CN115948038B - Low-shrinkage high-strength liquid cross-linking plugging material and preparation method and application thereof - Google Patents
Low-shrinkage high-strength liquid cross-linking plugging material and preparation method and application thereof Download PDFInfo
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- 239000000463 material Substances 0.000 title claims abstract description 121
- 239000007788 liquid Substances 0.000 title claims abstract description 39
- 238000004132 cross linking Methods 0.000 title claims abstract description 32
- 238000002360 preparation method Methods 0.000 title abstract description 13
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 27
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 23
- 239000004088 foaming agent Substances 0.000 claims abstract description 21
- 239000012744 reinforcing agent Substances 0.000 claims abstract description 20
- 239000004094 surface-active agent Substances 0.000 claims abstract description 7
- VTYYLEPIZMXCLO-UHFFFAOYSA-L Calcium carbonate Chemical class [Ca+2].[O-]C([O-])=O VTYYLEPIZMXCLO-UHFFFAOYSA-L 0.000 claims description 9
- FAMRKDQNMBBFBR-BQYQJAHWSA-N diethyl azodicarboxylate Substances CCOC(=O)\N=N\C(=O)OCC FAMRKDQNMBBFBR-BQYQJAHWSA-N 0.000 claims description 7
- FAMRKDQNMBBFBR-UHFFFAOYSA-N ethyl n-ethoxycarbonyliminocarbamate Chemical compound CCOC(=O)N=NC(=O)OCC FAMRKDQNMBBFBR-UHFFFAOYSA-N 0.000 claims description 7
- WFUGQJXVXHBTEM-UHFFFAOYSA-N 2-hydroperoxy-2-(2-hydroperoxybutan-2-ylperoxy)butane Chemical compound CCC(C)(OO)OOC(C)(CC)OO WFUGQJXVXHBTEM-UHFFFAOYSA-N 0.000 claims description 5
- DBMJMQXJHONAFJ-UHFFFAOYSA-M Sodium laurylsulphate Chemical compound [Na+].CCCCCCCCCCCCOS([O-])(=O)=O DBMJMQXJHONAFJ-UHFFFAOYSA-M 0.000 claims description 5
- -1 sodium fatty alcohol Chemical class 0.000 claims description 5
- WYKYCHHWIJXDAO-UHFFFAOYSA-N tert-butyl 2-ethylhexaneperoxoate Chemical compound CCCCC(CC)C(=O)OOC(C)(C)C WYKYCHHWIJXDAO-UHFFFAOYSA-N 0.000 claims description 5
- ICGLPKIVTVWCFT-UHFFFAOYSA-N 4-methylbenzenesulfonohydrazide Chemical compound CC1=CC=C(S(=O)(=O)NN)C=C1 ICGLPKIVTVWCFT-UHFFFAOYSA-N 0.000 claims description 4
- GVGUFUZHNYFZLC-UHFFFAOYSA-N dodecyl benzenesulfonate;sodium Chemical compound [Na].CCCCCCCCCCCCOS(=O)(=O)C1=CC=CC=C1 GVGUFUZHNYFZLC-UHFFFAOYSA-N 0.000 claims description 4
- 239000003365 glass fiber Substances 0.000 claims description 4
- 229940080264 sodium dodecylbenzenesulfonate Drugs 0.000 claims description 4
- GJBRNHKUVLOCEB-UHFFFAOYSA-N tert-butyl benzenecarboperoxoate Chemical compound CC(C)(C)OOC(=O)C1=CC=CC=C1 GJBRNHKUVLOCEB-UHFFFAOYSA-N 0.000 claims description 4
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims description 3
- VJRITMATACIYAF-UHFFFAOYSA-N benzenesulfonohydrazide Chemical compound NNS(=O)(=O)C1=CC=CC=C1 VJRITMATACIYAF-UHFFFAOYSA-N 0.000 claims description 3
- 239000010445 mica Substances 0.000 claims description 3
- 229910052618 mica group Inorganic materials 0.000 claims description 3
- 239000000843 powder Substances 0.000 claims description 3
- VVWRJUBEIPHGQF-UHFFFAOYSA-N propan-2-yl n-propan-2-yloxycarbonyliminocarbamate Chemical compound CC(C)OC(=O)N=NC(=O)OC(C)C VVWRJUBEIPHGQF-UHFFFAOYSA-N 0.000 claims description 3
- QAOWNCQODCNURD-UHFFFAOYSA-L Sulfate Chemical compound [O-]S([O-])(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-L 0.000 claims 2
- 239000011734 sodium Substances 0.000 claims 2
- 229910052708 sodium Inorganic materials 0.000 claims 2
- 239000000454 talc Substances 0.000 claims 2
- 229910052623 talc Inorganic materials 0.000 claims 2
- 238000003756 stirring Methods 0.000 abstract description 30
- 229920006305 unsaturated polyester Polymers 0.000 abstract description 20
- 239000000203 mixture Substances 0.000 abstract description 18
- 238000000034 method Methods 0.000 abstract description 13
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- 230000000052 comparative effect Effects 0.000 description 17
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- 239000000126 substance Substances 0.000 description 6
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- 239000002253 acid Substances 0.000 description 4
- 238000002347 injection Methods 0.000 description 4
