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CN113955919B - Phase transfer agent for high-water-content oil sludge - Google Patents

Phase transfer agent for high-water-content oil sludge Download PDF

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CN113955919B
CN113955919B CN202011394525.XA CN202011394525A CN113955919B CN 113955919 B CN113955919 B CN 113955919B CN 202011394525 A CN202011394525 A CN 202011394525A CN 113955919 B CN113955919 B CN 113955919B
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water
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phase transfer
sludge
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CN113955919A (en
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胡幼元
段征宇
徐菊花
龙承冬
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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
    • C02F11/12Treatment of sludge; Devices therefor by de-watering, drying or thickening
    • C02F11/14Treatment of sludge; Devices therefor by de-watering, drying or thickening with addition of chemical agents
    • C02F11/147Treatment of sludge; Devices therefor by de-watering, drying or thickening with addition of chemical agents using organic substances
    • 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
    • C10G1/04Production of liquid hydrocarbon mixtures from oil-shale, oil-sand, or non-melting solid carbonaceous or similar materials, e.g. wood, coal by extraction

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  • Engineering & Computer Science (AREA)
  • Oil, Petroleum & Natural Gas (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • General Chemical & Material Sciences (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Organic Chemistry (AREA)
  • Wood Science & Technology (AREA)
  • Hydrology & Water Resources (AREA)
  • Environmental & Geological Engineering (AREA)
  • Water Supply & Treatment (AREA)
  • Production Of Liquid Hydrocarbon Mixture For Refining Petroleum (AREA)
  • Treatment Of Sludge (AREA)

Abstract

The invention is suitable for the field of high-water-content oil sludge treatment, and provides a phase transfer agent for high-water-content oil sludge, which comprises alcohol Rm- (OH) n or low-carbon alcohol ether solvent with the weight percentage being 10-80% according to the higher water content in the high-water-content oil sludge, wherein m=1-4, n=1-3, and aromatic hydrocarbon solvent or mineral oil with the weight percentage being higher according to the higher oil content in the high-water-content oil sludge, and the weight percentage is 20-90%. The defect in the prior art is overcome, and the pollution influence of the oil sludge on the environment can be reduced; and then the oil and water in the oil sludge can be recovered, so that the aim of recycling the resource is fulfilled.

Description

Phase transfer agent for high-water-content oil sludge
Technical Field
The invention belongs to the field of high-water-content oil sludge treatment, and particularly relates to a phase transfer agent for high-water-content oil sludge.
Background
Sludge is generally classified into three categories: oilfield sludge, refining sludge and storage and transportation sludge. The oilfield sludge refers to sludge produced in the petroleum drilling and production process and mainly comprises floor sludge, drilling waste sludge and sedimentation sludge of an oil extraction and water injection system. The oil sludge is a mixture formed by the overflow and leakage of crude oil, infiltration of ground, soil, sand, water and the like during petroleum drilling. Drilling waste mud is a complex multiphase system formed by mud, sewage, cuttings and the like discharged from drilling. In addition, the oil extraction water injection system can generate a large amount of oily sewage in the secondary oil extraction and tertiary oil extraction processes, and the oily sewage is separated and settled to generate settled oil sludge of the oil extraction water injection system. The refined oil sludge, namely the oil sludge of the oil refinery, mainly refers to three-sludge of oil refinery wastewater, and comprises oil separation tank bottom sludge, floatation tank scum, biochemical tank residual activated sludge, a small amount of tank bottom sludge of a dirty oil tank and the like generated in the treatment process of the oil refinery wastewater. The storage and transportation fatlute refers to fatlute generated by depositing a small amount of mechanical impurities, sand grains, mud, heavy metal salts, paraffin, smart blue and other heavy components on the bottom of a container in the storage and transportation processes of crude oil and petroleum products, and fatlute generated in the transportation processes is still treated by adopting an outward transportation limiting stacking method after preliminary sedimentation and dehydration in a plurality of enterprises at present. Along with the stricter environmental protection laws and regulations of various countries in the world, the demands of oil sludge reduction, stabilization and recycling treatment are higher and higher.
The three kinds of oil sludge have complex organic matter components, high water content, good stability and high treatment difficulty, and belong to high-water-content oil sludge. The oil content is generally 8% -10%, the water content is 60% -80%, and the oil sludge contains about 10% -15% of solid substances (mud, sand and the like), and the high-water-content oil sludge is a complex system formed by mixing water, solid substances and oil, so that the interfacial film between the water and the oil prevents coalescence among water drops/oil drops, and the interfacial film is very stable due to the surface active substances (including colloid and asphaltene) existing between the interfaces. There are two different types of emulsions in sludge: one is an oil-in-water emulsion, i.e., an O/W emulsion, with water as the continuous phase and a water-insoluble organic liquid as the dispersed phase; the other is a water-in-oil emulsion, i.e., a W/O emulsion, which uses water as the dispersed phase and a water-insoluble organic liquid as the continuous phase. In addition, the solid forms vary in size, and multiple emulsions such as water-in-oil-in-water (W/O/W) or oil-in-water-in-oil (O/W/O) may be encapsulated. So the treatment of high water content sludge becomes a great difficulty in hazardous waste treatment.
