CN104556492B - A kind of method of the recycling of fracturing outlet liquid - Google Patents
A kind of method of the recycling of fracturing outlet liquid Download PDFInfo
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Abstract
The method that the invention provides the recycling of a kind of fracturing outlet liquid, including: i) fracturing outlet liquid after natural subsidence is carried out air-flotation process and obtain the first treatment fluid, to remove major part suspension greasy dirt, insoluble Organic substance and suspended solids thing；Ii) in the first treatment fluid, addition flocculant, to carry out chemical flocculation process, obtains the second treatment fluid through precipitation and filtration treatment the most again, to remove suspension greasy dirt, insoluble Organic substance and suspended solids thing etc. further；Iii) in the second treatment fluid, dissolve alkaline matter, then carry out electricity flocculation treatment and obtain the 3rd treatment fluid, to remove dissolved organic matter and metal ion；Iv) precipitating described 3rd treatment fluid and filtration treatment, and by the pH of the product after filtration treatment to regulation to 69, obtain end product water distribution liquid, described water distribution liquid can be used in configuring fracturing fluid.
Description
Technical field
The method that the present invention relates to the recycling of a kind of fracturing outlet liquid, can be applicable to utilize fracturing skill
The recycling returning discharge opeing of art exploitation shale gas.
Background technology
Unconventional gas resource amount is more and more higher at the proportion of natural gas total amount, along with horizontal drilling technology, water
The development of power fracturing technique, shale gas is as a kind of important unconventional gas resource, it has also become global Oil Gas
The new highlight of development of resources.2012, China the most formally pulled open the curtain of shale gas exploitation.
Utilize hydraulic fracturing technology exploitation shale gas not only to consume substantial amounts of water, also to discharge substantial amounts of high concentration
Waste water, the treatment for reuse technology of the waste water produced in exploratory development recovery process, China's shale gas exploitation is sent out
Exhibition important in inhibiting.
At present, have been developed for some simple processing methods for fracturing outlet liquid, but all do not reach recovery profit again
Degree, recycling referred herein refers to preparation water preparing fracturing fluid as fracturing fluid again, property
Can remain to meet requirement.There is research to be used as oil field reinjection water after being flocculated by fracturing outlet liquid, also study profit
The method combined with biological and materialization carries out process and also serves as oil field reinjection water use.But for shale gas pressure break
Return discharge opeing, due to the restriction of geographical conditions, it is impossible to move oil field the most again to and carry out re-injection use, the
One step carries out harmless treatment, is exactly further the reuse water distribution as fracturing fluid.But fracturing fluid to be reached
Performance requirement it is necessary to there is certain requirement to water distribution.But fracturing outlet liquid have innage, COD is high, salt high,
Hardness high, these all can affect the performance of fracturing fluid.Described COD is COD, its be with
Chemical method measures the amount needing oxidized reducing substances in water sample.
In view of the above problems, developing simplicity, process technique effectively and rapidly, after process, water quality can reach
The requirement of preparing fracturing fluid, can reach environment and economic double benefit by waste water local use.
Summary of the invention
It is an object of the invention to provide a kind of simplicity, effectively and rapidly processing method, in order to process utilization pressure
Split technology exploitation shale gas returns discharge opeing, effectively removes oil therein, COD, hardness etc., makes processed waste water
The requirement of fracturing fluid preparation water can be reached, reach water saving, the purpose reduced discharging, it is achieved environment is double with economy
Weight benefit.
The invention provides a kind of fracturing outlet liquid processing shale gas exploitation, fracturing fluid can be reached after process and join
The requirement of water processed.For reaching above-mentioned purpose, the present invention adopts the following technical scheme that
The invention provides a kind of recycling method of fracturing outlet liquid, including:
I) fracturing outlet liquid after natural subsidence is carried out air-flotation process and obtain the first treatment fluid, to remove
State major part suspension greasy dirt, insoluble Organic substance and suspended solids thing in fracturing outlet liquid；
Ii) in the first treatment fluid, addition flocculant is to carry out chemical flocculation process, the most again at precipitation and filtration
Reason obtains the second treatment fluid, with remove further the suspension greasy dirt in the first treatment fluid, insoluble Organic substance and
Suspended solids thing etc.；
Iii) in the second treatment fluid, dissolve alkaline matter, then carry out electricity flocculation treatment and obtain the 3rd treatment fluid,
To remove the dissolved organic matter in the second treatment fluid and metal ion；
Iv) described 3rd treatment fluid is precipitated and filtration treatment, and by the pH of the product after filtration treatment extremely
Regulation, to 6-9, obtains end product water distribution liquid, and described water distribution liquid can be used in configuring fracturing fluid.
