CN108690584A - A kind of compound profile control agent - Google Patents
A kind of compound profile control agent Download PDFInfo
- Publication number
- CN108690584A CN108690584A CN201810481234.0A CN201810481234A CN108690584A CN 108690584 A CN108690584 A CN 108690584A CN 201810481234 A CN201810481234 A CN 201810481234A CN 108690584 A CN108690584 A CN 108690584A
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- China
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- weight
- agent
- surfactant
- cyclodextrin
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
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- 150000001875 compounds Chemical class 0.000 title claims abstract description 64
- 239000004094 surface-active agent Substances 0.000 claims abstract description 262
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 232
- 150000007942 carboxylates Chemical class 0.000 claims abstract description 193
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 135
- 238000002347 injection Methods 0.000 claims abstract description 105
- 239000007924 injection Substances 0.000 claims abstract description 105
- 238000007789 sealing Methods 0.000 claims abstract description 74
- WZCQRUWWHSTZEM-UHFFFAOYSA-N 1,3-phenylenediamine Chemical compound NC1=CC=CC(N)=C1 WZCQRUWWHSTZEM-UHFFFAOYSA-N 0.000 claims abstract description 70
- 229940018564 m-phenylenediamine Drugs 0.000 claims abstract description 70
- 239000002245 particle Substances 0.000 claims abstract description 69
- 229920002401 polyacrylamide Polymers 0.000 claims abstract description 69
- 239000002981 blocking agent Substances 0.000 claims abstract description 63
- 239000003431 cross linking reagent Substances 0.000 claims abstract description 54
- 229940123973 Oxygen scavenger Drugs 0.000 claims abstract description 52
- HFHDHCJBZVLPGP-UHFFFAOYSA-N schardinger α-dextrin Chemical class O1C(C(C2O)O)C(CO)OC2OC(C(C2O)O)C(CO)OC2OC(C(C2O)O)C(CO)OC2OC(C(O)C2O)C(CO)OC2OC(C(C2O)O)C(CO)OC2OC2C(O)C(O)C1OC2CO HFHDHCJBZVLPGP-UHFFFAOYSA-N 0.000 claims abstract description 30
- 239000000463 material Substances 0.000 claims abstract description 18
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 168
- BWHMMNNQKKPAPP-UHFFFAOYSA-L potassium carbonate Chemical compound [K+].[K+].[O-]C([O-])=O BWHMMNNQKKPAPP-UHFFFAOYSA-L 0.000 claims description 115
- 238000002360 preparation method Methods 0.000 claims description 85
- 239000002994 raw material Substances 0.000 claims description 84
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 81
- NIXOWILDQLNWCW-UHFFFAOYSA-N 2-Propenoic acid Natural products OC(=O)C=C NIXOWILDQLNWCW-UHFFFAOYSA-N 0.000 claims description 75
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 75
- -1 octyl alkyl dimethyl ammonium chlorides Chemical class 0.000 claims description 72
- 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 63
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims description 61
- FSSPGSAQUIYDCN-UHFFFAOYSA-N 1,3-Propane sultone Chemical compound O=S1(=O)CCCO1 FSSPGSAQUIYDCN-UHFFFAOYSA-N 0.000 claims description 59
- KRKNYBCHXYNGOX-UHFFFAOYSA-N citric acid Chemical compound OC(=O)CC(O)(C(O)=O)CC(O)=O KRKNYBCHXYNGOX-UHFFFAOYSA-N 0.000 claims description 59
- 238000010792 warming Methods 0.000 claims description 59
- 238000006243 chemical reaction Methods 0.000 claims description 57
- 229910000027 potassium carbonate Inorganic materials 0.000 claims description 57
- 238000009413 insulation Methods 0.000 claims description 54
- CBCKQZAAMUWICA-UHFFFAOYSA-N 1,4-phenylenediamine Chemical compound NC1=CC=C(N)C=C1 CBCKQZAAMUWICA-UHFFFAOYSA-N 0.000 claims description 49
- SMZOUWXMTYCWNB-UHFFFAOYSA-N 2-(2-methoxy-5-methylphenyl)ethanamine Chemical compound COC1=CC=C(C)C=C1CCN SMZOUWXMTYCWNB-UHFFFAOYSA-N 0.000 claims description 49
- 238000003756 stirring Methods 0.000 claims description 48
- HUMNYLRZRPPJDN-UHFFFAOYSA-N benzaldehyde Chemical compound O=CC1=CC=CC=C1 HUMNYLRZRPPJDN-UHFFFAOYSA-N 0.000 claims description 45
- HNPSIPDUKPIQMN-UHFFFAOYSA-N dioxosilane;oxo(oxoalumanyloxy)alumane Chemical class O=[Si]=O.O=[Al]O[Al]=O HNPSIPDUKPIQMN-UHFFFAOYSA-N 0.000 claims description 42
- 239000008367 deionised water Substances 0.000 claims description 35
- 229910021641 deionized water Inorganic materials 0.000 claims description 35
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- UMGDCJDMYOKAJW-UHFFFAOYSA-N thiourea Chemical compound NC(N)=S UMGDCJDMYOKAJW-UHFFFAOYSA-N 0.000 claims description 30
- GMGLGUFSJCMZNT-UHFFFAOYSA-N BrCCCCCC.BrCCCCCC Chemical compound BrCCCCCC.BrCCCCCC GMGLGUFSJCMZNT-UHFFFAOYSA-N 0.000 claims description 29
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- SNRUBQQJIBEYMU-UHFFFAOYSA-N Dodecane Natural products CCCCCCCCCCCC SNRUBQQJIBEYMU-UHFFFAOYSA-N 0.000 claims description 26
- 239000001116 FEMA 4028 Substances 0.000 claims description 26
- 235000011175 beta-cyclodextrine Nutrition 0.000 claims description 26
- 229960004853 betadex Drugs 0.000 claims description 26
- DWAQJAXMDSEUJJ-UHFFFAOYSA-M Sodium bisulfite Chemical compound [Na+].OS([O-])=O DWAQJAXMDSEUJJ-UHFFFAOYSA-M 0.000 claims description 25
- 238000002156 mixing Methods 0.000 claims description 25
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- NFDRPXJGHKJRLJ-UHFFFAOYSA-N edtmp Chemical compound OP(O)(=O)CN(CP(O)(O)=O)CCN(CP(O)(O)=O)CP(O)(O)=O NFDRPXJGHKJRLJ-UHFFFAOYSA-N 0.000 claims description 24
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- 239000011734 sodium Substances 0.000 claims description 24
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- 230000002829 reductive effect Effects 0.000 claims description 16
- KWSLGOVYXMQPPX-UHFFFAOYSA-N 5-[3-(trifluoromethyl)phenyl]-2h-tetrazole Chemical compound FC(F)(F)C1=CC=CC(C2=NNN=N2)=C1 KWSLGOVYXMQPPX-UHFFFAOYSA-N 0.000 claims description 14
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- 230000003213 activating effect Effects 0.000 claims description 12
- 239000000203 mixture Substances 0.000 claims description 12
- OMPJBNCRMGITSC-UHFFFAOYSA-N Benzoylperoxide Chemical compound C=1C=CC=CC=1C(=O)OOC(=O)C1=CC=CC=C1 OMPJBNCRMGITSC-UHFFFAOYSA-N 0.000 claims description 11
- 238000000034 method Methods 0.000 claims description 11
- 235000019441 ethanol Nutrition 0.000 claims description 10
- NBVXSUQYWXRMNV-UHFFFAOYSA-N fluoromethane Chemical compound FC NBVXSUQYWXRMNV-UHFFFAOYSA-N 0.000 claims description 9
