CN112607981B - Method and system for recycling waste mineral oil sludge - Google Patents

Method and system for recycling waste mineral oil sludge Download PDF

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CN112607981B
CN112607981B CN202011432690.XA CN202011432690A CN112607981B CN 112607981 B CN112607981 B CN 112607981B CN 202011432690 A CN202011432690 A CN 202011432690A CN 112607981 B CN112607981 B CN 112607981B
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mineral oil
waste mineral
oil sludge
oil
pyrolysis
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CN112607981A (en
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王鸣
刘然升
张帅
周光林
孟家平
戚新军
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Ningbo Zhongxun Environmental Protection Technology Co ltd
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    • C—CHEMISTRY; METALLURGY
    • C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F11/00—Treatment of sludge; Devices therefor
    • C—CHEMISTRY; METALLURGY
    • C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F11/00—Treatment of sludge; Devices therefor
    • C02F11/18—Treatment of sludge; Devices therefor by thermal conditioning
    • C—CHEMISTRY; METALLURGY
    • C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10B—DESTRUCTIVE DISTILLATION OF CARBONACEOUS MATERIALS FOR PRODUCTION OF GAS, COKE, TAR, OR SIMILAR MATERIALS
    • C10B55/00—Coking mineral oils, bitumen, tar, and the like or mixtures thereof with solid carbonaceous material
    • C—CHEMISTRY; METALLURGY
    • C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10B—DESTRUCTIVE DISTILLATION OF CARBONACEOUS MATERIALS FOR PRODUCTION OF GAS, COKE, TAR, OR SIMILAR MATERIALS
    • C10B57/00—Other carbonising or coking processes; Features of destructive distillation processes in general
    • C10B57/04—Other carbonising or coking processes; Features of destructive distillation processes in general using charges of special composition
    • C10B57/045—Other carbonising or coking processes; Features of destructive distillation processes in general using charges of special composition containing mineral oils, bitumen, tar or the like or mixtures thereof
    • C—CHEMISTRY; METALLURGY
    • C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10G—CRACKING HYDROCARBON OILS; PRODUCTION OF LIQUID HYDROCARBON MIXTURES, e.g. BY DESTRUCTIVE HYDROGENATION, OLIGOMERISATION, POLYMERISATION; RECOVERY OF HYDROCARBON OILS FROM OIL-SHALE, OIL-SAND, OR GASES; REFINING MIXTURES MAINLY CONSISTING OF HYDROCARBONS; REFORMING OF NAPHTHA; MINERAL WAXES
    • C10G67/00—Treatment of hydrocarbon oils by at least one hydrotreatment process and at least one process for refining in the absence of hydrogen only
    • C10G67/02—Treatment of hydrocarbon oils by at least one hydrotreatment process and at least one process for refining in the absence of hydrogen only plural serial stages only
    • C—CHEMISTRY; METALLURGY
    • C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F2101/00—Nature of the contaminant
    • C02F2101/10—Inorganic compounds
    • C02F2101/12—Halogens or halogen-containing compounds
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02W—CLIMATE CHANGE MITIGATION TECHNOLOGIES RELATED TO WASTEWATER TREATMENT OR WASTE MANAGEMENT
    • Y02W10/00—Technologies for wastewater treatment
    • Y02W10/40—Valorisation of by-products of wastewater, sewage or sludge processing

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

Abstract

The invention relates to the technical field of deep processing and comprehensive utilization of waste mineral oil sludge, in particular to a method and a system for recycling the waste mineral oil sludge. The invention not only can solve the problem of deep processing and utilization of the waste mineral oil sludge, but also saves the environmental protection cost for the deep processing and utilization of the sludge; and certain products with high added value can be obtained, and the economic benefit is increased. Meanwhile, better raw materials can be provided for the hydrofining reactor, and the recovery rate of the lubricating oil in the whole process of the waste mineral oil regeneration device is improved. And the process has the characteristics of high yield, less carbon deposition of ash, difficult coking of pipelines and easy continuous operation.

Description

Method and system for recycling waste mineral oil sludge
Technical Field
The invention relates to the technical field of deep processing and comprehensive utilization of waste mineral oil sludge, in particular to a method and a system for recycling waste mineral oil sludge.
Background
The raw material of the waste mineral oil generally enters a factory in a barreling mode or a tank truck transportation mode, and the waste mineral oil is transferred to a raw material tank of a storage tank area for temporary storage after entering the factory. The crude filtration is carried out in a storage tank area of raw materials, and then the raw materials enter a settling tank, and substances such as oil sludge in the mineral oil are settled at a specific temperature. The waste mineral oil sludge contains about 55% of lubricating oil base oil, and is mixed with a small amount of water, metal scrap particles generated by abrasion, and impurities such as carboxylic acid, salts of organic acid, asphaltene, colloid, carbon residue and the like generated by oxidation.
In the waste mineral oil recycling enterprises, about 5% of oil sludge is produced in the storage and sedimentation stage of the waste mineral oil recycling process, and the oil sludge produced in the whole process is far larger than 5%. At the source, about 3% of the sludge is separated in the waste mineral oil collection facility before the waste mineral oil enters the regeneration facility, and this data is not statistically listed. From the source of the waste mineral oil to the core device of the waste mineral oil recycling enterprise, about 8% of oil sludge is separated and cannot be reasonably recycled.
The waste mineral oil comprehensive utilization enterprises are used for calculation, and small waste mineral oil recycling enterprises are gradually recombined or combined due to industry standardization. At present, the treatment capacity of most waste mineral oil recycling enterprises is 5-12 ten thousand tons per year, and the treatment capacity of the oil sludge is 2500-9600 tons calculated by 5-8 percent of oil sludge. If the treatment is carried out with dangerous waste, enterprises need to carry out the treatment at the price of 8000 yuan/ton, the cost is consumed between 2000 and 7680 ten thousand, and extremely high treatment cost is borne. Substances such as lubricating oil base oil and the like with recyclable value still exist in the oil sludge of the waste mineral oil; if the method can be used for recycling, the cost can be saved, certain products with high added values can be obtained, and the economic benefit is increased.
Chinese patent CN110803846A discloses a method for processing oil sludge by pyrolysis, which uses recovered oil component to directly spray pyrolysis vaporization, and makes solid oil sludge into flowable slurry. The prior molten metal heat carrier technology is combined to complete a series of technological production processes of preheating, mixing, separating, storing and the like of the oil sludge slurry. The patent adopts the blending of oil and raw material oil sludge, wastes the economic value of oil products, and can cause secondary cracking and coking of the oil products.
Chinese patent CN109385321A discloses a method for treating waste emulsion oil sludge, comprising the following steps: proportioning, namely proportioning waste emulsion oil sludge and fly ash quantitatively and then carrying out the next operation; mixing, namely mixing the materials prepared in the material preparing step, and repeatedly rolling, stirring and mixing the materials to prepare powdery particles; thirdly, discharging, and outputting the final product of the mixing step. The waste emulsion oil sludge and the fly ash are treated to obtain the product which can be used as fuel to be fully combusted, and the treatment cost is low. However, the waste emulsion oil sludge of the patent has high water content and large smell, a deodorant needs to be added, and the tail gas seriously pollutes the environment.
Chinese patent CN110451753A discloses a treatment method of hazardous solid waste oil sludge, wherein the oil sludge after impurity removal is pyrolyzed under the action of steam to obtain pyrolysis residue and pyrolysis oil gas of carbon deposit; separating the pyrolysis oil gas by a condensation separation system to obtain pyrolysis oil and pyrolysis gas; the carbon deposit pyrolysis slag and the pyrolysis gas enter a waste heat boiler for combustion and heat supply, and steam is generated for the pyrolysis process; the reaction time of the method is 10-90min, the reaction time is long, the heat conduction is not uniform, and the pipe wall is perforated due to severe coking, so that the production is influenced. And the patent is an experimental device and is only suitable for the experimental exploration stage.
At present, the industrial industrialization of the waste mineral oil sludge is not deeply researched by waste mineral oil recycling enterprises, the comprehensive utilization of the sludge needs a feasible regeneration method and technology, the yield and the cost of the enterprises are increased and reduced, and the method is also a key ring in a full-flow closed-loop chain for the waste mineral oil recycling.
Disclosure of Invention
The invention aims to provide a method for recycling waste mineral oil sludge, which can solve the problem of deep processing and utilization of the waste mineral oil sludge, save the environmental protection cost for deep processing and utilization of the sludge; and certain products with high added value can be obtained, and the economic benefit is increased. Meanwhile, better raw materials can be provided for the hydrofining reactor, and the recovery rate of the lubricating oil in the whole process of the waste mineral oil regeneration device is improved. And the process has the characteristics of high yield, less carbon deposition of ash, difficult coking of pipelines and easy continuous operation. The invention also provides a system for recycling the waste mineral oil sludge.
