CN116640320B - Anti-collapse plugging agent and preparation method thereof - Google Patents
Anti-collapse plugging agent and preparation method thereof Download PDFInfo
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- CN116640320B CN116640320B CN202310623946.2A CN202310623946A CN116640320B CN 116640320 B CN116640320 B CN 116640320B CN 202310623946 A CN202310623946 A CN 202310623946A CN 116640320 B CN116640320 B CN 116640320B
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- monomer
- nano particles
- plugging agent
- quaternary ammonium
- silane coupling
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- 238000002360 preparation method Methods 0.000 title claims abstract description 16
- 239000002105 nanoparticle Substances 0.000 claims abstract description 53
- 239000000178 monomer Substances 0.000 claims abstract description 52
- 238000006243 chemical reaction Methods 0.000 claims abstract description 36
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 34
- 238000000034 method Methods 0.000 claims abstract description 24
- 239000006087 Silane Coupling Agent Substances 0.000 claims abstract description 19
- 239000002904 solvent Substances 0.000 claims abstract description 17
- 150000003242 quaternary ammonium salts Chemical class 0.000 claims abstract description 12
- 125000002924 primary amino group Chemical group [H]N([H])* 0.000 claims abstract description 10
- 239000003054 catalyst Substances 0.000 claims abstract description 4
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical group CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 48
- ISKQADXMHQSTHK-UHFFFAOYSA-N [4-(aminomethyl)phenyl]methanamine Chemical compound NCC1=CC=C(CN)C=C1 ISKQADXMHQSTHK-UHFFFAOYSA-N 0.000 claims description 13
- AFOSIXZFDONLBT-UHFFFAOYSA-N divinyl sulfone Chemical compound C=CS(=O)(=O)C=C AFOSIXZFDONLBT-UHFFFAOYSA-N 0.000 claims description 10
- -1 sulfone compound Chemical class 0.000 claims description 6
- OXIKYYJDTWKERT-UHFFFAOYSA-N [4-(aminomethyl)cyclohexyl]methanamine Chemical compound NCC1CCC(CN)CC1 OXIKYYJDTWKERT-UHFFFAOYSA-N 0.000 claims description 5
- 125000003277 amino group Chemical group 0.000 claims description 4
- NZEDMAWEJPYWCD-UHFFFAOYSA-N 3-prop-2-enylsulfonylprop-1-ene Chemical compound C=CCS(=O)(=O)CC=C NZEDMAWEJPYWCD-UHFFFAOYSA-N 0.000 claims description 3
- PPJWCUOWPVSSSW-UHFFFAOYSA-N N,N,N-Trimethylethenaminium Chemical compound C[N+](C)(C)C=C PPJWCUOWPVSSSW-UHFFFAOYSA-N 0.000 claims description 2
- KEAOYAMQUMDVOO-UHFFFAOYSA-N ethenyl(triethyl)azanium Chemical compound CC[N+](CC)(CC)C=C KEAOYAMQUMDVOO-UHFFFAOYSA-N 0.000 claims description 2
- CDDLWPFLCVHZFU-UHFFFAOYSA-N trimethyl(pent-1-enyl)azanium Chemical compound CCCC=C[N+](C)(C)C CDDLWPFLCVHZFU-UHFFFAOYSA-N 0.000 claims description 2
- 239000012530 fluid Substances 0.000 abstract description 19
- 238000005553 drilling Methods 0.000 abstract description 9
- 239000003112 inhibitor Substances 0.000 abstract description 3
- 239000012752 auxiliary agent Substances 0.000 abstract description 2
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 23
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 16
- JCAPHLPCWXAZLG-UHFFFAOYSA-M ethenyl(trimethyl)azanium;chloride Chemical compound [Cl-].C[N+](C)(C)C=C JCAPHLPCWXAZLG-UHFFFAOYSA-M 0.000 description 13
- XLOMVQKBTHCTTD-UHFFFAOYSA-N Zinc monoxide Chemical compound [Zn]=O XLOMVQKBTHCTTD-UHFFFAOYSA-N 0.000 description 10
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 8
- 239000000376 reactant Substances 0.000 description 8
- 239000000377 silicon dioxide Substances 0.000 description 8
- ONCZQWJXONKSMM-UHFFFAOYSA-N dialuminum;disodium;oxygen(2-);silicon(4+);hydrate Chemical compound O.[O-2].[O-2].[O-2].[O-2].[O-2].[O-2].[O-2].[O-2].[O-2].[O-2].[O-2].[O-2].[Na+].[Na+].[Al+3].[Al+3].[Si+4].[Si+4].[Si+4].[Si+4] ONCZQWJXONKSMM-UHFFFAOYSA-N 0.000 description 7
- 239000007788 liquid Substances 0.000 description 7
- 239000005543 nano-size silicon particle Substances 0.000 description 7
- 229940080314 sodium bentonite Drugs 0.000 description 7
- 229910000280 sodium bentonite Inorganic materials 0.000 description 7