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- 244000025254 Cannabis sativa Species 0.000 claims 1
- BFNBIHQBYMNNAN-UHFFFAOYSA-N ammonium sulfate Chemical compound N.N.OS(O)(=O)=O BFNBIHQBYMNNAN-UHFFFAOYSA-N 0.000 claims 1
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- 235000011130 ammonium sulphate Nutrition 0.000 claims 1
- JIRRNZWTWJGJCT-UHFFFAOYSA-N carbamothioylthiourea Chemical compound NC(=S)NC(N)=S JIRRNZWTWJGJCT-UHFFFAOYSA-N 0.000 claims 1
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- VAZSKTXWXKYQJF-UHFFFAOYSA-N ammonium persulfate Chemical compound [NH4+].[NH4+].[O-]S(=O)OOS([O-])=O VAZSKTXWXKYQJF-UHFFFAOYSA-N 0.000 description 24
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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
- C09K8/512—Compositions based on water or polar solvents containing organic compounds macromolecular compounds containing cross-linking agents
-
- 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
- C09K8/5045—Compositions based on water or polar solvents containing inorganic compounds
-
- 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
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Abstract
The present invention provides a kind of compound profile control agent, and by weight, the compound profile control agent includes 20-50 parts of surfactant type sealing agent, 30-70 parts of increasing injection agent, 5-20 parts of particle blocking agent;Wherein, the surfactant type sealing agent is by polyacrylamide, water, multiple crosslinking agent, modified cyclodextrin, m-phenylene diamine (MPD), oxygen scavenger and carboxylate gemini surfactant by weight 1:(110-131):(0.05-0.12):(0.2-0.8):(0.1-0.3):(0.05-0.2):The ratio of (0.3-1) is prepared, the present invention is using three kinds of surfactant type sealing agent, increasing injection agent and particle blocking agent coupling transfer drive critical materials, by carrying out have combination of the water plugging and profiling technology with increasing injection technology, realize that water plugging and profile controlling, increasing injection and technology of reservoir sweep are effectively unified.
Description
Technical field
The present invention relates to profile control, increasing injection and the technology of reservoir sweep fields used in oil exploitation, and in particular to a kind of
Compound profile control agent.
Background technology
Low permeability oil field refers to the oil field that Oil Layer Reservoir permeability is low, abundance is low, single well productivity is low.Low permeability oil and gas field exists
Important in inhibiting in China's oil and gas development, China's Low Permeability Oil/gas resource distribution is with oily is more, Oil-gas Accumulation Types are more, divides
Cloth region is wide and the characteristics of " oil under upper gas, based on marine facies gassiness, terrestrial facies oil gas has concurrently ", hypotonic in explored reserves
The ratio of saturating reservoir reserve is very high, accounts for about 2/3 or more of national reserves, potentiality to be exploited is huge.
In the development process of low-permeability oilfield, waterflooding extraction is that current the most successful one raising efficiently, economic is adopted
Yield technology.In the injecting process in oil field, interlayer caused by injecting water is gradually shown with horizontal contradiction in the water filling middle and later periods in layer
Expose, become apparent particularly with the compact reservoir in crack, microcrack development, for example, the shape of injection water coning, well pattern waterline
At etc., cause the rising of low-permeability oilfield development cost and the decline of recovery ratio.For these problems, generally require using water blockoff tune
The technology cutd open blocks big pore throat and crack.Meanwhile low-permeability oilfield can face another question again, be exactly water injection well
" shorting " problem, that is, practical water injection rate cannot reach " daily water-injection rate " of oil field development setting, make the reservoir energy of oil field development
Effectively it cannot be supplied and be supplemented, influenced correspondence and declined by effect oil well and well group yield, maximally efficient technology is exactly
Increasing injection technology reduces the water injection pressure of water injection well, improves water injection rate.
Therefore, in view of the above-mentioned problems, the present invention provides a kind of compound profile control agent, carry out water plugging and profiling technology and increase with decompression
Note technology has combination, realizes the water blockoff adjustment in water logging crack, improves the water injection rate of matrix reservoirs, improves the drive of heterogeneous reservoir
Oily effect.
Invention content
In view of the above-mentioned problems, by the evaluation of hyposmosis microcrack geologic characteristics and flood effectiveness, of the invention one
It is a to be designed to provide a kind of compound profile control agent, by effective combination of water plugging and profiling technology and increasing injection technology, realize
Water plugging and profile controlling, increasing injection and technology of reservoir sweep are effectively unified.
Another object of the present invention is to provide grinding for the development of increasing injection acid solution, the development of profile control agent and particle blocking agent
System.
It is compound using this another object of the present invention is to the exploitation that the compound profile control agent is applied to low permeability oil field
Profile control agent can release the tamper of water injection well, while reach the displacement of reservoir oil effect to oil well.
The technical solution adopted in the present invention is as follows:
A kind of compound profile control agent, by weight, the compound profile control agent include surfactant type sealing agent 20-
50 parts, 30-70 parts of increasing injection agent, 5-20 parts of particle blocking agent;Wherein, the surfactant type sealing agent is by polyacrylamide
Amine, water, multiple crosslinking agent, modified cyclodextrin, m-phenylene diamine (MPD), oxygen scavenger and carboxylate gemini surfactant are by weight 1:
(110-131):(0.05-0.12):(0.2-0.8):(0.1-0.3):(0.05-0.2):The ratio of (0.3-1) is prepared.
