CN115772392A - High-polymer oil-based crosslinking curing plugging agent for drilling fluid and preparation method thereof - Google Patents
High-polymer oil-based crosslinking curing plugging agent for drilling fluid and preparation method thereof Download PDFInfo
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- CN115772392A CN115772392A CN202111042564.8A CN202111042564A CN115772392A CN 115772392 A CN115772392 A CN 115772392A CN 202111042564 A CN202111042564 A CN 202111042564A CN 115772392 A CN115772392 A CN 115772392A
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- 238000005553 drilling Methods 0.000 title claims abstract description 45
- 239000012530 fluid Substances 0.000 title claims abstract description 41
- 238000004132 cross linking Methods 0.000 title claims abstract description 26
- 229920000642 polymer Polymers 0.000 title claims abstract description 18
- 238000002360 preparation method Methods 0.000 title claims abstract description 18
- 239000003822 epoxy resin Substances 0.000 claims abstract description 162
- 229920000647 polyepoxide Polymers 0.000 claims abstract description 162
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 66
- 239000002002 slurry Substances 0.000 claims abstract description 20
- 239000012744 reinforcing agent Substances 0.000 claims abstract description 17
- 238000003756 stirring Methods 0.000 claims description 26
- 238000002156 mixing Methods 0.000 claims description 23
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 20
- 239000004593 Epoxy Substances 0.000 claims description 19
- 229920000459 Nitrile rubber Polymers 0.000 claims description 19
- 125000003178 carboxy group Chemical group [H]OC(*)=O 0.000 claims description 19
- 239000000741 silica gel Substances 0.000 claims description 17
- 229910002027 silica gel Inorganic materials 0.000 claims description 17
- 229920000768 polyamine Polymers 0.000 claims description 14
- RAXXELZNTBOGNW-UHFFFAOYSA-N imidazole Natural products C1=CNC=N1 RAXXELZNTBOGNW-UHFFFAOYSA-N 0.000 claims description 12
- 238000006243 chemical reaction Methods 0.000 claims description 11
- 125000001931 aliphatic group Chemical group 0.000 claims description 9
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 8
- 238000001816 cooling Methods 0.000 claims description 8
- 238000011049 filling Methods 0.000 claims description 8
- VTYYLEPIZMXCLO-UHFFFAOYSA-L Calcium carbonate Chemical compound [Ca+2].[O-]C([O-])=O VTYYLEPIZMXCLO-UHFFFAOYSA-L 0.000 claims description 6
- 239000000203 mixture Substances 0.000 claims description 6
- 125000003118 aryl group Chemical group 0.000 claims description 5
- 239000002041 carbon nanotube Substances 0.000 claims description 5
- 229910021393 carbon nanotube Inorganic materials 0.000 claims description 5
- 238000000034 method Methods 0.000 claims description 5
- 239000000835 fiber Substances 0.000 claims description 4
- 229920000728 polyester Polymers 0.000 claims description 4
- 150000003512 tertiary amines Chemical class 0.000 claims description 4
- 229910000019 calcium carbonate Inorganic materials 0.000 claims description 3
- 239000006229 carbon black Substances 0.000 claims description 3
- 229910021389 graphene Inorganic materials 0.000 claims description 3
- 229920002521 macromolecule Polymers 0.000 claims description 3
- 239000002131 composite material Substances 0.000 claims description 2
- 230000000694 effects Effects 0.000 abstract description 6
- 239000000463 material Substances 0.000 description 8
- 230000032683 aging Effects 0.000 description 7
- 238000012360 testing method Methods 0.000 description 6
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 6
- OSSNTDFYBPYIEC-UHFFFAOYSA-N 1-ethenylimidazole Chemical compound C=CN1C=CN=C1 OSSNTDFYBPYIEC-UHFFFAOYSA-N 0.000 description 3
- 238000011161 development Methods 0.000 description 3
- 230000018109 developmental process Effects 0.000 description 3
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- 238000012986 modification Methods 0.000 description 3
- 230000004048 modification Effects 0.000 description 3
- WZCQRUWWHSTZEM-UHFFFAOYSA-N 1,3-phenylenediamine Chemical group NC1=CC=CC(N)=C1 WZCQRUWWHSTZEM-UHFFFAOYSA-N 0.000 description 2
- -1 amino, carboxyl Chemical group 0.000 description 2
- 239000012267 brine Substances 0.000 description 2