At home and abroad, various treatment technologies of high-water-content oil sludge are developed, mainly including landfill method, incineration method, solvent extraction method, centrifugal dewatering method, thermal analysis method, thermochemical demulsification method, microwave treatment method, microorganism treatment method and the like. The landfill method is most adopted at present, occupies a large amount of land resources, and wastes resources and pollutes the environment because the high-water-content oil sludge cannot be treated. The incineration method has the advantages that the water content in the high-water-content oil sludge is higher than 80%, so that the energy consumption is extremely high, a large amount of waste gas is generated, and the equipment investment and the operation cost are high. The solvent extraction method uses a large amount of extractant in the solvent extraction process, so that the cost is high, and the equipment maintenance cost, depreciation cost and treatment cost are high in the process; the centrifugal dehydration method is only a pure decrement method, and because the water in the high-water-content oil sludge is mainly in an emulsified state, the dehydration is difficult, and the aim of treating the high-water-content oil sludge cannot be really achieved. The thermal analysis method also has the problems of high energy consumption, waste gas generation and the like, and also has the problems of inflammability, explosiveness, equipment coking and blockage. Various agents used in the thermochemical demulsification method have certain effects on simple high-water-content oil sludge, and have no obvious demulsification effect on high-water-content oil sludge with complex components, high viscosity, high colloid and high asphaltene. At present, the microwave treatment method is only researched in a laboratory and has the defects of high energy consumption, high safety risk of an operation site and the like. The microbiological method has large occupied area, long treatment period and limited environmental climate temperature, and can only treat the oily sludge with the oil content lower than 5 percent, and the treatment is limited.
In recent years, some domestic enterprises treat the oil sludge by adopting a method of drying and reducing after sulfuric acid acidification treatment, but the oil sludge cannot continue to operate due to the problems of safety risks such as hydrogen sulfide generation, inflammability and explosiveness of low-flash-point substances and the like. In general, no set of mature treatment methods exist in China, and particularly, long, stable, safe, full and excellent operation treatment methods can be achieved.
Disclosure of Invention
The invention aims to provide a phase transfer agent for high-water-content oil sludge, which overcomes the defects in the prior art and can reduce the pollution influence of the oil sludge on the environment; and then the oil and water in the oil sludge can be recovered, so that the aim of recycling the resource is fulfilled.
The present invention is achieved by a phase transfer agent for high water-containing sludge comprising transferring free water, capillary water and emulsified water of oil-in-water/water-in-oil type in high water-containing sludge from a stable high water-containing sludge colloid system to the phase transfer agent and having a weight percentage of 10% -80% of an alcohol Rm- (OH) n or a low alcohol ether solvent according to a higher water content in the high water-containing sludge, wherein m=1 to 4, n=1 to 3, and dissolving oil in the high water-containing sludge colloid system and eliminating charges in the oil, colloid in the oil, asphaltenes, thereby destroying the phase balance inherent in the high water-containing sludge colloid system, reconstructing the sludge colloid system, and having a weight percentage of 20% -90% of an aromatic hydrocarbon solvent or mineral oil according to a higher oil content in the high water-containing sludge.
The invention further adopts the technical scheme that: the phase transfer agent also comprises a surfactant which promotes the mutual solubility of the alcohol Rm- (OH) n or the low-carbon alcohol ether solvent and the aromatic hydrocarbon solvent or the mineral oil and plays roles in demulsification, oil displacement and auxiliary phase transfer in a high-water-content oil sludge system, and the weight percentage of the surfactant is 0.2% -2% of the total metering of the alcohol Rm- (OH) n or the low-carbon alcohol ether solvent and the aromatic hydrocarbon solvent or the mineral oil.
The invention further adopts the technical scheme that: the phase transfer agent also comprises an organic phenol antioxidant and a polymerization inhibitor for preventing high-water-content oil sludge from coking and scaling in the processes of drying and recycling oil and water, and the weight percentage of the phase transfer agent is 0.2% -1% of the total metering of the alcohol Rm- (OH) n or the low-carbon alcohol ether solvent and the aromatic hydrocarbon solvent or the mineral oil.
