CN111253964B - Method for treating polymer-containing oil sludge - Google Patents

Method for treating polymer-containing oil sludge Download PDF

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CN111253964B
CN111253964B CN202010088972.6A CN202010088972A CN111253964B CN 111253964 B CN111253964 B CN 111253964B CN 202010088972 A CN202010088972 A CN 202010088972A CN 111253964 B CN111253964 B CN 111253964B
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oil
oil sludge
sludge
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CN111253964A (en
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薛广海
李强
刘庆
王瑀辉
台广峰
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BGRIMM Technology Group Co Ltd
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    • 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
    • C10G1/002Production of liquid hydrocarbon mixtures from oil-shale, oil-sand, or non-melting solid carbonaceous or similar materials, e.g. wood, coal in combination with oil conversion- or refining processes
    • CCHEMISTRY; METALLURGY
    • C10PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10GCRACKING HYDROCARBON OILS; PRODUCTION OF LIQUID HYDROCARBON MIXTURES, e.g. BY DESTRUCTIVE HYDROGENATION, OLIGOMERISATION, POLYMERISATION; RECOVERY OF HYDROCARBON OILS FROM OIL-SHALE, OIL-SAND, OR GASES; REFINING MIXTURES MAINLY CONSISTING OF HYDROCARBONS; REFORMING OF NAPHTHA; MINERAL WAXES
    • C10G1/00Production of liquid hydrocarbon mixtures from oil-shale, oil-sand, or non-melting solid carbonaceous or similar materials, e.g. wood, coal
    • CCHEMISTRY; METALLURGY
    • C10PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10GCRACKING HYDROCARBON OILS; PRODUCTION OF LIQUID HYDROCARBON MIXTURES, e.g. BY DESTRUCTIVE HYDROGENATION, OLIGOMERISATION, POLYMERISATION; RECOVERY OF HYDROCARBON OILS FROM OIL-SHALE, OIL-SAND, OR GASES; REFINING MIXTURES MAINLY CONSISTING OF HYDROCARBONS; REFORMING OF NAPHTHA; MINERAL WAXES
    • C10G2300/00Aspects relating to hydrocarbon processing covered by groups C10G1/00 - C10G99/00
    • C10G2300/10Feedstock materials
    • C10G2300/1003Waste materials

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  • Engineering & Computer Science (AREA)
  • Oil, Petroleum & Natural Gas (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Wood Science & Technology (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • General Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Separation Of Suspended Particles By Flocculating Agents (AREA)
  • Treatment Of Sludge (AREA)

Abstract

The invention belongs to the field of solid waste separation and treatment, and particularly relates to a treatment process for polymer-containing oil sludge. Sequentially carrying out the treatments of pulping, breaking and polymerizing, pre-stripping oil sludge, separating oil sludge and refining oil products on polymer-containing oil sludge to be treated; the oil sludge is pre-stripped by performing strong friction on the oil sludge after pulping and breaking aggregation by using one or more of a ball mill, a scrubbing machine or a kneading machine. The oil sludge separation is to make the material subjected to the oil sludge pre-stripping treatment circularly flow at a high speed, so as to realize the separation of oil-containing floating slag and silt. According to the invention, through the treatment of oil sludge pre-stripping and oil sludge separation, the desorption effect of crude oil from the surfaces of sand and clay is greatly improved, and the difficulty of the treatment of the crude oil at the later stage is obviously reduced.

Description

Method for treating polymer-containing oil sludge
Technical Field
The invention belongs to the field of solid waste separation and treatment, and particularly relates to a treatment process for polymer-containing oil sludge.
Background
In the production, storage and transportation and oily sewage treatment processes of oil fields and oil refineries, a large amount of oily sludge is generated as an important pollutant listed in national hazardous waste records, the oily sludge has a large proportion in solid wastes, and if the oily sludge is directly discharged into the environment without reasonable treatment, the oily sludge not only harms the environment, but also wastes valuable petroleum resources.
The polymer flooding plays an irreplaceable important role in the crude oil exploitation process in China, and along with the large-scale application of the polymer flooding, a large amount of polymer-containing oil sludge is formed in the oilfield produced liquid. Compared with the traditional oily sludge, the oily sludge containing polymer greatly increases the treatment difficulty because of containing a large amount of polymers and chemical agents added in the treatment process of produced liquid.
At present, there are three main techniques for treating the traditional oily sludge: a reduction processing technique such as a tempering technique, an ultrasonic processing technique, or the like; stabilization treatment techniques such as biological treatment techniques, solidification treatment techniques, incineration treatment techniques, and the like; resource treatment technologies, such as thermal desorption treatment technology, solvent extraction technology, thermochemical washing technology and the like. Due to the complexity of polymer-containing oil sludge, the traditional oil sludge treatment technology has the defects of poor treatment effect, long treatment time, high treatment cost and the like.
For example, chinese patent 201410061927.6 reports a method for treating polymer-containing oil sludge and recovering crude oil, but the oil content in the tailings after treatment and the water content in the recovered crude oil are both high, and the treatment effect is not ideal. Chinese patent 201210335234.2 reports a separation method and equipment for polymer-containing oil sludge, which utilizes ultrasonic technology to treat polymer-containing oil sludge and has low energy conversion rate and high treatment cost. Chinese patent 201310091778.3 reports a low-temperature dry distillation device and method for oil sand, oil sludge, oil shale and biomass, wherein an external heating type rotary dry distillation furnace is used for realizing the pyrolysis of the oil sand, the oil sludge, the oil shale and the biomass, the treatment effect is good, but the device is complex and the treatment cost is high.