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- 239000011435 rock Substances 0.000 description 4
- 239000002689 soil Substances 0.000 description 4
- 239000003513 alkali Substances 0.000 description 3
- 229910000019 calcium carbonate Inorganic materials 0.000 description 3
- 230000006835 compression Effects 0.000 description 3
- 238000007906 compression Methods 0.000 description 3
- 230000002708 enhancing effect Effects 0.000 description 3
- 239000006260 foam Substances 0.000 description 3
- 239000003292 glue Substances 0.000 description 3
- 229920000642 polymer Polymers 0.000 description 3
- 229940051841 polyoxyethylene ether Drugs 0.000 description 3
- 229920000056 polyoxyethylene ether Polymers 0.000 description 3
- 238000007711 solidification Methods 0.000 description 3
- 230000008023 solidification Effects 0.000 description 3
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- 230000008859 change Effects 0.000 description 2
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- FPAFDBFIGPHWGO-UHFFFAOYSA-N dioxosilane;oxomagnesium;hydrate Chemical compound O.[Mg]=O.[Mg]=O.[Mg]=O.O=[Si]=O.O=[Si]=O.O=[Si]=O.O=[Si]=O FPAFDBFIGPHWGO-UHFFFAOYSA-N 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 150000002191 fatty alcohols Chemical class 0.000 description 2
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- 229920001187 thermosetting polymer Polymers 0.000 description 2
- 239000004634 thermosetting polymer Substances 0.000 description 2
- 229920006337 unsaturated polyester resin Polymers 0.000 description 2
- 229920003171 Poly (ethylene oxide) Polymers 0.000 description 1
- PMZURENOXWZQFD-UHFFFAOYSA-L Sodium Sulfate Chemical compound [Na+].[Na+].[O-]S([O-])(=O)=O PMZURENOXWZQFD-UHFFFAOYSA-L 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 150000007513 acids Chemical class 0.000 description 1
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- 230000000903 blocking effect Effects 0.000 description 1
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- 230000004048 modification Effects 0.000 description 1
- 239000003129 oil well Substances 0.000 description 1
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 description 1
- 230000035699 permeability Effects 0.000 description 1
- 238000006068 polycondensation reaction Methods 0.000 description 1
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- 229910052938 sodium sulfate Inorganic materials 0.000 description 1
- 235000011152 sodium sulphate Nutrition 0.000 description 1
- 239000011343 solid material Substances 0.000 description 1
- 230000000087 stabilizing effect Effects 0.000 description 1
- 239000012258 stirred mixture Substances 0.000 description 1
Classifications
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P20/00—Technologies relating to chemical industry
- Y02P20/141—Feedstock
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- Compositions Of Macromolecular Compounds (AREA)
Abstract
The invention discloses a low-shrinkage high-strength liquid cross-linking plugging material, which consists of the following components: 30-90 parts of unsaturated polyester; 1-5 parts of surfactant/foaming agent; 1-10 parts of curing agent/reinforcing agent. The invention also discloses a preparation method of the low-shrinkage high-strength liquid cross-linking plugging material, which comprises (1) adding a formula surfactant into the formula amount unsaturated polyester, and uniformly stirring to obtain a mixed material; (2) Adding a formula amount of curing agent into the mixture, and uniformly stirring the mixture to obtain a mixed material; (3) Adding a formula amount reinforcing agent into the mixture, and uniformly stirring the mixture to obtain a mixed material; (4) Adding a formula amount of foaming agent into the mixture, and uniformly stirring the mixture to obtain a mixed material; (5) Sealing the mixture materials, and placing the mixture materials in an oven for heating reaction to obtain the low-shrinkage high-strength liquid cross-linked plugging material. The invention also discloses a method for using the low-shrinkage high-strength liquid cross-linked plugging material as an oil field underground water shutoff profile control agent and an oil field underground crack plugging agent.