The invention further adopts the technical scheme that: the weight percentage of the alcohol Rm- (OH) n or the low-carbon alcohol ether solvent is 40-65%.
The invention further adopts the technical scheme that: the weight percentage of the aromatic hydrocarbon solvent or mineral oil is 35% -60%.
The invention further adopts the technical scheme that: the alcohol Rm- (OH) n is one or more of ethanol, isopropanol, ethylene glycol or diethylene glycol, and the low-carbon alcohol ether solvent is one or more of ethylene glycol monomethyl ether, ethylene glycol dimethyl ether, diethylene glycol dimethyl ether, cyclohexanediol monomethyl ether or ethylene glycol butyl ether.
The invention further adopts the technical scheme that: the aromatic hydrocarbon solvent is one or more of benzene, toluene, mixed xylene, mixed trimethylbenzene, tetramethylbenzene or ethylbenzene, and the mineral oil is one or more of gasoline, diesel oil, raffinate oil or aromatic hydrocarbon solvent oil.
The invention further adopts the technical scheme that: the surfactant comprises one or more of propylene glycol embedded polyether, alkylphenol ethoxylate, castor oil/hydrogenated castor oil polyoxyethylene ether, polyoxyethylene polyoxypropylene ether, phenol aldehyde resin polyoxypropylene polyoxyethylene ether or acrylamide modified copolymer.
The invention further adopts the technical scheme that: the organic phenol, the amine antioxidant and the polymerization inhibitor are one or more of p-phenylenediamine, hydroquinone, p-tert-butyl catechol or p-benzyl aminophenol.
The beneficial effects of the invention are as follows: the phase transfer agent performs phase transfer separation drying treatment on the oil sludge with high water content in the oil refinery, effectively abandons the problems of large consumption and high consumption of the hydrogen sulfide gas and the extractant discharged by acidification tempering, has the advantages of recycling utilization of the phase transfer agent, good drying effect, simple operation, low safety risk, low energy consumption and small investment, and has remarkable reduction and recycling effects.
Detailed Description
The invention provides a phase transfer agent for high-water-content oil sludge, which comprises the steps of transferring free water, capillary water and oil-in-water/water-in-oil emulsified water in the high-water-content oil sludge from a stable high-water-content oil sludge colloid system to the phase transfer agent, wherein the weight percentage of an alcohol Rm- (OH) n or a low-carbon alcohol ether solvent is 10-80% according to the higher water content in the high-water-content oil sludge, m=1-4 and n=1-3, and dissolving oil in the high-water-content oil sludge colloid system and eliminating charges in the oil, colloid and asphaltene in the oil, so that the original phase balance of the high-water-content oil sludge colloid system is damaged, the oil sludge colloid system is reconstructed, and the weight percentage of an aromatic hydrocarbon solvent or mineral oil is 20-90% according to the higher oil content in the high-water-content oil sludge. In the process of reconstructing the oil sludge colloid system, the electric double layers and the interfacial film of various colloidal particles are broken, so that on one hand, oil molecules are favorably transferred into a phase transfer agent, the effect that oil is transferred into phase transfer agent liquid from the surface of a solid substance and the inside of the solid substance is wrapped, the oil is favorably recovered, on the other hand, the aggregation and sedimentation of the solid substance such as silt, dust, solid biomass and the like are favorably realized, and according to the general composition of the current oil sludge, the weight percentage of an alcohol Rm- (OH) n or low-carbon alcohol ether solvent is preferably in the range of 40-65%. Preferably, the weight percentage of the aromatic solvent or mineral oil is in the range of 35% -60% according to the current general composition of the sludge.
The alcohol Rm- (OH) n is one or more of ethanol, isopropanol, ethylene glycol or diethylene glycol, and the low-carbon alcohol ether solvent is one or more of ethylene glycol monomethyl ether, ethylene glycol dimethyl ether, diethylene glycol dimethyl ether, cyclohexanediol monomethyl ether or ethylene glycol butyl ether. The aromatic hydrocarbon solvent is one or more of benzene, toluene, mixed xylene, mixed trimethylbenzene, tetramethylbenzene or ethylbenzene, etc., and the mineral oil is one or more of gasoline, diesel oil, raffinate oil or aromatic hydrocarbon solvent oil, etc.
