CN111333767A - Polyion liquid nano hydrogel plugging agent and water-based drilling fluid - Google Patents

Polyion liquid nano hydrogel plugging agent and water-based drilling fluid Download PDF

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CN111333767A
CN111333767A CN202010286553.3A CN202010286553A CN111333767A CN 111333767 A CN111333767 A CN 111333767A CN 202010286553 A CN202010286553 A CN 202010286553A CN 111333767 A CN111333767 A CN 111333767A
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谢刚
范莉
邓明毅
白杨
王平全
罗平亚
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Southwest Petroleum University
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Abstract

The invention discloses a polyion liquid nano hydrogel plugging agent and a water-based drilling fluid. The plugging agent used by the water-based drilling fluid is polyion liquid nano hydrogel, and the polyion liquid nano hydrogel plugging agent is prepared by a step method; the drilling fluid comprises 100 parts by weight of water, 1-10 parts by weight of bentonite, 0.2-1 part by weight of xanthan gum, 0.4-1.2 parts by weight of salt-resistant filtrate reducer, 0.4-1.2 parts by weight of temperature-resistant filtrate reducer, 4-10 parts by weight of potassium chloride, 10-20 parts by weight of polyion liquid nano hydrogel plugging agent, 0.4-2 parts by weight of lubricant, 20-50 parts by weight of calcium carbonate and 0.1-0.4 part by weight of sodium hydroxide. The invention adopts the polyion liquid nanometer hydrogel prepared by the fractional step method as the nanometer plugging agent, the particle size distribution of the polyion liquid nanometer hydrogel is approximately between 30 and 200nm, and the polyion liquid nanometer hydrogel can effectively plug micro-and nanometer-sized pores in a shale well wall, thereby stabilizing the well wall and preventing collapse.

Description

Polyion liquid nano hydrogel plugging agent and water-based drilling fluid
Technical Field
The invention relates to the technical field of oil and gas field drilling, in particular to a polyion liquid nano hydrogel plugging agent and a water-based drilling fluid containing the plugging agent.
Background
In the process of developing petroleum and natural gas resources, the exploitation of shale gas has been a research hotspot of researchers. Shale is very susceptible to hydration swelling due to its low permeability and the rich clay matrix in its pores. Drilling fluid easily enters a stratum along the micro-cracks of the shale, so that the micro-cracks are spread and expanded, and the well wall is unstable. The stability of the shale is a technical difficulty for shale development, so that effective plugging of the microcracks of the shale is one of the key measures for solving the instability of the shale borehole wall. At present, the commonly used plugging agent has the problem of large particle size, and can only effectively plug micron-level cracks, but the plugging of nanometer-level cracks becomes extremely difficult. Therefore, the preparation of nano-grade nano-plugging materials with good plugging effect is a problem which needs to be solved by the technical personnel in the field.
The ionic liquid is a salt which is in a liquid state at room temperature or close to room temperature and consists of anions and cations, and is also called low-temperature molten salt. The synthesis method is simple and comprises a direct synthesis method and a two-step synthesis method. The ionic liquid has excellent chemical properties, ionic conductivity, thermal stability and the like. The ionic liquid is polymerized to obtain the polyionic liquid which has various excellent performances of the ionic liquid. Aiming at the problem that the nano-scale microcracks in the shale cannot be effectively blocked, in order to block the microcracks to ensure the stability of the shale well wall, the preparation of the novel nano-blocking agent is urgently needed, and the polyion liquid nano-hydrogel becomes a research hotspot of the future nano-blocking agent due to the excellent performance of the polyion liquid nano-hydrogel.
Disclosure of Invention
Aiming at the problem of borehole wall instability caused by the fact that the conventional plugging agent cannot effectively plug micro cracks in the shale at present, the invention provides the polyion liquid nano hydrogel plugging agent, the particle size of which is nano-scale, and the polyion liquid nano hydrogel plugging agent can effectively plug micron-scale and nano-scale cracks in a shale stratum, so that the aim of stabilizing the borehole wall is fulfilled.
