CN105527379A - Three-hole rock core kettle and ultra-low-permeability reservoir fluid damage evaluation test apparatus and method - Google Patents
Three-hole rock core kettle and ultra-low-permeability reservoir fluid damage evaluation test apparatus and method Download PDFInfo
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- 239000011435 rock Substances 0.000 title claims abstract description 144
- 239000012530 fluid Substances 0.000 title claims abstract description 118
- 238000012360 testing method Methods 0.000 title claims abstract description 63
- 230000006378 damage Effects 0.000 title claims abstract description 30
- 238000011156 evaluation Methods 0.000 title claims abstract description 26
- 238000000034 method Methods 0.000 title abstract description 16
- 230000015572 biosynthetic process Effects 0.000 claims abstract description 49
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims abstract description 42
- 238000011144 upstream manufacturing Methods 0.000 claims abstract description 35
- 239000007789 gas Substances 0.000 claims abstract description 24
- 229910052757 nitrogen Inorganic materials 0.000 claims abstract description 21
- 230000000694 effects Effects 0.000 claims abstract description 16
- 238000012544 monitoring process Methods 0.000 claims abstract description 6
- 239000007788 liquid Substances 0.000 claims description 100
- 230000035699 permeability Effects 0.000 claims description 53
- 238000004088 simulation Methods 0.000 claims description 34
- 230000000994 depressogenic effect Effects 0.000 claims description 27
- 238000002474 experimental method Methods 0.000 claims description 23
- 239000003822 epoxy resin Substances 0.000 claims description 20
- 229920000647 polyepoxide Polymers 0.000 claims description 20
- 230000001105 regulatory effect Effects 0.000 claims description 17
- 239000005662 Paraffin oil Substances 0.000 claims description 12
- 238000005259 measurement Methods 0.000 claims description 12
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 12
- 238000004891 communication Methods 0.000 claims description 11
- 239000011148 porous material Substances 0.000 claims description 7
- 239000012153 distilled water Substances 0.000 claims description 6
- 239000003292 glue Substances 0.000 claims description 6
- 238000002360 preparation method Methods 0.000 claims description 6
- ZZUFCTLCJUWOSV-UHFFFAOYSA-N furosemide Chemical group C1=C(Cl)C(S(=O)(=O)N)=CC(C(O)=O)=C1NCC1=CC=CO1 ZZUFCTLCJUWOSV-UHFFFAOYSA-N 0.000 claims description 4
- 238000007789 sealing Methods 0.000 claims description 4
- 229910001220 stainless steel Inorganic materials 0.000 claims description 4
- 239000010935 stainless steel Substances 0.000 claims description 4
- 230000001276 controlling effect Effects 0.000 claims description 3
- 230000008878 coupling Effects 0.000 claims description 3
- 238000010168 coupling process Methods 0.000 claims description 3
- 238000005859 coupling reaction Methods 0.000 claims description 3
- 238000009826 distribution Methods 0.000 claims description 3
- 238000011065 in-situ storage Methods 0.000 claims description 3
- 229920000573 polyethylene Polymers 0.000 claims description 3
- 238000000926 separation method Methods 0.000 claims description 3
- 239000011800 void material Substances 0.000 claims description 3
- 239000002699 waste material Substances 0.000 claims description 3
- 239000000463 material Substances 0.000 claims description 2
- 230000005540 biological transmission Effects 0.000 abstract description 5
- 230000003204 osmotic effect Effects 0.000 abstract description 3
- 230000008859 change Effects 0.000 abstract description 2
- 238000011109 contamination Methods 0.000 abstract 1
- 230000035515 penetration Effects 0.000 abstract 1
- 238000010998 test method Methods 0.000 abstract 1
- 238000000502 dialysis Methods 0.000 description 4
- 208000027418 Wounds and injury Diseases 0.000 description 3
- 238000011161 development Methods 0.000 description 3
- 208000014674 injury Diseases 0.000 description 3
- 238000010586 diagram Methods 0.000 description 2
- 238000006073 displacement reaction Methods 0.000 description 2
- 231100000053 low toxicity Toxicity 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 230000008569 process Effects 0.000 description 2
- 230000009467 reduction Effects 0.000 description 2
- 230000035945 sensitivity Effects 0.000 description 2
- 229910000831 Steel Inorganic materials 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- -1 acrylic compounds Chemical class 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000013461 design Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- LNEPOXFFQSENCJ-UHFFFAOYSA-N haloperidol Chemical compound C1CC(O)(C=2C=CC(Cl)=CC=2)CCN1CCCC(=O)C1=CC=C(F)C=C1 LNEPOXFFQSENCJ-UHFFFAOYSA-N 0.000 description 1
- 239000011159 matrix material Substances 0.000 description 1
- 230000000149 penetrating effect Effects 0.000 description 1
- 239000004417 polycarbonate Substances 0.000 description 1
- 229920000515 polycarbonate Polymers 0.000 description 1
- 238000004321 preservation Methods 0.000 description 1
- 230000003068 static effect Effects 0.000 description 1
- 239000010959 steel Substances 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
Classifications
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N33/00—Investigating or analysing materials by specific methods not covered by groups G01N1/00 - G01N31/00
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N15/00—Investigating characteristics of particles; Investigating permeability, pore-volume or surface-area of porous materials
- G01N15/08—Investigating permeability, pore-volume, or surface area of porous materials
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- General Physics & Mathematics (AREA)
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Abstract
The present invention is a three-hole rock core kettle and an ultra-low-permeability reservoir fluid damage evaluation test apparatus and method, the three-hole rock core kettle takes upper and lower cover bodies for clamping a rock core sample, and the upper and lower cover bodies are respectively provided with through holes communicating rock core sample surface. The ultra-low-permeability reservoir fluid damage evaluation test apparatus includes the three-hole rock core kettle, an upstream simulated formation fluid intermediate vessel, a downstream simulated formation fluid intermediate vessel, a to-be-tested fluid intermediate vessel, a plunger pump, a vacuum pump and a nitrogen bottle; the various components are connected by pipes, and corresponding control valves, gas pressure regulation valves and back-pressure valves are arranged. The ultra-low-permeability reservoir fluid damage evaluation test method is as follows: simulated reservoir fluids with same activity are contacted with upper and lower surfaces of the rack core sample, meanwhile the simulated reservoir fluid continuously flows on the upper surface of the simulated reservoir fluid, osmotic pressure transmission is eliminated, and by monitoring of the change with time of downstream fluid pressure, penetration rates of the sample before and after contamination can be obtained, and further damage degree can be evaluated. The three-hole rock core kettle is simple in structure, the test apparatus and method are easy to use, the test pressure is reduced, and experimental data is reliable.