The phase transfer agent also comprises a surfactant which promotes the mutual solubility of the alcohol Rm- (OH) n or the low-carbon alcohol ether solvent and the aromatic hydrocarbon solvent or the mineral oil and plays roles in demulsification, oil displacement and auxiliary phase transfer in a high-water-content oil sludge system, and the weight percentage of the surfactant is 0.2% -2% of the total metering of the alcohol Rm- (OH) n or the low-carbon alcohol ether solvent and the aromatic hydrocarbon solvent or the mineral oil. The surfactant comprises one or more of propylene glycol embedded polyether, alkylphenol ethoxylate, castor oil/hydrogenated castor oil polyoxyethylene ether, polyoxyethylene polyoxypropylene ether, phenol aldehyde resin polyoxypropylene polyoxyethylene ether or acrylamide modified copolymer and the like.
The phase transfer agent also comprises organic phenol, amine antioxidant and polymerization inhibitor for preventing high-water-content oil sludge from coking and scaling in the processes of drying and recycling oil and water, and the weight percentage of the phase transfer agent is 0.2% -1% of the total weight of the alcohol Rm- (OH) n or the low-carbon alcohol ether solvent and the aromatic solvent or the mineral oil. The organic phenol antioxidant and the polymerization inhibitor are one or more of p-phenylenediamine, hydroquinone, p-tert-butyl catechol or p-benzyl aminophenol and the like.
Specific examples of phase transfer agents employing such high water-bearing sludge.
Embodiment one.
The sample treated in this example was a high water content sludge (88.74% water content, 7.79% oil content, 3.47% solids content) from a petrochemical plant in Lanzhou, phase transfer agent (in weight ratio): 80% of diethylene glycol dimethyl ether, 20% of mixed xylene, 1.5% of propylene glycol embedded polyether and 0.5% of p-phenylenediamine.
In the embodiment S1, 300g of the high-water-content fatlute and 150g of the special phase transfer agent are weighed and added into a 1000ml open container, the temperature is raised to 50 ℃, and the mixture is put into a homogenizer to be homogenized for 5min at the rotation speed of 5000rpm, so as to prepare a phase transfer mixture;
in this example S2, 450g of the phase transfer mixture containing the phase transfer agent obtained in S1 was subjected to centrifugal separation at room temperature to obtain 264.4g of an oil, water and agent mixed supernatant and 183.2g of a reconstituted sludge.
In the embodiment S3, the mixed clear liquid obtained in the step S2 is kept stand for 24 hours at room temperature to separate an oil phase and a water phase, and 137g of an upper oil phase and 125.5g of a lower water phase are separated;
in the embodiment S4, 180.1g of the reconstructed oil sludge obtained by the separation of S2 is added into a 500ml rotary evaporator for normal pressure drying, the temperature is slowly increased, the final temperature is controlled at 240 ℃ for drying treatment, and 145.2g of distillate and 32.88g of dried oil sludge are obtained;
in this example S5, 137g of the oil phase obtained by separating S3 and 145.2g of the distillate obtained by separating S4 were fed into a 500ml vacuum rotary evaporator, the vacuum degree was controlled at-0.09 MPPa, the temperature was slowly raised to 150℃to recover 145.19g of the phase transfer agent, 109.3g of the wastewater and 16.2g of the distilled residual oil.
The embodiment reduces the high-water-content oil sludge by more than 88.85 percent, and the recovery of the oil component in the high-water-content oil sludge is nearly 70 percent, so that the reduction and recycling effects are remarkable.
Embodiment two.
The sample treated in this example is a high water content sludge (68.58% water content, 16.81% oil content, 14.61% solids content) from a petrochemical plant, and the phase transfer agent is (in weight ratio): 70% of diethylene glycol dimethyl ether, 30% of mixed xylene, 0.5% of propylene glycol embedded polyether and 0.5% of p-phenylenediamine.
In the embodiment S1, 300g of the high-water-content oil sludge and 150g of the special phase transfer agent are weighed and added into a 1000ml open container, and the mixture is put into a homogenizer at room temperature and homogenized for 5min at a rotation speed of 5000rpm to prepare a phase transfer mixture;
in this example S2, 450g of the phase transfer mixture containing the phase transfer agent obtained in S1 was subjected to centrifugal separation at room temperature to obtain 229g of an oil, water and agent mixed supernatant and 217.5g of a reconstituted sludge.
In the embodiment S3, the mixed clear liquid obtained in the step S2 is heated to 50 ℃ and kept stand for 8 hours so that an oil phase and a water phase are separated, and 157g of an upper oil phase and 72g of a lower water phase are separated;
in the embodiment S4, 212.3g of the reconstructed oil sludge obtained by separating the S2 is added into a 500ml rotary evaporator for vacuum drying, the vacuum degree is controlled to be-0.09 MPPa, the temperature is slowly increased, the final temperature is controlled to be 120 ℃ for drying treatment, 132.3g of distillate is obtained, and 79.4g of dried oil sludge is obtained;
in this example S5, 157g of the oil phase obtained by separating S3 and 132.3g of the distillate obtained by separating S4 were fed into a 500ml vacuum rotary evaporator, the vacuum degree was controlled at-0.09 MPPa, the temperature was slowly raised to 120℃to recover 143.7g of the phase transfer agent, 103.4g of the wastewater and 32.1g of the distilled residual oil.
