CN106315934A - Experiment device for treatment of fracturing flow-back fluid - Google Patents

Experiment device for treatment of fracturing flow-back fluid Download PDF

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Publication number
CN106315934A
CN106315934A CN201610767496.4A CN201610767496A CN106315934A CN 106315934 A CN106315934 A CN 106315934A CN 201610767496 A CN201610767496 A CN 201610767496A CN 106315934 A CN106315934 A CN 106315934A
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China
Prior art keywords
room
oxidation
chemical
flocculation
glue
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CN201610767496.4A
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Chinese (zh)
Inventor
胡琼
许剑
张正禄
李文权
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Sinopec Oilfield Equipment Corp
Research Institute of Sinopec Oilfield Equipment Co Ltd
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Research Institute of Sinopec Petroleum Engineering Machinery Co Ltd
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Priority to CN201610767496.4A priority Critical patent/CN106315934A/en
Publication of CN106315934A publication Critical patent/CN106315934A/en
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    • CCHEMISTRY; METALLURGY
    • C02TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02FTREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F9/00Multistage treatment of water, waste water or sewage
    • CCHEMISTRY; METALLURGY
    • C02TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02FTREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F1/00Treatment of water, waste water, or sewage
    • C02F1/46Treatment of water, waste water, or sewage by electrochemical methods
    • C02F1/461Treatment of water, waste water, or sewage by electrochemical methods by electrolysis
    • C02F1/463Treatment of water, waste water, or sewage by electrochemical methods by electrolysis by electrocoagulation
    • CCHEMISTRY; METALLURGY
    • C02TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02FTREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F1/00Treatment of water, waste water, or sewage
    • C02F1/46Treatment of water, waste water, or sewage by electrochemical methods
    • C02F1/461Treatment of water, waste water, or sewage by electrochemical methods by electrolysis
    • C02F1/467Treatment of water, waste water, or sewage by electrochemical methods by electrolysis by electrochemical disinfection; by electrooxydation or by electroreduction
    • C02F1/4672Treatment of water, waste water, or sewage by electrochemical methods by electrolysis by electrochemical disinfection; by electrooxydation or by electroreduction by electrooxydation
    • CCHEMISTRY; METALLURGY
    • C02TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02FTREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F1/00Treatment of water, waste water, or sewage
    • C02F1/52Treatment of water, waste water, or sewage by flocculation or precipitation of suspended impurities
    • C02F1/5236Treatment of water, waste water, or sewage by flocculation or precipitation of suspended impurities using inorganic agents
    • C02F1/5245Treatment of water, waste water, or sewage by flocculation or precipitation of suspended impurities using inorganic agents using basic salts, e.g. of aluminium and iron
    • CCHEMISTRY; METALLURGY
    • C02TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02FTREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F1/00Treatment of water, waste water, or sewage
    • C02F1/52Treatment of water, waste water, or sewage by flocculation or precipitation of suspended impurities
    • C02F1/54Treatment of water, waste water, or sewage by flocculation or precipitation of suspended impurities using organic material
    • C02F1/56Macromolecular compounds
    • CCHEMISTRY; METALLURGY
    • C02TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02FTREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F1/00Treatment of water, waste water, or sewage
    • C02F1/72Treatment of water, waste water, or sewage by oxidation
    • CCHEMISTRY; METALLURGY
    • C02TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02FTREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F1/00Treatment of water, waste water, or sewage
    • C02F1/72Treatment of water, waste water, or sewage by oxidation
    • C02F1/78Treatment of water, waste water, or sewage by oxidation with ozone

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  • Life Sciences & Earth Sciences (AREA)
  • Hydrology & Water Resources (AREA)
  • Engineering & Computer Science (AREA)
  • Environmental & Geological Engineering (AREA)
  • Water Supply & Treatment (AREA)
  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Water Treatment By Electricity Or Magnetism (AREA)
  • Treatment Of Water By Oxidation Or Reduction (AREA)

Abstract

The invention discloses an experiment device for treatment of a fracturing flow-back fluid. The device comprises a chemical oxidation gel breaking chamber, an ozone oxidation gel breaking chamber, a chemical flocculation pipe mixer, an electric flocculation reactor, a chemical oxidation chamber, an electrochemical oxidation chamber and a filter, wherein the chemical oxidation gel breaking chamber and the ozone oxidation gel breaking chamber are arranged in parallel, and outlets of the two gel breaking chambers are connected with an inlet of the chemical flocculation pipe mixer; the chemical flocculation pipe mixer, the electric flocculation reactor, the chemical oxidation chamber and the electrochemical oxidation chamber are connected in series sequentially, an outlet of the electric flocculation reactor and an outlet of the electrochemical oxidation chamber are both connected with an inlet of a filtering pipe, and an outlet of the filtering pipe is connected with a clean water tank. The experiment device can realize the continuous treatment process including oxidation, gel breaking, flocculation, deep oxidation, filtering and the like of the fracturing flow-back fluid, and can realize different treatment processes through valve switching; the experiment device is easy to operate and applicable to treatment experiments on different systems of the fracturing flow-back fluids such as guanidine gum fracturing flow-back fluids, slick water fracturing flow-back fluids and the like, and the practicality is high.

