CN1020047C - Method and equipment for clay expansion experiment - Google Patents

Method and equipment for clay expansion experiment Download PDF

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CN1020047C
CN1020047C CN 91104255 CN91104255A CN1020047C CN 1020047 C CN1020047 C CN 1020047C CN 91104255 CN91104255 CN 91104255 CN 91104255 A CN91104255 A CN 91104255A CN 1020047 C CN1020047 C CN 1020047C
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test
clay
cylinder
housed
test tube
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CN1056578A (en
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张建民
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Drilling Technology Int Research Inst Of Petroleum Exploration Development (c
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Drilling Technology Int Research Inst Of Petroleum Exploration Development (c
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Abstract

The present invention relates to a clay swelling test method and a device thereof, which can simulate pressure and infiltrating conditions in drilling wells of petroleum geology. The present invention is the improvement of the existing clay swelling test and is mainly characterized in that the pressure of test liquid in a test cylinder is made to be within the range of 98 to 4400 KPa, and the bottom of a test block is made to be communicated with the atmosphere; test liquid filtered out from the clay test block 5, and simultaneously, the clay swelling degree is calculated by measuring a displacement rod 3. The device is composed of a nitrogen cylinder 18, a test cylinder 2, a heating jacket 9, a dial indicator 11, a recorder 23, a liquid filling cylinder 14 for prepressurization, etc., wherein the liquid filling cylinder 14 is communicated with the test cylinder 2 through a pipeline, and holes communicated with the atmosphere are arranged on the bottom of the test cylinder 2.

