CN109233773A - The non-linear self-degradation diverting agent of more cluster fracturing reforms and preparation method in a kind of section - Google Patents
The non-linear self-degradation diverting agent of more cluster fracturing reforms and preparation method in a kind of section Download PDFInfo
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- CN109233773A CN109233773A CN201811310508.6A CN201811310508A CN109233773A CN 109233773 A CN109233773 A CN 109233773A CN 201811310508 A CN201811310508 A CN 201811310508A CN 109233773 A CN109233773 A CN 109233773A
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- 230000007281 self degradation Effects 0.000 title claims abstract description 51
- 238000002360 preparation method Methods 0.000 title claims abstract description 16
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 117
- 239000000203 mixture Substances 0.000 claims abstract description 33
- 230000015556 catabolic process Effects 0.000 claims abstract description 27
- 238000006731 degradation reaction Methods 0.000 claims abstract description 27
- 239000012744 reinforcing agent Substances 0.000 claims abstract description 20
- 239000003999 initiator Substances 0.000 claims abstract description 19
- AEMRFAOFKBGASW-UHFFFAOYSA-N Glycolic acid Polymers OCC(O)=O AEMRFAOFKBGASW-UHFFFAOYSA-N 0.000 claims abstract description 18
- 229920000954 Polyglycolide Polymers 0.000 claims abstract description 18
- 239000000314 lubricant Substances 0.000 claims abstract description 18
- 239000004372 Polyvinyl alcohol Substances 0.000 claims abstract description 17
- 229920002451 polyvinyl alcohol Polymers 0.000 claims abstract description 17
- 239000000463 material Substances 0.000 claims abstract description 16
- 239000000126 substance Substances 0.000 claims abstract description 10
- 238000006243 chemical reaction Methods 0.000 claims description 17
- PNEYBMLMFCGWSK-UHFFFAOYSA-N Alumina Chemical compound [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims description 15
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 claims description 12
- 229920000858 Cyclodextrin Polymers 0.000 claims description 9
- 239000001116 FEMA 4028 Substances 0.000 claims description 9
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 9
- 229920002472 Starch Polymers 0.000 claims description 9
- WHGYBXFWUBPSRW-FOUAGVGXSA-N beta-cyclodextrin Chemical compound OC[C@H]([C@H]([C@@H]([C@H]1O)O)O[C@H]2O[C@@H]([C@@H](O[C@H]3O[C@H](CO)[C@H]([C@@H]([C@H]3O)O)O[C@H]3O[C@H](CO)[C@H]([C@@H]([C@H]3O)O)O[C@H]3O[C@H](CO)[C@H]([C@@H]([C@H]3O)O)O[C@H]3O[C@H](CO)[C@H]([C@@H]([C@H]3O)O)O3)[C@H](O)[C@H]2O)CO)O[C@@H]1O[C@H]1[C@H](O)[C@@H](O)[C@@H]3O[C@@H]1CO WHGYBXFWUBPSRW-FOUAGVGXSA-N 0.000 claims description 9
- 235000011175 beta-cyclodextrine Nutrition 0.000 claims description 9
- 229960004853 betadex Drugs 0.000 claims description 9
- 235000019698 starch Nutrition 0.000 claims description 9
- 239000008107 starch Substances 0.000 claims description 9
- DOIRQSBPFJWKBE-UHFFFAOYSA-N dibutyl phthalate Chemical compound CCCCOC(=O)C1=CC=CC=C1C(=O)OCCCC DOIRQSBPFJWKBE-UHFFFAOYSA-N 0.000 claims description 8
- 125000002496 methyl group Chemical group [H]C([H])([H])* 0.000 claims description 8
- BWHMMNNQKKPAPP-UHFFFAOYSA-L potassium carbonate Chemical compound [K+].[K+].[O-]C([O-])=O BWHMMNNQKKPAPP-UHFFFAOYSA-L 0.000 claims description 8
- TVWTZAGVNBPXHU-FOCLMDBBSA-N dioctyl (e)-but-2-enedioate Chemical compound CCCCCCCCOC(=O)\C=C\C(=O)OCCCCCCCC TVWTZAGVNBPXHU-FOCLMDBBSA-N 0.000 claims description 7
- 238000010438 heat treatment Methods 0.000 claims description 7
- LRHPLDYGYMQRHN-UHFFFAOYSA-N N-Butanol Chemical compound CCCCO LRHPLDYGYMQRHN-UHFFFAOYSA-N 0.000 claims description 6
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 claims description 6
- 238000001816 cooling Methods 0.000 claims description 4
- 229910000027 potassium carbonate Inorganic materials 0.000 claims description 4
- 238000007873 sieving Methods 0.000 claims description 4
- 239000000377 silicon dioxide Substances 0.000 claims description 4
- 238000010792 warming Methods 0.000 claims description 4
- 229910000029 sodium carbonate Inorganic materials 0.000 claims description 3
- UIIMBOGNXHQVGW-DEQYMQKBSA-M Sodium bicarbonate-14C Chemical compound [Na+].O[14C]([O-])=O UIIMBOGNXHQVGW-DEQYMQKBSA-M 0.000 claims description 2
- JBSLOWBPDRZSMB-FPLPWBNLSA-N dibutyl (z)-but-2-enedioate Chemical compound CCCCOC(=O)\C=C/C(=O)OCCCC JBSLOWBPDRZSMB-FPLPWBNLSA-N 0.000 claims description 2