The technical scheme adopted by the invention for solving the technical problems is as follows:
the method for recycling the waste mineral oil sludge comprises the following steps:
(1) filter unit
And the waste mineral oil sludge obtained after the three-phase separation or solvent treatment of the waste mineral oil enters an oil sludge tank, is mixed with the viscosity reducer injected by a viscosity reducer pump, exchanges heat firstly, is filtered by a filtering device, and enters a dechlorination unit.
(2) Dechlorination unit
The filtered waste mineral oil sludge exchanges heat with distillation fractions of original waste oil generated by three-phase separation, dechlorinating agent is injected into the heat-exchanged waste mineral oil sludge through a dechlorinating agent pump, and the mixture is stirred and mixed under the action of a strong mixing emulsifying pump and then enters a dechlorinating buffer tank for dechlorinating reaction; and the distillation fraction of the original waste oil generated by three-phase separation enters a hydrofining unit after heat exchange.
(3) Tubular reaction unit
Mixing dechlorinated waste mineral oil sludge with a coking inhibitor injected by a coking inhibitor pump, firstly exchanging heat, rapidly heating by a heating furnace, injecting soft water through a water injection pump, and then entering a tubular reactor to obtain an oil product; a certain amount of soft water is injected before entering the tubular reactor, so that the oil gas in the reactor reaches a certain linear speed, the coking of the tubular reactor is delayed to the maximum extent, the yield of the oil gas is increased, and the generation of residue coke is reduced.
(4) Delayed pyrolysis unit
The oil product obtained by the tubular reactor is decompressed by a high-temperature pressure reducing valve, enters a buffer pyrolysis tower to stay for coke formation, distillate oil and pyrolysis gas are generated at the top of the buffer pyrolysis tower, the distillate oil and the pyrolysis gas enter a fractionation unit to be subjected to gas-liquid separation, and a small amount of ash is generated at the bottom of the buffer pyrolysis tower and can be removed at regular time. The two buffer pyrolysis towers are arranged, one is used and the other is prepared, and the continuous operation of the device is ensured.
(5) Fractionation unit
Carrying out gas-liquid separation on distillate oil and pyrolysis gas in a fractionating tower, separating the gas phase, then removing a torch system, and extracting a liquid phase side line to be divided into two sections; and (3) gasoline and diesel fractions are extracted from the upper section, one part of gasoline and diesel fractions is mixed with the waste mineral oil sludge subjected to heat exchange in the step (2) for circular viscosity reduction dechlorination or full-reflux online cleaning, the other part of gasoline and diesel fractions is mixed with the lubricating oil fractions extracted from the lower section to obtain fraction mixed oil, and the fraction mixed oil enters a hydrofining unit. The liquid level of the fractionating tower is controlled by a non-contact differential pressure transmitter and a pneumatic regulating valve.
(6) Hydrorefining unit
And the distillate mixed oil is converged with the distillation distillate of the original waste oil after heat exchange, enters a hydrofining reactor after the heat exchange of a heat exchanger, and is reduced to obtain high-quality distillate oil and high-quality II-type lubricating oil base oil products through a hydrotreating, hydrodewaxing and complementary isomerization refining reaction section and unsaturated hydrocarbon saturation reaction.
Wherein:
in the step (1), the aperture of the filter screen of the filter device is 120-200 meshes; the filtration can adopt a mode of combining filter screen filtration and metal magnetic filtration.
In the step (1), the addition amount of the viscosity reducer is 0.05-0.2 wt.% of the amount of the waste mineral oil sludge, and the viscosity reducer is obtained by compounding polyamides or alcohol amines with polyoxyethylene ethers and monoterpene compounds, wherein the mass ratio of the polyamides or alcohol amines to the polyoxyethylene ethers to the monoterpene compounds is 50-70:15-25: 15-25;
the polyamide is a polymer of 2-acrylamide-2-methylpropanesulfonic acid and maleic anhydride, and the mass ratio of the 2-acrylamide-2-methylpropanesulfonic acid to the maleic anhydride is 2: 1;
the alcamines are N-dodecyl-1, 3-propanol diamine or N, N-diethylethanolamine;
the polyoxyethylene ether is stearyl amine polyoxyethylene ether, coco amine polyoxyethylene ether or octadecyl amine polyoxyethylene ether;
the monoterpene compound is myrcene, limonene or citral.
In the step (1), the outlet temperature is 80-120 ℃ after heat exchange.
In the step (1), the solvent adopted in the solvent treatment process is 90# solvent naphtha or 150-.
In the step (2), the addition amount of a dechlorinating agent is 0.05-0.2 wt% of the amount of the waste mineral oil sludge in the step (1), the dechlorinating agent is obtained by compounding ethylenediamine, organic quaternary ammonium base and strongly basic ionic liquid, wherein the mass ratio of the ethylenediamine to the organic quaternary ammonium base to the strongly basic ionic liquid is 20-40:25-45: 15-35;
the organic quaternary ammonium base is cetyl trimethyl ammonium hydroxide, tetrabutyl ammonium hydroxide or tetrapropyl ammonium hydroxide;
the strongly alkaline ionic liquid is polyethylene glycol functionalized diimidazole ionic liquid, 1-butyl-3-methylimidazole ionic liquid or 1, 3-dimethylimidazole ionic liquid.
In the step (2), the temperature of the dechlorination reaction is 200-280 ℃; the pressure of the dechlorination reaction is 1-2MPa, and the pressure feedback adjustment can be carried out through a differential pressure controller; the retention time of the waste mineral oil sludge in the dechlorination buffer tank is 10-30min, and a clapboard type reaction kettle or a conical reaction tank can be adopted to increase the retention time.
In the step (3), the addition amount of the coking inhibitor is 0.5-1 wt.% of the amount of the waste mineral oil sludge in the step (1), and the dechlorinating agent is obtained by compounding a sulfonic amine salt with polyoxyalkylamine and arylamine-based polymeric substances, wherein the mass ratio of the sulfonic amine salt to the polyoxyalkylamine to the arylamine-based polymeric substances is 30-50: 50-70;
the sulfonic acid amine salt is thiophosphate alkylbenzene sulfonic acid diamine salt or dodecyl benzene sulfonic acid isopropanol amine salt;
the polymeric substances of polyoxyalkylamine and arylamine are octadecylamine polyoxyethylene ether, dodecylamine polyoxyethylene ether, fatty amine polyoxyethylene ether, polyolefin succinimide or polyoxyethylene dodecylamine.
In the step (3), the adding amount of the soft water is 0.5-2 wt% of the using amount of the waste mineral oil sludge in the step (1), and a medium-pressure inlet diaphragm water injection pump with the outlet pressure of 7-10MPa is adopted as the water injection pump and is made of 316 SS.
In the step (3), the pyrolysis temperature of the tubular reactor is 500-560 ℃, the reaction pressure is 5-7MPa, and the retention time is 3-8 seconds. The material of the tubular reactor is 316SS, corrosion-resistant hastelloy C276 or incoloy 800.
In the step (3), the heat exchange is carried out to 300-320 ℃.
In the step (4), the pressure at the top of the tower of the buffer pyrolysis tower is 1-1.5MPa, and is controlled by a pressure sensor and a pneumatic regulating valve in a matching way; the reaction temperature is 510-555 ℃; the retention time of the buffer pyrolysis tower is 1-2 hours, and when the operation time is up, the buffer pyrolysis tower can be switched to a standby buffer pyrolysis tank.
In the step (5), the pressure in the fractionating tower is 0.15-0.35MPa, the temperature of the reduced pressure outlet of the fractionating tower is 180-.
In the step (6), the pressure of the hydrogen refining reactor is 12-16MPa, the reaction temperature is 350-390 ℃, and the volume hydrogen-oil ratio is 300-850: 1.
Mixing the waste mineral oil sludge and the viscosity reducer, and filtering after heat exchange; dechlorinating the filtered oil sludge under the action of a dechlorinating agent, mixing the dechlorinated oil product with a coke inhibitor and soft water, quickly passing through a tubular reactor at a high temperature for a short time, then entering a buffer pyrolysis tower for staying and coke formation to generate a small amount of ash, recovering the generated distillate oil and pyrolysis gas through a fractionating tower, and extracting a liquid phase side line into two sections; and (3) extracting gasoline and diesel oil fractions at the upper section, mixing one part of gasoline and diesel oil fractions with waste mineral oil sludge for circulating viscosity reduction and dechlorination, mixing the other part of gasoline and diesel oil fractions with lubricating oil fractions extracted at the lower section and distillation fractions of original waste mineral oil, and feeding the mixture into a hydrofining unit to reduce the mixture to obtain high-quality distillate oil and high-quality II-type lubricating oil base oil products.