In order to achieve the purpose, the technical scheme of the invention is as follows: the polyion liquid nano hydrogel plugging agent is prepared from 1-isopropyl-2-methylimidazole, 4-vinylbenzyl chloride, acrylic acid and N, N' -methylene bisacrylamide, and comprises the following preparation steps:
s1, adding 0.01-0.05 mol of 1-isopropyl-2-methylimidazole and 0.01-0.05 mol of 4-vinylbenzyl chloride into a reactor, adding 10-30mL of deionized water, introducing nitrogen at 20-40 ℃, stirring for reacting for 6-8h, standing for 24-30h after the reaction is finished, washing with 10-20mL of diethyl ether, transferring into a rotary evaporator, performing rotary evaporation at 20-30 ℃ for 40-50min to remove the solvent, and repeating for 3-5 times to obtain 1-isopropyl 3- (4-vinylbenzyl) imidazole chloride;
s2, preparing 120mL of sodium hydroxide aqueous solution by using deionized water, adding acrylic acid, stirring and neutralizing to enable the neutralization degree of the acrylic acid solution to reach 0.6-0.8;
s3, adding 0.015-0.02 mol of 1-isopropyl 3- (4-vinyl benzyl) imidazole chloride prepared in the step S1 and 0.0005-0.0075 mol of N, N' -methylene bisacrylamide to the acrylic acid solution prepared in the step S2, stirring for 40-50min under the protection of nitrogen, standing for 2-3h, dissolving 0.0005-0.008 mol of sodium persulfate in 10-20mL of deionized water, adding the dissolved sodium persulfate into the reaction system, continuing to react for 6-8h at 50-70 ℃, cleaning with 20-30mL of deionized water to remove impurities, repeating for 3-5 times, and finally placing the mixture at 50-60 ℃ for vacuum drying to obtain the polyion liquid hydrogel nano plugging agent.
The molar ratio of 1-isopropyl-2-methylimidazole to 4-vinylbenzyl chloride in step S1 is 1: 1-1.25.
The mass fraction of the sodium hydroxide aqueous solution in the step S2 is 20% -32%, and the neutralization degree is the ratio of the amount of acrylic acid to the amount of sodium hydroxide substances.
In step S3, the amount of N, N' -methylenebisacrylamide added is 1.6% to 4.3% and the amount of sodium persulfate added is 2.5% to 5.5% based on the weight of 1-isopropyl 3- (4-vinylbenzyl) imidazole chloride.
The invention also provides a water-based drilling fluid which contains the polyion liquid nano hydrogel plugging agent and comprises the following components in parts by weight: 100 parts of water, 1-10 parts of bentonite, 0.2-1 part of xanthan gum, 0.4-1.2 parts of salt-resistant fluid loss additive, 0.4-1.2 parts of cooling fluid loss additive, 4-10 parts of potassium chloride, 10-20 parts of polyion liquid nano hydrogel plugging agent, 0.4-2 parts of lubricant, 20-50 parts of calcium carbonate and 0.1-0.4 part of sodium hydroxide.
The pH value of the water-based drilling fluid is 8-11.
The density of the water-based drilling fluid is 1.2-1.5g/cm 3.
The invention has the following beneficial effects:
the particle size distribution of the polyion liquid nano hydrogel plugging agent prepared by the invention is 30-200nm, and micro and nano level cracks in a shale stratum can be effectively plugged, so that the effect of stabilizing a well wall is achieved; in addition, the water-based drilling fluid used by the invention has good performances in the aspects of rheological property, plugging property and the like under the condition of a shale stratum.
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FIG. 1 is a graph showing the distribution of particle sizes of the polyion liquid nano-hydrogel in the first example;
FIG. 2 is a particle size distribution diagram of the polyion liquid nano-hydrogel in example two.
Detailed Description
The technical solutions of the present invention will be described clearly and completely with reference to the following embodiments of the present invention, and it should be understood that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Example 1:
1. synthesizing a polyion liquid nano hydrogel plugging agent: adding 2.5g of 1-isopropyl-2-methylimidazole and 3.1g of 4-vinylbenzyl chloride into a reactor, adding 20mL of deionized water, introducing nitrogen at 25 ℃, stirring for reacting for 6h, standing for 24h after the reaction is finished, washing with 15mL of diethyl ether to remove impurities, transferring into a rotary evaporator, performing rotary evaporation at 25 ℃ for 40min to remove the solvent, and repeating for 3 times to obtain 1-isopropyl 3- (4-vinylbenzyl) imidazole chloride;
weighing 24g of sodium hydroxide solid, dissolving the sodium hydroxide solid in a reaction container filled with 120mL of deionized water, adding 28g of acrylic acid, stirring and neutralizing to enable the neutralization degree of an acrylic acid solution to reach 0.65;
adding 3.5g of 1-isopropyl 3- (4-vinyl benzyl) imidazole chloride and 0.077g of N, N' -methylene bisacrylamide into the solution, stirring for 40min under the protection of nitrogen, standing for 2h, dissolving 0.12g of sodium persulfate in 10mL of deionized water, adding the sodium persulfate into the reaction system, continuing to react for 6h at 50 ℃, washing with 20mL of deionized water to remove impurities, repeating for 3 times, and finally placing the solution at 50 ℃ for vacuum drying to obtain the polyion liquid nano hydrogel plugging agent.