The raw material of the increasing injection agent forms, by weight, including 30-35 parts of double octyl alkyl dimethyl ammonium chlorides,
3-7 parts of fluorocarbon surfactant, 3-5 parts of nonionic surfactant, 5-10 parts of ethylene diamine tetra methylene phosphonic acid sodium, (Z) -3,3,4-
Trimethyl -2-5 parts of piperazine ketoxime, 38-57 parts of deionized water;The fluorocarbon surfactant is fluorine carbon FC-4430, it is described it is non-from
Sub- surfactant is ethoxylated dodecyl alcohol.
The raw material of the particle blocking agent forms, by weight, including 20-50 parts of acrylamide, 20-50 parts of acrylic acid,
1-15 parts of sodium hydroxide, 2-10 parts of modified zeolite, 0.1-0.5 parts of ammonium persulfate, 0.05-0.25 parts of sodium hydrogensulfite, N, N- are sub-
0.1-0.5 parts of bisacrylamide, 1-5 parts of lauryl ester, 40-60 parts of water;
The modified zeolite is acrylic acid modified zeolite, and the acrylic acid modified zeolite is by zeolite powder, acrylic acid, peroxidating
Dibenzoyl is by weight 100:(12-20):(0.13-0.2) is formed;Preparation method includes the following steps:By zeolite powder plus
It is, by weight acrylic acid and dibenzoyl peroxide is added, after stirring 2-3h, to go out in 50-70 DEG C of mixing machine to enter barrel temperature
Material, after mixing machine barrel temperature is risen to 110-120 DEG C, above-mentioned material is refunded in mixing machine, is discharged after high-speed stirred 1-2h,
Obtain acrylic acid modified zeolite.
The preparation method of the surfactant type sealing agent includes the following steps:Formula ratio is added into reactor first
Polyacrylamide and water, be 5.0 with careless acid for adjusting pH value after stirring and dissolving, place 1-3h fully to cure;Then add successively
Oxygen scavenger, multiple crosslinking agent, modified cyclodextrin, the m-phenylene diamine (MPD) for entering formula ratio after stirring evenly, are warming up to 80-90 DEG C, heat preservation
After 20-40h, then it is cooled to 55-60 DEG C, the carboxylate gemini surfactant of formula ratio is added, stirred 1-2h, be cooled to room
Temperature is to get the surfactant type sealing agent.
The modified cyclodextrin is citric acid-modified beta-cyclodextrin, and the citric acid-modified beta-cyclodextrin is by citric acid, secondary
Sodium phosphite, deionized water, beta-cyclodextrin and absolute ethyl alcohol are by weight 1:(0.1-0.3):(1-3):(0.5-1):(3-6)
Composition;The preparation method of the citric acid-modified beta-cyclodextrin includes the following steps:It is sequentially added by weight into reactor
Citric acid, sodium hypophosphite and deionized water are added the beta-cyclodextrin of formula ratio, are warming up to 70-80 after stirring is completely dissolved
DEG C, insulation reaction 2-3h, then it is warming up to 100-110 DEG C, then insulation reaction 4-6h is cooled to room temperature, be slowly dropped to anhydrous
In ethyl alcohol, after being added dropwise, 1-2h is stirred, filtering, 60 DEG C are dried under reduced pressure 16-20h, obtain the real citric acid-modified β-ring paste
Essence.
The carboxylate gemini surfactant is by carboxylate gemini surfactant A and carboxylate gemini surfactant
B is by weight 1:(0.1-0.7) is mixed.
The carboxylate gemini surfactant A is by 1,3-propane sultone, absolute ethyl alcohol, p-phenylenediamine, methanol, anhydrous
Potassium carbonate, bromododecane, acetone are by weight 1:(4-8):(0.3-0.7):(8-12):(1-1.3):(0.8-1.2):(3-
6) ratio is prepared;
The preparation method of the carboxylate gemini surfactant A includes the following steps:Add successively first into reactor
Entering the 1,3-propane sultone of formula ratio, absolute ethyl alcohol, p-phenylenediamine, stirring is warming up to 55-60 DEG C, insulation reaction 20-25h,
It is concentrated to dryness;Then the methanol, Anhydrous potassium carbonate, bromododecane for sequentially adding formula ratio are warming up to 60-70 DEG C, protect
Temperature reaction 30-35h, filtering, filtrate decompression are concentrated to dryness;The acetone for being eventually adding formula ratio is recrystallized, and 60 DEG C of decompressions are dry
Dry 10-12h obtains the carboxylate gemini surfactant A.
It includes 1,3-propane sultone, absolute ethyl alcohol, to benzene two that the carboxylate gemini surfactant B, which prepares raw material,
Amine, methanol, Anhydrous potassium carbonate, hexyl bromide 1 bromohexane, acetone are by weight 1:(4-7):(0.4-0.6):(9-12):(1-1.3):
(0.9-1.1):The ratio of (3-6) is prepared;
The preparation method of the carboxylate gemini surfactant B includes the following steps:Add successively first into reactor
Entering the 1,3-propane sultone of formula ratio, absolute ethyl alcohol, p-phenylenediamine, stirring is warming up to 55-60 DEG C, insulation reaction 20-25h,
It is concentrated to dryness;Then the methanol, Anhydrous potassium carbonate, hexyl bromide 1 bromohexane for sequentially adding formula ratio are warming up to 60-70 DEG C, heat preservation
30-35h, filtering are reacted, filtrate decompression is concentrated to dryness;The acetone for being eventually adding formula ratio is recrystallized, and 60 DEG C are dried under reduced pressure
10-12h obtains the carboxylate gemini surfactant B.
The multiple crosslinking agent is by benzaldehyde and benzenediol by weight 1:The ratio of (0.3-0.6) mixes.
The oxygen scavenger includes thiocarbamide, 2,4- dithiobiurets, semicarbazides, thiosemicarbazide, the bis- (sulphur of Isosorbide-5-Nitrae-phenylene
Urea) in it is one or more.
The oxygen scavenger is semicarbazides, Isosorbide-5-Nitrae-phenylene bis- (thiocarbamides) by weight 1:The ratio of (0.3-2) mixes.
The compound profile control agent is applied to the exploitation of low permeability oil field.
The present invention has the following advantages:
The present invention passes through three kinds of surfactant type sealing agent, increasing injection agent and particle blocking agent coupling transfer drive key materials
Material carries out have combination of the water plugging and profiling technology with increasing injection technology, realizes that water plugging and profile controlling, increasing injection and technology of reservoir sweep are effective
It is unified.By the continuous variation of the multi-parameters such as injection process viscosity of material, state, flow resistance, wetability, flowing pressure, adjust
Whole injection water passes through energy automatic coupling, flow direction auto-steering, the self balancing mistake of Fluid pressure to advantageous azimuthal flow
Journey reduces the injected water volume for flowing to macropore, and expansion flows to the hypotonic hypotonic area not employed, realizes the water blockoff tune in water logging crack
Agent, the water injection rate for improving matrix reservoirs, improve the oil displacement efficiency of heterogeneous reservoir.
