CN112881265B - Quantitative in-situ evaluation method for pore connectivity in well cementation cement slurry solidification process - Google Patents
Quantitative in-situ evaluation method for pore connectivity in well cementation cement slurry solidification process Download PDFInfo
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- 239000004568 cement Substances 0.000 title claims abstract description 135
- 239000002002 slurry Substances 0.000 title claims abstract description 122
- 239000011148 porous material Substances 0.000 title claims abstract description 54
- 238000000034 method Methods 0.000 title claims abstract description 28
- 230000008569 process Effects 0.000 title claims abstract description 17
- 238000011065 in-situ storage Methods 0.000 title claims abstract description 16
- 238000007711 solidification Methods 0.000 title claims abstract description 13
- 230000008023 solidification Effects 0.000 title claims abstract description 13
- 238000011156 evaluation Methods 0.000 title claims abstract description 10
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 15
- 230000015572 biosynthetic process Effects 0.000 claims abstract description 10
- 238000012360 testing method Methods 0.000 claims abstract description 10
- 230000005415 magnetization Effects 0.000 claims abstract description 7
- 238000005481 NMR spectroscopy Methods 0.000 claims abstract description 5
- 230000036571 hydration Effects 0.000 claims description 21
- 238000006703 hydration reaction Methods 0.000 claims description 21
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 14
- 229910052757 nitrogen Inorganic materials 0.000 claims description 7
- 230000001939 inductive effect Effects 0.000 claims description 4
- 230000006698 induction Effects 0.000 claims description 2
- 239000002245 particle Substances 0.000 claims description 2
- 230000018044 dehydration Effects 0.000 claims 1
- 238000006297 dehydration reaction Methods 0.000 claims 1
- 239000007789 gas Substances 0.000 abstract description 11
- 230000005465 channeling Effects 0.000 abstract description 7
- 238000005516 engineering process Methods 0.000 abstract description 7
- 239000000463 material Substances 0.000 abstract description 5
- 230000007246 mechanism Effects 0.000 abstract description 4
- 238000011158 quantitative evaluation Methods 0.000 abstract description 2
- 125000004435 hydrogen atom Chemical group [H]* 0.000 abstract 1
- 230000002265 prevention Effects 0.000 abstract 1
- 230000001965 increasing effect Effects 0.000 description 6
- 239000012530 fluid Substances 0.000 description 4
- QSHDDOUJBYECFT-UHFFFAOYSA-N mercury Chemical compound [Hg] QSHDDOUJBYECFT-UHFFFAOYSA-N 0.000 description 4
- 229910052753 mercury Inorganic materials 0.000 description 4
- 238000011160 research Methods 0.000 description 4
- 238000001179 sorption measurement Methods 0.000 description 4
- 230000001186 cumulative effect Effects 0.000 description 3
- 238000005070 sampling Methods 0.000 description 3
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- 230000008859 change Effects 0.000 description 2
- 239000003795 chemical substances by application Substances 0.000 description 2
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- QAOWNCQODCNURD-UHFFFAOYSA-L Sulfate Chemical compound [O-]S([O-])(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-L 0.000 description 1
- 239000000654 additive Substances 0.000 description 1
- 230000000996 additive effect Effects 0.000 description 1
- 238000004364 calculation method Methods 0.000 description 1
- 238000010835 comparative analysis Methods 0.000 description 1
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Abstract
The invention discloses a quantitative in-situ evaluation method for pore connectivity in a well cementation cement slurry solidification process, which comprises the following steps: determining a formation factor of cement slurry by testing the resistivity of the well cementation cement slurry and the resistivity of a cement slurry pore solution in situ; the low-field nuclear magnetic resonance technology is applied to the in-situ test of the transverse relaxation time and magnetization intensity signals of the hydrogen protons in the pore water, so that the porosity of the cement paste can be calculated; and finally, based on the formation factor and the porosity of the well cementation cement slurry, the pore connectivity of the plastic state of the well cementation cement slurry can be obtained by utilizing a multiphase phenomenological model. The invention has the advantages that: the quantitative evaluation method for the pore connectivity in the solidification process of the well cementation cement slurry is provided, and has important significance for researching the early gas channeling mechanism of well cementation of an oil-gas well and researching and developing well cementation gas channeling prevention materials and technologies.
Description
Technical Field
The invention belongs to the field of oil and gas well cementing engineering, and particularly relates to a quantitative in-situ evaluation method for pore connectivity in a cementing slurry solidification process, which has important significance for researching and developing a gas channeling mechanism in the early stage of well cementation of a gas well and researching and developing a channeling-preventing cement slurry system and technology.