Description

Method and equipment for clay expansion experiment
The present invention relates to study the test method and the device thereof of clay performance, more particularly, is a kind of clay swelling test method and the device thereof that can simulate oil geology drilling well borehole pressure and percolation condition.
Description of drawings of the present invention is as follows:
Fig. 1 is people's such as Roehl clay swelling test device and a test routine synoptic diagram;
Fig. 2 is clay swelling test device of the present invention and test routine synoptic diagram;
Fig. 3 is a clay swelling test device experiment tube assembly wiring layout;
Fig. 4 is clay test block expansion curve figure under the different test solution pressure;
Fig. 5 is the curve maps of different polymkeric substance test solutions to clay test block expansion inhibition (R);
Fig. 6 is Na bentonitic clay and the expansion curve of Ca POLARGEL NF test block in different test solutions and the atomic absorption analysis result of test solution.
In oil and geological drilling, the mud shale that the clay mineral of underground hydration swelling is formed is very big to the technology and the quality influence of drilling well, so understand their hydration swelling and the effect and the Evaluation on effect of used clay swelling inhibitor is very important.
At present, when research of hydration and expansion of clay mechanism and the evaluation of clay swelling inhibitor, what often use is the test method of test clay swelling under longitudinal pressure.As September nineteen eighty-two in the 57th petroleum engineer's annual meeting that the U.S. holds, people such as Roehl propose a kind of clay experimental technique and device (No. 11117, the SPE of american petroleum Engineering society collection of thesis), its experimentation is: earlier the sample clay powders is pressed into clay test block 5 in test tube 2, put into constant temperature test solution groove 9 together with test tube 2, put into filter paper 6 more successively, porous disc 27, fluid distributor 40, O-ring seal 29, fluid injection piston 41, add certain longitudinal pressure for clay test block 5 from top to bottom by cylinder 42 then, use peristaltic pump 43 injection test liquid again.Liquid is by gap between porous disc 27 and the fluid distributor 40, on one side to clay test block 5 in naturally osmotic, one side overflows in the constant temperature test solution groove 9 from test tube 2 upper limbs, supplies to recycle.Clay test block 5 hydration swellings upwards promote piston 42, can note the polar expansion value of clay test block 5 by displacement transducer 44, for the usefulness of analysis.
This clay swelling test method, its clay sample are to adopt nature to contact with the way of contact of test solution, have following problem when the clay mineral hydration swelling of estimating the mud shale layer and inhibitor performance thereof:
1. applying a constant longitudinal pressure with piston, to come the liquid press force of dummy activity on mud shale be irrational.Reason is: in fact mud shale all has certain net porosity and permeability, particularly in the anadiagenesis stage, occur smectite to she-deceive people mixed layer clay mineral when changing, its net porosity and permeability all can unusually increase from original downward trend with suddenling change.Therefore, except mud shale itself absorbed water from drilling fluid, under the pressure differential effect between drilling fluid column pressure and the mud shale pore pressure, drilling fluid also can be to the inner diafiltration of mud shale.Permeate this and just do not exist in the clay swelling test under vertical piston pressure, test solution can only lean on clay sample to suck naturally.Vertically piston force is big more, and water enters clay sample inside difficulty all the better, also is difficult to improve even prolong test period.
2. from clay particle stressed, the press force of solid piston formula is different with the liquid press force.Because suffered power P1 is the poor of external force P2 and pore pressure P between the clay particle, that is: P1=P2-P, the expansion of clay under constant solid piston pressure P 2, because be the nature water sucting mode, so when difference expands constantly, its pore pressure P all constant (equal atmospheric pressure, gauge pressure is 0), so P1 is also constant.But for the expansion under the constant fluid pressure, just different, owing to liquid permeates in hole, so pore pressure is changed with depth of penetration, therefore the stressed P1 of clay particle also has corresponding a variation: on same cross section, P1 infiltrates along with the depth of pressure fluid and reduces.And perviousness is good more, and pressure reduces soon more.
3. when the higher polymkeric substance test solution of evaluation test molecular weight, because test solution viscosity is higher, migration velocity is slow, is not easy to go deep into clay sample inside, therefore tests consuming time longer.In addition, polymer molecule easily adsorbs in infiltration plate hole crack, like this, the one, can cause certain obstruction to the duct, prolong test period, the 2nd, consume a part of polymer molecule and influenced test findings.
This shows, condition in the unreasonable simulation real well, just can not obtain clay swelling test and the evaluation result close with actual conditions, particularly be unsuitable for estimating the treating agent that mud shale hole and microfracture are had the shutoff blocking action, as higher polymkeric substance of coating agent, sulfonated gilsonite and molecular weight etc.
The present invention is intended to overcome above-mentioned shortcoming, provides a kind of easier, and condition in the feasible simulation real well is more suitable for a kind of clay swelling test method and the device thereof of petroleum drilling reality.
The present invention is the improvement to above-mentioned clay swelling test, the main program of its test method is: the sample clay powder is added in the test tube 2 earlier, under pressure, make clay test block 5, the feasible simulation conditions down-hole, 2 injection test solutions make clay test block 5 hydration swellings in the test tube under predetermined temperature, the pressure of test solution is 98KPa to 4400KPa in the test tube 2, then, clay test block 5 bottoms are communicated with atmosphere, allow clay test block 5 upper surfaces and lower surface produce pressure differential, the test solution that collection is leached by clay test block 5 is for the usefulness of analysis, simultaneously by the porous platen 4 and displacement bar 3 meters that are placed in the clay test block are calculated the degree of expansion of clay.
The device that is used for above-mentioned clay swelling test method mainly is made up of nitrogen cylinder 18, test tube 2, heating jacket 9, dial gauge 11, registering instrument 23, graduated cylinder 21 etc., what also have precharge between nitrogen cylinder 18 and test tube 2 adds fluid cylinder 14, adding fluid cylinder 14 communicates with test tube 2 usefulness pipelines, valve 12 is housed therebetween, and test tube 2 bottoms have the hole that communicates with atmosphere.
In the above-mentioned clay swelling test device, test tube 2 is made up of top cylinder 28 and doffing 26, in the test tube 2 porous platen 4 is housed, displacement bar 3 is housed on the porous platen 4, fluid skirt 30, feed liquor skirt 31 are equipped with in top cylinder 28 tops, between top cylinder 28 and fluid skirt 35, feed liquor skirt 31, displacement bar 3, doffing 26, O-ring seal 29 is housed all, on doffing 26 bottom through-holes trap valve 8 is housed.
Below in conjunction with accompanying drawing in detail the embodiment of the invention is described in detail: the clay swelling test program is as follows:
1. clay sample crushing screening.For the mud shale sample, cross 160 mesh sieves, cross 100 mesh sieves for bentonitic clay.
2. clay sample was 95 ℃~100 ℃ oven dry 6 hours.
3. test solution is packed into add in the fluid cylinder 14 and seal, add nitrogen pressure predetermined under the simulation well, pressure limit is decided according to the down-hole actual pressure of being simulated, general 3000KPa.
4. set test solution and test tube 2 heating-up temperatures, open test solution heating jacket 9.
5. take off test tube 2 doffings 26, on infiltration plate 7, put two filter paper 6 that diameter is identical with it.Measure its degree of depth with pit gauge.
6. the clay samples that take by weighing 15 ± 0.01 grams are put on the filter paper 6 in the doffing 26 claps gently, presses down 5 minutes at the pressure of 34000KPa, measures its degree of depth with pit gauge again, calculates the thickness and the density of compacting test block.