Description

A kind of fracturing outlet liquid processes experimental provision
Technical field
The present invention relates to relate to the unconventionaloil pool field development processes such as oil field, natural gas, coal bed gas are returned after pressing crack construction Discharge opeing processing technology field, particularly relates to a kind of fracturing outlet liquid and processes assay device.
Background technology
China, since actively developing petroleum resources strategic investigation and exploration and development, have ignored exploitation in a very long time The problems such as middle water resource challenge, environmental pollution and the placement measure that may bring.Wherein, pressure break is as new well gas testing, old liberated area oil One of measure that gas well is taped the latent power and individual well volume increase is conventional, can produce and produce waste liquid in a large number, including front activated water clean-out service of constructing The well-flushing waste water that produces, constructed after return the pressure break breaking glue solution ejected and formation fluid and the pressure break of constructed residual from pit shaft Base fluid.Along with carrying out on a large scale of fracturing technique, necessarily face the process problem of fracturing outlet liquid.
After wherein guanidine glue laminated splits the end of job, the fracturing fluid of the row of returning both contained a large amount of guanidine glue, formaldehyde, petroleum-type and various Additive, clay particle that depths, stratum is taken out of and landwaste so that fracturing outlet liquid have high COD, high stability, high viscosity and The features such as high concentrtion, particularly some of them are difficult to the hydrophilic organic additive purified, it is difficult to remove from waste water.Slippery water The slippery water formula that pressing crack construction uses is simple, have excellent fall resistance, reduce discharging, steady viscosity energy, but after ground is returned out due to Receiving formation rock absorption and reservoir pollution, composition also becomes complex, and it is big to return lifting rate.
The most on-the-spot many employing down-stream ponds or big tank storage, rely on sewage self to volatilize for a long time or heavy Fall, exist time-consuming long, efficiency is low, infiltration or the problem such as excessive risk is high;Or consolidated delivery focus on to somewhere, time-consuming take Power and cost are high.Therefore, fracturing outlet liquid is carried out treatment in situ and is used for recycling or arranges outward, be that oil field development produces urgently Need research and the technology solved.
Treatment technology for fracturing outlet liquid is concentrated mainly on pretreatment, flocculation, advanced oxidation, separates, inhales in recent years The combination of the different order of the different disposal methods such as attached, light electrolysis, and the fracturing outlet liquid for different systems need to use difference Processing means complete long run test.In view of fracturing outlet liquid water quality characteristic is changeable, laboratory testing rig require numerous, do not exist together The features such as seriality is the strongest between reason method, it is necessary to develop effective integrated fracturing outlet liquid and process assay device, evaluate not The science and engineering that the exists together skill treatment effect to fracturing outlet liquid, the development to fracturing outlet liquid processing means has important guidance work With.
Summary of the invention
The technical problem to be solved is the not enough offer one operation letter existed for above-mentioned prior art Single, experimental provision can be processed for the fracturing outlet liquid that different types of fracturing outlet liquid carries out processing.
