged at the periphery of the pyrolysis furnace 3 and surrounds the base 32 of the pyrolysis furnace, and waste gas in the pyrolysis furnace is secondarily utilized, so that the heat efficiency of the pyrolysis furnace is improved. The connection joints at both ends of the exhaust gas circulation channel are well sealed and have means for preventing backflow of the gas flow.
Claims (11)
1. A shale oil base drill chip resourceful treatment device comprises an electromagnetic induction heater (1), an electromagnetic induction voltage regulator (2), a pyrolysis furnace (3), a temperature sensor (7), a pressure sensor (5), a vacuum pump (6), a condenser (8), a PH sensor (9), a temperature controller (13) and an ECU (electronic control unit) control unit (14), and is characterized in that the pyrolysis furnace (3) comprises an upper cover (31), a base (32), a heat insulation layer (33) and an exhaust gas circulation channel (34), the upper cover is provided with the temperature sensor (7) and a three-channel one-way valve (4), the first channel of the three-channel one-way valve is connected with the pressure sensor (5) and the vacuum pump (6), the second channel is connected with the exhaust gas circulation channel (34), and the third channel is connected with the condenser (; one end of the condenser is connected with the waste gas circulation channel and the three-channel one-way valve, the other end of the condenser is connected with the two-channel one-way valve (10) through the PH sensor (9), and the two-channel one-way valve is respectively connected with the tail gas processor through an alkaline solution (11-1) and an acidic solution (11-2); the pyrolysis furnace is internally provided with an electromagnetic induction heater (1), the electromagnetic induction heater is sequentially connected with an electromagnetic induction voltage regulator (2), a temperature controller (13) and an ECU (electronic control unit) (ECU) control unit (14), and the temperature sensor, the three-channel check valve, the two-channel check valve and the PH sensor are connected with the ECU control unit.
2. The recycling device for shale oil-based drill cuttings as claimed in claim 1, wherein a heat insulation handle (35) is arranged above the upper cover (31) of the pyrolysis furnace, and a sealing steel ring (36) is arranged between the upper cover and the base (32).
3. The shale oil-based drill cuttings recycling device according to claim 1, wherein the electromagnetic induction heater heats the pyrolysis furnace at a temperature ranging from 100 ℃ to 1000 ℃.
4. The shale oil-based drill cuttings recycling device according to claim 1, wherein the electromagnetic induction heaters are evenly distributed on the base of the pyrolysis furnace.
5. The shale oil-based drill cuttings recycling device as claimed in claim 1, wherein the exhaust gas circulation channel is arranged at the periphery of the pyrolysis furnace, and the exhaust gas in the pyrolysis furnace is reused, so that the thermal efficiency of the pyrolysis furnace is improved.
6. The shale oil-based drill cuttings recycling device according to claim 1, wherein the pH sensor enables tail gas to be classified and processed through a dual-channel one-way valve.
7. A method for resource treatment of shale oil-based drill cuttings by using the device of claim 1, 2, 3, 4, 5 or 6, comprising the following steps in sequence:
(1) opening the pyrolysis furnace, putting the shale oil-based drilling cuttings into the pyrolysis furnace, and switching on a power supply;
(2) inputting a set thermal desorption temperature and a heat preservation time after the pyrolysis furnace reaches a preset temperature through an ECU control unit, and setting an opening temperature and a closing temperature of an exhaust gas circulation channel through the ECU control unit;
(3) the vacuum pump vacuumizes the interior of the pyrolysis furnace to ensure that the interior of the pyrolysis furnace is in an anaerobic state;
(4) the electromagnetic induction heater is started, the temperature of the electromagnetic induction heater is gradually increased to a preset thermal desorption temperature, the processes of temperature rise, water vapor evaporation, oil gas desorption, condensation, classification treatment and tail gas treatment are sequentially completed in the anaerobic state of the pyrolysis furnace, and the shale oil-based drilling cuttings are recycled.
8. The method of claim 7, wherein the temperature of the thermal desorption set by the ECU control unit in the step (2) is 600 ℃ to 850 ℃, and the holding time after the set temperature is reached is 50 to 90 min.
9. The method of claim 7, wherein the temperature of the opened exhaust gas circulation channel in the step (2) is 500 ℃, and the efficiency of the pyrolysis furnace is improved by activating the exhaust gas circulation channel after the pyrolysis furnace reaches the preset temperature.
10. The method as set forth in claim 7, wherein the vacuum pump stops when a pressure gauge of the vacuum pump reaches-0.1 Mpa while the vacuum pump is vacuumized in the step (3).
11. The method of claim 7, wherein the acidic solution used in the classification treatment in step (4) is 10% HNO3Solution and 10% H2O2The mixed solution of the solution and the alkaline solution is 10 percent of NaOH solution and 5 percent of Na2CO3And (3) a mixed solution of the solution.
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Citations (18)
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