Disclosure of Invention
Aiming at the problems of unsatisfactory treatment effect, high cost and complex equipment in the process of treating polymer-containing sludge in the prior art, the invention provides a novel method for treating polymer-containing sludge.
The method comprises the steps of sequentially carrying out treatments of pulping, breaking and polymerizing, pre-stripping oil sludge, separating oil sludge and refining oil products on polymer-containing oil sludge to be treated;
the oil sludge pre-stripping is to perform strong friction on the oil sludge after pulping and breaking aggregation by using one or more of a ball mill, a scrubbing machine or a kneading machine;
the oil sludge separation is to make the material subjected to the oil sludge pre-stripping treatment circularly flow at a high speed, so as to realize the separation of oil-containing floating slag and silt.
According to the method, the polymer-containing oil sludge is subjected to pre-stripping treatment through strong friction, and the combined production between crude oil and sand is loosened and falls off while the oil sludge is crushed; carrying out high-speed circulating flow on the mixed slurry, and realizing the stripping of crude oil and silt through flow friction and permeation effects; the separation condition of the oil and the silt can be effectively improved through the treatment, and the oil and the silt with high purity can be obtained finally.
Preferably, in the process of strongly scrubbing by using the ball mill, the medium used by the ball mill is ceramic balls, and the size and the proportion of the ceramic balls are as follows: 35-45% of 100mm, 20-30% of 20mm, 20-30% of 40mm, 5-15% of 80mm and 20-40 min of treatment time.
Preferably, in the process of processing by adopting the scrubbing machine, the scrubbing time is 15-25 min.
Preferably, the scouring machine is a scouring machine commonly used in the industry.
Preferably, the high-speed circulation flow is carried out in two stages, the first stage only carries out the high-speed circulation flow, the second stage introduces air while carrying out the high-speed circulation flow, and the oil-containing scum moves upwards along with the upward discharge of the air, so that the separation from the silt is realized;
the first stage only carries out high-speed circulation flow, can promote the effective separation of oil and mud, and the second stage lets in air, and the oily material is because density is little, easily floats along with the air, finally realizes the separation of oily dross and silt particle.
Preferably, the high-speed circulation flow of the materials is realized by high-speed jet flow, and/or air is introduced into the system by an air compressor.
Preferably, in the oil-sludge separation process, the high-speed circulating flow speed of the material is 1-3 m/s; the flowing time of the first stage is 10-15 min, and the flowing time of the second stage is 5-10 min. Through the above operation, not only can the oil be sufficiently separated from the sand surface, but also the oil-containing scum and the silt can be sufficiently separated.
Preferably, the oil product refining comprises the following specific steps:
and mixing the oil-containing floating slag obtained after the oil sludge is separated with an organic solvent and water, after the upper organic phase is separated from the lower water phase, pumping the upper organic phase, continuously introducing the upper water phase into the lower water phase, circularly washing, and separating the upper oil phase after the washing is finished to obtain the diluted crude oil.
Preferably, the organic solvent is one or a mixture of two or more of hexane, pentane, heptane, naphtha, petroleum ether, toluene and xylene.
For oil-containing scum, the separation condition of oil and small-particle silt can be effectively improved through the treatment, and oil with higher purity is obtained.
As a preferred mode of operation, the resulting diluted crude oil is pumped to a distillation system for recovery of the crude oil and reuse of the solvent. The distillation system is one of flash evaporation, a single-effect evaporator, a multi-effect evaporator and an MVR evaporator.
Preferably, the flocculant is added to the mixed system before the upper organic phase is separated, and the circulating washing is carried out again to settle the solid phase particles therein. If the particle size of the scum solid material in the oil product refining system is small, the solid material is not easy to settle, and the flocculant is added to promote the settling of the material and the separation of the material and oil.
Preferably, separating the silt obtained after the oil sludge is separated; separating the obtained coarse mortar to obtain sand, carrying out secondary separation on the obtained fine ore pulp, carrying out oil sludge pre-stripping and oil sludge separation treatment on the oil-containing material subjected to secondary separation again to obtain oil-containing floating slag again, and carrying out oil product refining treatment again; and conveying the tailings obtained after secondary separation to a tailing flocculation section.
Preferably, the specific operation of the pulping and polymer breaking is to mix the polymer-containing oil sludge to be treated with water or brine with the total salt content of 1-8%, and then add one or two of a dispersant or a polymer breaking agent to carry out pulping and polymer breaking;
preferably, the mass ratio of the polymer-containing oil sludge to be treated to water or the salt-containing water with the total salt content of 1-8% is 1:1 to 1.5; in the process of mixing the polymer-containing oil sludge to be treated with water, controlling the temperature of a mixing system to be 50-90 ℃, and in the process of mixing the polymer-containing oil sludge to be treated with water with the total salt content of 1-8%, controlling the temperature of the mixing system to be 25-30 ℃;
preferably, the dispersant is Na2SiO3,Na2CO3One or more of NaOH, sodium polyphosphate or washing powder;
more preferably, the addition amount of the dispersing agent is 0-3% of the mass of the mixed system;
preferably, the polymerization breaking agent is one or more of a Fenton reagent, hydrogen peroxide, persulfate or hypochlorite;
more preferably, the addition amount of the dispersing agent is 0-3% of the mass of the mixed system;
preferably, the dispersing agent is added firstly, and then the polymerization breaking agent is added to treat the materials.
