CN104946291A - Method for treating drill cuttings through supercritical CO2 extraction - Google Patents
Method for treating drill cuttings through supercritical CO2 extraction Download PDFInfo
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- CN104946291A CN104946291A CN201510309224.5A CN201510309224A CN104946291A CN 104946291 A CN104946291 A CN 104946291A CN 201510309224 A CN201510309224 A CN 201510309224A CN 104946291 A CN104946291 A CN 104946291A
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Abstract
The invention specifically provides a method for treating drill cuttings through supercritical CO2 extraction. The method comprises the following steps: (1) pretreating oil-bearing drill cuttings through a drill cutting pretreatment unit to screen out oil-based drill cuttings of which the particle sizes are larger than or equal to 800 micrometers; (2), treating gas CO2 in a CO2 supply unit into liquid CO2 through a liquefaction unit; (3) treating liquid CO2 through a pressurization and heating unit to obtain supercritical liquid CO2; (4) conducting several hours' extraction on supercritical liquid CO2 mixed with an entrainer and the oil-based drill cuttings in an extraction unit to isolate drill cuttings and an oil-bearing CO2 supercritical fluid; (5) conducting cooling and depressurization treatment on the oil-bearing CO2 supercritical fluid to ensure that supercritical liquid CO2 is converted into gas CO2, and oil and gas CO2 are separated by a separator. The invention is simple and convenient in process, small in occupied area, pollution-free, low in energy consumption and high in extraction rate; the oil content of the treated drill cuttings is lower than or equal to 1%, and meets the technical indicator requirement.
Description
Technical field
The invention belongs to oily waste treatment technical field, be specifically related to a kind of supercritical CO
2the method of extraction treatment oil-contained drilling cuttings, drilling cuttings oleaginousness≤1% (before process, oleaginousness is 10% ~ 20%) after making process, and realize reusing of oil-base mud.
Background technology
Oil-contained drilling cuttings contains a large amount of oil and other objectionable impuritiess, not up to standardly produces huge harm by environment as dealt with improperly or processing.
At present, generally adopt that Thermal desorption is separated to oil-contained drilling cuttings abroad, buried, the biological degradation of de-oiling purification, burning etc. focus on method, the method for the employing reinjection into reservoir (U.S.'s forbidding) also had processes.Buried after the simple de-oiling of domestic current employing, burn, the degraded of pre-treatment artifact or several treatment process such as reinjection into reservoir.Burn and can produce new pollution to environment, also waste a large amount of base oil resources, when environmental protection pressure continues to increase at home, the method is eliminated simultaneously.
Stratum reinjection technology is carried out to oil-contained drilling cuttings and also there is the shortcomings such as technical difficulty is large, risk is high, processing costs is high, be not suitable for large-scale promotion application.Reinjection technology was once carried out to oil-contained drilling cuttings in 19-3 oil field, Peng Lai as CNOOC and the exploitation of Kang Fei petroleum cooperation, was altogether about 4800m to 24 mouthfuls of wells
3oil-contained drilling cuttings carries out re-injection, and processing costs is up to more than 9,000 ten thousand yuans.
Great Wall drilling project company adopts biological degradation method process oil-contained drilling cuttings, treating, in the oil base landwaste that improvement is stacked, gas blower and evacuator are installed, be pressed in process material by force by adding biological modeling, microbial nutrition additive, synergistic agent and pH adjusting agent etc. in air, lower boiling volatile organic matter is directly drawn out of with air, and high boiling heavy constituent is under the effect of biological modeling, be thoroughly degraded to CO
2and H
2o, after 20 days, test landwaste oleaginousness is 0.8%.Although the biological degradation method of Great Wall probing is environment friendly and pollution-free, long processing period, production efficiency is low, and occupied ground is large.
Thermal desorption partition method is a kind of oil-contained drilling cuttings treatment process that SWACO company adopts, drilling cuttings is heated to the distillation temperature of the oil polluting drilling cuttings, then this temperature is kept, until remove all oil, after all contaminants is all separated, starting to remove steam, condensate, is water and oil by liquid phase separation.Thermal desorption method is a kind of method that application is comparatively ripe at present, but its power consumption is high, and equipment flowsheet is complicated, and processing cost is high.
For the defect that current oil-contained drilling cuttings treatment process exists, need to find a kind of economical and effective, object that environmental friendliness, the oil-contained drilling cuttings treatment process technology that safe and reliable, production efficiency is high process on a large scale to reach oil-contained drilling cuttings.