Description
Technical field
The invention relates to a kind of oil and gas reservoir damage assessment technique, particularly relate to a kind of three hole rock core stills, Oil in Super-low Permeability Reservoirs liquid damage evaluation experimental provision and method.
Background technology
At present, hypotonic in explored oil and gas reserves, special hypotonic reserves account for the ratio of about 2/3rds, and hypotonic, Oil in Super-low Permeability reserves will be the exploratory development emphasis that China's oil output is taken over, and are also difficult points.In exploratory development production run, hypotonic, Oil in Super-low Permeability Reservoirs is more prone to come to harm in production operation process than the middle and high reservoir that oozes, and the harmfulness brought after reservoir comes to harm is larger, remove injury also more difficult.So will improve the exploratory development effect of ultra-permeable reservior, the protection work of reservoir is extremely important.The experiment of Oil in Super-low Permeability Reservoirs liquid damage evaluation is basis and the foundation of Oil in Super-low Permeability Reservoirs protection work.
In current Oil in Super-low Permeability Reservoirs liquid damage evaluation, people also just follow conventional lines the SY/T5358-2010 " reservoir sensitivity flowing experiment evaluation method " of the evaluation method of middle and high permeable reservoir strata, i.e. revision in 2010 simply.Explicitly point out in SY/T5358-2010 standard, this standard is applicable to air permeability and is greater than 1 × 10
-3um
2the sensitivity assessment experimental technique of clastic reservoir rock rock sample, and Oil in Super-low Permeability Reservoirs perm-plug method is generally lower than 1 × 10
-3um
2, adopt above-mentioned evaluation method to have following problem: on the one hand, need very high displacement pressure reduction and very long flow speed stability time, very high to equipment requirement, with permeability for 0.1 × 10
-3um
2rock sample is example, and under diameter 2.54 centimetres, length 5 centimetres, flow 1 ml/min, displacing medium are water condition, displacement pressure reduction is more than 16MPa, and the flow velocity basicly stable time needs more than 5 hours.On the other hand, this steady method based on Darcy's law, corresponding permeability is calculated mainly through the flow measured under steady state conditions, current flow metering method affects larger by environment and human factor, for ultra-permeable reservior, steady state flow in experimentation is very low, which in turns increases metering difficulty and error.
In addition, super-low permeability reservoir has certain semi-permeable diaphragm characteristic, namely hydrone and a part of lewis' acid is allowed to pass through, at the certain osmotic pressure of its both sides induced synthesis, existing liquid surveys the impact that permeability method does not consider osmotic pressure usually, and this can increase the error of permeability determination and reservoir damage evaluation result further.
Thus, the present inventor relies on experience and the practice of being engaged in relevant industries for many years, proposes a kind of three hole rock core stills, Oil in Super-low Permeability Reservoirs liquid damage evaluation experimental provision and method, to overcome the defect of prior art.
Summary of the invention
The object of the present invention is to provide a kind of three hole rock core stills, Oil in Super-low Permeability Reservoirs liquid damage evaluation experimental provision and method, can meet the evaluation requirement of working fluid to Oil in Super-low Permeability Reservoirs degree of damage, and test unit is simple, process of the test is simple, test figure is reliable.
The object of the present invention is achieved like this, a kind of three hole rock core stills, and described three hole rock core stills comprise:
Upper cover body, the lower surface of described upper cover body is provided with the first groove, is provided with the first through hole and second through hole of its upper surface through and described first groove in described upper cover body;
Lower cover, the upper surface of described lower cover is provided with depressed part, is provided with the third through-hole of its lower surface through and described depressed part in described lower cover; The bottom surface of described depressed part is provided with the second groove, and described third through-hole is communicated with described second groove;
Core sample, the middle part of described core sample is rock core, and the side wrap of described rock core has epoxy resin; Described core sample to be embedded in described depressed part and with the form fit of described depressed part, the thickness of described core sample is identical with the degree of depth of described depressed part;
The upper surface that the lower surface of described upper cover body is fastened on described lower cover is bolted; The upper surface of described rock core adjoins described first groove; Gap is formed between described first groove and the upper surface of described rock core; The lower surface of described rock core adjoins described second groove, forms lower gap between described second groove and the lower surface of described rock core.
In a better embodiment of the present invention, described rock core is discoid, and described epoxy resin is wrapped in the circumference side of described rock core; Described first groove, described second groove and described depressed part are circle.
In a better embodiment of the present invention, the position that described first through hole lower end is communicated with described first groove is provided with crisscross communication groove, and described communication groove is arranged on the end face of described first groove, and described first through hole is communicated with described communication groove.
In a better embodiment of the present invention, between described epoxy resin and described upper cover body, be equipped with O-ring seal between described epoxy resin and the bottom surface of described depressed part and seal.
In a better embodiment of the present invention, described upper cover body and described lower cover are the cylindrical that stainless steel material is made, and described third through-hole is positioned at the central authorities of described lower cover;
Described upper cover body and described lower cover are provided with the distribution of multiple even circumferential and perforation corresponding to position, and coupling bolt is each passed through described perforation and connects described upper cover body and described lower cover by nut.