2. Preparation of the water-based drilling fluid: stirring 100 parts by mass of tap water and 8 parts by mass of bentonite for 1 hour under the condition of 25 ℃ in a high-speed stirrer with the rotating speed of 2500r/min, and then standing for 24 hours;
taking the mixed solution, stirring the mixed solution in a high-speed stirrer with the rotating speed of 6000r/min for 10min, and then sequentially adding 0.6 part by weight of yellow collagen, 0.8 part by weight of salt-resistant filtrate reducer, 0.8 part by weight of temperature-resistant filtrate reducer, 4 parts by weight of potassium chloride and 10 parts by weight of polyion liquid sodium saltThe water-based drilling fluid is prepared from 0.6 part by weight of lubricant, 30 parts by weight of calcium carbonate and 0.2 part by weight of sodium hydroxide, the pH value of the drilling fluid is 9.5, and the density is 1.21g/cm3
Example 2:
1. synthesizing a polyion liquid nano hydrogel plugging agent: adding 3.5g of 1-isopropyl-2-methylimidazole and 4.4g of 4-vinylbenzyl chloride into a reactor, adding 30mL of deionized water, introducing nitrogen at 30 ℃, stirring for reacting for 8 hours, standing for 24 hours after the reaction is finished, washing with 20mL of diethyl ether to remove impurities, transferring the mixture into a rotary evaporator, performing rotary evaporation for 50min at the temperature of 30 ℃ to remove the solvent, and repeating for 3 times to obtain 1-isopropyl 3- (4-vinylbenzyl) imidazole chloride;
weighing 20g of sodium hydroxide solid, dissolving the sodium hydroxide solid in a reaction container filled with 100mL of deionized water, adding 29g of acrylic acid, stirring and neutralizing to enable the neutralization degree of an acrylic acid solution to reach 0.8;
adding 4.5g of 1-isopropyl 3- (4-vinyl benzyl) imidazole chloride and 0.12g of N, N' -methylene bisacrylamide into the solution, stirring for 45min under the protection of nitrogen, standing for 2h, dissolving 0.14g of sodium persulfate by using 15mL of deionized water, adding the sodium persulfate into the reaction system, continuing to react for 8h at 60 ℃, cleaning by using 25mL of deionized water to remove impurities, repeating for 4 times, and finally placing the solution at 60 ℃ for vacuum drying to obtain the polyion liquid nano hydrogel plugging agent.
2. Preparation of the water-based drilling fluid: stirring 100 parts by mass of tap water and 6 parts by mass of bentonite for 1 hour under the condition of 25 ℃ in a high-speed stirrer with the rotating speed of 2500r/min, and then standing for 24 hours;
taking the mixed solution, stirring the mixed solution in a high-speed stirrer at the rotating speed of 6000r/min for 10min, and then adding 0.8 part by weight of yellow collagen, 0.9 part by weight of salt-resistant filtrate reducer, 0.9 part by weight of temperature-resistant filtrate reducer, 6 parts by weight of potassium chloride, 15 parts by weight of polyion liquid nano hydrogel plugging agent, 0.8 part by weight of lubricant, 35 parts by weight of calcium carbonate and 0.2 part by weight of sodium hydroxide into the mixed solution in turn every 15min to prepare the water-based drilling fluid, wherein the pH value of the drilling fluid is 10.5, and the density of the drilling fluid is 0.2 part by weight of sodium hydroxideIs 1.24g/cm3
To further illustrate the effects of the polyion liquid nano-hydrogel plugging agent and the drilling fluid of the present invention, the polyion liquid nano-hydrogel plugging agent and the water-based drilling fluid of examples 1 and 2 were subjected to performance tests.