The technical solution adopted in the present invention is: a kind of fracturing outlet liquid processes experimental provision, it is characterised in that: including Glue room, chemical flocculation pipe-line mixer, electricity flocculation reactor, chemical oxidation room, electrochemistry are broken in the broken glue room of oxidation, ozone oxidation Oxidizing chamber, filter, described chemical oxidation breaks glue room and ozone oxidation is broken glue room and is set up in parallel, and both entrances are all and cesspool Being connected, both outlet all entrances with chemical flocculation pipe-line mixer are connected, the outlet of described chemical flocculation pipe-line mixer Being connected with the entrance of electricity flocculation reaction room, the electricity outlet of flocculation reaction room is connected with the entrance of chemical oxidation room, described chemical oxygen The outlet changing room is connected with the entrance of electrochemical oxidation room, the outlet of described electricity flocculation reaction room and the outlet of electrochemical oxidation room All being connected with the entrance of filter pipe, the outlet of filter pipe is connected with clear water reserviors, on chemical flocculation pipe-line mixer respectively Connect have flocculant tank and flocculation aid tank, break glue room at chemical oxidation, ozone oxidation breaks glue room, electricity flocculation reaction room, chemical oxygen Change room, the entrance and exit of electrochemical oxidation room is respectively equipped with valve, realizes different process technique by valve transfer.
By technique scheme, the entrance and exit end in described electricity flocculation reaction room has been arranged in parallel a pipeline, at pipe Road is provided with valve, passes through control valve, it is achieved chemical flocculation pipe-line mixer and the series connection of electricity flocculation reaction room and parallel connection.
By technique scheme, breaking glue room at chemical oxidation and break glue tank with chemistry and be connected, the outlet of the broken glue tank of chemistry is provided with Effusion meter, breaks glue indoor at chemical oxidation and is provided with the first agitator, is chemical oxidation gel breaker solution in the broken glue tank of chemistry, chemistry Oxidation gel breaker solution is the one in the complex of Ammonium persulfate., potassium peroxydisulfate, peroxide and oxychlorination compound.
By technique scheme, described ozone oxidation is broken the bottom of glue room and is connected with ozonator, ozonator Top is provided with micro porous aeration head, is provided with manganese sand catalyst filling floor, breaks glue room in ozone oxidation in ozone oxidation breaks glue room Top connects ozone tail gas abatement device.
By technique scheme, flocculant tank is inorganic polymer flocculant solution, inorganic polymer flocculant solution For at least one in aluminium polychlorid, polyaluminium sulfate, bodied ferric sulfate, poly-ferric chloride and bodied ferric sulfate;Flocculation aid It tank is flocculation aid polyacrylamide solution;The outlet of flocculant tank and flocculation aid tank is equipped with effusion meter.
By technique scheme, it is carved with in electricity flocculation reaction room and is easy to sulculus that is fixing and that change electrode, described electrode Use aluminum electrode or iron electrode.
By technique scheme, it is provided with pipeline coarse filter in the porch of chemical oxidation room.
By technique scheme, described chemical oxidation room is connected with chemical oxidizing agent tank, the chemical oxygen in chemical oxidation room Being chemical oxidation agent solution in agent tank, chemical oxidation agent solution is Fenton reagent or liquor natrii hypochloritis, chemical oxidizing agent tank Outlet connect have effusion meter.
By technique scheme, the anode of described electrochemical oxidation room use Lead oxide brown, titanium dioxide, platinumiridio and One in boron-doped diamond, negative electrode uses the one in lead, titanium and graphite.
By technique scheme, break glue room at chemical oxidation, ozone oxidation breaks glue room, chemical flocculation pipe-line mixer, electricity Flocculation reaction room, chemical oxidation room, the outlet of electrochemical oxidation room are equipped with sample tap, at cesspool, electricity flocculation reaction room, electricity The outlet of chemical oxidation room is equipped with delivery pump.
Have the beneficial effect that this assay device can realize the oxidation of fracturing outlet liquid and break glue, flocculation, deep acquired by the present invention The continuous processing processes such as degree oxidation and filtration, and different process technique can be realized by valve transfer;Assay device operation letter Single, be applicable to the process test of the different system fracturing outlet liquids such as guanidine glue fracturing outlet liquid, slippery water fracturing outlet liquid, obtain Test processing parameter has important directive function for the development of on-the-spot fracturing outlet liquid device.
Accompanying drawing explanation
Fig. 1 is the structure chart of the present invention.
Detailed description of the invention
The invention will be further described below in conjunction with the accompanying drawings.