7. will test tube 2 top cylinders 28 and install with doffing 26 and put into heating jacket 9, connect the feed liquor pipeline.Liquid outlet 35 when doing envelope test need not, so the valve on this pipe adapter 35 should be closed.
8. displacement bar 3 is pushed and make it porous platen 4 and clay test block 5 surperficial contacts.Regulate the zero point of dial gauge 11.Open record device 23 mixes up zero point of instrument.
9. when treating that temperature all reaches predetermined value, open the trap valve 8 of test tube 2 bottoms, clay test block 5 bottoms are communicated with atmosphere, open the valve 12 on the feed liquor skirt 31 then, test solution is pressed in the test tube 2, the beginning of expanding sees through time that clay test block 2 oozes out and speed etc. by polar expansion value, the test solution of dial gauge 11 and registering instrument 23 record clays.
10. test finishes, and unloads test tube 2 etc., cleans stand-by.
This test clay test block relative expansion size is weighed with degree of expansion S%, and test solution is weighed with the R value the inhibition size that expands, and can be calculated as follows:
S%=s/△
S=[S%]-S%
R=S/[S%]
In the formula:
The original depth of △-test block (mm)
S-swell value (mm) constantly
The degree of expansion in [S%]-test block a certain moment in distilled water.
The present invention according to above test method design and produce out a kind of can simulation well in the clay swelling test device of pressure reduction, percolation condition and temperature.
Pressurization partly is made up of nitrogen cylinder 18, reduction valve 17, rain glass 16 gentle pipelines 15.The fluid cylinder 14 that adds in the heating jacket 9 links to each other with tracheae line 15, adding fluid cylinder 14 is common anti-corrosion containers, can add the test solution rear enclosed, its bottom joins by the feed liquor skirt 31 of pipeline with test tube 2, valve 12 is equipped with in the centre, test solution can enter in the test tube 2 under predetermined nitrogen pressure, clay test block this moment 5 just can absorb water and upwards expand, promote porous platen 4, make displacement bar 3 drive dial gauge 11, swell value can be read on dial plate, what dial gauge 11 can be with the standard machinery formula, also can use to have displacement transducer, or only use sensor, as the 0-50mm of Beijing radio 15 factories, if there is the displacement transducer just can be with displacement signal by lead 19 input registering instruments 23, expansion curve writes down and draws.Registering instrument 23 can be selected the common registering instrument that voltage amplification is arranged of general experiment usefulness for use, as: the Shanghai Instruments Factory X-Y recorder.
Test solution finally passes the test block bottom in meeting diafiltration in the hole of clay test block under the effect of pressure, oozes through trap valve 8, is collected by the graduated cylinder on the support 20 21.Filtrate oozes the time and drips a number can pass through drop recorder 22 and registering instrument 23 records, and drop recorder 22 can adopt the principle of power on/off switch to make, also can, and employing manual record.
Test tube 2 is made up of doffing 26 and top cylinder 28, and doffing 26 is connected for the spiral shell mosquito with top cylinder 28, by O-ring seal 29 sealings.Fluid skirt 35 and feed liquor skirt 31 are equipped with in top cylinder 28 tops, can be connected with exterior tubing by pipe adapter.29 are the O-ring seal on importing and exporting.The other end of fluid skirt 35 and feed liquor skirt 31 had been both: 10,25 places, can connect ebullator, and make the test solution band press circulation, artificial ground, generalized case can.Displacement bar 3 bottoms are connected with porous platen 4, and the upper end passes from top cylinder 28 center pits, contact with dial gauge 11.Displacement bar 3 is by O-ring seal 29 sealings, and its sealing elasticity can realize by the dial framework 36 that turn is threaded with top cylinder 28.38 is the dial gauge screw.One powder of stainless steel sintering infiltration plate 7 is housed in the doffing 26, and for supporting clay test block 5 and making filtrate seeing through, its also available porous plate replaces.It in being equipped with on doffing 26 bottom through-holes trap valve 8 of a band O-ring seal 29.
Method of the present invention and test unit be based upon reasonably analyze and the basis of the interior condition of simulation well on, emphasize interior fluid pressure difference, percolation condition and the temperature of simulation well simultaneously, therefore widened the scope that clay swelling test and treating agent are estimated, the gained result also more approaches reality, and matches with practical experience.Following test method can be as the example of real example.
<1〉fluid pressure differential is to the influence of hydration and expansion of clay
Fig. 4 for same shale sample under different test solution pressure differentials expansion curve and leach discharge curve.The initial pore pressure of shale test block is identical with atmosphere in the test, and gauge pressure is zero.The former test solution pressure differential initial value that is added on the shale test block sample also just equals to be added in the pressure (in like manner following) on the test solution.Test solution is a distilled water.As seen raise with difference test solution pressure among the figure, the test solution amount of leaching W also raises, but the degree of expansion S% of shale test block sample descends.This explanation increases pressure reduction by the raising fluid pressure and helps to reduce expansion.This is equivalent to by the proportion that increases drilling fluid fluid column pressure to be raise in the scene and strengthens the chip hold down of fluid column-pore pressure difference to the mud stone borehole wall.
<2〉polymkeric substance is to the inhibition evaluation test of hydration and expansion of clay
Fig. 5 is the R value curve that 6 kinds of polymer solutions are estimated the bentonite inflated inhibition of Na.Test solution concentration is 0.5%, pressure 14Kg/cm, and 21.1 ℃ of temperature, PH is that other are 8.5 9.5 except that HPAN.Visible these polymkeric substance to the size sequence of clay swelling inhibition are among the figure: NH4PAN>KPHP>Drispac>CPA 〉=PHP, both: ammonium polyacrylonitrile>hydrolysed polyacrylic potassium>polyanion cellulose>calcium polyacrylate (CPA) 〉=hydro-polyacrylamide.The conclusion of this result and theoretical analysis and on-site experience matches.
<3〉the cation exchange test in the clay swelling process
Clay is in the hydration swelling process, and the kation of its surface adsorption can exchange with the kation in the solution, and different exchange cations is also different to the influence of clay swelling.Utilize this test unit to have the characteristics of leak-off function, can collect the test filtrate that sees through the clay test block in the expansion process and analyze, the relation of research clay swelling and cation exchange.Test as shown in Figure 6.Earlier carry out bloating test with 5% Kcl solution, it is in a basic balance and allow the solution filter that is added use up until degree of expansion S% to collect filter liquor simultaneously, then adds second kind of solution again, adds 5%NaCl for the Na bentonitic clay, adds 5%CaCl for the Ca bentonitic clay 2Collect filter liquor in the same way and go into the distilled water test to the greatest extent more in addition until filter.Ca, Mg, K, the atomic absorption method assay determination of Na ion concentration in the filtrate.Measure the dool lattice spacing of clay test block sample after the off-test with X-ray diffraction.
As seen from Figure 6, in the Kcl of phase one solution trial, for the Na bentonitic clay, the Na ion that is come out by K ion-exchange is 15100ppm, is Ca13350ppm and Mg1420ppm for the Ca bentonitic clay.In the test in second step, the Na bentonitic clay is after the effect of experience 5%NaCl, and S% has a bit slightly to be increased, and the K ion is come out by Na ion-exchange again, is 9840ppm.For the Ca bentonitic clay, at 5%CaCl 2Effect under, its result is also similar, but the K ion that is gone out by Ca ion-exchange is more relatively, is 118400.The degree of expansion S% of two kinds of soil increases greatly after the phase III adds distilled water.Last X-ray measurement result, its dool value is 19.64A.
Can find that from this test the K ion after exchange absorption enters in the clay, still can be come out by other ion-exchange, and also bigger expansion can take place when meeting distilled water.Therefore hardly thereby it was once in vogue for a time when the inhibition mechanism of explanation K ion pair clay swelling to make clay almost no longer expand this " iron chains embedding " viewpoint in the full hexagonal ring that embeds clay lattice after other ion-exchanges in K ion and the clay in the actual well drilled.