Object of the present invention can also realize like this, a kind of Oil in Super-low Permeability Reservoirs liquid damage evaluation experimental provision, described experimental provision comprises described three hole rock core stills, and described experimental provision also comprises upstream simulated formation fluid intermediate receptacle, downstream simulation resident fluid intermediate receptacle and testing liquid intermediate receptacle;
The first end of the first end of described upstream simulated formation fluid intermediate receptacle, described downstream simulation resident fluid intermediate receptacle connects ram pump respectively by pipeline; Described first through hole connects the second end of described upstream simulated formation fluid intermediate receptacle by pipeline; Described third through-hole connects the second end and the vacuum pump of described downstream simulation resident fluid intermediate receptacle by pipeline; Described second through hole connects the described first end of testing liquid intermediate receptacle, the first end of check valve and vacuum pump by pipeline; Second end of described check valve connects waste liquid cylinder by pipeline; 3rd end of described check valve, the second end of described testing liquid intermediate receptacle connect gas pressure regulating valve by pipeline, and described gas pressure regulating valve connects nitrogen cylinder.
In a better embodiment of the present invention, described third through-hole place is connected with the first pressure unit; Described second through hole is connected with the second pressure unit; The three-terminal link of described check valve has the 3rd pressure unit.
In a better embodiment of the present invention, described three hole rock core stills, described upstream simulated formation fluid intermediate receptacle, described downstream simulation resident fluid intermediate receptacle and described testing liquid intermediate receptacle are all arranged in constant temperature oven.
In a better embodiment of the present invention, described upstream simulated formation fluid intermediate receptacle comprises a cylindrical shell, piston is provided with in described cylindrical shell, the interior separation of described cylindrical shell is become the first chamber and the second chamber by described piston, described first chamber is positioned at first end, and described second chamber is positioned at the second end;
Described downstream simulation resident fluid intermediate receptacle is identical with the structure of described upstream simulated formation fluid intermediate receptacle with the structure of described testing liquid intermediate receptacle.
In a better embodiment of the present invention, pipeline described in each is provided with the operation valve controlling this respective line break-make.
Object of the present invention can also realize like this, a kind of experimental technique adopting described Oil in Super-low Permeability Reservoirs liquid damage evaluation experimental provision, and described experimental technique comprises:
S1, prepares described core sample, and the simulated formation fluid that preparation is identical with original void fluid activity;
S2, loads described three hole rock core stills by the described core sample prepared, and by the pipeline connection between described vacuum pump and described third through-hole, described second through hole, remaining connecting line is all closed; Start described vacuum pump evacuation;
S3, by the pipeline connection between described ram pump, described downstream simulation resident fluid intermediate receptacle and described third through-hole, remaining connecting line is all closed; Described ram pump injects working fluid with set pressure to described third through-hole, and pressure stability postscript is downstream original pressure P
0; P
0should be identical with rock sample in-situ pore pressure;
S4, by the pipeline connection between described ram pump, described upstream simulated formation fluid intermediate receptacle, described first through hole and described second through hole, described check valve, described gas pressure regulating valve, described nitrogen cylinder, remaining connecting line is all closed; Described simulated formation fluid is made to continue flowing at described rock core upper surface, continuously the pressure of the described rock core lower surface of monitoring, until the pressure of described rock core lower surface equals the pressure of described rock core upper surface; Utilize the relation between each pressure to calculate the first liquid and survey permeability k
1;
S5, by the pipeline connection between described second through hole, described testing liquid intermediate receptacle, described gas pressure regulating valve and described nitrogen cylinder, remaining connecting line is all closed; Regulate the set pressure of described gas pressure regulating valve to be 4.5MPa, at this pressure the testing liquid in described testing liquid intermediate receptacle be pushed into the upper surface of described rock core and continue 5 hours;
S6, duplicate measurements first liquid surveys permeability k
1step S3 to step S4, record described rock core and surveyed permeability k by the second liquid after described testing liquid pollutes
2; Permeability k is surveyed by the first liquid
1permeability k is surveyed with the second liquid
2value calculate the loss ratio λ of described testing liquid to described rock core
d.
In a better embodiment of the present invention, prepare described core sample in step S1 and comprise the following steps:
The first step, also wraps up rock core Polythene Bag at once at wellhead rock core, is put in sealing bucket and preserves;
Second step, is put in paraffin oil by described rock core, then drills through with rig and paraffin oil the core column that diameter is 2 inches, length is 4 inches;
3rd step, fully mixes epoxide-resin glue and rigidizer in 1:1 ratio, then pours that external diameter is 2.5 inches, internal diameter is 2.125 inches, length is in the heat resistant plastice pipe of 8 inches into;
4th step, puts into described heat resistant plastice pipe by described core column, and makes described core column be placed in described heat resistant plastice tube hub, leaves standstill 24 hours;
5th step, is placed in baking oven by described core column and described heat resistant plastice pipe, heats 1 hour under 110 DEG C of conditions;
6th step, makes described core sample with annular saw and paraffin oil by the thin slice that the described core column of parcel epoxide-resin glue is cut to 0.25 inch, described core sample is placed in paraffin oil and preserves.
In a better embodiment of the present invention, in step sl, testing original hole fluid water activity is 0.85, and the simulation reservoir fluid KCl solution that preparation is identical with original pore fluid activity.
In a better embodiment of the present invention, be used for filling in the first chamber of described upstream simulated formation fluid intermediate receptacle and described downstream simulation resident fluid intermediate receptacle transmitting simulated formation fluid described in filling in the distilled water of described ram pump driving force, the second chamber;
Filling in testing liquid, the second chamber described in filling in first chamber of described testing liquid intermediate receptacle is used for the nitrogen transmitting described nitrogen cylinder driving force.
In a better embodiment of the present invention, controlled connection and the closedown of respective line by described operation valve.
In a better embodiment of the present invention, by downstream original pressure P described in described first pressure transmitter measurement in step S3
0; The pressure of the upper surface of rock core described in step S4 is flowing pressure P
m, described check valve pressure be back pressure P
b, described rock core lower surface pressure be P (l, t), P
mbe greater than P
b; P
mby described second pressure transmitter measurement, P
bby described 3rd pressure transmitter measurement; P (l, t) is by described first pressure transmitter measurement; Calculate described first liquid and survey permeability k
1formula be:
Wherein: the viscosity of μ-fluid, mPas;
β-hydrostatic compressibility, MPa
-1;
V-rock core lower end enclosed fluid volume (supposing that upper end fluid volume is infinitely great), cm
3;
L-rock core length, cm;
The cross-sectional area of A-rock core, cm
2;
The Δ t-mistiming, s;
P (l, t)-rock sample lower end t pressure, MPa.
