CN108892348B - Method and device for synchronously dehydrating and recovering oil from oily sludge - Google Patents

Method and device for synchronously dehydrating and recovering oil from oily sludge Download PDF

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CN108892348B
CN108892348B CN201810658636.3A CN201810658636A CN108892348B CN 108892348 B CN108892348 B CN 108892348B CN 201810658636 A CN201810658636 A CN 201810658636A CN 108892348 B CN108892348 B CN 108892348B
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oil
preheating
sludge
unit
oily sludge
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CN108892348A (en
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仝坤
张哲娜
张明栋
孙静文
谢水祥
任雯
刘晓辉
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China National Petroleum Corp
CNPC Research Institute of Safety and Environmental Technology Co Ltd
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China National Petroleum Corp
CNPC Research Institute of Safety and Environmental Technology Co Ltd
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    • CCHEMISTRY; METALLURGY
    • C02TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02FTREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F11/00Treatment of sludge; Devices therefor
    • C02F11/10Treatment of sludge; Devices therefor by pyrolysis
    • CCHEMISTRY; METALLURGY
    • C02TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02FTREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F11/00Treatment of sludge; Devices therefor
    • C02F11/12Treatment of sludge; Devices therefor by de-watering, drying or thickening
    • C02F11/121Treatment of sludge; Devices therefor by de-watering, drying or thickening by mechanical de-watering
    • C02F11/122Treatment of sludge; Devices therefor by de-watering, drying or thickening by mechanical de-watering using filter presses
    • CCHEMISTRY; METALLURGY
    • C10PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10GCRACKING 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
    • C10G1/00Production of liquid hydrocarbon mixtures from oil-shale, oil-sand, or non-melting solid carbonaceous or similar materials, e.g. wood, coal
    • CCHEMISTRY; METALLURGY
    • C02TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02FTREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F2103/00Nature of the water, waste water, sewage or sludge to be treated
    • C02F2103/10Nature of the water, waste water, sewage or sludge to be treated from quarries or from mining activities
    • CCHEMISTRY; METALLURGY
    • C02TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02FTREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F2103/00Nature of the water, waste water, sewage or sludge to be treated
    • C02F2103/34Nature of the water, waste water, sewage or sludge to be treated from industrial activities not provided for in groups C02F2103/12 - C02F2103/32
    • C02F2103/36Nature of the water, waste water, sewage or sludge to be treated from industrial activities not provided for in groups C02F2103/12 - C02F2103/32 from the manufacture of organic compounds
    • C02F2103/365Nature of the water, waste water, sewage or sludge to be treated from industrial activities not provided for in groups C02F2103/12 - C02F2103/32 from the manufacture of organic compounds from petrochemical industry (e.g. refineries)
    • CCHEMISTRY; METALLURGY
    • C02TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02FTREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F2303/00Specific treatment goals
    • C02F2303/06Sludge reduction, e.g. by lysis
    • CCHEMISTRY; METALLURGY
    • C10PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10GCRACKING 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
    • C10G2300/00Aspects relating to hydrocarbon processing covered by groups C10G1/00 - C10G99/00
    • C10G2300/10Feedstock materials
    • C10G2300/1003Waste materials
    • CCHEMISTRY; METALLURGY
    • C10PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10GCRACKING 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
    • C10G2300/00Aspects relating to hydrocarbon processing covered by groups C10G1/00 - C10G99/00
    • C10G2300/70Catalyst aspects

Abstract

The invention provides a method and a device for synchronously dehydrating and recovering oil from oily sludge. The method comprises the following steps: mixing the oily sludge with a conditioning agent for preheating; then further heating to make the oily sludge and the conditioning agent perform hydrothermal reaction to obtain hydrothermal oil sludge; then flash evaporation is rapidly carried out to realize the separation of water vapor, oil gas and solid-phase residue, and the generated flash evaporation steam is used for preheating to realize heat recovery; carrying out filter pressing dehydration on the separated flash evaporation oil sludge to obtain solid phase residue and a liquid phase oil-water mixture, standing and layering the oil-water mixture, recovering oil from the upper layer, and recovering organic wastewater from the lower layer; wherein, the conditioning medicament consists of thermosensitive metal oxide, a catalyst and a demulsifier. The process can achieve better effects of reducing and recovering oil at lower hydrothermal temperature, greatly reduces reaction energy consumption, greatly reduces COD (chemical oxygen demand) of the generated waste liquid, reduces toxicity and is easy for biochemical treatment.