- 230000001681 protective effect Effects 0.000 claims description 2
- 150000002085 enols Chemical class 0.000 claims 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 abstract description 14
- 229910001868 water Inorganic materials 0.000 abstract description 14
- 238000004090 dissolution Methods 0.000 abstract description 12
- 238000010276 construction Methods 0.000 abstract description 8
- 238000003825 pressing Methods 0.000 abstract description 7
- 238000004519 manufacturing process Methods 0.000 abstract description 2
- UIIMBOGNXHQVGW-UHFFFAOYSA-M Sodium bicarbonate Chemical compound [Na+].OC([O-])=O UIIMBOGNXHQVGW-UHFFFAOYSA-M 0.000 description 7
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 6
- 239000003921 oil Substances 0.000 description 6
- 239000000853 adhesive Substances 0.000 description 5
- 230000001070 adhesive effect Effects 0.000 description 5
- ROOXNKNUYICQNP-UHFFFAOYSA-N ammonium persulfate Chemical compound [NH4+].[NH4+].[O-]S(=O)(=O)OOS([O-])(=O)=O ROOXNKNUYICQNP-UHFFFAOYSA-N 0.000 description 4
- 230000000694 effects Effects 0.000 description 4
- 239000003431 cross linking reagent Substances 0.000 description 3
- 238000011161 development Methods 0.000 description 3
- JJTUDXZGHPGLLC-UHFFFAOYSA-N lactide Chemical compound CC1OC(=O)C(C)OC1=O JJTUDXZGHPGLLC-UHFFFAOYSA-N 0.000 description 3
- 238000000034 method Methods 0.000 description 3
- 238000002407 reforming Methods 0.000 description 3
- 238000007789 sealing Methods 0.000 description 3
- 229910000030 sodium bicarbonate Inorganic materials 0.000 description 3
- 235000017557 sodium bicarbonate Nutrition 0.000 description 3
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 2
- 229910001870 ammonium persulfate Inorganic materials 0.000 description 2
- 239000002981 blocking agent Substances 0.000 description 2
- 238000000354 decomposition reaction Methods 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 239000012530 fluid Substances 0.000 description 2
- 238000005461 lubrication Methods 0.000 description 2
- 239000002609 medium Substances 0.000 description 2
- 238000011056 performance test Methods 0.000 description 2
- 230000035699 permeability Effects 0.000 description 2
- -1 potassium ferricyanide Chemical compound 0.000 description 2
- 239000000243 solution Substances 0.000 description 2
- 238000003756 stirring Methods 0.000 description 2
- 238000012360 testing method Methods 0.000 description 2
- RKDVKSZUMVYZHH-UHFFFAOYSA-N 1,4-dioxane-2,5-dione Chemical compound O=C1COC(=O)CO1 RKDVKSZUMVYZHH-UHFFFAOYSA-N 0.000 description 1
- HRPVXLWXLXDGHG-UHFFFAOYSA-N Acrylamide Chemical compound NC(=O)C=C HRPVXLWXLXDGHG-UHFFFAOYSA-N 0.000 description 1
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 1
- ZLMJMSJWJFRBEC-UHFFFAOYSA-N Potassium Chemical compound [K] ZLMJMSJWJFRBEC-UHFFFAOYSA-N 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 150000001408 amides Chemical class 0.000 description 1
- 239000012736 aqueous medium Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000000903 blocking effect Effects 0.000 description 1
- 230000006835 compression Effects 0.000 description 1
- 238000007906 compression Methods 0.000 description 1
- 238000000280 densification Methods 0.000 description 1
- 238000013461 design Methods 0.000 description 1
- 239000006185 dispersion Substances 0.000 description 1
- 238000005553 drilling Methods 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- YAGKRVSRTSUGEY-UHFFFAOYSA-N ferricyanide Chemical compound [Fe+3].N#[C-].N#[C-].N#[C-].N#[C-].N#[C-].N#[C-] YAGKRVSRTSUGEY-UHFFFAOYSA-N 0.000 description 1
- 239000003292 glue Substances 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 150000004702 methyl esters Chemical class 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 229920000379 polypropylene carbonate Polymers 0.000 description 1
- 229910052700 potassium Inorganic materials 0.000 description 1
- 239000011591 potassium Substances 0.000 description 1
- QQONPFPTGQHPMA-UHFFFAOYSA-N propylene Natural products CC=C QQONPFPTGQHPMA-UHFFFAOYSA-N 0.000 description 1
- 125000004805 propylene group Chemical group [H]C([H])([H])C([H])([*:1])C([H])([H])[*:2] 0.000 description 1
- 239000011347 resin Substances 0.000 description 1
- 229920005989 resin Polymers 0.000 description 1
- 239000004576 sand Substances 0.000 description 1
- 229910052710 silicon Inorganic materials 0.000 description 1
- 239000010703 silicon Substances 0.000 description 1
- 230000003068 static effect Effects 0.000 description 1
