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 |