In a preferred embodiment of the present invention, described air-flotation process also adds in being included in that described pressure break is counter and arranging
Enter flocculant.The pneumatically supported flocculant that is simultaneously introduced carries out flocculation treatment to described fracturing outlet liquid, strengthens air supporting
The effect processed.It is higher that shale gas returns usual oil content in discharge opeing, and the recycling of discharge opeing is returned in the existence impact of oil,
Utilizing air-flotation process to return discharge opeing, oil can effectively be removed, simultaneously the suspension material in the most removable water,
Remove returning the material that discharge opeing reuse impacts further.
In further preferred embodiment of the present invention, described flocculant is selected from aluminium polychlorid (PAC), poly-
At least one in acrylamide (PAM) and poly-ferric chloride (PFS).
In a preferred embodiment of the present invention, the addition of described aluminium polychlorid is pending liquid
0.03-1 weight %, the addition of polyacrylamide is 0.0002-0.001 weight % of pending liquid, polyaluminium
The addition of ferrum is 0.03-1 weight % of pending liquid.
In a preferred embodiment of the present invention, described alkaline matter is in alkali-metal hydroxide
At least one, preferably sodium hydroxide.
In a preferred embodiment of the present invention, when the basicity of water is less than 100mg/L with calcium carbonate,
And when in water, barium, content of strontium are higher than 5mg/L, add containing Na2CO3Alkaline matter.
In a preferred embodiment of the present invention, the addition of described alkaline matter is can be by described second
The pH value for the treatment of fluid regulates the amount to 10-12.The high price gold in the second treatment fluid can be effectively removed in this scope
Belong to ion, reduce the high volence metal ion impact on fracturing fluid property, reach the purpose of reuse dosing.
In a preferred embodiment of the present invention, described electricity flocculation treatment uses organizes positive and negative electrode more, can root
Arbitrarily set according to actual demand, preferably 5 groups positive and negative electrodes, being selected from ferrum, aluminum or stone of described anelectrode
Electrode ink.
In a preferred embodiment of the present invention, the voltage in described electricity flocculation treatment is 2-150V.
In a preferred embodiment of the present invention, between the often group both positive and negative polarity in described electricity flocculation treatment
Away from for 10-100cm.
Specifically, fracturing outlet liquid after natural subsidence in collecting pit can initially entered air-dissolving air-float
Device processes, and main removal returns major part suspension oil, Organic substance and float etc., Qi Zhongsuo in discharge opeing
In the flocculant such as adding medicament is aluminium polychlorid (PAC), polyacrylamide (PAM), poly-ferric chloride (PFS)
One or more, its concrete consumption is as follows: according to mass percent measure, the addition of PAC is pending
0.03-1 weight % of liquid, the addition of PAM is 0.0002-0.001 weight % of pending liquid, and PFS adds
Dosage is 0.03-1 weight % of pending liquid.After air-flotation process, in fracturing outlet liquid, the clearance of oil is big
In 90%, COD clearance is 50-80%, and turbidity removal rate is more than 80%.
After air supporting water outlet again through flocculation reaction in order to remove further the row of returning after air-flotation process
Remaining suspension oil, Organic substance and float etc. in liquid, added medicament is aluminium polychlorid (PAC),
Polyacrylamide (PAM), one or more in the flocculant such as poly-ferric chloride (PFS), its concrete consumption is as follows:
Measuring according to mass percent, the addition of PAC is 0.03-1 weight % of pending liquid, the interpolation of PAM
Amount is 0.0002-0.001 weight % of pending liquid, and the addition of PFS is 0.03-1 weight % of pending liquid.
After flocculation treatment, then in fracturing outlet liquid, the clearance of oil is more than 90% after precipitation filters, COD clearance
At 20-40%, turbidity is less than 5NTU.Sedimentation tank upflow velocity is less than 1.5m/h.
