CN117777356A - Temporary plugging agent for fracturing and acidizing and preparation method thereof - Google Patents
Temporary plugging agent for fracturing and acidizing and preparation method thereof Download PDFInfo
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- CN117777356A CN117777356A CN202311647857.8A CN202311647857A CN117777356A CN 117777356 A CN117777356 A CN 117777356A CN 202311647857 A CN202311647857 A CN 202311647857A CN 117777356 A CN117777356 A CN 117777356A
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- temporary plugging
- plugging agent
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- itaconic acid
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- 238000002360 preparation method Methods 0.000 title claims abstract description 14
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 117
- 238000006243 chemical reaction Methods 0.000 claims abstract description 54
- 239000003999 initiator Substances 0.000 claims abstract description 25
- JAHNSTQSQJOJLO-UHFFFAOYSA-N 2-(3-fluorophenyl)-1h-imidazole Chemical compound FC1=CC=CC(C=2NC=CN=2)=C1 JAHNSTQSQJOJLO-UHFFFAOYSA-N 0.000 claims abstract description 23
- 239000003638 chemical reducing agent Substances 0.000 claims abstract description 23
- LVHBHZANLOWSRM-UHFFFAOYSA-N methylenebutanedioic acid Natural products OC(=O)CC(=C)C(O)=O LVHBHZANLOWSRM-UHFFFAOYSA-N 0.000 claims abstract description 23
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 21
- 230000001105 regulatory effect Effects 0.000 claims abstract description 20
- 238000000034 method Methods 0.000 claims abstract description 18
- KGIGUEBEKRSTEW-UHFFFAOYSA-N 2-vinylpyridine Chemical compound C=CC1=CC=CC=N1 KGIGUEBEKRSTEW-UHFFFAOYSA-N 0.000 claims abstract description 15
- MAGFQRLKWCCTQJ-UHFFFAOYSA-N 4-ethenylbenzenesulfonic acid Chemical compound OS(=O)(=O)C1=CC=C(C=C)C=C1 MAGFQRLKWCCTQJ-UHFFFAOYSA-N 0.000 claims abstract description 15
- CQHKDHVZYZUZMJ-UHFFFAOYSA-N [2,2-bis(hydroxymethyl)-3-prop-2-enoyloxypropyl] prop-2-enoate Chemical compound C=CC(=O)OCC(CO)(CO)COC(=O)C=C CQHKDHVZYZUZMJ-UHFFFAOYSA-N 0.000 claims abstract description 15
- 239000008367 deionised water Substances 0.000 claims abstract description 13
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 13
- 239000002994 raw material Substances 0.000 claims abstract description 13
- 238000001035 drying Methods 0.000 claims abstract description 11
- 238000003756 stirring Methods 0.000 claims abstract description 11
- 239000000337 buffer salt Substances 0.000 claims abstract description 9
- 238000010438 heat treatment Methods 0.000 claims abstract description 6
- 239000000243 solution Substances 0.000 claims description 56
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 40
- 229910052757 nitrogen Inorganic materials 0.000 claims description 20
- 239000007864 aqueous solution Substances 0.000 claims description 14
- ROOXNKNUYICQNP-UHFFFAOYSA-N ammonium persulfate Chemical compound [NH4+].[NH4+].[O-]S(=O)(=O)OOS([O-])(=O)=O ROOXNKNUYICQNP-UHFFFAOYSA-N 0.000 claims description 12
- 239000002245 particle Substances 0.000 claims description 12
- GEHJYWRUCIMESM-UHFFFAOYSA-L sodium sulfite Chemical compound [Na+].[Na+].[O-]S([O-])=O GEHJYWRUCIMESM-UHFFFAOYSA-L 0.000 claims description 8
- 229910001870 ammonium persulfate Inorganic materials 0.000 claims description 6
- 229910000403 monosodium phosphate Inorganic materials 0.000 claims description 6
- 235000019799 monosodium phosphate Nutrition 0.000 claims description 6
- AJPJDKMHJJGVTQ-UHFFFAOYSA-M sodium dihydrogen phosphate Chemical compound [Na+].OP(O)([O-])=O AJPJDKMHJJGVTQ-UHFFFAOYSA-M 0.000 claims description 6
- LFVGISIMTYGQHF-UHFFFAOYSA-N ammonium dihydrogen phosphate Chemical compound [NH4+].OP(O)([O-])=O LFVGISIMTYGQHF-UHFFFAOYSA-N 0.000 claims description 5
- 229910000387 ammonium dihydrogen phosphate Inorganic materials 0.000 claims description 5
- 235000019837 monoammonium phosphate Nutrition 0.000 claims description 5
- 229910000402 monopotassium phosphate Inorganic materials 0.000 claims description 5
- 235000019796 monopotassium phosphate Nutrition 0.000 claims description 5
- USHAGKDGDHPEEY-UHFFFAOYSA-L potassium persulfate Chemical compound [K+].[K+].[O-]S(=O)(=O)OOS([O-])(=O)=O USHAGKDGDHPEEY-UHFFFAOYSA-L 0.000 claims description 5
- LCPVQAHEFVXVKT-UHFFFAOYSA-N 2-(2,4-difluorophenoxy)pyridin-3-amine Chemical compound NC1=CC=CN=C1OC1=CC=C(F)C=C1F LCPVQAHEFVXVKT-UHFFFAOYSA-N 0.000 claims description 4
- ZPWVASYFFYYZEW-UHFFFAOYSA-L dipotassium hydrogen phosphate Chemical compound [K+].[K+].OP([O-])([O-])=O ZPWVASYFFYYZEW-UHFFFAOYSA-L 0.000 claims description 4
- PJNZPQUBCPKICU-UHFFFAOYSA-N phosphoric acid;potassium Chemical compound [K].OP(O)(O)=O PJNZPQUBCPKICU-UHFFFAOYSA-N 0.000 claims description 4
- BHZRJJOHZFYXTO-UHFFFAOYSA-L potassium sulfite Chemical compound [K+].[K+].[O-]S([O-])=O BHZRJJOHZFYXTO-UHFFFAOYSA-L 0.000 claims description 4
- 235000019252 potassium sulphite Nutrition 0.000 claims description 4
- 238000010926 purge Methods 0.000 claims description 4
- CHQMHPLRPQMAMX-UHFFFAOYSA-L sodium persulfate Substances [Na+].[Na+].[O-]S(=O)(=O)OOS([O-])(=O)=O CHQMHPLRPQMAMX-UHFFFAOYSA-L 0.000 claims description 4
- 235000010265 sodium sulphite Nutrition 0.000 claims description 4
- DWAQJAXMDSEUJJ-UHFFFAOYSA-M Sodium bisulfite Chemical compound [Na+].OS([O-])=O DWAQJAXMDSEUJJ-UHFFFAOYSA-M 0.000 claims description 3
