CN104140142A - Coupling treatment method for fracturing flow-back fluid - Google Patents
Coupling treatment method for fracturing flow-back fluid Download PDFInfo
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- CN104140142A CN104140142A CN201410342970.XA CN201410342970A CN104140142A CN 104140142 A CN104140142 A CN 104140142A CN 201410342970 A CN201410342970 A CN 201410342970A CN 104140142 A CN104140142 A CN 104140142A
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- outlet liquid
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Abstract
The invention discloses a coupling treatment method for fracturing flow-back fluid. The coupling treatment method includes the following step that under the condition that ultrasound and/or an oxidizing agent exists, electrochemical treatment is performed on the fracturing flow-back fluid, which means the treatment performed on the fracturing flow-back fluid is achieved, wherein the electrochemical treatment is performed in an electrolytic tank. The coupling treatment method can be finished in one set of equipment at the same time, while treatment efficiency is improved, the equipment is simplified, and the cost is reduced. According to the treatment method, petroleum, suspended solids, organic pollutants and other harmful ingredients in the fracturing flow-back fluid can be efficiently removed, the treatment effect is obviously better than the treatment effect of a single technology, and the coupling treatment method has industrialized application prospects.
Description
Technical field
The present invention relates to a kind of coupled processing method of fracturing outlet liquid, belong to the sewage treatment area of oil-gas field development.
Background technology
Fracturing outlet liquid is the inevitable outcome in low-permeability oilfield pressing crack construction performance history, has intermittently discrete discharge, the large (100～300m of quantity discharged
3/ well time), pollutant component complexity, environment be there is to the features such as pollution hidden trouble, stable system, high chemical oxygen demand (COD), high stability, high viscosity, common process method is difficult to realize efficient processing.
Conventional fracturing outlet liquid treatment process mainly comprises Coagulation Method, oxidation style, microelectrode method, biochemical process etc. at present.
(1) Coagulation Method
Most oil fields, before advanced treatment pressure break waste water, often adopt Coagulation Method to remove suspended particulate and the partial organic substances in waste water as pre-treatment.Tai-Ace S 150, polymerize aluminum chloride, PAFS are the most common coagulating agent.But, due to return in discharge opeing, exist the macromolecule organic of a large amount of complicated components and viscosity large, often hinder coagulating agent and play a role; conventionally can strengthen in this case the dosage of coagulating agent; but inevitably produce great quantity of floc, form mud, cause secondary pollution.
(2) oxidation style
Oxidation style refers to oxygenant and relevant auxiliary agent is added among fracturing outlet liquid according to certain way, oxygenant utilizes the physics such as light, sound, electricity, magnetic or chemical action to produce the hydroxyl radical free radical of tool strong oxidizing property in water treatment procedure, macromole hardly degraded organic substance in water body is oxidized to low toxicity or nontoxic small-molecule substance, is even directly degraded to CO
2and H
2o, approaches permineralization.Oxidation style mainly comprises several classes such as Fenton oxidation style, photocatalytic oxidation, Ozonation, ultrasonic assisted oxidation method, wet oxidation process and supercritical water oxidation method.Study and show at present, single oxidation style is unsatisfactory to the treatment effect of fracturing outlet liquid, and in most cases, COD clearance is only 20% left and right.
(3) micro-electrolysis method
Micro-electrolysis method is the corrosion electrochemistry principle based on metallic substance (iron, aluminium etc.), the metal of Different electrodes current potential or metal are directly contacted with metal, be immersed in and have in conductive electrolyte solution, produce battery effect, form countless small corrosion galvanic cells (comprising macroscopical battery and microcosmic battery).Useless Fe bits/activated carbon microbattery is to utilize the iron carbide of nano sized particles distributions and the chemical potential of impurities to cause higher than pure iron; The useless Fe bits/activated carbon battery of macroscopic view is in iron filings, to add macroscopical cathode material iron, carbon material are directly contacted and form as graphite, activated carbon etc.Microelectrode method is processed the problem that the fracturing outlet liquid ubiquity treatment time is long, processing efficiency is low.