Specific implementation mode
The detailed description for preferred implementation method of the invention below of participating in the election of and including embodiment this hair can be more easily understood
Bright content.Unless otherwise defined, all technologies used herein and scientific terminology have common with fields of the present invention
The normally understood identical meaning of technical staff, when there is a conflict, the definition in this specification shall prevail.
As used herein term " by ... prepare " it is synonymous with "comprising".Term "comprising" used herein, " comprising ",
" having ", " containing " or its any other deformation, it is intended that cover non-exclusionism includes.For example, the combination comprising listed elements
Object, step, method, product or device are not necessarily limited to those elements, but may include not expressly listed other elements or
Such composition, step, method, product or the intrinsic element of device.
Conjunction " Consists of " excludes any element that do not point out, step or component.If in claim, this
Phrase will make claim be closed, so that it is not included the material in addition to the material of those descriptions, but relative normal
Except rule impurity.When being rather than immediately following after theme in the clause that phrase " Consists of " appears in claim main body,
It is only limited to the element described in the clause;Other elements are not excluded except the claim as a whole.
Equivalent, concentration or other values or parameter are excellent with range, preferred scope or a series of upper limit preferred values and lower limit
When the Range Representation that choosing value limits, this, which should be understood as, specifically discloses by any range limit or preferred value and any range
Any pairing of lower limit or preferred value is formed by all ranges, regardless of whether the range separately discloses.For example, when open
When range " 1 to 5 ", described range should be interpreted as including range " 1 to 4 ", " 1 to 3 ", " 1 to 2 ", " 1 to 2 and 4 to
5 ", " 1 to 3 and 5 " etc..When numberical range is described herein, unless otherwise stated, otherwise range intention includes its end
Value and all integers and score in the range.
Singulative includes that plural number discusses object, unless the context clearly dictates otherwise." optional " or it is " arbitrary
It is a kind of " refer to that the item described thereafter or event may or may not occur, and the description include situation that event occurs and
The situation that event does not occur.
Approximate term in specification and claims is used for modifying quantity, and it is specific to indicate that the present invention is not limited to this
Quantity further includes the modified part of the acceptable change without lead to related basic function close to the quantity.Phase
It answers, modifies a numerical value with " about ", " about " etc., mean that the present invention is not limited to the exact numericals.In some examples, approximate
Term likely corresponds to the precision of the instrument of measured value.In present specification and claims, range limits can be with
Combination and/or exchange, these ranges include all subranges contained therebetween if not stated otherwise.
In addition, indefinite article "an" before element of the present invention or component and "one" quantitative requirement to element or component
(i.e. occurrence number) unrestriction.Therefore "one" or "an" should be read as including one or at least one, and odd number
The element or component of form also include plural form, unless the apparent purport of the quantity refers to singulative.
" polymer " means the polymerizable compound prepared by the monomer by the identical or different type of polymerization.Generic term
" polymer " includes term " homopolymer ", " copolymer ", " terpolymer " and " copolymer ".
" copolymer " means the polymer prepared by polymerizeing at least two different monomers.Generic term " copolymer " includes
(it is general with term " terpolymer " for term " copolymer " (its generally to refer to the polymer prepared by two kinds of different monomers)
To refer to the polymer prepared by three kinds of different monomers).It also includes the polymer manufactured by polymerizeing more kinds of monomers.
" blend " means the polymer that two or more polymer is formed by mixing jointly by physics or chemical method.
The present invention is specifically described below by embodiment.It is necessarily pointed out that following embodiment is only used
In the invention will be further described, it should not be understood as limiting the scope of the invention, professional and technical personnel in the field
Some the nonessential modifications and adaptations made according to the content of aforementioned present invention, still fall within protection scope of the present invention.
In addition, if without other explanations, it is raw materials used to be all commercially available, it is purchased from traditional Chinese medicines chemical reagent.
Embodiment 1
The present invention provides a kind of compound profile control agents, calculate by weight, and the compound profile control agent includes that surface is lived
20-50 parts of dosage form sealing agent of property, 30-70 parts of increasing injection agent, 5-20 parts of particle blocking agent;Wherein, the surfactant type envelope
Blocking agent is by polyacrylamide, water, multiple crosslinking agent, modified cyclodextrin, m-phenylene diamine (MPD), oxygen scavenger and carboxylate gemini surface-active
Agent is by weight 1:(110-131):(0.05-0.12):(0.2-0.8):(0.1-0.3):(0.05-0.2):The ratio of (0.3-1)
Example is prepared.
The present invention passes through three kinds of surfactant type sealing agent, increasing injection agent and particle blocking agent coupling transfer drive key materials
Material carries out have combination of the water plugging and profiling technology with increasing injection technology, realizes that water plugging and profile controlling, increasing injection and technology of reservoir sweep are effective
It is unified.By the continuous variation of the multi-parameters such as injection process viscosity of material, state, flow resistance, wetability, flowing pressure, adjust
Whole injection water passes through energy automatic coupling, flow direction auto-steering, the self balancing mistake of Fluid pressure to advantageous azimuthal flow
Journey reduces the injected water volume for flowing to macropore, and expansion flows to the hypotonic hypotonic area not employed, realizes the water blockoff tune in water logging crack
Agent, the water injection rate for improving matrix reservoirs, improve the oil displacement efficiency of heterogeneous reservoir.
Embodiment 2
On the basis of embodiment 1, the surfactant type sealing agent prepare raw material include polyacrylamide, it is compound
Crosslinking agent, modified cyclodextrin, m-phenylene diamine (MPD), oxygen scavenger, carboxylate gemini surfactant.Wherein, the polyacrylamide is
The conventional widely used raw material of water plugging profile control agent, shrinkage crimping when molecule encounters oil phase, and when encountering water phase, molecule chain-unfolding
Backwater is expanded, selectivity is good.But since such polymer and stratum are mainly by Hydrogen Binding Adsorption, adsorption strength is weak, is unable to undergo water
Wash away, in addition, formation water salinity is high, polyacrylamide salt resistance effect is weak, salt neutralized it is electrical on polyacrylamide group,
The charge on polyacrylamide ionic group is set to be shielded, the electrostatic repulsion between ion weakens, the curling of polymer long-chain.