Water outlet after flocculation, then carry out electricity flocculation reaction in order to remove partial solubility Organic substance and high price
Metal ions etc., electricity flocculation positive pole can be selected for ferrum or aluminum or graphite electrode, and first two is for consuming electrode, latter
For not consuming electrode, voltage is 2-150V, and the spacing of pole plate group is 10-100cm, the most often between group both positive and negative polarity
Distance, electricity flocculation apparatus can be selected for 1-5 group electrode.Flocculation reaction groove adds with sodium hydroxide for main one-tenth
The alkaline matter divided, pH regulator to 10-12.Barium, content of strontium when in water, basicity is less than 100mg/L or in water
During higher than 5mg/L, need to add a certain amount of with Na2CO3It it is main alkaline matter.Response time is 30-60min.
Containing substantial amounts of flco in electricity flocculation water outlet, needing first to precipitate, sedimentation tank upflow velocity is less than 2m/h.Warp
After precipitation, still containing a certain amount of float in fracturing outlet liquid, need to carry out filtration treatment, after filtration, pressure break is returned
The turbidity of discharge opeing is 20-30% less than 5NTU, COD clearance, and the clearance of high volence metal ion is more than 50%.
Water outlet selects acid (sulphuric acid or hydrochloric acid) to carry out pH readjustment, and regulation pH value is to 6-9, the dosing after i.e. being processed
Water.
The technical characteristic of the present invention is as follows:
The present invention be mainly used to process utilize hydraulic fracturing technology exploitation shale gas return discharge opeing, recyclable after process
Recycling.
The present invention selects the technological process of " air supporting-chemical flocculation-precipitation-filtration-electricity flocculation-precipitation-filter " first
Process fracturing outlet liquid.
In the present invention, pneumatically supported added medicament is aluminium polychlorid (PAC), polyacrylamide (PAM), is polymerized chlorine
Changing one or more in the cationic flocculants such as ferrum (PFS), its concrete consumption is as follows: according to mass percent
Metering, the addition of PAC is 0.03-1 weight % of pending liquid, and the addition of PAM is pending liquid
0.0002-0.001 weight %, the addition of PFS is 0.03-1 weight % of pending liquid.
The added medicament that flocculates in the present invention is aluminium polychlorid (PAC), polyacrylamide (PAM), polyaluminium
One or more in the cationic flocculants such as ferrum (PFS), its concrete consumption is as follows: according to mass percent
Amount, the addition of PAC is 0.03-1 weight % of pending liquid, and the addition of PAM is pending liquid
0.0002-0.001 weight %, the addition of PFS is 0.03-1 weight % of pending liquid.
The present invention flocculates final settling tanks upflow velocity less than 1.5m/h.
Electricity of the present invention flocculation positive pole can be selected for ferrum or aluminum or graphite electrode, and first two is for consuming electrode, and latter is
Not consuming electrode, the response time is 30-60min, and voltage is 2-150V, and electricity flocculation apparatus can be selected for 1-5 group electricity
Pole, the spacing of pole plate group is 10-100cm, the most often the distance between group both positive and negative polarity.Flocculation reaction groove adds with
Sodium hydroxide is the alkaline matter of main component, pH regulator to 10-11.5.When water basicity with calcium carbonate
During less than 100mg/L, and when in water, barium, content of strontium are higher than 5mg/L, need to add a certain amount of with Na2CO3
It it is main alkaline matter.
Pressure break after the present invention utilizes " air supporting-flocculation-precipitation-filtration-electricity flocculation-precipitation-filter " PROCESS FOR TREATMENT is returned
Discharge opeing, can use by preparing fracturing fluid again, and performance meets requirement (SY/T6376-2008).