- 239000007795 chemical reaction product Substances 0.000 description 6
- 239000006185 dispersion Substances 0.000 description 6
- 238000012360 testing method Methods 0.000 description 6
- 238000009210 therapy by ultrasound Methods 0.000 description 6
- 239000003921 oil Substances 0.000 description 5
- 125000001453 quaternary ammonium group Chemical group 0.000 description 5
- 239000007790 solid phase Substances 0.000 description 5
- 238000003756 stirring Methods 0.000 description 5
- 239000011787 zinc oxide Substances 0.000 description 5
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 description 4
- 230000002579 anti-swelling effect Effects 0.000 description 4
- 239000004927 clay Substances 0.000 description 4
- 238000004821 distillation Methods 0.000 description 4
- 239000003814 drug Substances 0.000 description 4
- 239000012467 final product Substances 0.000 description 4
- 239000007789 gas Substances 0.000 description 4
- 229910052757 nitrogen Inorganic materials 0.000 description 4
- 150000003141 primary amines Chemical class 0.000 description 4
- 230000008569 process Effects 0.000 description 4
- 238000011084 recovery Methods 0.000 description 4
- 238000005096 rolling process Methods 0.000 description 4
- 235000012239 silicon dioxide Nutrition 0.000 description 4
- 239000003381 stabilizer Substances 0.000 description 4
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 description 3
- 229920002907 Guar gum Polymers 0.000 description 3
- 238000006845 Michael addition reaction Methods 0.000 description 3
- 235000011114 ammonium hydroxide Nutrition 0.000 description 3
- 230000000694 effects Effects 0.000 description 3
- 238000011156 evaluation Methods 0.000 description 3
- 238000002474 experimental method Methods 0.000 description 3
- 238000013100 final test Methods 0.000 description 3
- 239000000665 guar gum Substances 0.000 description 3
- 235000010417 guar gum Nutrition 0.000 description 3
- 229960002154 guar gum Drugs 0.000 description 3
- 230000005764 inhibitory process Effects 0.000 description 3
- 239000000203 mixture Substances 0.000 description 3
- 230000035699 permeability Effects 0.000 description 3
- 239000000047 product Substances 0.000 description 3
- 150000003335 secondary amines Chemical group 0.000 description 3
- 239000000243 solution Substances 0.000 description 3
- 238000005406 washing Methods 0.000 description 3
- HRPVXLWXLXDGHG-UHFFFAOYSA-N Acrylamide Chemical compound NC(=O)C=C HRPVXLWXLXDGHG-UHFFFAOYSA-N 0.000 description 2
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 2
- UQSXHKLRYXJYBZ-UHFFFAOYSA-N Iron oxide Chemical compound [Fe]=O UQSXHKLRYXJYBZ-UHFFFAOYSA-N 0.000 description 2
- WYURNTSHIVDZCO-UHFFFAOYSA-N Tetrahydrofuran Chemical compound C1CCOC1 WYURNTSHIVDZCO-UHFFFAOYSA-N 0.000 description 2
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 2
- 238000001035 drying Methods 0.000 description 2
- 229910021389 graphene Inorganic materials 0.000 description 2
- 230000036571 hydration Effects 0.000 description 2
- 238000006703 hydration reaction Methods 0.000 description 2
- 238000002347 injection Methods 0.000 description 2
- 239000007924 injection Substances 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 239000001301 oxygen Substances 0.000 description 2
- 229910052760 oxygen Inorganic materials 0.000 description 2
- 230000020477 pH reduction Effects 0.000 description 2
- 239000002002 slurry Substances 0.000 description 2
- 229910000029 sodium carbonate Inorganic materials 0.000 description 2
- 239000000230 xanthan gum Substances 0.000 description 2
- 235000010493 xanthan gum Nutrition 0.000 description 2
- 229920001285 xanthan gum Polymers 0.000 description 2
- 229940082509 xanthan gum Drugs 0.000 description 2
- HMUNWXXNJPVALC-UHFFFAOYSA-N 1-[4-[2-(2,3-dihydro-1H-inden-2-ylamino)pyrimidin-5-yl]piperazin-1-yl]-2-(2,4,6,7-tetrahydrotriazolo[4,5-c]pyridin-5-yl)ethanone Chemical compound C1C(CC2=CC=CC=C12)NC1=NC=C(C=N1)N1CCN(CC1)C(CN1CC2=C(CC1)NN=N2)=O HMUNWXXNJPVALC-UHFFFAOYSA-N 0.000 description 1