In the present embodiment, the polyacrylamide is the partially hydrolyzed polyacrylamide (PHPA) of degree of hydrolysis 18%, and molecular weight is 14,000,000.
The multiple crosslinking agent is by benzaldehyde and benzenediol by weight 1:0.4 ratio mixes.
The beta-cyclodextrin is one kind of cyclodextrin, and the cyclodextrin glycosyltransferase generated by bud pole bacterium acts on
Starch and one kind for generating by 7 D- glucopyranoses passes through cyclic oligosaccharide made of α-Isosorbide-5-Nitrae glucosides key connection.In this implementation
In example, the modified cyclodextrin is citric acid-modified beta-cyclodextrin.
The citric acid-modified beta-cyclodextrin is by citric acid, sodium hypophosphite, deionized water, beta-cyclodextrin and absolute ethyl alcohol
By weight 1:(0.1-0.3):(1-3):(0.5-1):(3-6) is formed;The preparation method of the citric acid-modified beta-cyclodextrin
Include the following steps:By weight citric acid, sodium hypophosphite and deionized water is sequentially added into reactor, stirring is completely molten
The beta-cyclodextrin of formula ratio is added in Xie Hou, is warming up to 70-80 DEG C, insulation reaction 2-3h, then be warming up to 100-110 DEG C, and heat preservation is anti-
4-6h is answered, room temperature is then cooled to, is slowly dropped in absolute ethyl alcohol, after being added dropwise, stirs 1-2h, filtering, 60 DEG C of decompressions
Dry 16-20h obtains the real citric acid-modified beta-cyclodextrin.The present invention by using citric acid-modified cyclodextrin, containing-
NH2 ,-COOH ,-OH and cyclodextrin cavity can reduce its crystallinity, increase water solubility, obtain a kind of environmentally protective, price
Cheap polysaccharide crosslinking agent.
The oxygen scavenger includes thiocarbamide, 2,4- dithiobiurets, semicarbazides, thiosemicarbazide, the bis- (sulphur of Isosorbide-5-Nitrae-phenylene
Urea) in it is one or more.
Embodiment 3
On the basis of embodiment 2, the carboxylate gemini surfactant include carboxylate gemini surfactant A and
Carboxylate gemini surfactant B, the carboxylate gemini surfactant A by 1,3-propane sultone, absolute ethyl alcohol, to benzene
Diamines, methanol, Anhydrous potassium carbonate, bromododecane, acetone are by weight 1:(4-8):(0.3-0.7):(8-12):(1-1.3):
(0.8-1.2):The ratio of (3-6) is prepared;The preparation method of the carboxylate gemini surfactant A includes following step
Suddenly:The 1,3-propane sultone of formula ratio, absolute ethyl alcohol, p-phenylenediamine are sequentially added into reactor first, stirring is warming up to
55-60 DEG C, insulation reaction 20-25h is concentrated to dryness;Then the methanol, Anhydrous potassium carbonate, bromo of formula ratio are sequentially added
Dodecane is warming up to 60-70 DEG C, insulation reaction 30-35h, and filtering, filtrate decompression is concentrated to dryness;It is eventually adding the third of formula ratio
Ketone is recrystallized, and 60 DEG C are dried under reduced pressure 10-12h, obtains the carboxylate gemini surfactant A.
It includes 1,3-propane sultone, absolute ethyl alcohol, to benzene two that the carboxylate gemini surfactant B, which prepares raw material,
Amine, methanol, Anhydrous potassium carbonate, hexyl bromide 1 bromohexane, acetone are by weight 1:(4-7):(0.4-0.6):(9-12):(1-1.3):
(0.9-1.1):The ratio of (3-6) is prepared;The preparation method of the carboxylate gemini surfactant B includes following step
Suddenly:The 1,3-propane sultone of formula ratio, absolute ethyl alcohol, p-phenylenediamine are sequentially added into reactor first, stirring is warming up to
55-60 DEG C, insulation reaction 20-25h is concentrated to dryness;Then the methanol, Anhydrous potassium carbonate, 1- bromines of formula ratio are sequentially added
Hexane is warming up to 60-70 DEG C, insulation reaction 30-35h, and filtering, filtrate decompression is concentrated to dryness;It is eventually adding the acetone of formula ratio
It is recrystallized, 60 DEG C are dried under reduced pressure 10-12h, obtain the carboxylate gemini surfactant B.
Carboxylate gemini surfactant A described in the carboxylate gemini surfactant and the carboxylate gemini table
The weight ratio of face activating agent B is 1:(0.1-0.7);Preferably, the carboxylate gemini surfactant A and the carboxylate are double
The weight ratio of sub- surfactant B is 1:0.24.
In the present embodiment, the surfactant type sealing agent by polyacrylamide, water, oxygen scavenger, multiple crosslinking agent,
Modified cyclodextrin, m-phenylene diamine (MPD) and carboxylate gemini surfactant be by weight being 1:(110-131):(0.05-0.12):
(0.2-0.8):(0.1-0.3):(0.05-0.2):(0.3-1) is formed.The preparation method packet of the surfactant type sealing agent
Include following steps:The molecular weight that formula ratio is added first into reactor is 14,000,000, the partial hydrolysis poly- third of degree of hydrolysis 18%
Acrylamide, salinity is the water of 125520mg/L, is 5.0 with careless acid for adjusting pH value after stirring and dissolving, places 1-3h with fully ripe
Change;Then oxygen scavenger, multiple crosslinking agent, modified cyclodextrin, the m-phenylene diamine (MPD) for sequentially adding formula ratio, after stirring evenly, heating
To 80-90 DEG C, after keeping the temperature 20-40h, then it is cooled to 55-60 DEG C, the carboxylate gemini surfactant of formula ratio is added, stirred
1-2h is cooled to room temperature to get the surfactant type sealing agent.It is each alternate that the addition of surfactant can reduce underground
Interfacial tension causes emulsification, reduces rock stratum to the adsorption capacity of oil and increases the solubility of oil in water, reduces the viscous of crude oil
Degree, to produce the oil fettered by hole.
Surfactant type sealing agent passes through polyacrylamide, multiple crosslinking agent, modified cyclodextrin, isophthalic two in the present invention
Amine, oxygen scavenger, carboxylate gemini surfactant synergistic effect, obtained surfactant type sealing agent can use high mineralization
Water configuration is spent, crosslinking ability is strong, and there are long-time stability, high temperature resistant high salinity there is resistance to water flooding to wash away for a long time required
Intensity.