In the embodiment, the high-water-content oil sludge is high in solid content, so that the reduction of the treated high-water-content oil sludge reaches 72.88%, but the oil component in the recovered high-water-content oil sludge exceeds 63.65%, and the reduction and recycling effects are remarkable.
Embodiment three.
The sample treated in this example was a high water content sludge (88.74% water content, 7.79% oil content, 3.47% solids content) from a petrochemical plant in Lanzhou, phase transfer agent (in weight ratio): 60% of diethylene glycol dimethyl ether, 40% of mixed xylene, 1.5% of propylene glycol embedded polyether and 0.5% of p-phenylenediamine.
In the embodiment S1, 300g of the high-water-content fatlute and 150g of the special phase transfer agent are weighed and added into a 1000ml open container, the temperature is raised to 50 ℃, and the mixture is put into a homogenizer to be homogenized for 5min at the rotation speed of 5000rpm, so as to prepare a phase transfer mixture;
in this example S2, 450g of the phase transfer mixture containing the phase transfer agent obtained in S1 was subjected to centrifugal separation at room temperature to obtain 262.4g of a clear mixture of oil, water and agent and 184.2g of a reconstituted sludge.
In the embodiment S3, the mixed clear liquid obtained in the step S2 is kept stand for 24 hours at room temperature to separate an oil phase and a water phase, and 137.8g of an upper oil phase and 124.5g of a lower water phase are separated;
in the embodiment S4, 176.1g of the reconstructed oil sludge obtained by the separation of S2 is added into a 500ml rotary evaporator for normal pressure drying, the temperature is slowly raised, the final temperature is controlled at 240 ℃ for drying treatment, and 144.2g of distillate and 27.7g of dried oil sludge are obtained;
in this example S5, 137.8g of the oil phase obtained by separating S3 and 144.2g of the distillate obtained by separating S4 were fed into a 500ml vacuum rotary evaporator, the vacuum degree was controlled at-0.09 MPPa, the temperature was slowly raised to 150℃to recover 142.57g of the phase transfer agent, 111.6g of the waste water and 16.44g of the distilled residual oil.
In the embodiment, the high-water-content oil sludge is reduced by 90.34 percent, and the oil component in the recovered high-water-content oil sludge exceeds 70 percent, so that the reduction and recycling effects are remarkable.
Example four.
The sample treated in this example is a high water content sludge (68.58% water content, 16.81% oil content, 14.61% solids content) from a petrochemical plant, and the phase transfer agent is (in weight ratio): 50% of diethylene glycol dimethyl ether, 50% of mixed xylene, 0.5% of propylene glycol embedded polyether and 0.5% of p-phenylenediamine.
In the embodiment S1, 300g of the high-water-content oil sludge and 150g of the special phase transfer agent are weighed and added into a 1000ml open container, and the mixture is put into a homogenizer at room temperature and homogenized for 5min at a rotation speed of 5000rpm to prepare a phase transfer mixture;
in the present example S2, 450g of the phase transfer mixture containing the phase transfer agent prepared in the step S1 was subjected to centrifugation at room temperature for 20min to separate, thereby obtaining 227g of an oil, water and agent mixed clear liquid and 217.8g of a reconstituted sludge.
In the embodiment S3, the mixed clear liquid obtained in the step S2 is heated to 50 ℃ and kept stand for 8 hours so that the oil phase and the water phase are separated, and 156g of an upper oil phase and 71g of a lower water phase are separated;
in the embodiment S4, 214.8g of the reconstruction obtained by the separation of S2 is added into a 500ml rotary evaporator for vacuum drying, the vacuum degree is controlled to be-0.09 MPPa, the temperature is slowly increased, the final temperature is controlled to be 120 ℃ for drying treatment, 134.3g of distillate is obtained, and 68.1g of dried oil sludge is obtained;
in this example S5, 156g of the oil phase obtained by separating S3 and 134.3g of the distillate obtained by separating S4 were fed into a 500ml vacuum rotary evaporator, the vacuum degree was controlled at-0.09 MPPa, the temperature was slowly raised to 120℃to recover 144.2g of the phase transfer agent, 100.5g of the wastewater and 35.65g of the distilled residual oil.
In the embodiment, the high-water-content oil sludge has high solid content, the decrement of the treated high-water-content oil sludge only reaches 76.98 percent, but the oil component in the recovered high-water-content oil sludge still exceeds 70 percent, and the reduction and recycling effects are obvious.