In a better embodiment of the present invention, calculate described second liquid in step S6 and survey permeability k
2formula and step S4 in calculate described first liquid and survey permeability k
1formula identical, variable P wherein
0, P
m, P (l, t) corresponding be value measured after described rock core is polluted by testing liquid.
In a better embodiment of the present invention, calculate the loss ratio λ of described rock core
dformula be:
From the above mentioned, three hole rock core still structures of the present invention are simple, experimental provision is easy to use, by the simulated formation fluid making core sample upper and lower surface contact identical activity, and fluid continues flowing to eliminate the transmission of dialysis pressure at upper surface, to make only there is hydraulic pressure transmission between core sample upstream and downstream, and then monitoring downstream liquid pressure over time.This experimental technique significantly reduces test pressure, and eliminates dialysis pressure, and experimental data is reliable, therefore is specially adapted to Oil in Super-low Permeability Reservoirs liquid damage evaluation, for such reservoir working fluid preferably provides foundation.
Accompanying drawing explanation
The following drawings is only intended to schematically illustrate the present invention and explain, not delimit the scope of the invention.Wherein:
Fig. 1: be the structural representation of the present invention three hole rock core still.
Fig. 2: be the upward view of upper cover body in the rock core still of the present invention three hole.
Fig. 3: be the cut-open view in A-A cross section in Fig. 2.
Fig. 4: be the partial enlarged drawing at I place in Fig. 2.
Fig. 5: be the partial enlarged drawing at II place in Fig. 3.
Fig. 6: be the vertical view of lower cover in the rock core still of the present invention three hole.
Fig. 7: be the cut-open view in B-B cross section in Fig. 6.
The partial enlarged drawing at III place in Fig. 8: Fig. 7.
Fig. 9: be the structural representation of core sample in the rock core still of the present invention three hole.
Figure 10: be the cut-open view in C-C cross section in Fig. 9.
Figure 11: be the structural representation of experimental provision of the present invention.
Figure 12: be the variation diagram of the contaminated front rock core downstream pressure of rock core in experimental technique of the present invention and rock core upstream pressure.
Figure 13: be the variation diagram of the contaminated rear rock core downstream pressure of rock core in experimental technique of the present invention and rock core upstream pressure.
Embodiment
In order to there be understanding clearly to technical characteristic of the present invention, object and effect, now contrast accompanying drawing and the specific embodiment of the present invention is described.
Embodiment 1
As shown in Figure 1, the invention provides a kind of three hole rock core stills 100, be used for being clamped in by core sample wherein to test, three hole rock core stills 100 comprise upper cover body 10, lower cover 20, core sample 30.Upper cover body 10 is the right cylinder adopting stainless steel to make, and the diameter of upper cover body 10 is 3.86 inches, thickness is 1.25 inches.As shown in Fig. 2, Fig. 3, Fig. 4 and Fig. 5, the lower surface of upper cover body 10 is provided with the first circular groove 101, first groove 101 is positioned at the center position of upper cover body 10, is provided with the first through hole 102 and the second through hole 103 of its upper surface through and the first groove 101 in upper cover body 10.First through hole 102 and the second through hole 103 can be formed by the method for boring in upper cover body 10, and the aperture of the first through hole 102 and the second through hole 103 is 1/16 inch.First through hole 102 and the second through hole 103 are arranged about the Central Symmetry of upper cover body 10.
The right cylinder of lower cover 20 also for adopting stainless steel to make, its diameter is identical with upper cover body 10 with thickness.As shown in Figure 6 and Figure 7, the upper surface of lower cover 20 is provided with circular depressed part 201, and this depressed part 201 is positioned at the center of lower cover 20 upper surface, and the diameter of depressed part 201 is 2.5 inches, the degree of depth is 0.25 inch.This depressed part 201 is for placing core sample 30.The third through-hole 202 penetrating into depressed part 201 from lower surface is provided with in lower cover 20.This third through-hole 202 is positioned at the center of lower cover 20, and its internal diameter is 1/8 inch.As shown in Figure 8, the bottom surface of depressed part 201 is provided with the second circular groove 203, and third through-hole 202 is communicated with the second groove 203.
The middle part of core sample 30 is rock core 301, and the side wrap of rock core 301 has epoxy resin 302.Core sample 30 to be embedded in depressed part 201 and with the form fit of depressed part 201, the thickness of core sample 30 is identical with the degree of depth of depressed part 201.As shown in Figure 9 and Figure 10, in this embodiment, rock core 301 is discoid, and epoxy resin 302 is wrapped in the circumference side of rock core 301, thus core sample 30 is also discoid, and the diameter of core sample 30 is 2.5 inches, thickness is 0.25 inch.The upper surface that the lower surface of upper cover body 10 is fastened on lower cover 20 is bolted.Upper cover body 10 and lower cover 20 are provided with the distribution of multiple even circumferential and perforation 40 corresponding to position, and coupling bolt 50 is each passed through perforation 40 and connects upper cover body 10 and lower cover 20 by nut 60.Adjacent first groove 101 of upper surface of rock core 301; Form gap between first groove 101 and the upper surface of rock core 301, the first through hole 102 is communicated with by gap on this with the lower end of the second through hole 103, makes liquid form flowing at the upper surface of rock core 301.The lower surface of rock core 301 is adjacent forms lower gap between second groove 203, second groove 203 and the lower surface of rock core 301.Utilize third through-hole 202 to be passed into by simulated formation fluid in this lower gap to be used for the hydraulic pressure in simulation core 301 downstream.
