CN118599505B - Degradable oil-based coring sealing fluid - Google Patents
Degradable oil-based coring sealing fluid Download PDFInfo
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- CN118599505B CN118599505B CN202411090166.7A CN202411090166A CN118599505B CN 118599505 B CN118599505 B CN 118599505B CN 202411090166 A CN202411090166 A CN 202411090166A CN 118599505 B CN118599505 B CN 118599505B
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
- C09K8/00—Compositions for drilling of boreholes or wells; Compositions for treating boreholes or wells, e.g. for completion or for remedial operations
- C09K8/42—Compositions for cementing, e.g. for cementing casings into boreholes; Compositions for plugging, e.g. for killing wells
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F2/00—Processes of polymerisation
- C08F2/38—Polymerisation using regulators, e.g. chain terminating agents, e.g. telomerisation
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F220/00—Copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and only one being terminated by only one carboxyl radical or a salt, anhydride ester, amide, imide or nitrile thereof
- C08F220/02—Monocarboxylic acids having less than ten carbon atoms; Derivatives thereof
- C08F220/10—Esters
- C08F220/26—Esters containing oxygen in addition to the carboxy oxygen
- C08F220/32—Esters containing oxygen in addition to the carboxy oxygen containing epoxy radicals
- C08F220/325—Esters containing oxygen in addition to the carboxy oxygen containing epoxy radicals containing glycidyl radical, e.g. glycidyl (meth)acrylate
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Abstract
本发明公开了一种易降解油基取心密闭液，涉及钻井取心技术领域。该易降解油基取心密闭液，包括成膜增稠剂、纳米颗粒、增稠剂和水；其中，所述成膜增稠剂的制备方法包括以下步骤：配置链转移剂的水溶液，在持续搅拌的条件下，滴加单体和/或其溶液直至反应液中单体浓度为15~35wt%，同时滴加引发剂溶液，滴加完毕后反应1~4h，反应结束后，对其进行分离提纯即得。本发明的易降解油基取心密闭液，其相对于常规的密闭液来讲，由于采用了短链的成膜增稠剂，因此，其降解性能较好，具有较强的环保性能；同时，粘度在高温条件下的下降程度较低，能够耐受较高的温度，因此能够适用于深井的密闭取心。The invention discloses a degradable oil-based coring sealing fluid, and relates to the technical field of drilling coring. The degradable oil-based coring sealing fluid comprises a film-forming thickener, nanoparticles, a thickener and water; wherein the preparation method of the film-forming thickener comprises the following steps: preparing an aqueous solution of a chain transfer agent, dripping a monomer and/or its solution under continuous stirring until the monomer concentration in the reaction solution is 15-35wt%, and dripping an initiator solution at the same time, reacting for 1-4h after the dripping is completed, and separating and purifying the fluid after the reaction is completed. Compared with conventional sealing fluids, the degradable oil-based coring sealing fluid of the invention has better degradation performance and stronger environmental protection performance due to the use of a short-chain film-forming thickener; at the same time, the viscosity decreases less under high temperature conditions, and can withstand higher temperatures, so it can be suitable for closed coring of deep wells.
Description
Technical Field
The invention belongs to the technical field of drilling coring, and particularly relates to an easily degradable oil-based coring sealing liquid.
Background
The airtight coring technology is a coring technology commonly used in oil fields, and is characterized in that an airtight coring device comprising a coring barrel is used for coring, airtight liquid is arranged in the airtight coring device, when the airtight coring device reaches a target layer, the airtight liquid in the coring barrel is discharged, meanwhile, a coring bit starts to work, and the airtight liquid is coated on the surface of a drilled core, so that external fluid such as drilling fluid is prevented from entering the core, the state of the extracted core in a stratum can be maintained to the greatest extent, and a person skilled in the art can obtain the fluid distribution condition in the stratum to the greatest extent.