- VZSRBBMJRBPUNF-UHFFFAOYSA-N 2-(2,3-dihydro-1H-inden-2-ylamino)-N-[3-oxo-3-(2,4,6,7-tetrahydrotriazolo[4,5-c]pyridin-5-yl)propyl]pyrimidine-5-carboxamide Chemical compound C1C(CC2=CC=CC=C12)NC1=NC=C(C=N1)C(=O)NCCC(N1CC2=C(CC1)NN=N2)=O VZSRBBMJRBPUNF-UHFFFAOYSA-N 0.000 description 1
- WZFUQSJFWNHZHM-UHFFFAOYSA-N 2-[4-[2-(2,3-dihydro-1H-inden-2-ylamino)pyrimidin-5-yl]piperazin-1-yl]-1-(2,4,6,7-tetrahydrotriazolo[4,5-c]pyridin-5-yl)ethanone Chemical compound C1C(CC2=CC=CC=C12)NC1=NC=C(C=N1)N1CCN(CC1)CC(=O)N1CC2=C(CC1)NN=N2 WZFUQSJFWNHZHM-UHFFFAOYSA-N 0.000 description 1
- 108010054404 Adenylyl-sulfate kinase Proteins 0.000 description 1
- PNEYBMLMFCGWSK-UHFFFAOYSA-N Alumina Chemical compound [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 1
- 244000007835 Cyamopsis tetragonoloba Species 0.000 description 1
- 102100039024 Sphingosine kinase 1 Human genes 0.000 description 1
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 1
- 229940117913 acrylamide Drugs 0.000 description 1
- 230000009471 action Effects 0.000 description 1
- 239000000654 additive Substances 0.000 description 1
- 230000000996 additive effect Effects 0.000 description 1
- 230000000844 anti-bacterial effect Effects 0.000 description 1
- 239000003899 bactericide agent Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000005540 biological transmission Effects 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 230000000052 comparative effect Effects 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- 239000003431 cross linking reagent Substances 0.000 description 1
- 238000005520 cutting process Methods 0.000 description 1
- 125000000113 cyclohexyl group Chemical group [H]C1([H])C([H])([H])C([H])([H])C([H])(*)C([H])([H])C1([H])[H] 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 229940079593 drug Drugs 0.000 description 1
- 229920013818 hydroxypropyl guar gum Polymers 0.000 description 1
- 230000002401 inhibitory effect Effects 0.000 description 1
- 239000003350 kerosene Substances 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 230000007246 mechanism Effects 0.000 description 1
- WSFSSNUMVMOOMR-NJFSPNSNSA-N methanone Chemical compound O=[14CH2] WSFSSNUMVMOOMR-NJFSPNSNSA-N 0.000 description 1
- 238000002715 modification method Methods 0.000 description 1
- 125000001997 phenyl group Chemical group [H]C1=C([H])C([H])=C(*)C([H])=C1[H] 0.000 description 1
- 150000003839 salts Chemical class 0.000 description 1
- 150000003384 small molecules Chemical class 0.000 description 1
- YLQBMQCUIZJEEH-UHFFFAOYSA-N tetrahydrofuran Natural products C=1C=COC=1 YLQBMQCUIZJEEH-UHFFFAOYSA-N 0.000 description 1
- 239000002562 thickening agent Substances 0.000 description 1
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 description 1
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- C08G83/00—Macromolecular compounds not provided for in groups C08G2/00 - C08G81/00
- C08G83/001—Macromolecular compounds containing organic and inorganic sequences, e.g. organic polymers grafted onto silica
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Abstract
The invention provides an anti-collapse plugging agent and a preparation method thereof, and relates to the technical field of auxiliary agents for oil fields. The inhibitor is prepared by the following method: modifying the nano particles by adopting an amino-containing silane coupling agent to obtain modified nano particles, wherein the mass ratio of the nano particles to the amino-containing silane coupling agent is 10:3-7; dissolving a first monomer and a second monomer in a solvent, continuously reacting for 0.5-2 h at 40-70 ℃ under the condition of deoxidizing, adding monoalkenyl quaternary ammonium salt to continuously react for 1-2 h after the reaction is finished, adding modified nano particles to continuously react for 1-3 h, and removing the solvent to obtain the catalyst. The collapse-preventing plugging agent has good compatibility with conventional drilling fluid, and the performance of the drilling fluid is not affected after the collapse-preventing plugging agent is added; meanwhile, the shale plugging agent has good temperature resistance, can resist the temperature of 220 ℃ and can effectively plug shale.