The invention relates to a system for recycling waste mineral oil sludge, which comprises the following steps: comprises a waste mineral oil tank, an oil sludge tank, a dechlorination buffer tank, a tubular reactor, a buffer pyrolysis tower, a fractionating tower, a hydrofining reactor and a product tank which are connected in sequence; a fourth heat exchanger, a filtering device, a first heat exchanger and a strong mixing emulsification pump are sequentially arranged on a pipeline between the oil sludge tank and the dechlorination buffer tank; a third heat exchanger and a heating furnace are sequentially arranged on a pipeline between the dechlorination buffer tank and the tubular reactor; a second heat exchanger is arranged between the fractionating tower and the hydrofining reactor;
a three-phase separator is arranged between the mineral oil tank and the oil sludge tank, the three-phase separator is connected with a first heat exchanger through a distillation tower, and the first heat exchanger is also connected with a pipeline between the fractionating tower and a second heat exchanger; the fractionating tower is also connected with a pipeline between the first heat exchanger and the intensive mixing emulsion pump through a pipeline.
A viscosity reducer pump is connected on a pipeline between the oil sludge tank and the fourth heat exchanger, a dechlorinating agent pump is connected on a pipeline between the first heat exchanger and the strong mixing emulsion pump, a coke inhibitor pump is connected on a pipeline between the dechlorinating buffer tank and the third heat exchanger, and a water injection pump is connected on a pipeline between the heating furnace and the tubular reactor.
The buffering pyrolysis tower comprises a first buffering pyrolysis tower and a second buffering pyrolysis tower, and the first buffering pyrolysis tower and the second buffering pyrolysis tower are respectively connected with the ash tank; a solvent treatment tank is also arranged between the mineral oil tank and the oil sludge tank; the three-phase separator is connected with a flare system, and the flare system is also connected with the top of the fractionating tower.
The invention has the following beneficial effects:
(1) the invention adopts a pretreatment dechlorination process to carry out pretreatment on the waste mineral oil sludge, thereby reducing the content of chloride in the waste mineral oil sludge, reducing the corrosion to equipment and prolonging the service life of the equipment.
(2) The invention increases side extraction, and extracts part of kerosene, diesel oil and other fractions while keeping the lubricating oil fraction to the maximum extent and entering the hydrofining reactor, thereby increasing the fluidity of oil sludge in a pipeline. The device can be cleaned on line when the side line is fully opened.
(3) The tubular reactor is adopted, so that the retention time is reduced; the waste mineral oil sludge is injected with a certain amount of soft water before entering the tubular reactor, so that the oil gas in the reactor reaches a certain linear speed, the coking of the tubular reactor is delayed to the maximum extent, the yield of the oil gas is increased, and the generation of residue coke is reduced.
(4) The invention adopts the delayed pyrolysis process, has enough time for reaction and residence, generates residual coke therein, and continuously produces new pyrolysis oil gas components. And meanwhile, two buffer pyrolysis towers are adopted for switching, so that the continuous production of the device is ensured to the maximum extent.
(5) A part of gasoline and diesel oil fractions obtained by fractionation enter a pretreatment working section for circular viscosity reduction and dechlorination, main heavy fractions are stored and used as hydrogenation base oil raw materials, and in a three-stage hydrogenation refining reactor, hydrogenation treatment, hydrodewaxing and complementary isomerization refining are carried out, and high-quality distillate oil and high-quality II-type lubricating oil base oil products are obtained by reduction.
(6) The pyrolysis oil obtained by the invention fully exchanges heat with the raw material waste mineral oil sludge, and the heat is recycled.
(7) The invention does not need to add an organic solvent additionally; the side stream distillate can be supplemented and mixed in variable quantities according to the flowing condition of the oil sludge, so that the environment is protected, and the cost is reduced.
Drawings
FIG. 1 is a process flow diagram of the present invention;
wherein: 1. a waste mineral oil tank; 2. a solvent treatment tank; 3. a three-phase separator; 4. a sludge tank; 5. a viscosity reducer pump; 6. a dechlorination agent pump; 7. a scorch retarder pump; 8. a water injection pump; 9. a filtration device; 10. a first heat exchanger; 11. a forced mixing emulsion pump; 12. a dechlorination buffer tank; 13. heating furnace; 14. a tubular reactor; 15. a first buffer pyrolysis tower; 16. a second buffer pyrolysis tower; 17. a fractionating column; 18. a second heat exchanger; 19. a hydrofining reactor; 20. a fourth heat exchanger; 21. a third heat exchanger; 22. a distillation column; 23. a flare system; 24. a slag tank; 25. and (5) a product tank.
Detailed Description
The present invention is further described below with reference to examples.
Example 1
(1) Filter unit
The waste mineral oil sludge obtained after the waste mineral oil in the waste mineral oil tank 1 is separated by the three-phase separator 3 or treated by the solvent treatment tank 2 enters the sludge tank 4, is mixed with the viscosity reducer injected by the viscosity reducer pump 5, exchanges heat to 100 ℃ by the fourth heat exchanger 20, is filtered by the filtering device 9, and enters the dechlorination unit. The raw waste oil from the three-phase separation of the waste mineral oil is fed to a distillation column 22 to produce a distillation cut and the resulting gas is fed to a flare system 23. Wherein the aperture of the filter screen of the filter device 9 is 120 meshes; the processing solvent in the solvent processing tank 2 is 90# solvent oil; the addition amount of the viscosity reducer is 0.1 wt.% of the amount of the waste mineral oil sludge, and the viscosity reducer is obtained by compounding polyamides, polyoxyethylene ethers and monoterpene compounds, wherein the mass ratio of the polyamides, the polyoxyethylene ethers and the monoterpene compounds is 50:25: 25;
the polyamide is a polymer generated by copolymerizing 2-acrylamide-2-methylpropanesulfonic acid and maleic anhydride, and the mass ratio of the 2-acrylamide-2-methylpropanesulfonic acid to the maleic anhydride is 2: 1; the polyoxyethylene ether is stearyl amine polyoxyethylene ether; the monoterpene compound is myrcene.
(2) Dechlorination unit
Exchanging heat between the filtered waste mineral oil sludge and the distillation fraction of original waste oil generated by three-phase separation in a first heat exchanger 10, injecting a dechlorinating agent into the heat-exchanged waste mineral oil sludge through a dechlorinating agent pump 6, wherein the addition amount of the dechlorinating agent is 0.2 wt% of the amount of the waste mineral oil sludge in the step (1), stirring and mixing under the action of a strong mixing emulsification pump 11, then entering a dechlorinating buffer tank 12, and performing dechlorination reaction at 250 ℃; a pressure difference controller is adopted for feedback regulation, and the pressure of the dechlorination buffer tank 12 is maintained to be 2 MPa; the residence time of the waste mineral oil sludge in the dechlorination buffer tank 12 is increased by adopting the clapboard type reaction kettle, so that the residence time of the waste mineral oil sludge in the dechlorination buffer tank is 10 min. And the distillation fraction of the original waste oil generated by three-phase separation enters a hydrofining unit after heat exchange.
The dechlorinating agent is obtained by compounding ethylenediamine, organic quaternary ammonium base and strong basic ionic liquid, wherein the mass ratio of the ethylenediamine to the organic quaternary ammonium base to the strong basic ionic liquid is 40:45: 15;
the organic quaternary ammonium base is cetyl trimethyl ammonium hydroxide; the strongly alkaline ionic liquid is polyethylene glycol functionalized bisimidazole type ionic liquid.
(3) Tubular reaction unit
Mixing dechlorinated waste mineral oil sludge with a coking inhibitor injected by a coking inhibitor pump 7, firstly exchanging heat to 300 ℃ through a third heat exchanger 21, rapidly heating through a heating furnace 13, injecting soft water through a water injection pump 8, and then entering a tubular reactor 14 to obtain an oil product; before entering the tubular reactor 14, a certain amount of soft water is injected to ensure that the oil gas in the reactor reaches a certain linear speed, so that the coking of the tubular reactor 14 is delayed to the maximum extent, the yield of the oil gas is increased, and the generation of residual coke is reduced.
The addition amount of the coke inhibitor is 1 wt% of the amount of the waste mineral oil sludge in the step (1), the dechlorinating agent is obtained by compounding a sulfonic acid amine salt with polyoxyalkylamine and aromatic amine based polymeric substances, wherein the mass ratio of the sulfonic acid amine salt to the polyoxyalkylamine and the aromatic amine based polymeric substances is 30: 70; the sulfonic amine salt is thiophosphate alkylbenzene sulfonic acid diamine salt; the polymeric substance of polyoxyalkylamine and arylamine is octadecylamine polyoxyethylene ether;
the adding amount of the soft water is 1 wt% of the using amount of the waste mineral oil sludge in the step (1), and a medium-pressure inlet diaphragm water injection pump with the outlet pressure of 8MPa is adopted as the water injection pump 8 and is made of 316 SS; the pyrolysis temperature of the tubular reactor 14 was 550 ℃, the reaction pressure was 7MPa, and the residence time was 5 seconds. The material of the tubular reactor 14 is hastelloy C276 which is corrosion resistant.