The water or saline water can be conventional industrial water such as shallow groundwater, city tap water, factory circulating water and the like, can also be seawater and the like, and can be selected according to the properties of oily sludge, operation requirements, operation environment and other conditions. And under the condition of selecting the method of the invention, the ideal treatment effect can be obtained by selecting any one of the water.
Preferably, before the slurry making and the breaking, the method also comprises the treatment of impurity separation of the materials to be treated, and various impurities carried in the raw materials can be effectively separated by various means and modes such as screening, manual selection, magnetic separation and the like.
As a preferred mode of operation, the method of the present invention comprises the steps of:
1) impurity separation: various impurities carried in the polymer-containing oil sludge to be treated are effectively separated by various means and modes such as screening, manual separation, magnetic separation and the like;
2) pulping and breaking polymerization: mixing polymer-containing oil sludge subjected to impurity separation with water or brine with the total salt content of more than 1-8%, and adding one or two of a dispersing agent or a polymer breaking agent to carry out slurry making and polymer breaking;
3) pre-stripping oil sludge: performing strong friction on the slurried and broken and aggregated oil sludge by using one or more of a ball mill, a scrubbing machine or a kneading machine;
4) oil-sludge separation: the material subjected to oil sludge pre-stripping treatment is subjected to high-speed circulating flow, so that separation of oil-containing scum and silt is realized;
5) oil product refining: mixing the oil-containing floating slag obtained after oil sludge separation treatment with an organic solvent and water, after an upper organic phase is separated from a lower water phase, pumping the upper organic phase, continuously introducing the upper organic phase into the lower water phase, performing circulating washing, and separating an upper oil phase after washing is completed to obtain diluted crude oil;
6) separating the silt obtained after the oil sludge is separated; separating the obtained coarse mortar to obtain sand, carrying out secondary separation on the obtained fine ore pulp, carrying out oil sludge pre-stripping and oil sludge separation treatment on the oil-containing material subjected to secondary separation again to obtain oil-containing floating slag again, and carrying out oil product refining treatment again; and conveying the tailings obtained after secondary separation to a tailing flocculation section.
The invention also aims to protect a treatment system containing polymer sludge, which comprises a sludge pre-stripping device, a sludge separation device and an oil product refining device which are connected in sequence;
the oil sludge pre-stripping device is one or more of a ball mill, a scrubbing machine or a kneading machine;
the oil sludge separation device comprises a tank body, an oil-containing scum outlet is formed in the top of the tank body, a silt product is formed in the bottom of the tank body, a feed port and a discharge port are formed in the outer wall of the tank body, a circulating pipeline is arranged between the feed port and the discharge port, a feed tee joint connected with the oil sludge pre-stripping device is arranged on the circulating pipeline, and a jet pump and an air inlet are arranged on the circulating pipeline between the feed tee joint and the feed port;
the oil refining device comprises a tank body, an organic phase outlet arranged at the top of the tank body and a fine soil tailing outlet arranged at the bottom of the tank body, wherein the outer wall of the tank body is provided with an organic phase agent inlet corresponding to the horizontal position of the water phase in the tank body, the organic phase outlet is connected with the organic phase inlet through a circulating pipeline, the circulating pipeline is provided with a circulating pump and a flocculating agent inlet, the outer wall of the tank body is provided with an oil-containing scum feed inlet and a water and organic solvent inlet, and the feed inlet is connected with a scum outlet of the oil sludge separation device.
Preferably, a silt outlet of the silt separator is connected with a silt separator, and a large-particle sand outlet of the silt separator is connected with a solid-liquid separator;
a small particle material outlet of the sand-mud separator is reversely connected to a feed inlet of the oil-mud stripping device;
or the small particle material outlet of the silt separator is connected to the oil product refining device;
or a small-particle material outlet of the sand-mud separator is connected to a separator, oil-containing scum and fine mud are further separated, the oil-containing scum obtained after separation is introduced into a feed inlet of the oil-mud stripping device again, and the fine mud obtained is introduced into a flocculating machine.
The connection mode is flexibly adjusted according to the condition of the small-particle materials, and if the small-particle materials are mainly oil-containing scum, the small-particle materials are introduced into a feed inlet of an oil product refining device; if the particle size of the small-particle materials is larger, the small-particle materials contain scum and materials which are not completely separated, the small-particle materials are led into an oil sludge pre-stripping device, and if the small-particle materials mainly contain scum and fine sand which is completely separated, the small-particle materials are led into a sorting machine.
The mud-sand separator is one or more of a vibrating screen, a centrifugal machine and a cyclone.
The device is suitable for the process.
The invention has the following beneficial effects:
according to the invention, through the treatment of oil sludge pre-stripping and oil sludge separation, the desorption effect of crude oil from the surfaces of sand and clay is greatly improved, and the difficulty of the treatment of the crude oil at the later stage is obviously reduced.
According to the invention, coarse sand and fine clay minerals in the polymer-containing oil sludge are separated, and the fine clay minerals are subjected to targeted treatment, so that the treatment effect and efficiency are obviously improved.