Claims (3)

1, a kind of clay swelling test method, its main program is: earlier the sample clay powder is added in the test tube, make the clay test block under pressure; Under predetermined temperature, in the test tube, inject test solution and make clay test block imbibition; By base plate in the clay test block and displacement bar are measured the degree of expansion that compute goes out clay, it is characterized in that: the pressure that makes above-mentioned test solution in test tube is 98KPa to 4400KPa; Clay test block bottom is communicated with atmosphere; The test solution that collection is leached by the clay test block.
2, a kind of device that is used for above-mentioned clay swelling test method, mainly forms, it is characterized in that by nitrogen cylinder 18, test tube 2, heating jacket 9, dial gauge 11, registering instrument 23, graduated cylinder 21: nitrogen cylinder 18 with test precharge also is housed between tins 2 add fluid cylinder 14; Add fluid cylinder 14 and communicate, valve 12 is housed therebetween with test tube 2 usefulness pipelines; Test tube 2 is made up of top cylinder 28 and doffing 26, and feed liquor skirt 31 is equipped with at top cylinder 28 tops; In the test tube 2 porous platen 4 is housed, displacement bar 3 is housed on the porous platen 4, the bottom has the hole that communicates with atmosphere.
3, according to claim 2 or 3 described clay swelling test devices, it is characterized in that: between top cylinder 28 and feed liquor skirt 31, displacement bar 3, doffing 26, O-ring seal 29 is housed all; On doffing 26 bottom through-holes trap valve 8 is housed.
CN 91104255 1991-06-29 1991-06-29 Method and equipment for clay expansion experiment Expired - Fee Related CN1020047C (en)

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