Description
Technical Field
The invention belongs to the field of functional polymers and oilfield chemical products, and particularly relates to a low-shrinkage high-strength liquid cross-linked plugging material, and a preparation method and application thereof.
Background
Most of the oil fields in China are developed to the middle and later stages, so that the stratum energy is reduced, and the recovery ratio is reduced. Due to the heterogeneity and complexity of the formation, reservoir, water "kick" and "blow-by" phenomena in the reservoir can occur. As the water injection rate increases, the non-uniformity of the water injection profile increases, resulting in a large amount of water output from the well.
Aiming at the problems of the increase of the water content of the oil field, the reduction of the water injection utilization rate and the like, the water shutoff and profile control technology is often adopted to improve the oil recovery ratio. The water shutoff and profile control technology has the working principle that a specific plugging material is used for plugging a high permeable layer, and the water absorption profile of a water injection layer section is adjusted, so that the water content of produced oil is reduced. After the chemical plugging agent is injected into the reservoir, the chemical plugging agent can be crosslinked and solidified under certain stratum temperature, pressure and other conditions, so that the permeable cracks are plugged, and the subsequent displacement process is facilitated. Unsaturated polyesters are a commonly used chemical plugging agent, typically produced by polycondensation of dibasic acids and glycols. Under the condition of underground temperature and pressure, the high-strength thermosetting polymer material can be formed through crosslinking, so that the high-strength thermosetting polymer material can be used for plugging oil reservoir cracks.
Chinese patent CN 104694096B discloses a plugging agent for oil field development, which consists of unsaturated polyester emulsion, curing agent and coupling agent. The plugging agent system is suitable for stratum with the temperature of 30-90 ℃, has strong plugging capability, good salt tolerance, long effective period and low cost, and has good plugging effect on stratum with high permeability.
The cured unsaturated polyester has higher mechanical strength in stretching, compressing, bending and other aspects, and the weight of the unsaturated polyester is 1.1-1.2 g/cm 3 The density of the polymer is such that the polymer will naturally settle to the bottom of an oil well when used as a plugging material, and the polymer can exert a long-term plugging effect due to the resistance to water, acid, alkali and other substances. However, in the curing process, the unsaturated polyester resin has a larger curing volume shrinkage rate, generally up to 7-8%, and is easy to cause shrinkage deformation of a cured product, so that the unsaturated polyester resin is not firmly contacted with underground rock and soil in the use process, looseness, falling and the like are generated, and the usability is affected. The method for reducing the volume shrinkage rate of the unsaturated polyester is to add a foaming agent, and the foaming agent can be subjected to chemical reaction or physical change under the action of underground temperature and the like to generate a large amount of gas, so that the volume after expansion can counteract the shrinkage during curing, and the shape of the material is kept stable.
Disclosure of Invention
The invention aims to: aiming at the defects of the prior art, the invention provides a low-shrinkage high-strength liquid cross-linking plugging material, a preparation method and application thereof.
The unsaturated polyester is water-resistant, acid-resistant, alkali-resistant and the like, and can play a long-acting water shutoff role in the pit. The linear skeleton main chain of the unsaturated polyester has ester bonds and carbon-carbon double bonds, has higher curing volume shrinkage, and the chemical foaming agent is added into a curing system of the unsaturated polyester, so that the volume expansion in curing can partially offset the shrinkage of resin, thereby achieving the effect of tightly connecting a plugging material with underground rock and soil and obtaining better plugging effect. Meanwhile, in order to prevent the strength of the resin matrix from being reduced due to the addition of the foaming agent, the reinforcing agent is added into the resin matrix, and in the curing process, the reinforcing agent is distributed in the resin matrix, and is partially enriched at the interface between the foam and the resin, so that the foaming agent can not only play a role in stabilizing the foam and enhancing the strength of the foam, but also play a role in enhancing the strength of the matrix, and can realize the purposes of plugging water, profile control, crack plugging, casing pipe repairing and the like in the oil field.