Description

Method and device for synchronously dehydrating and recovering oil from oily sludge
Technical Field
The invention belongs to the technical field of environmental protection in the petroleum and petrochemical industry, and relates to a method and a device for synchronously dehydrating and recovering oil from oily sludge.
Background
Oil fields and oil refineries generate and accumulate a large amount of oily sludge every year, such as tank bottom sludge generated in crude oil dehydration, dehydration tanks, oil storage tanks, dirty oil tanks and the like, and oil separation tank bottom sludge, flotation tank scum, biochemical section sludge and the like generated in sewage treatment fields of the oil fields and the oil refineries. These sludges generally have high oil contents (3-50%) and are quite complex in composition; and the oil sludge particles are fine and are flocculent, the water content is high, the water holding capacity is strong, the sludge, the oil and the water are mutually wrapped together, the emulsification is sufficient, the viscosity is high, the dehydration is difficult, and the oil-water-sludge three-phase separation is difficult to realize. The existing oil recovery technology for dehydrating the oily sludge mainly comprises high-temperature steam injection, solvent extraction, pyrolysis and thermal desorption, and the technologies can realize the dehydration of the oily sludge with high water content, but the high-temperature steam injection technology has high operation cost and small treatment capacity, the solvent extraction technology has difficulty in recovering an extractant, and the pyrolysis thermal desorption treatment has high energy consumption and secondary pollution. The heat drying technology can further reduce the water content of the sludge to be below 50 percent, but because the heat energy is directly utilized to quickly evaporate the water in the sludge, the energy consumption is huge, the operation difficulty and the investment cost are high, and the oil gas cannot be effectively recovered. The water absorbent solidification drying technology is simple to operate, but the medicament cost is too high, and the treatment amount is small. The solar drying technology has the advantages of low energy consumption, simple operation and maintenance, low operation and management cost, large occupied area, large influence of weather and seasons on the treatment effect, and odor generation under most conditions.
The sludge hydro-thermal treatment technology is that under higher temperature and pressure (100 ℃, more than 0.101 MPa), the viscous organic matters in the sludge are hydrolyzed, the colloid structure of the sludge is destroyed, and the sludge dehydration performance is effectively improved. According to the difference of the hydrothermal temperature, the method is divided into thermal hydrolysis (100-. The thermal hydrolysis can dissolve part of solid organic matters in the oil sludge, hydrolyze macromolecular organic matters and crack flocs, so that the separation of oil, water and sludge is realized, and further mechanical equipment is adopted to accelerate the liquid-solid separation; the hydrothermal carbonization can coke the sludge and generate a small amount of liquid oil and gas; the sludge is in a liquid state through hydrothermal liquefaction; the hydrothermal gasification temperature exceeds the critical point of water, so that the sludge mainly exists in the form of fuel gas. The pyrohydrolysis and subsequent dehydration process are used as a pretreatment means of municipal sludge, so that the water content of the sludge can be reduced to below 50 percent, and the sludge is gradually accepted by the industry.
The prior perfect hydro-thermal treatment process of the oily sludge is less, the reaction temperature is usually higher, the oil recovery is difficult, the generated organic wastewater has high biological toxicity and the treatment difficulty is high. Based on the characteristics of high oil content and high treatment difficulty of the oil-containing sludge and from the aspects of process safety, energy conservation, sewage treatment and resource recovery, the pyrohydrolysis technology at lower temperature can greatly reduce the viscosity of the oil sludge, does not crack organic matters, does not generate non-condensable gas, malodorous gas and refractory organic matters, is favorable for dehydration of the oil-containing sludge and deep drying of residues and treatment of wastewater, and realizes reduction, harmlessness and recycling of the oil-containing sludge. Therefore, the development of the low-temperature, low-cost and high-efficiency oil sludge hydrothermal dehydration, oil extraction and drying technology is significant.