(4) Delayed pyrolysis unit
The oil obtained from the tubular reactor 14 is depressurized by a high-temperature pressure reducing valve and then enters a first buffer pyrolysis tower 15. The pressure sensor and the pneumatic regulating valve are matched to control the tower top pressure of the first buffer pyrolysis tower 15 to be 1 MPa. The reaction temperature in the first buffer pyrolysis tower 15 is 545 ℃; the residence time in the first buffer pyrolysis column 15 was 1.5 hours. The oil products stay in the first buffer pyrolysis tower 15 to generate coke, the top of the first buffer pyrolysis tower 15 generates distillate oil and pyrolysis gas, the distillate oil and the pyrolysis gas enter a fractionation unit to carry out gas-liquid separation, and a small amount of ash residues are generated at the bottom and can be removed at regular time. The second buffer pyrolysis tower 16 is a standby pyrolysis tower, and when the first buffer pyrolysis tower 15 reaches the operation time, the second buffer pyrolysis tower 16 can be switched to the standby second buffer pyrolysis tower, so that the continuous operation of the device is ensured.
(5) Fractionation unit
The distillate oil and the pyrolysis gas coming out from the top of the buffer pyrolysis tower enter a fractionating tower 17 for gas-liquid separation, the pressure in the fractionating tower 17 is 0.35MPa, and the temperature of a reduced pressure outlet of the fractionating tower 17 is 300 ℃. The gas phase is separated and then is discharged to a torch system 23, and the liquid phase side line is extracted and divided into two sections; and (3) extracting gasoline and diesel fractions at the upper section, mixing a part of gasoline and diesel fractions with the waste mineral oil sludge subjected to heat exchange in the step (2) for cyclic viscosity reduction and dechlorination, wherein the cyclic proportion of the gasoline and diesel fractions is 25%, or carrying out total reflux on-line cleaning, mixing the other part of gasoline and diesel fractions with the lubricating oil fractions extracted at the lower section to obtain fraction mixed oil, and feeding the fraction mixed oil into a hydrofining unit. The liquid level of the fractionating tower 17 is controlled by a non-contact differential pressure transmitter and a pneumatic regulating valve.
(6) Hydrorefining unit
The distillate mixed oil is converged with the distillation distillate of the original waste oil after heat exchange, enters a hydrofining reactor 19 after heat exchange by a second heat exchanger 18, the pressure of the hydrofining reactor 19 is 15MPa, the reaction temperature is 360 ℃, and the volume hydrogen-oil ratio is 350: 1. Through the reaction sections of hydrogenation treatment, hydrodewaxing, complementary isomerization refining and the like, high-quality distillate oil and high-quality II-type lubricating oil base oil products are obtained through the reduction of unsaturated hydrocarbon saturation reaction.
Example 2
(1) Filter unit
The waste mineral oil sludge obtained after the waste mineral oil in the waste mineral oil tank 1 is separated by the three-phase separator 3 or treated by the solvent treatment tank 2 enters the sludge tank 4, is mixed with the viscosity reducer injected by the viscosity reducer pump 5, exchanges heat to 90 ℃ by the fourth heat exchanger 20, is filtered by the filtering device 9, and enters the dechlorination unit. The raw waste oil from the three-phase separation of the waste mineral oil is fed to a distillation column 22 to produce a distillation cut and the resulting gas is fed to a flare system 23. Wherein the diameter of the filter screen of the filter device 9 is 150 meshes; the treatment solvent in the solvent treatment tank 2 is 150-200 ℃ straight-run gasoline; the addition amount of the viscosity reducer is 0.15 wt.% of the amount of the waste mineral oil sludge, and the viscosity reducer is obtained by compounding alcohol amines, polyoxyethylene ethers and monoterpene compounds, wherein the mass ratio of the alcohol amines to the polyoxyethylene ethers to the monoterpene compounds is 55:25: 20;
the alcamines are N-dodecyl-1, 3-propanol diamine; the polyoxyethylene ether is octadecyl amine polyoxyethylene ether; the monoterpene compound is citral.
(2) Dechlorination unit
Exchanging heat between the filtered waste mineral oil sludge and a distillation fraction of original waste oil generated by three-phase separation in a first heat exchanger 10, injecting a dechlorinating agent into the heat-exchanged waste mineral oil sludge through a dechlorinating agent pump 6, wherein the addition amount of the dechlorinating agent is 0.1 wt% of the amount of the waste mineral oil sludge in the step (1), stirring and mixing under the action of a strong mixing emulsifying pump 11, then entering a dechlorinating buffer tank 12, and performing dechlorination reaction at 230 ℃; a pressure difference controller is adopted for feedback regulation, and the pressure of the dechlorination buffer tank 12 is maintained to be 1.5 MPa; and the residence time of the waste mineral oil sludge in the dechlorination buffer tank 12 is increased by adopting the clapboard type reaction kettle to be 30 min. And the distillation fraction of the original waste oil generated by three-phase separation enters a hydrofining unit after heat exchange.
The dechlorinating agent is obtained by compounding ethylenediamine, organic quaternary ammonium base and strong basic ionic liquid, wherein the mass ratio of the ethylenediamine to the organic quaternary ammonium base to the strong basic ionic liquid is 30:35: 35;
the organic quaternary ammonium base is tetrabutyl ammonium hydroxide; the strongly alkaline ionic liquid is 1-butyl-3-methylimidazole ionic liquid.
(3) Tubular reaction unit
Mixing dechlorinated waste mineral oil sludge with a coking inhibitor injected by a coking inhibitor pump 7, firstly exchanging heat to 300 ℃ through a third heat exchanger 21, rapidly heating through a heating furnace 13, injecting soft water through a water injection pump 8, and then entering a tubular reactor 14 to obtain an oil product; before entering the tubular reactor 14, a certain amount of soft water is injected to ensure that the oil gas in the reactor reaches a certain linear speed, so that the coking of the tubular reactor 14 is delayed to the maximum extent, the yield of the oil gas is increased, and the generation of residual coke is reduced.
The addition amount of the anti-coking agent is 0.5 wt.% of the amount of the waste mineral oil sludge in the step (1), the dechlorinating agent is obtained by compounding sulfonic amine salt with polyoxyalkylamine and arylamine group polymerization substances, and the mass ratio of the sulfonic amine salt to the polyoxyalkylamine and arylamine group polymerization substances is 50: 50; the sulfonic acid amine salt is dodecyl benzene sulfonic acid isopropyl alcohol amine salt; the polymeric substance of polyoxyalkylamine and arylamine is polyolefin succinimide;
the adding amount of the soft water is 2 wt.% of the using amount of the waste mineral oil sludge in the step (1), and a medium-pressure inlet diaphragm water injection pump with the outlet pressure of 10MPa is adopted as the water injection pump 8 and is made of 316 SS; the pyrolysis temperature of the tubular reactor 14 was 530 ℃, the reaction pressure was 6MPa, and the residence time was 4 seconds. The material of the tubular reactor 14 is 316 SS.
(4) Delayed pyrolysis unit
The oil obtained from the tubular reactor 14 is depressurized by a high-temperature pressure reducing valve and then enters a first buffer pyrolysis tower 15. The pressure sensor and the pneumatic regulating valve are matched to control the tower top pressure of the first buffer pyrolysis tower 15 to be 1.5 MPa. The reaction temperature in the first buffer pyrolysis tower 15 is 525 ℃; the residence time in the first buffer pyrolysis column 15 was 1 hour. The oil products stay in the first buffer pyrolysis tower 15 to generate coke, the top of the first buffer pyrolysis tower 15 generates distillate oil and pyrolysis gas, the distillate oil and the pyrolysis gas enter a fractionation unit to carry out gas-liquid separation, and a small amount of ash residues are generated at the bottom and can be removed at regular time. The second buffer pyrolysis tower 16 is a standby pyrolysis tower, and when the first buffer pyrolysis tower 15 reaches the operation time, the second buffer pyrolysis tower 16 can be switched to the standby second buffer pyrolysis tower, so that the continuous operation of the device is ensured.
(5) Fractionation unit
The distillate oil and the pyrolysis gas coming out from the top of the buffer pyrolysis tower enter a fractionating tower 17 for gas-liquid separation, the pressure in the fractionating tower 17 is 0.25MPa, and the temperature of a pressure reduction outlet of the fractionating tower 17 is 295 ℃. The gas phase is separated and then is discharged to a torch system 23, and the liquid phase side line is extracted and divided into two sections; and (3) extracting gasoline and diesel fractions at the upper section, mixing a part of gasoline and diesel fractions with the waste mineral oil sludge subjected to heat exchange in the step (2) for cyclic viscosity reduction and dechlorination, wherein the cyclic proportion of the gasoline and diesel fractions is 50%, or performing total reflux on-line cleaning, mixing the other part of gasoline and diesel fractions with the lubricating oil fractions extracted at the lower section to obtain fraction mixed oil, and feeding the fraction mixed oil into a hydrofining unit. The liquid level of the fractionating tower 17 is controlled by a non-contact differential pressure transmitter and a pneumatic regulating valve.