Beneficial effects of the present invention:
1) method of the present invention is simple to operation, it is possible to meet the requirement of in-situ processing
2) fracturing outlet liquid is processed by the method for the present invention, it is possible to make the clearance of oil in fracturing outlet liquid
More than 90%, COD clearance is 50-80%, and turbidity removal rate is more than 80%；
3) the water distribution liquid that the method for the present invention obtains can use by preparing fracturing fluid again, and performance meets requirement
(SY/T6376-2008)。
3) flow process of the present invention easily realizes, simple to operate, with low cost, and effect is obvious, can integrated skid mounted equipment,
The shortcoming that can overcome shale gas block exploitation repeated construction sewage disposal device, reduces investment.After sewage disposal completely
Foot requirement, is reused, and more overcomes shale gas and exploits the drawback of a large amount of consumption of water resources.
Detailed description of the invention
Below in conjunction with embodiment, the present invention is described in detail, but the scope of the present invention is not limited to following enforcement
Example.
In embodiment, the analysis method of total hardness, calcium hardness and total alkalinity is with reference to " water and effluent monitoring analyze method
(fourth edition) " (China Environmental Science Press's publication).
Embodiment 1
Shale gas well 1, fracturing outlet liquid total oil content 11608mg/L, COD content 2410mg/L, turbidity
For 3130NTU, total hardness is (with CaCO3Meter) it is 1094mg/L, calcium hardness is (with CaCO3Meter) it is 954mg/L,
Total alkalinity is (with CaCO3Meter) be 65mg/L, ferrum, manganese, barium ions content be respectively 37mg/L, 1.02mg/L,
3.3mg/L。
0.3 weight % and 0.002 weight %(is added in terms of fracturing outlet liquid weight) in described fracturing outlet liquid
Aluminium polychlorid and polyacrylamide carry out air-flotation process and obtain the first treatment fluid, described first treatment fluid
Oil and COD concentration are respectively 19.44mg/L and 950mg/L, and turbidity is 20NTU, oil, COD and turbid
The clearance of degree is respectively 99.8%, 60.6% and 99.4%.First treatment fluid adds 0.1 weight % and
0.0002 weight %(is in terms of the first treatment fluid weight) aluminium polychlorid and polyacrylamide, with at first
Reason liquid carry out chemical flocculation process obtain the second treatment fluid, described second treatment fluid through precipitation filter after, oil and
COD concentration is respectively 1.32mg/L and 640mg/L, and turbidity is 1NTU, going of oil, COD and turbidity
Except rate is respectively 93.2%, 32.6% and 95%.Sodium carbonate and sodium hydroxide is added in described second treatment fluid,
Sodium carbonate dosage more than or equal to 100mg/L, regulates the pH value of described second treatment fluid with basicity in regulation water
Carrying out electricity flocculation treatment to 11 again and obtain the 3rd treatment fluid, electricity flocculation positive pole selects iron electrode, and voltage is 40V,
The spacing of pole plate group is 100cm, 1 group of electrode, and the response time is 30min.Described 3rd treatment fluid is through precipitation
Using acid to regulate its pH value after filtration and obtain described water distribution liquid to 6, COD content is 550mg/L, total hardness
(with CaCO3Meter) it is 263mg/L, calcium hardness is (with CaCO3Meter) it is 203mg/L, clearance is respectively 76%,
78.7%, ferrum, manganese, barium ions content are respectively 1.33mg/L, 0.05mg/L, 1.31mg/L, and clearance divides
It is not 96.4%, 95.1%, 60.3%.The water distribution liquid obtained after above-mentioned process for preparing clean fracturing fluid,
Property indices meets pressure break requirement.
Embodiment 2
Shale gas well 2, fracturing outlet liquid total oil content 23.2mg/L, COD content 1708mg/L, turbidity is
44NTU, total hardness is (with CaCO3Meter) it is 632mg/L, calcium hardness is (with CaCO3Meter) it is 511mg/L, always
Basicity is (with CaCO3Meter) it is 115mg/L, Fe and Mn content is respectively 7mg/L, 32.5mg/L.
In described fracturing outlet liquid, add 0.04 weight %(in terms of fracturing outlet liquid weight) poly-ferric chloride
And carry out air-flotation process obtain the first treatment fluid, the oil of described first treatment fluid and COD concentration be respectively
2.0mg/L and 848mg/L, turbidity is 6.3NTU, oil, the clearance of COD and turbidity be respectively 91.3%,
50.4% and 85.7%.In the first treatment fluid, add 0.05 weight % and 0.0002 weight %(process with first
Liquid weight meter) aluminium polychlorid and polyacrylamide, with the first treatment fluid is carried out chemical flocculation process obtain
Second treatment fluid, described second treatment fluid through precipitation filter after, oil and COD concentration be respectively 0.2mg/L and
525mg/L, turbidity is 1NTU, and the clearance of oil, COD and turbidity is respectively 90%, 38.1% and 84.1%.