Summary of the invention
The object of the invention is to overcome existing oil-contained drilling cuttings treatment process equipment flowsheet complexity, power consumption and cost high, and the problem that extraction yield is low.
For this reason, the invention provides a kind of supercritical CO
2the method of extraction treatment oil-contained drilling cuttings, comprises the steps:
1) oil-contained drilling cuttings thing is carried out pre-treatment through drilling cuttings pretreatment unit, filter out the oil-based drill cuttings thing of particle diameter >=800 μm;
2) by CO
2gaseous state CO in feeding unit
2liquid CO is processed into through liquefaction unit
2;
3) by step 2) in the liquid CO that obtains
2through supercharging intensification cell processing to supercritical state;
4) by step 3) CO of supercritical state that obtains
2mixing entrainment agent and step 1) the oil-based drill cuttings thing that obtains contacts and extracts a few hours in extraction cells, isolates the CO of drilling cuttings slag and oil-containing
2supercutical fluid;
5) by the CO of oil-containing
2supercutical fluid through decrease temperature and pressure process, supercritical state CO
2become gaseous state CO
2, oil and gaseous state CO
2be separated through separator, oil carries out detection storage, gaseous state CO
2recycle.
Above-mentioned steps 4) in the CO of supercritical state
2flow be 35g/min.
Above-mentioned steps 4) in entrainment agent be methyl alcohol or ethanol.
Above-mentioned steps 4) in the extraction temperature of extraction cells be 50 ~ 80 DEG C.
Above-mentioned steps 4) in the extracting pressure of extraction cells be 15 ~ 30MPa.
Above-mentioned steps 4) in the CO of supercritical state
2contacting the time extracted with oil-based drill cuttings thing is 1 ~ 3h.
Above-mentioned steps 4) in the dosage of entrainment agent be 5 ~ 10mL/100g.
Above-mentioned steps 5) in cooling to process the minimum temperature of being down to be 32 DEG C.
Above-mentioned steps 5) in the step-down process pressure of being down to be below 7MPa.
Beneficial effect of the present invention:
(1) this supercritical CO provided by the invention
2the method treatment temp of extraction treatment oil-contained drilling cuttings is low, supercritical CO
2close to room temperature (30 ~ 70 DEG C) and CO
2extract under gas blanket, effectively prevent oxidation and the loss of heat-sensitive substance, complete retains biological activity, and can high boiling point, the material of low volatility, easily pyrolysis extracts below its boiling temperature.
(2) this supercritical CO provided by the invention
2the method of extraction treatment oil-contained drilling cuttings changes CO in system by changing pressure and temperature
2solubility property, thus improve the yield of product, its extraction yield >95%.
(3) this supercritical CO provided by the invention
2the method of extraction treatment oil-contained drilling cuttings is pollution-free, whole process, without organic solvent, effectively prevent the residual of solvent toxicity under traditional extraction conditions, also prevent the murder by poisoning of leaching process to human body and the pollution to environment simultaneously, without waste gas, waste water, even waste residue also can fully utilize.
(4) this supercritical CO provided by the invention
2the method energy consumption of extraction treatment oil-contained drilling cuttings is low, when the Co 2 supercritical fluid being full of solute flows through separator, because pressure drop makes CO
2reply rapidly with extract the two-phase (gas-liquid separation) that becomes and be separated and separate immediately, there is not the phase transition process of material, save a large amount of heat of phase transformation, significantly reduce production cost, and simplify technical process; CO
2recycle, without the need to recycling design, not only extraction efficiency is high and energy consumption is less, cost-saving.
(5) this supercritical CO provided by the invention
2supercritical CO in the method for extraction treatment oil-contained drilling cuttings
2solubility property can change, under certain temperature condition, as long as change pressure or add the material that suitable entrainment agent can extract opposed polarity, often change a CO
2solubility property, just equal, at a kind of new solvent of use, thus to realize a set of supercritical CO
2extraction plant is applicable to the extraction of tens kinds, tens kinds materials.
(6) this supercritical CO provided by the invention
2the method treatment scheme of extraction treatment oil-contained drilling cuttings is easy, and floor space is little, and after the method process drilling cuttings oleaginousness≤1% (process before oleaginousness be 10% ~ 20%).
Below with reference to accompanying drawing, the present invention is described in further details.
Accompanying drawing explanation
Fig. 1 is supercritical CO of the present invention
2the process flow sheet of the method for extraction treatment oil-contained drilling cuttings.