Disclosure of Invention
Based on the problems in the prior art, the invention aims to provide a device for synchronously dehydrating and recovering oil from oily sludge; the invention also aims to provide a method for synchronously dehydrating and recovering oil from oily sludge by using the device, the process method has low energy consumption and high treatment efficiency, the water content of the treated residue is less than or equal to 50 percent, the mineral oil is effectively recovered, and the volume reduction rate of solid waste is more than 70 percent.
The purpose of the invention is realized by the following technical scheme:
in one aspect, the invention provides a method for synchronously dehydrating and recovering oil from oily sludge, which comprises the following steps:
firstly, mixing oil-containing sludge and a conditioning agent for preheating;
step two, further heating the preheated mixed solution of the oily sludge and the conditioning agent to enable the oily sludge and the conditioning agent to carry out hydrothermal reaction to obtain hydrothermal oil sludge;
quickly flashing the hydrothermal oil sludge at the reaction temperature to separate water vapor, oil gas and solid-phase residues, expanding the flashing volume by 3-10 times, and using the generated flashing vapor (the pressure is 0.3-1.0MPa, the temperature is 95-100 ℃) for preheating in the first step to realize heat recovery; carrying out filter pressing dehydration on the separated flash evaporation oil sludge to obtain solid phase residue and a liquid phase oil-water mixture, standing and layering the oil-water mixture, recovering oil on the upper layer, recovering organic wastewater on the lower layer, and conveying the mixture serving as a carbon source to a sewage treatment plant;
wherein, the conditioning medicament consists of thermosensitive metal oxide, a catalyst and a demulsifier.
In the above method, the organic wastewater is treated in different ways according to the field conditions. If a sewage treatment plant is nearby, the organic wastewater can be conveyed to the sewage treatment plant for treatment, and if the sewage treatment plant does not exist, the organic wastewater is treated by physicochemical, biochemical, advanced treatment and other processes to realize recycling or discharge after reaching the standard. And removing VOCs generated in the treatment process by adopting a biodegradation mode after the VOCs are collected, or recycling, concentrating, treating and disposing.
In the method, the recovered oil can be refined by a butterfly centrifuge and then returned to the system or sold; the dried solid-phase residue can be used as auxiliary fuel, adsorbent or regenerated rubber additive for recycling, and can be reduced and harmless by incineration, pyrolysis and other treatments.
In the above method, preferably, the conditioner comprises 5% -10% of heat-sensitive metal oxide, 60% -80% of catalyst and 10% -30% of demulsifier by mass of the conditioner as 100%.
In the above method, preferably, the amount of the conditioning agent added is 0.3-2.0% of the mass of the oily sludge.
In the above method, preferably, the heat-sensitive metal oxide includes one or more of calcium oxide, iron oxide, titanium oxide, molybdenum oxide, zinc oxide, and the like in combination.
In the above method, preferably, the catalyst comprises one or more of sodium chloride, sodium carbonate, calcium chloride, calcium hydroxide, sodium silicate and the like. The catalyst is a multi-electron electrolyte, and can reduce the temperature and pressure of hydrothermal reaction and reduce the energy consumption of the reaction.
In the above method, preferably, the demulsifier is an ionic surfactant including one or more of carboxylate, sulfate, polyether, quaternary ammonium salt, sulfonate and the like. More preferably, the demulsifier is sodium lauryl sulfate. The demulsifier has the effect of mainly promoting demulsification of oil sludge and realizing high-efficiency separation of oil and water.
In the above method, preferably, in the first step, the preheating is performed by using a preheating tank capable of performing electric preheating, steam preheating, microwave preheating or heat conducting oil preheating. When the system is started, steam can be introduced for preheating or heating in other modes, and the oil gas recovered by subsequent flash evaporation is adopted for preheating after continuous operation, so that the energy consumption of the subsequent process is saved.
In the above method, preferably, the preheating temperature is 90 to 99 ℃.
In the above method, preferably, in the second step, the hydrothermal reaction is a reaction kettle capable of being electrically heated, steam heated, microwave heated or heat-conducting oil heated and capable of stirring.
In the above method, the temperature of the hydrothermal reaction is preferably 120-. After hydrothermal treatment, solid organic matters (colloid and asphaltene) in the high-water-content oil sludge are dissolved, macromolecular organic matters are hydrolyzed into micromolecular organic matters, and floc is broken to realize three-phase separation of oil, water and sludge.