(6) Hydrorefining unit
The distillate mixed oil is converged with the distillation distillate of the original waste oil after heat exchange, enters a hydrofining reactor 19 after heat exchange by a second heat exchanger 18, the pressure of the hydrofining reactor 19 is 14MPa, the reaction temperature is 380 ℃, and the volume hydrogen-oil ratio is 400: 1. Through the reaction sections of hydrogenation treatment, hydrodewaxing, complementary isomerization refining and the like, and through the saturated reaction of unsaturated hydrocarbons, high-quality distillate oil and high-quality II-type lubricating oil base oil products are obtained by reduction.
Example 3
(1) Filter unit
The waste mineral oil sludge obtained after the waste mineral oil in the waste mineral oil tank 1 is separated by the three-phase separator 3 or treated by the solvent treatment tank 2 enters the sludge tank 4, is mixed with the viscosity reducer injected by the viscosity reducer pump 5, exchanges heat to 95 ℃ by the fourth heat exchanger 20, is filtered by the filtering device 9, and enters the dechlorination unit. The raw waste oil from the three-phase separation of the waste mineral oil is fed to a distillation column 22 to produce a distillation cut and the resulting gas is fed to a flare system 23. Wherein the filter mesh diameter of the filter device 9 is 180 meshes; the treatment solvent in the solvent treatment tank 2 is 150-200 ℃ straight-run gasoline; the addition amount of the viscosity reducer is 0.05 wt.% of the amount of the waste mineral oil sludge, and the viscosity reducer is obtained by compounding polyamides, polyoxyethylene ethers and monoterpene compounds, wherein the mass ratio of the polyamides, the polyoxyethylene ethers and the monoterpene compounds is 60:20: 20;
the polyamide is a polymer generated by copolymerizing 2-acrylamide-2-methylpropanesulfonic acid and maleic anhydride, and the mass ratio of the 2-acrylamide-2-methylpropanesulfonic acid to the maleic anhydride is 2: 1; the polyoxyethylene ether is octadecyl amine polyoxyethylene ether; the monoterpene compound is limonene.
(2) Dechlorination unit
Exchanging heat between the filtered waste mineral oil sludge and the distillation fraction of original waste oil generated by three-phase separation in a first heat exchanger 10, injecting a dechlorinating agent into the heat-exchanged waste mineral oil sludge through a dechlorinating agent pump 6, wherein the addition amount of the dechlorinating agent is 0.05 wt% of the amount of the waste mineral oil sludge in the step (1), stirring and mixing under the action of a strong mixing emulsion pump 11, then entering a dechlorinating buffer tank 12, and performing dechlorination reaction at 280 ℃; a pressure difference controller is adopted for feedback regulation, and the pressure of the dechlorination buffer tank 12 is maintained to be 1 MPa; and the residence time of the waste mineral oil sludge in the dechlorination buffer tank 12 is 15min by adopting the clapboard type reaction kettle. And the distillation fraction of the original waste oil generated by three-phase separation enters a hydrofining unit after heat exchange.
The dechlorinating agent is obtained by compounding ethylenediamine, organic quaternary ammonium base and strong basic ionic liquid, wherein the mass ratio of the ethylenediamine to the organic quaternary ammonium base to the strong basic ionic liquid is 25:45: 30;
the organic quaternary ammonium base is cetyl trimethyl ammonium hydroxide; the strong-alkaline ionic liquid is 1, 3-dimethyl imidazole ionic liquid.
(3) Tubular reaction unit
Mixing dechlorinated waste mineral oil sludge with a coking inhibitor injected by a coking inhibitor pump 7, firstly exchanging heat to 300 ℃ through a third heat exchanger 21, rapidly heating through a heating furnace 13, injecting soft water through a water injection pump 8, and then entering a tubular reactor 14 to obtain an oil product; before entering the tubular reactor 14, a certain amount of soft water is injected to ensure that the oil gas in the reactor reaches a certain linear speed, so that the coking of the tubular reactor 14 is delayed to the maximum extent, the yield of the oil gas is increased, and the generation of residual coke is reduced.
The addition amount of the coking inhibitor is 0.8 wt.% of the amount of the waste mineral oil sludge in the step (1), the dechlorination agent is obtained by compounding sulfonic amine salt with polyoxyalkylamine and arylamine group polymerization substances, and the mass ratio of the sulfonic amine salt to the polyoxyalkylamine and arylamine group polymerization substances is 40: 60; the sulfonic amine salt is thiophosphate alkylbenzene sulfonic acid diamine salt; the polymeric substances of polyoxyalkylamine and arylamine are fatty amine polyoxyethylene ether;
the adding amount of the soft water is 1.5 wt.% of the using amount of the waste mineral oil sludge in the step (1), and a medium-pressure inlet diaphragm water injection pump with the outlet pressure of 10MPa is adopted as the water injection pump 8 and is made of 316 SS; the tubular reactor 14 had a pyrolysis temperature of 560 ℃, a reaction pressure of 6MPa and a residence time of 6 seconds. The material of the tubular reactor 14 is incoloy 800.
(4) Delayed pyrolysis unit
The oil obtained from the tubular reactor 14 is depressurized by a high-temperature pressure reducing valve and then enters a first buffer pyrolysis tower 15. The pressure sensor and the pneumatic regulating valve are matched to control the tower top pressure of the first buffer pyrolysis tower 15 to be 1.2 MPa. The reaction temperature in the first buffer pyrolysis tower 15 is 550 ℃; the residence time in the first buffer pyrolysis column 15 was 1.5 hours. The oil products stay in the first buffer pyrolysis tower 15 to generate coke, the top of the first buffer pyrolysis tower 15 generates distillate oil and pyrolysis gas, the distillate oil and the pyrolysis gas enter a fractionation unit to carry out gas-liquid separation, and a small amount of ash residues are generated at the bottom and can be removed at regular time. The second buffer pyrolysis tower 16 is a standby pyrolysis tower, and when the first buffer pyrolysis tower 15 reaches the operation time, the second buffer pyrolysis tower 16 can be switched to the standby second buffer pyrolysis tower, so that the continuous operation of the device is ensured.
(5) Fractionation unit
The distillate oil and the pyrolysis gas coming out from the top of the buffer pyrolysis tower enter a fractionating tower 17 for gas-liquid separation, the pressure in the fractionating tower 17 is 0.15MPa, and the temperature of a reduced pressure outlet of the fractionating tower 17 is 300 ℃. The gas phase is separated and then is discharged to a torch system 23, and the liquid phase side line is extracted and divided into two sections; and (3) extracting gasoline and diesel fractions at the upper section, mixing a part of gasoline and diesel fractions with the waste mineral oil sludge subjected to heat exchange in the step (2) for cyclic viscosity reduction and dechlorination, wherein the cyclic proportion of the gasoline and diesel fractions is 60%, or performing full-reflux online cleaning, mixing the other part of gasoline and diesel fractions with the lubricating oil fractions extracted at the lower section to obtain fraction mixed oil, and feeding the fraction mixed oil into a hydrofining unit. The liquid level of the fractionating tower 17 is controlled by a non-contact differential pressure transmitter and a pneumatic regulating valve.
(6) Hydrorefining unit
The distillate mixed oil is merged with the distillation distillate of the original waste oil after heat exchange, enters a hydrofining reactor 19 after heat exchange by a second heat exchanger 18, the pressure of the hydrofining reactor 19 is 16MPa, the reaction temperature is 370 ℃, and the volume hydrogen-oil ratio is 600: 1. Through the reaction sections of hydrogenation treatment, hydrodewaxing, complementary isomerization refining and the like, and through the saturated reaction of unsaturated hydrocarbons, high-quality distillate oil and high-quality II-type lubricating oil base oil products are obtained by reduction.