Further, as shown in Figure 4 and Figure 5, the position that the first through hole 102 lower end is communicated with the first groove 101 is provided with crisscross communication groove 104, and communication groove 104 is arranged on the end face of the first groove 101, and the first through hole 102 is communicated with communication groove 104.This communication groove 104 is arranged in the certain area around the first through hole 102 lower end, its effect is that the simulated formation fluid making to pass into from the first through hole 102 forms liquid at the upper surface of rock core 301, simulated formation fluid is through the upper surface diverging flow of communication groove 104 at rock core 301, and through upper Clearance Flow to the second through hole 103 place, flow out from the second through hole 103.
In order to make core sample 30 better be sealed between upper cover body 10 and lower cover 20, between epoxy resin 302 and upper cover body 10, being equipped with O-ring seal between epoxy resin 302 and the bottom surface of depressed part 201 and sealing.Concrete, the lower surface of upper cover body 10 and the bottom surface of depressed part 201 are equipped with the o-ring groove 71 of a ring shape, and o-ring groove 71 seals contact ring epoxy resins 302 built with O RunddichtringO 70, O RunddichtringO 70 and seals.
Core sample 30 is clamped in centre by upper cover body 10 and lower cover 20 by this three holes rock core still 100, upper cover body 10 is arranged the first through hole 102 and the second through hole 103, and made by the first groove 101 the simulated formation fluid passed into form liquid at the upper surface of rock core 301.The hydraulic pressure in simulation core 301 downstream is used in the lower gap that simulated formation fluid is passed into rock core 301 lower surface place by the third through-hole 202 arranged in lower cover 20, can the original hole seepage state of simulation core 301 objectively, structure is simple, easy to use.
Embodiment 2
Present invention also offers a kind of Oil in Super-low Permeability Reservoirs liquid damage evaluation experimental provision 1000 adopting this three holes rock core still 100, as shown in figure 11, this experimental provision 1000 comprises three hole rock core stills 100, upstream simulated formation fluid intermediate receptacle 200, downstream simulation resident fluid intermediate receptacle 300 and testing liquid intermediate receptacle 400.
The first end of upstream simulated formation fluid intermediate receptacle 200, the first end of downstream simulation resident fluid intermediate receptacle 300 connect ram pump 500 respectively by pipeline, and the pipeline between the first end and ram pump 500 of upstream simulated formation fluid intermediate receptacle 200 is provided with operation valve a1; Pipeline between the first end of downstream simulation resident fluid intermediate receptacle 300 and ram pump 500 is provided with operation valve a2.
First through hole 102 connects the second end of upstream simulated formation fluid intermediate receptacle 200 by pipeline, and the first through hole 102 with the connecting line of upstream simulated formation fluid intermediate receptacle 200 second end are provided with operation valve a3.Third through-hole 202 connects the second end and the vacuum pump 600 of downstream simulation resident fluid intermediate receptacle 300 by pipeline; Pipeline between second end of downstream simulation resident fluid intermediate receptacle 300 and third through-hole 202 is provided with operation valve a4; Pipeline between vacuum pump 600 and third through-hole 202 is provided with operation valve a5.Second through hole 103 connects the first end of testing liquid intermediate receptacle 400, the first end of check valve 700 and vacuum pump 600 by pipeline.Connection control valve a6 on pipeline between second through hole 103 and the first end of testing liquid intermediate receptacle 400; Pipeline between second through hole 103 and the first end of check valve 700 is connected with operation valve a7; Connection control valve a8 on pipeline between second through hole 103 and vacuum pump 600.Second end of check valve 700 connects waste liquid cylinder 800 by pipeline.3rd end of check valve 700, the second end of testing liquid intermediate receptacle 400 connect gas pressure regulating valve 900 by pipeline, and gas pressure regulating valve 900 connects nitrogen cylinder N; Pipeline between 3rd end of check valve 700 and gas pressure regulating valve 900 is provided with operation valve a9; Pipeline between second end of testing liquid intermediate receptacle 400 and gas pressure regulating valve 900 is provided with operation valve a10.Each operation valve is for controlling connection and the closedown of place pipeline.
Further, the pipeline between the second end of downstream simulation resident fluid intermediate receptacle 300 and third through-hole 202 is connected with the first pressure unit R1, and such as the first pressure unit R1 is connected to third through-hole 202 place.Pipeline between the first end of check valve 700 and the second through hole 103 is connected with the second pressure unit R2, and such as the second pressure unit R2 is connected to the second through hole 103 place.Pipeline between 3rd end of check valve 700 and gas pressure regulating valve 900 is connected with the 3rd pressure unit R3, such as the 3rd pressure unit R3 is connected to the 3rd end of check valve 700.Each pressure unit is for testing the force value in its connecting line.
Further, three hole rock core stills 100, upstream simulated formation fluid intermediate receptacle 200, downstream simulation resident fluid intermediate receptacle 300 and testing liquid intermediate receptacle 400 and the associated line between them are arranged on (shown in the dotted line frame in Figure 11) in constant temperature oven TM, and experiment is carried out under the condition of formation temperature.
Wherein, each intermediate receptacle is existing structure, upstream simulated formation fluid intermediate receptacle 200 comprises a steel cylinders, rubber seal piston is provided with in cylindrical shell, the interior separation of cylindrical shell is become the first chamber and the second chamber by piston, the liquid that the first chamber and the second chamber can experimentally need filling different or gas.Piston can slide the size changing the first chamber and the second chamber in cylinder body.First chamber is positioned at first end, and by first end and pipeline connection, the second chamber is positioned at the second end, by the second end and pipeline connection.Downstream simulation resident fluid intermediate receptacle 300 is identical with the structure of upstream simulated formation fluid intermediate receptacle 200 with the structure of testing liquid intermediate receptacle 400.That is, downstream simulation resident fluid intermediate receptacle 300 the first chamber is positioned at first end, the second chamber is positioned at the second end; First chamber of testing liquid intermediate receptacle 400 is positioned at first end, the second chamber is positioned at the second end.