The confining liquid is a key technology in the process of confining the core, and relates to whether the core is polluted by external fluid or not. The sealing liquid in the prior art mainly comprises an oil-based sealing liquid, a synthetic-based sealing liquid and a water-based sealing liquid, wherein the oil-based sealing liquid is mainly castor oil-based sealing liquid, and is formed by stirring castor oil, spinning perchloroethylene resin and the like, wherein the cost of raw materials is high, and meanwhile, toxic and harmful gases such as chlorine gas, hydrogen chloride and the like are generated in the production process, so that the performance stability is poor, and the degradation is difficult; the synthetic base sealing liquid mainly adopts a plasticizer as a solvent, and simultaneously adds corresponding resin as a film forming agent in the solvent, and adds a certain plugging agent to increase the sealing effect, however, the synthetic base sealing liquid has higher cost and is difficult to degrade; the water-based sealing liquid is mainly prepared from hydroxyethyl cellulose, polyacrylamide, potassium chloride and the like, however, the temperature resistance is poor, and meanwhile, the water-based sealing liquid adopts high-viscosity high-molecular-weight polyacrylamide and is difficult to degrade.
Disclosure of Invention
In order to solve at least one of the problems, the invention provides the easily degradable oil-based coring sealing liquid, which has better temperature resistance and stronger environmental protection performance.
The technical scheme of the invention is as follows: the mass ratio of the components is 12-25:5-10: 100 film forming thickeners, nanoparticles, and solvents;
The preparation method of the film forming thickener comprises the following steps: preparing an aqueous solution of a chain transfer agent, dropwise adding a monomer and/or a solution thereof under the condition of continuous stirring until the concentration of the monomer in a reaction solution is 15-35 wt%, simultaneously dropwise adding an initiator solution, reacting for 1-4 h after the dropwise adding is finished, and separating and purifying after the reaction is finished to obtain the chain transfer agent; wherein, the monomer comprises the following components in percentage by mass of 10:5-15: 1-3 parts of acrylic acid, glycidyl methacrylate and 2-methacryloyloxyethyl phosphorylcholine, wherein the addition amount of an initiator is 1-5wt% of the total amount of monomers, and the addition amount of a chain transfer agent is 10-50wt% of the total amount of monomers.
In the embodiment, the prepared film-forming thickener is a short-chain polymer, and has a number average molecular weight of about 2000-8000 according to the difference of monomer concentration, initiator addition, chain transfer agent addition and reaction time, and is easier to degrade compared with a long-chain polymer; meanwhile, glycidyl methacrylate and 2-methacryloyloxyethyl phosphorylcholine in the monomer can be degraded under certain conditions. According to the test of the inventor, the degradation rate of the film forming thickener can reach more than 50% under the irradiation of ultraviolet light for about 10-23 hours; the degradation rate can reach more than 50% after the material is placed for 8-20 days in a natural environment.
Meanwhile, the prepared film-forming thickener contains a large amount of ether bonds and quaternary ammonium groups, can be well adsorbed on the rock core and forms a layer of protective film, and prevents external fluid from entering the inside of the rock core. Although the molecular weight is low, the side chain length of the monomer is different, so that comb-shaped molecules are easy to form, and the viscosity is high. Meanwhile, the polymer has higher solubility, so that the addition amount of the polymer can be increased to increase the viscosity of the sealing liquid; when the addition amount is larger, the viscosity is reduced with the temperature to a lower degree, so that the viscosity still has stronger viscosity under the condition of higher temperature.
The nanoparticle may be used in existing nanoparticle commercial products such as one of conventional nanosilica, nanosilica. The nanoparticles used are usually hydrophobic nanoparticles such as fumed silica, nanoparticles modified by hydrophobic properties, etc. from the practical point of view, and these are conventional commercial products. On the one hand, the nano particles can form a certain degree of blocking, and meanwhile, under the action of the nano particles, the viscosity and the stability of the sealing liquid can be increased to a certain degree.