- 239000004568 cement Substances 0.000 description 2
- 230000006835 compression Effects 0.000 description 2
- 238000007906 compression Methods 0.000 description 2
- 150000004985 diamines Chemical class 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 125000003700 epoxy group Chemical group 0.000 description 2
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- HPALAKNZSZLMCH-UHFFFAOYSA-M sodium;chloride;hydrate Chemical compound O.[Na+].[Cl-] HPALAKNZSZLMCH-UHFFFAOYSA-M 0.000 description 2
- RPNUMPOLZDHAAY-UHFFFAOYSA-N Diethylenetriamine Chemical compound NCCNCCN RPNUMPOLZDHAAY-UHFFFAOYSA-N 0.000 description 1
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 description 1
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- 238000010276 construction Methods 0.000 description 1
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- 229920001971 elastomer Polymers 0.000 description 1
- 238000001914 filtration Methods 0.000 description 1
- 239000000499 gel Substances 0.000 description 1
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- LNEPOXFFQSENCJ-UHFFFAOYSA-N haloperidol Chemical compound C1CC(O)(C=2C=CC(Cl)=CC=2)CCN1CCCC(=O)C1=CC=C(F)C=C1 LNEPOXFFQSENCJ-UHFFFAOYSA-N 0.000 description 1
- 229940018564 m-phenylenediamine Drugs 0.000 description 1
- FPYJFEHAWHCUMM-UHFFFAOYSA-N maleic anhydride Chemical compound O=C1OC(=O)C=C1 FPYJFEHAWHCUMM-UHFFFAOYSA-N 0.000 description 1
- 239000011159 matrix material Substances 0.000 description 1
- WCPAKWJPBJAGKN-UHFFFAOYSA-N oxadiazole Chemical compound C1=CON=N1 WCPAKWJPBJAGKN-UHFFFAOYSA-N 0.000 description 1
- 125000003367 polycyclic group Chemical group 0.000 description 1
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- 239000011347 resin Substances 0.000 description 1
- 238000007789 sealing Methods 0.000 description 1
- 239000011780 sodium chloride Substances 0.000 description 1
- 239000000243 solution Substances 0.000 description 1
- 238000010998 test method Methods 0.000 description 1
- 239000012745 toughening agent 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)
- Epoxy Resins (AREA)
Abstract
The invention relates to the technical field of leakage control and plugging of oil and gas drilling, in particular to a high polymer oil-based crosslinking curing plugging agent for drilling fluid and a preparation method thereof, wherein the plugging agent comprises the following components in percentage by mass: 60-80% of modified epoxy resin, 15-30% of curing agent, 1-5% of curing regulator and 4-10% of reinforcing agent; the preparation method comprises the steps of preparing modified epoxy resin, preparing epoxy resin slurry and curing treatment. The plugging agent and the preparation method thereof can effectively solve the problems of poor pollution resistance and poor plugging effect.
Description
Technical Field
The invention relates to the technical field of leakage control and plugging of oil and gas drilling, in particular to a high polymer oil-based cross-linking curing plugging agent for drilling fluid and a preparation method thereof.
Background
Along with the continuous deepening of exploration and development of unconventional oil and gas resources such as shale gas and the like and the continuous expansion of drilling scales of risk exploratory wells, development wells and the like in complex areas, the demand on the oil-based drilling fluid is more and more extensive, the development and application of a leakage stopping technology of the oil-based drilling fluid as a matching technology of the oil-based drilling fluid are immature, and particularly, a technical means for effectively treating the oil-based drilling fluid leakage caused by the well leakage on site is lacked due to the lack of a special leakage stopping agent for the oil-based drilling fluid with good leakage stopping effect and high leakage stopping success rate. At present, most of materials used for field oil-based drilling fluid plugging are conventional bridge plug plugging materials for water-based drilling fluid, the plugging success rate is not high, and once the oil-based drilling fluid is leaked and is difficult to effectively solve, more serious loss is caused, even a series of complex conditions such as drilling sticking, blowout, well collapse and the like occur.
