CN104743723A - Photocatalytic treatment process for fracturing flow-back fluid - Google Patents
Photocatalytic treatment process for fracturing flow-back fluid Download PDFInfo
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- CN104743723A CN104743723A CN201510173271.1A CN201510173271A CN104743723A CN 104743723 A CN104743723 A CN 104743723A CN 201510173271 A CN201510173271 A CN 201510173271A CN 104743723 A CN104743723 A CN 104743723A
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02W—CLIMATE CHANGE MITIGATION TECHNOLOGIES RELATED TO WASTEWATER TREATMENT OR WASTE MANAGEMENT
- Y02W10/00—Technologies for wastewater treatment
- Y02W10/30—Wastewater or sewage treatment systems using renewable energies
- Y02W10/37—Wastewater or sewage treatment systems using renewable energies using solar energy
Abstract
The invention provides a combined treatment process for fracturing flow-back fluid in an oil and gas field. The process comprises the following steps: (1) adding a certain amount of iron-carbon microelectrode catalyst to a crude fracturing flow-back fluid, and reacting for 0.5-5h under air aeration; (2) sequentially adding a certain amount of pH regulator, coagulant, flocculant and other auxiliaries to the waste liquid which is subjected to gel breaking by virtue of the iron-carbon microelectrode, stirring and settling for 0.1-2.0h, and filtering a supernatant; (3) guiding the filtered supernatant to a photocatalytic reactor, and carrying out circular reaction under the co-action of the catalyst, light and air for 0.5-10h; and (4) carrying out deep treatment on effluent obtained from a light-catalyzed reaction by virtue of a membrane bioseparation technology, wherein under the condition that hydraulic retention time is 2-24h, effluent CODcr can drop to be less than 100(mg/L), total nitrogen can drop to be less than 20(mg/L), total phosphor can drop to be less than 3(mg/L), SS can drop to be less than 30(mg/L) and chromaticity (dilution ratio) can drop to be less than 40, so as to achieve discharge on standard.
Description
Technical field
The present invention relates to a kind for the treatment of process of fracturing outlet liquid, especially relate to the efficient deep treatment method of the fracturing outlet liquid produced when providing a kind of oil-gas field stimulation work, belong to the water treatment field of oil-gas field development.
Background technology
Pressure break has been used widely as the well stimulation that oil reservoir is main and has developed rapidly.Fracturing liquid type mainly contains aqueous fracturing fluid, oil base fracturing fluid, emulsus fracturing liquid and foamed fracturing fluid, and wherein the most frequently used is aqueous fracturing fluid.Returning by stratum the liquid being discharged to ground after pressing crack construction terminates is exactly fracturing outlet liquid, has the features such as suspension content is high, salinity is high, high COD, high chroma, high viscosity and high toxicity.Generally, the pollutant component of fracturing outlet liquid is relatively stable, is a kind of heterogeneous dispersion system of complexity, and discharge, in intermittent, have dispersion and discontinuous feature, is difficult to focus on.If do not added fracturing outlet liquid, process is just directly outer arranges, can to surrounding environment, and especially farm crop and surface drainage system cause very big pollution.
Recent two decades, has carried out further investigation oil field compression fracture being returned to discharge opeing treatment process both at home and abroad.Treatment technology common at present has: biological process, landfill, burning, re-injection and advanced oxidation treatment technology etc.
Biological process has stronger specific aim and feasibility, but the cycle is longer, needs to inoculate and culture out the multiple dominant bacteria returning discharge opeing water quality for difference.CN102776128A provides 2 kinds to carry out taming the special bacterial classification cultivated using melon glue as nutrition, but fracturing outlet liquid complicated components, except melon glue resistates, also may have inhibiting additive (as halo surfactant) to biological activity containing some, the suitability of bacterial classification is greatly limited.In addition, the high COD of process, high sticky return discharge opeing in, the not good and high expensive of biological treatment effect, does not have an industrial value.
Although the requirement of landfill method to environment is lower, region limitation is very large, and is substantially in the superseded stage.
Although burning method to high concentration organic waste Direct Resolution, can control the Sewage Water Emissions of a part, can produce a large amount of pollutent, cause secondary pollution in burning process.