As it can be seen, present embodiments provide a kind of fracturing outlet liquid to process experimental provision, including cesspool, chemical oxidation Glue room 5, chemical flocculation pipe-line mixer 7, electricity flocculation reactor 8, chemical oxidation room 10, electrochemistry are broken in broken glue room 2, ozone oxidation Oxidizing chamber 11, filter 12, described chemical oxidation breaks glue room 2 and ozone oxidation is broken glue room 5 and is set up in parallel, and both entrances are the most logical Piping is connected with cesspool, is respectively equipped with valve valve A2, A1 on the pipeline of both entrances, and both outlets are led to respectively Piping is connected with the entrance of chemical flocculation pipe-line mixer 7, is respectively equipped with valve B1, B2 on the pipeline of both outlets; The outlet of described chemical flocculation pipe-line mixer 7 is connected by the entrance of pipeline with electricity flocculation reaction room 8, electricity flocculation reaction room 8 Outlet be connected by the entrance of pipeline with chemical oxidation room 10;Entrance and exit in electricity flocculation reaction room 8 is equipped with valve D1, D3, the entrance and exit end in described electricity flocculation reaction room 8 has been arranged in parallel a pipeline, has been provided with valve D2 on pipeline, logical Overregulate valve D2, it is achieved chemical flocculation pipe-line mixer and the series connection of electricity flocculation reaction room and parallel connection.Described chemical oxidation room The outlet of 10 is connected by the entrance of pipeline with electrochemical oxidation room 11, is provided with pipeline coarse filter 9, at chemistry on this pipeline Valve E1 and E4, the outlet of described electricity flocculation reaction room 8 and electricity it is respectively equipped with on the inlet duct of oxidizing chamber 10 and outlet conduit The outlet of chemical oxidation room 11 is connected with the entrance of filter pipe 12 by pipeline respectively, is respectively equipped with on these two pipelines Valve E2, E3, the outlet of filter pipe 12 is connected with clear water reserviors by pipeline, is provided with valve F2 on this pipeline.In chemical oxygen Glue room 5, chemical flocculation pipe-line mixer 7, electricity flocculation reaction room 8, chemical oxidation room 10, electrification are broken in the broken glue room 2 of change, ozone oxidation The outlet learning oxidizing chamber 11 is equipped with sample tap, in cesspool, electricity flocculation reaction room 8, the outlet difference of electrochemical oxidation room 11 It is provided with delivery pump 1-1,1-2,1-3.
Described chemical oxidation breaks glue room 2 and breaks glue tank 6-1 with chemistry and be connected, and breaks glue for chemical oxidation in the broken glue tank 6-1 of chemistry Agent solution, chemical oxidation gel breaker solution is in the complex of Ammonium persulfate., potassium peroxydisulfate, peroxide and oxychlorination compound Kind.The outlet of the broken glue tank 6-1 of chemistry is provided with effusion meter, is provided with the first agitator 3-1 in chemical oxidation breaks glue room 2, for real The accurate interpolation of existing chemical oxidation gel breaker, and guarantee that chemical oxidation gel breaker fully reacts with fracturing outlet liquid.
Being provided with manganese sand catalyst filling floor in ozone oxidation breaks glue room, its particle diameter is 10-12mm, and ozone can be excited to generate Hydroxyl radical free radical, forms the effect of O3 catalytic oxidation, improves ozone decomposed efficiency, sewage also can be made to mix all with ozone simultaneously Even, it is ensured that the response time;Described ozone oxidation is broken the bottom of glue room 5 and is connected with ozonator 4, the top of ozonator 4 Being provided with micro porous aeration head, ozone enters to return in discharge opeing after micro porous aeration head dispersion bubble and sends out with returning after pollutant contact in discharge opeing Raw ozone oxidation reaction, reacted tail gas enters in air after ozone tail gas digestion device 14.
Chemical flocculation pipe-line mixer 7 is connected to flocculant tank 6-2 and flocculation aid tank 6-3, flocculant tank and The outlet of flocculation aid tank is equipped with valve and effusion meter, for realizing the accurate interpolation of flocculant and flocculation aid, and completes chemistry Flocculation process.Being inorganic polymer flocculant solution in flocculant tank 6-2, inorganic polymer flocculant solution is polyaluminium At least one in aluminum, polyaluminium sulfate, bodied ferric sulfate, poly-ferric chloride and bodied ferric sulfate;For helping in flocculation aid tank 6-3 Solidifying agent polyacrylamide solution, wherein, chemical flocculation process uses tubular reactor, when can effectively shorten the stop for the treatment of fluid Between, increase the contact area for the treatment of fluid and flocculant, improve flocculating effect.