In the above method, preferably, in the third step, a high-pressure filter press is used for filter-pressing dehydration, and the high-pressure filter press presses the filter plate through a hydraulic oil cylinder to realize sludge dehydration.
In the above method, preferably, the dewatering pressure of the high-pressure filter press is 0.5 to 2.0 MPa; the dehydration time is 30-240 min.
In another aspect, the present invention further provides an apparatus for synchronously dewatering and recovering oil from oily sludge, comprising:
the system comprises a preheating unit, a reaction unit, a flash evaporation unit, a dehydration unit and a recovery unit;
the preheating unit, the reaction unit, the flash evaporation unit and the dehydration unit are communicated in sequence;
the preheating unit is used for preheating the oily sludge and the conditioning agent;
the reaction unit is used for heating and stirring to carry out thermal hydrolysis reaction on the oily sludge and the conditioning agent;
the flash evaporation unit is used for separating water vapor, oil gas and solid-phase residues, and flash evaporation steam generated by the flash evaporation unit flows back to the preheating unit for recycling heat;
the dehydration unit is used for removing water in the oily sludge; the recovery unit is used for layering a liquid-phase oil-water mixture and recovering an oil phase;
the conditioning agent consists of a thermosensitive metal oxide, a catalyst and a demulsifier.
The invention has the following beneficial effects:
(1) the water content is greatly reduced after treatment, the volume is greatly reduced, and deep drying and further resource utilization and disposal of the oil sludge are facilitated;
(2) the oil can be effectively recovered, the resource recovery is realized, and the oil recovery rate can be improved by more than 20% after the conditioning separating agent is added;
(3) the treatment temperature is below 200 ℃, partial waste heat can be recycled, the energy consumption and the treatment cost are reduced, and the safety risk is low;
(4) the oil sludge does not need pretreatment, the process is simple, and the efficiency is high;
(5) compared with high-temperature (above 230 ℃) hydrothermal treatment, the amount of non-condensable gas generated by low-temperature pyrohydrolysis below 200 ℃ is reduced, and no odor is generated; organic matters in the solid phase are less carbonized, the COD of the generated waste liquid is greatly reduced, the toxicity is reduced, and the biochemical treatment is easy;
(6) the high-pressure filter press adopted by the invention has the advantages of pressure of over 10MPa, good dehydration effect and capability of recovering part of oil.
Drawings
FIG. 1 is a device for synchronously dehydrating and recovering oil from oily sludge in the embodiment of the invention;
description of the symbols of the drawings:
1 preheating tank, 2 hydrothermal reaction kettle, 3 flash tank, 4 high-pressure filter press and 5 recovery tank.
Detailed Description
The technical solutions of the present invention will be described in detail below in order to clearly understand the technical features, objects, and advantages of the present invention, but the present invention is not limited to the practical scope of the present invention.
Example 1
The embodiment provides a device of oily sludge synchronous dehydration recovered oil, and the device includes:
the system comprises a preheating unit, a reaction unit, a flash evaporation unit, a dehydration unit and a recovery unit;
the preheating unit, the reaction unit, the flash evaporation unit and the dehydration unit are communicated in sequence;
the preheating unit is used for preheating the oily sludge and the conditioning agent;
the reaction unit is used for heating and stirring to carry out thermal hydrolysis reaction on the oily sludge and the conditioning agent;
the flash evaporation unit is used for separating water vapor, oil gas and solid-phase residues, and flash evaporation steam generated by the flash evaporation unit flows back to the preheating unit for recycling heat;
the dehydration unit is used for removing water in the oily sludge; the recovery unit is used for layering the liquid-phase oil-water mixture and recovering the oil phase.
In a preferred embodiment of the present invention, as shown in fig. 1, the preheating unit is a preheating tank 1 capable of performing electric preheating, steam preheating, microwave preheating or heat conducting oil preheating; the reaction unit is a hydrothermal reaction kettle 2 which can be electrically heated, steam heated, microwave heated or heat-conducting oil heated and can be stirred; the flash evaporation unit is a flash evaporation tank 3 and can be used for separating water vapor, oil gas and solid-phase residues; the dehydration unit is a high-pressure filter press 4, the high-pressure filter press 4 is independently developed, the filter plate is extruded by a hydraulic oil cylinder to realize oil sludge dehydration, the pressure can reach more than 10MPa, the dehydration effect is good, and part of oil can be recovered; the recycling unit is a recycling tank 5, the recycling tank 5 can realize layering of oil-water mixtures, oil recycling is realized on the upper layer, and organic wastewater on the lower layer is transported to a sewage treatment plant as a carbon source to be utilized.