If make the processing of fracturing outlet liquid reach national emission standard, current technique is that aforesaid method is combined according to different order substantially, successively fracturing outlet liquid is processed, and this part technology is focus at home always.Due to the complicated component of fracturing waste liquor, difficult treatment, all there are some defects in these technology, as low in processing efficiency, technique is loaded down with trivial details, flow process is long, processing costs is expensive, treatment facility is complicated or technology realizability requires high more or less.In sum, current treatment technology can not meet the efficient processing demands of fracturing outlet liquid.
Summary of the invention
The object of this invention is to provide the coupled processing method that a kind of oil field compression fracture returns discharge opeing, utilize electrochemistry-ultrasonic or electrochemistry-advanced oxidation coupling technique or their combination, fracturing outlet liquid is processed, particularly can efficiently remove COD.
The coupled processing method of fracturing outlet liquid provided by the present invention, comprises the steps:
Under condition ultrasonic and/or that oxygenant exists, fracturing outlet liquid is carried out to electrochemical treatment, realize the processing to described fracturing outlet liquid;
Described electrochemical treatment is carried out in electrolyzer.
In above-mentioned coupled processing method, in described electrolyzer, be provided with anode and negative electrode;
Described anode is inert composite electrode, specifically refers to transition metal-type combined electrode, as ruthenium iridium combined electrode, ruthenium tin titanium combined electrode, ruthenium-iridium-tantalum combined electrode or ruthenium tin iridium titanium combined electrode etc.;
Described negative electrode is active electrode, concrete as metal electrodes such as iron active electrode, aluminium active electrodes.
In above-mentioned coupled processing method, the condition of described electrochemical treatment is as follows:
PH value can be 3～7, as is 3;
Spacing between described anode and described negative electrode can be 1～6cm, and as 6cm, Faradaic current can be 1～6A, as 5.5A;
Ratio between the useful area of described anode and described negative electrode and pending fracturing outlet liquid can be 0.05～0.1cm
2/ L, as 0.1cm
2/ L.
In above-mentioned coupled processing method, the time of described electrochemical treatment can be 30～90min, specifically can be 30min～60min, 30min, 60min or 90min.
In above-mentioned coupled processing method, described ultrasonic power can be 100～200W, and as 200W, described ultrasonic frequency can be 40～80kHz, specifically can be 60～80kHz, 60kHz or 80kHz.
In above-mentioned coupled processing method, described oxygenant can be at least one in ozone, potassium ferrate, Fenton reagent and hypochlorous acid;
In described fracturing outlet liquid, the concentration of described oxygenant can be 100～5000mg/L.
In above-mentioned coupled processing method, when described oxygenant is potassium ferrate and/or Fenton reagent, need to regulate the pH value of described fracturing outlet liquid to can be 3～5.
Coupled processing method of the present invention utilizes ultrasonic or advanced oxidization method assisted electrochemical reaction.Electrochemistry-ultrasonic coupling technology refers to introduces ultrasound source in electrolyzer, adds highfield mass transfer electrochemistry-advanced oxidation coupling technique and refer to introduce oxygenant in electrolyzer, the collaborative active intermediate (OH) that produces large measurer strong oxidizing property.The two all can realize the efficient processing of fracturing outlet liquid.Under optimum operation condition, after electrochemistry-ultrasonic or electrochemistry-advanced oxidation coupling technique are processed, fracturing outlet liquid water quality becomes clear, and petroleum-type and solid suspension content can be down to below national secondary discharge standard prescribed value, and COD clearance can be up to 50%～60%.
Coupled processing method of the present invention can complete in a set of equipment simultaneously, simplified apparatus and reduced cost when intensive treatment efficiency.Treatment process of the present invention can efficiently be removed the objectionable constituent such as fracturing outlet liquid petroleum class, suspended solid and organic pollutant, and treatment effect is obviously better than monotechnics, has industrial applications prospect.
Brief description of the drawings
Fig. 1 is the structural representation of electrochemistry-ultrasonic coupling reactor of use in the embodiment of the present invention 1.
In figure, each mark is as follows:
1 electrolyzer, 2 fluid inlets, 31 ultrasonic sources, 4 liquid outlets.
Fig. 2 is the structural representation of electrochemistry-oxidation coupling reactor of use in the embodiment of the present invention 2.
In figure, each mark is as follows:
1 electrolyzer, 2 fluid inlets, 32 oxidant inlets, 4 liquid outlets.
