CN111763506A - Temporary plugging diverting agent and preparation method and application thereof - Google Patents
Temporary plugging diverting agent and preparation method and application thereof Download PDFInfo
- Publication number
- CN111763506A CN111763506A CN202010657698.XA CN202010657698A CN111763506A CN 111763506 A CN111763506 A CN 111763506A CN 202010657698 A CN202010657698 A CN 202010657698A CN 111763506 A CN111763506 A CN 111763506A
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- Prior art keywords
- temporary plugging
- polyglycolic acid
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- 239000003795 chemical substances by application Substances 0.000 claims abstract description 127
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- 239000004633 polyglycolic acid Substances 0.000 claims abstract description 103
- AEMRFAOFKBGASW-UHFFFAOYSA-N Glycolic acid Chemical compound OCC(O)=O AEMRFAOFKBGASW-UHFFFAOYSA-N 0.000 claims abstract description 69
- 229920001577 copolymer Polymers 0.000 claims abstract description 22
- 229920001519 homopolymer Polymers 0.000 claims abstract description 12
- 239000002994 raw material Substances 0.000 claims abstract description 6
- 238000005187 foaming Methods 0.000 claims description 48
- 238000006243 chemical reaction Methods 0.000 claims description 27
- 230000000903 blocking effect Effects 0.000 claims description 24
- 238000000034 method Methods 0.000 claims description 24
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- 239000002245 particle Substances 0.000 claims description 15
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- 125000005587 carbonate group Chemical group 0.000 claims description 3
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- VTYYLEPIZMXCLO-UHFFFAOYSA-L Calcium carbonate Chemical compound [Ca+2].[O-]C([O-])=O VTYYLEPIZMXCLO-UHFFFAOYSA-L 0.000 description 6
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- DOIRQSBPFJWKBE-UHFFFAOYSA-N dibutyl phthalate Chemical compound CCCCOC(=O)C1=CC=CC=C1C(=O)OCCCC DOIRQSBPFJWKBE-UHFFFAOYSA-N 0.000 description 4
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- VEZXCJBBBCKRPI-UHFFFAOYSA-N beta-propiolactone Chemical group O=C1CCO1 VEZXCJBBBCKRPI-UHFFFAOYSA-N 0.000 description 2
- 230000015572 biosynthetic process Effects 0.000 description 2
- BJQHLKABXJIVAM-UHFFFAOYSA-N bis(2-ethylhexyl) phthalate Chemical compound CCCCC(CC)COC(=O)C1=CC=CC=C1C(=O)OCC(CC)CCCC BJQHLKABXJIVAM-UHFFFAOYSA-N 0.000 description 2
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- 229920000747 poly(lactic acid) Polymers 0.000 description 2
- 229920001606 poly(lactic acid-co-glycolic acid) Polymers 0.000 description 2
- 229920002961 polybutylene succinate Polymers 0.000 description 2
- 239000004631 polybutylene succinate Substances 0.000 description 2
- 238000006068 polycondensation reaction Methods 0.000 description 2
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- 238000007789 sealing Methods 0.000 description 2
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 2
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- YFHICDDUDORKJB-UHFFFAOYSA-N trimethylene carbonate Chemical group O=C1OCCCO1 YFHICDDUDORKJB-UHFFFAOYSA-N 0.000 description 2
- 238000005303 weighing Methods 0.000 description 2
- ZNLAHAOCFKBYRH-UHFFFAOYSA-N 1,4-dioxane-2,3-dione Chemical group O=C1OCCOC1=O ZNLAHAOCFKBYRH-UHFFFAOYSA-N 0.000 description 1
- WSQZNZLOZXSBHA-UHFFFAOYSA-N 3,8-dioxabicyclo[8.2.2]tetradeca-1(12),10,13-triene-2,9-dione Chemical compound O=C1OCCCCOC(=O)C2=CC=C1C=C2 WSQZNZLOZXSBHA-UHFFFAOYSA-N 0.000 description 1
- YEJRWHAVMIAJKC-UHFFFAOYSA-N 4-Butyrolactone Chemical group O=C1CCCO1 YEJRWHAVMIAJKC-UHFFFAOYSA-N 0.000 description 1
- 239000005995 Aluminium silicate Substances 0.000 description 1
- 208000003643 Callosities Diseases 0.000 description 1
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical group [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- 241000196324 Embryophyta Species 0.000 description 1
- IAYPIBMASNFSPL-UHFFFAOYSA-N Ethylene oxide Chemical compound C1CO1 IAYPIBMASNFSPL-UHFFFAOYSA-N 0.000 description 1
- 206010020649 Hyperkeratosis Diseases 0.000 description 1
- 241001465754 Metazoa Species 0.000 description 1
- 229910019142 PO4 Inorganic materials 0.000 description 1
- 239000004698 Polyethylene Substances 0.000 description 1
- 239000004743 Polypropylene Substances 0.000 description 1
- 229920002472 Starch Polymers 0.000 description 1
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- 239000000654 additive Substances 0.000 description 1
- 239000000853 adhesive Substances 0.000 description 1
- 230000001070 adhesive effect Effects 0.000 description 1
- WNLRTRBMVRJNCN-UHFFFAOYSA-L adipate(2-) Chemical compound [O-]C(=O)CCCCC([O-])=O WNLRTRBMVRJNCN-UHFFFAOYSA-L 0.000 description 1
- 230000002411 adverse Effects 0.000 description 1
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- 238000004364 calculation method Methods 0.000 description 1
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- 230000000739 chaotic effect Effects 0.000 description 1
- 239000013043 chemical agent Substances 0.000 description 1
- KRKNYBCHXYNGOX-UHFFFAOYSA-N citric acid Chemical class OC(=O)CC(O)(C(O)=O)CC(O)=O KRKNYBCHXYNGOX-UHFFFAOYSA-N 0.000 description 1
- 238000004140 cleaning Methods 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 239000012153 distilled water Substances 0.000 description 1
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- JBFHTYHTHYHCDJ-UHFFFAOYSA-N gamma-caprolactone Chemical group CCC1CCC(=O)O1 JBFHTYHTHYHCDJ-UHFFFAOYSA-N 0.000 description 1
- 238000009776 industrial production Methods 0.000 description 1
- 239000003999 initiator Substances 0.000 description 1
- NLYAJNPCOHFWQQ-UHFFFAOYSA-N kaolin Chemical compound O.O.O=[Al]O[Si](=O)O[Si](=O)O[Al]=O NLYAJNPCOHFWQQ-UHFFFAOYSA-N 0.000 description 1
- 235000014655 lactic acid Nutrition 0.000 description 1
- 239000000314 lubricant Substances 0.000 description 1
- 229920002521 macromolecule Polymers 0.000 description 1
- 239000010445 mica Substances 0.000 description 1
- 229910052618 mica group Inorganic materials 0.000 description 1
- 244000005700 microbiome Species 0.000 description 1
- 239000003607 modifier Substances 0.000 description 1
- BDJRBEYXGGNYIS-UHFFFAOYSA-N nonanedioic acid Chemical compound OC(=O)CCCCCCCC(O)=O BDJRBEYXGGNYIS-UHFFFAOYSA-N 0.000 description 1