Example 4
(1) Filter unit
The waste mineral oil sludge obtained after the separation of the waste mineral oil in the waste mineral oil tank 1 by the three-phase separator 3 or the treatment of the solvent treatment tank 2 enters the sludge tank 4, is mixed with the viscosity reducer injected by the viscosity reducer pump 5, exchanges heat to 120 ℃ by the fourth heat exchanger 20, is filtered by the filtering device 9, and enters the dechlorination unit. The raw waste oil produced by three-phase separation of waste mineral oil is fed into a distillation column 22 to produce a distillation fraction, and the produced gas is fed into a flare system 23. Wherein the aperture of the filter screen of the filter device 9 is 120 meshes; the processing solvent in the solvent processing tank 2 is 90# solvent oil; the addition amount of the viscosity reducer is 0.2 wt.% of the dosage of the waste mineral oil sludge, and the viscosity reducer is obtained by compounding polyamides, polyoxyethylene ethers and monoterpene compounds, wherein the mass ratio of the polyamides, the polyoxyethylene ethers and the monoterpene compounds is 65:20: 15;
the polyamide is a polymer generated by copolymerizing 2-acrylamide-2-methylpropanesulfonic acid and maleic anhydride, and the mass ratio of the 2-acrylamide-2-methylpropanesulfonic acid to the maleic anhydride is 2: 1; the polyoxyethylene ether is coconut oil amine polyoxyethylene ether; the monoterpene compound is citral.
(2) Dechlorination unit
Exchanging heat between the filtered waste mineral oil sludge and the distillation fraction of original waste oil generated by three-phase separation in a first heat exchanger 10, injecting a dechlorinating agent into the heat-exchanged waste mineral oil sludge through a dechlorinating agent pump 6, wherein the addition amount of the dechlorinating agent is 0.08 wt% of the amount of the waste mineral oil sludge in the step (1), stirring and mixing under the action of a strong mixing emulsification pump 11, then entering a dechlorinating buffer tank 12, and performing dechlorination reaction at 260 ℃; a pressure difference controller is adopted for feedback regulation, and the pressure of the dechlorination buffer tank 12 is maintained to be 1 MPa; and the residence time of the waste mineral oil sludge in the dechlorination buffer tank 12 is increased by adopting the clapboard type reaction kettle to be 20 min. And the distillation fraction of the original waste oil generated by three-phase separation enters a hydrofining unit after heat exchange.
The dechlorinating agent is obtained by compounding ethylenediamine, organic quaternary ammonium base and strongly basic ionic liquid, wherein the mass ratio of the ethylenediamine to the organic quaternary ammonium base to the strongly basic ionic liquid is 40:40: 20;
the organic quaternary ammonium base is tetrapropylammonium hydroxide; the strongly alkaline ionic liquid is polyethylene glycol functionalized bisimidazole type ionic liquid.
(3) Tubular reaction unit
Mixing dechlorinated waste mineral oil sludge with a coking inhibitor injected by a coking inhibitor pump 7, firstly exchanging heat to 300 ℃ through a third heat exchanger 21, rapidly heating through a heating furnace 13, injecting soft water through a water injection pump 8, and then entering a tubular reactor 14 to obtain an oil product; before entering the tubular reactor 14, a certain amount of soft water is injected to ensure that the oil gas in the reactor reaches a certain linear speed, so that the coking of the tubular reactor 14 is delayed to the maximum extent, the yield of the oil gas is increased, and the generation of residual coke is reduced.
The addition amount of the coking inhibitor is 0.8 wt.% of the amount of the waste mineral oil sludge in the step (1), the dechlorination agent is obtained by compounding sulfonic amine salt with polyoxyalkylamine and arylamine group polymerization substances, and the mass ratio of the sulfonic amine salt to the polyoxyalkylamine and arylamine group polymerization substances is 45: 55; the sulfonic acid amine salt is dodecyl benzene sulfonic acid isopropyl alcohol amine salt; the polymeric substance of polyoxyalkylamine and arylamine is polyoxyethylene dodecylamine;
the adding amount of the soft water is 0.5 wt% of the using amount of the waste mineral oil sludge in the step (1), and a medium-pressure inlet diaphragm water injection pump with the outlet pressure of 10MPa is adopted as the water injection pump 8 and is made of 316 SS; the pyrolysis temperature of the tubular reactor 14 was 540 ℃, the reaction pressure was 5MPa, and the residence time was 7 seconds. The material of the tubular reactor 14 is hastelloy C276.
(4) Delayed pyrolysis unit
The oil obtained from the tubular reactor 14 is depressurized by a high-temperature pressure reducing valve and then enters a first buffer pyrolysis tower 15. The pressure sensor and the pneumatic regulating valve are matched to control the tower top pressure of the first buffer pyrolysis tower 15 to be 1.5 MPa. The reaction temperature in the first buffer pyrolysis tower 15 is 535 ℃; the residence time in the first buffer pyrolysis column 15 was 2 hours. The oil products stay in the first buffer pyrolysis tower 15 to generate coke, distillate oil and pyrolysis gas are generated at the top of the first buffer pyrolysis tower 15 and enter the fractionation unit to be subjected to gas-liquid separation, and a small amount of ash is generated at the bottom and can be removed at regular time. The second buffer pyrolysis tower 16 is a standby pyrolysis tower, and when the first buffer pyrolysis tower 15 reaches the operation time, the second buffer pyrolysis tower 16 can be switched to the standby second buffer pyrolysis tower, so that the continuous operation of the device is ensured.
(5) Fractionation unit
The distillate oil and the pyrolysis gas coming out from the top of the buffer pyrolysis tower enter a fractionating tower 17 for gas-liquid separation, the pressure in the fractionating tower 17 is 0.2MPa, and the temperature of a reduced pressure outlet of the fractionating tower 17 is 300 ℃. The gas phase is separated and then is subjected to a torch firing system 23, and the liquid phase side line extraction is divided into two sections; and (3) extracting gasoline and diesel fractions at the upper section, mixing a part of gasoline and diesel fractions with the waste mineral oil sludge subjected to heat exchange in the step (2) for cyclic viscosity reduction and dechlorination, wherein the cyclic proportion of the gasoline and diesel fractions is 30%, or performing total reflux on-line cleaning, mixing the other part of gasoline and diesel fractions with the lubricating oil fractions extracted at the lower section to obtain fraction mixed oil, and feeding the fraction mixed oil into a hydrofining unit. The liquid level of the fractionating tower 17 is controlled by a non-contact differential pressure transmitter and a pneumatic regulating valve.
(6) Hydrorefining unit
The distillate mixed oil is converged with the distillation distillate of the original waste oil after heat exchange, enters a hydrofining reactor 19 after heat exchange by a second heat exchanger 18, the pressure of the hydrofining reactor 19 is 15MPa, the reaction temperature is 360 ℃, and the volume hydrogen-oil ratio is 500: 1. Through the reaction sections of hydrogenation treatment, hydrodewaxing, complementary isomerization refining and the like, and through the saturated reaction of unsaturated hydrocarbons, high-quality distillate oil and high-quality II-type lubricating oil base oil products are obtained by reduction.
Example 5
(1) Filter unit
The waste mineral oil sludge obtained after the waste mineral oil in the waste mineral oil tank 1 is separated by the three-phase separator 3 or treated by the solvent treatment tank 2 enters the sludge tank 4, is mixed with the viscosity reducer injected by the viscosity reducer pump 5, exchanges heat to 110 ℃ by the fourth heat exchanger 20, is filtered by the filtering device 9, and enters the dechlorination unit. The raw waste oil from the three-phase separation of the waste mineral oil is fed to a distillation column 22 to produce a distillation cut and the resulting gas is fed to a flare system 23. Wherein the filter mesh diameter of the filter device 9 is 160 meshes; the processing solvent in the solvent processing tank 2 is 90# solvent oil; the addition amount of the viscosity reducer is 0.1 wt.% of the amount of the waste mineral oil sludge, and the viscosity reducer is obtained by compounding alcohol amines, polyoxyethylene ethers and monoterpene compounds, wherein the mass ratio of the alcohol amines, the polyoxyethylene ethers and the monoterpene compounds is 70:15: 15;
the alcamines are N, N-diethylethanolamine; the polyoxyethylene ether is coco amine polyoxyethylene ether; the monoterpene compound is myrcene.
(2) Dechlorination unit
Heat exchange is carried out on the filtered waste mineral oil sludge and the distillation fraction of original waste oil generated by three-phase separation in a first heat exchanger 10, dechlorinating agent is injected into the heat-exchanged waste mineral oil sludge through a dechlorinating agent pump 6, the addition amount of the dechlorinating agent is 0.15 wt% of the amount of the waste mineral oil sludge in the step (1), the waste mineral oil sludge is stirred and mixed under the action of a strong mixing emulsification pump 11, and then the mixture enters a dechlorinating buffer tank 12 to carry out dechlorination reaction at 270 ℃; a pressure difference controller is adopted for feedback regulation, and the pressure of the dechlorination buffer tank 12 is maintained to be 1.5 MPa; and the residence time of the waste mineral oil sludge in the dechlorination buffer tank 12 is 25min by adopting the clapboard type reaction kettle. And the distillation fraction of the original waste oil generated by three-phase separation enters a hydrofining unit after heat exchange.