Embodiment
The experimental technique using in following embodiment if no special instructions, is ordinary method.
Material, reagent etc. used in following embodiment, if no special instructions, all can obtain from commercial channels.
The coupling processing of embodiment 1, fracturing outlet liquid
Following embodiment uses the electrochemistry-ultrasonic coupling reactor for treatment fracturing outlet liquid shown in Fig. 1, this electrochemistry-ultrasonic coupling reactor comprises an electrolyzer 1, in this electrolyzer 1, be provided with anode (not shown) and negative electrode (not shown), and spacing between anode and negative electrode can be adjusted in the scope of 1～6cm.Wherein, anode is inert composite electrode, and negative electrode is active electrode, by electrochemical reaction, fracturing outlet liquid is carried out to electrochemicial oxidation.Be provided with fluid inlet 2 and liquid outlet 4 on the top of electrolyzer 1, fluid inlet 2 is for to the pending fracturing outlet liquid of the interior injection of electrolyzer 1, and liquid outlet 4 is for discharging electrolyzer 1 by fracturing outlet liquid after treatment.Ultrasonic auxiliary in order to apply in fracturing outlet liquid treating processes simultaneously, this electrolyzer 1 is connected with a ultrasonic source 31.
Certain oilfield fracturing outlet liquid, stoste pH value is that 6, COD, oleaginousness and solid suspension content are respectively 300mg/L, 12mg/L and the 200mg/L that 5012mg/L, 80mg/L and 500mg/L are all greater than national Specification.
4L fracturing outlet liquid is placed in to the electrode shown in Fig. 1-ultrasonic-oxidation coupling reactor, electrode plate groups is set and is combined into ruthenium iridium combined electrode (anode)-aluminium electrode (negative electrode), the ratio between the useful area of battery lead plate and fracturing outlet liquid is 0.1cm
2/ L.PH value is adjusted to 3, and battery lead plate spacing is 6.0cm, and Faradaic current is 5.5A, and ultrasonic power is 200W, and frequency is 60kHz, processes 30min, and COD value is down to 820mg/L by the 5012mg/L of stoste, and COD clearance is 83.6%.Meanwhile, oleaginousness is almost 0mg/L, and suspended solid is 50mg/L, all lower than the limit value specifying in national secondary discharge standard.
The coupling processing of embodiment 2, fracturing outlet liquid
Following embodiment uses the electrochemistry-advanced oxidation coupled reactor shown in Fig. 2 to process fracturing outlet liquid, this electrochemistry-advanced oxidation coupled reactor comprises an electrolyzer 1, in this electrolyzer 1, be provided with anode (not shown), negative electrode (not shown), and spacing between anode and negative electrode can be adjusted in the scope of 1～6cm.Wherein, anode is inert composite electrode, and negative electrode is active electrode, and third electrode is activated carbon electrodes, by electrochemical reaction, fracturing outlet liquid is carried out to electrochemical oxidation.Be provided with fluid inlet 2, oxidant inlet 32 and liquid outlet 4 on the top of electrolyzer 1, fluid inlet 2 and oxidant inlet 32 are respectively used to fracturing outlet liquid and the oxygenant pending to the interior injection of electrolyzer 1, and liquid outlet 4 is for discharging electrolyzer 1 by the fracturing outlet liquid after oxide treatment.
Certain oilfield fracturing outlet liquid, stoste pH value is that 6, COD value, oleaginousness and solid suspension content are respectively 300mg/L, 12mg/L and the 200mg/L that 5012mg/L, 80mg/L and 500mg/L are all greater than national Specification.
4L fracturing outlet liquid is placed in to the electrode-oxidation coupling reactor shown in Fig. 1, electrode plate groups is set and is combined into ruthenium iridium combined electrode (anode)-aluminium electrode (negative electrode), the ratio between the useful area of battery lead plate and fracturing outlet liquid is 0.1cm
2/ L.PH value is adjusted to 3, and battery lead plate spacing is 6.0cm, and Faradaic current is 5.5A, adds Fenton reagent (oxygenant (H
2o
2) be 5.0g/L, exclusive catalyzer (Fe
2+) 1.2g/L), process 60min, COD value is down to 655mg/L by the 5012mg/L of stoste, and COD clearance is up to 86.9%.Meanwhile, oleaginousness is almost 0mg/L, and suspended solid is about 40mg/L, all lower than the limit value specifying in national standard.