Embodiment
Embodiment 1:
High in order to overcome existing oil-contained drilling cuttings treatment process equipment flowsheet complexity, power consumption and cost, and the problem that extraction yield is low, present embodiments provide a kind of supercritical CO as shown in Figure 1
2the method of extraction treatment oil-contained drilling cuttings, comprises the steps:
1) oil-contained drilling cuttings thing is carried out pre-treatment through drilling cuttings pretreatment unit, filter out the oil-based drill cuttings thing of particle diameter >=800 μm.
2) by CO
2gaseous state CO in feeding unit
2liquid CO is processed into through liquefaction unit
2.
3) by step 2) in the liquid CO that obtains
2through supercharging intensification cell processing to supercritical state.
4) by step 3) CO of supercritical state that obtains
2mixing entrainment agent and step 1) the oil-based drill cuttings thing that obtains contacts and extracts a few hours in extraction cells, isolates the CO of drilling cuttings slag and oil-containing
2supercutical fluid.
5) by the CO of oil-containing
2supercutical fluid through decrease temperature and pressure process, supercritical state CO
2become gaseous state CO
2, oil and gaseous state CO
2be separated through separator, oil carries out detection storage, gaseous state CO
2recycle.
This invention adopts supercritical CO
2technology abstraction technique, selects a kind of entrainment agent simultaneously, in the supercritical state by the CO of presetting flow
2with the oil-contained drilling cuttings material contact number hour of particle diameter>=800 μm, it is made selectively the composition of polarity size, boiling point height and molecular size range to be extracted successively, then the method by decompression, intensification makes supercutical fluid become common gases, base oil is then separated out completely, thus reaches the object of separating-purifying.
This supercritical CO provided by the invention
2the method treatment scheme of extraction treatment oil-contained drilling cuttings is easy, floor space is little, pollution-free, energy consumption is low, whole process is without organic solvent, effectively prevent the residual of solvent toxicity under traditional extraction conditions, prevent the murder by poisoning of leaching process to human body and the pollution to environment, without waste gas, waste water, even waste residue also can fully utilize, CO simultaneously
2can be recycled, without the need to recycling design, not only extraction efficiency is high and energy consumption is less, cost-saving; In addition, supercritical CO
2solubility property can change, under certain temperature condition, as long as change pressure or add the material that suitable entrainment agent can extract opposed polarity, often change a CO
2solubility property, just equal, at a kind of new solvent of use, thus to realize a set of supercritical CO
2extraction plant is applicable to the extraction of tens kinds, tens kinds materials.
Embodiment 2:
Present embodiments provide a kind of supercritical CO
2the method of extraction treatment oil-contained drilling cuttings, comprises the steps:
1) oil-contained drilling cuttings thing is carried out pre-treatment through drilling cuttings pretreatment unit, filter out the oil-based drill cuttings thing of particle diameter >=800 μm.
2) by CO
2gaseous state CO in feeding unit
2liquid CO is processed into through liquefaction unit
2, wherein CO
2feeding unit is CO
2gas holder, liquefaction unit is membrane compressor.
3) by step 2) in the liquid CO that obtains
2through supercharging intensification cell processing to supercritical state, wherein supercharging intensification unit is accumulator still.
4) by step 3) CO of supercritical state that obtains
2mixing entrainment agent and step 1) the oil-based drill cuttings thing that obtains contacts and extracts a few hours in extraction cells, isolates the CO of drilling cuttings slag and oil-containing
2supercutical fluid, wherein, extraction cells is extraction kettle, and entrainment agent is methyl alcohol, and the dosage of entrainment agent is the CO of 5mL/100g, supercritical state
2flow be 35g/min, the extraction temperature of extraction cells is 80 DEG C, and the extracting pressure of extraction cells is the CO of 15MPa, supercritical state
2contacting the time extracted with oil-based drill cuttings thing is 3h.
5) by the CO of oil-containing
2supercutical fluid is through decrease temperature and pressure process, and it is 32 DEG C that temperature is reduced to minimum temperature from extraction temperature, and pressure is reduced to below 7MPa from extracting pressure, supercritical state CO
2become gaseous state CO
2, oil and gaseous state CO
2be separated through separator, oil carries out detection storage, isolated gaseous state CO
2enter purification system, after dehydrating and removing impurities, return membrane compressor recycle or then return in gas holder after extraction terminates and store for future use.
Embodiment 3:
Present embodiments provide a kind of supercritical CO
2the method of extraction treatment oil-contained drilling cuttings, comprises the steps:
1) oil-contained drilling cuttings thing is carried out pre-treatment through drilling cuttings pretreatment unit, filter out the oil-based drill cuttings thing of particle diameter >=800 μm.