Description
Technical Field
The invention belongs to the technical field of auxiliary agents for oil fields, and particularly relates to an anti-collapse plugging agent and a preparation method thereof.
Background
In the drilling process, as the shale stratum absorbs water, the shale stratum gradually expands, the volume of the shale stratum expands, the drill cuttings below the drill bit are prevented from being removed, friction between the drill string and the side wall of the drill hole is increased, circulation loss or pipe blockage is caused, meanwhile, well wall instability is caused, and well wall instability caused by hydration expansion and dispersion of the shale is always a technical problem in oil and gas well engineering.
For shale, the current method for controlling instability of shale in the industry mainly comprises the following steps: the inhibitor is used for inhibiting hydration of the shale, and the plugging agent is used for plugging the shale, or both. Due to the medicament with both the inhibitor and the plugging agent, the current effect is relatively poor in consideration of the compatibility problem of the medicament and the drilling fluid, so that the development of the medicament is limited.
Disclosure of Invention
In order to solve at least one of the problems, the invention provides an anti-collapse plugging agent which has better compatibility with conventional fracturing fluid and also has better temperature resistance.
The technical scheme of the invention is as follows: a preparation method of an anti-collapse plugging agent comprises the following steps:
modifying the nano particles by adopting an amino-containing silane coupling agent to obtain modified nano particles, wherein the mass ratio of the nano particles to the amino-containing silane coupling agent is 10:3-7;
dissolving a first monomer and a second monomer in a solvent, continuously reacting for 0.5-2 h at 40-70 ℃ under the condition of deoxidizing, adding monoalkenyl quaternary ammonium salt to continuously react for 1-2 h after the reaction is finished, adding modified nano particles to continuously react for 1-3 h, and removing the solvent to obtain the catalyst;
Wherein the mol ratio of the first monomer to the mono-alkenyl quaternary ammonium salt is 1:5-8.5, and the addition amount of the second monomer is 0.5-5% of the total mass of the first monomer and the mono-alkenyl quaternary ammonium salt; the first monomer is at least one of p-xylylenediamine or 1, 4-cyclohexanedimethylamine, the second monomer is a sulfone compound containing two olefinic bonds, and the addition of the modified nano particles is 20-50% of the mass of the monoalkenyl quaternary ammonium salt.
One embodiment of the present invention is that the solvent is ethanol.
One embodiment of the invention is that the mono alkenyl quaternary ammonium salt monomer is one of trimethyl vinyl ammonium, triethyl vinyl ammonium and trimethyl-1-pentenyl ammonium.
One embodiment of the present invention is that the amino group-containing silane coupling agent is one of KH550, KH540, KH792, KH 602.
Further, the amino-containing silane coupling agent is one of KH792 and KH 602.
One embodiment of the present invention is that the second monomer is one of divinyl sulfone and diallyl sulfone.
One embodiment of the present invention is that the nanoparticle is one of nanosilicon dioxide and graphene oxide.
The invention also aims to provide an anti-collapse plugging agent which is prepared by adopting any one of the methods. Compared with the conventional fracturing fluid, the anti-collapse plugging agent is characterized by comprising a main component.
The invention has the beneficial effects that:
The collapse-preventing plugging agent has good compatibility with conventional drilling fluid, and the performance of the drilling fluid is not affected after the collapse-preventing plugging agent is added; meanwhile, the shale plugging agent has good temperature resistance, can resist the temperature of 220 ℃ and can effectively plug shale.
Detailed Description
In order to make the technical scheme and technical advantages of the present invention more clear, the technical scheme in the implementation process of the present invention will be clearly and completely described below with reference to the embodiments.
