CN104500047B - Probe material is to evaluate the method for fracturing effect in analysis multistage fracturing fluid recovery (backflow) liquid - Google Patents

Probe material is to evaluate the method for fracturing effect in analysis multistage fracturing fluid recovery (backflow) liquid Download PDF

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Publication number
CN104500047B
CN104500047B CN201410850962.6A CN201410850962A CN104500047B CN 104500047 B CN104500047 B CN 104500047B CN 201410850962 A CN201410850962 A CN 201410850962A CN 104500047 B CN104500047 B CN 104500047B
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sample
liquid
fracturing fluid
backflow
filter
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CN104500047A (en
Inventor
张洪君
王浩
郑猛
闫峰
郭韬
何强
张西子
亢思丹
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China Petroleum and Natural Gas Co Ltd
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China Petroleum and Natural Gas Co Ltd
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    • EFIXED CONSTRUCTIONS
    • E21EARTH OR ROCK DRILLING; MINING
    • E21BEARTH OR ROCK DRILLING; OBTAINING OIL, GAS, WATER, SOLUBLE OR MELTABLE MATERIALS OR A SLURRY OF MINERALS FROM WELLS
    • E21B47/00Survey of boreholes or wells
    • E21B47/10Locating fluid leaks, intrusions or movements
    • E21B47/11Locating fluid leaks, intrusions or movements using tracers; using radioactivity
    • EFIXED CONSTRUCTIONS
    • E21EARTH OR ROCK DRILLING; MINING
    • E21BEARTH OR ROCK DRILLING; OBTAINING OIL, GAS, WATER, SOLUBLE OR MELTABLE MATERIALS OR A SLURRY OF MINERALS FROM WELLS
    • E21B43/00Methods or apparatus for obtaining oil, gas, water, soluble or meltable materials or a slurry of minerals from wells
    • E21B43/25Methods for stimulating production
    • E21B43/26Methods for stimulating production by forming crevices or fractures

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  • Physics & Mathematics (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Geology (AREA)
  • Mining & Mineral Resources (AREA)
  • Geophysics (AREA)
  • Environmental & Geological Engineering (AREA)
  • Fluid Mechanics (AREA)
  • General Life Sciences & Earth Sciences (AREA)
  • Geochemistry & Mineralogy (AREA)
  • Treatment Of Liquids With Adsorbents In General (AREA)
  • Water Treatment By Sorption (AREA)

Abstract

The invention provides probe material in a kind of analysis multistage fracturing fluid recovery (backflow) liquid to evaluate the method for fracturing effect, the method comprising the steps of:Sampled in producing well and carry out sample treatment;The concentration for returning various probe materials in discharge fracturing fluid after detection process;According to the concentration of probe material, the fracturing effect of every layer of evaluation.The pressure break situation that the method for the present invention judges is intuitively accurate, and can quantify, and error is small, has important directive function to the fracture job of same interval, for the situation optimizing design scheme of Different Strata, improves pressure break efficiency, reduces cost.