1. Particle size test of polyion liquid nano hydrogel plugging agent
The particle size of the polyion liquid nano hydrogel plugging agent prepared in the embodiment 1 is shown in figure 1, and the particle size of the polyion liquid nano hydrogel plugging agent prepared in the embodiment 2 is shown in figure 2, as can be seen from figures 1 and 2, the particle size of the polyion liquid nano hydrogel plugging agent is approximately distributed between 30-200nm and is intensively distributed between 40-60nm, and the pore throat of the shale which is used as a rock type with the smallest pore size is between 5-60 nm, so that the polyion liquid nano hydrogel has higher matching degree with the pore throat of the shale at the nano level, and can be effectively plugged.
2. Test of blocking performance of polyion liquid nano hydrogel blocking agent
And (3) taking 200mL of distilled water, adding 14g of bentonite and 0.6g of sodium carbonate into the distilled water, stirring the mixture for 4 hours at the rotating speed of 600r/min, and standing the mixture for 24 hours to obtain soil slurry.
140g of barite, 35g of calcium carbonate and 2g of polyacrylamide are added into the soil slurry in sequence, and are stirred at a low speed of 600r/min for 2 hours and then at a high speed of 9000r/min for 30 minutes. And then transferring the mixture into a high-temperature high-pressure dehydration instrument, setting the temperature at 25 ℃ and the pressure at 3.5MPa, dehydrating for 30min, and preparing a filter cake.
Preparing filter cakes according to the method, selecting the filter cakes with approximately same permeability, taking the polyion liquid nano hydrogel blocking agent in the embodiment 1 and the embodiment 2, taking deionized water as a solvent, preparing 100mL of polyion liquid nano hydrogel with different adding amounts respectively, performing ultrasonic dispersion for 10min, transferring into a high-temperature high-pressure dehydration instrument filled with the filter cakes, sequentially testing under the same conditions of 25 ℃ and 3.5MPa, and recording the reading every 5minAnd measuring for 30min, taking out the filter cake, and measuring the thickness after blowing by a blower. According to the formula K ═ q μ l/(A)ΔP) formula, calculating the permeability of the polyion liquid nano hydrogel plugging agent with different adding amounts, and the result is shown in table 1.
Table 1 test data for mud cake
Figure BDA0002448727880000041
Figure BDA0002448727880000051
According to the above table, the polyion liquid nano hydrogel can effectively reduce the permeability of mud cakes as a nano plugging agent, when the addition amount is 1%, the permeability of the mud cakes in examples 1 and 2 is reduced by about 80%, the plugging effect is better along with the increase of the addition amount of the polyion liquid nano hydrogel, and when the addition amount exceeds 3%, the permeability of the mud cakes is not obviously reduced, which indicates that the effect is best when the addition amount of the polyion liquid nano hydrogel is 3%.
3. Water-based drilling fluid performance testing
The water-based drilling fluids prepared in example 1 and example 2 were respectively heated and rolled for 16h at 105 ℃, and the rheological property and the fluid loss were measured, and the results are shown in table 2. In order to further embody the performance of the water-based drilling fluid prepared by the polyion liquid nano hydrogel plugging agent synthesized by the invention, according to the drilling fluid formulas of the embodiment 1 and the embodiment 2, the polyion liquid nano hydrogel plugging agent is replaced by a common plugging material PM-2 (belonging to polymeric alcohol and having a cloud point of 90-100 ℃) with the same weight, two water-based drilling fluids are prepared for comparison, and then the comparative example 1 and the comparative example 2 are placed under the same condition for performing the drilling fluid performance test.
TABLE 2 Water-based drilling fluid Performance parameters
Figure BDA0002448727880000052
Note: the HTHP had a temperature of 105 ℃ and a pressure of 3.5 MPa.
As can be seen from the above table, the YP/PV values of the water-based drilling fluids prepared by using the polyion liquid nano hydrogel as the nano plugging agent in the embodiments 1 and 2 are both 0.43 and fall within the range of 0.36-0.48, and the flow type of the drilling fluid in the annular space belongs to flat laminar flow, and the water-based drilling fluid has the characteristics of high rock carrying capacity under low viscosity and small scouring effect on the well wall, so that the water-based drilling fluid has good rheological property. In addition, compared with the performance of the water-based drilling fluid taking the rigid plugging material PM-2 as a plugging agent, the performance of the water-based drilling fluid of the embodiment 1 and the embodiment 2 is lower than that of the water-based drilling fluid taking the rigid plugging material PM-2 as a plugging agent in both API and high-temperature and high-pressure filtration loss, so that the performance of the drilling fluid prepared by the polyion liquid nano hydrogel plugging agent synthesized by the invention is better.