A preparation method of an anti-collapse plugging agent comprises the following steps:
modifying the nano particles by adopting an amino-containing silane coupling agent to obtain modified nano particles, wherein the mass ratio of the nano particles to the amino-containing silane coupling agent is 10:3-7;
dissolving a first monomer and a second monomer in a solvent, continuously reacting for 0.5-2 h at 40-70 ℃ under the condition of deoxidizing, adding monoalkenyl quaternary ammonium salt to continuously react for 1-2 h after the reaction is finished, adding modified nano particles to continuously react for 1-3 h, and removing the solvent to obtain the catalyst;
Wherein the mol ratio of the first monomer to the mono-alkenyl quaternary ammonium salt is 1:5-8.5, and the addition amount of the second monomer is 0.5-5% of the total mass of the first monomer and the mono-alkenyl quaternary ammonium salt; the first monomer is at least one of p-xylylenediamine or 1, 4-cyclohexanedimethylamine, the second monomer is a sulfone compound containing two olefinic bonds, and the addition of the modified nano particles is 20-50% of the mass of the monoalkenyl quaternary ammonium salt.
Specifically, in the preparation process, the first monomer and the second monomer are reacted first to form a pre-reactant with relatively long chain length under the action of the second monomer, and meanwhile, the second monomer can only react with a small amount of the first monomer due to the small addition amount of the second monomer, so that a large amount of free first monomer is in the final product.
After the first monomer and the second monomer react, monoalkenyl quaternary ammonium salt is added, wherein the monoalkenyl quaternary ammonium salt can react with primary amine and secondary amine groups remained after the previous reaction in polarity, and meanwhile, due to the fact that the monoalkenyl quaternary ammonium salt is added in a large amount, the remaining primary amine and secondary amine in the first monomer can be reacted basically, so that a sufficient amount of quaternary ammonium groups can be grafted on a final product, whether a pre-reactant with a relatively long chain length or the first monomer, water solubility of the final product is improved, and inhibition performance of the final product is improved.
After the monoalkenyl quaternary ammonium salt is added, the modified nano particles are added, so that the water dispersibility of the nano particles can be enhanced by grafting the quaternary ammonium group on the modified nano particles, and meanwhile, the quaternary ammonium group can be adsorbed on the well wall, so that the stability of the plugging layer can be improved, and the inhibition performance of the plugging layer can be further improved.
Those skilled in the art will appreciate that for the multiple reactions described above: the reaction of the first monomer and the second monomer, the subsequent reaction of the mono alkenyl quaternary ammonium salt and the subsequent reaction of the modified nano particles are all Michael addition reactions.
Meanwhile, one of the p-xylylenediamine or 1, 4-cyclohexanedimethylamine is selected as the first monomer, the first monomer has two primary amine groups, can perform multiple Michael addition reactions, and the second monomer contains benzene rings or cyclohexane groups, has certain rigidity, and can increase the hydrophobicity and temperature and salt resistance of the product.
Taking the first monomer as p-xylylenediamine, mono-alkenyl quaternary ammonium salt monomer as trimethyl vinyl ammonium chloride, second monomer as divinyl sulfone, nano-particle as nano-silica and silane coupling agent as KH602 as an example, in a complete reaction state, the following reactions mainly occur from front to back: KH602 and nano-silica, a pre-reactant of the para-xylylenediamine and the divinyl sulfone, a reaction of the pre-reactant and the trimethyl vinyl ammonium chloride, a reaction of the para-xylylenediamine and the trimethyl vinyl ammonium chloride, and a reaction of the modified nano-silica and the trimethyl vinyl ammonium chloride.
Among them, the reaction product of p-xylylenediamine and trimethyl vinyl ammonium chloride is a small molecule product, usually 1mol of p-xylylenediamine and 1 to 4 mol of trimethyl vinyl ammonium chloride are reacted, and it has a certain water solubility.
The pre-reactants of p-xylylenediamine and divinyl sulfone are insoluble in water, but in the subsequent process they react with the trimethyl vinyl ammonium chloride, which is usually water-soluble due to the high amount of grafted quaternary ammonium groups on the pre-reactants.
The reaction product of the modified nano silicon dioxide and trimethyl vinyl ammonium chloride has certain hydrophilicity: the modified nano silica grafted with KH602 has corresponding hydrophilic performance due to KH602 containing a primary amine and a secondary amine, and after the KH602 reacts with trimethyl vinyl ammonium chloride, quaternary ammonium groups are grafted to further enhance the hydrophilicity of the modified nano silica, so that the modified nano silica has better water dispersion performance.
From the above, it is clear that the molecular weight of the product is small, and the reactants have a corresponding branching degree because the addition amount of each reactant is controlled in the examples of the present invention and the mechanism of the Michael addition reaction and the structure of the first monomer are combined.