Electricity flocculation reaction room is carved with and is easy to sulculus that is fixing and that change electrode, it is possible to adjust polar plate spacing, described Electrode uses aluminum electrode or iron electrode, in order to generated the precipitate of the hydroxide of ferrum or aluminum by electrode reaction.
Described chemical oxidation room 10 is connected with chemical oxidizing agent tank 6-4, is provided with the second agitator in chemical oxidation room 10 3-2, is chemical oxidation agent solution in chemical oxidizing agent tank 6-4, and chemical oxidation agent solution is Fenton reagent or liquor natrii hypochloritis, The outlet of chemical oxidizing agent tank connects effusion meter.
The anode of described electrochemical oxidation room 11 uses in Lead oxide brown, titanium dioxide, platinumiridio and boron-doped diamond One, negative electrode uses the one in lead, titanium and graphite.According to the water quality characteristic of water outlet after flocculation, be provided with chemical oxidation and Electrochemical oxidation two-stage, realizes two-stage oxidation by control valve and processes or individual event oxidation processes, it is ensured that effectively reduce water outlet COD value.
Described filter pipe 12 is double-filtration pipeline 12-1, and 12-2 is connected in series, and is provided with on the pipeline both connecting Valve F1, the filter medium wherein filled and medium size depend on the performance for the treatment of fluid, optional magnetic iron ore, activated carbon, manganese Sand filtering material and nanofiltration material etc..
Described pipeline coarse filter 9, is more than the granule of 20 μm for filtering diameter in solid suspension thing.
Above-mentioned assay device can realize the oxidation of fracturing outlet liquid and break the continuous processings such as glue, flocculation, deep oxidation and filtration Process, and can realize the closedown by valve of the different process technique by valve transfer, such as, can realize following locating science and engineering Skill: 1, can carry out chemical oxidation and break glue or ozone oxidation breaks glue, chemical flocculation is or/and electricity flocculation, chemical oxidation and electrochemistry The steps such as oxidation;2, ozone oxidation can be carried out and break glue, electricity flocculation, chemical oxidation and electrochemical oxidation etc.;3, can also carry out Electricity flocculation, chemical oxidation are or/and steps such as electrochemical oxidations;
Illustrate with instantiation below:
Embodiment 1:
The present embodiment is the hydroxypropyl guar system fracturing outlet liquid produced for oil well production increasing operation, it is achieved arrange outward.Hydroxyl Propyl guanidine colloid system fracturing outlet liquid influent quality: PH=7.5, in water float be 893mg/L, COD be 3700mg/L, at it Reason method is:
1), open valve A1, start delivery pump 1-1, take guanidine glue fracturing outlet liquid in cesspool and break glue room to ozone oxidation In, open ozonator and valve C simultaneously, guanidine glue fracturing outlet liquid reacts with ozone, and ozone concentration is ozone concentration For 50-80mg/L, it is 5-10min that ozone breaks the glue response time.Preferably, ozone concentration is 50mg/L, and ozone breaks the glue response time For 5min, generate HO (hydroxyl radical free radical) by reaction, reach brokenly glue effect.Valve closing C is closed also after returning discharge opeing viscosity and declining Open valve B2 and D1;
2) discharge opeing of returning after, processing flow to (this step in electricity flocculation reaction room 8 after chemical flocculation pipe-line mixer 7 Carry out electricity flocculation step), start power supply, regulate voltage and current size, regulate polar plate spacing if desired and change pole plate;Electricity wadding The solidifying electricity flocculation reaction time be 2min-4min, preferably response time be 2min.By forming aluminum or the hydroxide of ferrum, i.e. " micro- Floccule body " realize returning particle and colloid pollution thing unstability and floccule body in discharge opeing;
3), after floccule body is formed, open valve D3, delivery pump 1-2 and valve E1, electricity flocculation reaction room returns discharge opeing Entering chemical oxidation room after flowing through pipeline coarse filter, and inwardly add liquor natrii hypochloritis, addition is 2000-3000mg/ L, preferably addition are 2000mg/L, start agitator 2,
4), treat that chemical oxidation reaction 20-30min, preferably chemical oxidation reaction time are 20min;After open valve E4, to change Learning the discharge opeing of returning after oxidation and carry out electroxidation process, regulate voltage and current size, current range is 5-10A, preferably current value For 10A, the electrochemistry deep oxidation response time is 10-20min, preferably 15min.