Example five.
The sample treated in this example is a high water content sludge (68.58% water content, 16.81% oil content, 14.61% solids content) from a petrochemical plant, and the phase transfer agent is (in weight ratio): 40% of ethylene glycol monomethyl ether, 60% of mixed xylene, 1.0% of acrylamide-xylene sulfonamide copolymer and 0.5% of p-benzyl aminophenol.
In this example S1, 300g of the above-mentioned high-water-content oil sludge and 150g of the special phase transfer agent were weighed and put into a 1000ml open container, and homogenized for 5 minutes at room temperature in a homogenizer at a rotation speed of 5000rpm, to prepare a phase transfer mixture.
In the embodiment S2, 450g of the phase transfer mixture containing the phase transfer agent prepared in the step S1 is subjected to vacuum suction filtration for 20min at room temperature under the vacuum degree of-0.075 MPPa, so as to obtain 223.1g of oil, water and agent mixed clear liquid and 221g of reconstituted sludge.
In the embodiment S3, the mixed clear liquid obtained in the step S2 is heated to room temperature and kept stand for 24 hours so that oil phase and water phase are separated, and 159.5g of upper oil phase and 83.6g of lower water phase are separated;
in the embodiment S4, 214.5g of the reconstruction obtained by the separation of S2 is added into a 500ml rotary evaporator for normal pressure drying, the temperature is slowly raised, the final temperature is controlled at 200 ℃ for drying treatment, 139.2g of distillate is obtained, and 69.4g of dried oil sludge is obtained;
in this example S5, 159.5g of the oil phase obtained by separating S3 and 139.2g of the distillate obtained by separating S4 were fed into a 500ml vacuum rotary evaporator, the vacuum degree was controlled at-0.09 MPPa, the temperature was slowly raised to 120℃to recover 142.7g of the phase transfer agent, 112.2g of the waste water and 32.65g of the distilled residual oil.
In the embodiment, the high-water-content oil sludge is high in solid content, so that the weight reduction of the treated high-water-content oil sludge is 76.16%, but the oil component in the recovered high-water-content oil sludge is only 64.7%, and the reduction and recycling effects are remarkable.
Example six.
The sample treated in this example is a high water content sludge (68.58% water content, 16.81% oil content, 14.61% solids content) from a petrochemical plant, and the phase transfer agent is (in weight ratio): 30% of ethylene glycol monomethyl ether, 70% of mixed xylene, 1.0% of acrylamide-xylene sulfonamide copolymer and 0.5% of p-benzyl aminophenol.
In the embodiment S1, 300g of the high-water-content oil sludge and 150g of the special phase transfer agent are weighed and added into a 1000ml open container, and the mixture is put into a homogenizer at room temperature and homogenized for 5min at a rotation speed of 5000rpm to prepare a phase transfer mixture;
in the present example S2, 450g of the phase transfer mixture containing the phase transfer agent prepared in the step S1 was centrifuged at room temperature for 20 minutes in a centrifuge, and 224.6g of the oil, water and agent mixture clear liquid and 219.7g of the reconstituted sludge were separated.
In the present example S3, the mixed supernatant obtained in the step S2 was heated to room temperature and allowed to stand for 24 hours to separate the oil phase from the water phase, and 163.6g of the upper oil phase and 79.5g of the lower water phase were separated;
in the embodiment S4, 214.7g of the reconstruction obtained by the separation of S2 is added into a 500ml rotary evaporator for normal pressure drying, the temperature is slowly raised, the final temperature is controlled at 200 ℃ for drying treatment, 137.2g of distillate is obtained, and 77.4g of dried oil sludge is obtained;
in this example S5, 163.6g of the oil phase obtained by separating S3 and 137.2g of the distillate obtained by separating S4 were fed into a 500ml vacuum rotary evaporator, the vacuum degree was controlled at-0.09 MPPa, the temperature was slowly raised to 120℃to recover 144.6g of the phase transfer agent, 102.1g of the wastewater and 35.1g of the distilled residual oil.
In the embodiment, the high-water-content oil sludge is high in solid content, so that the reduction amount of the treated high-water-content oil sludge is only 73.6%, the oil component in the recovered high-water-content oil sludge is 69.6%, and the reduction and recycling effects are remarkable.
Example seven.
The sample treated in this example is a high water content sludge (68.58% water content, 16.81% oil content, 14.61% solids content) from a petrochemical plant, and the phase transfer agent is (in weight ratio): 20% of ethylene glycol monomethyl ether, 80% of mixed xylene, 1.0% of acrylamide-xylene sulfonamide copolymer and 0.5% of p-benzyl aminophenol.