The solvent is a mixture of a first solvent and glycerin, wherein the first solvent is at least one of n-butanol and n-propanol, and the mass ratio of the first solvent to the glycerin is 5-20:10. These solvents can well dissolve the film forming thickener, and n-butanol and n-propanol are added, on the one hand, in order to dilute viscous glycerin, so that the film forming agent can be well dissolved, nanoparticles can be well dispersed, and meanwhile, the sealing performance of the sealing liquid can be improved.
According to one embodiment of the invention, the sealing liquid further comprises phosphate, the mass ratio of the phosphate to the solvent is 1-15:100, and the added phosphate not only can adjust the density of the sealing liquid, but also can enhance the high-temperature stability of the sealing liquid.
One embodiment of the present invention is that the chain transfer agent is isopropanol, which is a common chain transfer agent in the art.
In one embodiment of the present invention, in the method for preparing a film-forming thickener, the glycidyl methacrylate is dissolved with methanol or ethanol to prepare a solution; the 2-methacryloyloxyethyl phosphorylcholine is prepared into a solution by using water. In the case of glycidyl methacrylate, which is insoluble in water but soluble in most organic solvents, methanol or ethanol is used in the present invention because it does not affect the reaction, and at the same time, methanol or ethanol is miscible with water, so that glycidyl methacrylate is more easily contacted and reacted with the rest of the material.
In one embodiment of the invention, the initiator is one of potassium persulfate, ammonium persulfate and sodium persulfate, and the reaction temperature is 50-70 ℃, and when the initiator is used, the initiator is prepared into a solution by using water. Generally, the reaction temperature is related to the type of initiator, and the persulfate initiator adopted in the embodiment has a proper temperature of 50-70 ℃; it is also possible to use the remaining initiators, for example of the oxidation-reduction type, and to adjust the reaction temperature in dependence on these initiators.
The invention has the advantages that:
Compared with the conventional sealing liquid, the easily degradable oil-based coring sealing liquid adopts a short-chain film-forming thickener, so that the easily degradable oil-based coring sealing liquid has better degradation performance and stronger environmental protection performance compared with the rest sealing liquids in the field; meanwhile, the viscosity is lower in the reduction degree under the high-temperature condition, and the high-temperature-resistant sealing core is capable of resisting high temperature, so that the sealing core is applicable to sealing core taking of a deep well.
Detailed Description
The invention will be further illustrated with reference to the following examples, it being understood that the preferred embodiments described herein are for the purpose of illustration and explanation only and are not intended to limit the invention.
In the following examples, unless otherwise indicated, the procedures used were those conventional in the art.
In the examples which follow, materials used, unless otherwise specified, are all conventional materials in the art, mature commercial products.
In the following examples, the parts are parts by mass unless otherwise specified.
Example 1: in this embodiment, the composition of the easily degradable oil-based coring sealing liquid is as follows: 18 parts of film forming thickener, 8 parts of nano silicon dioxide and 100 parts of solvent, wherein the 100 parts of solvent consists of 60 parts of n-butanol and 40 parts of glycerol; when in use, the solvent is added to carry out ultrasonic dispersion on the nano silicon dioxide, and then the film forming thickener is added and continuously stirred to be evenly mixed, thus obtaining the nano silicon dioxide.
The preparation method of the film forming thickener is as follows: adding 12 parts of glycidyl methacrylate into ethanol to prepare a solution, adding 1.5 parts of 2-methacryloyloxyethyl phosphorylcholine into water to prepare a solution, and adding 0.5 part of potassium persulfate into water to prepare a solution;
Adding 4.3 parts of isopropanol into 100 parts of water, stirring to dissolve, adding 10 parts of acrylic acid, glycidyl methacrylate solution, 2-methacryloyloxyethyl phosphorylcholine solution and potassium persulfate solution into the aqueous solution of a chain transfer agent under the conditions of introducing nitrogen to remove oxygen and 65 ℃, preserving heat for 2 hours after the dripping is finished, and removing low-boiling substances by reduced pressure distillation after the heat preservation is finished.