5), open valve E3, F1 and F2, start delivery pump 1-3, the discharge opeing of returning in electrochemical oxidation room is delivered to two-stage Filtering in filter pipe, finally flow into clear water reserviors, water quality reaches national grade one discharge standard.
In treatment method, fracturing outlet liquid carries out first ozone oxidation and completes brokenly glue pretreatment, reduces fluid inlet end and glues Spend, and the intervention again of chemical solubility interfering ion in discharge opeing is returned in alleviation, reduces secondary pollution risk;And by using electricity wadding Solidifying and electrochemical oxidation substituted chemistry flocculates and chemical oxidation, is aided with air-dissolving air-float and filtration, effectively reduces new chemical agent Introduce and consumption, alleviate the intervention again of chemical solubility interfering ion in waste water, contribute to reducing secondary pollution risk and dropping Discharge opeing of returning after low cost, and process is capable of recycling preparing fracturing fluid or reinjection into reservoir;
Effluent quality measurement result after treated by the present method:
Embodiment 2:
The present embodiment is for processing the slippery water system fracturing outlet liquid processed without the broken glue of oxidation, it is achieved arrange outward.Its Operating procedure is:
1), open valve A2 and valve B1, start delivery pump 1-1, take slippery water fracturing outlet liquid, flowing through in cesspool It is directly entered in chemical flocculation pipe-line mixer 7 after learning the broken glue room of oxidation (this step is made without chemical oxidation and breaks glue reaction) Carrying out chemical flocculation, and add flocculant poly aluminum chloride and flocculation aid polyacrylamide, flocculant dosage is 1000- 2000mg/L, flocculation aid dosage be 10-20mg/L, preferably flocculant dosage be 1500mg/L, flocculation aid dosage is 15mg/L;
2), opening valve D1, the discharge opeing of returning after chemical flocculation enters in electricity flocculation reaction room, starts power supply, regulates voltage And size of current, regulate polar plate spacing if desired and change pole plate, the electricity flocculation reaction time is 3min;
3), after floccule body is formed, open valve D3, delivery pump 1-2 and valve E1, electricity flocculation reaction room returns discharge opeing Entering chemical oxidation room after flowing through pipeline coarse filter, and inwardly add liquor natrii hypochloritis, addition is 1000-2000mg/ L, preferably addition are 1000mg/L, start agitator 2;
4), treat that chemical oxidation reaction 20-30min, preferably chemical oxidation reaction time are 30min, after chemical oxidation Return discharge opeing and carry out electroxidation process, regulate voltage and current size, current range be 5-10A, preferably current value be 5A, electrochemistry The deep oxidation response time is 10-20min, preferably 10min.
5), open valve E3, F1 and F2, start delivery pump 1-3, the discharge opeing of returning in electrochemical oxidation room 11 is delivered to two Filtering in level filter pipe, finally flow into clear water reserviors, water quality reaches national grade one discharge standard.
Effluent quality measurement result after treated by the present method:
Embodiment 3:
The present embodiment is for processing the slippery water system fracturing outlet liquid processed without the broken glue of oxidation, it is achieved repeat profit With.Its operating procedure is:
1), open valve A2, valve B1 and valve D1, start delivery pump 1, take slippery water fracturing outlet liquid in cesspool, Flow through chemical oxidation break glue room and chemical flocculation pipe-line mixer after (this step be made without chemical oxidation break glue reaction and change Learn flocculation reaction) it is directly entered in electricity flocculation reaction room, start power supply, regulate voltage and current size, regulate pole plate if desired Spacing also changes pole plate.Particle therein, colloid pollution thing etc. lose stable under electric field action and tie with tiny flocculation agent Closing and form big flocculating body, the electricity flocculation reaction time is 4min;
2), after floccule body is formed, valve D3, delivery pump 1-2, valve E1 and E4 are opened, the row of returning after electricity flocculation treatment Liquid stream enters electrochemical oxidation room through pipeline coarse filter and chemical oxidation room and carries out electroxidation process, and regulation voltage and current is big Little, current range be 5-10A, preferably current value be 8A, the electrochemistry deep oxidation response time is 10-20min, preferably 20min.