When testing, in the first chamber of the first chamber of upstream simulated formation fluid intermediate receptacle 200 and downstream simulation resident fluid intermediate receptacle 300 filling be distilled water as central fluid, transmitted the driving force of ram pump 500 by distilled water.In second chamber of the second chamber of upstream simulated formation fluid intermediate receptacle 200 and downstream simulation resident fluid intermediate receptacle 300, filling is simulated formation fluid.In first chamber of testing liquid intermediate receptacle 400, filling is testing liquid, in the second chamber filling be nitrogen as central fluid, transmitted the driving force of nitrogen cylinder N by nitrogen.The principle of work of each intermediate receptacle is that drive source (ram pump 500 or nitrogen cylinder N) is moved by central fluid (distilled water or nitrogen) driven plunger, being pushed in the pipeline be connected by driving liquid (simulated formation fluid or testing liquid) of piston opposite side is gone.
This experimental provision uses simple, easy to connect, uses can obtain reliable experimental data in conjunction with three hole rock core stills 100.
Embodiment 3
China somewhere has abundant shale gas resource, and shale reservoir matrix is fine and close, belongs to typical Oil in Super-low Permeability Reservoirs, the exploitation of shale gas resource, needing extensive hydraulic fracturing job to transform reservoir, in order to form complicated volume seam net, intending adopting slippery water fracturing fluid system.For mini-frac liquid is to the extent of injury of this area's shale reservoir, present invention also offers a kind of experimental technique adopting above-mentioned experimental provision 1000, this experimental technique comprises:
S1, prepares the core sample 30 that diameter is 2.5 inches, thickness is 0.25 inch, and the simulated formation fluid that preparation is identical with original void fluid activity.
S2, is loaded three hole rock core stills 100, is connected by all parts by pipeline by the core sample 30 prepared.By the pipeline connection between vacuum pump 600 and third through-hole 202, second through hole 103, remaining connecting line is all closed; Start vacuum pump 600 to vacuumize, the time vacuumized is at least 20 minutes.
S3, by the pipeline connection between ram pump 500, downstream simulation resident fluid intermediate receptacle 300 and third through-hole 202, remaining connecting line is all closed; Ram pump 500 injects working fluid with the pressure of the 0.2MPa of setting to third through-hole 202, and pressure stability postscript is downstream original pressure P
0; P
0should be identical with rock sample in-situ pore pressure, the liquid volume that record injects rock core 301 downstream is V=38.5cm
3.
S4, by the pipeline connection between ram pump 500, upstream simulated formation fluid intermediate receptacle 200, first through hole 102 and the second through hole 103, check valve 700, gas pressure regulating valve 900, nitrogen cylinder N, remaining connecting line is all closed; Simulated formation fluid is made to continue flowing at rock core 301 upper surface, the pressure (or being called rock sample downstream pressure) of continuous monitoring rock core 301 lower surface, until the pressure of rock core 301 lower surface equals the pressure (or being called rock sample upstream pressure) of rock core 301 upper surface, as shown in figure 12; Utilize the relation between each pressure to calculate the first liquid and survey permeability k
1, the k calculated
1=6.48 × 10
-9um
2, the shale permeability range 10 disclosed with article SPE-27496
-6-10
-12um
2match.
S5, by the pipeline connection between the second through hole 103, testing liquid intermediate receptacle 400, gas pressure regulating valve 900 and nitrogen cylinder N, remaining connecting line is all closed; The set pressure of adjustments of gas pressure regulator valve 900 is 4.5MPa, at this pressure the testing liquid in testing liquid intermediate receptacle 400 is pushed into the upper surface of rock core 301 and continues 5 hours, rock core 301 is polluted by testing liquid.
S6, duplicate measurements first liquid surveys permeability k
1time step S3 to step S4, record rock core 301 polluted by testing liquid after second liquid survey permeability k
2; The k that each force value of obtaining calculates is remeasured according to repeating step S3 and step S4
2=2.96 × 10
-9um
2.Permeability k is surveyed at this measurement second liquid
2step in the pressure of rock core 301 lower surface rise until equal the pressure of rock core 301 upper surface gradually, as shown in figure 13; Pass through k
1and k
2value calculate testing liquid to the loss ratio λ of rock core 301
d.
Wherein, connection and the closedown of respective line is controlled by opening and closing operation valve.
Further, the method preparing core sample 30 comprises the following steps:
The first step, at wellhead rock core 301 and at once by rock core 301 thick Polythene Bag parcel, is put into the interior preservation of sealing bucket; Reduce the duration of contact of rock core 301 and air, to protect the water activity of the original pore fluid of rock core 301 inside as far as possible.
Second step, in laboratory, is put in paraffin oil by rock core 301, then drills through with the paraffin oil of rig and low toxicity the core column that diameter is 2 inches, length is 4 inches.
3rd step, fully mixes epoxide-resin glue and rigidizer in 1:1 ratio, then pours that external diameter is 2.5 inches, internal diameter is 2.125 inches, length is in the heat resistant plastice pipe (polycarbonate or acrylic compounds) of 8 inches into.
4th step, puts into heat resistant plastice pipe by core column, and makes core column be placed in heat resistant plastice tube hub, leaves standstill 24 hours.
5th step, is placed in baking oven by core column and heat resistant plastice pipe, heats 1 hour under 110 DEG C of conditions; Detect core column and whether epoxy resin is cementing is integrated.
6th step, cementing be integrated after, with the paraffin oil of annular saw and low toxicity, the thin slice that the core column of parcel epoxide-resin glue is cut to 0.25 inch is made core sample 30, core sample 30 is placed in paraffin oil and preserves.
Further, in step sl, testing original hole fluid water activity is 0.85, and the simulation reservoir fluid KCl solution that preparation is identical with original pore fluid activity, at room temperature (20 DEG C) record this KCl solution viscosity μ is 1mPas, and static compressibility β is 4.5 × 10
-4mPa
-1.
Further, during this experimental technique also comprises upstream simulated formation fluid intermediate receptacle 200 and downstream simulation resident fluid intermediate receptacle 300 the first chamber, filling is used for transmitting filling simulation resident fluid in the distilled water of ram pump 500 driving force, the second chamber; Filling in filling testing liquid, the second chamber in first chamber of testing liquid intermediate receptacle 400 is used for the nitrogen transmitting nitrogen cylinder N driving force.