- QIQXTHQIDYTFRH-UHFFFAOYSA-N octadecanoic acid Chemical compound CCCCCCCCCCCCCCCCCC(O)=O QIQXTHQIDYTFRH-UHFFFAOYSA-N 0.000 description 1
- 238000004806 packaging method and process Methods 0.000 description 1
- 230000035699 permeability Effects 0.000 description 1
- NBIIXXVUZAFLBC-UHFFFAOYSA-K phosphate Chemical compound [O-]P([O-])([O-])=O NBIIXXVUZAFLBC-UHFFFAOYSA-K 0.000 description 1
- 239000010452 phosphate Substances 0.000 description 1
- XNGIFLGASWRNHJ-UHFFFAOYSA-N phthalic acid Chemical class OC(=O)C1=CC=CC=C1C(O)=O XNGIFLGASWRNHJ-UHFFFAOYSA-N 0.000 description 1
- 229920005586 poly(adipic acid) Polymers 0.000 description 1
- 239000005014 poly(hydroxyalkanoate) Substances 0.000 description 1
- 229920002401 polyacrylamide Polymers 0.000 description 1
- 229920001610 polycaprolactone Polymers 0.000 description 1
- 229920000728 polyester Polymers 0.000 description 1
- 229920000573 polyethylene Polymers 0.000 description 1
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- 239000002861 polymer material Substances 0.000 description 1
- 229920005862 polyol Polymers 0.000 description 1
- 229920001155 polypropylene Polymers 0.000 description 1
- 239000011148 porous material Substances 0.000 description 1
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- 230000001105 regulatory effect Effects 0.000 description 1
- 239000012744 reinforcing agent Substances 0.000 description 1
- 239000005060 rubber Substances 0.000 description 1
- 229940116351 sebacate Drugs 0.000 description 1
- CXMXRPHRNRROMY-UHFFFAOYSA-L sebacate(2-) Chemical compound [O-]C(=O)CCCCCCCCC([O-])=O CXMXRPHRNRROMY-UHFFFAOYSA-L 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 239000008107 starch Substances 0.000 description 1
- 235000019698 starch Nutrition 0.000 description 1
- 239000007858 starting material Substances 0.000 description 1
- 229940114926 stearate Drugs 0.000 description 1
- 229920003048 styrene butadiene rubber Polymers 0.000 description 1
- 239000006228 supernatant Substances 0.000 description 1
- 239000000725 suspension Substances 0.000 description 1
- 230000008961 swelling Effects 0.000 description 1
- 239000000454 talc Substances 0.000 description 1
- 229910052623 talc Inorganic materials 0.000 description 1
- KKEYFWRCBNTPAC-UHFFFAOYSA-L terephthalate(2-) Chemical compound [O-]C(=O)C1=CC=C(C([O-])=O)C=C1 KKEYFWRCBNTPAC-UHFFFAOYSA-L 0.000 description 1
- 239000002562 thickening agent Substances 0.000 description 1
- 239000012745 toughening agent Substances 0.000 description 1
- 238000012546 transfer Methods 0.000 description 1
- 239000011787 zinc oxide Substances 0.000 description 1
- PAPBSGBWRJIAAV-UHFFFAOYSA-N ε-Caprolactone Chemical group O=C1CCCCCO1 PAPBSGBWRJIAAV-UHFFFAOYSA-N 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
- C09K8/00—Compositions for drilling of boreholes or wells; Compositions for treating boreholes or wells, e.g. for completion or for remedial operations
- C09K8/50—Compositions for plastering borehole walls, i.e. compositions for temporary consolidation of borehole walls
- C09K8/504—Compositions based on water or polar solvents
- C09K8/506—Compositions based on water or polar solvents containing organic compounds
- C09K8/508—Compositions based on water or polar solvents containing organic compounds macromolecular compounds
- C09K8/5086—Compositions based on water or polar solvents containing organic compounds macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds
-
- E—FIXED CONSTRUCTIONS
- E21—EARTH OR ROCK DRILLING; MINING
- E21B—EARTH OR ROCK DRILLING; OBTAINING OIL, GAS, WATER, SOLUBLE OR MELTABLE MATERIALS OR A SLURRY OF MINERALS FROM WELLS
- E21B33/00—Sealing or packing boreholes or wells
- E21B33/10—Sealing or packing boreholes or wells in the borehole
- E21B33/13—Methods or devices for cementing, for plugging holes, crevices or the like
- E21B33/138—Plastering the borehole wall; Injecting into the formation
-
- E—FIXED CONSTRUCTIONS
- E21—EARTH OR ROCK DRILLING; MINING
- E21B—EARTH OR ROCK DRILLING; OBTAINING OIL, GAS, WATER, SOLUBLE OR MELTABLE MATERIALS OR A SLURRY OF MINERALS FROM WELLS
- E21B43/00—Methods or apparatus for obtaining oil, gas, water, soluble or meltable materials or a slurry of minerals from wells
- E21B43/25—Methods for stimulating production
- E21B43/26—Methods for stimulating production by forming crevices or fractures
Landscapes
- Life Sciences & Earth Sciences (AREA)
- Engineering & Computer Science (AREA)
- Geology (AREA)
- General Life Sciences & Earth Sciences (AREA)
- Mining & Mineral Resources (AREA)
- Chemical & Material Sciences (AREA)
- Fluid Mechanics (AREA)
- Environmental & Geological Engineering (AREA)
- Geochemistry & Mineralogy (AREA)
- Physics & Mathematics (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Materials Engineering (AREA)
- Organic Chemistry (AREA)
- Biological Depolymerization Polymers (AREA)
Abstract
The invention discloses a temporary plugging diverting agent and a preparation method and application thereof. The temporary plugging diverter comprises the following raw materials: polyglycolic acid having a first weight average molecular weight and polyglycolic acid having a second weight average molecular weight; wherein the difference between the second weight average molecular weight and the first weight average molecular weight is not less than 10,000 and not more than 290,000; the polyglycolic acid is a homopolymer of glycolic acid and/or a copolymer having glycolic acid as a main repeating unit. The temporary plugging diverting agent can be used for temporary plugging diverting fracturing of oil and gas wells.
Description
Technical Field
The invention belongs to the technical field of oil-gas field fracturing modification, and relates to a foaming type degradable temporary plugging diverter as well as a preparation method and application thereof.
Background
As is well known, oil and gas resources such as oil and gas are produced by exploiting wells (oil wells or gas wells, which may be collectively referred to as "wells") containing porous and permeable underground layers. However, in recent years, as oil and gas fields are continuously produced, the quality of reservoirs is gradually reduced year by year, and for this reason, related oil and gas producers often adopt a reservoir fracturing modification mode to improve the permeability of underground reservoirs so as to continuously and effectively extract oil and gas resources from the underground reservoirs.