The technical scheme is as follows: the low-shrinkage high-strength liquid cross-linking plugging material comprises the following components in parts by weight:
further, the surfactant is one or more of sodium dodecyl sulfate, sodium dodecyl benzene sulfonate, alkylphenol polyoxyethylene and fatty alcohol polyoxyethylene sodium sulfate.
Further, the curing agent is one or more of tert-butyl peroxy-2-ethyl caproate, tert-butyl peroxybenzoate and methyl ethyl ketone peroxide.
Further, the reinforcing agent is one or more of active calcium carbonate, alumina, talcum powder, mica powder or glass fiber.
Further, the foaming agent is one or more of diethyl azodicarboxylate, diisopropyl azodicarboxylate, benzenesulfonyl hydrazide and p-toluenesulfonyl hydrazide.
A preparation method of a low-shrinkage high-strength liquid cross-linking plugging material comprises the following steps:
(1) Adding a formula amount of surfactant into the formula amount of unsaturated polyester, and uniformly stirring to obtain a mixed material;
(2) Adding a curing agent with a formula amount into the mixed material obtained in the step (1), and uniformly stirring to obtain the mixed material;
(3) Adding a formula amount of reinforcing agent into the mixed material obtained in the step (2), and uniformly stirring to obtain the mixed material;
(4) Adding a foaming agent with a formula amount into the mixed material obtained in the step (3), and uniformly stirring to obtain the mixed material;
(5) And (3) sealing the mixture material obtained in the step (4), and placing the mixture material in an oven for heating reaction to obtain the low-shrinkage high-strength liquid cross-linked plugging material.
Further, the mixture in the step (5) is reacted in an oven at 90-150 ℃ for 2-24 h.
The low-shrinkage high-strength liquid cross-linking plugging material is used as an underground water plugging profile control agent for an oil field.
The low-shrinkage high-strength liquid cross-linking plugging material is used as an oilfield downhole crack plugging agent.
The invention has the following effects: the low-shrinkage high-strength liquid cross-linking plugging material and the preparation method thereof disclosed by the invention have the following beneficial effects:
1. the plugging material provided by the invention is a solid material with good mechanical properties, acid and alkali resistance and the like after being crosslinked, and is suitable for plugging an underground water outlet layer;
2. the foaming agent is added in the plugging material provided by the invention, so that the foaming agent can be foamed in an underground environment to promote the volume expansion of a resin matrix, thereby reducing the solidification volume shrinkage rate of unsaturated polyester, enhancing the connection performance between the resin and underground rock and soil and improving the plugging effect;
3. the reinforcing agent is added into the plugging material provided by the invention, so that the strength reduction possibly caused by the addition of the foaming agent can be compensated, and the good mechanical property of the matrix resin can be maintained.
4. The preparation method is simple and easy to implement, has good effect and higher application value.
Drawings
FIG. 1 is a graph showing the mechanical properties of examples 1-4 and comparative examples 1-2 under test conditions.
The specific embodiment is as follows:
the following detailed description of specific embodiments of the invention.
The following examples will provide those skilled in the art with a more complete understanding of the present invention and are not intended to limit the scope of the present invention in any way.
The characterization method of the invention is as follows:
the rheological property testing method comprises the following steps: the viscosity was measured using an RS6000 rotarheometer manufactured by HAAKE corporation, germany, and the dynamic viscosity at the time of the initial curing of the liquid resin curing system was measured at room temperature using a twin cylinder method.
The mechanical property testing method comprises the following steps: and (3) standing the uniformly stirred mixture for a period of time (no bubbles exist), then injecting the mixture into a compression mold, then placing the compression mold into 120 ℃ for solidification, taking out solidified compression bars after 12 hours, and carrying out compression test. The resulting bars were cylindrical bars, 12mm in diameter and about 30mm in height. The compression test adopts a Zwick/Roell Z020 universal material tester, the force sensing type is 20kN, the preload force is 3N, the elastic modulus speed is 1mm/min, and the test temperature is room temperature. At least 5 bars per sample were tested in parallel and the results averaged.