The oil-containing scum is treated by adopting a solvent refining system, so that the oil content of clay in the tailings is further reduced, the contents of solid and water in the recovered crude oil are obviously reduced, and the further treatment requirement of a refinery is met.
The oil content of the dry base of the tailings treated by the method is less than 1 percent, the recovery rate of the crude oil is higher than 95 percent, and the solid and water content in the recovered crude oil is less than 0.5 percent.
Drawings
FIG. 1 is a flow chart of the liquid phase treatment process of polymer-containing oil sludge according to the present invention;
FIG. 2 is a sludge separation unit according to the present invention;
FIG. 3 illustrates an oil refining apparatus according to the present invention;
in the figure, 1 is a tank body of an oil sludge separation device, 2 is an oil-containing scum outlet, 3 is a silt product, 4 is a feed inlet, 5 is a discharge outlet, 6 is a circulating pipeline, 7 is a feed tee, 8 is a jet pump, 9 is an air inlet, 10 is a tank body of an oil product refining device, 11 is an organic phase outlet, 12 is a fine soil tailing outlet, 13 is an organic phase agent inlet, 14 is a circulating pump, 15 is an oil-containing scum feed inlet, 16 is a water and organic solvent inlet, and 17 is a flocculant inlet.
Detailed Description
The following examples are intended to illustrate the invention but are not intended to limit the scope of the invention.
Example 1
(1) And (4) conveying the polymer-containing oil sludge to a vibrating screen by a screw to remove impurities mechanically, and screening out large stones and other impurities which are not suitable for pumping.
(2) Mixing the polymer-containing oil sludge after impurity removal with hot water at 50 ℃, wherein the mass ratio of the hot water to the polymer-containing oil sludge is 1:2, and then adding Na into the mixture2CO3,Na2CO3The adding amount is 0.2 percent of the mass of the ore pulp, the oil sludge is completely dispersed by stirring for 5min, and the stirring speed is 60r/min, so that the excessive emulsification of the oil sludge containing the polymer sludge is prevented. After the slurry is manufactured, adding hydrogen peroxide into the slurry for polymerization breaking, wherein the adding amount of the hydrogen peroxide is 0.2 percent of the mass of the slurry, stirring for polymerization breaking for 5min, and the stirring speed is 100 r/min.
(3) And (3) conveying the oil sludge subjected to slurry making and aggregation breaking in the step (2) to a scrubbing machine for mechanical scrubbing treatment for 20min, so that crude oil is stripped from the surface of the sand.
(4) As shown in fig. 2, the oil sludge scrubbed in the step (3) is conveyed to a tank body (9) by a slurry pump (7), and then is subjected to circulation separation for 5min in equipment connected with a discharge port (3), a feed tee (6), the slurry pump (7), a jet pump (10), an air inlet (5) and a feed port (2); air is filled in through the air inlet (5), the liquid phase is circulated for 5min, and scum is conveyed to a scum refining system through a scum outlet (1);
(5) and (3) after the scum is basically collected, pumping the ore pulp to a cyclone for cyclone desanding, conveying coarse sand ore pulp generated by cyclone to solid-liquid separation equipment, conveying fine ore pulp generated by cyclone to groove type separation equipment for secondary separation, returning the scum obtained by secondary separation to scrubbing treatment equipment in the step (3), and conveying the tailings to a tailing flocculation section.
(6) Conveying the scum obtained in the step (4) and the step (5) to a scum refining tank (11) by a pump (20), adding organic solvents of hexane and water into the scum by a pump (19), wherein the mass ratio of hexane to scum to water is 1:1:1, pumping the upper layer hexane diluted crude oil to a bottom layer water phase by a pump (18), circulating the solvent for extraction for 10min, adding a polyacrylamide flocculant in an amount of 0.03 percent of the mass of the pulp, and circulating for 2min again to settle fine solid phases in the scum. After washing, the diluted crude oil on the upper layer is conveyed to a solvent recovery system from an oil outlet (13), the ore pulp on the lower layer is discharged to a solid-liquid separation system by a pump (21), the solid-liquid separation equipment is a plate-and-frame filter press or a high-pressure filter, the solid phase is discharged outside, the water is recycled after oil-water separation of the liquid phase, and the oil enters a triple-effect evaporation system to recover the solvent.
(7) And (4) conveying the diluted crude oil generated in the step (6) to a three-effect evaporator for solvent recovery, recovering hexane for solvent refining, and using heat generated by hexane steam condensation for supplementing heat loss of process water.
(8) And (3) flocculating the tailings generated in the step (5), and reusing water generated after flocculation and sedimentation in the step (2), wherein the used flocculating agent is polyacrylamide, and the addition amount of the flocculating agent is 0.005 percent of the mass of the ore pulp.
(9) And (4) carrying out plate-and-frame filter pressing on the coarse sand pulp generated in the step (5) and the flocculated pulp obtained in the step (8). The flow chart of the above process is shown in FIG. 1.
Figure BDA0002383071770000081
Example 2
(1) And (4) conveying the polymer-containing oil sludge to a vibrating screen by a screw to remove impurities mechanically, and screening out large stones and other impurities which are not suitable for pumping.
