CN112414820A - Preparation method of thick mud cake simulating shale - Google Patents

Preparation method of thick mud cake simulating shale Download PDF

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CN112414820A
CN112414820A CN202011422999.0A CN202011422999A CN112414820A CN 112414820 A CN112414820 A CN 112414820A CN 202011422999 A CN202011422999 A CN 202011422999A CN 112414820 A CN112414820 A CN 112414820A
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mud cake
shale
drilling fluid
pressure
loss
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CN112414820B (en
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王平全
鲁劲松
何龙
王秋润
冉雨鹭
冉超
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Southwest Petroleum University
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    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N1/00—Sampling; Preparing specimens for investigation
    • G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N1/00—Sampling; Preparing specimens for investigation
    • G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
    • G01N1/38—Diluting, dispersing or mixing samples
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N1/00—Sampling; Preparing specimens for investigation
    • G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
    • G01N1/44—Sample treatment involving radiation, e.g. heat
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N1/00—Sampling; Preparing specimens for investigation
    • G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
    • G01N1/38—Diluting, dispersing or mixing samples
    • G01N2001/386—Other diluting or mixing processes

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  • Life Sciences & Earth Sciences (AREA)
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Abstract

The invention discloses a novel method for simulating a shale pore structure by using a thick mud cake. The preparation materials are as follows: bentonite, sodium carbonate, API barite, nano barite, chromium-free sulfonated lignite, sulfonated phenolic resin and HF-1. The preparation method comprises the following steps: adding hot water into the enamel cup, slowly adding bentonite and sodium carbonate under the action of a high-speed stirrer, uniformly stirring, and hydrating and dispersing for 24 hours; adding API barite, nano barite, chromium-free sulfonated lignite, sulfonated phenolic resin and HF-1 into the hydrated soil slurry, and uniformly stirring; aging the prepared drilling fluid for 16 hours; and pouring the aged drilling fluid into a high-temperature high-pressure water loss instrument to form a mud cake. The average permeability of the mud cake formed by the method is 4.825 multiplied by 10‑4mD, in shale permeability level range; the thickness of the mud cake is 9-11mm, the shale has more authenticity than the thin mud cake,the obtained mud cake has low cost, simple method and good repeatability.