The film forming thickener of this example has degradation rates of 50% under different conditions, respectively: and the ultraviolet condition is about 17 hours, and the natural environment is about 15 days. Indicating that it has good self-degradation properties. Therefore, the sealing liquid of the embodiment has good degradation performance.
Example 2: in this embodiment, the composition of the easily degradable oil-based coring sealing liquid is as follows: 22 parts of film forming thickener, 9 parts of nano zinc oxide and 100 parts of solvent, wherein the 100 parts of solvent consists of 40 parts of n-butanol and 60 parts of glycerin; when in use, the solvent is added to carry out ultrasonic dispersion on the nano zinc oxide, and then the film forming thickener is added and continuously stirred to be evenly mixed, thus obtaining the nano zinc oxide.
The preparation method of the film forming thickener is as follows: 8 parts of glycidyl methacrylate is added into ethanol to prepare a solution, 2.5 parts of 2-methacryloyloxyethyl phosphorylcholine is added into water to prepare a solution, and 0.25 part of potassium persulfate is added into water to prepare a solution;
Adding 2.8 parts of isopropanol into water, stirring to dissolve, adding 10 parts of acrylic acid, glycidyl methacrylate solution, 2-methacryloyloxyethyl phosphorylcholine solution and potassium persulfate solution into the aqueous solution of a chain transfer agent under the conditions of introducing nitrogen to remove oxygen and 65 ℃, preserving heat for 2 hours after the dripping is finished, and removing low-boiling substances by reduced pressure distillation after the heat preservation is finished.
The film forming thickener of this example has degradation rates of 50% under different conditions, respectively: and the ultraviolet condition is about 30 hours, and the natural environment is about 18 days. Indicating that it has good self-degradation properties. Therefore, the sealing liquid of the embodiment has good degradation performance.
Example 3: this comparative example differs from example 1 in that 12g of potassium phosphate was also added, and the remainder was the same.
Example 4: the comparative example differs from example 1 in that in the preparation of the film-forming thickener, the amount of isopropyl alcohol added was 12 parts, the amount of glycidyl methacrylate added was 17 parts, the amount of 2-methacryloyloxyethyl phosphorylcholine added was 2.5 parts, the amount of acrylic acid added was 12 parts, and the rest was the same.
The film forming thickener of this example has degradation rates of 50% under different conditions, respectively: and the ultraviolet condition is about 16 hours, and the natural environment is about 9 days. Indicating that it has good self-degradation properties. Therefore, the sealing liquid of the embodiment has good degradation performance.
Example 5: this embodiment differs from embodiment 1 in that the sealing liquid includes: 14 parts of film forming thickener, 5.5 parts of nano silicon dioxide and 100 parts of solvent, wherein the 100 parts of solvent consists of 60 parts of n-butanol and 40 parts of glycerol, and the rest parts are the same.
Example 6: this embodiment differs from embodiment 1 in that the sealing liquid includes: 24 parts of film forming thickener, 9.5 parts of nano silicon dioxide and 100 parts of solvent, wherein the 100 parts of solvent consists of 50 parts of n-propanol and 50 parts of glycerol, and the rest parts are the same.
Comparative example 1
This comparative example differs from example 1 in that no nanoparticles were contained, the remainder being the same.
Comparative example 2
This comparative example differs from example 1 in that the film forming thickener was prepared without 2-methacryloyloxyethyl phosphorylcholine and the remainder was the same.
Comparative example 3
This comparative example differs from example 1 in that the film forming thickener was prepared without glycidyl methacrylate, the remainder being the same.
In order to further highlight the technical effects of the present invention, performance tests were performed on the above-described embodiments.
1. Salt spray resistance test
The sealing solutions of examples 1 to 6 and comparative examples 1 to 3 were taken, the viscosity thereof was measured at normal temperature, then, the sealing solutions were aged at 120℃for 24 hours, and after the aging was completed, the viscosity thereof was measured, and the final results are shown in Table 1.