The dechlorinating agent is obtained by compounding ethylenediamine, organic quaternary ammonium base and strongly basic ionic liquid, wherein the mass ratio of the ethylenediamine to the organic quaternary ammonium base to the strongly basic ionic liquid is 35:40: 25;
the organic quaternary ammonium base is tetrabutyl ammonium hydroxide; the strong-alkaline ionic liquid is 1, 3-dimethyl imidazole ionic liquid.
(3) Tubular reaction unit
Mixing dechlorinated waste mineral oil sludge with a coking inhibitor injected by a coking inhibitor pump 7, firstly exchanging heat to 300 ℃ through a third heat exchanger 21, rapidly heating through a heating furnace 13, injecting soft water through a water injection pump 8, and then entering a tubular reactor 14 to obtain an oil product; before entering the tubular reactor 14, a certain amount of soft water is injected to ensure that the oil gas in the reactor reaches a certain linear speed, so that the coking of the tubular reactor 14 is delayed to the maximum extent, the yield of the oil gas is increased, and the generation of residual coke is reduced.
The addition amount of the anti-coking agent is 1 wt.% of the amount of the waste mineral oil sludge in the step (1), the dechlorination agent is obtained by compounding sulfonic amine salt with polyoxyalkylamine and arylamine group polymerization substances, wherein the mass ratio of the sulfonic amine salt to the polyoxyalkylamine and arylamine group polymerization substances is 35: 65; the sulfonic amine salt is thiophosphate alkylbenzene sulfonic acid diamine salt; the polymeric substance of polyoxyalkylamine and arylamine is dodecyl amine polyoxyethylene ether;
the adding amount of the soft water is 1.5 wt.% of the using amount of the waste mineral oil sludge in the step (1), and a medium-pressure inlet diaphragm water injection pump with the outlet pressure of 10MPa is adopted as the water injection pump 8 and is made of 316 SS; the tubular reactor 14 had a pyrolysis temperature of 550 ℃, a reaction pressure of 5MPa and a residence time of 8 seconds. The material of the tubular reactor 14 is incoloy 800.
(4) Delayed pyrolysis unit
The oil obtained from the tubular reactor 14 is depressurized by a high-temperature pressure reducing valve and then enters a first buffer pyrolysis tower 15. The pressure sensor and the pneumatic regulating valve are matched to control the tower top pressure of the first buffer pyrolysis tower 15 to be 1 MPa. The reaction temperature in the first buffer pyrolysis tower 15 is 540 ℃; the residence time in the first buffer pyrolysis column 15 was 1 hour. The oil products stay in the first buffer pyrolysis tower 15 to generate coke, the top of the first buffer pyrolysis tower 15 generates distillate oil and pyrolysis gas, the distillate oil and the pyrolysis gas enter a fractionation unit to carry out gas-liquid separation, and a small amount of ash residues are generated at the bottom and can be removed at regular time. The second buffer pyrolysis tower 16 is a standby pyrolysis tower, and when the first buffer pyrolysis tower 15 reaches the operation time, the second buffer pyrolysis tower 16 can be switched to the standby second buffer pyrolysis tower, so that the continuous operation of the device is ensured.
(5) Fractionation unit
The distillate oil and the pyrolysis gas coming out from the top of the buffer pyrolysis tower enter a fractionating tower 17 for gas-liquid separation, the pressure in the fractionating tower 17 is 0.3MPa, and the temperature of a reduced pressure outlet of the fractionating tower 17 is 280 ℃. The gas phase is separated and then is subjected to a torch firing system 23, and the liquid phase side line extraction is divided into two sections; and (3) extracting gasoline and diesel fractions at the upper section, mixing a part of gasoline and diesel fractions with the waste mineral oil sludge subjected to heat exchange in the step (2) for cyclic viscosity reduction and dechlorination, wherein the cyclic proportion of the gasoline and diesel fractions is 50%, or performing total reflux on-line cleaning, mixing the other part of gasoline and diesel fractions with the lubricating oil fractions extracted at the lower section to obtain fraction mixed oil, and feeding the fraction mixed oil into a hydrofining unit. The liquid level of the fractionating tower 17 is controlled by a non-contact differential pressure transmitter and a pneumatic regulating valve.
(6) Hydrorefining unit
The distillate mixed oil is converged with the distillation distillate of the original waste oil after heat exchange, enters a hydrofining reactor 19 after heat exchange by a second heat exchanger 18, the pressure of the hydrofining reactor 19 is 13MPa, the reaction temperature is 350 ℃, and the volume hydrogen-oil ratio is 800: 1. Through the reaction sections of hydrogenation treatment, hydrodewaxing, complementary isomerization refining and the like, and through the saturated reaction of unsaturated hydrocarbons, high-quality distillate oil and high-quality II-type lubricating oil base oil products are obtained by reduction.
The results of the material balance measurements performed throughout the recycling of the waste mineral oil sludge of examples 1-5 are shown in table 1 below.
TABLE 1 tables of material balance data for examples 1-5
Figure BDA0002827168090000141
Figure BDA0002827168090000151
The gas composition generated during the entire recycling of the waste mineral oil sludge in examples 1-5 was analyzed and the data is shown in table 2.
TABLE 2 gas composition analysis data sheet for examples 1-5
Figure BDA0002827168090000152
Figure BDA0002827168090000161
The properties of the waste mineral oil, the waste mineral oil sludge and the obtained product in example 2 were measured, and the data are shown in Table 3.
Table 3 table of data on measurement of properties of waste mineral oil, waste mineral oil sludge, and obtained product in example 2
Figure BDA0002827168090000162
Figure BDA0002827168090000171
According to the data, the method can solve the problem of deep processing and utilization of the waste mineral oil sludge, saves the environmental protection cost for deep processing and utilization of the sludge; and certain products with high added value can be obtained, and the economic benefit is increased. Meanwhile, better raw materials can be provided for the hydrofining reactor, and the recovery rate of the lubricating oil in the whole process of the waste mineral oil regeneration device is improved. And the process has the characteristics of high yield, less carbon deposition of ash, difficult coking of pipelines and easy continuous operation.
The system for recycling the waste mineral oil sludge comprises a waste mineral oil tank 1, a sludge tank 4, a dechlorination buffer tank 12, a tubular reactor 14, a buffer pyrolysis tower, a fractionating tower 17, a hydrofining reactor 19 and a product tank 25 which are sequentially connected with one another, wherein the waste mineral oil tank 1 is connected with the other end of the buffer pyrolysis tower; a fourth heat exchanger 20, a filtering device 9, a first heat exchanger 10 and a forced mixing emulsification pump 11 are sequentially arranged on a pipeline between the oil sludge tank 4 and the dechlorination buffer tank 12; a third heat exchanger 21 and a heating furnace 13 are sequentially arranged on a pipeline between the dechlorination buffer tank 12 and the tubular reactor 14; a second heat exchanger 18 is arranged between the fractionating tower 17 and the hydrofining reactor 19;
a three-phase separator 3 is arranged between the mineral oil tank 1 and the oil sludge tank 4, the three-phase separator 3 is connected with a first heat exchanger 10 through a distillation tower 22, and the first heat exchanger 10 is also connected with a pipeline between a fractionating tower 17 and a second heat exchanger 18; the fractionating column 17 is also connected to the line between the first heat exchanger 10 and the intensive mixing emulsification pump 11 via a line.
A viscosity reducer pump 5 is connected on a pipeline between the oil sludge tank 4 and the fourth heat exchanger 20, a dechlorinating agent pump 6 is connected on a pipeline between the first heat exchanger 10 and the strong mixing emulsifying pump 11, a coking inhibitor pump 7 is connected on a pipeline between the dechlorinating buffer tank 12 and the third heat exchanger 21, and a water injection pump 8 is connected on a pipeline between the heating furnace 13 and the tubular reactor 14.
The buffer pyrolysis tower comprises a first buffer pyrolysis tower 15 and a second buffer pyrolysis tower 16, and the first buffer pyrolysis tower 15 and the second buffer pyrolysis tower 16 are respectively connected with an ash tank 24; a solvent treatment tank 2 is also arranged between the mineral oil tank 1 and the oil sludge tank 4; the three-phase separator 3 is connected to a flare system 23, and the flare system 23 is also connected to the top of the fractionation column 17.