In the technical field of reservoir fracturing modification, the temporary blocking steering fracturing technology is that a temporary blocking steering agent is added in real time in fracturing construction, old cracks or added sand cracks are temporarily blocked, and fluid is steered through the change of fracture pressure and fracture extension pressure, so that new cracks are created. The temporary blocking diverting agent and the action principle thereof in the cracks are that after the temporary blocking diverting agent is added in the fracturing construction based on the particle material bridging principle, because the hydraulic fracturing crack has the largest dynamic crack width near a shaft and has smaller and smaller crack width farther away from a well, when the temporary blocking diverting agent and the propping agent simultaneously enter the fracturing crack in a certain proportion, under the combined action of the propping agent and the temporary blocking diverting agent, the particle size of the temporary blocking diverting agent solid particles is larger than 1/3-2/3 of the dynamic width of the crack, the temporary blocking diverting agent solid particles form bridging at the position and block the road where the subsequent temporary blocking diverting agent particles advance, thereby forming accumulation. However, as the subsequent temporary plugging diversion agent is continuously added, more and more temporary plugging diversion agent particles generate bridge plugging and accumulation, a plugging zone with certain thickness and length can be formed in a main channel of the fracture, the continuous extension and development of the fracture are hindered and limited, the fracture is positioned in the fracture volume between the shaft and the plugging zone, the net pressure of the fracture is continuously increased along with the continuous addition of the subsequent sand carrying fluid, when the net pressure in the fracture reaches the opening pressure of the micro-fracture or the fracture pressure of a new fracture, the micro-fracture or the new fracture is opened, and along with the continuous addition of the subsequent sand carrying fluid, the opened micro-fracture or the new fracture can be extended and expanded into a new branch fracture.
In the temporary plugging diversion fracturing technology, a temporary plugging material with excellent performance is the key for realizing effective temporary plugging fracturing. However, in practical application, the conventional oil-soluble temporary plugging diversion agent and the water-soluble temporary plugging diversion agent both need to rely on formation fluid to realize plugging removal, but in some reservoirs, the problem of incomplete plugging removal may exist, and the application of the conventional oil-soluble temporary plugging diversion agent and the water-soluble temporary plugging diversion agent is limited. Different from conventional oil-soluble temporary plugging diversion agents and water-soluble temporary plugging diversion agents, the temporary plugging diversion agent prepared from the self-degradable material can be self-degraded under the conditions of formation temperature and pressure, and is gradually a research hotspot in the technical field of fracturing temporary plugging diversion of oil and gas wells. At present, relevant research works have been carried out at home and abroad aiming at the research of the degradable temporary plugging diversion agent in the fracturing process.
The invention patent application with publication number CN102653673A discloses a biodegradable temporary plugging agent, which contains a biodegradable agent, an organic swelling material and a thickening agent, wherein the biodegradable agent is a granule mixture of soybean and corn, and the granule mixture is prepared by effectively combining a chemical agent and the biodegradable agent to prepare temporary plugging granules with controllable degradation time. Although the temporary plugging agent disclosed in the patent can be completely degraded in a certain time under the stratum condition, the compatibility between the particle mixture of the soybeans and the corns and the organic expansion material is poor, and the particles are difficult to be uniformly mixed, so that the expansion speeds of different point positions are different greatly, and uniform and rapid plugging of blast hole leakage channels is difficult to realize.
The invention patent application with publication number CN105482799A discloses a self-degradation hydraulic temporary plugging diverting agent and a preparation method thereof, wherein the temporary plugging diverting agent is prepared by taking polypropylene carbonate resin as a self-degradation adhesive, adding a plasticizer, a modifier, an accelerator and a density regulator, and extruding and granulating by a screw. The temporary plugging diverter is added with nano calcium carbonate as a plasticizer, so that the strength of a temporary plugging diverter product is improved, nano calcium carbonate particles are small enough to flow out along with return liquid, and no harm and secondary pollution are caused to the stratum, but the plasticizer and the density regulator in the system are both inorganic substances, the compatibility between the plasticizer and the polypropylene carbonate resin is poor, the plasticizer and the density regulator are difficult to uniformly disperse in the polypropylene carbonate resin, and the strength and the density of a final product are influenced.
The invention patent application with publication number CN108531152A discloses a low-density high-strength degradable temporary plugging agent and a preparation method thereof, the temporary plugging agent is prepared by constructing a blending material system by using polylactic acid as a continuous parent phase, starch as a filler, styrene butadiene rubber as a toughening agent and glycerol as a solubilizer and then performing extrusion molding. The temporary plugging agent has certain rigidity, can form bridge plugging in the existing cracks, can be automatically degraded and cannot cause secondary damage to a reservoir stratum, but the temporary plugging agent product can be easily bonded when meeting water at normal temperature and is not beneficial to pump injection.
Under the existing chemical technical conditions, polyglycolic acid is known to have a completely decomposable ester structure with a minimum number of carbon units, and can be prepared by polycondensation of glycolic acid or ring-opening polymerization of glycolide. Unlike conventional polymer materials (e.g., plastics, rubbers, etc.) having stable properties, polyglycolic acid as a material is gradually degraded after a certain period of time and finally becomes water and carbon dioxide harmless to human bodies, animals, plants and natural environments. Therefore, polyglycolic acid, a novel environmentally-friendly and degradable material with good biodegradability and biocompatibility, has been encouraged and supported by national policy, and has been gradually applied to the technical fields of medicine, agriculture, packaging, oil and gas exploitation, and the like.
At present, some researches have been carried out at home and abroad aiming at the technical field that polyglycolic acid materials are used for oil-gas well fracturing temporary plugging diversion.
The invention patent application with the publication number of CN106520094A discloses a soluble temporary plugging agent for acid fracturing, which consists of magnesium alloy granules, magnesium alloy sheets and fibers, wherein the fibers can adopt polyglycolic acid fibers. The temporary plugging agent is mainly applied to acidizing and fracturing operations, and can be completely dissolved in a short time by means of the backflow of residual acid in stratum operations after the acidizing and fracturing operations are completed, so that an oil-gas channel of a reservoir can be quickly recovered.
The invention patent application with publication number CN107245330A discloses a composite temporary plugging agent and a temporary plugging method for horizontal well repeated fracturing, wherein the temporary plugging agent comprises a component a and a component B, the component a is selected from at least one of polyester polymers (such as polyglycolic acid), and the component B is selected from at least one of acrylamide polymers, polymethyl fibers and polyvinyl alcohol. In the composite temporary plugging agent, the component A is a rigid temporary plugging agent component capable of being slowly dissolved or degraded, the rigid propping agent is exerted in the early stage of temporary plugging, the synergistic temporary plugging effect is exerted in the later stage, the component B is a temporary plugging agent component capable of being rapidly expanded, the rapid onset temporary plugging effect can be exerted, and the two components have the synergistic effect to jointly maintain the high-efficiency temporary plugging effect of oil well cracks.
The invention patent application with publication number CN109233773A discloses a nonlinear self-degradation temporary plugging agent for intrastage multi-cluster fracturing modification, which is prepared by using a mixture consisting of polyglycolide, polylactide-glycolide and polyvinyl alcohol as a body, and an initiator, a lubricant, a forming agent, a reinforcing agent and a degradation promoting agent as auxiliary materials through extrusion granulation. The temporary plugging agent does not adhere to water at normal temperature, is beneficial to pump injection, is slowly degraded in limited time, has a nonlinear relation between the dissolution rate and the time at the reservoir temperature, and meets the technical requirements of multi-cluster fracturing construction in a horizontal well section.