Further, downstream original pressure P is measured by the first pressure unit R1 in step S3
0; In step S4, the pressure (or being called rock sample upstream pressure) of rock core 301 upper surface is flowing pressure P
m, check valve 700 pressure be back pressure P
b, rock core 301 lower surface pressure (or being called rock sample downstream pressure) be P (l, t), P
mbe greater than P
b; Concrete, P
0=0.2MPa, P
m=2MPa, P
b=1.5MPa; P
mmeasured by the second pressure unit R2, P
bmeasured by the 3rd pressure unit R3; P (l, t) is changing along with the time, is monitored by the first pressure unit R1; Calculate the first liquid and survey permeability k
1formula be:
Wherein: the viscosity of μ-fluid, mPas;
β-hydrostatic compressibility, MPa
-1;
V-rock core lower end enclosed fluid volume (supposing that upper end fluid volume is infinitely great), cm
3;
L-rock core length, cm;
The cross-sectional area of A-rock core, cm
2;
The Δ t-mistiming, s;
P (l, t)-rock sample lower end t pressure, MPa.
Further, calculate the second liquid in step S6 and survey permeability k
2formula with calculate the first liquid survey permeability k
1formula identical, variable P wherein
0, P
m, P (l, t) corresponding be value measured after rock core 301 is polluted by testing liquid.Calculate the loss ratio λ of rock core 301
dformula be:
The simulated formation fluid of this experimental technique by making core sample 30 upper and lower surface contact identical activity, continue flowing by fluid at rock core 301 upper surface and eliminate the transmission of dialysis pressure, to make only there is hydraulic pressure transmission between core sample 30 upstream and downstream, and then monitoring downstream liquid pressure over time, try to achieve the permeability that core sample 30 pollutes front and back, and evaluate the extent of injury of testing liquid to core sample 30 by the change of permeability.This experimental technique significantly reduces test pressure, and eliminates dialysis pressure, and experimental data is reliable, therefore is specially adapted to Oil in Super-low Permeability Reservoirs liquid damage evaluation, for such reservoir working fluid preferably provides foundation.
The foregoing is only the schematic embodiment of the present invention, and be not used to limit scope of the present invention.Any those skilled in the art, equivalent variations done under the prerequisite not departing from design of the present invention and principle and amendment, all should belong to the scope of protection of the invention.
Claims (18)
1. three hole rock core stills, is characterized in that, described three hole rock core stills comprise:
Upper cover body, the lower surface of described upper cover body is provided with the first groove, is provided with the first through hole and second through hole of its upper surface through and described first groove in described upper cover body;
Lower cover, the upper surface of described lower cover is provided with depressed part, is provided with the third through-hole of its lower surface through and described depressed part in described lower cover; The bottom surface of described depressed part is provided with the second groove, and described third through-hole is communicated with described second groove;
Core sample, the middle part of described core sample is rock core, and the side wrap of described rock core has epoxy resin; Described core sample to be embedded in described depressed part and with the form fit of described depressed part, the thickness of described core sample is identical with the degree of depth of described depressed part;
The upper surface that the lower surface of described upper cover body is fastened on described lower cover is bolted; The upper surface of described rock core adjoins described first groove; Gap is formed between described first groove and the upper surface of described rock core; The lower surface of described rock core adjoins described second groove, forms lower gap between described second groove and the lower surface of described rock core.
2. three hole rock core stills as claimed in claim 1, it is characterized in that, described rock core is discoid, and described epoxy resin is wrapped in the circumference side of described rock core; Described first groove, described second groove and described depressed part are circle.
3. three hole rock core stills as claimed in claim 1, it is characterized in that, the position that described first through hole lower end is communicated with described first groove is provided with crisscross communication groove, and described communication groove is arranged on the end face of described first groove, and described first through hole is communicated with described communication groove.
4. three hole rock core stills as claimed in claim 1, is characterized in that, between described epoxy resin and described upper cover body, be equipped with O-ring seal seal between described epoxy resin and the bottom surface of described depressed part.
5. three hole rock core stills as claimed in claim 1 or 2, it is characterized in that, described upper cover body and described lower cover are the cylindrical that stainless steel material is made, and described third through-hole is positioned at the central authorities of described lower cover;
Described upper cover body and described lower cover are provided with the distribution of multiple even circumferential and perforation corresponding to position, and coupling bolt is each passed through described perforation and connects described upper cover body and described lower cover by nut.
6. an Oil in Super-low Permeability Reservoirs liquid damage evaluation experimental provision, it is characterized in that, described experimental provision comprises three hole rock core stills as described in any one of claim 1 to 5, and described experimental provision also comprises upstream simulated formation fluid intermediate receptacle, downstream simulation resident fluid intermediate receptacle and testing liquid intermediate receptacle;
The first end of the first end of described upstream simulated formation fluid intermediate receptacle, described downstream simulation resident fluid intermediate receptacle connects ram pump respectively by pipeline; Described first through hole connects the second end of described upstream simulated formation fluid intermediate receptacle by pipeline; Described third through-hole connects the second end and the vacuum pump of described downstream simulation resident fluid intermediate receptacle by pipeline; Described second through hole connects the described first end of testing liquid intermediate receptacle, the first end of check valve and vacuum pump by pipeline; Second end of described check valve connects waste liquid cylinder by pipeline; 3rd end of described check valve, the second end of described testing liquid intermediate receptacle connect gas pressure regulating valve by pipeline, and described gas pressure regulating valve connects nitrogen cylinder.
7. Oil in Super-low Permeability Reservoirs liquid damage evaluation experimental provision as claimed in claim 6, it is characterized in that, described third through-hole place is connected with the first pressure unit; Described second through hole is connected with the second pressure unit; The three-terminal link of described check valve has the 3rd pressure unit.
8. Oil in Super-low Permeability Reservoirs liquid damage evaluation experimental provision as claimed in claim 6, it is characterized in that, described three hole rock core stills, described upstream simulated formation fluid intermediate receptacle, described downstream simulation resident fluid intermediate receptacle and described testing liquid intermediate receptacle are all arranged in constant temperature oven.