The self-deformation capability of the plugging material in the plugging process is poor or the plugging material basically does not have the deformation capability, and the size and the shape of the plugging material are not matched with the pore and the crack of the leaking layer, so that the plugging material is difficult to enter the leaking layer and only can form accumulation on the surface of the leaking layer to form a door sealing phenomenon; the conventional plugging material has insufficient pressure bearing capacity and fails to play a role in effectively plugging formation fracture pores; the plugging material with certain deformation capacity, such as cement paste or gel plugging agent, has the cementing and setting time which is difficult to control, or is quickly diluted underground, has not reached the ideal curing strength under the action of high temperature and high pressure, is lost and cannot form a complete cured body; high filtration loss and cement slurry leakage stoppage are still insufficient in the aspects of construction safety, pollution resistance and the like.
Disclosure of Invention
In order to solve the technical problems, the invention provides a high-molecular oil-based crosslinking curing plugging agent for drilling fluid and a preparation method thereof, which can effectively solve the problems of poor pollution resistance and poor plugging effect.
The invention is realized by adopting the following technical scheme:
a macromolecule oil-based crosslinking curing plugging agent for drilling fluid is characterized in that: the composite material comprises the following components in percentage by mass: 60-80% of modified epoxy resin, 15-30% of curing agent, 1-5% of curing regulator and 4-10% of reinforcing agent.
The modified epoxy resin is obtained by mixing modified first epoxy resin with second epoxy resin, wherein the viscosity of the first epoxy resin is greater than that of the second epoxy resin.
The first epoxy resin is epoxy resin E-51, and the second epoxy resin is epoxy resin E-44.
The epoxy value of the epoxy resin E-51 is 0.48 to 0.54, and the viscosity is 10-169a.s; the epoxy value of the epoxy resin E-44 is 0.41 to 0.47.
The curing agent is one or a mixture of aliphatic polyamine and aromatic polyamine.
The curing regulator is one or a mixture of tertiary amine and imidazole.
The reinforcing agent is one or a mixture of more of graphene, nano calcium carbonate, carbon nano tubes, white carbon black and short-cut polyester fibers.
A preparation method of a macromolecule oil-based crosslinking curing plugging agent for drilling fluid is characterized by comprising the following steps: the method comprises the following steps:
S 1 preparing modified epoxy resin;
S 2 adding other components into the modified epoxy resin, and slowly stirring until the components are uniformly mixed to obtain bubble-free epoxy resin slurry;
S 3 and filling the epoxy resin slurry into a silica gel mold, putting the silica gel mold into an oven, and carrying out curing reaction at 120 ℃.
Said step S 1 The preparation of the modified epoxy resin specifically comprises the following steps:
S 11 preparing epoxy resin E-51, epoxy resin E-44 and 10% of carboxyl nitrile rubber;
S 12 adding the carboxyl nitrile rubber into the epoxy resin E-51, and stirring at 140 ℃;
S 13 stirring for 2 hours and then cooling to room temperature;
S 14 then adding epoxy resin E-44, and mixing uniformly to obtain the modified epoxy resin.
Compared with the prior art, the invention has the beneficial effects that:
1. the curing plugging agent is a cross-linking curing plugging agent which is not melted and dissolved and has a three-dimensional network structure through the chemical reaction between amino, carboxyl, anhydride, oxadiazole and other groups and polycyclic groups of a resin matrix with a linear or branched molecular structure. The cross-linking curing plugging agent has curing strength of over 30MPa, is in a flowing state before curing, can plug longitudinal bottom cracks, and has no obvious strength attenuation after aging at 160 ℃.
2. The cross-linking curing plugging agent can resist the pollution of drilling fluids such as water-based drilling fluid, oil-based drilling fluid, brine and the like, the concentration of an epoxy resin curing system is not obviously changed under the condition of no stirring, and the plugging agent can still be cured, thereby playing the roles of treating leakage and plugging.
3. According to the invention, two epoxy resins are mixed for use, the epoxy resin E-51 is used for modifying with carboxyl nitrile rubber, the viscosity of the modified epoxy resin E-51 is increased, and the modified epoxy resin E-51 still has good fluidity, so that the pumpable requirement of the mud pump for a drilling site is met; due to the reaction of the epoxy groups with the carboxyl groups of the carboxylated nitrile rubber, the modified epoxy groups are reduced and still the effect of being crosslinkable by the crosslinking agent is met. Then mixing with epoxy resin E-44 with slightly low viscosity and epoxy value, and taking the epoxy resin E-51 modified by the carboxyl nitrile rubber as a toughening agent as a whole, so that the finally obtained plugging agent has better plugging effect.