The invention patent application with publication number US20160298017a1 discloses a temporary plugging agent for well drilling, which contains a synthetic resin having a temporary plugging function in a temperature range of 93 ℃ (200 ° F) to 204 ℃ (400 ° F) for no more than 40 days; further disclosed is a temporary plugging agent having a temporary plugging function of not less than 2 days and not more than 40 days, wherein the synthetic resin contains a polyglycolic acid-based resin.
The temporary plugging agent which has low density and good dispersibility and is beneficial to pump injection is urgently needed to be provided in the field.
Disclosure of Invention
The invention aims to provide a foaming type degradable temporary plugging diverter which has the characteristics of low density of a foaming material and the characteristics of self degradation and complete dissolution of a degradable material.
The invention also aims to provide a preparation method of the foaming type degradable temporary plugging diversion agent.
The invention also aims to provide application of the foaming type degradable temporary plugging diversion agent.
In a first aspect of the present invention, there is provided a temporary plugging diverter having a cell structure whose raw material components comprise polyglycolic acid; the polyglycolic acid is a homopolymer of glycolic acid and/or a copolymer having glycolic acid as a main repeating unit.
In another embodiment, the temporary blocking diverter is prepared by a foaming process using raw materials comprising polyglycolic acid of different molecular weights.
In another embodiment, the temporary blocking diverter employs polyglycolic acid having a first weight average molecular weight and polyglycolic acid having a second weight average molecular weight, where the second weight average molecular weight is greater than the first weight average molecular weight, and the difference between the second weight average molecular weight and the first weight average molecular weight is not less than 10,000 and not more than 290,000;
the mass ratio of the polyglycolic acid having the second weight average molecular weight to the polyglycolic acid having the first weight average molecular weight is 1:0.05 to 0.95.
In another embodiment, the copolymer comprises one or more units selected from the group consisting of: vinyl oxalate ester units, hydroxycarboxylic acid units, lactone units, carbonate units, and amide units.
In another embodiment, the starting material further comprises 0.1 to 1.2 wt% of a dispersing agent, based on the total weight of polyglycolic acid; preferably, the dispersing agent is polyether nonionic surfactant.
In another embodiment, the temporary blocking diverter has an apparent density of 0.45 to 1.6g/cm3。
In another embodiment, the time to complete degradation of the temporary blocking diverter in water at 90-110 ℃ is not less than 2 hours.
In a second aspect of the present invention, there is provided a method for preparing the temporary plugging diversion agent provided by the present invention as described above, the method comprising the steps of: supercritical CO generation2The polyglycolic acid having the first weight average molecular weight, the polyglycolic acid having the second weight average molecular weight, and the dispersant are mixed to obtain the temporary blocking diverting agent provided by the present invention as described above.
In another embodiment, the method comprises the steps of:
(1) putting polyglycolic acid with a first weight average molecular weight, polyglycolic acid with a second weight average molecular weight and a dispersing agent in a closed high-pressure reaction kettle;
(2) introducing CO into the autoclave2Diffusing into polyglycolic acid after reaching a supercritical state; and
(3) and cooling and depressurizing the high-pressure reaction kettle to normal temperature and normal pressure to obtain the temporary plugging diverting agent.
In a third aspect of the invention, there is provided a use of the temporary plugging diversion agent provided by the invention as described above in temporary plugging diversion fracturing of an oil and gas well.
Therefore, the temporary plugging agent provided by the invention has the advantages of low density, good dispersibility and convenience for pump injection.
Detailed Description
The inventors have made extensive and intensive studies by using two polyglycolic acids having different molecular weights by a foaming process, for example, using supercritical CO2Foaming process, mixing two polyglycolic acids with different molecular weights, and supercritical CO2Under the condition of (3), the molecular chain of the polyglycolic acid is subjected to large-range plastic deformation to change the oriented crystalline structure of the polyglycolic acid, thereby regulating the supercritical CO2The solubility in the polyglycolic acid crystalline phase/amorphous phase is used for preparing polyglycolic acid temporary plugging diverter foaming particles which are uniform in particles, fine in foaming and fine, low in density, good in dispersibility, beneficial to pump injection and applicable to temporary plugging diversion fracturing of oil and gas wells. On the basis of this, the present invention has been completed.
Specifically, the present invention provides (1) an intumescent degradable temporary blocking diverter prepared using expanded polyglycolic acid comprising at least one of a homopolymer of glycolic acid or a copolymer of glycolic acid. As a specific embodiment of the invention relating to the foamed degradable temporary plugging diversion agent provided by the present invention, there is provided a foamed degradable temporary plugging diversion agent described in the following (2) to (9).
(2) The foamable degradable temporary plugging diversion agent according to the above (1), wherein the foamed polyglycolic acid is prepared by a foaming process using at least two polyglycolic acids different in molecular weight.
(3) The foamable degradable temporary plugging diversion agent according to the above (2), wherein polyglycolic acid having a first weight average molecular weight and polyglycolic acid having a second weight average molecular weight are used for foaming.
(4) The foamable degradable temporary plugging diverter according to the item (3), wherein the difference between the second weight average molecular weight and the first weight average molecular weight is not less than 10,000 and not more than 290,000.
(5) The foamable degradable temporary blocking diverter as described in (4), wherein preferably the first weight average molecular weight is 10,000-80,000, more preferably 30,000-50,000, and preferably the second weight average molecular weight is 90,000-300,000, more preferably 130,000-220,000.
(6) The foaming type degradable temporary plugging diversion agent according to any one of the items (2) to (5), wherein the mass ratio of polyglycolic acid having a larger molecular weight to another polyglycolic acid of the two polyglycolic acids is 1:0.05 to 0.95, preferably 1:0.15 to 0.65.
(7) The foaming-type degradable temporary plugging diverting agent as described in (1), wherein the apparent density of the temporary plugging diverting agent is from 0.45 to 1.6g/cm3And the sphericity is 0.4-0.9.
(8) The foaming-type degradable temporary plugging diverter according to the (1), wherein the time for complete degradation of the temporary plugging diverter in clear water with the temperature of 90-110 ℃ is not less than 2 hours.
(9) The foamable degradable temporary blocking diverter according to the item (1), wherein the repeating units of the copolymer of glycolic acid contain at least one of a vinyl oxalate unit, a hydroxycarboxylic acid unit (for example, a lactic acid unit, a 3-hydroxypropionic acid unit, a 3-hydroxybutyric acid unit, a 4-hydroxybutyric acid unit, a 6-hydroxyhexanoic acid unit, etc.), a lactone unit (for example, a β -propiolactone unit, a β -butyrolactone unit, a γ -butyrolactone unit, a caprolactone unit, etc.), a carbonate unit (for example, a trimethylene carbonate unit, etc.), or an amide unit (for example, a caprolactam unit, etc.) in addition to the glycolic acid unit.
In the present invention, the mass content of the glycolic acid repeating unit (i.e., [ -O-CH2-CO- ]) in the "glycolic acid copolymer" or the "copolymer having glycolic acid as a main repeating unit" is 50% or more, preferably 75% or more, more preferably 85% or more, and still more preferably 90% or more.