Partial open operation is returned discharge opeing and is transported to water-injection plant reinjection into reservoir by re-injection method, although solve the process problem of this part water, suitable reinjection well compares shortage.
Advanced oxidation treatment technology refers to the larger molecular organics permineralization of difficult degradation in water body or decomposition under the effect of High Temperature High Pressure, electricity, sound, photoirradiation, catalysis, but usually needs AOP technology to combine with other method its maximum treatment efficiency of competence exertion.CN102161536A provides a kind of Fenton of utilization technology carries out oxide treatment method to fracturing outlet liquid, but adopts separately this high-level oxidation technology to be difficult to realize wastewater treatment standard discharge, even if realize, processing costs is also difficult to accept.
Summary of the invention
Object of the present invention be exactly the treatment effect existed for prior art poor, cannot process continuously and the higher problem of cost, propose a kind ofly to process efficient, that processing costs is moderate fracturing outlet liquid serialization advanced treatment process.Realize especially by following technological step:
1. as shown in Figure 1, first in iron carbon reaction tower 1, add a certain amount of Fe/C microelectrode filler 2, the dosage of iron C catalyst is 5 ~ 15% (v), iron carbon mass ratio 1: 1 ~ 20: 1, and iron carbon granules footpath is 5 ~ 30mm.Add acid-conditioning solution ph value to 2 ~ 5, react 0.5 ~ 2 hour under air aeration.Due to the difference in Electrode Potential between iron and carbon, numerous micro-galvanic cell in waste water, can be formed.Electrochemical reaction is there is in containing the aqueous solution of acidic electrolyte bath, produce [H] and [O] of a large amount of nascent state, under the condition of slant acidity, these activeconstituentss all can with the many component generation redox reactions in waste water, make organic macromolecule generation chain-scission degradation and then reach brokenly the effect of glue viscosity reduction;
2., before entering coagulation tank 3, add a certain amount of ph conditioning agent (7 ~ 12), coagulating agent, flocculation agent and other auxiliary agent to the fracturing outlet liquid after broken glue viscosity reduction, complete coagulation-flocculation-sedimentation-sepn process.Above-mentioned ph conditioning agent can be one in sodium hydroxide, potassium hydroxide, calcium hydroxide, calcium oxide or (with) several.Coagulating agent can be a kind of in Tai-Ace S 150, iron(ic) chloride, polymerization oxidation iron, polymer alumina, polymerization oxidation iron aluminium or (with) several.Coagulating agent dosage is 5ppm ~ 100ppm.Flocculation agent can be one in bodied ferric sulfate, PAFS, polyacrylamide or (with) several.Flocculation agent dosage is 1ppm ~ 20ppm.Returning discharge opeing COD value and can reduce 30%-50% after coagulating treatment, SS concentration significantly reduces, and colourity reduces about 80%, for follow-up light-catalyzed reaction creates condition;
3. by the supernatant liquor lead-in light catalyticreactor 4 circulating reaction 0.5-10 after broken glue-coagulating treatment hour.Light source can be UV-light, sunlight, other visible ray one or (with) several.Photo catalysis reactor can be one in slurry reactor, tubular reactor, plate-type reactor, plug flow reactor, fluidized bed reactor or (with) several.Photocatalyst can be transition metal oxide one or (with) several, comprising: SiO
2, SnO
2, Fe
2o
3, Fe
3o
4, CeO
2, ZnO, TiO
2, WO
3, BiTO
3deng.
4. the fracturing outlet liquid after above-mentioned three processing units has shown low sticky, lower COD and the good feature of biological degradability, utilize film biologic treating technique to carry out advanced treatment to the water outlet after light-catalyzed reaction in membrane bioreactor 5, realize qualified discharge.
In the present invention, the catalyzed oxidation that described step 3 mainly make use of light reaches degraded object organic in waste water.