- 239000002352 surface water Substances 0.000 description 1
- 239000004408 titanium dioxide Substances 0.000 description 1
- 230000009466 transformation Effects 0.000 description 1
Classifications
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- 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
- C09K8/5083—Compositions based on water or polar solvents containing organic compounds macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds
-
- 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
- C09K8/514—Compositions based on water or polar solvents containing organic compounds macromolecular compounds of natural origin, e.g. polysaccharides, cellulose
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- 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
- C09K2208/00—Aspects relating to compositions of drilling or well treatment fluids
- C09K2208/18—Bridging agents, i.e. particles for temporarily filling the pores of a formation; Graded salts
-
- 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
- C09K2208/00—Aspects relating to compositions of drilling or well treatment fluids
- C09K2208/34—Lubricant additives
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- Chemical & Material Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- General Life Sciences & Earth Sciences (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Compositions Of Macromolecular Compounds (AREA)
Abstract
The present invention provides the non-linear self-degradation diverting agent of cluster fracturing reforms more in a kind of section and preparation methods, by the material composition of following weight percent: ontology 80-90%, initiator 2-5%, lubricant 2-5%, forming agent 5-10%, reinforcing agent 0.2-0.8% promote degradation agent 1-3%, wherein, ontology is the mixture being made of polyglycolide, polylactide-co-glycolide and polyvinyl alcohol.Water is met under room temperature not bond, and is conducive to pump note；Degradation is slow in finite time, and non-linear relation is presented in rate of dissolution and time under reservoir temperature, meets more cluster pressing crack construction technical requirements in net horizontal section；With microdilatancy ability, the intensity that the later period is blocked in crack is improved；It also can slowly degrade in media environment variation, it is small to reservoir damage.It is combined by batch stirred reactor with double screw extruder, improving temperature change in production process influences diverting agent product, and product physical and chemical index is more stable.
Description
Technical field
The invention belongs to gas field fracturing reform yield-increasing technology fields, and in particular to more cluster fracturing reforms are non-linear in a kind of section
Self-degradation diverting agent and preparation method.
Background technique
With the continuous development of oil gas field, the quality of reservoir declines year by year, and each oil field strengthens the side of reservoir fracturing improvement
It is horizontal constantly to promote hyposmosis densification oil-gas Layer fracturing reform for formula tackling key problem.The more cluster fracturing reform modes of horizontal well in segments gradually at
For an important technical of low permeability oil and gas field transformation, but there is a problem of that more shower hole unlatching rates are low in construction,
Reservoir reconstruction degree is limited, and correctional effect is affected.
Temporarily stifled fracturing technique is to carry out pressing off new oil gas circulation road after temporarily blocking up to old crack by the effect of chemical plugging
A kind of reforming mode important function has effectively been played in terms of reservoir reconstruction by the development of many years and perfect.But with
The continuous development of oil-gas field fracturing reforming technology, temporarily the reforming mode of stifled fracturing material shows slightly single at present, it is difficult to meet part
The demand of technique.In oilfield horizontal well section in more cluster pressing crack constructions, there are the low problems of intensity for oil-soluble temporary plugging agent；Gas field is horizontal
Water-soluble diverting agent dissolves too fast, dissolution within effective time and is not thorough in more cluster pressing crack constructions in well section, and adhesion problem is serious.