The invention also provides a preparation method (10) of the foaming type degradable temporary plugging diversion agent, which comprises the following steps:
step i): at normal temperature, placing at least two polyglycolic acids with different molecular weights into a high-pressure reaction kettle, adding a dispersing agent, and then sealing the high-pressure reaction kettle;
step ii): introducing low-pressure CO into the closed high-pressure reaction kettle2So as to completely replace the air in the high-pressure reaction kettle and then introduce high-pressure CO2Until the pressure of the high-pressure reaction kettle is increased to the set valueSetting the value, starting stirring, and then gradually heating the high-pressure reaction kettle by adopting a heat source until the CO in the high-pressure reaction kettle2Fully mixing polyglycolic acid with different molecular weights under the action of a dispersant to obtain homogeneous and uniform particles, and maintaining the pressure for a period of time to ensure that supercritical CO is obtained2(ii) diffusional dissolution into the polyglycolic acid particles;
step iii): and removing the heat source, quickly reducing the temperature of the high-pressure reaction kettle to room temperature, and then relieving the pressure to normal pressure to prepare the foamed polyglycolic acid (namely the foamed degradable temporary plugging diversion agent).
As a specific embodiment of the invention relating to the method for producing a foamed degradable temporary plugging diversion agent according to the present invention, there is provided a method for producing a foamed degradable temporary plugging diversion agent described in the following (11) to (17).
(11) In the process for producing the foaming type temporary plugging diversion agent according to the above (10), the dispersant used in the step i) is a polyether nonionic surfactant which is a condensate of an alkylphenol and ethylene oxide and is further selected from commercially available OP series dispersants, for example, but not limited thereto, commercially available OP-9, OP-10, OP-11 and the like.
(12) In the method for preparing the foaming type degradable temporary plugging diversion agent according to the item (10), the amount of the dispersant used in the step i) is 0.1 to 1.2%, preferably 0.8 to 1% of the total weight of the polyglycolic acid.
(13) In the process for preparing the foaming type degradable temporary plugging diversion agent according to the item (10), in the step ii), after the air in the high-pressure reaction kettle is completely replaced, high-pressure CO is introduced2Until the pressure of the autoclave is raised to about 10MPa, and then the autoclave is gradually heated to about 150 ℃ and 250 ℃ by using a heat source and maintained at the pressure of about 10-50MPa for about 10-240 minutes.
(14) The method for preparing the foaming type degradable temporary plugging diversion agent according to the above (13), further preferably, in the step ii), after the air in the high-pressure reaction kettle is completely replaced, introducing high-pressure CO2Until the pressure of the autoclave is raised to about 10MPa, and then the autoclave is gradually heated to about 10MPa by a heat source180 ℃ and 220 ℃ and is maintained at a pressure of about 20-30MPa for about 40-120 minutes.
(15) In the process for preparing a foaming type degradable temporary plugging diversion agent as described in (10), in the step iii), the temperature reduction rate of the high-pressure reaction kettle is about 5 to 15 ℃/min.
(16) In the process for preparing an intumescent degradable temporary plugging diversion agent as described in (10), in the step iii), the pressure relief rate of the high-pressure reaction kettle is about 2 to 30 MPa/min.
(17) The process for producing an intumescent degradable temporary plugging diversion agent as described in (16), further preferably, in the step iii), the pressure-releasing rate of the high-pressure reactor is about 10 to 20 MPa/min.
The heat source used in the above preparation method is a heating/heat supplying heat source conventional in the art, including but not limited to an electric heating device, a hydrothermal device, a heat transfer oil circulation heating device, etc., which are conventional in the art, and preferably an electric heating device.
The invention also provides application of the foaming type degradable temporary plugging diverter.
As an embodiment (18) of the invention related to the application of the foaming type degradable temporary plugging diversion agent provided by the invention, the foaming type degradable temporary plugging diversion agent is directly applied to temporary plugging diversion fracturing of an oil-gas well.
In another embodiment (19) of the invention related to the application of the foamed degradable temporary plugging diversion agent provided by the invention, the foamed degradable temporary plugging diversion agent is compounded with other auxiliary agents and/or other degradable polymers except foamed polyglycolic acid and then used for temporary plugging diversion fracturing of oil and gas wells.
According to the invention, after the temporary plugging diversion agent is compounded with other auxiliary agents and/or other degradable polymers except for foamed polyglycolic acid, the plugging pressure-bearing strength is more than 5MPa under the condition that the width of a steel rock crack is 1-3 mm.
As a specific mode of the application of the foamed degradable temporary plugging diversion agent provided by the present invention in another embodiment (19), the other auxiliary agents include, but are not limited to, any one or more of plasticizers, fillers or compatibilizers.
As a specific mode of another embodiment (19) of the application of the foaming type degradable temporary plugging diversion agent provided by the invention, the foamed polyglycolic acid has a mass content of 50-99.9% by mass and the balance of other auxiliary agents, wherein the mass percentage is 100% by mass.
As a specific mode of another embodiment (19) of the application of the foamed degradable temporary plugging diversion agent provided by the present invention, the other degradable polymer is, for example, a degradable polymer having a biodegradable property or a hydrolytic property, wherein the biodegradable property means that the degradable polymer can be decomposed by using microorganisms under a well, and the hydrolytic property means that the degradable polymer can be decomposed by using a liquid under a well, particularly by using water, more preferably a water body containing an acid or a base. In addition, the resin originally has a reduced strength and is therefore brittle due to a low degree of polymerization or the like, and as a result, it can be easily disintegrated to lose its original shape by applying a very small mechanical force, and such a resin also conforms to a degradable polymer.
As yet another specific mode of the present invention providing another embodiment (19) of the use of the foamed degradable temporary plugging diversion agent, the other degradable polymers include, but are not limited to, any one or more of polylactic acid, poly (-caprolactone), polylactic-co-polyglycolic acid (PLGA), poly adipic acid/butylene terephthalate (PBAT), polybutylene succinate (PBS), polypropylene carbonate (PPC), polyethylene adipate (PEA), Polyhydroxyalkanoate (PHA), polyethylene terephthalate (PET), polybutylene terephthalate (PBT), polypropylene terephthalate (PTT), or polyethylene naphthalate (PEN).
As still another specific mode of the application of the foamed degradable temporary plugging diversion agent provided by the invention, the foamed polyglycolic acid accounts for 50-90% by mass, other degradable polymers account for 8-49% by mass and other auxiliary agents account for 100% by mass of the total mass fraction.
As used herein, "ambient temperature" or "room temperature" means 15 to 40 deg.C, preferably 20 to 30 deg.C.
As used herein, "atmospheric pressure" means open to the atmosphere and not bearing pressure; for example, at 25 ℃, atmospheric pressure is one atmosphere.
It should be noted that in the development of any such actual implementation, numerous implementation-specific decisions must be made to achieve the developers' specific goals, such as compliance with system-related and business-related constraints, which will vary from one implementation to another. Moreover, it will be appreciated that such a development effort might be complex and time-consuming, but would nevertheless be a routine undertaking for those of ordinary skill in the art having the benefit of this disclosure.
In the context of the present invention and this detailed description, the term "about" when used to modify a numerical value means a margin of error measured within ± 5% of the numerical value.