Photocatalysis oxidation technique is a kind of emerging high-level oxidation technology.Since last century the seventies, various countries have carried out a large amount of development works, and photocatalysis oxidation technique is developed rapidly, and successfully this technology have been applied in the field of waste water control.At present, photocatalysis treatment technology is mainly used in the industries such as dyeing waste water, cyanide wastewater, coking chemical waste water and drinking water disinfection, and the present invention is then first by the treatment process of this technology for fracturing outlet liquid.By photocatalytic advanced oxidation technology being combined with traditional materialization, biochemical technology, the fracturing outlet liquid treatment process mentioned in the present invention is made to possess following outstanding feature:
1. pre-treatment additive is less, mild condition, and running cost is lower;
2. photocatalysis treatment unit has reaction conditions gentleness, energy consumption is low, easy and simple to handle;
3. photocatalysis treatment unit can the most organism of mineralising, also can improve the biodegradability that pressure returns liquid, achieve flexible combination and the collocation of different treatment method;
4. adopt special catalyst can make full use of the energy of visible natural light, highlight minimizing secondary pollution and lower-cost advantage that this technique possesses, there is the advantage that other traditional water technologies are incomparable;
5. efficient, energy-conservation, clean nontoxic, continuous treatment.
In sum, compare other fracturing outlet liquid treatment technology, the maximum feature of the present invention is then combined with Traditional materialized, biochemical technology by optical radiation degradation technique, defines a kind of combined treatment process with features such as process is efficient, moderate cost, steady and continuous.Owing to have employed unique photocatalytic advanced oxidation technology, both reduced processing cost, again can efficient organics removal.Adopt treatment process water outlet COD of the present invention to meet state sewage emission standard, thoroughly solve current water-based fracturing and return the problem that discharge opeing process arranges outward, there is comparatively wide and practical application prospect.
Accompanying drawing explanation
Fig. 1 is that water-based fracturing provided by the invention returns discharge opeing processing technological flow schematic diagram.
1-iron carbon reaction tower; 2-iron carbon filler; 3-coagulation tank; 4-photo catalysis reactor; 5-MBR reactor
Fig. 2 is photo catalysis reactor structural representation of the present invention.
1-beaker; 2-photochemical catalysis catalyzer; 3-magnetic stirring apparatus; 4-magnetic stick; 5-air aeration machine;
6-aeration head; 7-UV optical controller; 8-UV fluorescent tube; 9-air filled cavity
Embodiment
The fracturing outlet liquid of certain pressing crack construction well domestic is adopted to be indoor handling object.This fracturing liquid is aqueous fracturing fluid, and thickening material is hydroxypropyl level guar gum (HPG), in addition also containing additives such as a certain amount of gel breaker, cleanup additive, sterilant, tensio-active agents.Outward appearance thickness, in brown color.Water quality analysis is in table 1:
Table 1 fracturing outlet liquid Analysis Results of Water Quality
| Index | PH | Viscosity (mpa.S) | SS(mg/L) | COD cr(mg/L) | Colourity (extension rate) | BOD 5(mg/L) | TDS(mg/L) |
| Numerical value | 7.4 | 13 | 700 | 7300 | 55 | 220 | 7700 |
As seen from Table 1, this fracturing outlet liquid is the trade effluent that typical height is sticky, high COD, high chroma, biochemical are extremely low.Single materialization or biochemical technology is adopted almost to be difficult to process standard discharge.
Embodiment one
400ml stoste is poured respectively in 6 500ml beakers, by reaction ph value 3,5,7,9,11,13, coagulating agent dosage 10ppm, 20ppm, 50ppm, 100ppm, 200ppm, 500ppm, flocculation agent dosage 1ppm, 2ppm, 5ppm, 10ppm, 20ppm, 50ppm, 100ppm do coagulation orthogonal test, getting best one group of supernatant liquor water-quality guideline is optimum, and its water quality analysis data are in table 2:
Table 2 fracturing outlet liquid coagulation-flocculation orthogonal experiment optimal set supernatant liquor Analysis Results of Water Quality
| Index | PH | Viscosity (mpa.S) | SS(mg/L) | COD cr(mg/L) | Colourity (extension rate) | BOD 5(mg/L) | TDS(mg/L) |
| Numerical value | 7.6 | 12.5 | 555 | 7100 | 52 | 220 | 7600 |
Be not difficult to find out by table 2, because fracturing outlet liquid has high sticky, coagulating agent and flocculation agent are difficult to high-effective penetrating, therefore the non-constant of coagulation effect, and every data are almost unchanged.