2) by CO
2gaseous state CO in feeding unit
2liquid CO is processed into through liquefaction unit
2, wherein CO
2feeding unit is CO
2gas holder, liquefaction unit is membrane compressor.
3) by step 2) in the liquid CO that obtains
2through supercharging intensification cell processing to supercritical state, wherein supercharging intensification unit is accumulator still.
4) by step 3) CO of supercritical state that obtains
2mixing entrainment agent and step 1) the oil-based drill cuttings thing that obtains contacts and extracts a few hours in extraction cells, isolates the CO of drilling cuttings slag and oil-containing
2supercutical fluid, wherein, extraction cells is extraction kettle, and entrainment agent is methyl alcohol, and the dosage of entrainment agent is the CO of 7.5mL/100g, supercritical state
2flow be 35g/min, the extraction temperature of extraction cells is 60 DEG C, and the extracting pressure of extraction cells is the CO of 20MPa, supercritical state
2contacting the time extracted with oil-based drill cuttings thing is 2h.
5) by the CO of oil-containing
2supercutical fluid is through decrease temperature and pressure process, and it is 32 DEG C that temperature is reduced to minimum temperature from extraction temperature, and pressure is reduced to below 7MPa from extracting pressure, supercritical state CO
2become gaseous state CO
2, oil and gaseous state CO
2be separated through separator, oil carries out detection storage, isolated gaseous state CO
2enter purification system, after dehydrating and removing impurities, return membrane compressor recycle or then return in gas holder after extraction terminates and store for future use.
Embodiment 4:
Present embodiments provide a kind of supercritical CO
2the method of extraction treatment oil-contained drilling cuttings, comprises the steps:
1) oil-contained drilling cuttings thing is carried out pre-treatment through drilling cuttings pretreatment unit, filter out the oil-based drill cuttings thing of particle diameter >=800 μm.
2) by CO
2gaseous state CO in feeding unit
2liquid CO is processed into through liquefaction unit
2, wherein CO
2feeding unit is CO
2gas holder, liquefaction unit is membrane compressor.
3) by step 2) in the liquid CO that obtains
2through supercharging intensification cell processing to supercritical state, wherein supercharging intensification unit is accumulator still.
4) by step 3) CO of supercritical state that obtains
2mixing entrainment agent and step 1) the oil-based drill cuttings thing that obtains contacts and extracts a few hours in extraction cells, isolates the CO of drilling cuttings slag and oil-containing
2supercutical fluid, wherein, extraction cells is extraction kettle, and entrainment agent is methyl alcohol, and the dosage of entrainment agent is the CO of 10mL/100g, supercritical state
2flow be 35g/min, the extraction temperature of extraction cells is 50 DEG C, and the extracting pressure of extraction cells is the CO of 30MPa, supercritical state
2contacting the time extracted with oil-based drill cuttings thing is 1h.
5) by the CO of oil-containing
2supercutical fluid is through decrease temperature and pressure process, and it is 32 DEG C that temperature is reduced to minimum temperature from extraction temperature, and pressure is reduced to below 7MPa from extracting pressure, supercritical state CO
2become gaseous state CO
2, oil and gaseous state CO
2be separated through separator, oil carries out detection storage, isolated gaseous state CO
2enter purification system, after dehydrating and removing impurities, return membrane compressor recycle or then return in gas holder after extraction terminates and store for future use.
Embodiment 5:
The present embodiment to the processing parameter setting that embodiment 2, embodiment 3 and embodiment 4 relate to go forward side by side row relax test, process after drilling cuttings sample be labeled as 1#, 2# and 3# respectively; Adopt Infrared Oil Determination Instrument (JKY-2B), measure drilling cuttings 1# and 2# after process and 3# sample total oil content amount with reference to " CJ/T 221-2205 infrared spectrophotometry ", detected result is in table 1.
Table 1:
As shown in Table 1, all≤1%, reach technical requirement, wherein embodiment 3 treatment effect is best for the drilling cuttings oleaginousness after embodiment 2, embodiment 3 and embodiment 4 three kinds of art breading.
Detect the main performance index of the base oil reclaimed after process, main performance index contrast before and after base oil process, result is as shown in table 2.