3), open valve E3 and F2, start delivery pump 1-3, the discharge opeing of returning in electrochemical oxidation room is delivered to two-stage mistake Filtering in chimney filter road, finally flow into clear water reserviors, water quality reaches recycling standard.
Effluent quality measurement result after treated by the present method:
Experimentation pH Float (mg/L) Petroleum-type (mg/L) CODCr(mg/L)
Before process 6.9 1000 30.7 2702.3
After process 6.7 18.5 3.2 925
Recycling standard 6-9 25 5 1000

Claims (10)

1. a fracturing outlet liquid processes experimental provision, it is characterised in that: include that chemical oxidation breaks glue room, ozone oxidation breaks glue Room, chemical flocculation pipe-line mixer, electricity flocculation reactor, chemical oxidation room, electrochemical oxidation room, filter, described chemical oxygen Changing broken glue room and ozone oxidation is broken glue room and is set up in parallel, both entrances are all connected with cesspool, and both outlets are all with chemical The entrance of flocculation pipe-line mixer is connected, the outlet of described chemical flocculation pipe-line mixer and the entrance phase of electricity flocculation reaction room Even, the electricity outlet of flocculation reaction room is connected with the entrance of chemical oxidation room, the outlet of described chemical oxidation room and electrochemical oxidation The entrance of room is connected, the outlet of the outlet of flocculation reaction room of described electricity and electrochemical oxidation room all with the entrance phase of filter pipe Even, the outlet of filter pipe is connected with clear water reserviors, is connected to flocculant tank and helps solidifying on chemical flocculation pipe-line mixer Agent tank, break glue room at chemical oxidation, ozone oxidation breaks glue room, electricity flocculation reaction room, chemical oxidation room, the entering of electrochemical oxidation room Mouth and outlet are respectively equipped with valve.
A kind of fracturing outlet liquid the most according to claim 1 processes experimental provision, it is characterised in that: anti-in described electricity flocculation The entrance and exit end answering room has been arranged in parallel a pipeline, is provided with valve, passes through control valve, it is achieved chemical flocculation on pipeline Pipe-line mixer and the electricity series connection of flocculation reaction room and parallel connection.
Fracturing outlet liquid the most according to claim 1 and 2 processes experimental provision, it is characterised in that: break glue at chemical oxidation Room is broken glue tank and is connected with chemistry, and the outlet of the broken glue tank of chemistry is provided with effusion meter, breaks glue indoor at chemical oxidation and is provided with the first stirring Device, is chemical oxidation gel breaker solution in the broken glue tank of chemistry, and chemical oxidation gel breaker solution is Ammonium persulfate., potassium peroxydisulfate, mistake One in the complex of oxygen and oxychlorination compound.
Fracturing outlet liquid the most according to claim 1 and 2 processes experimental provision, it is characterised in that: described ozone oxidation is broken The bottom of glue room is connected with ozonator, and the top of ozonator is provided with micro porous aeration head, in ozone oxidation breaks glue room Being provided with manganese sand catalyst filling layer, the top connection breaking glue room in ozone oxidation has ozone tail gas abatement device.
Fracturing outlet liquid the most according to claim 1 and 2 processes experimental provision, it is characterised in that: flocculant tank is nothing Machine flocculating polymer agent solution, inorganic polymer flocculant solution is aluminium polychlorid, polyaluminium sulfate, bodied ferric sulfate, gathers Close at least one in iron chloride and bodied ferric sulfate;It flocculation aid tank is flocculation aid polyacrylamide solution;Flocculant tank and The outlet of flocculation aid tank is equipped with effusion meter.
Fracturing outlet liquid the most according to claim 1 and 2 processes experimental provision, it is characterised in that: in electricity flocculation reaction room In be carved with and be easy to sulculus that is fixing and that change electrode, described electrode uses aluminum electrode or iron electrode.