Embodiment two
Get fracturing outlet liquid stoste 400ml to join in 500ml beaker, put into iron carbon microelectrode particle 30g (particle size ￠ 7mm × 10mm; Iron carbon mass ratio 5: 1), about regulating ph value to 3.0 with dilute sulphuric acid, open air aeration device reaction after 90 minutes, take out solution, add alkali and regulate ph value to 7.5 ~ 8.0, then order adds coagulating agent 50ppm, flocculation agent 5ppm, stir, static, get supernatant liquor and do water quality analysis, data are in table 3:
Table 3 fracturing outlet liquid breaks glue-coagulation supernatant liquor Analysis Results of Water Quality
| Index | PH | Viscosity (mPa.S) | SS(mg/L) | COD cr(mg/L) | Colourity (extension rate) | BOD 5(mg/L) | TDS(mg/L) |
| Numerical value | 7.7 | 2.5 | 107 | 3200 | 15 | 520 | 6600 |
As can be seen from Table 3, break the supernatant liquor viscosity after glue-coagulation through iron carbon microelectrode and reduced 81%, COD and reduce 56%, colourity reduces 73%.Although biodegradable increases, directly biochemical process is adopted still to be difficult to process up to standard.
Embodiment three
As shown in Figure 2, the supernatant liquor 350ml that Example two obtains pours in 500ml beaker 1, adds the special photocatalyst 2 of 0.15g, under the effect of magnetic stirring apparatus 3, and magneton 4 Stirring solution.Meanwhile, open air aeration machine 5, be filled with air by aeration head 6 to solution.Now, open UV optical controller 7, under the acting in conjunction of UV lamp 8, catalyzer 2 and air filled cavity 9, by recycle pump 10, circulating reaction 5 ~ 10 hours, utilizes photocatalytic oxidation degradation until pollutent in mineralizing solution.Carry out water quality analysis by thief hole to solution after reaction, data are in table 4:
Table 4 fracturing outlet liquid breaks glue-coagulation-photochemical catalysis solution Analysis Results of Water Quality _ 1
| Index | PH | Viscosity (mPa.S) | SS(mg/L) | COD cr(mg/L) | Colourity (extension rate) | TDS(mg/L) |
| Numerical value | 7.4 | 0.7 | 22 | 75 | 10 | 3300 |
Can be clear that by table 4, the pressure after photocatalysis treatment returns the emission standard that liquid water outlet can reach national regulations completely.
Embodiment four
In embodiment three, changing the light-catalyzed reaction time is 2 ~ 5 hours, and measure water quality parameter after being filtered by solution, data are in table 5:
Table 5 fracturing outlet liquid breaks glue-coagulation-photochemical catalysis solution Analysis Results of Water Quality _ 2
| Index | PH | Viscosity (mPa.S) | SS(mg/L) | COD cr(mg/L) | Colourity (extension rate) | BOD 5(mg/L) | TDS(mg/L) |
| Numerical value | 7.5 | 1.5 | 30 | 770 | 12 | 345 | 3200 |
Clearly, although water outlet does not now reach the numerical value that emission standard specifies yet, BOD
5/ COD
crvalue is greater than 0.3, and biological process rule of thumb can be adopted to carry out subsequent disposal.Membrane bioreaction technology (MBR) is used membrane separation technique to be combined with activated sludge process, sludge sewage is selected to do mud kind, maintain MLSS7500 (mg/L), dissolved oxygen concentration 4 ~ 6 (mg/L), biochemical reaction 6 ~ 8 hours, after membrane sepn, effluent quality analytical data is in table 6:
Table 6 fracturing outlet liquid breaks glue-coagulation-photochemical catalysis-bio-chemical solution Analysis Results of Water Quality
| Index | PH | Viscosity (mPa.S) | SS(mg/L) | COD cr(mg/L) | Colourity (extension rate) | TDS(mg/L) |
| Numerical value | 7.4 | 0.5 | 23 | 70 | 5 | 3100 |
Found out by table 6, return liquid due to the pressure after photocatalysis treatment and there is good bio-degradable, adopt bioremediation just can realize organic matter degradation and the target of standard discharge, again illustrate fracturing outlet liquid treatment process provided by the present invention and there is extraordinary suitability and handiness.