Claims (7)
1. a coupled processing method for fracturing outlet liquid, comprises the steps:
Under condition ultrasonic and/or that oxygenant exists, fracturing outlet liquid is carried out to electrochemical treatment, realize the processing to described fracturing outlet liquid;
Described electrochemical treatment is carried out in electrolyzer.
2. coupled processing method according to claim 1, is characterized in that: in described electrolyzer, be provided with anode and negative electrode;
Described anode is inert composite electrode, and described negative electrode is active electrode.
3. coupled processing method according to claim 1 and 2, is characterized in that: the condition of described electrochemical treatment is as follows:
PH value is 3～7;
Spacing between described anode and described negative electrode is 1～6cm, and Faradaic current is 1～6A;
Ratio between the useful area of described anode and described negative electrode and pending fracturing outlet liquid is 0.05～0.1cm
2/ L.
4. according to the coupled processing method described in any one in claim 1-3, it is characterized in that: the time of described electrochemical treatment is 30～90min.
5. according to the coupled processing method described in any one in claim 1-4, it is characterized in that: described ultrasonic power is 100～200W, described ultrasonic frequency is 40～80kHz.
6. according to the coupled processing method described in any one in claim 1-5, it is characterized in that: described oxygenant is at least one in ozone, potassium ferrate, Fenton reagent and hypochlorous acid;
In described fracturing outlet liquid, the concentration of described oxygenant is 100～5000mg/L.
7. integrated processing method according to claim 6, is characterized in that: when described oxygenant is potassium ferrate and/or Fenton reagent, needing to regulate the pH value of described fracturing outlet liquid is 3～5.
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105217850A (en) * | 2015-11-02 | 2016-01-06 | 北京联众华禹环保科技有限公司 | The innocuity disposal system of fracturing outlet liquid and method |
| CN109851105A (en) * | 2019-02-25 | 2019-06-07 | 中国石油天然气股份有限公司 | A kind of measure waste liquid multistage treatment method and its processing system |
| CN110282787A (en) * | 2019-06-17 | 2019-09-27 | 苏州博创环保科技有限公司 | A kind of processing method of fracturing outlet liquid compounding reuse |
| CN110407668A (en) * | 2018-04-27 | 2019-11-05 | 中国石油化工股份有限公司 | A kind of method of iron tramp in removing aluminum alkoxide |
| CN114436451A (en) * | 2020-11-05 | 2022-05-06 | 北京国海能源技术研究院 | Fracturing flowback fluid treatment method |
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| CN103539234A (en) * | 2013-11-06 | 2014-01-29 | 中国海洋石油总公司 | Integrated processing method of fracturing flow-back fluid |
| CN103539297A (en) * | 2013-11-06 | 2014-01-29 | 中国海洋石油总公司 | Treatment method suitable for fracturing waste fluid from offshore oilfield |
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN105217850A (en) * | 2015-11-02 | 2016-01-06 | 北京联众华禹环保科技有限公司 | The innocuity disposal system of fracturing outlet liquid and method |
| CN110407668A (en) * | 2018-04-27 | 2019-11-05 | 中国石油化工股份有限公司 | A kind of method of iron tramp in removing aluminum alkoxide |
| CN110407668B (en) * | 2018-04-27 | 2021-12-17 | 中国石油化工股份有限公司 | Method for removing iron impurities in alkoxy aluminum |
| CN109851105A (en) * | 2019-02-25 | 2019-06-07 | 中国石油天然气股份有限公司 | A kind of measure waste liquid multistage treatment method and its processing system |
| CN109851105B (en) * | 2019-02-25 | 2022-02-01 | 中国石油天然气股份有限公司 | Multi-stage treatment method and treatment system for measure waste liquid |
| CN110282787A (en) * | 2019-06-17 | 2019-09-27 | 苏州博创环保科技有限公司 | A kind of processing method of fracturing outlet liquid compounding reuse |
| CN114436451A (en) * | 2020-11-05 | 2022-05-06 | 北京国海能源技术研究院 | Fracturing flowback fluid treatment method |
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Application publication date: 20141112 |