- MNNHAPBLZZVQHP-UHFFFAOYSA-N diammonium hydrogen phosphate Chemical compound [NH4+].[NH4+].OP([O-])([O-])=O MNNHAPBLZZVQHP-UHFFFAOYSA-N 0.000 claims description 3
- 229910000388 diammonium phosphate Inorganic materials 0.000 claims description 3
- 235000019838 diammonium phosphate Nutrition 0.000 claims description 3
- BNIILDVGGAEEIG-UHFFFAOYSA-L disodium hydrogen phosphate Chemical compound [Na+].[Na+].OP([O-])([O-])=O BNIILDVGGAEEIG-UHFFFAOYSA-L 0.000 claims description 3
- DJEHXEMURTVAOE-UHFFFAOYSA-M potassium bisulfite Chemical compound [K+].OS([O-])=O DJEHXEMURTVAOE-UHFFFAOYSA-M 0.000 claims description 3
- 235000010259 potassium hydrogen sulphite Nutrition 0.000 claims description 3
- 235000010267 sodium hydrogen sulphite Nutrition 0.000 claims description 3
- 239000000047 product Substances 0.000 abstract description 17
- 230000015556 catabolic process Effects 0.000 abstract description 10
- 238000006731 degradation reaction Methods 0.000 abstract description 10
- 230000015572 biosynthetic process Effects 0.000 abstract description 6
- 230000008569 process Effects 0.000 abstract description 6
- 238000003786 synthesis reaction Methods 0.000 abstract description 4
- 238000010521 absorption reaction Methods 0.000 abstract description 3
- 239000006227 byproduct Substances 0.000 abstract description 3
- 239000003208 petroleum Substances 0.000 abstract description 2
- 230000007281 self degradation Effects 0.000 abstract description 2
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 48
- 230000035699 permeability Effects 0.000 description 14
- 230000000052 comparative effect Effects 0.000 description 9
- 239000002253 acid Substances 0.000 description 8
- 230000000903 blocking effect Effects 0.000 description 8
- 238000012360 testing method Methods 0.000 description 8
- 239000007789 gas Substances 0.000 description 7
- 239000007788 liquid Substances 0.000 description 7
- 238000010276 construction Methods 0.000 description 6
- 238000011084 recovery Methods 0.000 description 6
- 230000000694 effects Effects 0.000 description 5
- 229920001661 Chitosan Polymers 0.000 description 4
- 108010010803 Gelatin Proteins 0.000 description 4
- 125000002057 carboxymethyl group Chemical group [H]OC(=O)C([H])([H])[*] 0.000 description 4
- 239000008987 corocalm Substances 0.000 description 4
- 238000002474 experimental method Methods 0.000 description 4
- 239000008273 gelatin Substances 0.000 description 4
- 229920000159 gelatin Polymers 0.000 description 4
- 235000019322 gelatine Nutrition 0.000 description 4
- 235000011852 gelatine desserts Nutrition 0.000 description 4
- 229920000642 polymer Polymers 0.000 description 4
- 239000003431 cross linking reagent Substances 0.000 description 3
- 230000006378 damage Effects 0.000 description 3
- 239000000203 mixture Substances 0.000 description 3
- 239000000178 monomer Substances 0.000 description 3
- BVKZGUZCCUSVTD-UHFFFAOYSA-L Carbonate Chemical compound [O-]C([O-])=O BVKZGUZCCUSVTD-UHFFFAOYSA-L 0.000 description 2
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 2
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 2
- 125000003178 carboxy group Chemical group [H]OC(*)=O 0.000 description 2
- 230000001276 controlling effect Effects 0.000 description 2
- 238000004132 cross linking Methods 0.000 description 2
- 238000001914 filtration Methods 0.000 description 2
- 239000000499 gel Substances 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 230000020477 pH reduction Effects 0.000 description 2
- 238000010008 shearing Methods 0.000 description 2
- 239000012745 toughening agent Substances 0.000 description 2
- JTNCEQNHURODLX-UHFFFAOYSA-N 2-phenylethanimidamide Chemical compound NC(=N)CC1=CC=CC=C1 JTNCEQNHURODLX-UHFFFAOYSA-N 0.000 description 1
- JJPWJEGNCRGGGA-UHFFFAOYSA-N 4-[[2-[5-[2-(2,3-dihydro-1H-inden-2-ylamino)pyrimidin-5-yl]-1,3,4-oxadiazol-2-yl]acetyl]amino]benzoic acid Chemical compound C1C(CC2=CC=CC=C12)NC1=NC=C(C=N1)C1=NN=C(O1)CC(=O)NC1=CC=C(C(=O)O)C=C1 JJPWJEGNCRGGGA-UHFFFAOYSA-N 0.000 description 1
- 208000027418 Wounds and injury Diseases 0.000 description 1
- 230000002378 acidificating effect Effects 0.000 description 1
- -1 acrylic ester Chemical class 0.000 description 1
- 239000000654 additive Substances 0.000 description 1
- 230000000996 additive effect Effects 0.000 description 1
- 125000003277 amino group Chemical group 0.000 description 1
- 239000012267 brine Substances 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 239000013043 chemical agent Substances 0.000 description 1
- 230000006835 compression Effects 0.000 description 1
- 238000007906 compression Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000006073 displacement reaction Methods 0.000 description 1
- 238000004090 dissolution Methods 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000005530 etching Methods 0.000 description 1
- 239000000835 fiber Substances 0.000 description 1
- 239000012530 fluid Substances 0.000 description 1
- 239000011521 glass Substances 0.000 description 1
- 230000002209 hydrophobic effect Effects 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 238000002347 injection Methods 0.000 description 1
- 239000007924 injection Substances 0.000 description 1
- 208000014674 injury Diseases 0.000 description 1
- 239000011229 interlayer Substances 0.000 description 1
- 238000011031 large-scale manufacturing process Methods 0.000 description 1