In the embodiment S1, 300g of the high-water-content oil sludge and 150g of the special phase transfer agent are weighed and added into a 1000ml open container, and the mixture is put into a homogenizer at room temperature and homogenized for 5min at a rotation speed of 5000rpm to prepare a phase transfer mixture;
in the embodiment S2, 450g of the phase transfer mixture containing the phase transfer agent prepared in the step S1 is subjected to vacuum suction filtration for 20min at room temperature under the vacuum degree of-0.075 MPPa, and 221.4g of the oil, water and agent mixed clear liquid and 222.3g of the reconstituted sludge are obtained.
In the present example S3, the mixed supernatant obtained in the step S2 was heated to room temperature and allowed to stand for 24 hours to separate the oil phase from the water phase, and 147.4g of the upper oil phase and 73.7g of the lower water phase were separated;
in the embodiment S4, 222.3g of the reconstruction obtained by the separation of S2 is added into a 500ml rotary evaporator for normal pressure drying, the temperature is slowly raised, the final temperature is controlled at 200 ℃ for drying treatment, 140.2g of distillate is obtained, and 60.4g of dried oil sludge is obtained;
in this example S5, 147.4g of the oil phase obtained by separating S3 and 140.2g of the distillate obtained by separating S4 were fed into a 500ml vacuum rotary evaporator, the vacuum degree was controlled at-0.09 MPPa, the temperature was slowly raised to 120℃to recover 143.7g of the phase transfer agent, 104.9g of the wastewater and 34.95g of the distilled residual oil.
In the embodiment, the high-water-content oil sludge is high in solid content, so that the reduction of the treated high-water-content oil sludge is only 72.8%, the recovery of the oil component in the high-water-content oil sludge is nearly 70%, and the reduction and recycling effects are remarkable.
Example eight.
The sample treated in this example is a high water content sludge (68.58% water content, 16.81% oil content, 14.61% solids content) from a petrochemical plant, and the phase transfer agent is (in weight ratio): ethylene glycol monomethyl ether 10%, mixed xylene 90%, acrylamide-xylene sulfonamide copolymer 1.0% and p-benzyl aminophenol 0.5%.
In the embodiment S1, 300g of the high-water-content oil sludge and 150g of the special phase transfer agent are weighed and added into a 1000ml open container, and the mixture is put into a homogenizer at room temperature and homogenized for 5min at a rotation speed of 5000rpm to prepare a phase transfer mixture;
in this example S2, 450g of the phase transfer mixture containing the phase transfer agent obtained in S1 was subjected to centrifugal separation at room temperature to obtain 213.1g of an oil, water and agent mixed supernatant and 235.7g of a reconstituted sludge.
In the embodiment S3, the mixed clear liquid obtained in the step S2 is heated to room temperature and kept stand for 24 hours so that an oil phase and a water phase are separated, and 152g of an upper oil phase and 81g of a lower water phase are separated;
in the embodiment S4, 227.1g of the reconstruction obtained by the separation of S2 is added into a 500ml rotary evaporator for normal pressure drying, the temperature is slowly raised, the final temperature is controlled at 200 ℃ for drying treatment, 131.5g of distillate is obtained, and 79.9g of dried oil sludge is obtained;
in this example S5, 152g of the oil phase obtained by separating S3 and 131.5g of the distillate obtained by separating S4 were fed into a 500ml vacuum rotary evaporator, the vacuum degree was controlled at-0.09 MPPa, the temperature was slowly raised to 120℃to recover 142.4g of the phase transfer agent, 99.7g of the wastewater and 34.3g of the distilled residual oil.
In the embodiment, the high-water-content oil sludge has high solid content, the decrement of the treated high-water-content oil sludge is only 72.36 percent, but the oil component in the recovered high-water-content oil sludge is 68 percent, and the decrement and recycling effects are better than those of other modes, but are not as good as those of other proportioning effects.
Example nine.
The sample treated in this example was a high water content sludge (68.58% oil content, 16.81% oil content, 14.61% solids content) from a petrochemical plant, jiujiang, and the phase transfer agent was: the recovered phase transfer agent of example four was used 90% with 10% fresh phase transfer agent being replenished.
In the embodiment S1, 300g of the high-water-content oil sludge and 150g of the special phase transfer agent are weighed and added into a 1000ml open container, and the mixture is put into a homogenizer at room temperature and homogenized for 5min at a rotation speed of 5000rpm to prepare a phase transfer mixture;
in the embodiment S2, 450g of the phase transfer mixture containing the phase transfer agent prepared in the step S1 is centrifuged for 20min at room temperature by a centrifuge, and 224g of the oil, water and agent mixed clear liquid and 222.2g of the reconstituted sludge are separated.