For the solvent in the above operation, it is the same as the conventional requirement for the solvent: the first monomer, the second monomer, and the monoalkenyl quaternary ammonium salt are all capable of being dissolved in a solvent. Solvents satisfying these conditions are many, such as tetrahydrofuran, ethanol, etc., and ethanol is preferable in terms of difficulty in removal in the subsequent process, difficulty in obtaining, and cost.
The second monomer functions similarly to the crosslinking agent, and in view of the property that the longer the molecular chain is, the worse the water solubility is, the second monomer is generally required to have a certain water solubility, and therefore, the second monomer is preferably one of divinyl sulfone and diallyl sulfone.
For the modification of nano particles, which belongs to a relatively mature method in the prior art, a plurality of documents and patents propose a method for grafting a silane coupling agent on the surface of the nano particles, which can be applied to the invention, and meanwhile, commercially available silane coupling agent modified nano particles can be purchased. However, for the convenience of understanding of those skilled in the art, a modification method is proposed in the present invention: dispersing nano particles into water, adding ammonia water to adjust the pH value to 9-11, dissolving an amino-containing silane coupling agent into ethanol, reacting for 3-12 h under the condition of continuous stirring and 50-70 ℃, removing the solvent, and washing the solid phase with ethanol for several times to obtain the nano-particle.
It is known to those skilled in the art that although the above gives a method of grafting a silane coupling agent, modified nanoparticles prepared by the remaining grafting methods in the art can still be applied to the present invention.
Meanwhile, as for the nanoparticles, there are various types of nanoparticles capable of achieving the above-mentioned requirements, such as nano silica, graphene oxide, nano iron oxide, nano titanium oxide, nano aluminum oxide, nano zinc oxide, etc., but nano silica, nano zinc oxide are preferable from the practical viewpoint.
As the amino group-containing silane coupling agent, there are various ones in the prior art such as KH550, KH540, KH792, KH602, etc., but polyamino group-containing silane coupling agents such as KH602, KH792, etc. are preferable.
The anti-collapse plugging agent prepared by the method has good anti-collapse plugging performance, good temperature resistance, good compatibility with conventional fracturing fluid and good shale inhibition effect.
In order to further illustrate the method of the present invention, specific examples are described below.
The experimental methods used in the following examples are conventional methods unless otherwise specified.
Materials, reagents and the like used in the examples described below are commercially available unless otherwise specified.
Example 1
Preparation of modified nanoparticles: adding 50g of nano silicon dioxide into 60ml of water, adding ammonia water to adjust the pH to 10, carrying out ultrasonic treatment for 30min to uniformly disperse the nano silicon dioxide, adding 25g of KH792 into 100ml of ethanol, uniformly stirring the mixture, adding an ethanol solution of KH792 into the nano silicon dioxide dispersion liquid, reacting for 6h under the condition of continuous stirring at 65 ℃, removing the solvent after the reaction is finished, washing the solid phase with ethanol for a plurality of times, and drying the solid phase at 90 ℃ to obtain the nano silicon dioxide.
Preparation of anti-collapse plugging agent: adding 28g of modified nano particles into 60ml of ethanol, and carrying out ultrasonic treatment for 30min to uniformly disperse the modified nano particles; 13.6g of p-xylylenediamine and 1.5g of divinyl sulfone are taken and added into 300ml of ethanol, nitrogen is introduced to remove oxygen for 10min, the temperature is raised to 60 ℃ for reaction for 1h, 72g of trimethyl vinyl ammonium chloride is added after the reaction is finished, the reaction is continued for 1.5h, after the reaction is finished, the modified nanoparticle dispersion liquid is added into the reaction product and is continued to react for 2h, and after the reaction is finished, the ethanol is removed by reduced pressure distillation, thus obtaining the nano-particle.
Example 2
Preparation of modified nanoparticles: the same as in example 1.
Preparation of anti-collapse plugging agent: adding 28g of modified nano particles into 60ml of ethanol, and carrying out ultrasonic treatment for 30min to uniformly disperse the modified nano particles; 13.6g of p-xylylenediamine and 3.5g of divinyl sulfone are taken and added into 400ml of ethanol, nitrogen is introduced to deoxidize for 10min, the temperature is raised to 60 ℃ for reaction for 1.5h, 66g of trimethyl vinyl ammonium chloride is added after the reaction is finished, the reaction is continued for 1.5h, after the reaction is finished, the modified nanoparticle dispersion liquid is added into the reaction product and is continued to react for 2h, and after the reaction is finished, the ethanol is removed by reduced pressure distillation.