The polyglycolic acid used in the present invention is a polyglycolic acid having a structure represented by the formula (1) - (-O-CH)2The proportion of the repeating unit represented by the formula 1 in the polymer is usually about 50 wt% or more, preferably about 80 wt% or more, more preferably about 85 wt% or more, further preferably about 90 wt% or more, particularly preferably about 95 wt% or more, most preferably about 99 wt% or more, if the proportion of the repeating unit represented by the formula 1 is less than about 50 wt%, toughness, crystallinity, heat resistance, hardness and the like tend to decrease, and in many cases, it is most preferable to use a homopolymer of polyglycolic acid having a proportion of the repeating unit represented by the formula 1 of 100 wt%, and for a copolymer of glycolic acid, in addition to the repeating unit represented by the formula 1, other repeating units such as an ethylene oxalate unit, a hydroxybutyric acid unit (e.g., a lactic acid unit, a 3-hydroxypropionic acid unit, a 3-hydroxybutyric acid unit, a 4-hydroxybutyric acid unit, a 6-hydroxyhexanoic acid unit and the like), a lactone unit (e.g., a β -propiolactone unit, a β -butyrolactone unit, a gamma-caprolactone unit, a caprolactam unit and the like, and the copolymer of glycolic acid is not limited to a caprolactam unit, but not limited to the caprolactam unit.
In the present invention, polyglycolic acid can be produced by polycondensation of glycolic acid or ring-opening polymerization of glycolide.
In this regard, in general, the homopolymer of glycolic acid in the present invention may be referred to as a homopolymer of glycolide, and the copolymer of glycolic acid may be referred to as a copolymer of glycolide. The scope of protection of the claims of the present invention therefore covers the case of homopolymers of glycolide, copolymers of glycolide.
The features mentioned above with reference to the invention, or the features mentioned with reference to the embodiments, can be combined arbitrarily. All features disclosed in this specification may be combined in any combination, provided that there is no conflict between such features and the combination, and all possible combinations are to be considered within the scope of the present specification. Each feature disclosed in this specification may be replaced by an alternative feature serving the same, equivalent, or similar purpose. Thus, unless expressly stated otherwise, the features disclosed are merely generic examples of equivalent or similar features.
The main advantages of the invention are:
1. the invention is characterized in that polyglycolic acid with different molecular weights is subjected to supercritical CO2The molecular chain is subjected to large-scale plastic deformation by medium mixing, the free volume of the molecular chain is increased, the entanglement of the molecular chain is reduced, the oriented crystalline structure of the polyglycolic acid is changed, and the supercritical CO can be adjusted2Solubility in the crystalline phase/amorphous phase of polyglycolic acid, forming polyglycolic acid foam material with different cell sizes (pore diameters of about 10-1000 μm), uniform particles and fine foaming.
2. The foaming type degradable temporary plugging diverter provided by the invention not only has the low-density characteristic of a foaming material (the apparent density of the temporary plugging diverter is 0.45-1.6 g/cm)3Preferably 0.68 to 1.2g/cm3) And the characteristics of autonomous degradation and complete dissolution of the degradable material (the complete degradation time is not less than 2 hours in clear water at the temperature of 90-110 ℃), does not adhere when meeting water at normal temperature, is beneficial to pump injection, can be completely degraded, has no harm to a reservoir stratum, has simple preparation process steps, and is beneficial to realizing industrial production.
3. In practical application, the foaming type degradable temporary plugging diversion agent provided by the invention can be compounded with other auxiliary agents and/or other degradable polymers except foamed polyglycolic acid, and has excellent plugging bearing strength (for example, under the condition that the width of a steel rock fracture is 1-3mm, the plugging bearing strength is more than 5MPa, and particularly the plugging bearing strength can be as high as 26.1MPa), so that fracturing operation can be performed practically, old fractures or fractures with sand are plugged temporarily, and fluid is diverted through the change of fracture extension pressure, so that new fractures are created, and the yield and energy increase of an oil and gas well are realized.
In one aspect of the present invention, the foamed type degradable temporary plugging diverter of examples 1-10 is prepared by using foamed polyglycolic acid, and the specific preparation process comprises the following steps:
i. at normal temperature, putting A type polyglycolic acid and B type polyglycolic acid into a high-pressure reaction kettle, wherein the A type polyglycolic acid is polyglycolic acid with the weight-average molecular weight M, the B type polyglycolic acid is polyglycolic acid with the weight-average molecular weight N, the mass ratio of the A type polyglycolic acid to the B type polyglycolic acid is O, adding a commercially available dispersing agent OP-11 accounting for 1 percent of the total weight of the A type polyglycolic acid and the B type polyglycolic acid, and then sealing the high-pressure reaction kettle;
ii, introducing low pressure CO2(CO2Pressure intensity<4MPa) completely replacing air in the high-pressure reaction kettle, and then introducing high-pressure CO2(CO2Pressure intensity>10MPa) and the pressure in the high-pressure reaction kettle reaches 10MPa, simultaneously, the stirring paddle is started, and then the high-pressure reaction kettle is gradually heated to P until CO in the high-pressure reaction kettle2Reaching supercritical state, and maintaining at pressure of Q for a certain time R to obtain supercritical CO2Diffusing and dissolving into two kinds of polyglycolic acid;
and iii, removing a heat source of the high-pressure reaction kettle, quickly cooling to room temperature, and then releasing the pressure to normal pressure at the pressure relief speed of S.
The foaming type degradable temporary plugging diverter prepared in the examples 1-10 is tested for apparent density and sphericity by SY/T5108-2006 fracturing propping agent performance index and test recommendation method, which is specifically shown in Table 1.
Table 1 examples 1-10 preparation of foamed degradable temporary plugging diversion agent process parameters and apparent density and sphericity
Note: in Table 1, M represents the weight average molecular weight of type A polyglycolic acid; n is the weight average molecular weight of the B-type polyglycolic acid; o is the mass ratio of the A-type polyglycolic acid to the B-type polyglycolic acid; p is the temperature of the high-pressure reaction kettle; q is the pressure of the high-pressure reaction kettle; r is the pressure maintaining time; and S is the pressure relief speed.
Both polyglycolic acid type a and polyglycolic acid type B in each example in table 1 are homopolymers of glycolic acid.
The degradation performance of the foaming type degradable temporary plugging diversion agent prepared by the invention is tested, the test result is shown in table 2, and the specific test method is as follows:
I) putting the prepared temporary plugging agent into a constant-temperature drying box, and drying for 48 hours at the temperature of 60 ℃;
II) weighing 5.00g of dried temporary plugging agent, placing the temporary plugging agent in 100mL of clear water, and placing the clear water in a thermostat with set temperature;
III) taking out the degraded sample on time, and extracting supernatant to separate residual solid phase;
IV) cleaning the separated residual solid phase with distilled water, putting the cleaned residual solid phase into a constant-temperature drying oven, drying the solid phase for 24 hours at the temperature of 60 ℃, weighing the dried solid phase, and recording the weight of the residual solid phase as w;
v) calculating the degradation rate R of the temporary plugging agent in clear waterAThe calculation formula is as follows:
TABLE 2 degradation test results for foaming type degradable temporary plugging diverter
From the test results in table 2, it can be seen that under the same temperature conditions, the temporary blocking diverting agent with higher apparent density is degraded at a lower rate than the temporary blocking diverting agent with lower apparent density. The time for complete degradation of the temporary plugging diversion agent prepared by the invention in clear water at 90-110 ℃ is not less than 2 hours, for example, the time for complete degradation of the temporary plugging diversion agent prepared in the embodiment 1 in clear water at 110 ℃ is 16 hours; the time for complete degradation of the temporary plugging diversion agent prepared in the example 9 in clear water at 90 ℃ is 5 hours; the time for complete degradation of the temporary plugging diversion agent prepared in the example 10 in clear water at 100 ℃ is 10 hours.