Description

Probe material is to evaluate the method for fracturing effect in analysis multistage fracturing fluid recovery (backflow) liquid
Technical field
The present invention relates to the correlation technique in fracturing fluid recovery (backflow) tracer field, in specifically a kind of fracturing fluid recovery (backflow) liquid to multistage Probe material is analyzed to evaluate the method for fracturing effect.
Background technology
The large-scale development of horizontal well at present, multi-layer multi-stage pressure break is the preferred technique of stratum transformation, but layer position selects During there is no specific aim.All it is to select to be layered by experience especially in prospect pit during pressure break.Therefore for pressure Data acquisition and issuance fracturing effect after splitting just is particularly important.
Fracture intensity after pressure break can be monitored and analyzed in the prior art by micro seismic method, potentiometry etc., but all There is complex process, cost is high the shortcomings of, and often due to strata condition is complicated, disturbing factor is more, it is difficult to every layer of feelings Condition is accurately explained.In conventional staged fracturing of horizontal well, by return discharge opeing be only capable of recognizing return lifting rate and whether There is oil to have liquid, and can not specifically judge the fracturing effect of each interval and go out liquid situation.
On the tracer technique of fracturing outlet liquid, correlative study report both domestic and external is also seldom at present, simply selects in the past Chlorion mineral ion etc. is used as reference target, and accuracy of detection is low, disturbing factor is more, is intended only as supplementary means reference.It is and more The layering tracer of level pressure break is even more to have no first to close report.
The content of the invention
It is a primary object of the present invention to provide in a kind of analysis multistage fracturing fluid recovery (backflow) liquid probe material to evaluate pressure break The method of effect.
To achieve the above object, for the present invention mainly in multistage fracturing outlet liquid, periodic detection returns tracer in discharge opeing The change of concentration, then judge the row's of returning situation by accumulating the amount of tracer and returning isostere product, and then understand each lamination and split Effect, reach the purpose of evaluation fracturing effect.
The invention provides probe material in analysis multistage fracturing fluid recovery (backflow) liquid to evaluate the method for fracturing effect, this method Including:
(1) sampled in producing well and carry out sample treatment;
(2) concentration for returning various probe materials in discharge fracturing fluid after detection process;
(3) according to the concentration of probe material, the fracturing effect of every layer of evaluation.
According to specific embodiments of the present invention, in method of the invention, the sample handling procedure includes:By disappearing Solve, adsorb, being filtered to remove the impurity interfered to Instrument measuring, eluting.
According to specific embodiments of the present invention, in method of the invention, the sample handling procedure is to utilize a kind of pressure Split liquid and return discharge opeing sample processing device, the device includes digestion instrument, adsorbent equipment and the filter concatenated by pipeline;Disappear The container that device is accommodating fracturing fluid recovery (backflow) liquid sample is solved, its top is provided with injection port, H2O2Import, N2It is passed through mouth and puts Gas port;Inlet is set at the top of adsorbent equipment, and bottom sets liquid outlet, adsorbing medium is filled with adsorbent equipment;Filter Top sets inlet, and bottom is provided with tap hole, and medium position sets 0.45 μm of filter membrane in filter, and filter membrane top is to treat Fluid space is filtered, bottom is filtered fluid space, and filter is also configured with vacuum extractor, for filter membrane bottom to be taken out Vacuum and filtering power is provided;The first valve is provided with pipeline between digestion instrument and adsorbent equipment;In adsorbent equipment The second valve is provided with pipeline between filter;3rd valve is set at the tap hole of filter;
The fracturing fluid recovery (backflow) liquid sample treatment includes:
Sample is added into digestion instrument by injection port, by H2O2Import adds H2O2, and by N2Mouth is passed through into sample Nitrogen is continually fed into, makes sample and H2O2Fully reaction resolution;
The first valve, the second valve are opened, opens vavuum pump pumping, sample after resolution is pumped into adsorbent equipment, removing has Machine foreign pigment;
Sample is pumped into filter by adsorbent equipment, and by 0.45 μm of filter membrane, it is mechanical miscellaneous more than 0.45 μm to remove particle diameter Matter.
According to specific embodiments of the present invention, in sample handling procedure of the invention, per 20ml fracturing fluid recovery (backflow) liquid samples Product, the hydrogen peroxide of the preferred concentration of 100ml 30% of 80~120ml is added, can be in normal temperature and pressure or appropriate rising pressure environment, simultaneously Holding reacts 5-7min under conditions of being passed through nitrogen, makes sample and H2O2Fully reaction resolution.