Background
Cement-based materials have been widely used in oil and gas well cementing operations, requiring hydrostatic column pressure of liquid cement slurry to balance high pressure of formation fluid, and the hardened cement sheath effectively seals the formation fluid. However, in the process of cementing, the hydrostatic column pressure drop (also referred to in the industry as "weight loss") increases as the cement slurry hydrates, providing a driving force for the formation fluid to flow into the annular cement slurry, causing an "early flow-through" problem. However, in addition to the driving force required to drive formation fluids into the cement slurry in the setting process, channeling channels should be provided. The cement slurry is used as a solid-liquid two-phase time-varying material, the solid-phase component permeability of the cement slurry is extremely low, and a pore structure filled with the liquid-phase component, particularly a communicating pore structure, can be a main part for providing a channeling channel, so that the control of the pore connectivity in the cement slurry solidification process has important significance for researching the early stage gas channeling problem of well cementation and ensuring the safety of the well cementation operation of an oil-gas well.
The pore structure of the well cementation cement slurry is complex, and pores with different shapes, sizes and connectivity exist. At present, many quantitative research methods are used for the pore structure of solid cement stones, such as mercury intrusion method and nitrogen adsorption method. The results of the closed porosity and porosity of the rings in the samples were tested by mercury intrusion and nitrogen adsorption methods, and the authors also established a method of calculating the porosity connectivity of the samples (He Rui, Ma Hongyan, Hafiz Rezwana B., Fu Chuanqing, Jin Xianyu, He Jiahao.determining porosity and pore network connectivity of the center-based Materials by a modified non-contact electrical connectivity measure: Experiment and the term [ J ] Materials and Design,2018,156: 82-92.). However, the mercury intrusion method and the nitrogen adsorption method both require sample drying, and the drying process will seriously damage the pore structure of the cement slurry due to the low strength and the unfixed shape of the cement slurry in the waiting setting stage, thereby making the mercury intrusion method and the nitrogen adsorption method difficult to be used for testing the pore connectivity of the cement slurry in the waiting setting process. Therefore, a new quantitative evaluation method capable of accurately representing the pore connectivity of the cement slurry in the waiting setting stage is needed to be established.
Disclosure of Invention
The invention provides a quantitative in-situ evaluation method for pore connectivity in a well cementation cement slurry solidification process aiming at the defects of the prior art.
In order to realize the purpose, the technical scheme adopted by the invention is as follows:
a quantitative in-situ evaluation method for pore connectivity in a well cementation cement slurry solidification process comprises the following steps:
and 3, pouring 400mL of well cementation cement slurry into a high-temperature high-pressure water loss instrument (460mL, Shenyang aerospace university application and technology research institute), and curing for 1 hour at 30 ℃. Injecting nitrogen with the pressure of 0.1MPa into the high-temperature high-pressure water loss instrument, opening a valve at the bottom of the high-temperature high-pressure water loss instrument, and collecting pore solution of the well cementation cement slurry until no pore solution seeps out of the well cementation cement slurry;
and 8, combining the true density of the cement particles and the water-cement ratio of the cement slurry to obtain the porosity of the well cementation cement slurry at the initial moment, wherein the porosity of the well cementation cement slurry is in direct proportion to the accumulated pore size distribution, so that the porosity (theta) of the cement slurry is obtained based on the pore size distribution of the well cementation cement slurryp)；
Step 9, porosity (theta) of the combined cement slurryp) And forming factor (F) results, using a multiphasic phenomenological model
The pore communicating porosity (beta) of the well cementation cement slurry can be obtainedp)；
Compared with the prior art, the invention has the advantages that:
can provide a foundation for researching the gas channeling mechanism and the cement slurry early hydration mechanism in the well cementation early stage of the oil-gas well and establishing the evaluation technology of the anti-channeling capability of the well cementation cement slurry, and has important significance for the development of anti-channeling well cementation cement slurry systems and technologies.
Drawings
FIG. 1 is a flow chart of a quantitative in-situ evaluation method for pore connectivity in a cementing slurry solidification process according to an embodiment of the present invention;
FIG. 2 shows the resistivity in situ test results of the well cementation cement slurry formulation of the embodiment of the present invention;
FIG. 3 is the resistivity results of the cementing slurry pore solution of the embodiments of the present invention;
FIG. 4 is a calculation result of a well cementation cement slurry formation factor according to an embodiment of the present invention;
FIG. 5 shows in-situ test results of transverse relaxation times of a well-cementing slurry according to an embodiment of the present invention;
FIG. 6 shows the cumulative pore size distribution analysis of the well cementation cement slurry according to the embodiment of the present invention;
FIG. 7 shows the results of porosity analysis of a well-cementing slurry according to an embodiment of the present invention;
FIG. 8 is a pore connectivity result for an example cement slurry analyzed using a multiphase phenomenological model in accordance with an embodiment of the present invention.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the present invention will be further described in detail below with reference to the accompanying drawings by way of examples.