Example 3
Preparation of modified nanoparticles: adding 50g of nano zinc oxide into 100ml of water, adding ammonia water to adjust the pH to 10, carrying out ultrasonic treatment for 30min to uniformly disperse the nano zinc oxide, adding 200ml of ethanol into 35g of KH792, uniformly stirring the mixture, adding an ethanol solution of KH792 into nano silicon dioxide dispersion liquid, reacting for 6h under the condition of continuous stirring at 65 ℃, removing a solvent after the reaction is finished, washing a solid phase with ethanol for a plurality of times, and drying the solid phase at 90 ℃ to obtain the nano zinc oxide.
Preparation of anti-collapse plugging agent: adding 28g of modified nano particles into 100ml of ethanol, and carrying out ultrasonic treatment for 30min to uniformly disperse the modified nano particles; 13.6g of 1, 4-cyclohexanedimethylamine and 0.8g of divinyl sulfone are taken and added into 300ml of ethanol, nitrogen is introduced to deoxidize for 10min, the temperature is raised to 50 ℃ for reaction for 1h, 72g of trimethyl vinyl ammonium chloride is added after the reaction is finished, the reaction is continued for 1.5h, after the reaction is finished, the modified nanoparticle dispersion liquid is added into the reaction product and is continued to react for 2h, and after the reaction is finished, the ethanol is removed by reduced pressure distillation, thus obtaining the nano-particle.
Example 4
Preparation of modified nanoparticles: the same as in example 1.
Preparation of anti-collapse plugging agent: adding 35g of modified nano particles into 60ml of ethanol, and carrying out ultrasonic treatment for 30min to uniformly disperse the modified nano particles; 13.6g of p-xylylenediamine and 1.5g of divinyl sulfone are taken and added into 300ml of ethanol, nitrogen is introduced to remove oxygen for 10min, the temperature is raised to 60 ℃ for reaction for 1h, 72g of trimethyl vinyl ammonium chloride is added after the reaction is finished, the reaction is continued for 1.5h, after the reaction is finished, the modified nanoparticle dispersion liquid is added into the reaction product and is continued to react for 2h, and after the reaction is finished, the ethanol is removed by reduced pressure distillation, thus obtaining the nano-particle.
1. Compatibility of medicines
The compatibility of the clay stabilizer in the guar gum fracturing fluid is tested by referring to the method in SY/T5971-2016 oil and gas field fracturing acidification and clay stabilizer performance evaluation method for water injection, and the final test result is shown in Table 1. Wherein, the composition of the base liquid of the guar gum fracturing fluid is 0.4 percent of hydroxypropyl guar gum, 0.1 percent of formaldehyde, 0.2 percent of cleanup additive ME-2, 0.05 percent of sodium carbonate and 0.1 percent of bactericide SK-1. The viscosity was measured using a rotational viscometer with a shear rate of 170s -1. The final test results are shown in table 1.
Table 1 compatibility test
| Sample of | Concentration wt% | Viscosity mPs s |
| Example 1 | 1 | 71.3 |
| Example 2 | 1 | 70.8 |
| Example 3 | 1 | 72.5 |
| Example 4 | 1 | 69.7 |
| Blank space | —— | 68.4 |
As can be seen from Table 1, the anti-collapse plugging agent provided by the embodiment of the invention has good compatibility with the existing common guar fracturing fluid. In essence, the inventor does not give all experimental results due to space limitation, but experiments of the inventor find that the anti-collapse plugging agent, the acrylamide fracturing fluid and the xanthan gum fracturing fluid in the embodiment of the invention have good compatibility. Meanwhile, although the description of the "fracturing fluid" is adopted, in practice, guar gum, acrylamide or xanthan gum is a common thickener in fracturing fluid and drilling fluid, so that the fracturing fluid has corresponding compatibility compared with the conventional drilling fluid.