Although the present invention has been described with reference to a preferred embodiment, it should be understood that various changes, substitutions and alterations can be made herein without departing from the spirit and scope of the invention as defined by the appended claims.

Claims (6)

1. The polyion liquid nano hydrogel plugging agent is characterized by being prepared from 1-isopropyl-2-methylimidazole, 4-vinylbenzyl chloride, acrylic acid and N, N' -methylene bisacrylamide, and prepared by the following steps:
s1, adding 0.01-0.05 mol of 1-isopropyl-2-methylimidazole and 0.01-0.05 mol of 4-vinylbenzyl chloride into a reactor, adding 10-30mL of deionized water, introducing nitrogen at 20-40 ℃, stirring for reacting for 6-8h, standing for 24-30h after the reaction is finished, washing with 10-20mL of diethyl ether, transferring into a rotary evaporator, performing rotary evaporation at 20-30 ℃ for 40-50min to remove the solvent, and repeating for 3-5 times to obtain 1-isopropyl 3- (4-vinylbenzyl) imidazole chloride;
s2, preparing 120mL of 20-30% sodium hydroxide aqueous solution by using deionized water, and adding acrylic acid for stirring and neutralizing to enable the neutralization degree of the acrylic acid solution to reach 0.6-0.8;
s3, adding 0.015-0.02 mol of 1-isopropyl 3- (4-vinylbenzyl) imidazole chloride prepared in the step S1 and 0.0005-0.0075 mol of N, N' -methylene bisacrylamide to the acrylic acid solution prepared in the step S2, stirring for 40-50min under the protection of nitrogen, standing for 2-3h, dissolving 0.0005-0.008 mol of sodium persulfate in 10-20mL of deionized water, adding the dissolved sodium persulfate into the reaction system, continuing to react for 6-8h at 50-70 ℃, washing the product for 3-5 times with 20-30mL of deionized water, and finally drying the product for 8-12h at 50-60 ℃ to obtain the polyion liquid nano hydrogel plugging agent.
2. The polyion liquid nano-hydrogel blocking agent as claimed in claim 1, wherein the molar ratio of 1-isopropyl-2-methylimidazole to 4-vinylbenzyl chloride in step S1 is 1: 1-1.25.
3. The polyion liquid nano-hydrogel blocking agent as claimed in claim 1, wherein in step S3, based on the weight of 1-isopropyl 3- (4-vinylbenzyl) imidazole chloride, the N, N' -methylenebisacrylamide is added in an amount of 1.6% to 4.3%, and the sodium persulfate is added in an amount of 2.5% to 5.5%.
4. A water-based drilling fluid, which is characterized by comprising the polyion liquid nano-hydrogel plugging agent of claims 1-3, wherein the drilling fluid comprises the following components in parts by weight: 100 parts of water, 1-10 parts of bentonite, 0.2-1 part of xanthan gum, 0.4-1.2 parts of salt-resistant fluid loss additive, 0.4-1.2 parts of cooling fluid loss additive, 4-10 parts of potassium chloride, 10-20 parts of polyion liquid nano hydrogel plugging agent, 0.4-2 parts of lubricant, 20-50 parts of calcium carbonate and 0.1-0.4 part of sodium hydroxide.
5. The water-based drilling fluid of claim 4, wherein the water-based drilling fluid has a pH of from 8 to 11.
6. The water-based drilling fluid of claim 4, wherein the water-based drilling fluid has a density of 1.2 to 1.5g/cm3
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CN111808581A (en) * 2020-07-22 2020-10-23 西南石油大学 Chitosan graphene oxide nano hydrogel plugging agent and water-based drilling fluid
CN111808581B (en) * 2020-07-22 2022-04-19 西南石油大学 Chitosan graphene oxide nano hydrogel plugging agent and water-based drilling fluid
CN112096335A (en) * 2020-09-05 2020-12-18 西南石油大学 Shaft isolation method based on ionic liquid rubber plug
CN112096335B (en) * 2020-09-05 2022-06-21 西南石油大学 Shaft isolation method based on ionic liquid rubber plug
CN115260416B (en) * 2022-08-23 2023-10-13 中国石油天然气集团有限公司 Nano composite filtrate reducer for high-temperature-resistant water-based drilling fluid and preparation method thereof

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