Example 2
The embodiment provides a method for synchronously dehydrating and recovering oil from oily sludge, which adopts the device in the embodiment 1, and specifically comprises the following steps:
step one, 500g of scum oil sludge (with the water content of 80-85%) of an oil extraction plant in Xinjiang oil field and 2.5g of conditioning agents (5% of calcium oxide, 70% of sodium chloride and 25% of sodium dodecyl sulfate) are injected into a preheating tank and preheated to 90-99 ℃;
injecting the preheated mixed solution of the oily sludge and the conditioning agent into a hydrothermal reaction kettle, heating the oil sludge to 180 ℃ by electric heating, and reacting for 20-50 minutes to obtain hydrothermal oil sludge;
step three, quickly injecting the hydrothermal oil sludge into a flash tank to separate water vapor, oil gas and solid phase residues, and refluxing the generated flash steam to the preheating tank in the step one to realize heat recovery; the separated flash evaporation oil sludge enters a high-pressure filter press for filter pressing and dehydration to obtain solid phase residue and a liquid phase oil-water mixture, the oil-water mixture enters a recovery tank for standing and layering, the upper layer realizes oil recovery, and the lower layer realizes organic wastewater recovery;
in the embodiment, the water content of the residue obtained after filter pressing and dehydration is 45.3-49.8%, the volume reduction rate is 71-76%, the recovery rate of the oil phase after recovery and stratification is 65.3-72.3%, and the energy recovery rate of flash steam flowing back to the preheating tank is 35.5-42.8%. The COD of the filtrate generated in the embodiment is less than 5000mg/L, and the biological toxicity is low; less non-condensable gas and no foul smell.
Example 3
The embodiment provides a method for synchronously dehydrating and recovering oil from oily sludge, which adopts the device in the embodiment 1, and specifically comprises the following steps:
step one, 500g of scum oil sludge (with the water content of 75-80%) of an oil extraction plant in Xinjiang oil field and 5g of conditioning agents (5% of calcium oxide, 70% of sodium carbonate and 25% of sodium dodecyl sulfate) are injected into a preheating tank and preheated to 90-99 ℃;
injecting the preheated mixed solution of the oily sludge and the conditioning agent into a hydrothermal reaction kettle, introducing 0.45-1.45MPa saturated steam, and reacting for 10-40 minutes to obtain hydrothermal oil sludge;
step three, quickly injecting the hydrothermal oil sludge into a flash tank to separate water vapor, oil gas and solid phase residues, and refluxing the generated flash steam to the preheating tank in the step one to realize heat recovery; the separated flash evaporation oil sludge enters a high-pressure filter press for filter pressing and dehydration to obtain solid phase residue and a liquid phase oil-water mixture, the oil-water mixture enters a recovery tank for standing and layering, the upper layer realizes oil recovery, and the lower layer realizes organic wastewater recovery;
in the embodiment, the water content of the residue obtained after filter pressing and dehydration is 41.5-46.3%, the volume reduction rate is 72-78%, the recovery rate of the oil phase after recovery and stratification is 68.2-74.6%, and the energy recovery rate of flash steam flowing back to the preheating tank is 35.2-40.3%. The COD of the filtrate generated in the embodiment is less than 5000mg/L, and the biological toxicity is low; less non-condensable gas and no foul smell.