Based on the test results in table 2, the degradation time of the foaming type degradable temporary plugging diverter of the invention can be adjusted by adjusting the weight average molecular weight of two polyglycolic acids and the preparation process. For example, in the case where the temperature P of the autoclave, the pressure Q of the autoclave, and the pressure relief rate S are determined, the degradation time of the foamable degradable temporary plugging diversion agent can be adjusted by changing the weight average molecular weights of the a-type polyglycolic acid and the B-type polyglycolic acid, the mass ratio of the a-type polyglycolic acid and the B-type polyglycolic acid, and the pressure holding time R of the autoclave, and it can be seen from table 2 that the degradable temporary plugging diversion agent of example 1 and example 8 has a degradation foaming ratio of 43% and 32% for 24 hours, a degradation ratio of 85% and 58% for 96 hours, and a degradation ratio of 95% and 74% for 168 hours, respectively, in clear water at 90 ℃.
It should be noted that the above degradation test is only an demonstration of the degradation performance of the foamed degradable temporary plugging diverter of the present invention, and the two polyglycolic acids with different molecular weights used in the preparation method of the present invention are essentially mixtures composed of many compounds with the same chain structure and different polymerization degrees, and the mixed system of the two polyglycolic acids can be regarded as "chaotic body", and its own properties may not exactly correspond to the process parameters in the preparation method, so the actual degradation condition of some foamed degradable temporary plugging diverter (i.e. foamed polyglycolic acid) prepared according to the method of the present invention is not limited to the data in table 2.
The following table 3 shows the preparation process parameters, apparent density and sphericity of the foamed degradable temporary plugging diversion agent of examples 11-17.
TABLE 3 EXAMPLES 11-17 preparation of foamable biodegradable temporary plugging diverter with Process parameters and apparent Density and sphericity
Note: in Table 3, M is the weight average molecular weight of type A polyglycolic acid; n is the weight average molecular weight of the B-type polyglycolic acid; o is the mass ratio of the A-type polyglycolic acid to the B-type polyglycolic acid; p is the temperature of the high-pressure reaction kettle; q is the pressure of the high-pressure reaction kettle; r is the pressure maintaining time; and S is the pressure relief speed.
In Table 3, the type A polyglycolic acid in example 11 is a copolymer of glycolic acid and lactic acid (i.e., a polyglycolic-lactic acid copolymer, PLGA for short), the proportion of glycolic acid repeating units is about 85% by weight, and the type B polyglycolic acid is a homopolymer of glycolic acid; in example 12, both of the polyglycolic acid type A and the polyglycolic acid type B were polyglycolic acid-lactic acid copolymers, and the proportion of glycolic acid repeating units was about 72% by weight; the polyglycolic acid type A in example 13 is a copolymer of glycolic acid and-caprolactone with a proportion of glycolic acid repeating units of about 53 wt%, while the polyglycolic acid type B is a copolymer of glycolic acid and trimethylene carbonate with a proportion of glycolic acid repeating units of about 90 wt%; the polyglycolic acid type A in example 14 is a homopolymer of glycolic acid, while the polyglycolic acid type B is a copolymer of glycolic acid and caprolactam, the proportion of glycolic acid repeat units being about 92 wt%; the polyglycolic acid type A in example 15 is a copolymer of glycolic acid and vinyl oxalate, the proportion of glycolic acid repeating units being about 88 wt%, while the polyglycolic acid type B is a copolymer of glycolic acid and 3-hydroxybutyric acid, the proportion of glycolic acid repeating units being about 82 wt%; both the type a and type B polyglycolic acids in examples 16 and 17 are homopolymers of glycolic acid.
As another aspect of the present invention, the foaming type temporary plugging diversion agent prepared in example 1 is compounded with other additives and/or other degradable polymers except for foamed polyglycolic acid (the existing blending extrusion granulation process can be used to prepare the compounded temporary plugging diversion agent, but the process of blending extrusion granulation is not limited by special technology and is not described herein), and the dosage relationship among the components can be found in examples 18 to 24 in table 4.
TABLE 4 relationship of the mass ratios of the foaming type degradable temporary plugging diverter and other components in examples 18-24
The filler used can improve the mechanical strength and heat resistance of the temporary blocking diverter. As the filler, a granular or powdery filler can be used. As particulate or powdered fillers, there may be included, but not limited to, any one or more of mica, talc, calcium carbonate, zinc oxide, kaolin, quartz powder, and the like. Preferably, the granular or powdery filler is selected from quartz powder.
The compatibilizer used is effective to reduce surface tension and improve interfacial adhesion between the dispersed and continuous phases in the blend. As the compatibilizer, a grafted maleic anhydride compatibilizer may be used, for example, including, but not limited to, any one of polyethylene grafted maleic anhydride (PE-g-MAH), polypropylene grafted maleic anhydride (PP-g-MAH), ethylene-vinyl acetate copolymer grafted maleic anhydride (EVA-g-MAH). Preferably, the compatibilizer is selected from ethylene-vinyl acetate copolymer grafted maleic anhydride (EVA-g-MAH).
The plasticizer used can weaken the acting force between macromolecules of the polymer, so that the mobility of polymer molecules is increased, and the processability of the polymer can be effectively improved. As the plasticizer, commercially available plasticizers of phthalate esters, aliphatic dibasic acid esters, citric acid esters or polyol esters, including, but not limited to, butyl phthalate, dioctyl phthalate, adipate, azelate, sebacate, stearate, phosphate, etc., may be used. Preferably, the plasticizer is selected from butyl phthalate or dioctyl phthalate.
The weight average molecular weights of the polylactic acid (PLA), the polybutylene adipate/terephthalate (PBAT) and the polyethylene terephthalate (PET) used are preferably 60,000-300,000, more preferably 100,000-300,000, 120,000-280,000 and particularly preferably 150,000-250,000.