Detailed Description
Example 1
The invention discloses a polymer oil-based crosslinking curing plugging agent for drilling fluid, which comprises the following components in percentage by mass: 60% of modified epoxy resin, 30% of curing agent, 1% of curing regulator and 9% of reinforcing agent. The modified epoxy resin is obtained by mixing modified first epoxy resin with second epoxy resin, wherein the first epoxy resin is epoxy resin E-51 with the epoxy value of 0.54 and the viscosity of 169a.s, and the second epoxy resin is epoxy resin E-44 with the epoxy value of 0.41. The curing agent is formed by mixing aromatic polyamine and aliphatic polyamine according to the mass ratio of 2. The curing regulator is imidazole, and is particularly vinyl imidazole. The reinforcing agent is nano calcium carbonate.
The preparation method of the curing plugging agent comprises the following steps:
S 1 preparing the modified epoxy resin, specifically comprising:
S 11 preparing epoxy resin E-51, epoxy resin E-44 and 10% of carboxyl nitrile rubber;
S 12 adding the carboxyl nitrile rubber into the epoxy resin E-51, and stirring at 140 ℃;
S 13 stirring for 2 hours and then cooling to room temperature;
S 14 then adding epoxy resin E-44, and mixing uniformly to obtain the modified epoxy resin.
S 2 Adding other components into the modified epoxy resin, and slowly stirring until the components are uniformly mixed to obtain the bubble-free epoxy resin slurry.
S 3 And filling the epoxy resin slurry into a silica gel mold, putting the silica gel mold into an oven, and carrying out curing reaction at 120 ℃.
Example 2
The invention discloses a polymer oil-based crosslinking curing plugging agent for drilling fluid, which comprises the following components in percentage by mass: 70% of modified epoxy resin, 20% of curing agent, 2% of curing regulator and 8% of reinforcing agent. The modified epoxy resin is obtained by mixing a first epoxy resin with a second epoxy resin after modification, wherein the first epoxy resin is an epoxy resin E-51 with an epoxy value of 0.48 and a viscosity of 12Pa.s, and the second epoxy resin is an epoxy resin E-44 with an epoxy value of 0.45. The curing agent is aliphatic polyamine; the aliphatic polyamine selects iso-fluorine pre-pregnane diamine and diethylenetriamine which are mixed according to the mass ratio of 1:1 are mixed. The curing regulator is imidazole, and is particularly vinyl imidazole. The reinforcing agent is white carbon black.
The preparation method of the curing plugging agent comprises the following steps:
S 1 preparing the modified epoxy resin, specifically comprising:
S 11 preparing epoxy resin E-51, epoxy resin E-44 and 10% of carboxyl nitrile rubber;
S 12 adding the carboxyl nitrile rubber into the epoxy resin E-51, and stirring at 140 ℃;
S 13 stirring for 2 hours and then cooling to room temperature;
S 14 then adding epoxy resin E-44, and mixing uniformly to obtain the modified epoxy resin.
S 2 Adding other components into the modified epoxy resin, and slowly stirring until the components are uniformly mixed to obtain the bubble-free epoxy resin slurry.
S 3 And filling the epoxy resin slurry into a silica gel mold, putting the silica gel mold into an oven, and carrying out curing reaction at 120 ℃.
The anti-pollution capability of the plugging agent provided by the embodiment is tested, and the test method is as follows:
an epoxy resin curing system (modified epoxy resin +20% curing agent J +2% curing accelerator +8% reinforcing agent) is prepared in a clean 100mL beaker, and 40mL of 20% volume fraction (8 mL) of contaminated fluid (clear water, 10% saline water, water-based drilling fluids with densities of 1.6g/cm3 and 2.0g/cm3, and oil-based drilling fluid with density of 2.0g/cm 3) is slowly added respectively. The curing reaction was carried out at 120 ℃ with and without stirring, respectively, and the curing time was measured, and it was considered that the epoxy resin curing system was not cured after being contaminated if the curing was not completely cured within 6 hours.