Claims (10)

1. A method for recycling waste mineral oil sludge is characterized by comprising the following steps:
(1) filter unit
The method comprises the following steps of (1) enabling waste mineral oil sludge obtained after three-phase separation or solvent treatment of waste mineral oil to enter an oil sludge tank, mixing the waste mineral oil sludge with a viscosity reducer injected by a viscosity reducer pump, firstly exchanging heat, filtering by a filtering device, and enabling the waste mineral oil sludge to enter a dechlorination unit;
(2) dechlorination unit
The filtered waste mineral oil sludge exchanges heat with distillation fractions of original waste oil generated by three-phase separation, dechlorinating agent is injected into the heat-exchanged waste mineral oil sludge through a dechlorinating agent pump, and the heat-exchanged waste mineral oil sludge is stirred and mixed under the action of a strong mixing emulsification pump and then enters a dechlorinating buffer tank for dechlorinating reaction; the distillation fraction of the original waste oil generated by three-phase separation enters a hydrofining unit after heat exchange;
(3) tubular reaction unit
Mixing the dechlorinated waste mineral oil sludge with a coking inhibitor injected by a coking inhibitor pump, firstly exchanging heat, heating by a heating furnace, injecting soft water through a water injection pump, and then entering a tubular reactor to obtain an oil product;
(4) delayed pyrolysis unit
After the pressure of the oil product obtained by the tubular reactor is reduced by a high-temperature pressure reducing valve, the oil product enters a buffer pyrolysis tower to stay for coke formation, distillate oil and pyrolysis gas are generated at the top of the buffer pyrolysis tower, ash is generated at the bottom of the buffer pyrolysis tower, and the distillate oil and the pyrolysis gas enter a fractionating unit to be subjected to gas-liquid separation;
(5) fractionation unit
Carrying out gas-liquid separation on distillate oil and pyrolysis gas in a fractionating tower, separating the gas phase, then removing the gas phase to a torch system, and dividing the liquid phase side line extraction into two sections; gasoline and diesel fractions are extracted from the upper section, one part of the gasoline and diesel fractions is mixed with the waste mineral oil sludge subjected to heat exchange in the step (2) for cyclic viscosity reduction dechlorination or total reflux on-line cleaning, the other part of the gasoline and diesel fractions is mixed with the lubricating oil fractions extracted from the lower section to obtain fraction mixed oil, and the fraction mixed oil enters a hydrofining unit;
(6) hydrorefining unit
And merging the distillate mixed oil with the distillation distillate of the original waste oil after heat exchange, performing heat exchange by a heat exchanger, entering a hydrofining reactor, and performing hydrotreating, hydrodewaxing and complementary isomerous refining reaction sections to obtain distillate oil and a II-type lubricating oil base oil product.
2. The method of recycling waste mineral oil sludge as claimed in claim 1, wherein: in the step (1), the aperture of the filter screen of the filter device is 120-200 meshes; the outlet temperature is 80-120 ℃ after heat exchange; the solvent adopted in the solvent treatment process is 90# solvent oil or 150-;
the addition amount of the viscosity reducer is 0.05-0.2 wt% of the amount of the waste mineral oil sludge, and the viscosity reducer is obtained by compounding polyamides or alkanolamines with polyoxyethylene ethers and monoterpene compounds, wherein the mass ratio of the polyamides or the alkanolamines to the polyoxyethylene ethers to the monoterpene compounds is 50-70:15-25: 15-25;
the polyamide is a polymer of 2-acrylamide-2-methylpropanesulfonic acid and maleic anhydride, and the mass ratio of the 2-acrylamide-2-methylpropanesulfonic acid to the maleic anhydride is 2: 1;
the alcamines are N-dodecyl-1, 3-propanol diamine or N, N-diethylethanolamine;
the polyoxyethylene ether is stearyl amine polyoxyethylene ether, coco amine polyoxyethylene ether or octadecyl amine polyoxyethylene ether;
the monoterpene compound is myrcene, limonene or citral.
3. The method of recycling waste mineral oil sludge as claimed in claim 1, wherein: in the step (2), the addition amount of a dechlorinating agent is 0.05-0.2 wt% of the amount of the waste mineral oil sludge in the step (1), the dechlorinating agent is obtained by compounding ethylenediamine, organic quaternary ammonium and strongly alkaline ionic liquid, wherein the mass ratio of the ethylenediamine to the organic quaternary ammonium to the strongly alkaline ionic liquid is 20-40:25-45: 15-35;
the organic quaternary ammonium base is cetyl trimethyl ammonium hydroxide, tetrabutyl ammonium hydroxide or tetrapropyl ammonium hydroxide;
the strongly alkaline ionic liquid is polyethylene glycol functionalized bisimidazole type ionic liquid, 1-butyl-3-methylimidazole type ionic liquid or 1, 3-dimethyl imidazole type ionic liquid;
the temperature of the dechlorination reaction is 200-280 ℃, the pressure of the dechlorination reaction is 1-2MPa, and the retention time of the waste mineral oil sludge in the dechlorination buffer tank is 10-30 min.
4. The method of recycling waste mineral oil sludge as claimed in claim 1, wherein: in the step (3), the addition amount of the coking inhibitor is 0.5-1 wt.% of the amount of the waste mineral oil sludge in the step (1), and the dechlorinating agent is obtained by compounding a sulfonic amine salt with polyoxyalkylamine and arylamine-based polymeric substances, wherein the mass ratio of the sulfonic amine salt to the polyoxyalkylamine to the arylamine-based polymeric substances is 30-50: 50-70;
the sulfonic acid amine salt is thiophosphate alkylbenzene sulfonic acid diamine salt or dodecyl benzene sulfonic acid isopropanol amine salt;
the polymeric substances of polyoxyalkylamine and arylamine are octadecyl amine polyoxyethylene ether, dodecyl amine polyoxyethylene ether, fatty amine polyoxyethylene ether, polyolefin succinimide or polyoxyethylene lauryl amine;
the adding amount of the soft water is 0.5-2 wt% of the using amount of the waste mineral oil sludge in the step (1), and a medium-pressure inlet diaphragm water injection pump with the outlet pressure of 7-10MPa is adopted as the water injection pump; the pyrolysis temperature of the tubular reactor is 500-560 ℃, the reaction pressure is 5-7MPa, and the retention time is 3-8 seconds; heat exchange is carried out to 300-320 ℃.
5. The method of recycling waste mineral oil sludge as claimed in claim 1, wherein: in the step (4), the pressure at the top of the buffer pyrolysis tower is 1-1.5MPa, and the reaction temperature is 510-555 ℃; the residence time of the buffer pyrolysis tower is 1-2 hours.
6. The method of recycling waste mineral oil sludge as claimed in claim 1, wherein: in the step (5), the pressure in the fractionating tower is 0.15-0.35MPa, the temperature of the reduced pressure outlet of the fractionating tower is 180-.
7. The method of recycling waste mineral oil sludge as claimed in claim 1, wherein: in the step (6), the pressure of the hydrogen refining reactor is 12-16MPa, the reaction temperature is 350-390 ℃, and the volume hydrogen-oil ratio is 300-850: 1.
8. A system for carrying out the method of recycling waste mineral oil sludge according to any one of claims 1 to 7, wherein: comprises a waste mineral oil tank (1), an oil sludge tank (4), a dechlorination buffer tank (12), a tubular reactor (14), a buffer pyrolysis tower, a fractionating tower (17), a hydrofining reactor (19) and a product tank (25) which are connected in sequence; a fourth heat exchanger (20), a filtering device (9), a first heat exchanger (10) and a strong mixing emulsification pump (11) are sequentially arranged on a pipeline between the sludge tank (4) and the dechlorination buffer tank (12); a third heat exchanger (21) and a heating furnace (13) are sequentially arranged on a pipeline between the dechlorination buffer tank (12) and the tubular reactor (14); a second heat exchanger (18) is arranged between the fractionating tower (17) and the hydrofining reactor (19);
a three-phase separator (3) is arranged between the waste mineral oil tank (1) and the oil sludge tank (4), the three-phase separator (3) is connected with a first heat exchanger (10) through a distillation tower (22), and the first heat exchanger (10) is also connected with a pipeline between a fractionating tower (17) and a second heat exchanger (18); the fractionating tower (17) is also connected with a pipeline between the first heat exchanger (10) and the intensive mixing emulsification pump (11) through a pipeline.
9. The system for recycling waste mineral oil sludge as claimed in claim 8, wherein: the viscosity reducer pump (5) is connected to a pipeline between the oil sludge tank (4) and the fourth heat exchanger (20), the dechlorination agent pump (6) is connected to a pipeline between the first heat exchanger (10) and the forced mixing emulsion pump (11), the coke inhibitor pump (7) is connected to a pipeline between the dechlorination buffer tank (12) and the third heat exchanger (21), and the water injection pump (8) is connected to a pipeline between the heating furnace (13) and the tubular reactor (14).
10. The system for recycling waste mineral oil sludge as claimed in claim 8, wherein: the buffering pyrolysis tower comprises a first buffering pyrolysis tower (15) and a second buffering pyrolysis tower (16), and the first buffering pyrolysis tower (15) and the second buffering pyrolysis tower (16) are respectively connected with an ash tank (24); a solvent treatment tank (2) is also arranged between the waste mineral oil tank (1) and the oil sludge tank (4); the three-phase separator (3) is connected with a flare system (23), and the flare system (23) is also connected with the top of the fractionating tower (17).
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