2. Expansion resistance rate
The anti-swelling rate of the clay stabilizer for oil and gas field fracturing acidification and water injection is tested by referring to the method in SY/T5971-2016 clay stabilizer performance evaluation method, and the specific method is as follows: adding 0.50g of sodium bentonite into a test tube, simultaneously adding 10ml of anti-collapse plugging agent solution, shaking uniformly, standing for 2 hours, centrifuging for 15 minutes at 1500r/min, and reading the volume V 1 of the sodium bentonite; adding 0.50g of sodium bentonite into a test tube, adding 10ml of water at the same time, shaking uniformly, standing for 2 hours, centrifuging for 15 minutes at 1500r/min, and reading the volume V 2 of the sodium bentonite; adding 0.50g of sodium bentonite into a test tube, adding 10ml of kerosene, shaking uniformly, standing for 2 hours, centrifuging at 1500r/min for 15min, and reading the volume V 0 of the sodium bentonite.
The calculation formula of the anti-swelling rate is as follows:
the final results of the anti-swelling test are shown in Table 2.
TABLE 2 results of anti-swelling test
As can be seen from Table 2, the anti-collapse plugging agent of the embodiment of the invention has an anti-expansion rate of more than 83% when the addition amount is 1%, which indicates that the anti-collapse plugging agent has better anti-expansion performance; when the addition amount thereof is gradually increased, the expansion preventing rate is continuously increased, but the increase width is small, and therefore, the addition amount is preferably 1% in view of cost and effect.
3. Rolling recovery rate
The anti-collapse plugging agents of the above examples and comparative examples were prepared into anti-collapse plugging agents with different concentrations by using clear water, the rolling recovery rates were measured by the method disclosed in the oil and gas industry standard SY/T6335-1997 evaluation method of anti-collapse plugging agent for drilling fluid, and the final test results are shown in Table 3
TABLE 3 Rolling recovery rate
As can be seen from Table 3, the anti-collapse plugging agent of the example of the present invention has a high rolling recovery rate and can withstand a temperature of 220 ℃.
4. Shale permeability
Shale core is taken, 2% of anti-collapse plugging agent is added into base slurry, the permeability of the shale core is measured by adopting a pressure transmission experiment under the condition of high temperature and high pressure, and the final result is shown in table 4. Wherein, the base slurry comprises the following components: 1000ml water +80g sodium bentonite +5g sodium carbonate.
Table 4 permeability change
From table 4, it can be seen that the anti-collapse plugging agent of the embodiment of the invention can effectively plug shale, and the plugging rate is relatively high.
The present invention is not limited to the preferred embodiments, and the present invention is described above in any way, but is not limited to the preferred embodiments, and any person skilled in the art will appreciate that the present invention is not limited to the embodiments described above, while the above disclosure is directed to various equivalent embodiments, which are capable of being modified or varied in several ways, any simple modification, equivalent variation and variation of the above embodiments according to the technical principles of the present invention will still fall within the scope of the present invention.
Claims (8)
1. The preparation method of the anti-collapse plugging agent is characterized by comprising the following steps of:
modifying the nano particles by adopting an amino-containing silane coupling agent to obtain modified nano particles, wherein the mass ratio of the nano particles to the amino-containing silane coupling agent is 10:3-7;
dissolving a first monomer and a second monomer in a solvent, continuously reacting for 0.5-2 h at 40-70 ℃ under the condition of deoxidizing, adding monoalkenyl quaternary ammonium salt to continuously react for 1-2 h after the reaction is finished, adding modified nano particles to continuously react for 1-3 h, and removing the solvent to obtain the catalyst;
Wherein the mol ratio of the first monomer to the mono-alkenyl quaternary ammonium salt is 1:5-8.5, and the addition amount of the second monomer is 0.5-5% of the total mass of the first monomer and the mono-alkenyl quaternary ammonium salt; the first monomer is at least one of p-xylylenediamine or 1, 4-cyclohexanedimethylamine, the second monomer is a sulfone compound containing two olefinic bonds, and the addition of the modified nano particles is 20-50% of the mass of the monoalkenyl quaternary ammonium salt.
2. The method of claim 1, wherein the solvent is ethanol.
3. The method of claim 1, wherein the mono-alkenyl quaternary ammonium salt monomer is one of trimethyl vinyl ammonium, triethyl vinyl ammonium, trimethyl-1-pentenyl ammonium.
4. The method according to claim 1, wherein the amino group-containing silane coupling agent is one of KH550, KH540, KH792, KH 602.
5. The method of claim 4, wherein the amino group-containing silane coupling agent is one of KH792, KH 602.
6. The method of claim 1, wherein the second monomer is one of divinyl sulfone and diallyl sulfone.
7. The method of claim 1, wherein the nanoparticle is one of nanosilica, nanosilica.
8. An anti-collapse plugging agent prepared by the method of any one of claims 1 to 7.
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