Embodiment 4
On the basis of embodiment 1, by weight, the raw material composition of the increasing injection agent includes double octyl diformazans
30-35 parts of ammonium chloride, 3-7 parts of fluorocarbon surfactant, 3-5 parts of nonionic surfactant, ethylene diamine tetra methylene phosphonic acid sodium
5-10 parts, (Z) -3,2-5 parts of 3,4- trimethyls-piperazine ketoxime, 38-57 parts of deionized water;Preferably, the increasing injection agent
It includes double 32 parts of octyl alkyl dimethyl ammonium chlorides, 4 parts of fluorocarbon surfactant, 3 parts of nonionic surfactant, second to prepare raw material
7 parts of four methene Alendronate of diamines, (Z) -3,3,4- trimethyls-piperazine ketoxime (CAS:74987-05-6) 3 parts, deionized water 50
Part.
The fluorocarbon surfactant is fluorine carbon FC-4430, and the nonionic surfactant is lauryl alcohol polyethylene glycol oxide
Ether.
The preparation method of the increasing injection agent includes the following steps:
Double octyl alkyl dimethyl ammonium chlorides, fluorine carbon FC-4430, laruyl alcohol polyoxy are sequentially added into reactor by weight
Vinethene, ethylene diamine tetra methylene phosphonic acid sodium, (Z) -3,3,4- trimethyls-piperazine ketoxime, deionized water are warming up to 50 DEG C, heat preservation
3h is reacted, room temperature is cooled to, obtains the increasing injection agent.
Increasing injection agent of the present invention deposits the ultra-thin molecular film to be formed using aqueous solution as transfer medium in rock surface;
Also have the function of changing core wettability and anti-clayswelling in addition to peeling off moisture film, and then reduce water injection pressure, the decompression increases
Injecting also has the multi-effects such as inhibition, scale inhibition, sterilization, can effectively prevent injection aqueous corrosion product, fouling, bacterium etc. to stratum
The influence of porosity, the introducing of piperazine group further increase antibacterial effect, greatly improve low permeability reservoir water injection well
Flood effectiveness.
Embodiment 5
On the basis of embodiment 1, by weight, the raw material composition of the particle blocking agent includes acrylamide 20-50
Part, 20-50 parts of acrylic acid, 1-15 parts of sodium hydroxide, 2-10 parts of modified zeolite, 0.1-0.5 parts of ammonium persulfate, sodium hydrogensulfite
0.05-0.25 parts, N, 0.1-0.5 parts of N- methylene-bisacrylamides, 1-5 parts of lauryl ester, 40-60 parts of water;
Preferably, the raw material for preparing of the particle blocking agent includes 35 parts of acrylamide, 21 parts of acrylic acid, 5 parts of sodium hydroxide, modified zeolite
5 parts, 0.3 part of ammonium persulfate, 0.1 part, N of sodium hydrogensulfite, 0.25 part of N- methylene-bisacrylamides, lauryl
3 parts of ester, 50 parts of water.
The modified zeolite is acrylic acid modified zeolite, and the acrylic acid modified zeolite is by zeolite powder, acrylic acid and peroxide
Change dibenzoyl by weight 100:(12-20):(0.13-0.2) is formed, and preparation method includes the following steps:By zeolite powder
It is that acrylic acid and dibenzoyl peroxide are added by weight in 50-70 DEG C of mixing machine that barrel temperature, which is added, after stirring 2-3h,
Discharging, after mixing machine barrel temperature is risen to 110-120 DEG C, above-mentioned material is refunded in mixing machine, is gone out after high-speed stirred 1-2h
Material, obtains acrylic acid modified zeolite.
The preparation method of the particle blocking agent includes the following steps:
Deionized water, the sodium hydroxide of formula ratio are added into reactor, after stirring evenly, the propylene of formula ratio is added
Acid is sufficiently stirred, and is sequentially added lauryl ester, acrylamide, the modified zeolite of formula ratio, is warming up to 45
DEG C, the N of formula ratio is then added, N- methylene-bisacrylamides are warming up to 80 DEG C, add formula ratio sodium hydrogensulfite,
Ammonium persulfate, insulation reaction 2h, is cooled to room temperature, shreds drying, is ground into powder, obtains the particle blocking agent.
Particle blocking agent of the present invention can be in sieve tube completion water plugging of horizontal well, not level of pollution section precise screen pipe,
Consolidation time is longer, moderate strength, high temperature resistant, the suspension of the particle of the particle blocking agent is good, good fluidity, sieving property are good,
High temperature resistant, easily to enter stratum, expense low, blocks that risk is low, the term of validity is long, blocks success rate to reach precise screen pipe horizontal well
It is high.
Embodiment 6
On the basis of the above embodiments, the compound profile control agent is applied to the exploitation of low permeability oil field.The present invention is also
A kind of coupling transfer drive technique is provided, is included the following steps:
(1) service shaft well head is opened, increasing injection agent is passed through under transfer drive pump truck injection well;
(2) surfactant type sealing agent, particle blocking agent are implanted sequentially by transfer drive pump truck;
(3) responding curve of well after injection operation, continues water injection work, promotion of the compound profile control agent in following injected water
Under reservoir vertical-depth react, achieve the purpose that transfer drive augmented injection.
Embodiment 7
A kind of compound profile control agent, by weight, the compound profile control agent include surfactant type sealing agent 35
Part, 55 parts of increasing injection agent, 10 parts of particle blocking agent;
Wherein, it includes polyacrylamide, multiple crosslinking agent, modified ring paste that the surfactant type sealing agent, which prepares raw material,
Essence, m-phenylene diamine (MPD), oxygen scavenger, carboxylate gemini surfactant, the polyacrylamide, water, multiple crosslinking agent, citric acid change
Property beta-cyclodextrin, m-phenylene diamine (MPD), oxygen scavenger, carboxylate gemini surfactant weight ratio be 1:120:0.1:0.5:0.2:
0.1:0.6.