(2) Mixing the polymer-containing oil sludge subjected to impurity removal with hot water at the temperature of 80 ℃, wherein the mass ratio of the hot water to the polymer-containing oil sludge is 1:3, then adding sodium polyphosphate into the mixture, wherein the addition amount of the sodium polyphosphate is 0.3 percent of the mass of the ore pulp, stirring for 5min to completely disperse the oil sludge, and the stirring speed is 60r/min to prevent excessive emulsification of the polymer-containing oil sludge. After the slurry is manufactured, adding hydrogen peroxide into the slurry for polymerization breaking, wherein the adding amount of the hydrogen peroxide is 0.3 percent of the mass of the slurry, stirring for polymerization breaking for 5min, and the stirring speed is 100 r/min.
(3) Conveying the oil sludge subjected to slurry making and aggregation breaking in the step (2) to a ball mill for mechanical ball milling treatment, wherein the ball mill uses ceramic balls as media, and the size and the proportion are as follows: 100mm accounts for 40%, 20mm accounts for 25%, 40mm accounts for 25%, and 80mm accounts for 10%. The treatment time is 30min, and the crude oil is stripped from the surface of the sand.
(4) As shown in fig. 2, the oil sludge scrubbed in the step (3) is conveyed to a tank body (9) by a slurry pump (7), and then is subjected to circulation separation for 5min in equipment connected with a discharge port (3), a feed tee (6), the slurry pump (7), a jet pump (10), an air inlet (5) and a feed port (2); air is filled in through the air inlet (5), the liquid phase is circulated for 5min, and scum is conveyed to a scum refining system through a scum outlet (1);
(5) and (3) after the scum is basically collected, pumping the ore pulp to a cyclone for cyclone desanding, conveying coarse sand ore pulp generated by cyclone to solid-liquid separation equipment, conveying fine ore pulp generated by cyclone to groove type flotation equipment for secondary separation, returning the scum obtained by secondary separation to the ball milling treatment equipment in the step (3), and conveying the tailings to a tailing flocculation section.
(6) Conveying the scum obtained in the step (4) and the step (5) to a scum refining tank (11) by a pump (20), adding organic solvents of hexane and water into the scum by a pump (19), wherein the mass ratio of hexane to scum to water is 1:1:1, pumping the upper layer hexane diluted crude oil to a bottom layer water phase by a pump (18), circulating the solvent for extraction for 10min, adding a polyacrylamide flocculant in an amount of 0.03 percent of the mass of the pulp, and circulating for 2min again to settle fine solid phases in the scum. After washing, the diluted crude oil on the upper layer is conveyed to a solvent recovery system from an oil outlet (13), the ore pulp on the lower layer is discharged to a solid-liquid separation system by a pump (21), the solid-liquid separation equipment is a plate-and-frame filter press or a high-pressure filter, the solid phase is discharged outside, the water is recycled after oil-water separation of the liquid phase, and the oil enters a triple-effect evaporation system to recover the solvent.
(7) And (4) conveying the diluted crude oil generated in the step (6) to a three-effect evaporator for solvent recovery, recovering hexane for solvent refining, and using heat generated by hexane steam condensation for supplementing heat loss of process water.
(8) And (3) flocculating the tailings generated in the step (5), and reusing water generated after flocculation and sedimentation in the step (2), wherein the used flocculating agent is polyacrylamide, and the adding amount of the flocculating agent is 0.002 percent of the mass of the ore pulp.
(9) And (4) dewatering the coarse sand pulp generated in the step (5) by using a drying machine, performing plate-frame filter pressing on the flocculated pulp obtained in the step (8), and recycling hot water.
Figure BDA0002383071770000101
Example 3
(1) And (4) conveying the polymer-containing oil sludge to a vibrating screen by a screw to remove impurities mechanically, and screening out large stones and other impurities which are not suitable for pumping.
(2) Mixing the polymer-containing oil sludge subjected to impurity removal with normal-temperature seawater, wherein the mass ratio of the seawater to the polymer-containing oil sludge is 1:3, then adding sodium polyphosphate into the mixture, wherein the addition amount of the sodium polyphosphate is 0.5% of the mass of the ore pulp, stirring for 5min to completely disperse the oil sludge, and the stirring speed is 40r/min to prevent excessive emulsification of the polymer-containing oil sludge. After the slurry is manufactured, adding hydrogen peroxide into the slurry for polymerization breaking, wherein the adding amount of the hydrogen peroxide is 0.5 percent of the mass of the slurry, stirring for polymerization breaking for 5min, and the stirring speed is 80 r/min.
(3) Conveying the oil sludge subjected to slurry making and aggregation breaking in the step (2) to a ball mill for mechanical ball milling treatment, wherein the ball mill uses ceramic balls as media, and the size and the proportion are as follows: 100mm accounts for 40%, 20mm accounts for 25%, 40mm accounts for 25%, and 80mm accounts for 10%. The treatment time is 30min, and the crude oil is stripped from the surface of the sand.
(4) As shown in fig. 2, the oil sludge scrubbed in the step (3) is conveyed to a tank body (9) by a slurry pump (7), and then is subjected to circulation separation for 10min in equipment connected with a discharge port (3), a feed tee (6), the slurry pump (7), a jet pump (10), an air inlet (5) and a feed port (2); air is filled in through the air inlet (5), the liquid phase is circulated for 5min, and scum is conveyed to a scum refining system through a scum outlet (1);
(5) and (3) after the scum is basically collected, pumping the ore pulp to a cyclone for cyclone desanding, conveying coarse sand ore pulp generated by cyclone to solid-liquid separation equipment, conveying fine ore pulp generated by cyclone to groove type flotation equipment for secondary separation, returning the scum obtained by secondary separation to the ball milling treatment equipment in the step (3), and conveying the tailings to a tailing flocculation section.