- 239000010410 layer Substances 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 239000006012 monoammonium phosphate Substances 0.000 description 1
- 238000006116 polymerization reaction Methods 0.000 description 1
- 239000011148 porous material Substances 0.000 description 1
- 229910000343 potassium bisulfate Inorganic materials 0.000 description 1
- GNSKLFRGEWLPPA-UHFFFAOYSA-M potassium dihydrogen phosphate Chemical compound [K+].OP(O)([O-])=O GNSKLFRGEWLPPA-UHFFFAOYSA-M 0.000 description 1
- WFIZEGIEIOHZCP-UHFFFAOYSA-M potassium formate Chemical compound [K+].[O-]C=O WFIZEGIEIOHZCP-UHFFFAOYSA-M 0.000 description 1
- LWIHDJKSTIGBAC-UHFFFAOYSA-K potassium phosphate Substances [K+].[K+].[K+].[O-]P([O-])([O-])=O LWIHDJKSTIGBAC-UHFFFAOYSA-K 0.000 description 1
- 230000008439 repair process Effects 0.000 description 1
- 239000011435 rock Substances 0.000 description 1
- 239000004576 sand Substances 0.000 description 1
- WBHQBSYUUJJSRZ-UHFFFAOYSA-M sodium bisulfate Chemical compound [Na+].OS([O-])(=O)=O WBHQBSYUUJJSRZ-UHFFFAOYSA-M 0.000 description 1
- 229910000342 sodium bisulfate Inorganic materials 0.000 description 1
- 239000011780 sodium chloride Substances 0.000 description 1
- HPALAKNZSZLMCH-UHFFFAOYSA-M sodium;chloride;hydrate Chemical compound O.[Na+].[Cl-] HPALAKNZSZLMCH-UHFFFAOYSA-M 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 239000003381 stabilizer Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 150000005846 sugar alcohols Polymers 0.000 description 1
- 239000004094 surface-active agent Substances 0.000 description 1
- 230000002522 swelling effect Effects 0.000 description 1
- 238000005303 weighing Methods 0.000 description 1
Landscapes
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The invention belongs to the technical field of petroleum exploitation, and particularly relates to a temporary plugging agent for fracturing and acidizing and a preparation method thereof. The preparation method comprises the following steps: sequentially adding itaconic acid, p-styrenesulfonic acid, 2-allyloxymethyl-2-hydroxymethyl propane-1, 3-diol, vinyl pyridine, pentaerythritol diacrylate, buffer salt and deionized water into a reactor, stirring, and adjusting the pH value until all raw materials are completely dissolved; dripping initiator from a high-level dripping tank, automatically heating the reaction, preserving heat for reaction, adding reducing agent, stopping the reaction, and regulating the pH value to obtain temporary plugging agent solution; and (3) drying and granulating the temporary plugging agent solution to obtain the product temporary plugging agent. The preparation method has the characteristics of simple synthesis process and no byproducts; the temporary plugging agent has the advantages of large water absorption, high plugging strength, high breakthrough pressure, self-degradation and capability of designing degradation time.
Description
Technical Field
The invention belongs to the technical field of petroleum exploitation, and particularly relates to a temporary plugging agent for fracturing and acidizing and a preparation method thereof.
Background
The low permeability oil and gas reservoirs in China are wide in distribution and large in reserves, and the low permeability oil and gas resources are found to account for more than 50% of the ascertained reserves at present. However, due to severe formation heterogeneity, small reservoir pore throats, and large inter-layer permeability coefficient of variation, modification of the formation is required.
Fracture acidizing is an important measure for large-scale production increase reconstruction of carbonate oil and gas fields. The main factors controlling the success of fracture acidizing are two, namely the effective length of the final acid fracturing fracture and the diversion capability of the acid etching fracture after acid fracturing. The acid liquor filtration has important influence on both factors, and the influence on the extension of the artificial main fracture is more obvious. When the large acid fracturing yield-increasing reconstruction of the fractured carbonate reservoir is carried out, acid liquor is seriously lost, a main fluid loss channel is a natural fracture, a temporary plugging agent needs to be added in the acid fracturing process to temporarily plug the natural fracture, and the artificial fracture is promoted to extend to a far well zone.
To solve this problem, temporary plugging fracture acidizing techniques have been developed, and the performance of temporary plugging agents is critical to the effective implementation of temporary plugging acidizing techniques.
The temporary plugging agent is a chemical agent with a temporary plugging effect and is used for protecting an unintended layer from operation injury in the operation of an oil-water well. The degradation performance of the temporary plugging agent is related to whether the temporary plugging agent can effectively plug cracks or not and whether the plugging removal can be realized or not. If the degradability of the temporary plugging agent is poor, the temporary plugging agent cannot be degraded quickly after the fracturing construction is finished, and the temporary plugging agent is filled between propping agents for a long time to prevent normal permeation of oil and gas, so that the purpose of fracturing can be achieved, but the yield of the oil and gas field cannot be increased, and the yield is affected.