Example 4
The embodiment provides a method for synchronously dehydrating and recovering oil from oily sludge, which adopts the device in the embodiment 1, and specifically comprises the following steps:
step one, 500g of thick oil scum (with the water content of 70-75%) of one oil extraction plant in Liaohe oil field and 7.5g of conditioning agents (5% of calcium oxide, 70% of calcium chloride and 25% of sodium dodecyl sulfate) are injected into a preheating tank and preheated to 90-99 ℃;
injecting the preheated mixed solution of the oily sludge and the conditioning agent into a hydrothermal reaction kettle, heating the oil sludge to 200 ℃ by electric heating, and reacting for 10-40 minutes to obtain hydrothermal oil sludge;
step three, quickly injecting the hydrothermal oil sludge into a flash tank to separate water vapor, oil gas and solid phase residues, and refluxing the generated flash steam to the preheating tank in the step one to realize heat recovery; the separated flash evaporation oil sludge enters a high-pressure filter press for filter pressing and dehydration to obtain solid phase residue and a liquid phase oil-water mixture, the oil-water mixture enters a recovery tank for standing and layering, the upper layer realizes oil recovery, and the lower layer realizes organic wastewater recovery;
in the embodiment, the water content of the residue obtained after filter pressing and dehydration is 32.5-38.3%, the volume reduction rate is 78.5-83.2%, the recovery rate of the oil phase after recovery and stratification is 67.2-75.3%, and the energy recovery rate of flash steam flowing back to the preheating tank is 36.7-41.2%. The COD of the filtrate generated in the embodiment is less than 5000mg/L, and the biological toxicity is low; less non-condensable gas and no foul smell.
Comparative example 1
The comparative example is a comparative experiment of example 2, and provides a method for synchronously dehydrating and recovering oil from oily sludge, which adopts the device of example 1, and specifically comprises the following steps:
step one, 500g of scum oil sludge (with the water content of 80-85%) of an oil extraction plant in Xinjiang oil field is injected into a preheating tank to be preheated to 90-99 ℃;
injecting the preheated oil-containing sludge into a hydrothermal reaction kettle, heating the oil sludge to 140 ℃ and 180 ℃ by electric heating, and reacting for 20-50 minutes to obtain hydrothermal oil sludge;
step three, quickly injecting the hydrothermal oil sludge into a flash tank to separate water vapor, oil gas and solid phase residues, and refluxing the generated flash steam to the preheating tank in the step one to realize heat recovery; the separated flash evaporation oil sludge enters a high-pressure filter press for filter pressing and dehydration to obtain solid phase residue and a liquid phase oil-water mixture, the oil-water mixture enters a recovery tank for standing and layering, the upper layer realizes oil recovery, and the lower layer realizes organic wastewater recovery;
in the embodiment, the water content of the residue obtained after filter pressing and dehydration is 55.3-59.7%, the volume reduction rate is 61-67%, the recovery rate of the oil phase after recovery and stratification is 32.1-35.3%, and the energy recovery rate of flash steam flowing back to the preheating tank is 34.5-40.8%. The COD of the filtrate generated in the embodiment is less than 5000mg/L, and the biological toxicity is low; less non-condensable gas and no foul smell.
Comparative example 2
The comparative example is a comparative experiment of example 2, and provides a method for synchronously dehydrating and recovering oil from oily sludge, which adopts the device of example 1, and specifically comprises the following steps:
step one, 500g of scum oil sludge (with the water content of 80-85%) of an oil extraction plant in Xinjiang oil field is injected into a preheating tank to be preheated to 90-99 ℃;
injecting the preheated oil-containing sludge into a hydrothermal reaction kettle, heating the oil sludge to 230-260 ℃ by electric heating, and reacting for 20-50 minutes to obtain hydrothermal oil sludge;
step three, quickly injecting the hydrothermal oil sludge into a flash tank to separate water vapor, oil gas and solid phase residues, and refluxing the generated flash steam to the preheating tank in the step one to realize heat recovery; the separated flash evaporation oil sludge enters a high-pressure filter press for filter pressing and dehydration to obtain solid phase residue and a liquid phase oil-water mixture, the oil-water mixture enters a recovery tank for standing and layering, the upper layer realizes oil recovery, and the lower layer realizes organic wastewater recovery;
in the embodiment, the water content of the residue obtained after filter pressing and dehydration is 46.2-51.7%, the volume reduction rate is 69-73%, the recovery rate of the oil phase after recovery and stratification is 52.1-65.3%, and the energy recovery rate of flash steam flowing back to the preheating tank is 28.1-31.2%. The COD of the filtrate generated in the embodiment is more than 20000mg/L, and the biotoxicity is virulent; a large amount of malodorous gas is produced.