Patent No. CN106010492A discloses a kind of degradable high-strength temporary blocking agent, is promoted to become agent, adhesive, propylene by viscosity
Amide, potassium ferricyanide solution, crosslinking agent, ammonium persulfate, sodium hydroxide and water are made；Preparation method is to promote to become by viscosity first
Agent, adhesive, acrylamide put into water and stir evenly；Potassium ferricyanide solution, crosslinking agent, ammonium persulfate are added, is added dropwise after stirring evenly
Sodium hydroxide, and be sufficiently stirred；Last temperature reaction obtains finished product.It is that there is shear shinning using remarkable result of the invention
Non-Newton fluid characteristic.System viscosity improves rapidly after static, i.e. the characteristic that enhances rapidly of structure, improves system for crosslinking agent
Intensity provides help.It is distributed in diverting agent material therein and issues raw gelatification in reservoir temperature, improve the strong of system
Degree forms high-intensitive gelling slug.The effect of chemical packer is realized, the note of water layer or the subsequent stratum blocking agent of auxiliary is blocked
Enter.Simultaneously after closure can self-breaking glue, restored the permeability on stratum.Patent No. CN105482799A discloses one
Diversion agent, including following components, mass percent shared by each component and each component are temporarily blocked up in kind self-degradation hydraulic fracturing are as follows: are increased
Mould agent 1~10%；Modifying agent 0.05~2%；Promotor 0.05~2%；Density adjuster 1~30%；Remaining group is divided into from drop
Adhesive is solved, the self-degradation adhesive is polypropylene carbonate resin.The temporary stall of self-degradation hydraulic fracturing that the patent provides
It is low to agent decomposition temperature, the time is short, decomposition product not will cause secondary pollution.
More cluster pressing crack construction requirements in the net horizontal section of gas field: diverting agent has higher bearing capacity and shut-off capacity；It is temporarily stifled
Agent is added in the slug liquid prepared, and diverting agent does not dissolve for 24 hours in normal-temperature water, does not bond mutually；Diverting agent has non-thread
Property degradation rate, i.e., in 8 hours do not dissolve or dissolve it is extremely slow, quickly dissolved in the 24-48h stage；Diverting agent finally has molten
Solve the performances such as thorough.
Using above-mentioned patent as the pressure break diverting agent product of representative, mainly there is the dissolution of chance oil and meet two aspect of water dissolution, it is temporarily stifled
Exist in the corresponding medium of agent and slowly at the uniform velocity dissolve, chance oil dissolution diverting agent is higher by pressure percentage of damage, meets water and is dissolved in water
Placement can be bonded mutually, influenced to pump, be not easily decomposed after sand plug in reservoir, and construction risk is increased.
Summary of the invention
The purpose of the present invention is to provide the non-linear self-degradation diverting agents of cluster fracturing reform more in a kind of section, overcome existing skill
Above-mentioned technical problem present in art.
It is another object of the present invention to provide the systems of the non-linear self-degradation diverting agents of cluster fracturing reform more in a kind of section
Preparation Method.
Technical solution provided by the invention is as follows:
More non-linear self-degradation diverting agents of cluster fracturing reform in a kind of section, by the material composition of following weight percent: ontology 80-
90%, initiator 2-5%, lubricant 2-5%, forming agent 5-10%, reinforcing agent 0.2-0.8% promote degradation agent 1-3%, wherein ontology is
The mixture being made of polyglycolide, polylactide-co-glycolide and polyvinyl alcohol.
By accounting in non-linear self-degradation diverting agent based on weight percent, polyglycolide 20-25%, polylactide-co-glycolide
50-60%, polyvinyl alcohol 10-15%.
The initiator is dibutyl phthalate, dibutyl maleate, a kind of in dioctyl maleate
Or it is several.
The lubricant is isopropanol, one or two kinds of in n-butanol.
The forming agent is made of methyl methacrylate-grafted starch and beta-cyclodextrin, is temporarily blocked up by non-linear self-degradation is accounted for
Weight percent meter in agent, methyl methacrylate-grafted starch 3-8%, beta-cyclodextrin 2-5%.
The reinforcing agent is one or more of nano silica, nano aluminium oxide, nano zine oxide.
The rush degradation agent is one or more of sodium carbonate, sodium bicarbonate, potassium carbonate.
Each substance of formula ratio is added the preparation method of more non-linear self-degradation diverting agents of cluster fracturing reform in a kind of section
Batch stirred reactor, is reacted vacuumizing protective condition, be delivered to later double screw extruder be granulated to get.