CN107090282a discloses a mixed temporary plugging agent, a temporary plugging agent mixture, a temporary plugging method and application, the mixed temporary plugging agent comprises the following components in parts by weight: 1-9 parts of water-soluble high molecular polymer, 3-29 parts of sand and 0-19 parts of soluble or degradable fiber. And preparing the mixed temporary plugging agent into a temporary plugging agent mixture by using 10-100 parts by weight of carrying liquid, and displacing the temporary plugging agent mixture into a preset position of an underground crack by using displacing liquid to form the temporary plugging wall with certain viscosity. The method can be applied to vertical well stratified fracturing, horizontal well staged fracturing and old well repeated fracturing, the plugging position of the method can be controlled by controlling the viscosity starting time (according to the concentration of temporary plugging agents) and the injection speed (according to the volume of a shaft and the displacement fluid), 100% plugging is achieved, the plugging strength is high, the subsequent fracturing to open new joints (increase new leakage flow areas) is facilitated, and the yield of an oil-gas well is further improved. However, after the construction is finished, the temporary plugging agent cannot be automatically degraded, and ammonium persulfate is required to be added for breaking the gel, so that the construction difficulty is increased.
CN106905940a discloses a middle-high density elastic liquid rubber plug and a well repairing method, which relate to the field of oil-gas chemical industry. The middle-high density elastic liquid rubber plug is mainly prepared from the following components in parts by weight through a crosslinking reaction: 3-5 parts of polymer, 0.25-1.5 parts of first cross-linking agent, 2-4 parts of second cross-linking agent, 0.015-0.035 parts of stabilizer, 0.2-0.8 parts of additive and 98-102 parts of weighting agent solution. The concentration of weighting agent solution is 40-85×10 4 mg/L aqueous potassium formate solution. The density can reach 1.2-1.3g/cm 3 . The preparation method of the middle-high density elastic liquid rubber plug has good fluidity at low temperature, can rapidly generate crosslinking reaction at high temperature in the pit, and has the advantages of adjustable density, temperature resistance, pressure resistance, good pumpability, good stability, no need of gel breaking process, high efficiency in flowback and the like. However, after the well repair is finished, the liquid rubber plug is broken into elastic rubber plug particles only through concentrated damage of a certain external force, and then the elastic rubber plug particles are circularly washed by using brine well control liquid, so that the process is complex.
CN113150758A discloses a pH-sensitive temporary plugging agent, a preparation method thereof and application thereof in exploitation of low-permeability oil reservoirs, and relates to the technical field of oil field exploitation. The temporary plugging agent provided by the invention comprises the following preparation raw materials in percentage by mass: 3 to 8 percent of carboxymethyl chitosan, 0.2 to 0.7 percent of gelatin, 0.1 to 0.6 percent of initiator, 5 to 15 percent of toughening agent and the balance of water. According to the invention, carboxymethyl chitosan and gelatin are used as main materials, the carboxymethyl chitosan and gelatin can be copolymerized, and a toughening agent and an initiator are used as auxiliary materials, so that the obtained temporary plugging agent is a pH sensitive temporary plugging agent, and when the pH value in a medium changes, the hydrophilic properties of free amino groups and carboxyl groups on the carboxymethyl chitosan and gelatin molecular chain can be obviously changed, and different swelling properties are shown. The pH sensitive temporary plugging agent provided by the invention has the advantages of good plugging effect, strong acid resistance, stable existence under acidic conditions, degradability by using an alkaline solvent and small damage to stratum. However, the plugging rate of the temporary plugging agent is only about 90%, and the plugging effect is still to be further improved.
Disclosure of Invention
The invention provides a temporary plugging agent for fracture acidizing and a preparation method thereof, aiming at the defects in the prior art. The preparation method has the characteristics of simple synthesis process and no byproducts; the temporary plugging agent has the advantages of large water absorption, high plugging strength, high breakthrough pressure, self-degradation and capability of designing degradation time.
The invention discloses a temporary plugging agent for fracture acidizing, which has the following molecular structural formula:
wherein:
a＝500-20000
b＝20000-200000
c＝4000-40000
d＝8000-80000
e＝4000-40000
f＝500-20000
g＝20000-200000
h＝4000-40000
i＝8000-80000
j＝4000-40000。
preferably, the temporary plugging agent has a viscosity average molecular weight of 25000000-35000000.
The invention further discloses a preparation method of the temporary plugging agent for fracture acidizing, which comprises the following specific steps:
(1) Sequentially adding itaconic acid, p-styrenesulfonic acid, 2-allyloxymethyl-2-hydroxymethyl propane-1, 3-diol, vinylpyridine, pentaerythritol diacrylate, buffer salt and deionized water into a reactor, purging a reaction kettle and a pipeline for 5-10min by nitrogen to ensure nitrogen micro-positive pressure, starting stirring, and adjusting pH to 7-7.5 until all raw materials are completely dissolved;
(2) Dripping initiator from a high-level dripping tank, automatically heating up the reaction, continuing the reaction for 10-20min after the temperature is not raised any more, heating up to 55-60 ℃, preserving heat for 30-60min, adding reducing agent, stopping the reaction, and regulating the pH value to 7-7.5 to obtain temporary plugging agent solution;
(3) And (3) drying and granulating the temporary plugging agent solution, wherein the particle size is 0.4-2mm, and obtaining the product temporary plugging agent.
Preferably, the p-styrenesulfonic acid, 2-allyloxymethyl-2-hydroxymethylpropane-1, 3-diol, vinylpyridine, pentaerythritol diacrylate are used in an amount of 0.1-0.2, 0.2-0.4, 0.1-0.2, 0.01-0.05, respectively, based on 1 mole part of itaconic acid.