The method for testing the shrinkage rate of the solidified volume comprises the following steps: the cured volume shrinkage of the samples was measured using a density method. First, the density of the glue solution prepared before curing was measured by a densitometer and found to be ρ1. In a mold of a certain shape, a grinding tool is cast, and after solidification, the density of a casting body is measured to be ρ2 by using a buoyancy method with reference to national standard GB 1463. With a cure volume shrinkage of Vs, the cure volume shrinkage of the resin can be calculated according to the following equation:
V s ＝(ρ 2 -ρ 1 )/ρ 2 ×100％
example 1
The low-shrinkage high-strength liquid cross-linking plugging material comprises the following components in parts by weight:
the preparation method of the low-shrinkage high-strength liquid cross-linking plugging material comprises the following steps:
(1) Adding 2 parts of sodium dodecyl sulfate into 70 parts of unsaturated polyester, and uniformly stirring to obtain a mixed material;
(2) Adding 5 parts of tert-butyl peroxy-2-ethyl hexanoate into the mixture, and uniformly stirring to obtain the mixture;
(3) Adding 5 parts of active calcium carbonate into the mixed material, and uniformly stirring to obtain the mixed material;
(4) Adding 3 parts of diethyl azodicarboxylate into the mixed material, and uniformly stirring to obtain the mixed material;
(5) And (3) sealing the mixed material, and placing the sealed mixed material in a baking oven at 120 ℃ for reaction for 12 hours to obtain the low-shrinkage high-strength liquid cross-linking plugging material.
The low-shrinkage high-strength liquid cross-linking plugging material is used as an underground water plugging profile control agent for an oil field.
The low-shrinkage high-strength liquid cross-linking plugging material is used as an oilfield downhole crack plugging agent.
Example 2
The low-shrinkage high-strength liquid cross-linking plugging material comprises the following components in parts by weight:
a preparation method of a low-shrinkage high-strength liquid cross-linking plugging material comprises the following steps:
(1) Adding 2 parts of sodium dodecyl benzene sulfonate into 90 parts of unsaturated polyester, and uniformly stirring to obtain a mixed material;
(2) Adding 2 parts of tert-butyl peroxy-2-ethyl hexanoate into the mixture, and uniformly stirring the mixture;
(3) Adding 1 part of aluminum oxide into the mixed material, and uniformly stirring to obtain the mixed material;
(4) Adding 5 parts of diethyl azodicarboxylate into the mixed material, and uniformly stirring to obtain the mixed material;
(5) Sealing the mixed material, and placing the sealed material in a 90 ℃ oven for reaction for 24 hours to obtain the low-shrinkage high-strength liquid cross-linked plugging material.
The low-shrinkage high-strength liquid cross-linking plugging material is used as an underground water plugging profile control agent for an oil field.
The low-shrinkage high-strength liquid cross-linking plugging material is used as an oilfield downhole crack plugging agent.
Example 3
The low-shrinkage high-strength liquid cross-linking plugging material comprises the following components in parts by weight:
a preparation method of a low-shrinkage high-strength liquid cross-linking plugging material comprises the following steps:
(1) Adding 1 part of alkylphenol polyoxyethylene ether into 50 parts of unsaturated polyester, and uniformly stirring to obtain a mixed material;
(2) Adding 4 parts of methyl ethyl ketone peroxide into the mixed material, and uniformly stirring to obtain the mixed material;
(3) Adding 10 parts of talcum powder into the mixed material, and uniformly stirring to obtain the mixed material;
(4) Adding 4 parts of diethyl azodicarboxylate into the mixed material, and uniformly stirring to obtain the mixed material;
(5) Sealing the mixed material, and placing the sealed material in a baking oven at 150 ℃ for 2 hours to obtain the low-shrinkage high-strength liquid cross-linking plugging material.
The low-shrinkage high-strength liquid cross-linking plugging material is used as an underground water plugging profile control agent for an oil field.
The low-shrinkage high-strength liquid cross-linking plugging material is used as an oilfield downhole crack plugging agent.
Example 4
The low-shrinkage high-strength liquid cross-linking plugging material comprises the following components in parts by weight:
a preparation method of a low-shrinkage high-strength liquid cross-linking plugging material comprises the following steps:
(1) Adding 5 parts of fatty alcohol polyoxyethylene ether sodium sulfate into 30 parts of unsaturated polyester, and uniformly stirring to obtain a mixed material;
(2) Adding 10 parts of tert-butyl peroxybenzoate into the mixed material, and uniformly stirring to obtain the mixed material;
(3) Adding 9 parts of glass fibers into the mixed material, and uniformly stirring to obtain the mixed material;
(4) Adding 1 part of p-toluenesulfonyl hydrazine into the mixed material, and uniformly stirring to obtain the mixed material;
(5) Sealing the mixed material, and placing the sealed material in a baking oven at 120 ℃ for reaction for 12 hours to obtain the low-shrinkage high-strength liquid cross-linking plugging material.