The preparation method of more non-linear self-degradation diverting agents of cluster fracturing reform in a kind of section, the specific steps are as follows:
The ontology of formula ratio is added batch stirred reactor and is warming up to 80 DEG C by step 1), and the initiator of formula ratio is then added
20-30min is reacted, the forming agent reaction 10-20min of formula ratio is added, the lubricant reaction of formula ratio is added later
30-40min adds the reinforcing agent reaction 10-15min of formula ratio, is eventually adding the rush degradation agent reaction 20- of formula ratio
30min；
Step 2 heating has a rest formula stirred reactor temperature to 120 DEG C, and temperature control speed is 1-2 DEG C/min, when temperature rises to 120 DEG C
When, unlatching vacuumizes, and reacts 30-40min, and stop batch stirred reactor later and heats, 0.5-1 DEG C of cooling rate of control/
Min, temperature are reduced to 100-105 DEG C and keep constant；
Material in stirred reactor is delivered to double screw extruder by step 3), and double screw extruder temperature is controlled in 100-105
DEG C, double screw extruder is squeezed out, is granulated, and sieve sieving control material diameter and length are temporarily blocked up to get non-linear self-degradation
Agent product.
The beneficial effects of the present invention are:
1, water is met under self-degradation diverting agent room temperature not bond, be conducive to pump note；Degradation is slow in finite time, dissolves under reservoir temperature
Non-linear relation is presented in rate and time, meets more cluster pressing crack construction technical requirements in net horizontal section.
Diverting agent is drawn on three kinds of polyglycolide, polylactide-co-glycolide and polyvinyl alcohol bulk materials by initiator
Enter methyl methacrylate-grafted starch and beta-cyclodextrin is modified, improves diverting agent hydrophobicity and dispersion performance, make it
Disperse in water, bond.The superelevation specific surface and super-hydrophobicity that reinforcing agent fills in diverting agent, hate diverting agent surface
Water is not dissolved at certain time (within 8h) or is dissolved slowly, dissolution quickening, diverting agent rate of dissolution and time after 24 hours
Non-linear relation is presented, meets in net horizontal section and is dissolved in 8h slowly in more cluster pressing crack constructions, substantially completely dissolved in 48h hours
It is required that.
2, self-degradation diverting agent has microdilatancy ability, and self-degradation diverting agent can be improved and block the strong of later period in crack
Degree.
It when polyvinyl alcohol starts degradation in water, first absorbs water, microdilatancy increases volume, has diverting agent in fracture end-face
Stronger sealing characteristics, this is the general temporarily stifled characteristic not having；Polyglycolide, polylactide-co-glycolide are in reservoir temperature 105
Under the conditions of DEG C, it will appear deformation after 2h, it is cross-laid between diverting agent, under micro- deformation condition, it will occur to be compacted phenomenon, into one
Step improves the sealing characteristics of diverting agent.By reinforcing agent, (nano effect improves the intrinsic adhesive force of diverting agent, mentions significantly
Diverting agent itself compression strength is risen, to improve the sealing characteristics of diverting agent.
3, self-degradation diverting agent also can slowly degrade when media environment changes, and residue is low after degradation, small to reservoir damage.
Polyglycolide, polylactide-co-glycolide and polyvinyl alcohol are degradable material, under the conditions of high temperature, long-time, can be dropped automatically
Solution；In aqueous media, oil-phase medium, (48h) temporarily stifled automatic degradation can be accelerated due to being added to rush degradation agent in diverting agent, and
After bulk degradation, environmental pollution is small, degradation residue is low, thus to reducing to reservoir damage.
4, it is combined by batch stirred reactor with double screw extruder in preparation method, improves temperature in production process
Variation influences diverting agent product, by the way that lubricant is added, improves material in batch stirred reactor mixing uniformity, leads to
Heating is crossed, is vacuumized, influence of the lubricant to diverting agent density is reduced, keeps product physical and chemical index more stable.
It is described in further details below in conjunction with attached drawing.
Detailed description of the invention
Fig. 1 is non-linear self-degradation diverting agent solubility curve under 90-120 DEG C of different temperatures；
Fig. 2 is the percentage of damage of the non-linear self-degradation diverting agent of different-grain diameter and the relation curve of pressure.
Specific embodiment
The present invention provides the non-linear self-degradation diverting agents of cluster fracturing reform more in a kind of section, by following weight percent
Material composition: ontology 80-90%, initiator 2-5%, lubricant 2-5%, forming agent 5-10%, reinforcing agent 0.2-0.8% promote degradation agent
1-3%, wherein ontology is the mixture being made of polyglycolide, polylactide-co-glycolide and polyvinyl alcohol.