In the embodiment S3, the mixed clear liquid obtained in the step S2 is heated to room temperature and kept stand for 24 hours so that an oil phase and a water phase are separated, and 155g of an upper oil phase and 69g of a lower water phase are separated;
in the embodiment S4, 220.2g of the reconstructed oil sludge obtained by the separation of S2 is added into a 500ml rotary evaporator for normal pressure drying, the temperature is slowly raised, the final temperature is controlled at 200 ℃ for drying treatment, 140.3g of distillate is obtained, and 72.9g of dried oil sludge is obtained;
in this example S5, 155g of the oil phase obtained by separating S3 and 140.3g of the distillate obtained by separating S4 were fed into a 500ml vacuum rotary evaporator, the vacuum degree was controlled at-0.09 MPPa, the temperature was slowly raised to 120℃to recover 142.3g of the phase transfer agent, 108.1g of the waste water and 35.7g of the distilled residual oil.
The recovery phase transfer agent used in the embodiment still reaches 75.47% in the reduction of the high-water-content oil sludge after treatment, and the oil component in the recovery high-water-content oil sludge also exceeds 70%, so that the reduction and recycling effects are quite obvious.
The phase transfer agent performs phase transfer separation drying treatment on the oil sludge with high water content in the oil refinery, effectively abandons the problems of large consumption and high consumption of the hydrogen sulfide gas and the extractant discharged by acidification tempering, has the advantages of recycling utilization of the phase transfer agent, good drying effect, simple operation, low safety risk, low energy consumption and small investment, and has remarkable reduction and recycling effects.
The foregoing description of the preferred embodiments of the invention is not intended to be limiting, but rather is intended to cover all modifications, equivalents, and alternatives falling within the spirit and principles of the invention.

Claims (5)

1. A phase transfer agent for high water-containing sludge, characterized in that the phase transfer agent comprises the steps of transferring free water, capillary water and oil-in-water/water-in-oil emulsified water in the high water-containing sludge from a stable high water-containing sludge colloid system to the phase transfer agent, and dissolving oil in the high water-containing sludge colloid system and eliminating charges, colloid and asphaltenes in the oil in the system according to the higher water content in the high water-containing sludge, wherein the weight percentage of the low alcohol ether solvent is 10-80%, so as to destroy the original phase balance of the high water-containing sludge colloid system, reconstruct the sludge colloid system, and the weight percentage of the aromatic hydrocarbon solvent or mineral oil is 20-90 according to the higher oil content in the high water-containing sludge; the phase transfer agent also comprises a surfactant which promotes the mutual solubility of the low-carbon alcohol ether solvent and the aromatic hydrocarbon solvent or mineral oil and plays roles in demulsification, oil displacement and auxiliary phase transfer in a high-water-content oil sludge system, wherein the weight percentage of the surfactant is 0.2% -2% of the total metering of the low-carbon alcohol ether solvent and the aromatic hydrocarbon solvent or 0.2% -2% of the total metering of the low-carbon alcohol ether solvent and the mineral oil; the low-carbon alcohol ether solvent is one or more of ethylene glycol monomethyl ether, ethylene glycol dimethyl ether, diethylene glycol dimethyl ether, cyclohexanediol monomethyl ether or ethylene glycol butyl ether; the surfactant comprises one or more of propylene glycol block polyether, alkylphenol ethoxylate, castor oil polyoxyethylene ether, hydrogenated castor oil polyoxyethylene ether and polyoxyethylene polyoxypropylene ether.
2. The phase transfer agent according to claim 1, further comprising one or more of p-phenylenediamine, hydroquinone, p-tert-butylcatechol or p-benzylaminophenol in an amount of 0.2 to 1% by weight based on the total amount of the low carbon alcohol ether solvent and the aromatic hydrocarbon solvent, or 0.2 to 1% by weight based on the total amount of the low carbon alcohol ether solvent and the mineral oil, for preventing coking or scaling of high water-content sludge during drying and recovery.
3. The phase transfer agent according to claim 2, wherein the weight percentage of the low carbon alcohol ether solvent is 40% -65%.
4. A phase transfer agent according to claim 3, wherein the aromatic solvent or mineral oil is present in an amount of 35% to 60% by weight.
5. The phase transfer agent according to any one of claims 1 to 4, wherein the aromatic hydrocarbon solvent is one or more of benzene, toluene, mixed xylenes, mixed trimethylbenzenes, tetramethylbenzenes, or ethylbenzene, and the mineral oil is one or more of gasoline, diesel oil, raffinate oil, or aromatic hydrocarbon solvent oil.
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