The low-shrinkage high-strength liquid cross-linking plugging material is used as an underground water plugging profile control agent for an oil field.
The low-shrinkage high-strength liquid cross-linking plugging material is used as an oilfield downhole crack plugging agent.
Comparative example 1
The plugging material without the foaming agent comprises the following components in parts by weight:
the preparation method of the plugging material without the foaming agent comprises the following steps:
(1) Adding 2 parts of sodium dodecyl sulfate into 71 parts of unsaturated polyester, and uniformly stirring to obtain a mixed material;
(2) Adding 5 parts of tert-butyl peroxy-2-ethyl hexanoate into the mixture, and uniformly stirring to obtain the mixture;
(3) Adding 5 parts of active calcium carbonate into the mixed material, and uniformly stirring to obtain the mixed material;
(4) Sealing the mixed material, and placing the sealed material in a baking oven at 120 ℃ for reacting for 12 hours to obtain the plugging material.
Comparative example 2
The plugging material without the reinforcing agent comprises the following components in parts by weight:
a method of preparing a plugging material without added reinforcing agent comprising:
(1) Adding 5 parts of alkylphenol polyoxyethylene ether into 85 parts of unsaturated polyester, and uniformly stirring to obtain a mixed material;
(2) Adding 7 parts of methyl ethyl ketone peroxide into the mixed material, and uniformly stirring to obtain the mixed material;
(3) Adding 4 parts of diethyl azodicarboxylate into the mixed material, and uniformly stirring to obtain the mixed material;
(4) Sealing the mixed material, and placing the sealed material in a baking oven at 120 ℃ for reaction for 12 hours to obtain the plugging material without the reinforcing agent.
The plugging materials obtained in examples 1 to 4 and comparative examples 1 to 2 were tested for rheological properties, mechanical properties and cure volume shrinkage, respectively, according to the methods described above.
Rheological properties
Table 1 shows the results of the dynamic viscosity test of the glue solutions of examples 1-4 and comparative examples 1, 2 when the glue solutions were uncured. When the shear rate was varied between 1 and 200r/s, the viscosity was almost unchanged, and the viscosity data with a shear rate of 100r/s was selected as the viscosity of the resin system.
TABLE 1 dynamic viscosity test results
As can be seen from table 1, the viscosity of the unsaturated polyester plugging material only changed with the change in the addition amount of the reinforcing agent in the plugging material. As shown in comparative example 2, the viscosity of the resin system to which the reinforcing agent was not added was 285 mPas, and after the reinforcing agent was added, the viscosity of the system increased to 400 to 500 mPas.
As can be seen from example 3, as the reinforcing agent was further increased, the viscosity increased to about 600 mPas. All examples and enhancements have viscosities less than 1Pa s and exhibit good flow behavior in the period of time during which curing begins, exhibiting typical newtonian flow behavior, and being suitable for in situ applications.
Mechanical properties
The cured plugging materials of examples 1-4 and comparative examples 1-2 were tested for compressive properties, respectively, to measure the mechanical properties of the materials.
Table 2 shows the results of the initial cure times and mechanical properties of the samples of examples 1-4 and comparative examples 1, 2. FIG. 1 is a graph showing the mechanical properties of examples 1-4 and comparative examples 1-2 under test conditions. As shown in FIG. 1, the compressive strength of all the samples of the examples was greatly improved compared with that of the comparative example 2, the compressive strength of the comparative example 2 without the reinforcing agent was 28.1MPa, the compressive strength of the comparative example 1 with the activated calcium carbonate was 37.2MPa, and the mechanical properties were greatly improved.
TABLE 2 results of mechanical Properties test
| Sample of | Compressive strength (MPa) | Modulus of elasticity (MPa) |
| Example 1 | 39.2 | 158 |
| Example 2 | 42.6 | 356 |
| Example 3 | 68.5 | 347 |
| Example 4 | 50.9 | 315 |
| Comparative example 1 | 43.1 | 283 |
| Comparative example 2 | 28.1 | 112 |
Shrinkage rate of cured volume
It can be seen from examples 1, 2 and comparative example 1 that the addition of different kinds of foaming agents does not affect the strength of the cured material. Therefore, in order to compensate for the possible decrease of mechanical properties caused by volume expansion, only the addition of the reinforcing agent is needed, and the influence of different foaming agent types on the material strength is not needed.