Described second treatment fluid adds sodium hydroxide with regulate described second treatment fluid pH value to 11.5,
Carrying out electricity flocculation treatment again and obtain the 3rd treatment fluid, electricity flocculation positive pole selects graphite electrode, and voltage is 70V, pole
The spacing of plate group is 20cm, 3 groups of electrodes, and the response time is 60min.Described 3rd treatment fluid filters through precipitation
Rear use acid regulates its pH value and obtains described water distribution liquid to 7, and COD content is 463mg/L, total hardness (with
CaCO3Meter) it is 287mg/L, calcium hardness is (with CaCO3Meter) it is 236mg/L, clearance is respectively 54.6%
With 53.8%, Fe and Mn content is respectively 0.37mg/L, 10.6mg/L, clearance is respectively 94.7%,
67.4%.The water distribution liquid obtained after above-mentioned process can be used for preparing clean fracturing fluid, and property indices meets
Pressure break requirement.
Embodiment 3
Shale gas well 3, fracturing outlet liquid total oil content 470.8mg/L, COD content 1922mg/L, turbidity is
311NTU, total hardness is (with CaCO3Meter) it is 1065mg/L, calcium hardness is (with CaCO3Meter) it is 879mg/L,
Total alkalinity is (with CaCO3Meter) be 123mg/L, ferrum, manganese, barium ions content be respectively 0.5mg/L, 15.2mg/L,
2.8mg/L。
Adding concentration in described fracturing outlet liquid is that 0.1 weight %(is in terms of fracturing outlet liquid weight) polymerization
Iron chloride also carries out air-flotation process and obtains the first treatment fluid, and the oil of described first treatment fluid and COD concentration are respectively
For 11.7mg/L and 866mg/L, turbidity is 10.2NTU, and the clearance of oil, COD and turbidity is respectively
97.5%, 54.9% and 96.7%.0.03 weight %(is added in terms of the first treatment fluid weight) in the first treatment fluid
Poly-ferric chloride, with the first treatment fluid is carried out chemical flocculation process obtain the second treatment fluid, at described second
Reason liquid is after precipitation filters, and oil and COD concentration are respectively 0.7mg/L and 643mg/L, and turbidity is 1.5NTU,
The clearance of oil, COD and turbidity is respectively 94%, 25.8% and 85.3%.Described second treatment fluid is thrown
Hydro-oxidation sodium regulate described second treatment fluid pH value to 10.5, then carry out electricity flocculation treatment obtain at the 3rd
Reason liquid, electricity flocculation positive pole aluminium electrode, voltage is 150V, and the spacing of pole plate group is 10cm, 5 groups of electrodes,
Response time is 50min.3rd treatment fluid use after precipitation filters acid regulate its pH value be 9 obtain final
Product water distribution liquid, COD content is 507mg/L, and total hardness is (with CaCO3Meter) it is 527mg/L, calcium hardness (with
CaCO3Meter) it is 432mg/L, clearance is respectively 50.5% and 50.9%, and ferrum, manganese, barium ions content are respectively
For 0.05mg/L, 4.8mg/L, 1.33mg/L, clearance is respectively 90%, 68.4%, 52.5%.Through above-mentioned
The water distribution liquid obtained after process is for preparing clean fracturing fluid, and property indices meets pressure break requirement.
Claims (12)
1. a method for the recycling of fracturing outlet liquid, including:
I) fracturing outlet liquid after natural subsidence is carried out air-flotation process and obtain the first treatment fluid, to remove
State major part suspension greasy dirt, insoluble Organic substance and suspended solids thing in fracturing outlet liquid；
Ii) in the first treatment fluid, addition flocculant is to carry out chemical flocculation process, the most again at precipitation and filtration
Reason obtains the second treatment fluid, with remove further the suspension greasy dirt in the first treatment fluid, insoluble Organic substance and
Suspended solids thing；
Iii) in the second treatment fluid, dissolve alkaline matter, then carry out electricity flocculation treatment and obtain the 3rd treatment fluid,
To remove the dissolved organic matter in the second treatment fluid and metal ion；
Iv) described 3rd treatment fluid is precipitated and filtration treatment, and the pH of the product after filtration treatment is adjusted
Joint, to 6-9, obtains end product water distribution liquid, and described water distribution liquid can be used in configuring fracturing fluid.