It is the pressure with 0.25~0.35MPa in sample handling procedure of the invention according to specific embodiments of the present invention Power is passed through nitrogen into digestion instrument.The time that is continually fed into of nitrogen should include sample and H2O2The whole process fully reacted, this It is 10~25min to be preferably continually fed into nitrogen in invention.The experimental study of inventor proves, with the pressure to digestion instrument In be passed through N2Contained part O in water can be removed2And certain protective effect can be played to the tracer complex compound in sample.
According to specific embodiments of the present invention, in sample handling procedure of the invention, the adsorbing medium is inhaled for macropore The mixture of attached resin and activated carbon.More specifically, the macroporous absorbent resin can include macroporous cross-linked polystyrene suction Attached resin and/or acrylic resin.These resins are commercially available, can be modified or not modified macroporous absorption trees Fat.
According to specific embodiments of the present invention, in sample handling procedure of the invention, the activated carbon is 2~20 purposes The activated carbon of activated carbon, preferably 4~14 mesh.
According to specific embodiments of the present invention, in sample handling procedure of the invention, the macroporous absorbent resin and work Property filling mass ratio of the charcoal in adsorbent equipment be 4~5:5~4.More specifically, the macroporous absorbent resin can with activated carbon To be loaded into adsorbent equipment or be layered section and be loaded into adsorbent equipment after mixing.
It is appreciated that in the sample handling procedure of the present invention, the loadings of the adsorbing medium can be held according to adsorbent equipment Depending on amount and pending liquid measure.
Method of the invention, it is after using ICP-MS detection process in step (2) according to specific embodiments of the present invention Fracturing fluid recovery (backflow) liquid in tracer goods and materials concentration.
According to specific embodiments of the present invention, method of the invention, monitoring accumulation tracer is also included in step (2) Measure and return isostere product.
The pressure break situation that the method for the present invention judges is intuitively accurate, and can quantify, and error is small, to the pressure break work of same interval Work has important directive function, for the situation optimizing design scheme of Different Strata, improves pressure break efficiency, reduces cost.Every layer Go out liquid situation to production in the future and important first-hand data, can determine main extraction layer.
Brief description of the drawings
Fig. 1 is the structural representation of fracturing fluid recovery (backflow) liquid sample processing device used in method of the invention.
Embodiment
The implementation of technical solution of the present invention and possessed beneficial effect are described in detail below by way of specific embodiment, but not Can regard as to the present invention can practical range any restriction.
Embodiment 1
1st, sample:Fracturing outlet liquid is directly taken from the sample tap of oil well.
2nd, sample treatment:
Shown in Figure 1, fracturing fluid recovery (backflow) liquid sample processing device of the invention includes the resolution concatenated by pipeline Device 1, adsorbent equipment 2 and filter 3.Digestion instrument 1 is provided with injection port 11, H2O2Import, N2It is passed through mouth 12 and deflates Mouthfuls 13, the first valve 12 is provided with the pipeline between digestion instrument 1 and adsorbent equipment 2, in adsorbent equipment 2 and filter The second valve 23 is provided with pipeline between 3, and filter 3 sets 0.45 μm of filter membrane 31, is additionally provided with tap hole, tap hole Place sets the 3rd valve 33, and filter is also configured with vacuum extractor (vavuum pump) 32.
When being handled using the device of the present embodiment fracturing fluid recovery (backflow) liquid sample, it can be carried out according to following operation:
20mL samples are added into digestion instrument by injection port, by H2O2Mouth adds the H of the concentration of 100mL 30%2O2, together When do not stop to be passed through N in a device with 0.3MPa pressure2(logical N2Shi Changyue 20min), reacting 5-7min at normal temperatures and pressures makes sample With H2O2Fully reaction resolution;
The first valve, the second valve are opened, opens vavuum pump pumping, sample after resolution is pumped into the suction equipped with mixed fillers Adsorption device, using commercially available macroporous cross-linked polystyrene polymeric adsorbent and activated carbon (4-14 mesh) according to quality in adsorbent equipment Than 5:4 mixing and absorption filler 20mL is as adsorbing medium;Sample solution after resolution organic has by being removed in adsorbent equipment Colored foreign;
Sample is pumped into filter by adsorbent equipment, and by 0.45 μm of filter membrane, it is mechanical miscellaneous more than 0.45 μm to remove particle diameter Matter.