(6) Conveying the scum obtained in the step (4) and the step (5) to a scum refining tank (11) by a pump (20), adding organic solvents of hexane and water into the scum by a pump (19), wherein the mass ratio of hexane to scum to water is 1:1:1, pumping the upper layer hexane diluted crude oil to a bottom layer water phase by a pump (18), circulating the solvent for extraction for 10min, adding a polyacrylamide flocculant in an amount of 0.05% of the mass of the pulp, circulating for 2min again, and settling fine solid phase in the scum. After washing, the diluted crude oil on the upper layer is conveyed to a solvent recovery system from an oil outlet (13), the ore pulp on the lower layer is discharged to a solid-liquid separation system by a pump (21), the solid-liquid separation equipment is a plate-and-frame filter press or a high-pressure filter, the solid phase is discharged outside, the water is recycled after oil-water separation of the liquid phase, and the oil enters a triple-effect evaporation system to recover the solvent.
(7) And (4) conveying the diluted crude oil produced in the step (6) to a three-effect evaporator for solvent recovery, and recovering hexane for solvent refining.
(8) And (3) flocculating the tailings generated in the step (5), and recycling water generated after flocculation and sedimentation in the step (2), wherein the used flocculating agent is polyacrylamide, and the addition amount of the flocculating agent is 0.003 percent of the mass of the ore pulp.
(9) And (4) dewatering the coarse sand pulp generated in the step (5) by using a drying machine, performing plate-frame filter pressing on the flocculated pulp obtained in the step (8), and recycling the seawater.
Figure BDA0002383071770000111
Figure BDA0002383071770000121
Example 4
The embodiment relates to an oil sludge treatment system, which comprises an oil sludge pre-stripping device, an oil sludge separation device and an oil product refining device which are connected in sequence;
the oil sludge pre-stripping device is a scrubbing machine;
the oil sludge separation device comprises a tank body 1, an oil-containing scum outlet 2 is arranged at the top of the tank body, a silt output 3 is arranged at the bottom of the tank body, a feed port 4 and a discharge port 5 are arranged on the outer wall of the tank body, a circulating pipeline 6 is arranged between the feed port and the discharge port, a feed tee 7 connected with the oil sludge pre-stripping device is arranged on the circulating pipeline, and a jet pump 8 and an air inlet 9 (the schematic diagram is shown in fig. 2) are arranged on the circulating pipeline between the feed tee 7 and the feed port 4;
the oil product refining device comprises a tank body 10, an organic phase outlet 11 arranged at the top of the tank body, a fine soil tailings outlet 12 arranged at the bottom of the tank body, an organic phase agent inlet 13 arranged on the outer wall of the tank body corresponding to the horizontal position of the water phase in the tank body, a circulating pipeline connected with the organic phase inlet 13 and provided with a circulating pump 14 and a flocculating agent inlet 17, an oil-containing scum feed inlet 15 and a water and organic solvent inlet 16 arranged on the outer wall of the tank body, and a scum outlet connected with the oil sludge separation device (the schematic diagram is shown in fig. 3).
A mud-sand outlet of the oil-mud separation device is connected with a mud-sand separator, and a large-particle sand outlet of the mud-sand separator is connected with a solid-liquid separator;
a small particle material outlet of the sand-mud separator is reversely connected to a feed inlet of the oil-mud stripping device;
or the small particle material outlet of the silt separator is connected to the oil product refining device;
or a small-particle material outlet of the sand-mud separator is connected to a separator, oil-containing scum and fine mud are further separated, the oil-containing scum obtained after separation is introduced into a feed inlet of the oil-mud stripping device again, and the fine mud obtained is introduced into a flocculating machine.
Although the invention has been described in detail hereinabove by way of general description, specific embodiments and experiments, it will be apparent to those skilled in the art that many modifications and improvements can be made thereto based on the invention. Accordingly, such modifications and improvements are intended to be within the scope of the invention as claimed.

Claims (24)

1. The method for treating the polymer-containing oil sludge is characterized by comprising the steps of sequentially carrying out the treatments of slurrying and breaking polymerization, oil sludge pre-stripping, oil sludge separation and oil product refining on the polymer-containing oil sludge to be treated;
the oil sludge pre-stripping is to perform strong friction on the oil sludge after pulping and breaking aggregation by using one or more of a ball mill, a scrubbing machine or a kneading machine;
the oil sludge separation is to make the material subjected to the oil sludge pre-stripping treatment circularly flow at a high speed, so as to realize the separation of oil-containing floating slag and silt.
2. The process of claim 1, wherein the media used in the ball mill during the high power scrubbing with the ball mill are ceramic balls having the following sizes and proportions: 35-45% of 100mm, 20-30% of 20mm, 20-30% of 40mm, 5-15% of 80mm and 20-40 min of treatment time;
and/or in the process of processing by adopting a scrubbing machine, the scrubbing time is 15-25 min.