The polyacrylamide is the partially hydrolyzed polyacrylamide (PHPA) of degree of hydrolysis 18%, and molecular weight is 14,000,000;It is described to change
Property cyclodextrin be citric acid-modified beta-cyclodextrin;The multiple crosslinking agent be benzaldehyde, hydroquinone, the benzaldehyde with it is described
The weight ratio 1 of hydroquinone:0.4;The oxygen scavenger is that semicarbazides, Isosorbide-5-Nitrae-phenylene are bis- (thiocarbamide), the semicarbazides with it is described
The weight ratio of Isosorbide-5-Nitrae-phenylene bis- (thiocarbamides) is 1:0.72;The carboxylate gemini surfactant includes carboxylate gemini surface
Activating agent A and carboxylate gemini surfactant B, it includes the third sulphurs of 1,3- that the carboxylate gemini surfactant A, which prepares raw material,
Acid lactone, absolute ethyl alcohol, p-phenylenediamine, methanol, Anhydrous potassium carbonate, bromododecane, acetone;It lives on the carboxylate gemini surface
It includes 1,3-propane sultone, absolute ethyl alcohol, p-phenylenediamine, methanol, Anhydrous potassium carbonate, hexyl bromide 1 bromohexane, third that property agent B, which prepares raw material,
Ketone;The weight ratio of the carboxylate gemini surfactant A and carboxylate gemini surfactant B is 1:0.24;
The preparation method of the surfactant type sealing agent includes the following steps:
It is 14,000,000 that molecular weight is added into reactor, the partially hydrolyzed polyacrylamide (PHPA) of degree of hydrolysis 18%, and salinity is
The water of 125520mg/L is 5.0 with careless acid for adjusting pH value after stirring and dissolving, places 2 hours fully to cure, then successively plus
Oxygen scavenger, multiple crosslinking agent, citric acid-modified beta-cyclodextrin, the m-phenylene diamine (MPD) for entering formula ratio, after stirring evenly, are warming up to 88
DEG C, 30h is kept the temperature, is cooled to 60 DEG C, carboxylate gemini surfactant is added, 1h is stirred, is cooled to room temperature, obtains the surface
Active agent formulation sealing agent.
The citric acid-modified beta-cyclodextrin is by citric acid, sodium hypophosphite, deionized water, beta-cyclodextrin, absolute ethyl alcohol
By weight 1:0.2:2:0.95:5 compositions;The preparation method of the citric acid-modified beta-cyclodextrin includes the following steps:To anti-
Beta-cyclodextrin is added after answering the citric acid for sequentially adding formula ratio in device, sodium hypophosphite, deionized water, stirring to be completely dissolved,
80 DEG C, insulation reaction 2h are warming up to, is warming up to 110 DEG C, insulation reaction 6h is cooled to room temperature, is slowly dropped to the nothing of formula ratio
In water-ethanol, after being added dropwise, 2h is stirred, filtering, 60 DEG C are dried under reduced pressure 16h, obtain the citric acid-modified beta-cyclodextrin.
The carboxylate gemini surfactant A is by 1,3-propane sultone, absolute ethyl alcohol, p-phenylenediamine, methanol, anhydrous
Potassium carbonate, bromododecane, acetone are by weight 1:6:0.5:10:1.2:1:4 ratio is prepared;The carboxylate gemini
The preparation method of surfactant A includes the following steps:
The 1,3-propane sultone of formula ratio, absolute ethyl alcohol, p-phenylenediamine are sequentially added into reactor, are stirred, heating
To 60 DEG C, insulation reaction 20h is concentrated to dryness, and sequentially adds the methanol, Anhydrous potassium carbonate, bromododecane of formula ratio,
70 DEG C, insulation reaction 30h are warming up to, filtering, filtrate decompression is concentrated to dryness, and the acetone that formula ratio is added is recrystallized, 60 DEG C
It is dried under reduced pressure 10h, obtains the carboxylate gemini surfactant A.
The carboxylate gemini surfactant B is by 1,3-propane sultone, absolute ethyl alcohol, p-phenylenediamine, methanol, anhydrous
Potassium carbonate, hexyl bromide 1 bromohexane, acetone are 1 by weight:6:0.5:10:1.2:1:4 ratio is prepared;The carboxylate gemini
The preparation method of surfactant B includes the following steps:
The 1,3-propane sultone of formula ratio, absolute ethyl alcohol, p-phenylenediamine are sequentially added into reactor, are stirred, heating
To 60 DEG C, insulation reaction 20h is concentrated to dryness, and sequentially adds the methanol, Anhydrous potassium carbonate, hexyl bromide 1 bromohexane of formula ratio, is risen
Temperature is to 70 DEG C, insulation reaction 30h, and filtering, filtrate decompression is concentrated to dryness, and the acetone that formula ratio is added is recrystallized, and 60 DEG C subtract
Dry 10h is pressed dry, the carboxylate gemini surfactant B is obtained.
The increasing injection agent prepare raw material include double 32 parts of octyl alkyl dimethyl ammonium chlorides, 4 parts of fluorine carbon FC-4430,
3 parts of ethoxylated dodecyl alcohol, 7 parts of ethylene diamine tetra methylene phosphonic acid sodium, (Z) -3,3 parts of 3,4- trimethyls-piperazine ketoxime, deionization
50 parts of water;
The preparation method of the increasing injection agent includes the following steps:
The double octyl alkyl dimethyl ammonium chlorides, fluorine carbon FC-4430, laruyl alcohol of above-mentioned parts by weight are sequentially added into reactor
Polyoxyethylene ether, ethylene diamine tetra methylene phosphonic acid sodium, (Z) -3,3,4- trimethyls-piperazine ketoxime, deionized water, are warming up to 50 DEG C,
Insulation reaction 3h, is cooled to room temperature, obtains the increasing injection agent.
The raw material for preparing of the particle blocking agent includes 35 parts of acrylamide, 21 parts of acrylic acid, 5 parts of sodium hydroxide, acrylic acid
5 parts of modified zeolite, 0.3 part of ammonium persulfate, 0.1 part, N of sodium hydrogensulfite, 0.25 part of N- methylene-bisacrylamides, metering system
3 parts of sour dodecane ester, 50 parts of water;
The preparation method of the particle blocking agent includes the following steps:
The deionized water of 50 parts by weight, the sodium hydroxide of 5 parts by weight are sequentially added into reactor, after stirring evenly, are added
The acrylic acid for entering 21 parts by weight, is sufficiently stirred, and sequentially adds the lauryl esters of 3 parts by weight, 35 parts by weight
The acrylic acid modified zeolite of acrylamide, 5 parts by weight is warming up to 45 DEG C, and the N of 0.25 parts by weight, N- methylene bisacrylamides is added
Amide is warming up to 80 DEG C, and the sodium hydrogensulfite of 0.1 parts by weight, the ammonium persulfate of 0.3 parts by weight, insulation reaction 2h, cooling is added
To room temperature, drying is shredded, powder is ground into, obtains the particle blocking agent.
The acrylic acid modified zeolite is 100 by weight by zeolite powder, acrylic acid and dibenzoyl peroxide (BPO):
16:0.18 ratio is prepared;The preparation method of the acrylic acid modified zeolite includes the following steps:
It is in 60 DEG C of mixing machines, by weight addition acrylic acid and dibenzoyl peroxide that barrel temperature, which is added, in zeolite powder
(BPO), after stirring 2h, discharging after mixing machine barrel temperature is risen to 120 DEG C, above-mentioned material is refunded in mixing machine, high-speed stirring
It discharges after mixing 1h, obtains acrylic acid modified zeolite.