Claims (6)
1. water-based fracturing returns a discharge opeing deep treatment method, it is characterized in that, comprises the following steps:
(1) regulate fracturing outlet liquid ph value to 2 ~ 5, under iron carbon microelectrode filler and air acting in conjunction, through the aeration of 0.5 ~ 5 hour, return discharge opeing viscosity drop to 4 (mPa.S) below;
(2) regulate solution ph to 7 ~ 12 after above-mentioned broken glue, order dosing coagulant and flocculation agent, stir, sedimentation is after 0.1 ~ 2.0 hour, to supernatant liquid filtering;
(3) supernatant liquor after above-mentioned filtration is entered photo catalysis reactor, under the acting in conjunction of catalyzer, light, air, the BOD of aqueous solution
5/ COD
crvalue is not less than 0.3;
(4) membrane bioreactor is adopted to carry out advanced treatment to the solution after above-mentioned photochemical catalysis, under the condition of hydraulic detention time 2-24 hour, water outlet COD
crcan be reduced to 100 (mg/L) below, total nitrogen is down to 20 (mg/L) below, and total phosphorus is down to 3 (mg/L) below, and SS is down to 30 (mg/L) below, and colourity (extension rate) is down to less than 40.
2. according to claim 1, regulate the conditioning agent of fracturing outlet liquid ph value, can be one in sodium hydroxide, potassium hydroxide, calcium hydroxide, calcium oxide or (with) several.
3. according to claim 1, said iron carbon microelectrode filler, its dosage is 5% ~ 15% (v), and iron carbon mass ratio is 1: 1 ~ 20: 1, and packing material size is 5 ~ 30mm.
4. according to claim 1, said coagulating agent can be one in Tai-Ace S 150, iron(ic) chloride, polymerization oxidation iron, polymer alumina, polymerization oxidation iron aluminium or (with) several, coagulating agent dosage is 5 ~ 100 (mg/L); Flocculation agent can be one in bodied ferric sulfate, PAFS, polyacrylamide or (with) several, flocculation agent dosage is 1 ~ 20 (mg/L).
5. according to claim 1, said photo catalysis reactor can be one in slurry reactor, tubular reactor, plate-type reactor, plug flow reactor, fluidized bed reactor or (with) several; Catalyzer can be transition metal oxide one or (with) several, as SiO
2, SnO
2, Fe
2o
3, Fe
3o
4, CeO
2, ZnO, TiO
2, WO3, BiTO
3deng; Light can be UV-light, sunlight, other visible ray one or (with) several.
6. according to claim 1, said membrane bioreactor is made up of bio-reaction zone and membrane separation zone, bio-reaction zone can be active sludge, settled organism filler, hold concurrently oxygen, anaerobism independent technique or (with) process combination; Membrane separation zone membrane module used can be independently tubular fibre, board-like, tubular type, butterfly or combination; Membrane process can be micro-filtration, ultrafiltration, nanofiltration, reverse osmosis independence use or process combination.
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Cited By (4)
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| CN107597151A (en) * | 2017-11-09 | 2018-01-19 | 西南石油大学 | The preparation method of Bi/Bi4O5X2 (X=Br, I) photochemical catalyst of organic boron is aoxidized under a kind of visible ray |
| CN109499587A (en) * | 2019-01-11 | 2019-03-22 | 西南石油大学 | The preparation of the ultra-thin U-BiOBr/BiOI photochemical catalyst of organic boron in a kind of processing fracturing outlet liquid |
| CN113908863A (en) * | 2021-11-16 | 2022-01-11 | 西南石油大学 | Fracturing flowback fluid purification experimental method based on photocatalytic reaction |
| CN115403181A (en) * | 2022-08-24 | 2022-11-29 | 成都苏坤环保科技有限公司 | Oil field produced water processing system |
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| CN107597151A (en) * | 2017-11-09 | 2018-01-19 | 西南石油大学 | The preparation method of Bi/Bi4O5X2 (X=Br, I) photochemical catalyst of organic boron is aoxidized under a kind of visible ray |
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Application publication date: 20150701 |