After sample all by filter membrane after, open the 3rd valve, sample will be handled well and released by tap hole, complete whole Pretreatment process.
In the case where being not connected to digestion instrument and adsorbent equipment (fracturing fluid recovery (backflow) liquid only passes through filter), measure pressure Split the rate of recovery data such as following table that liquid returns slight trace agent in discharge opeing:
Tracer element Nd Sm Dy Yb
The rate of recovery, % 82 83 83 85
In the case where only connecting the digestion instrument and filter of the present invention, slight trace in fracturing fluid recovery (backflow) liquid is determined The rate of recovery data such as following table of agent:
Tracer element Nd Sm Dy Yb
The rate of recovery, % 92 91 92 93
In the case of the digestion instrument and adsorbent equipment and filter that connect the present invention at the same time, fracturing fluid recovery (backflow) is determined The rate of recovery data such as following table of slight trace agent in liquid:
Tracer element Nd Sm Dy Yb
The rate of recovery, % 96 96 97 97
Device of the invention effectively can carry out pre-treatment to fracturing fluid recovery (backflow) liquid sample as can be seen here, be allowed to meet in next step The requirement of Instrumental Analysis.
It is some test datas of the present invention in research process below, wherein in addition to especially dated condition, other The same above-described embodiment of part.
(1) it is passed through nitrogen and is not passed through the part test of nitrogen
In the case where not being passed through nitrogen, the rate of recovery data such as following table of slight trace agent in fracturing fluid recovery (backflow) liquid is determined:
Tracer element Nd Sm Dy Yb
The rate of recovery, % 95 96 95 96
In the case where being passed through nitrogen 15min with 0.35MPa pressure, time of slight trace agent in fracturing fluid recovery (backflow) liquid is determined Yield data such as following table:
Tracer element Nd Sm Dy Yb
The rate of recovery, % 96 96 97 97
It can be seen that being passed through nitrogen removes contained partial oxidation in water, there is certain protection to make to the tracer complex compound in sample With.
(2) part test of different adsorbing mediums
Phenolic resin is used to determine time of slight trace agent in fracturing fluid recovery (backflow) liquid as absorption material in adsorbent equipment Yield data such as following table:
Tracer element Nd Sm Dy Yb
The rate of recovery, % 85 86 85 88
Activated alumina is used to determine slight trace agent in fracturing fluid recovery (backflow) liquid as absorption material in adsorbent equipment Rate of recovery data such as following table:
Tracer element Nd Sm Dy Yb
The rate of recovery, % 87 85 87 88
Acrylic acid series macroporous absorbent resin (the prosperous smooth board tree of the prosperous photoinitiator chemical Co., Ltd in Dacheng County is used in adsorbent equipment Fat D113 types) and the mixing and absorption of activated carbon (Zhengzhou bamboo grove activated carbon development corporation, Ltd., oil absorbent activated carbon, 4-14 mesh) fill out Material is used as adsorbing medium, both ratios 4:5, determine the rate of recovery data such as following table of slight trace agent in fracturing fluid recovery (backflow) liquid:
Tracer element Nd Sm Dy Yb
The rate of recovery, % 96 96 97 97
It can be seen that the mixing and absorption filler of macroporous cross-linked polystyrene type polymeric adsorbent and activated carbon is suitable for the present invention's The filler of fracturing fluid recovery (backflow) liquid processing.
In addition, in above-mentioned experiment, mixing and absorption medium 20mL of the invention, can recycle, with per treatment 20~ 50mL fracturing fluid recovery (backflow) liquid sample calculates, and can handle 50~150 times, slight trace agent in each experiment gained fracturing fluid recovery (backflow) liquid The basic indifference of the rate of recovery.
3rd, in the fracturing fluid recovery (backflow) liquid after ICP-MS detection process the concentration of tracer goods and materials experimental procedure:
(1) Ar atmospheric pressures are adjusted to 0.6MPa, start shooting ICP-MS analysis precisions debugging to analysis testing requirements:Machine is taken out very Sky, vacuum is set to reach instrument inspection requirements;The sample lifting time is set as 15-20s;Analytical element is tracer rare earth element; Scanning times are set as 3;Method is set as that total quality scans;Editor's sample message simultaneously sets standard liquid concentration;Instrument igniting is by carrying Show carry out sample analysis.(distinct device parameter is different.)
(2) concentration of tracer goods and materials in the fracturing fluid recovery (backflow) liquid after ICP-MS detection process is accurately used.This method is sensitive Degree reaches ppt (10-12) order of magnitude.
4th, according to the concentration of probe material, or the amount of tracer is further accumulated according to monitoring and returns isostere volume data, commented The fracturing effect of every layer of valency.The prior art that specific evaluation refers to art is carried out.