Wherein the curing time determination specifically refers to: observations were made every 5 minutes and the epoxy cure time was reported as the time the glass rod could not be inserted into the epoxy slurry in the mold. The results of the experiments are shown in the following table:
the data in the table show that the cross-linking curing plugging agent can resist the pollution of drilling fluids such as water-based drilling fluid, oil-based drilling fluid, brine and the like, can be cured, and has the effects of treating leakage and plugging.
Example 3
The invention discloses a polymer oil-based crosslinking curing plugging agent for drilling fluid, which comprises the following components in percentage by mass: 65% of modified epoxy resin, 24% of curing agent, 2% of curing regulator and 9% of reinforcing agent. The modified epoxy resin is obtained by mixing a first epoxy resin with a second epoxy resin after modification, wherein the first epoxy resin is an epoxy resin E-51 with an epoxy value of 0.50 and a viscosity of 10Pa.s, and the second epoxy resin is an epoxy resin E-44 with an epoxy value of 0.47. The curing agent is aromatic polyamine and aliphatic polyamine, and the mass ratio of the curing agent is 2:1, mixing; the aromatic polyamine is metaphenylene diamine, and the aliphatic polyamine is isofluo-tropine diamine. The curing regulator is imidazole, and is particularly vinyl imidazole. The reinforcing agent is formed by mixing carbon nanotubes and graphene according to a mass ratio of 2.
The preparation method of the curing plugging agent comprises the following steps:
S 1 preparing the modified epoxy resin, which specifically comprises:
S 11 preparing epoxy resin E-51, epoxy resin E-44 and 10% of carboxyl nitrile rubber;
S 12 adding the carboxyl nitrile rubber into the epoxy resin E-51, and stirring at 140 ℃;
S 13 stirring for 2 hours and then cooling to room temperature;
S 14 then adding epoxy resin E-44, and mixing uniformly to obtain the modified epoxy resin.
S 2 Adding other components into the modified epoxy resin, and slowly stirring until the components are uniformly mixed to obtain the bubble-free epoxy resin slurry.
S 3 And filling the epoxy resin slurry into a silica gel mold, putting the silica gel mold into an oven, and carrying out curing reaction at 120 ℃.
Example 4
The invention discloses a polymer oil-based crosslinking curing plugging agent for drilling fluid, which comprises the following components in percentage by mass: 80% of modified epoxy resin, 15% of curing agent, 1% of curing regulator and 4% of reinforcing agent. The modified epoxy resin is obtained by mixing a first epoxy resin with a second epoxy resin after modification, wherein the first epoxy resin is an epoxy resin E-51 with an epoxy value of 0.52 and a viscosity of 11Pa.s, and the second epoxy resin is an epoxy resin E-44 with an epoxy value of 0.45. The curing agent is formed by mixing m-phenylenediamine and maleic anhydride according to the mass ratio of 2.
The preparation method of the curing plugging agent comprises the following steps:
S 1 preparing the modified epoxy resin, which specifically comprises:
S 11 preparing epoxy resin E-51, epoxy resin E-44 and 10% of carboxyl nitrile rubber;
S 12 adding the carboxyl nitrile rubber into the epoxy resin E-51, and stirring at 140 ℃;
S 13 stirring for 2 hours and then cooling to room temperature;
S 14 then adding epoxy resin E-44, and mixing uniformly to obtain the modified epoxy resin.
S 2 Adding other components into the modified epoxy resin, and slowly stirring until the components are uniformly mixed to obtain the bubble-free epoxy resin slurry.
S 3 And filling the epoxy resin slurry into a silica gel mold, putting the silica gel mold into an oven, and carrying out curing reaction at 120 ℃.
Example 5
The invention discloses a polymer oil-based crosslinking curing plugging agent for drilling fluid, which comprises the following components in percentage by mass: 75% of modified epoxy resin, 15% of curing agent, 5% of curing regulator and 5% of reinforcing agent. The modified epoxy resin is obtained by mixing modified first epoxy resin with second epoxy resin, wherein the first epoxy resin is epoxy resin E-51 with the epoxy value of 0.49 and the viscosity of 169a.s, and the second epoxy resin is epoxy resin E-44 with the epoxy value of 0.43. The curing agent is aliphatic polyamine, and specifically selects the iso-fluorine Bayer diamine. The curing regulator is tertiary amine, and the reinforcing agent is formed by mixing chopped polyester fibers and carbon nanotubes according to a mass ratio of 1.