Embodiment 1:
The present invention provides the non-linear self-degradation diverting agents of cluster fracturing reform more in a kind of section, by the substance of following weight percent
Composition: ontology 85%, initiator 5%, lubricant 2%, forming agent 5%, reinforcing agent 0.4% promote degradation agent 2.6%, wherein ontology is served as reasons
The mixture of polyglycolide, polylactide-co-glycolide and polyvinyl alcohol composition.
Preparation process: the ontology of formula ratio is added batch stirred reactor and is warming up to 80 DEG C by step 1), is then added
The initiator for reaction 20min of formula ratio adds the forming agent reaction 10min of formula ratio, the profit of formula ratio is added later
Lubrication prescription reacts 30min, adds the reinforcing agent reaction 10min of formula ratio, is eventually adding the rush degradation agent reaction of formula ratio
20min；
Step 2 heating has a rest formula stirred reactor temperature to 120 DEG C, and temperature control speed is 2 DEG C/min, when temperature rises to 120 DEG C,
Unlatching vacuumizes, and reacts 40min, stops batch stirred reactor heating later, controls 1 DEG C/min of cooling rate, temperature drop
Down to 101 DEG C and keep constant；
Material in stirred reactor is delivered to double screw extruder by step 3), and double screw extruder temperature is controlled at 102 DEG C, double
Screw extruder is squeezed out, is granulated, and sieve sieving control material diameter and length produce to get non-linear self-degradation diverting agent
Product.
In the present embodiment, ontology is by the polyglycolide of 20% weight percent, polylactide-second of 55% weight percent
The polyvinyl alcohol of lactide and 10% weight percent composition；Initiator is by the dibutyl phthalate of 1% weight percent and 4%
The dioctyl maleate of weight percent forms；Lubricant is isopropanol；Forming agent by 3% weight percent methyl-prop
The beta-cyclodextrin of e pioic acid methyl ester graft starch and 2% amount percentage composition；Reinforcing agent by 0.2% weight percent nanometer titanium dioxide
The nano zine oxide of silicon and 0.2% weight percent composition；Promote degradation agent by the sodium carbonate and 0.6% weight hundred of 2% weight percent
Divide the sodium bicarbonate composition of ratio.
Embodiment 2:
The present invention provides the non-linear self-degradation diverting agents of cluster fracturing reform more in a kind of section, by the substance of following weight percent
Composition: ontology 85%, initiator 2%, lubricant 3%, forming agent 7%, reinforcing agent 0.5% promote degradation agent 2.5%, wherein ontology is served as reasons
The mixture of polyglycolide, polylactide-co-glycolide and polyvinyl alcohol composition.
In the present embodiment, ontology is by the polyglycolide of 20% weight percent, polylactide-second of 50% weight percent
The polyvinyl alcohol of lactide and 15% weight percent composition；Initiator is dioctyl maleate；Lubricant is for isopropanol and just
Butanol, mass percent are respectively 1% and 2%；Forming agent is by the methyl methacrylate-grafted starch of 4% weight percent and 3%
Measure the beta-cyclodextrin composition of percentage；Reinforcing agent by 0.3% weight percent nano silica and 0.2% weight percent
Nano aluminium oxide composition；Promote degradation agent to be made of the potassium carbonate of 0.5% weight percent and the sodium bicarbonate of 2% weight percent.
Preparation process: the ontology of formula ratio is added batch stirred reactor and is warming up to 80 DEG C by step 1), is then added
The initiator for reaction 30min of formula ratio adds the forming agent reaction 20min of formula ratio, the profit of formula ratio is added later
Lubrication prescription reacts 40min, adds the reinforcing agent reaction 15min of formula ratio, is eventually adding the rush degradation agent reaction of formula ratio
30min；
Step 2 heating has a rest formula stirred reactor temperature to 120 DEG C, and temperature control speed is 1 DEG C/min, when temperature rises to 120 DEG C,
Unlatching vacuumizes, and reacts 30min, stops batch stirred reactor heating later, controls 0.5 DEG C/min of cooling rate, temperature
It is reduced to 101 DEG C and keeps constant；
Material in stirred reactor is delivered to double screw extruder by step 3), and double screw extruder temperature is controlled at 102 DEG C, double
Screw extruder is squeezed out, is granulated, and sieve sieving control material diameter and length produce to get non-linear self-degradation diverting agent
Product.
Embodiment 3:
The present invention provides the non-linear self-degradation diverting agents of cluster fracturing reform more in a kind of section, by the substance of following weight percent
Composition: ontology 80%, initiator 5%, lubricant 5%, forming agent 6.2%, reinforcing agent 0.8% promote degradation agent 3%, wherein ontology is served as reasons
The mixture of polyglycolide, polylactide-co-glycolide and polyvinyl alcohol composition.