9. the Oil in Super-low Permeability Reservoirs liquid damage evaluation experimental provision as described in claim 6 or 7 or 8, it is characterized in that, described upstream simulated formation fluid intermediate receptacle comprises a cylindrical shell, piston is provided with in described cylindrical shell, the interior separation of described cylindrical shell is become the first chamber and the second chamber by described piston, described first chamber is positioned at first end, and described second chamber is positioned at the second end;
Described downstream simulation resident fluid intermediate receptacle is identical with the structure of described upstream simulated formation fluid intermediate receptacle with the structure of described testing liquid intermediate receptacle.
10. the Oil in Super-low Permeability Reservoirs liquid damage evaluation experimental provision as described in claim 6 or 7 or 8, is characterized in that, pipeline described in each is provided with the operation valve controlling this respective line break-make.
The experimental technique of 11. 1 kinds of employings Oil in Super-low Permeability Reservoirs liquid damage evaluation experimental provision according to any one of claim 6 to 10, it is characterized in that, described experimental technique comprises:
S1, prepares described core sample, and the simulated formation fluid that preparation is identical with original void fluid activity;
S2, loads described three hole rock core stills by the described core sample prepared, and by the pipeline connection between described vacuum pump and described third through-hole, described second through hole, remaining connecting line is all closed; Start described vacuum pump evacuation;
S3, by the pipeline connection between described ram pump, described downstream simulation resident fluid intermediate receptacle and described third through-hole, remaining connecting line is all closed; Described ram pump injects working fluid with set pressure to described third through-hole, and pressure stability postscript is downstream original pressure P
0; P
0should be identical with rock sample in-situ pore pressure;
S4, by the pipeline connection between described ram pump, described upstream simulated formation fluid intermediate receptacle, described first through hole and described second through hole, described check valve, described gas pressure regulating valve, described nitrogen cylinder, remaining connecting line is all closed; Described simulated formation fluid is made to continue flowing at described rock core upper surface, continuously the pressure of the described rock core lower surface of monitoring, until the pressure of described rock core lower surface equals the pressure of described rock core upper surface; Utilize the relation between each pressure to calculate the first liquid and survey permeability k
1;
S5, by the pipeline connection between described second through hole, described testing liquid intermediate receptacle, described gas pressure regulating valve and described nitrogen cylinder, remaining connecting line is all closed; Regulate the set pressure of described gas pressure regulating valve to be 4.5MPa, at this pressure the testing liquid in described testing liquid intermediate receptacle be pushed into the upper surface of described rock core and continue 5 hours;
S6, duplicate measurements first liquid surveys permeability k
1step S3 to step S4, record described rock core and surveyed permeability k by the second liquid after described testing liquid pollutes
2; Permeability k is surveyed by the first liquid
1permeability k is surveyed with the second liquid
2value calculate the loss ratio λ of described testing liquid to described rock core
d.
12. experimental techniques as claimed in claim 11, is characterized in that, prepare described core sample and comprise the following steps in step S1:
The first step, also wraps up rock core Polythene Bag at once at wellhead rock core, is put in sealing bucket and preserves;
Second step, is put in paraffin oil by described rock core, then drills through with rig and paraffin oil the core column that diameter is 2 inches, length is 4 inches;
3rd step, fully mixes epoxide-resin glue and rigidizer in 1:1 ratio, then pours that external diameter is 2.5 inches, internal diameter is 2.125 inches, length is in the heat resistant plastice pipe of 8 inches into;
4th step, puts into described heat resistant plastice pipe by described core column, and makes described core column be placed in described heat resistant plastice tube hub, leaves standstill 24 hours;
5th step, is placed in baking oven by described core column and described heat resistant plastice pipe, heats 1 hour under 110 DEG C of conditions;
6th step, makes described core sample with annular saw and paraffin oil by the thin slice that the described core column of parcel epoxide-resin glue is cut to 0.25 inch, described core sample is placed in paraffin oil and preserves.
13. experimental techniques as claimed in claim 11, is characterized in that, in step sl, testing original hole fluid water activity is 0.85, and the simulation reservoir fluid KCl solution that preparation is identical with original pore fluid activity.
14. experimental techniques as claimed in claim 11, it is characterized in that, be used for filling in the first chamber of described upstream simulated formation fluid intermediate receptacle and described downstream simulation resident fluid intermediate receptacle transmitting simulated formation fluid described in filling in the distilled water of described ram pump driving force, the second chamber;
Filling in testing liquid, the second chamber described in filling in first chamber of described testing liquid intermediate receptacle is used for the nitrogen transmitting described nitrogen cylinder driving force.
15. experimental techniques as claimed in claim 11, be is characterized in that, controlled connection and the closedown of respective line by described operation valve.
16. experimental techniques as claimed in claim 11, is characterized in that, by downstream original pressure P described in described first pressure transmitter measurement in step S3
0; The pressure of the upper surface of rock core described in step S4 is flowing pressure P
m, described check valve pressure be back pressure P
b, described rock core lower surface pressure be P (l, t), P
mbe greater than P
b; P
mby described second pressure transmitter measurement, P
bby described 3rd pressure transmitter measurement; P (l, t) is by described first pressure transmitter measurement; Calculate described first liquid and survey permeability k
1formula be:
Wherein: the viscosity of μ-fluid, mPas;
β-hydrostatic compressibility, MPa
-1;
V-rock core lower end enclosed fluid volume (supposing that upper end fluid volume is infinitely great), cm
3;
L-rock core length, cm;
The cross-sectional area of A-rock core, cm
2;
The Δ t-mistiming, s;
P (l, t)-rock sample lower end t pressure, MPa.
17. experimental techniques as claimed in claim 16, is characterized in that, calculate described second liquid and survey permeability k in step S6
2formula and step S4 in calculate described first liquid and survey permeability k
1formula identical, variable P wherein
0, P
m, P (l, t) corresponding be value measured after described rock core is polluted by testing liquid.
18. experimental techniques according to any one of claim 11 to 17, is characterized in that, calculate the loss ratio λ of described rock core
dformula be:
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