The preparation method of the curing plugging agent comprises the following steps:
S 1 preparing the modified epoxy resin, which specifically comprises:
S 11 preparing epoxy resin E-51, epoxy resin E-44 and 10% of carboxyl nitrile rubber;
S 12 adding the carboxyl nitrile rubber into the epoxy resin E-51, and stirring at 140 ℃;
S 13 stirring for 2 hours and then cooling to room temperature;
S 14 then adding epoxy resin E-44, and mixing uniformly to obtain the modified epoxy resin.
S 2 Adding other components into the modified epoxy resin, and slowly stirring until the components are uniformly mixed to obtain the bubble-free epoxy resin slurry.
S 3 And filling the epoxy resin slurry into a silica gel mold, putting the silica gel mold into an oven, and carrying out curing reaction at 120 ℃.
Example 6
The invention comprises a high polymer oil-based crosslinking curing plugging agent for drilling fluid, which comprises the following components in percentage by mass: 70% of modified epoxy resin, 19% of curing agent, 1% of curing regulator and 10% of reinforcing agent. The modified epoxy resin is obtained by mixing a modified first epoxy resin with a second epoxy resin, wherein the first epoxy resin is an epoxy resin E-51 with the epoxy value of 0.53 and the viscosity of 12Pa.s, and the second epoxy resin is an epoxy resin E-44 with the epoxy value of 0.46. The curing agent is aliphatic polyamine, and specifically selects the iso-fluorine Bayer diamine. The curing regulator is tertiary amine, and the reinforcing agent is formed by mixing short-cut polyester fibers and carbon nanotubes according to a mass ratio of 1.
The preparation method of the curing plugging agent comprises the following steps:
S 1 preparing the modified epoxy resin, which specifically comprises:
S 11 preparing epoxy resin E-51, epoxy resin E-44 and 10% of carboxyl nitrile rubber;
S 12 adding the carboxyl nitrile rubber into the epoxy resin E-51, and stirring at 140 ℃;
S 13 stirring for 2 hours and then cooling to room temperature;
S 14 then adding epoxy resin E-44, and mixing uniformly to obtain the modified epoxy resin.
S 2 Adding other components into the modified epoxy resin, and slowly stirring until the components are uniformly mixed to obtain the bubble-free epoxy resin slurry.
S 3 And filling the epoxy resin slurry into a silica gel mold, putting the silica gel mold into an oven, and carrying out curing reaction at 120 ℃.
The compressive strength of the plugging agent provided by the embodiments 1 to 6 of the invention is tested by the following method:
curing the epoxy resin rubber plug slurry at high temperature to form a cubic module with the length of 50mm, and testing the compressive strength of the cured epoxy resin by using a compressive strength tester. The compressive strength calculation formula is as follows:
P=F/(0.05×0.05×1000)（MPa）
wherein F represents the pressure acting on the cube module, which is a direct reading on the compression tester in kN. The results of the experimental tests are given in the following table:
as can be seen from the table above, the compressive strength of the plugging agent provided by the embodiment of the invention is greater than 30MPa, and the plugging agent can effectively plug a leaking layer and prevent leakage loss.
The compressive strength of the plugging agent provided by the embodiments 1-6 of the invention after high temperature aging is tested according to the following method: after being prepared, the epoxy resin plugging agent is slowly poured into a self-made silica gel mold with the thickness of 50mm multiplied by 50mm, and is taken out after being completely cured, cooled and demoulded. Dividing the samples into 4 groups, and performing aging experiments in a high-temperature aging tank at 160 deg.C with air and clear aging mediumWater and polysulfonate drilling fluid (density of 2.0 g/cm) 3 ) And oil-based drilling fluids (density of 2.0 g/cm) 3 ). And taking out the sample after aging for 72 hours, cleaning the sample, and testing the compressive strength of the sample. Here, the non-ultimate compression test is performed, and if the calculated compression strength is more than 30MPa, the test is stopped. The test results are shown in the following table:
as can be seen from the test data in the table above, the plugging agent is aged in different aging media for 72 hours at 160 ℃, the pressure intensity is greater than 30MPa, the compressive strength of the plugging agent is hardly attenuated, and the plugging agent shows excellent temperature resistance.