In the present embodiment, ontology is by the polyglycolide of 20% weight percent, polylactide-second of 50% weight percent
The polyvinyl alcohol of lactide and 10% weight percent composition；Initiator by dioctyl maleate, dibutyl phthalate and
The mixture of dioctyl maleate composition, weight percent is respectively 2%, 2% and 1%；Lubricant is isopropanol and positive fourth
Alcohol, mass percent are respectively 3% and 2%；Forming agent is by the methyl methacrylate-grafted starch of 4% weight percent and 2.2%
Measure the beta-cyclodextrin composition of percentage；Reinforcing agent by 0.4% weight percent nano silica and 0.4% weight percent
Nano aluminium oxide composition；Promote degradation agent to be made of the potassium carbonate of 1% weight percent and the sodium bicarbonate of 2% weight percent.
The preparation method is the same as that of Example 1.
Embodiment 4:
The present invention provides the non-linear self-degradation diverting agents of cluster fracturing reform more in a kind of section, by the substance of following weight percent
Composition: ontology 89.8%, initiator 2%, lubricant 2%, forming agent 5%, reinforcing agent 0.2% promote degradation agent 1%, wherein ontology is served as reasons
The mixture of polyglycolide, polylactide-co-glycolide and polyvinyl alcohol composition.
In the present embodiment, ontology is by the polyglycolide of 25% weight percent, the polylactide-of 49.8% weight percent
The polyvinyl alcohol of glycolide and 15% weight percent composition；Initiator is dioctyl maleate；Lubricant is isopropanol；
Forming agent is made of the methyl methacrylate-grafted starch of 4% weight percent and the beta-cyclodextrin of 1% amount percentage；Reinforcing agent
For nano aluminium oxide；Rush degradation agent is saleratus.
Preparation method is the same as embodiment 2.
In above embodiments, the relative molecular mass of polyglycolide is 20,000-4 ten thousand, opposite point of polylactide-co-glycolide
Protonatomic mass is 40,000-8 ten thousand, and the relative molecular mass of polyvinyl alcohol is 110,000-18 ten thousand.
In the non-linear self-degradation diverting agent product preparation process of embodiment 1, embodiment 3 and embodiment 4,1- is used respectively
The sieve of 1.8mm, 1.8-2.4mm and 2.4-3mm are sieved, and obtain the non-linear self-degradation diverting agent of different-grain diameter.
Dissolving test (such as Fig. 1) in water is carried out under different temperatures again to non-linear self-degradation diverting agent prepared by embodiment 2
Pressure-bearing test is carried out with non-linear self-degradation diverting agent of the residue performance test (being shown in Table 1) to different-grain diameter.
As shown in Figure 1, non-linear self-degradation diverting agent dissolves under 90-120 DEG C of different temperatures, trend is essentially identical, and 8 is small
When within dissolution rate within 5% or so, 10 hour dissolution rate 8%；After when the time is more than 10 small, rate of dissolution obviously adds
Fastly, 24 hours dissolution rates reach 50-60%, and for 48 hours dissolution rates more than 95%, nonlinear characteristic is obvious.
As shown in Fig. 2, pressure is when within 10MPa when the non-linear smaller bearing capacity of self-degradation diverting agent partial size is stronger
Non-linear self-degradation diverting agent percentage of damage is extremely low, average out to 3% or so, and when pressure is more than 13MPa, percentage of damage is increased.If with
10% percentage of damage thinks its bearing capacity, and the non-linear self-degradation diverting agent bearing capacity of the different-grain diameter is 13-15MPa or so.
The non-linear self-degradation diverting agent residue performance test of table 1
Table 1 shows that mass concentration is that 5%(accounts for the mass percent of water or drilling fluid) non-linear self-degradation diverting agent, in reservoir
At a temperature of, dissolving its residue content by 5 days is 215-245mg/L, is 15-36mg/ when dissolving its residue content by 15 days
L illustrates non-linear self-degradation diverting agent as time went on, and diverting agent itself can be decomposed further.
The foregoing examples are only illustrative of the present invention, does not constitute the limitation to protection scope of the present invention, all
It is within being all belonged to the scope of protection of the present invention with the same or similar design of the present invention.The component that embodiment does not describe in detail
With the well-known components and common structure or conventional means of the structure category industry, do not describe one by one here.