Fracturing outlet liquid the most according to claim 1 and 2 processes experimental provision, it is characterised in that: in chemical oxidation room Porch is provided with pipeline coarse filter.
Fracturing outlet liquid the most according to claim 1 and 2 processes experimental provision, it is characterised in that: described chemical oxidation room Being connected with chemical oxidizing agent tank, be chemical oxidation agent solution in the chemical oxidizing agent tank in chemical oxidation room, chemical oxidizing agent is molten Liquid is Fenton reagent or liquor natrii hypochloritis, and the outlet of chemical oxidizing agent tank connects effusion meter.
Fracturing outlet liquid the most according to claim 1 and 2 processes experimental provision, it is characterised in that: described electrochemical oxidation The anode of room uses the one in Lead oxide brown, titanium dioxide, platinumiridio and boron-doped diamond, and negative electrode uses lead, titanium and stone One in ink.
Fracturing outlet liquid the most according to claim 1 and 2 processes experimental provision, it is characterised in that: break glue at chemical oxidation Glue room, chemical flocculation pipe-line mixer, electricity flocculation reaction room, chemical oxidation room, the going out of electrochemical oxidation room are broken in room, ozone oxidation Mouth is equipped with sample tap, is equipped with delivery pump in cesspool, electricity flocculation reaction room, the outlet of electrochemical oxidation room.
CN201610767496.4A 2016-08-30 2016-08-30 Experiment device for treatment of fracturing flow-back fluid Pending CN106315934A (en)

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CN107673462A (en) * 2017-10-23 2018-02-09 成都恩承科技股份有限公司 The method that glue is broken to fracturing outlet liquid based on γ FeOOH catalysis ozone advanced oxidation systems
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CN111908567A (en) * 2019-05-08 2020-11-10 中国石油天然气集团有限公司 Volume fracturing waste liquid electric flocculation destabilization separation treatment device and method
CN112358027A (en) * 2020-11-03 2021-02-12 西南石油大学 Fracturing fluid treatment device for petroleum fracturing acidification
CN112374684A (en) * 2020-11-03 2021-02-19 中国石油天然气股份有限公司 Oil and gas field drilling waste liquid recycling treatment device and method

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CN106915849A (en) * 2017-04-22 2017-07-04 中国石油大学(华东) A kind of acidification of oil field fracturing fluid oily-water seperating equipment and technique
CN106915849B (en) * 2017-04-22 2020-07-07 中国石油大学(华东) Oil-water separation device and process for oilfield acidizing fracturing fluid
CN107673462A (en) * 2017-10-23 2018-02-09 成都恩承科技股份有限公司 The method that glue is broken to fracturing outlet liquid based on γ FeOOH catalysis ozone advanced oxidation systems
CN108585279A (en) * 2018-05-16 2018-09-28 中国石油天然气集团有限公司 A kind of processing method of guanidine glue fracturing outlet liquid
CN109160666A (en) * 2018-10-09 2019-01-08 中国石油集团川庆钻探工程有限公司 Fracturing flowback fluid recycling treatment method
CN111908567A (en) * 2019-05-08 2020-11-10 中国石油天然气集团有限公司 Volume fracturing waste liquid electric flocculation destabilization separation treatment device and method
CN111908567B (en) * 2019-05-08 2022-06-03 中国石油天然气集团有限公司 Volume fracturing waste liquid electric flocculation destabilization separation treatment device and method
CN110240315A (en) * 2019-06-19 2019-09-17 成都国盛环境保护技术有限公司 The method and device thereof that boron processing cycle recycles are removed for guanidine glue fracturing outlet liquid
CN110642334A (en) * 2019-09-27 2020-01-03 北京帝力伟业科技开发有限公司 Electrochemical treatment system and method for high-viscosity fracturing flow-back fluid
CN111646603A (en) * 2020-06-05 2020-09-11 湖北中油科昊机械制造有限公司 Flowing back purification treatment device is returned in oil field fracturing
CN112358027A (en) * 2020-11-03 2021-02-12 西南石油大学 Fracturing fluid treatment device for petroleum fracturing acidification
CN112374684A (en) * 2020-11-03 2021-02-19 中国石油天然气股份有限公司 Oil and gas field drilling waste liquid recycling treatment device and method

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