In summary, after reading the present disclosure, those skilled in the art can make various other corresponding changes without creative efforts according to the technical solutions and technical concepts of the present disclosure, which all belong to the protection scope of the present disclosure.
Claims (9)
1. A macromolecule oil-based crosslinking curing plugging agent for drilling fluid is characterized in that: the composite material comprises the following components in percentage by mass: 60-80% of modified epoxy resin, 15-30% of curing agent, 1-5% of curing regulator and 4-10% of reinforcing agent.
2. The polymer oil-based crosslinking curing plugging agent for the drilling fluid as claimed in claim 1, wherein: the modified epoxy resin is obtained by mixing modified first epoxy resin with second epoxy resin, wherein the viscosity of the first epoxy resin is greater than that of the second epoxy resin.
3. The polymer oil-based crosslinking curing plugging agent for the drilling fluid as claimed in claim 2, wherein: the first epoxy resin is epoxy resin E-51, and the second epoxy resin is epoxy resin E-44.
4. The polymer oil-based crosslinking curing plugging agent for the drilling fluid as claimed in claim 3, wherein: the epoxy value of the epoxy resin E-51 is 0.48 to 0.54, and the viscosity is 10-169a.s; the epoxy value of the epoxy resin E-44 is 0.41 to 0.47.
5. The polymer oil-based crosslinking curing plugging agent for the drilling fluid as claimed in claim 1, wherein: the curing agent is one or a mixture of aliphatic polyamine and aromatic polyamine.
6. The polymer oil-based crosslinking curing plugging agent for the drilling fluid as claimed in claim 1, wherein: the curing regulator is one or a mixture of tertiary amine and imidazole.
7. The polymer oil-based crosslinking curing plugging agent for the drilling fluid as claimed in claim 1, wherein: the reinforcing agent is one or a mixture of more of graphene, nano calcium carbonate, carbon nano tubes, white carbon black and chopped polyester fibers.
8. A preparation method of a high polymer oil-based cross-linking curing plugging agent for drilling fluid is characterized by comprising the following steps: the method comprises the following steps:
S 1 preparing modified epoxy resin;
S 2 adding other components into the modified epoxy resin, and slowly stirring until the components are uniformly mixed to obtain bubble-free epoxy resin slurry;
S 3 and filling the epoxy resin slurry into a silica gel mold, putting the silica gel mold into an oven, and carrying out curing reaction at 120 ℃.
9. The preparation method of the polymer oil-based crosslinking curing plugging agent for the drilling fluid, which is characterized by comprising the following steps of: said step S 1 The preparation of the modified epoxy resin specifically comprises the following steps:
S 11 preparing epoxy resin E-51, epoxy resin E-44 and 10% of carboxyl nitrile rubber;
S 12 adding the carboxyl nitrile rubber into the epoxy resin E-51, and stirring at 140 ℃;
S 13 stirring for 2 hours and then cooling to room temperature;
S 14 then adding epoxy resin E-44, and mixing uniformly to obtain the modified epoxy resin.
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| KR101144227B1 (en) * | 2012-02-10 | 2012-05-10 | (주) 바이오 특수 | Epoxy-resin composition for waterproof lining |
| CN111995994A (en) * | 2020-07-30 | 2020-11-27 | 东营东方化学工业有限公司 | High-pressure-bearing plugging agent for oil production casing pipe and processing technology thereof |
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2021
- 2021-09-07 CN CN202111042564.8A patent/CN115772392B/en active Active
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| KR101144227B1 (en) * | 2012-02-10 | 2012-05-10 | (주) 바이오 특수 | Epoxy-resin composition for waterproof lining |
| CN111995994A (en) * | 2020-07-30 | 2020-11-27 | 东营东方化学工业有限公司 | High-pressure-bearing plugging agent for oil production casing pipe and processing technology thereof |
Non-Patent Citations (1)
| Title |
|---|
| 常侠;聂小安;王义刚;陈洁;李科;: "无规则羧基丁腈橡胶改性环氧树脂的制备及性能研究", 生物质化学工程, no. 06, pages 1 - 5 * |
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| CN115772392B (en) | 2024-03-08 |
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