Claims (7)

1. probe material is to evaluate the method for fracturing effect in a kind of analysis multistage fracturing fluid recovery (backflow) liquid, the method comprising the steps of:
(1) sampled in producing well and carry out sample treatment;
(2) concentration for returning various probe materials in discharge fracturing fluid after detection process;
(3) according to the concentration of probe material, the fracturing effect of every layer of evaluation;
Wherein, the sample handling procedure is to utilize a kind of fracturing fluid recovery (backflow) liquid sample processing device, and the device includes passing through pipe Digestion instrument, adsorbent equipment and the filter of road concatenation;Digestion instrument is the container of accommodating fracturing fluid recovery (backflow) liquid sample, thereon Portion is provided with injection port, H2O2Import, N2It is passed through mouth and gas vent;Inlet is set at the top of adsorbent equipment, and bottom sets out liquid Mouthful, adsorbing medium is filled with adsorbent equipment, the adsorbing medium includes macroporous absorbent resin and activated carbon;At the top of filter Inlet is set, and bottom is provided with tap hole, and medium position sets 0.45 μm of filter membrane in filter, and filter membrane top is liquid to be filtered Body space, bottom is filtered fluid space, and filter is also configured with vacuum extractor, for filter membrane bottom to be vacuumized And provide filtering power;The first valve is provided with pipeline between digestion instrument and adsorbent equipment;In adsorbent equipment and mistake The second valve is provided with pipeline between filter device;3rd valve is set at the tap hole of filter;
The fracturing fluid recovery (backflow) liquid sample treatment includes:
Sample is added into digestion instrument by injection port, by H2O2Import adds H2O2, per 20ml fracturing fluid recovery (backflow) liquid samples, add Enter the hydrogen peroxide of the concentration of 80~120ml 30%, and by N2It is passed through mouth and nitrogen is continually fed into sample, is kept in normal temperature and pressure It is passed through under conditions of nitrogen and reacts 5~7min, makes sample and H2O2Fully reaction resolution;Wherein, it is with 0.25~0.35MPa Pressure is passed through nitrogen into digestion instrument;
The first valve, the second valve are opened, opens vavuum pump pumping, sample after resolution is pumped into adsorbent equipment, removing is organic to be had Colored foreign;
Sample is pumped into filter by adsorbent equipment, by 0.45 μm of filter membrane, removes mechanical admixture of the particle diameter more than 0.45 μm.
2. according to the method for claim 1, wherein, the sample handling procedure includes:By clearing up, adsorbing, cross and filter out The impurity interfered to Instrument measuring is removed, is eluted.
3. according to the method for claim 1, wherein, the macroporous absorbent resin includes macroporous cross-linked polystyrene absorption tree Fat and/or acrylic resin;The activated carbon is the activated carbon of 2~20 mesh.
4. the method according to claim 11, wherein, the macroporous absorbent resin and filling of the activated carbon in adsorbent equipment Mass ratio is 4~5:5~4.
5. according to the method for claim 1, wherein, the macroporous absorbent resin is loaded or divided after being mixed with activated carbon Interval is loaded into adsorbent equipment.
6. according to the method for claim 1, wherein, in step (2) returned with the fracturing fluid after ICP-MS detection process The concentration of tracer goods and materials in discharge opeing.
7. according to the method for claim 1, wherein, the amount of monitoring accumulation tracer is also included in step (2) and returns isostere Product.
CN201410850962.6A 2014-12-31 2014-12-31 Probe material is to evaluate the method for fracturing effect in analysis multistage fracturing fluid recovery (backflow) liquid Active CN104500047B (en)

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Publication number Priority date Publication date Assignee Title
CN108009716B (en) * 2017-11-28 2020-06-30 西南石油大学 Multi-level evaluation method for influence factors of horizontal well volume fracturing effect
RU2749223C1 (en) * 2020-03-27 2021-06-07 Общество с ограниченной ответственностью «ГеоСплит» Method of qualitative and quantitative estimation of downhole gas inflows in multistage hydraulic fracturing in a multiphase flow system

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GB2396412B (en) * 2002-11-27 2005-12-14 Schlumberger Holdings Assessing downhole wbm-contaminated connate water
CN1566000A (en) * 2003-06-27 2005-01-19 天津大港油田集团石油工程有限责任公司 Treatment method and equipment for fracturing flowback waste water
CN1887752A (en) * 2006-07-03 2007-01-03 濮阳市天地人环保工程技术有限公司 Oil field sludge resource treating process
WO2009070050A1 (en) * 2007-11-30 2009-06-04 Schlumberger Holdings Limited Method for monitoring the operation of an oil well using hydraulic fracturing technics
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