Claims (9)
1. more non-linear self-degradation diverting agents of cluster fracturing reform in a kind of section, which is characterized in that by the object of following weight percent
Matter composition: ontology 80-90%, initiator 2-5%, lubricant 2-5%, forming agent 5-10%, reinforcing agent 0.2-0.8% promote degradation agent 1-
3%, wherein ontology is the mixture being made of polyglycolide, polylactide-co-glycolide and polyvinyl alcohol.
2. more non-linear self-degradation diverting agents of cluster fracturing reform in a kind of section according to claim 1, it is characterised in that: press
Account for weight percent meter in non-linear self-degradation diverting agent, polyglycolide 20-25%, polylactide-co-glycolide 50-60%, poly- second
Enol 10-15%.
3. more non-linear self-degradation diverting agents of cluster fracturing reform in a kind of section according to claim 1, it is characterised in that: institute
It is one or more of in dibutyl phthalate, dibutyl maleate, dioctyl maleate for stating initiator.
4. more non-linear self-degradation diverting agents of cluster fracturing reform in a kind of section according to claim 1, it is characterised in that: institute
It is one or two kinds of in isopropanol, n-butanol for stating lubricant.
5. more non-linear self-degradation diverting agents of cluster fracturing reform in a kind of section according to claim 1, it is characterised in that: institute
It states forming agent to be made of methyl methacrylate-grafted starch and beta-cyclodextrin, by accounting for weight hundred in non-linear self-degradation diverting agent
Divide than meter, methyl methacrylate-grafted starch 3-8%, beta-cyclodextrin 2-5%.
6. more non-linear self-degradation diverting agents of cluster fracturing reform in a kind of section according to claim 1, it is characterised in that: institute
Stating reinforcing agent is one or more of nano silica, nano aluminium oxide, nano zine oxide.
7. more non-linear self-degradation diverting agents of cluster fracturing reform in a kind of section according to claim 1, it is characterised in that: institute
It states and promotees degradation agent as one or more of sodium carbonate, sodium bicarbonate, potassium carbonate.
8. the preparation method of more non-linear self-degradation diverting agents of cluster fracturing reform in a kind of section according to claim 1,
It is characterized in that: batch stirred reactor is added in each substance of formula ratio, is reacted vacuumizing protective condition, it is defeated later
Send to double screw extruder be granulated to get.
9. the preparation method of more non-linear self-degradation diverting agents of cluster fracturing reform in a kind of section according to claim 8,
It is characterized in that, the specific steps are as follows:
The ontology of formula ratio is added batch stirred reactor and is warming up to 80 DEG C by step 1), and the initiator of formula ratio is then added
20-30min is reacted, the forming agent reaction 10-20min of formula ratio is added, the lubricant reaction of formula ratio is added later
30-40min adds the reinforcing agent reaction 10-15min of formula ratio, is eventually adding the rush degradation agent reaction 20- of formula ratio
30min；
Step 2 heating has a rest formula stirred reactor temperature to 120 DEG C, and temperature control speed is 1-2 DEG C/min, when temperature rises to 120 DEG C
When, unlatching vacuumizes, and reacts 30-40min, and stop batch stirred reactor later and heats, 0.5-1 DEG C of cooling rate of control/
Min, temperature are reduced to 100-105 DEG C and keep constant；
Material in stirred reactor is delivered to double screw extruder by step 3), and double screw extruder temperature is controlled in 100-105
DEG C, double screw extruder is squeezed out, is granulated, and sieve sieving control material diameter and length are temporarily blocked up to get non-linear self-degradation
Agent product.
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| CN111965065B (en) * | 2020-08-28 | 2022-09-23 | 上海浦景化工技术股份有限公司 | Method for testing and evaluating degradation performance of organic temporary plugging agent for oil and gas field |
| CN111965065A (en) * | 2020-08-28 | 2020-11-20 | 上海浦景化工技术股份有限公司 | Method for testing and evaluating degradation performance of organic temporary plugging agent for oil and gas field |
| CN112011321A (en) * | 2020-08-28 | 2020-12-01 | 上海浦景化工技术股份有限公司 | Self-adaptive deformation composite temporary plugging agent and preparation method thereof |
| CN112745819B (en) * | 2021-02-05 | 2022-04-22 | 西南石油大学 | Degradable temporary plugging agent and preparation method thereof |
| CN112745819A (en) * | 2021-02-05 | 2021-05-04 | 西南石油大学 | Degradable temporary plugging agent and preparation method thereof |
| CN113372891A (en) * | 2021-07-09 | 2021-09-10 | 成都劳恩普斯科技有限公司 | High-strength high-temperature acid fracturing temporary plugging agent and preparation method and application thereof |
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