In the aspect of plugging performance testing, the specific implementation mode is mainly divided into the following two aspects:
firstly, the foaming type degradable temporary plugging diverter prepared in the embodiment 2, the embodiment 4, the embodiment 7 and the embodiment 14 is directly subjected to a plugging performance test, and the specific test method is as follows:
A) directly mixing the foaming type degradable temporary plugging diverter with a proper amount of clear water, and stirring for 30 minutes at 1000 revolutions per minute by using a stirrer to prepare temporary plugging slurry;
B) putting the wedge-shaped crack steel rock into a holder, wherein the wide surface of the steel rock crack is the inlet end of the temporary plugging diverting agent, applying confining pressure of 30MPa, and closing an outlet valve;
C) pouring the temporary plugging slurry into a clamp holder kettle body, and connecting an inlet pipeline and a pressure sensor;
D) opening pressure monitoring software, starting the displacement pump in a constant flow mode, and opening an outlet valve;
E) starting a displacement pump to gradually increase the pumping pressure from 0MPa to 1.0-2.0MPa each time, and stabilizing the pressure of each pressure point for 5-10 minutes;
F) and when the inlet pressure cannot be stabilized to a certain pressure point, taking the pressure stabilizing point closest to the pressure point as the pressure bearing capacity of the temporary plugging agent.
Secondly, the temporary plugging diversion agent prepared in the embodiment 20 and the embodiment 24 is subjected to a plugging performance test, and the specific test method is as follows:
A) directly mixing the temporary plugging diverter prepared by compounding with a proper amount of clear water, and stirring for 30 minutes at 1000 revolutions per minute by using a stirrer to prepare temporary plugging slurry;
B) putting the wedge-shaped crack steel rock into a holder, wherein the wide surface of the steel rock crack is the inlet end of the temporary plugging diverting agent, applying confining pressure of 30MPa, and closing an outlet valve;
C) pouring the temporary plugging slurry into a clamp holder kettle body, and connecting an inlet pipeline and a pressure sensor;
D) opening pressure monitoring software, starting the displacement pump in a constant flow mode, and opening an outlet valve;
E) starting a displacement pump to gradually increase the pumping pressure from 0MPa to 1.0-2.0MPa each time, and stabilizing the pressure of each pressure point for 5-10 minutes;
F) and when the inlet pressure cannot be stabilized to a certain pressure point, taking the pressure stabilizing point closest to the pressure point as the pressure bearing capacity of the temporary plugging agent.
The results of the plugging performance test of the above corresponding examples are shown in table 5.
Table 5 plugging test results
| Item | Crack width (mm) | Plugging pressure (MPa) |
| Example 2 | 1-3 | 5.6 |
| Example 4 | 1-3 | 22.4 |
| Example 4 | 3-5 | 15.8 |
| Example 7 | 3-5 | 8.3 |
| Example 14 | 1-3 | 20.3 |
| Example 20 | 1-3 | 22.5 |
| Example 24 | 1-3 | 26.1 |
In conclusion, the foaming type degradable temporary plugging diverter disclosed by the invention has the low density characteristic (namely, lower apparent density) of a foaming material, has higher sphericity and good suspension property, and is favorable for smoothly reaching the specified position of an underground reservoir and realizing effective plugging; in addition, the foaming type degradable temporary plugging diversion agent disclosed by the invention has a cellular structure, so that the strength of the foaming type degradable temporary plugging diversion agent is reduced to a certain extent, but the temporary plugging diversion agent still has good plugging performance (for example, when the foaming type degradable temporary plugging diversion agent is not compounded with other components, the plugging pressure is more than 5MPa under the condition that the crack width is 1-3mm, and even can be as high as 22.4 MPa). In practical application, the foaming type degradable temporary plugging diversion agent can be compounded with other auxiliary agents and/or other degradable polymers except for the foaming polyglycolic acid according to actual working conditions. For example, in order to suitably increase the strength, the foaming type degradable temporary plugging diversion agent of the invention can be compounded with a filler and/or a degradable polymer (such as PET) with larger hardness, due to the existence of a cellular structure, the filler can be provided with enough accommodation space, which is favorable for the filler to be sufficiently dispersed in the foaming type degradable temporary plugging diversion agent so as to suitably increase the strength of the foaming type degradable temporary plugging diversion agent, while the PET has relatively higher strength, the compounding of the PET with the foaming type degradable temporary plugging diversion agent is favorable for improving the strength of the composition system, and other non-degradable polymers with larger hardness can be suitably added, but it is required to be noted that the higher strength of the composition system is not better, if the strength is too high, the cost is increased on the one hand, and on the other hand, due to non-degradable components (such as the filler, Other non-degradable polymers) that remain after the temporary plug diversion fracturing has been performed, can adversely affect the reservoir downhole. Therefore, the amount of the filler and/or the degradable polymer with higher hardness in the composition system can be properly adjusted to obtain the expected strength according to the actual working conditions.
The foregoing is merely a preferred embodiment of the invention and is not intended to limit the scope of the invention, which is defined by the claims appended hereto, and any other technical entity or method that is encompassed by the claims as broadly defined herein, or equivalent variations thereof, is contemplated as being encompassed by the claims.
Claims (10)
1. A temporary blocking diverting agent is characterized in that the temporary blocking diverting agent has a cellular structure, and the raw material components of the temporary blocking diverting agent comprise polyglycolic acid; the polyglycolic acid is a homopolymer of glycolic acid and/or a copolymer having glycolic acid as a main repeating unit.
2. The temporary plugging diverting agent according to claim 1, wherein the temporary plugging diverting agent is prepared by a foaming process using raw materials containing polyglycolic acid with different molecular weights.
3. The temporary blocking diverter according to claim 1 or 2, wherein polyglycolic acid having a first weight average molecular weight and polyglycolic acid having a second weight average molecular weight are used, wherein the second weight average molecular weight is larger than the first weight average molecular weight, and the difference between the second weight average molecular weight and the first weight average molecular weight is not less than 10,000 and not more than 290,000;
the mass ratio of the polyglycolic acid having the second weight average molecular weight to the polyglycolic acid having the first weight average molecular weight is 1:0.05 to 0.95.
4. A diverting agent according to claim 1, wherein the copolymer comprises one or more units selected from: vinyl oxalate ester units, hydroxycarboxylic acid units, lactone units, carbonate units, and amide units.
5. The temporary plugging diversion agent according to claim 1, wherein said raw materials further comprise 0.1-1.2 wt% of a dispersing agent, based on the total weight of polyglycolic acid; preferably, the dispersing agent is polyether nonionic surfactant.
6. The temporary plugging diverter of claim 1, wherein the temporary plugging diverter has an apparent density of from 0.45 to 1.6g/cm3。
7. A temporary plugging diverter according to claim 1 wherein said temporary plugging diverter completely degrades in water at 90-110 ℃ for no less than 2 hours.
8. A process for preparing a diverting agent for temporary plugging according to any of claims 1 to 7, characterized in that it comprises the steps of: supercritical CO generation2Into a particle obtained by mixing polyglycolic acid having a first weight average molecular weight, polyglycolic acid having a second weight average molecular weight, and a dispersant to obtain the temporary closure diverter as set forth in any one of claims 1 to 7.
9. The method of claim 8, wherein the method comprises the steps of:
(1) putting polyglycolic acid with a first weight average molecular weight, polyglycolic acid with a second weight average molecular weight and a dispersing agent in a closed high-pressure reaction kettle;
(2) introducing CO into the autoclave2Diffusing into polyglycolic acid after reaching a supercritical state;
(3) and cooling and depressurizing the high-pressure reaction kettle to normal temperature and normal pressure to obtain the temporary plugging diverting agent.
10. Use of a diverting agent according to any of claims 1-7 in diverting fracturing of a diverting of an oil or gas well.
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