Preferably, in the step (1), the buffer salt is one of sodium dihydrogen phosphate, potassium dihydrogen phosphate, ammonium dihydrogen phosphate, disodium hydrogen phosphate, dipotassium hydrogen phosphate and diammonium hydrogen phosphate, and the weight ratio of the buffer salt to itaconic acid is 0.05-0.1:1.
more preferably, the buffer salt is one of sodium dihydrogen phosphate, potassium dihydrogen phosphate and ammonium dihydrogen phosphate.
Preferably, in the step (1), the weight ratio of deionized water to itaconic acid is 5-8:1.
preferably, in the step (2), the initiator is one of potassium persulfate aqueous solution, ammonium persulfate aqueous solution and sodium persulfate aqueous solution, the concentration is 8-12wt%, and the weight ratio of the initiator to itaconic acid is 0.1-0.3:1.
preferably, in the step (2), the reducing agent is one of sodium sulfite aqueous solution, potassium sulfite aqueous solution, sodium bisulfate aqueous solution and potassium bisulfate aqueous solution, the concentration is 8-12wt%, and the weight ratio of the reducing agent to the itaconic acid is 0.1-0.3:1.
the reaction equation of the synthesis of the temporary plugging agent for fracture acidizing is as follows:
the temporary plugging agent for fracturing and acidizing is a five-membered high molecular polymer, and the polymerization monomers are itaconic acid, p-styrenesulfonic acid, 2-allyloxymethyl-2-hydroxymethyl propane-1, 3-diol, vinyl pyridine and pentaerythritol diacrylate. Itaconic acid is a main polymer body, contains two carboxyl groups in the molecule, has very good water absorption, can greatly improve the volume of a product and improve the volume of blockage; the p-styrenesulfonic acid belongs to a hard surfactant, so that the shearing resistance of a product can be improved, the wettability and the permeability are improved, and the whole molecule can be closely contacted with the surface of rock, so that the blocking effect is greatly improved; 2-allyloxymethyl-2-hydroxymethyl propane-1, 3-diol belongs to polyalcohol, which can greatly improve the volume of the product and the volume of the blockage wave; the vinyl pyridine belongs to a rigid monomer, can improve the blocking strength and the shearing resistance of the product, has certain surface activity, and is beneficial to the improvement of blocking rate of a hydrophobic section of a soaked stratum; pentaerythritol diacrylate belongs to a cross-linking agent, can change the whole molecule from a one-dimensional structure into a two-dimensional structure and a three-dimensional structure, greatly increases the molecular weight, increases the swept volume, increases the blocking capacity of products, and increases the compression resistance, meanwhile, the acrylic ester can be hydrolyzed at high temperature, and the degradation time of the products can be controlled by adjusting the dosage.
Compared with the prior art, the invention has the following advantages and beneficial effects:
(1) The temporary plugging agent for fracturing and acidizing has the advantages of easily available synthetic raw materials, simple synthesis process and no byproducts;
(2) The temporary plugging agent for fracturing and acidizing can be automatically degraded by adjusting the proportion of the formula, and the degradation time is controlled to be 12-54h, so that the construction is simple;
(3) The temporary plugging agent for fracture acidizing has higher plugging rate and plugging removal rate, and both the plugging rate and the plugging removal rate reach more than 98 percent;
(4) The temporary plugging agent for fracture acidizing has higher plugging strength, the breakthrough pressure gradient of the low-permeability core can reach 265MPa/m at the highest, and the breakthrough pressure gradient of the high-permeability core can reach 190MPa/m at the highest.
Detailed Description
The endpoints and any values of the ranges disclosed herein are not limited to the precise range or value, and are understood to encompass values approaching those ranges or values. For numerical ranges, one or more new numerical ranges may be found between the endpoints of each range, between the endpoint of each range and the individual point value, and between the individual point value, in combination with each other, and are to be considered as specifically disclosed herein.
Example 1
(1) Sequentially adding 0.5mol of itaconic acid, 0.05mol of p-styrenesulfonic acid, 0.2mol of 2-allyloxymethyl-2-hydroxymethyl propane-1, 3-diol, 0.05mol of vinyl pyridine, 0.005mol of pentaerythritol diacrylate, 3.25g of sodium dihydrogen phosphate and 325g of deionized water into a reactor, purging a reaction kettle and a pipeline for 5min by using nitrogen, ensuring nitrogen slight positive pressure, starting stirring, and regulating pH to 7-7.5 by using sodium hydroxide solution until all raw materials are completely dissolved;
(2) Dropwise adding an initiator from a high-level dropwise adding tank, wherein the initiator is 13.4g of 8wt% potassium persulfate solution, the reaction is automatically heated, the reaction is continued for 20min after the temperature is not increased any more, the temperature is raised to 55 ℃, the reaction is kept for 60min, a reducing agent is added, the reducing agent is 12.8g of 8wt% potassium sulfite solution, the reaction is stopped, and the pH value is regulated to 7-7.5 by sodium hydroxide solution, so that a temporary plugging agent solution is obtained;
(3) And (3) drying and granulating the temporary plugging agent solution, wherein the particle size is 0.4-2mm, and obtaining the product temporary plugging agent.
Example 2
(1) 0.5mol of itaconic acid, 0.07mol of p-styrenesulfonic acid, 0.16mol of 2-allyloxymethyl-2-hydroxymethyl propane-1, 3-diol, 0.06mol of vinyl pyridine, 0.008mol of pentaerythritol diacrylate, 3.83g of sodium dihydrogen phosphate and 447g of deionized water are sequentially added into a reactor, a reaction kettle and a pipeline are purged with nitrogen for 6min, nitrogen slight positive pressure is ensured, stirring is started, and the pH value is regulated to 7-7.5 by a sodium hydroxide solution until all raw materials are completely dissolved;
(2) Dripping an initiator from a high-level dripping tank, wherein the initiator is 8.98g of 10wt% potassium persulfate solution, the reaction is automatically heated, the reaction is continued for 10min after the temperature is not raised any more, the temperature is raised to 60 ℃, the reaction is kept for 30min, a reducing agent is added, the reducing agent is 10.3g of 12wt% potassium sulfite solution, the reaction is stopped, and the pH value is regulated to 7-7.5 by sodium hydroxide solution, so as to obtain a temporary plugging agent solution;
(3) And (3) drying and granulating the temporary plugging agent solution, wherein the particle size is 0.4-2mm, and obtaining the product temporary plugging agent.