The experiments of the above examples and comparative examples show that the process of the invention can realize that the water content of the treated residue is less than 60%, the volume reduction rate reaches more than 60%, the oil phase is recovered by more than 30%, certain energy is recovered and the energy consumption is reduced at a lower reaction temperature (200 ℃). If the effect of reducing and recovering oil is further improved, the hydrothermal reaction temperature needs to be increased to more than 220 ℃ and 250 ℃, and a large amount of energy is consumed. After the conditioner is added, the hydrothermal reaction can achieve better effects of reducing and recovering oil at a lower hydrothermal temperature (200 ℃), so that the reaction energy consumption is greatly reduced, the COD (chemical oxygen demand) of the generated waste liquid is greatly reduced, the toxicity is reduced, and the biochemical treatment is easy.

Claims (7)

1. A method for synchronously dehydrating and recovering oil from oily sludge comprises the following steps:
firstly, mixing oil-containing sludge and a conditioning agent for preheating;
step two, further heating the preheated mixed solution of the oily sludge and the conditioning agent to enable the oily sludge and the conditioning agent to carry out hydrothermal reaction to obtain hydrothermal oil sludge; the temperature of the hydrothermal reaction is 120-;
step three, quickly carrying out flash evaporation on the hydrothermal oil sludge at the reaction temperature to realize the separation of water vapor, oil gas and solid-phase residues, and using the generated flash evaporation steam for preheating in the step one to realize heat recovery; carrying out filter pressing dehydration on the separated flash evaporation oil sludge to obtain solid phase residue and a liquid phase oil-water mixture, standing and layering the oil-water mixture, recovering oil on the upper layer, and recovering organic wastewater on the lower layer;
wherein the conditioning medicament consists of a thermosensitive metal oxide, a catalyst and a demulsifier; the heat-sensitive metal oxide comprises calcium oxide and/or molybdenum oxide; the catalyst comprises one or more of sodium chloride, sodium carbonate, calcium hydroxide and sodium silicate in combination; the demulsifier is sodium dodecyl sulfate;
the addition amount of the conditioning agent is 0.3-2.0% of the mass of the oily sludge.
2. The method of claim 1, wherein: in the first step, the preheating is performed by using a preheating tank capable of performing electric preheating, steam preheating, microwave preheating or heat conducting oil preheating.
3. The method of claim 2, wherein: the preheating temperature is 90-99 ℃.
4. The method of claim 1, wherein: in the second step, the hydrothermal reaction adopts a reaction kettle which can be heated by electricity, steam, microwaves or heat-conducting oil and can be stirred.
5. The method of claim 1, wherein: in the third step, a high-pressure filter press is adopted for filter pressing dehydration, and the high-pressure filter press extrudes the filter plate through a hydraulic oil cylinder to realize oil sludge dehydration.
6. The method of claim 5, wherein: the dehydration pressure of the high-pressure filter press is 0.5-2.0 MPa; the dehydration time is 30-240 min.
7. An apparatus for synchronously dehydrating and recovering oil from oily sludge, which comprises:
the system comprises a preheating unit, a reaction unit, a flash evaporation unit, a dehydration unit and a recovery unit;
the preheating unit, the reaction unit, the flash evaporation unit and the dehydration unit are communicated in sequence;
the preheating unit is used for preheating the oily sludge and the conditioning agent;
the reaction unit is used for heating and stirring to carry out thermal hydrolysis reaction on the oily sludge and the conditioning agent; the reaction temperature is 120-200 ℃, the pressure is 0.2-1.45MPa, and the stirring time is 10-50 min;
the flash evaporation unit is used for separating water vapor, oil gas and solid-phase residues, and flash evaporation steam generated by the flash evaporation unit flows back to the preheating unit for recycling heat;
the dehydration unit is used for removing water in the oily sludge; the recovery unit is used for layering a liquid-phase oil-water mixture and recovering an oil phase;
the conditioning agent consists of a thermosensitive metal oxide, a catalyst and a demulsifier; the heat-sensitive metal oxide comprises calcium oxide and/or molybdenum oxide; the catalyst comprises one or more of sodium chloride, sodium carbonate, calcium hydroxide and sodium silicate in combination; the demulsifier is sodium dodecyl sulfate;
the addition amount of the conditioning agent is 0.3-2.0% of the mass of the oily sludge.
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