Table 3 shows the results of the cure volume shrinkage test for the samples of examples 1-4 and comparative examples 1, 2.
TABLE 3 test results of cure volume shrinkage
As is clear from the data in table 3, when no foaming agent was added, the shrinkage rate of the cured volume of the unsaturated polyester plugging material was 9%, which indicates that the volume was largely shrunk during the curing process, and the adhesiveness between the matrix resin and the surrounding rock and soil was lowered, and the plugging was not effective. It can be seen from example 1 and comparative example 1 that the curing volume shrinkage of the resin system is greatly reduced from 9% to 1.1% after adding a certain amount of the foaming agent and the reinforcing agent, and the blocking performance can be effectively improved.
Examples 5 to 7
Substantially the same as in example 1, the difference is only that: the types of surfactants are different:
examples 8 to 10
Substantially the same as in example 1, the difference is only that: the types of curing agents are different:
examples 11 to 13
Substantially the same as in example 1, the difference is only that: the reinforcing agents are different:
examples 14 to 16
Substantially the same as in example 1, the difference is only that: the foaming agents are different:
the embodiments of the present invention have been described in detail. However, the present invention is not limited to the above-described embodiments, and various modifications may be made within the knowledge of those skilled in the art without departing from the spirit of the present invention.
Claims (10)
1. The application of the low-shrinkage high-strength liquid cross-linked plugging material as an underground water shutoff profile control agent of an oil field, wherein:
the low-shrinkage high-strength liquid cross-linking plugging material comprises the following components in parts by weight:
2. the use according to claim 1, wherein the surfactant is one or more of sodium dodecyl sulfate, sodium dodecyl benzene sulfonate, alkylphenol ethoxylates and sodium fatty alcohol ethoxylate sulfate.
3. The use according to claim 1, wherein the curing agent is one or more of tert-butyl peroxy-2-ethylhexanoate, tert-butyl peroxybenzoate and methyl ethyl ketone peroxide.
4. The use according to claim 1, wherein the reinforcing agent is one or more of activated calcium carbonate, alumina, talc, mica powder or glass fiber.
5. The use according to claim 1, wherein the foaming agent is one or more of diethyl azodicarboxylate, diisopropyl azodicarboxylate, benzenesulfonyl hydrazide and p-toluenesulfonyl hydrazide.
6. The application of the low-shrinkage high-strength liquid crosslinked plugging material as an oilfield downhole crack plugging agent comprises the following steps:
the low-shrinkage high-strength liquid cross-linking plugging material comprises the following components in parts by weight:
7. the use according to claim 6, wherein the surfactant is one or more of sodium dodecyl sulfate, sodium dodecyl benzene sulfonate, alkylphenol ethoxylates and sodium fatty alcohol ethoxylate sulfate.
8. The use according to claim 6, wherein the curing agent is one or more of tert-butyl peroxy-2-ethylhexanoate, tert-butyl peroxybenzoate and methyl ethyl ketone peroxide.
9. The use according to claim 6, wherein the reinforcing agent is one or more of activated calcium carbonate, alumina, talc, mica powder or glass fiber.
10. The use according to claim 6, wherein the foaming agent is one or more of diethyl azodicarboxylate, diisopropyl azodicarboxylate, benzenesulfonyl hydrazide and p-toluenesulfonyl hydrazide.
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| CN111218264A (en) * | 2018-11-27 | 2020-06-02 | 中国石油化工股份有限公司 | Resin plugging agent and preparation method thereof |
| CN112962577A (en) * | 2021-05-18 | 2021-06-15 | 北京城建道桥建设集团有限公司 | Water-carrying grouting plugging structure and plugging method for large-flow leakage stratum |
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| CN103936940A (en) * | 2014-04-25 | 2014-07-23 | 常州工程职业技术学院 | Compound unsaturated polyester resin foam insulation material and preparation method thereof |
| CN108641691A (en) * | 2018-03-27 | 2018-10-12 | 中国石油大学(华东) | A kind of high-intensity resin blocking agent and the preparation method and application thereof |
| CN111218264A (en) * | 2018-11-27 | 2020-06-02 | 中国石油化工股份有限公司 | Resin plugging agent and preparation method thereof |
| CN112962577A (en) * | 2021-05-18 | 2021-06-15 | 北京城建道桥建设集团有限公司 | Water-carrying grouting plugging structure and plugging method for large-flow leakage stratum |
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