Example 3
(1) 0.5mol of itaconic acid, 0.06mol of p-styrenesulfonic acid, 0.14mol of 2-allyloxymethyl-2-hydroxymethyl propane-1, 3-diol, 0.07mol of vinyl pyridine, 0.01mol of pentaerythritol diacrylate, 5.84g of monopotassium phosphate and 500g of deionized water are sequentially added into a reactor, a reaction kettle and a pipeline are purged with nitrogen for 8 minutes, nitrogen slight positive pressure is ensured, stirring is started, and the pH value is regulated to 7-7.5 by a sodium hydroxide solution until all raw materials are completely dissolved;
(2) Dropwise adding an initiator from a high-level dropwise adding tank, wherein the initiator is 6.5g of 12wt% potassium persulfate solution, the reaction is automatically heated, the reaction is continued for 15min after the temperature is not increased any more, the temperature is raised to 60 ℃, the reaction is kept for 30min, a reducing agent is added, the reducing agent is 6.5g of 12wt% potassium hydrogen sulfite solution, the reaction is stopped, and the pH value is regulated to 7-7.5 by sodium hydroxide solution to obtain a temporary plugging agent solution;
(3) And (3) drying and granulating the temporary plugging agent solution, wherein the particle size is 0.4-2mm, and obtaining the product temporary plugging agent.
Example 4
(1) 0.5mol of itaconic acid, 0.08mol of p-styrenesulfonic acid, 0.12mol of 2-allyloxymethyl-2-hydroxymethyl propane-1, 3-diol, 0.08mol of vinyl pyridine, 0.013mol of pentaerythritol diacrylate, 6.5g of dipotassium hydrogen phosphate and 474g of deionized water are sequentially added into a reactor, a reaction kettle and a pipeline are purged with nitrogen for 10 minutes, nitrogen slight positive pressure is ensured, stirring is started, and the pH value is regulated to 7-7.5 by a sodium hydroxide solution until all raw materials are completely dissolved;
(2) Dropwise adding an initiator from a high-level dropwise adding tank, wherein the initiator is 19.5g of 8wt% ammonium persulfate solution, the reaction is automatically heated, the reaction is continued for 15min after the temperature is not increased any more, the temperature is raised to 55 ℃, the reaction is kept for 60min, a reducing agent is added, the reducing agent is 11.3g of 12wt% sodium sulfite solution, the reaction is stopped, and the pH value is regulated to 7-7.5 by sodium hydroxide solution to obtain a temporary plugging agent solution;
(3) And (3) drying and granulating the temporary plugging agent solution, wherein the particle size is 0.4-2mm, and obtaining the product temporary plugging agent.
Example 5
(1) 0.5mol of itaconic acid, 0.09mol of p-styrenesulfonic acid, 0.14mol of 2-allyloxymethyl-2-hydroxymethyl propane-1, 3-diol, 0.09mol of vinyl pyridine, 0.017mol of pentaerythritol diacrylate, 4.76g of monoammonium phosphate and 520g of deionized water are sequentially added into a reactor, a reaction kettle and a pipeline are purged with nitrogen for 7min, nitrogen slight positive pressure is ensured, stirring is started, and the pH value is regulated to 7-7.5 by a sodium hydroxide solution until all raw materials are completely dissolved;
(2) Dropwise adding an initiator from a high-level dropwise adding tank, wherein the initiator is 12.7g of 10wt% ammonium persulfate solution, the reaction is automatically heated, the reaction is continued for 13min after the temperature is not increased any more, the temperature is raised to 58 ℃, the reaction is kept for 40min, a reducing agent is added, the reducing agent is 12.1g of 10wt% sodium bisulfite solution, the reaction is stopped, and the pH value is regulated to 7-7.5 by sodium hydroxide solution to obtain a temporary plugging agent solution;
(3) And (3) drying and granulating the temporary plugging agent solution, wherein the particle size is 0.4-2mm, and obtaining the product temporary plugging agent.
Example 6
(1) Sequentially adding 0.5mol of itaconic acid, 0.1mol of p-styrenesulfonic acid, 0.1mol of 2-allyloxymethyl-2-hydroxymethyl propane-1, 3-diol, 0.08mol of vinyl pyridine, 0.02mol of pentaerythritol diacrylate, 5.22g of disodium hydrogen phosphate and 383g of deionized water into a reactor, purging a reaction kettle and a pipeline for 10min by nitrogen, ensuring nitrogen slight positive pressure, starting stirring, and regulating pH to 7-7.5 by sodium hydroxide solution until all raw materials are completely dissolved;
(2) Dropwise adding an initiator from a high-level dropwise adding tank, wherein the initiator is 19.5g of 8wt% ammonium persulfate solution, the reaction is automatically heated, the reaction is continued for 18min after the temperature is not increased any more, the temperature is raised to 58 ℃, the reaction is kept for 30min, a reducing agent is added, the reducing agent is 19.5g of 8wt% potassium hydrogen sulfite solution, the reaction is stopped, and the pH value is regulated to 7-7.5 by sodium hydroxide solution to obtain a temporary plugging agent solution;
(3) And (3) drying and granulating the temporary plugging agent solution, wherein the particle size is 0.4-2mm, and obtaining the product temporary plugging agent.