Method the most according to claim 1, it is characterised in that described air-flotation process is included in described pressure
Split and return addition flocculant in discharge opeing.
Method the most according to claim 1 and 2, it is characterised in that described flocculant is selected from polymerization chlorine
Change aluminum, at least one in polyacrylamide and poly-ferric chloride.
Method the most according to claim 3, it is characterised in that the addition of described aluminium polychlorid is
0.03-1 weight % of pending liquid, the addition of polyacrylamide is the 0.0002-0.001 weight of pending liquid
%, the addition of poly-ferric chloride is 0.03-1 weight % of pending liquid.
Method the most according to claim 1, it is characterised in that described alkaline matter is selected from alkali-metal
At least one in hydroxide.
Method the most according to claim 4, it is characterised in that described alkaline matter is sodium hydroxide.
Method the most according to claim 1, it is characterised in that when the basicity of water is less than with calcium carbonate
During 100mg/L, and when in water, barium, content of strontium are higher than 5mg/L, add containing Na2CO3Alkaline matter.
Method the most according to claim 1, it is characterised in that the addition of described alkaline matter is energy
Enough amounts by the pH value regulation of described second treatment fluid to 10-12.
Method the most according to claim 1, it is characterised in that described electricity flocculation treatment includes that use is many
Group positive and negative electrode, described anelectrode chosen from Fe, aluminum or graphite electrode.
Method the most according to claim 1, it is characterised in that described electricity flocculation treatment includes using 5
Group positive and negative electrode, described anelectrode chosen from Fe, aluminum or graphite electrode.
11. methods according to claim 1, it is characterised in that the voltage in described electricity flocculation treatment is
2-150V。
12. methods according to claim 1, it is characterised in that the often group in described electricity flocculation treatment is just
Spacing between negative pole is 10-100cm.
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| CN105041268B (en) * | 2015-06-17 | 2018-02-13 | 中国石油化工股份有限公司 | A kind of more cluster abrasive perforating liquid recovery methods of coiled tubing and retracting device |
| CN105347542B (en) * | 2015-10-29 | 2018-02-02 | 中国石油集团渤海钻探工程有限公司 | One kind reuses technique after utilizing guar gum fracturing outlet liquid water process |
| CN105330065A (en) * | 2015-11-19 | 2016-02-17 | 黄河裕泰（宁夏）环保科技有限公司 | Device of fracturing fluid flowback equipment and technological process of device |
| CN105542740A (en) * | 2015-12-11 | 2016-05-04 | 中国石油天然气股份有限公司 | Preparation method of ternary compound flooding, ternary compound flooding and use of ternary compound flooding |
| CN106892513B (en) * | 2015-12-21 | 2019-10-11 | 中国石油天然气股份有限公司 | A kind of shale gas fracturing outlet liquid treatment for reuse method |
| CN107235580B (en) * | 2017-05-16 | 2023-07-28 | 方明环保科技(漳州)有限公司 | Treatment method and equipment for fracturing flowback fluid of oil and gas field drilling well |
| CN113150789A (en) * | 2020-12-30 | 2021-07-23 | 陕西品物皆春生态科技有限公司 | Guar gum-humic acid type oil and gas field fracturing fluid flowback fluid water retention and sand fixation agent and preparation method and application thereof |
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| US20120292259A1 (en) * | 2011-05-17 | 2012-11-22 | High Sierra Energy, LP | System and method for treatment of produced waters containing gel |
| US8877690B2 (en) * | 2011-08-31 | 2014-11-04 | Prochemtech International, Inc. | Treatment of gas well production wastewaters |
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| "页岩气压裂返排液处理新技术综述";许剑 等;《中国石油和化工标准与质量 》;20130630(第12期);第166、167页 * |
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