3. The treatment method according to claim 1 or 2, wherein the high-speed circulation flow is performed in two stages, the first stage performs only the high-speed circulation flow, the second stage introduces air while performing the high-speed circulation flow, and the oil-containing dross moves upward as the air is discharged upward, thereby achieving separation of the oil-containing dross from the sludge.
4. The treatment method according to claim 3, wherein the high-speed circulation flow of the materials is realized by high-speed jet flow, and/or air is introduced into the system by an air compressor.
5. The treatment method according to claim 4, wherein in the oil-sludge separation process, the speed of the high-speed material circulating flow is 1-3 m/s; the flowing time of the first stage is 10-15 min, and the flowing time of the second stage is 5-10 min.
6. The treatment method according to any one of claims 1 to 2 and 4 to 5, wherein the oil product refining comprises the following specific steps:
and mixing the oil-containing floating slag obtained after the oil sludge is separated with an organic solvent and water, after the upper organic phase is separated from the lower water phase, pumping the upper organic phase, continuously introducing the upper water phase into the lower water phase, circularly washing, and separating the upper oil phase after the washing is finished to obtain the diluted crude oil.
7. The process according to claim 6, wherein the organic solvent is one or a mixture of two or more selected from hexane, pentane, heptane, naphtha, petroleum ether, toluene and xylene.
8. The treatment method according to claim 3, wherein the oil refining comprises the following steps:
and mixing the oil-containing floating slag obtained after the oil sludge is separated with an organic solvent and water, after the upper organic phase is separated from the lower water phase, pumping the upper organic phase, continuously introducing the upper water phase into the lower water phase, circularly washing, and separating the upper oil phase after the washing is finished to obtain the diluted crude oil.
9. The process according to claim 8, wherein the organic solvent is one or a mixture of two or more selected from hexane, pentane, heptane, naphtha, petroleum ether, toluene and xylene.
10. The process according to claim 6, wherein the flocculant is added to the mixed system before the upper organic phase is separated, and the circulating washing is performed again to settle the solid particles in the organic phase.
11. The process according to any one of claims 7 to 9, wherein the flocculant is added to the mixed system before the upper organic phase is separated, and the circulating washing is performed again to settle the solid particles in the organic phase.
12. The treatment method according to any one of claims 1 to 2, 4 to 5, and 7 to 10, wherein the sludge and sand obtained after the separation of the oil sludge are separated; separating the obtained coarse mortar to obtain sand, carrying out secondary separation on the obtained fine ore pulp, carrying out oil sludge pre-stripping and oil sludge separation treatment on the oil-containing material subjected to secondary separation again to obtain oil-containing floating slag again, and carrying out oil product refining treatment again; and conveying the tailings obtained after secondary separation to a tailing flocculation section.
13. A treatment process according to claim 3, characterized in that the sand obtained after the separation of the sludge is separated; separating the obtained coarse mortar to obtain sand, carrying out secondary separation on the obtained fine ore pulp, carrying out oil sludge pre-stripping and oil sludge separation treatment on the oil-containing material subjected to secondary separation again to obtain oil-containing floating slag again, and carrying out oil product refining treatment again; and conveying the tailings obtained after secondary separation to a tailing flocculation section.
14. The treatment method according to claim 6, characterized in that the sand obtained after the separation of the oil sludge is separated; separating the obtained coarse mortar to obtain sand, carrying out secondary separation on the obtained fine ore pulp, carrying out oil sludge pre-stripping and oil sludge separation treatment on the oil-containing material subjected to secondary separation again to obtain oil-containing floating slag again, and carrying out oil product refining treatment again; and conveying the tailings obtained after secondary separation to a tailing flocculation section.
15. The process according to claim 11, wherein the sand is separated from the oil-containing sludge; separating the obtained coarse mortar to obtain sand, carrying out secondary separation on the obtained fine ore pulp, carrying out oil sludge pre-stripping and oil sludge separation treatment on the oil-containing material subjected to secondary separation again to obtain oil-containing floating slag again, and carrying out oil product refining treatment again; and conveying the tailings obtained after secondary separation to a tailing flocculation section.
16. The treatment method according to any one of claims 1 to 2, 4 to 5, 7 to 10 and 13 to 15, wherein the specific operation of pulping and breaking polymerization is to mix the polymer-containing oil sludge to be treated with water or brine with a total salt content of 1 to 8% and then add one or two of a dispersant and a breaker to carry out pulping and breaking polymerization;
and/or the dispersant is Na2SiO3,Na2CO3One or more of NaOH, sodium polyphosphate or washing powder; the addition amount of the dispersing agent is 0-3% of the mass of the mixed system;
and/or the polymerization breaking agent is one or more of a Fenton reagent, hydrogen peroxide, persulfate or hypochlorite; the addition amount of the aggregation breaking agent is 0-3% of the mass of the mixed system;
and/or adding the dispersing agent and then adding the polymerization breaking agent for treatment.
17. The treatment method according to claim 16, wherein the mass ratio of the polymer-containing oil sludge to be treated to water or saline water with total salt content of 1-8% is 1:1 to 1.5; in the process of mixing the polymer-containing oil sludge to be treated with water, the temperature of a mixing system is controlled to be 50-90 ℃, and in the process of mixing the polymer-containing oil sludge to be treated with water with the total salt content of 1-8%, the temperature of the mixing system is controlled to be 25-30 ℃.