Example 7
(1) 0.5mol of itaconic acid, 0.07mol of p-styrenesulfonic acid, 0.18mol of 2-allyloxymethyl-2-hydroxymethyl propane-1, 3-diol, 0.05mol of vinyl pyridine, 0.022mol of pentaerythritol diacrylate, 6.13g of dipotassium hydrogen phosphate and 417g of deionized water are sequentially added into a reactor, a reaction kettle and a pipeline are purged with nitrogen for 5 minutes, nitrogen micro-positive pressure is ensured, stirring is started, and the pH value is regulated to 7-7.5 by a sodium hydroxide solution until all raw materials are completely dissolved;
(2) Dripping an initiator from a high-level dripping tank, wherein the initiator is 16g of 12wt% sodium persulfate solution, the reaction is automatically heated, the reaction is continued for 15min after the temperature is not raised any more, the temperature is raised to 56 ℃, the reaction is kept for 50min, a reducing agent is added, the reducing agent is 15g of 12wt% sodium sulfite solution, the reaction is stopped, and the pH value is regulated to 7-7.5 by sodium hydroxide solution, so as to obtain a temporary plugging agent solution;
(3) And (3) drying and granulating the temporary plugging agent solution, wherein the particle size is 0.4-2mm, and obtaining the product temporary plugging agent.
Example 8
(1) 0.5mol of itaconic acid, 0.08mol of p-styrenesulfonic acid, 0.16mol of 2-allyloxymethyl-2-hydroxymethyl propane-1, 3-diol, 0.1mol of vinyl pyridine, 0.025mol of pentaerythritol diacrylate, 6.11g of diammonium hydrogen phosphate and 464g of deionized water are sequentially added into a reactor, a reaction kettle and a pipeline are purged with nitrogen for 8 minutes, nitrogen slight positive pressure is ensured, stirring is started, and the pH value is regulated to 7-7.5 by a sodium hydroxide solution until all raw materials are completely dissolved;
(2) Dropwise adding an initiator from a high-level dropwise adding tank, wherein the initiator is 18g of 8wt% sodium persulfate solution, the reaction is automatically heated, the reaction is continued for 20min after the temperature is not increased any more, the temperature is raised to 55 ℃, the reaction is kept for 60min, a reducing agent is added, the reducing agent is 18.8g of 10wt% sodium bisulfite solution, the reaction is stopped, and the pH value is regulated to 7-7.5 by sodium hydroxide solution to obtain a temporary plugging agent solution;
(3) And (3) drying and granulating the temporary plugging agent solution, wherein the particle size is 0.4-2mm, and obtaining the product temporary plugging agent.
Example 9
Adding 50000mg/L sodium chloride solution into a series of pressure-resistant wide-mouth bottles respectively, regulating pH to 1-1.5 with hydrochloric acid, heating to 90 ℃ with an oil bath, adding temporary plugging agent with certain mass, maintaining at 90 ℃, taking out the glass bottles for a while, pouring the temporary plugging agent into a standard sieve for filtration, putting the filtered water back into the wide-mouth bottles, rapidly weighing the mass of the temporary plugging agent, putting the temporary plugging agent back into the wide-mouth bottles, continuing to keep constant temperature at 90 ℃, calculating expansion multiple n, and carrying out a comparison experiment with JX temporary plugging agent of Dou Jian Xiangshu crown technology Co, wherein the test results are shown in table 1.
n＝m 1 /m 0
Wherein:
n-expansion times;
m 1 the mass of the temporary plugging agent after expansion, g;
m 0 temporary plugging agent mass, g.
As can be seen from table 1:
(1) The expansion coefficient of the temporary plugging agent (examples 1-8) for fracture acidification is more than 10 and reaches 12.6 (example 6) at the maximum at 90 ℃ for 15min, and the expansion coefficient of the JX temporary plugging agent (comparative example) of Shuxiang Shuguan science and technology Co., ltd.) is 6, which is obviously lower than that of the temporary plugging agent;
(2) The expansion coefficient of the temporary plugging agent (examples 1-8) for fracture acidification is more than 17 and reaches 20.7 at most (example 6) at 90 ℃ for 60min, and the expansion coefficient of the JX temporary plugging agent of Shuxiang Shuguan science and technology Co., ltd is 11, which is obviously lower than that of the temporary plugging agent;
(3) The expansion coefficient of the temporary plugging agent (examples 1-8) for fracture acidizing provided by the invention is more than 21 and is up to 25 (example 6) at the temperature of 90 ℃ for 150min, and the expansion coefficient of the JX temporary plugging agent (comparative example) is 14, which is obviously lower than that of the temporary plugging agent.
The temporary plugging agent for fracturing and acidizing has good water plugging effect.
Example 10
Example 9 after 150min of continuous test, the temporary plugging agent was not absorbed water, and after a period of time, the temporary plugging agent was gradually dissolved, and the time after complete dissolution, namely the degradation time of the temporary plugging agent, was used as a comparative experiment, and the test results are shown in table 2.
As can be seen from table 2: the degradation time of the temporary plugging agent (examples 1-8) for fracturing and acidizing is in the range of 12-54 h. The degradation time can be controlled by designing the proportion of the monomers of the temporary plugging agent according to the construction operation requirement. The comparative example needs to add a blocking remover to carry out blocking removal, and construction difficulty is increased.
Example 11
The temporary plugging rate and permeability recovery rate (plugging removal rate) were tested by referring to the method of Q/SH1020 2187-2018 general technical Condition for Water-soluble temporary plugging Agents, and comparative experiments were conducted with JX temporary plugging Agents, a Chengdu-Xiang Shuguan-Technical Co., ltd. And the test results are shown in Table 2.
As can be seen from table 2: the temporary plugging rate and the permeability recovery rate (plugging removal rate) of the temporary plugging agent (examples 1-8) for fracturing and acidizing are both more than 98%, wherein the temporary plugging rate is up to 99.5% (example 1), the permeability recovery rate (plugging removal rate) is up to 99.2% (example 8), and the temporary plugging rate and the permeability recovery rate of the JX temporary plugging agent (comparative example) of all-in-one Shuguan sciences Co., ltd are respectively 94% and 89.6%, which are obviously lower than the temporary plugging agent.