Description

Preparation method of thick mud cake simulating shale
Technical Field
The invention relates to a method for preparing mud cakes simulating a shale micro-pore structure by using a high-temperature high-pressure water loss instrument. By adjusting the formula of the drilling fluid and adopting a high-temperature high-pressure static water loss method, the prepared drilling fluid has the thickness of 9-11mm and the average permeability of 4.825 multiplied by 10-4mud of mDAnd (5) cake. Has lower permeability and higher thickness, and the mud cake is thick and compact. The prepared mud cake can better simulate shale, has higher thickness, can play a good guiding role in the aspect of a shale micro-plugging mechanism, avoids the defect of high difficulty in sampling the shale, and has low cost and good experimental reproducibility.
Background
The shale plugging is mainly used for plugging pores and cracks of a stratum, preventing pressure from being transmitted to the deep part of the stratum and preventing the shale from collapsing, so that the effect of stabilizing a well wall is achieved. At present, shale gas development becomes the key point of energy development in China, but due to the development of micro cracks and micro pores of a shale stratum, the water sensitivity is strong, the phenomenon of borehole wall instability is easy to occur in a long horizontal well section, the key point for solving the problem lies in improving the plugging performance of the drilling fluid, and from the point of plugging performance, the key point for evaluating the good and bad plugging performance lies in the establishment of a real shale physical environment, namely, the prepared shale has the permeability of 10-4The mD-level simulated rock core can restore the real shale low-permeability physical environment, and the best effect evaluation can be fundamentally carried out on the performance of the plugging agent, so that the most valuable data feedback is provided for the improvement and promotion of the effect of the plugging agent.
The shale coring operation is very difficult in a drilling site due to the problem that the shale stratum microcracks develop to collapse and break. And the porosity and permeability of the cored shale at different positions have great difference, so that the plugging problem of the cored shale is greatly influenced. Although there are many advanced simulation methods for simulating formation cores, the methods directly aiming at shale microporosity microcracks are few and have great limitations. Particularly, the method can simulate few and few 'simulated cores' with shale nano-micron level pores, and is complex and high in cost. Therefore, the prepared simulated rock core capable of better simulating the shale has a great effect on researching the plugging mechanism and plugging rule of the shale.
Disclosure of Invention
For shale plugging, aiming at the problem that the prior art can not directly and simply simulate natural shale nano-micron pore gaps and a simulation instrumentThe invention provides a method for simulating shale micro-nano pore gaps by using a drilling fluid mud cake, which can effectively simulate shale micro-nano pore gaps, and has the advantages of high equipment cost and poor effect, low cost and strong experimental repeatability. Through multiple experiments, compared with the permeability of real shale, the average permeability of the mud cake reaches 4.825 multiplied by 10-4And mD, the prepared mud cake can meet the requirement of simulated shale, and has important significance on the plugging mechanism of the shale and the screening and evaluation of the nano-micron plugging agent.
The mud cake preparation formula disclosed by the invention comprises the following raw materials:
Figure BDA0002823378260000021
the preparation method of the mud cake comprises the following steps:
step 1, measuring 100 parts of 80-100 ℃ hot water by using a measuring cylinder, pouring the hot water into an enamel cup, placing the enamel cup under a drilling fluid stirrer, slowly adding 6 parts of bentonite, continuously stirring, adding 0.3 part of sodium carbonate, stirring for 30min, and sealing the prepared drilling fluid base slurry for 24h to enable the drilling fluid base slurry to be pre-hydrated.
Step 2, taking 100 parts of pre-hydrated drilling fluid base slurry, adding 70 parts of API barite and 30 parts of nano barite while stirring, and stirring for 30 min; adding 5 parts of chromium-free sulfonated lignite and 5 parts of sulfonated phenolic resin, and stirring for 30 min; adding 0.4 part of HF-1, and stirring for 30 min; and pouring the stirred drilling fluid into a high-temperature aging tank, and aging for 16 hours at 105 ℃.
And 3, taking the aged drilling fluid, stirring for 30min by using an electric high-speed stirrer at the rotating speed of 12000r/min, pouring the uniformly stirred drilling fluid into a high-temperature high-pressure water loss instrument, adjusting the pressure and the temperature, and recording the water loss after water loss.
And 4, further, simulating the low-permeability mud cake of the shale formation, wherein the permeability of the mud cake prepared by the method is 4-6 multiplied by 10-4mD and the thickness is 9-11 mm.
Further, the low permeability mud cake simulating shale formation is characterized by API bariteMedian particle diameter (D)50) The particle size of the nano barite is 18.303 μm, and is the median particle size (D)50) 8.476 μm, it can assist bentonite in forming a dense mud cake.
Further, the method for simulating the low permeability mud cake of the shale formation is characterized in that the pressure difference of 3.5MPa (the upper pressure is 4MPa, and the lower pressure is 0.5MPa), the temperature of 105 ℃ and the filtration time of 30min are used as filtration conditions.
Further, the mud cake simulating low permeability of the shale formation is characterized in that the calculation method of the mud cake permeability obtained in the step 4 is as follows: osmotic fluid loss is combined with darcy's law.
Further, the calculation formula of the simulated mud cake permeability is as follows:
Figure BDA0002823378260000031
Figure BDA0002823378260000032
wherein V30: high temperature and high pressure filtration loss, cm, for 30min3；
Q: fluid loss velocity, cm3/s；
K: fluid loss media Permeability, 10-1μm2；
μ: viscosity at 105 ℃ of water, 0.27 mPas;
l: the thickness of the mud cake is cm;
a: effective filtration area of high-temperature high-pressure water loss instrument, 22.6cm2；
P1: fluid loss upper pressure, 4.0 MPa;
P2: pressure under fluid loss, 0.5 MPa.
Detailed Description
The method for making a mudcake simulating shale is described more fully below by combining with specific examples, which are only a part of examples, but not all examples, and are only used for illustrating and not limiting the technical solution of the present invention.
Example 1: mud cake preparation for simulating shale formation
The preparation method of the thick mud cake for preparing the simulated shale needs to prepare the following materials: bentonite, API barite, nano barite, chromium-free sulfonated lignite, sulfonated phenolic resin, HF-1:
the preparation method comprises accurately measuring hot water (300 ml) with temperature of 80-100 deg.C with a measuring cylinder, pouring into an enamel cup, stirring at low speed, slowly adding bentonite (18 g), stirring, adding anhydrous sodium carbonate (0.9 g), stirring for 30min, sealing the prepared bentonite slurry for 24 hr, and pre-hydrating. Taking 300ml of prehydrated bentonite-based slurry, stirring for 30min, adding 210g of API barite, continuing to stir for 30min, adding 90g of nano barite, continuing to stir for 30min, adding 15g of chromium-free sulfonated lignite, continuing to stir for 30min, and adding 15g of sulfonated phenolic resin; and (3) continuously stirring for 30min, adding 1.2g of HF-1 treating agent, continuously stirring for 60min, loading into a high-temperature aging tank, and hot rolling in a high-temperature roller furnace at 105 ℃ for 16 h. And (3) taking the aged drilling fluid, stirring for 30min by using an electric high-speed stirrer at the rotating speed of 12000r/min, pouring the uniformly stirred drilling fluid into a high-temperature high-pressure water loss instrument, adjusting the pressure (the upper pressure is 4MPa and the lower pressure is 0.5MPa) and the temperature (105 ℃), and recording the water loss after water loss. And after the filtration experiment is finished, opening the high-temperature high-pressure filtration instrument kettle body, pouring out the redundant drilling fluid, adding distilled water, slightly shaking the kettle body, and washing away the redundant drilling fluid on the surface of the mud cake. Continuously pouring distilled water to the scale mark of the kettle body of the high-temperature high-pressure dehydration instrument, adjusting the pressure (upper pressure is 4MPa and lower pressure is 0.5MPa) and the temperature (105 ℃), and recording the water loss (V) after dehydration30) The mud cake was removed and the mud cake thickness (L) was measured.
Through multiple sets of experiments, the prepared mud cake data are as follows:
TABLE 1 Multi-group mud cake data
Group number Mud cake thickness (mm) Mud cake 30min dehydration (ml) Mud cake permeability (10)-4md)
1 10.43 2.2 4.35
2 11.06 2.5 5.24
3 9.68 2.6 4.77
4 10.42 2.5 4.94
Average 10.40 2.4 4.825
As can be seen from Table 1 above, the permeability of the mudcake of the simulated shale is completely 10-4And the shale can be effectively simulated by the mD level. The thickness, the filtration loss and the permeability of the mud cake data are all in a certain range, and the experimental reappearance degree of the mud cake is high.