18. The treatment method according to claim 3, wherein the specific operation of slurrying and breaking is to mix the polymer-containing oil sludge to be treated with water or brine with the total salt content of 1-8%, and then add one or two of a dispersant or a breaker to carry out slurrying and breaking;
and/or, the divisionThe powder is Na2SiO3,Na2CO3One or more of NaOH, sodium polyphosphate or washing powder; the addition amount of the dispersing agent is 0-3% of the mass of the mixed system;
and/or the polymerization breaking agent is one or more of a Fenton reagent, hydrogen peroxide, persulfate or hypochlorite; the addition amount of the aggregation breaking agent is 0-3% of the mass of the mixed system;
and/or adding the dispersing agent and then adding the polymerization breaking agent for treatment.
19. The treatment method according to claim 6, wherein the specific operation of slurrying and breaking is to mix the polymer-containing oil sludge to be treated with water or brine with the total salt content of 1-8%, and then add one or two of a dispersant or a breaker to carry out slurrying and breaking;
and/or the dispersant is Na2SiO3,Na2CO3One or more of NaOH, sodium polyphosphate or washing powder; the addition amount of the dispersing agent is 0-3% of the mass of the mixed system;
and/or the polymerization breaking agent is one or more of a Fenton reagent, hydrogen peroxide, persulfate or hypochlorite; the addition amount of the aggregation breaking agent is 0-3% of the mass of the mixed system;
and/or adding the dispersing agent and then adding the polymerization breaking agent for treatment.
20. The treatment method according to claim 11, wherein the specific operation of slurrying and breaking is to mix the polymer-containing oil sludge to be treated with water or brine with a total salt content of 1-8%, and then add one or both of a dispersant and a breaker to carry out slurrying and breaking;
and/or the dispersant is Na2SiO3,Na2CO3One or more of NaOH, sodium polyphosphate or washing powder; the addition amount of the dispersing agent is 0-3% of the mass of the mixed system;
and/or the polymerization breaking agent is one or more of a Fenton reagent, hydrogen peroxide, persulfate or hypochlorite; the addition amount of the aggregation breaking agent is 0-3% of the mass of the mixed system;
and/or adding the dispersing agent and then adding the polymerization breaking agent for treatment.
21. The treatment method according to claim 12, wherein the specific operation of slurrying and breaking is to mix the polymer-containing oil sludge to be treated with water or brine with a total salt content of 1-8%, and then add one or both of a dispersant and a breaker to carry out slurrying and breaking;
and/or the dispersant is Na2SiO3,Na2CO3One or more of NaOH, sodium polyphosphate or washing powder; the addition amount of the dispersing agent is 0-3% of the mass of the mixed system;
and/or the polymerization breaking agent is one or more of a Fenton reagent, hydrogen peroxide, persulfate or hypochlorite; the addition amount of the aggregation breaking agent is 0-3% of the mass of the mixed system;
and/or adding the dispersing agent and then adding the polymerization breaking agent for treatment.
22. The treatment method according to any one of claims 18 to 21, wherein the mass ratio of the polymer-containing oil sludge to be treated to water or saline water with total salt content of 1 to 8% is 1:1 to 1.5; in the process of mixing the polymer-containing oil sludge to be treated with water, the temperature of a mixing system is controlled to be 50-90 ℃, and in the process of mixing the polymer-containing oil sludge to be treated with water with the total salt content of 1-8%, the temperature of the mixing system is controlled to be 25-30 ℃.
23. A treatment system containing polymer sludge is characterized by comprising a sludge pre-stripping device, a sludge separation device and an oil product refining device which are sequentially connected;
the oil sludge pre-stripping device is one or more of a ball mill, a scrubbing machine or a kneading machine;
the oil sludge separation device comprises a tank body, an oil-containing scum outlet is formed in the top of the tank body, a silt product is formed in the bottom of the tank body, a feed port and a discharge port are formed in the outer wall of the tank body, a circulating pipeline is arranged between the feed port and the discharge port, a feed tee joint connected with the oil sludge pre-stripping device is arranged on the circulating pipeline, and a jet pump and an air inlet are arranged on the circulating pipeline between the feed tee joint and the feed port;
the oil refining device comprises a tank body, an organic phase outlet arranged at the top of the tank body and a fine soil tailing outlet arranged at the bottom of the tank body, wherein the outer wall of the tank body is provided with an organic phase agent inlet corresponding to the horizontal position of the water phase in the tank body, the organic phase outlet is connected with the organic phase inlet through a circulating pipeline, the circulating pipeline is provided with a circulating pump and a flocculating agent inlet, the outer wall of the tank body is provided with an oil-containing scum feed inlet and a water and organic solvent inlet, and the feed inlet is connected with a scum outlet of the oil sludge separation device.
24. The treatment system of claim 23, wherein the silt outlet of the sludge separation unit is connected to a silt separator, and the large particle sand outlet of the silt separator is connected to the solid-liquid separator;
a small particle material outlet of the sand-mud separator is reversely connected to a feed inlet of the oil sludge pre-stripping device;
or the small particle material outlet of the silt separator is connected to the feeding hole of the oil product refining device;
or a small-particle material outlet of the sand-mud separator is connected to a separator, oil-containing scum and tailings are further separated, the oil-containing scum obtained after separation is introduced into a feed inlet of the oil-mud pre-stripping device again, and the obtained tailings are introduced into a flocculating agent.
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