Example 12
Artificially-sealed cores with different permeabilities (low permeability core permeability 0.0472 μm) are used at 90deg.C 2 The length is 6.3cm; the permeability of the hypertonic core is 0.286 mu m 2 6.5cm in length) was extruded with a 1PV concentration of 10g/L temporary plugging agent, the breakthrough pressure and the breakthrough pressure gradient of the temporary plugging agent were tested, and comparative experiments were conducted with JX temporary plugging agent, a product of Duxiang Shuguan science and technology Co., ltd., and the test results are shown in Table 3.
TABLE 1 results of testing expansion times at different times
TABLE 2 test results of degradation time, temporary blocking Rate, permeability recovery Rate
| Temporary plugging agent | Degradation time, h | Temporary blocking rate, percent | Permeability recovery% |
| Example 1 | 54 | 99.5 | 98.1 |
| Example 2 | 46 | 99.2 | 98.4 |
| Example 3 | 37 | 99 | 98.5 |
| Example 4 | 28 | 98.8 | 98.6 |
| Example 5 | 22 | 98.5 | 98.7 |
| Example 6 | 17 | 98.4 | 99 |
| Example 7 | 15 | 99.3 | 98.4 |
| Example 8 | 12 | 98.2 | 99.2 |
| Comparative example | Does not degrade | 94 | 89.6 |
Table 3 results of breakthrough pressure and breakthrough pressure gradient tests for different cores
From table 3 it can be seen that: the temporary plugging agent for fracture acidizing (examples 1-8) has higher plugging strength, wherein the breakthrough pressure gradient of a low-permeability core reaches more than 195MPa/m, the maximum value reaches 265MPa/m (example 8), the breakthrough pressure gradient of a high-permeability core reaches more than 130MPa/m, and the maximum value reaches 190MPa/m; the breakthrough pressure gradients of the low-permeability core and the high-permeability core of the JX temporary plugging agent of the Shu Guanyu science and technology Co., ltd.in the comparative example are 87.3MPa/m and 64.6MPa/m respectively, which are obviously lower than that of the temporary plugging agent of the invention.
The preferred embodiments of the present invention have been described in detail above, but the present invention is not limited thereto. Within the scope of the technical idea of the invention, a number of simple variants of the technical solution of the invention are possible, including combinations of the individual technical features in any other suitable way, which simple variants and combinations should likewise be regarded as being disclosed by the invention, all falling within the scope of protection of the invention.
Claims (9)
1. The preparation method of the temporary plugging agent for fracture acidizing is characterized by comprising the following specific steps:
(1) Sequentially adding itaconic acid, p-styrenesulfonic acid, 2-allyloxymethyl-2-hydroxymethyl propane-1, 3-diol, vinylpyridine, pentaerythritol diacrylate, buffer salt and deionized water into a reactor, purging a reaction kettle and a pipeline for 5-10min by nitrogen to ensure nitrogen micro-positive pressure, starting stirring, and adjusting pH to 7-7.5 until all raw materials are completely dissolved;
(2) Dripping initiator from a high-level dripping tank, automatically heating up the reaction, continuing the reaction for 10-20min after the temperature is not raised any more, heating up to 55-60 ℃, preserving heat for 30-60min, adding reducing agent, stopping the reaction, and regulating the pH value to 7-7.5 to obtain temporary plugging agent solution;
(3) And (3) drying and granulating the temporary plugging agent solution, wherein the particle size is 0.4-2mm, and obtaining the product temporary plugging agent.
2. The method for preparing a temporary plugging agent for fracture acidizing according to claim 1, wherein the dosage of the p-styrenesulfonic acid, the 2-allyloxymethyl-2-hydroxymethylpropane-1, 3-diol, the vinylpyridine and the pentaerythritol diacrylate is 0.1-0.2, 0.2-0.4, 0.1-0.2 and 0.01-0.05 mole parts respectively based on 1 mole part of itaconic acid.
3. The method for preparing a temporary plugging agent for fracture acidizing as claimed in claim 1, wherein in the step (1), the buffer salt is one of sodium dihydrogen phosphate, potassium dihydrogen phosphate, ammonium dihydrogen phosphate, disodium hydrogen phosphate, dipotassium hydrogen phosphate and diammonium hydrogen phosphate, and the weight ratio of the buffer salt to the itaconic acid is 0.05-0.1:1.
4. the method for preparing a temporary plugging agent for fracture acidizing as claimed in claim 3, wherein the buffer salt is one of sodium dihydrogen phosphate, potassium dihydrogen phosphate and ammonium dihydrogen phosphate.
5. The method for preparing the temporary plugging agent for fracture acidizing as claimed in claim 1, wherein in the step (1), the weight ratio of deionized water to itaconic acid is 5-8:1.
6. the preparation method of the temporary plugging agent for fracture acidizing according to claim 1, wherein in the step (2), the initiator is one of a potassium persulfate aqueous solution, an ammonium persulfate aqueous solution and a sodium persulfate aqueous solution, the concentration is 8-12wt%, and the weight ratio of the initiator to itaconic acid is 0.1-0.3:1.
7. the method for preparing a temporary plugging agent for fracture acidizing according to claim 1, wherein in the step (2), the reducing agent is one of sodium sulfite aqueous solution, potassium sulfite aqueous solution, sodium bisulfite aqueous solution and potassium hydrogen sulfite aqueous solution, the concentration is 8-12wt%, and the weight ratio of the reducing agent to itaconic acid is 0.1-0.3:1.
8. the temporary plugging agent for fracture acidizing is characterized by comprising the following molecular structural formula:
wherein:
a＝500-20000
b＝20000-200000
c＝4000-40000
d＝8000-80000
e＝4000-40000
f＝500-20000
g＝20000-200000
h＝4000-40000
i＝8000-80000
j＝4000-40000。
9. the temporary plugging agent for fracture acidizing of claim 8, wherein said temporary plugging agent has a viscosity average molecular weight of 25000000-35000000.
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