Claims (6)

1. A preparation method of thick mud cakes simulating shale is characterized by comprising the following steps:
step 1, measuring 100 parts of 80-100 ℃ hot water by using a measuring cylinder, pouring the hot water into an enamel cup, placing the enamel cup under a drilling fluid stirrer, slowly adding 6 parts of bentonite, continuously stirring, adding 0.3 part of sodium carbonate, stirring for 30min, and sealing the prepared drilling fluid base slurry for 24h to enable the drilling fluid base slurry to be pre-hydrated;
step 2, taking 100 parts of pre-hydrated drilling fluid base slurry, adding 70 parts of API barite and 30 parts of nano barite while stirring, and stirring for 30 min; adding 5 parts of chromium-free sulfonated lignite and 5 parts of sulfonated phenolic resin, and stirring for 30 min; adding 0.4 part of HF-1, and stirring for 30 min; pouring the well-stirred drilling fluid into a high-temperature aging tank, and aging for 16 hours at 105 ℃;
step 3, taking the aged drilling fluid, stirring for 30min by using an electric high-speed stirrer at the rotating speed of 12000r/min, pouring the uniformly stirred drilling fluid into a high-temperature high-pressure water loss instrument, adjusting the pressure and the temperature, and recording the water loss amount after water loss;
step 4, opening the kettle body of the high-temperature high-pressure filtration loss instrument, pouring out the redundant drilling fluid, adding distilled water, slightly shaking the kettle body, and washing away the redundant drilling fluid on the surface of the mud cake; and pouring distilled water to the scale line of the kettle body of the high-temperature high-pressure water loss instrument, adjusting the pressure and the temperature, recording the water loss amount after water loss, taking out and measuring the thickness of the mud cake.
2. A method of making a shale simulating mudcake as claimed in claim 1 wherein the mudcake produced by the method has a permeability of 4-6 x 10-4mD and the thickness is 9-11 mm.
3. The method of making a shale simulating mudcake as claimed in claim 1 wherein the API barite has a median particle size (D)50) The particle size of the nano barite is 18.303 μm, and is the median particle size (D)50) 8.476 μm, a dense mud cake can be formed.
4. The method for preparing a thick cake simulating shale according to claim 1, wherein the fluid loss conditions are a pressure difference of 3.5MPa (upper pressure of 4MPa and lower pressure of 0.5MPa), a temperature of 105 ℃ and a fluid loss time of 30 min.
5. The method for preparing a thick mudcake simulating shale according to claim 1, wherein the method for calculating the permeability of the mudcake obtained in the step 4 comprises the following steps: osmotic fluid loss is combined with darcy's law.
6. The simulated mudcake permeability of claim 5 calculated as:
Figure FDA0002823378250000011
Figure FDA0002823378250000012
wherein V30: high temperature and high pressure filtration loss, cm, for 30min3；
Q: fluid loss velocity, cm3/s；
K: fluid loss media Permeability, 10-1μm2；
μ: viscosity at 105 ℃ of water, 0.27 mPas;
l: the thickness of the mud cake is cm;
a: effective filtration area of high-temperature high-pressure water loss instrument, 22.6cm2；
P1: fluid loss upper pressure, 4.0 MPa;
P2: pressure under fluid loss, 0.5 MPa.
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CN114112850A (en) * 2021-11-30 2022-03-01 西南石油大学 Preparation method of thick mud cake and construction method of three-dimensional digital core of thick mud cake
CN115584251A (en) * 2021-07-06 2023-01-10 中国石油化工股份有限公司 Strong plugging drilling fluid and preparation method thereof

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CN114112850A (en) * 2021-11-30 2022-03-01 西南石油大学 Preparation method of thick mud cake and construction method of three-dimensional digital core of thick mud cake

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