As shown in figure 1, the quantitative in-situ evaluation method for the pore connectivity in the solidification process of the well cementation cement slurry comprises the following steps:
(1) weighing 800G of high-sulfate-resistance G-grade oil well cement, 16G of fluid loss additive and 352G of water, and preparing cement slurry according to GB/T19139-2012 standard;
(2) taking about 150mL of cement paste into a beaker, immersing the beaker containing the cement paste into a 30 ℃ water bath kettle and fixing; then inserting an inductive conductivity meter (DM-200, Gantai Kaimeisi Instrument Co., Ltd.) into the cement slurry, and starting to collect the resistivity (rho (t)) of the cement slurry until the resistivity is hydrated for 20 hours;
(3) pouring 400mL of cement slurry into a high-temperature high-pressure water loss instrument (460mL, Shenyang aerospace university application and technology research institute), curing at 30 ℃ for 1 hour, injecting 0.1MPa of nitrogen, opening a bottom valve of the high-temperature high-pressure water loss agent, and collecting a cement slurry pore solution;
(4) the conductivity (rho) of the pore solution of the well cementation cement slurry is tested at 30 ℃ by using an inductive conductivity meter (DM-200, Nicoti Kaimeisi instruments, Ltd.)p(t))；
(5) Combining the cement slurry resistivity (rho (t)) and the cement slurry pore solution resistivity (rho (t))p(t)), using the formula
The formation factor (F) of the cement slurry in different hydration times can be obtained;
(6) taking 5mL of cement slurry into a sample bottle without a nuclear magnetic signal, placing the sample bottle containing the cement slurry into a low-field nuclear magnetic resonance instrument (Micro MRI 12-025V, Jiangsu Newman instrument), and in-situ and continuously acquiring the transverse relaxation time (T) of the cement slurry2) And the magnetization;
(7) the experimental parameters of the low-field nuclear magnetic resonance apparatus are as follows: the RF signal frequency has a dominant value (SF) of 11MHz, a RF 90 degree pulse width (P1) of 2.48 μ s, and a RF 180 degree pulse width (P2) 6.48 mus, 250KHz of sampling frequency (SW), 0.002ms of Radio Frequency Delay (RFD), 2000ms of repeated sampling interval Time (TW), 20 of analog gain (RG1), 3 of digital gain (DRG1), 32 of accumulated sampling times (NS), 0.1ms of echo Time (TE) and 6000 of echo Number (NECH);
(8) the high sulfate-resistant G-grade oil well cement has a true density of 3.15G/cm3The fluid loss agent is a water-soluble polymer material, and the water cement ratio of all cement slurries is 0.44 in the experiment, so that the initial stage of the well cementation cement slurry can be determinedThe porosity is 58%;
(9) according to the formula
The surface relaxation rate (gamma) of the hydrated product of the cement slurry is 5.51 mu m/s, namely the transverse relaxation time (T)2) Calculating the pore size distribution of the cement slurry as a result;
(10) combining the initial porosity and the cumulative pore size distribution of the cement paste, the porosity (theta) of the cement paste at different hydration times can be obtained according to the cumulative pore size distribution result of the cement paste at different hydration timesp)；
(11) Porosity (theta) of the combined cement slurryp) And forming factor (F) results using a multiphasic phenomenological model, formula
The connected porosity (beta) of the cement slurry in different hydration time can be calculatedp)。
As shown in fig. 2, no significant change in resistivity of the cement slurry was found 12 hours prior to hydration; after 12 hours of hydration, the resistivity of the well cementation cement slurry is rapidly increased;
as shown in FIG. 3, the resistivity of the pore solution of the cementing slurry of the continuous test example is found to be about 30.63 Ω & cm after 6 times of continuous tests, and no obvious change exists;
as shown in FIG. 4, since the resistivity of the pore solution of the well cementing Cement slurry is not significantly changed after 1 hour of early hydration of the well cementing Cement slurry (Lianzhen Xiao, Zongjin Li. early-age hydration of front Cement monitored by non-contact electrical resistivity measurement [ J ]. center and Cement Research,2008,38(3): 312-;
as shown in fig. 5, it can be found that within 6h of hydration, the transverse relaxation time of the cementing slurry of the example is mainly distributed between 2 and 14 ms. Then, as the hydration time increases, the transverse relaxation time of the cement slurry decreases significantly. When the cement paste is hydrated for 10 hours, a peak begins to appear at 0.02-0.03 ms, the peak strength at 0.02-0.03 ms is obviously increased along with the continuous increase of the hydration time, the peak value range at the position is obviously increased, and when the cement paste is hydrated for 16 hours, the peak value range at the position is increased to 0.13 ms. In addition, the transverse relaxation time peak of the well cementation cement slurry in the comparative analysis example is strong, and the total magnetization intensity of the transverse relaxation time of the cement slurry is obviously reduced along with the increase of the hydration time of the cement slurry, which also proves that the porosity in the cement slurry is reduced along with the increase of the hydration time.