TABLE 1 salt spray resistance test results
As can be seen from Table 1, the sealing liquid prepared by the embodiment of the invention has stronger temperature resistance and can meet the actual coring requirement.
2. Sealing performance test
Taking the sealing solutions of examples 1-6 and comparative examples 1-3, and then taking a core and placing the core in the sealing solution for soaking for 10min; an aqueous solution of an ammonium nitrate tracer with a concentration of 1% was prepared, the soaked core was taken out and placed in the aqueous solution of the tracer for 16 hours, after the completion of which the invasion amount of the aqueous solution of the tracer was measured while the core not soaked with the sealing liquid was used as a blank, and finally the sealing performance thereof was as shown in table 2.
Wherein, the calculation formula of the sealing rate is as follows: In which, in the process, In order to achieve the sealing rate, the sealing device,The equivalent invasion amount of the non-soaked closed liquid core is represented, and b represents the equivalent invasion amount of the soaked closed liquid core. Meanwhile, the equivalent intrusion amount is obtained by the following method: taking the tested core, cutting a piece of core along the axis of the core in a certain fixed area, crushing, adding 10ml of water, continuously stirring to extract for 10min, and measuring the concentration of the core by adopting an ultraviolet spectrophotometer.
Table 2 results of the tightness test
As can be seen from Table 2, the sealing liquid prepared by the embodiment of the invention has a strong sealing effect and can be suitable for sealing and coring operation of oil fields.
The present invention is not limited to the above-mentioned embodiments, but is not limited to the above-mentioned embodiments, and any simple modification, equivalent changes and modification made to the above-mentioned embodiments according to the technical matters of the present invention can be made by those skilled in the art without departing from the scope of the present invention.
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102977864A (en) * | 2011-09-03 | 2013-03-20 | 中国石油化工股份有限公司 | High-temperature coring sealing fluid and production process thereof |
| CN110950995A (en) * | 2018-09-27 | 2020-04-03 | 中石化石油工程技术服务有限公司 | Low-molecular thickening agent for drilling fluid and preparation method thereof |
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| FR2863617B1 (en) * | 2003-12-15 | 2006-01-21 | Rhodia Chimie Sa | ZWITTERIONIC POLYMERS COMPRISING BETAINE - TYPE UNITS AND USE OF ZWITTERIONIC POLYMERS IN BOREHOLE FLUIDS. |
| DK2180004T3 (en) * | 2008-10-22 | 2011-09-05 | Clariant Finance Bvi Ltd | Olefinically unsaturated phosphonate compounds, polymers prepared therefrom and their use |
| EP2381065B1 (en) * | 2010-04-20 | 2016-11-16 | Services Pétroliers Schlumberger | System and method for improving zonal isolation in a well |
| CA3061408A1 (en) * | 2017-04-27 | 2018-11-01 | Bp Exploration Operating Company Limited | Microparticles and method for modifying the permeability of a reservoir zone |
| CN114426633A (en) * | 2020-09-02 | 2022-05-03 | 中国石油化工股份有限公司 | Calcium salt-resistant and temperature-resistant tackifier and preparation method thereof |
| CN116948609A (en) * | 2023-06-30 | 2023-10-27 | 西南石油大学 | Preparation of nano plugging agent and oil-based drilling fluid |
| CN117659293A (en) * | 2023-10-30 | 2024-03-08 | 大庆中联信实石油科技开发有限公司 | Thickening agent for fracturing and preparation method thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN102977864A (en) * | 2011-09-03 | 2013-03-20 | 中国石油化工股份有限公司 | High-temperature coring sealing fluid and production process thereof |
| CN110950995A (en) * | 2018-09-27 | 2020-04-03 | 中石化石油工程技术服务有限公司 | Low-molecular thickening agent for drilling fluid and preparation method thereof |
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