Table 2:
Sequence number | Test item | Base oil before process | Base oil after reclaiming |
1 | Density (g/cm 3) | 778 | 776 |
2 | Kinematic viscosity (mm 2/s) | 2.6 | 2.7 |
3 | Flash-point (DEG C) | 85 | 88 |
As shown in Table 2, after reclaiming, base oil is compared without considerable change with base oil performance before process.
In addition, prepare oil-base mud with the base oil after reclaiming, and detect oil-base mud performance, detected result is in table 3.
Table 3:
As shown in Table 3, the oil-base mud performance index prepared by refiltered oil are substantially unchanged compared with oil-base mud index index before process, stable performance, meet and reclaim service requirements.
In sum, this supercritical CO provided by the invention
2the method treatment scheme of extraction treatment oil-contained drilling cuttings is easy, and floor space is little, pollution-free, and energy consumption is low, and extraction yield is high, and drilling cuttings oleaginousness≤1% after process, meets technical requirement.
More than exemplifying is only illustrate of the present invention, does not form the restriction to protection scope of the present invention, everyly all belongs within protection scope of the present invention with the same or analogous design of the present invention.
Claims (9)
1. a supercritical CO
2the method of extraction treatment oil-contained drilling cuttings, is characterized in that: comprise the steps:
1) oil-contained drilling cuttings thing is carried out pre-treatment through drilling cuttings pretreatment unit, filter out the oil-based drill cuttings thing of particle diameter >=800 μm;
2) by CO
2gaseous state CO in feeding unit
2liquid CO is processed into through liquefaction unit
2;
3) by step 2) in the liquid CO that obtains
2through supercharging intensification cell processing to supercritical state;
4) by step 3) CO of supercritical state that obtains
2mixing entrainment agent and step 1) the oil-based drill cuttings thing that obtains contacts and extracts a few hours in extraction cells, isolates the CO of drilling cuttings slag and oil-containing
2supercutical fluid;
5) by the CO of oil-containing
2supercutical fluid through decrease temperature and pressure process, supercritical state CO
2become gaseous state CO
2, oil and gaseous state CO
2be separated through separator, oil carries out detection storage, gaseous state CO
2recycle.
2. supercritical CO as claimed in claim 1
2the method of extraction treatment oil-contained drilling cuttings, is characterized in that: described step 4) in the CO of supercritical state
2flow be 35g/min.
3. supercritical CO as claimed in claim 1
2the method of extraction treatment oil-contained drilling cuttings, is characterized in that: described step 4) in entrainment agent be methyl alcohol or ethanol.
4. supercritical CO as claimed in claim 1
2the method of extraction treatment oil-contained drilling cuttings, is characterized in that: described step 4) in the extraction temperature of extraction cells be 50 ~ 80 DEG C.
5. supercritical CO as claimed in claim 1
2the method of extraction treatment oil-contained drilling cuttings, is characterized in that: described step 4) in the extracting pressure of extraction cells be 15 ~ 30MPa.
6. supercritical CO as claimed in claim 1
2the method of extraction treatment oil-contained drilling cuttings, is characterized in that: described step 4) in the CO of supercritical state
2contacting the time extracted with oil-based drill cuttings thing is 1 ~ 3h.
7. supercritical CO as claimed in claim 1
2the method of extraction treatment oil-contained drilling cuttings, is characterized in that: described step 4) in the dosage of entrainment agent be 5 ~ 10mL/100g.
8. supercritical CO as claimed in claim 1
2the method of extraction treatment oil-contained drilling cuttings, is characterized in that: described step 5) in cooling to process the minimum temperature of being down to be 32 DEG C.
9. supercritical CO as claimed in claim 1
2the method of extraction treatment oil-contained drilling cuttings, is characterized in that: described step 5) in the step-down process pressure of being down to be below 7MPa.
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CN111410981A (en) * | 2019-01-07 | 2020-07-14 | 中国石油天然气股份有限公司 | Supercritical CO with entrainer assistance2Method for extracting oil in drilling waste |
CN110451745A (en) * | 2019-07-10 | 2019-11-15 | 合肥通用机械研究院有限公司 | A kind of oil base drilling wastes supercritical processing system |
CN110451745B (en) * | 2019-07-10 | 2021-11-23 | 合肥通用机械研究院有限公司 | Oil-based drilling waste supercritical treatment system |
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CN111006933B (en) * | 2019-12-02 | 2020-10-23 | 中国石油大学(北京) | Method and device for determining the quantity of oil extracted by an extraction experiment |
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CN115261051A (en) * | 2022-06-24 | 2022-11-01 | 重庆工商大学 | Extraction method and equipment for oil-based drilling cuttings |
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