As shown in FIG. 6, it can be seen that the pore size distribution of the cement slurry at the initial stage is between 11 and 75nm, and the pore size of the cement slurry is not obviously changed 6h before hydration; when the cement paste is hydrated for 10 hours, a peak appears at 0.2 nm; and as the hydration time is increased, the peak value is obviously enhanced, and the range is continuously expanded. The results may also demonstrate that at this stage the nanopore-containing hydration product begins to form rapidly in the cement slurry.
As shown in fig. 7, the porosity of the cement slurry gradually decreased during the setting process.
As shown in fig. 8, the pore connectivity of the cement slurry decreased with increasing hydration time.
It will be appreciated by those of ordinary skill in the art that the examples described herein are intended to assist the reader in understanding the manner in which the invention is practiced, and it is to be understood that the scope of the invention is not limited to such specifically recited statements and examples. Those skilled in the art can make various other specific changes and combinations based on the teachings of the present invention without departing from the spirit of the invention, and these changes and combinations are within the scope of the invention.
Claims (1)
1. A quantitative in-situ evaluation method for pore connectivity in a well cementation cement slurry solidification process is characterized by comprising the following steps:
step 1, preparing well cementation cement slurry according to GB/T19139-2012 standard;
step 2, pouring 150mL of well cementation cement slurry into a beaker, immersing the beaker in a 30 ℃ water bath and fixing the beaker; then placing the inductive conductivity meter into the cement slurry, and continuously collecting the resistivity rho (t) of the cement slurry for 20 hours;
step 3, pouring 400mL of well cementation cement slurry into a high-temperature high-pressure dehydration instrument, and curing for 1 hour at the temperature of 30 ℃; injecting nitrogen with the pressure of 0.1MPa into the high-temperature high-pressure water loss instrument, opening a valve at the bottom of the high-temperature high-pressure water loss instrument, and collecting pore solution of the well cementation cement slurry until no pore solution seeps out of the well cementation cement slurry;
step 4, testing the resistivity rho of the pore solution of the well cementation cement slurry at 30 ℃ by using an induction type conductivity meterp(t)；
Step 5, combining the resistivity rho (t) of the cement paste and the resistivity rho (t) of the pore solution of the cement pastep(t) according to the formula
Obtaining formation factors F of the cement slurry in different hydration times;
step 6, injecting 5mL of well cementation cement slurry into a sample bottle without nuclear magnetic signals, placing the sample bottle containing water slurry into a low-field nuclear magnetic resonance instrument, and collecting the transverse relaxation time T of the well cementation cement slurry at the temperature of 30 ℃ every 2 hours2And a magnetization signal;
step 7, according to the formula
The surface relaxation rate gamma of the hydration product of the cement slurry is 5.51 mu m/s, the hole radius R of the well cementation cement slurry can be calculated, and the pore diameter distribution of the well cementation cement slurry is obtained by combining the magnetization intensity signal of the well cementation cement slurry;
and 8, combining the true density of the cement particles and the water-cement ratio of the cement slurry to obtain the porosity of the well cementation cement slurry at the initial moment, wherein the porosity of the well cementation cement slurry is in direct proportion to the accumulated pore size distribution, so that the porosity theta of the cement slurry is obtained based on the pore size distribution of the well cementation cement slurryp；
Step 9, porosity θ of the bound cement pastepAnd forming factor F results using a multiphasic phenomenological model
Hole capable of obtaining well cementing cement slurryPore-interconnected porosity betap；
Step 10, continuously testing the resistivity rho (t) of the well cementation cement slurry and the resistivity rho (t) of the pore solution in situp(T) and transverse relaxation time T of well cementing slurry2And the time-varying characteristic of the porosity of the pore-communicated well-cementing slurry in the solidification process can be obtained.
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