Embodiment 8
A kind of compound profile control agent, calculates by weight, and the compound profile control agent includes surfactant type sealing agent
20 parts, 70 parts of increasing injection agent, 10 parts of particle blocking agent;
Wherein, it includes polyacrylamide, multiple crosslinking agent, modified ring paste that the surfactant type sealing agent, which prepares raw material,
Essence, m-phenylene diamine (MPD), oxygen scavenger, carboxylate gemini surfactant, the polyacrylamide are the partial hydrolysis of degree of hydrolysis 18%
Polyacrylamide, molecular weight are 14,000,000;The modified cyclodextrin is citric acid-modified beta-cyclodextrin;The multiple crosslinking agent is
Benzaldehyde, hydroquinone, the weight ratio 1 of the benzaldehyde and the hydroquinone:0.4;The oxygen scavenger is semicarbazides, Isosorbide-5-Nitrae-
Phenylene is bis- (thiocarbamide), and the weight ratio of the semicarbazides and the Isosorbide-5-Nitrae-phenylene bis- (thiocarbamides) is 1:0.72;The carboxylate
Gemini surface active agent includes carboxylate gemini surfactant A and carboxylate gemini surfactant B, the carboxylate gemini
It includes 1,3-propane sultone, absolute ethyl alcohol, p-phenylenediamine, methanol, Anhydrous potassium carbonate, bromo that surfactant A, which prepares raw material,
Dodecane, acetone;It includes 1,3-propane sultone, absolute ethyl alcohol, to benzene that the carboxylate gemini surfactant B, which prepares raw material,
Diamines, methanol, Anhydrous potassium carbonate, hexyl bromide 1 bromohexane, acetone;The carboxylate gemini surfactant A and carboxylate gemini surface
The weight ratio of activating agent B is 1:0.24;
The increasing injection agent prepare raw material include double 32 parts of octyl alkyl dimethyl ammonium chlorides, 4 parts of fluorine carbon FC-4430,
3 parts of ethoxylated dodecyl alcohol, 7 parts of ethylene diamine tetra methylene phosphonic acid sodium, (Z) -3,3 parts of 3,4- trimethyls-piperazine ketoxime, deionization
50 parts of water;
The raw material for preparing of the particle blocking agent includes 35 parts of acrylamide, 21 parts of acrylic acid, 5 parts of sodium hydroxide, acrylic acid
5 parts of modified zeolite, 0.3 part of ammonium persulfate, 0.1 part, N of sodium hydrogensulfite, 0.25 part of N- methylene-bisacrylamides, metering system
3 parts of sour dodecane ester, 50 parts of water;
The preparation method of the surfactant type sealing agent, the preparation method of the increasing injection agent, the particle are stifled
The preparation method of agent is the same as embodiment 7.
Embodiment 9
A kind of compound profile control agent, calculates by weight, and the compound profile control agent includes surfactant type sealing agent
50 parts, 30 parts of increasing injection agent, 10 parts of particle blocking agent;
Wherein, it includes polyacrylamide, multiple crosslinking agent, modified ring paste that the surfactant type sealing agent, which prepares raw material,
Essence, m-phenylene diamine (MPD), oxygen scavenger, carboxylate gemini surfactant, the polyacrylamide are the partial hydrolysis of degree of hydrolysis 18%
Polyacrylamide, molecular weight are 14,000,000;The modified cyclodextrin is citric acid-modified beta-cyclodextrin;The multiple crosslinking agent is
Benzaldehyde, hydroquinone, the weight ratio 1 of the benzaldehyde and the hydroquinone:0.4;The oxygen scavenger is semicarbazides, Isosorbide-5-Nitrae-
Phenylene is bis- (thiocarbamide), and the weight ratio of the semicarbazides and the Isosorbide-5-Nitrae-phenylene bis- (thiocarbamides) is 1:0.72;The carboxylate
Gemini surface active agent includes carboxylate gemini surfactant A and carboxylate gemini surfactant B, the carboxylate gemini
It includes 1,3-propane sultone, absolute ethyl alcohol, p-phenylenediamine, methanol, Anhydrous potassium carbonate, bromo that surfactant A, which prepares raw material,
Dodecane, acetone;It includes 1,3-propane sultone, absolute ethyl alcohol, to benzene that the carboxylate gemini surfactant B, which prepares raw material,
Diamines, methanol, Anhydrous potassium carbonate, hexyl bromide 1 bromohexane, acetone;The carboxylate gemini surfactant A and carboxylate gemini surface
The weight ratio of activating agent B is 1:0.24;
The increasing injection agent prepare raw material include double 32 parts of octyl alkyl dimethyl ammonium chlorides, 4 parts of fluorine carbon FC-4430,
3 parts of ethoxylated dodecyl alcohol, 7 parts of ethylene diamine tetra methylene phosphonic acid sodium, (Z) -3,3 parts of 3,4- trimethyls-piperazine ketoxime, deionization
50 parts of water;
The raw material for preparing of the particle blocking agent includes 35 parts of acrylamide, 21 parts of acrylic acid, 5 parts of sodium hydroxide, acrylic acid
5 parts of modified zeolite, 0.3 part of ammonium persulfate, 0.1 part, N of sodium hydrogensulfite, 0.25 part of N- methylene-bisacrylamides, metering system
3 parts of sour dodecane ester, 50 parts of water;
The preparation method of the surfactant type sealing agent, the preparation method of the increasing injection agent, the particle are stifled
The preparation method of agent is the same as embodiment 7.
Embodiment 10
A kind of compound profile control agent, calculates by weight, and the compound profile control agent includes surfactant type sealing agent
35 parts, 55 parts of increasing injection agent, 10 parts of particle blocking agent;
Wherein, it includes polyacrylamide, multiple crosslinking agent, modified ring paste that the surfactant type sealing agent, which prepares raw material,
Essence, m-phenylene diamine (MPD), oxygen scavenger, carboxylate gemini surfactant, the polyacrylamide are the partial hydrolysis of degree of hydrolysis 18%
Polyacrylamide, molecular weight are 14,000,000;The modified cyclodextrin is citric acid-modified beta-cyclodextrin;The multiple crosslinking agent is
Benzaldehyde, hydroquinone, the weight ratio 1 of the benzaldehyde and the hydroquinone:0.4;The oxygen scavenger is semicarbazides, Isosorbide-5-Nitrae-
Phenylene is bis- (thiocarbamide), and the weight ratio of the semicarbazides and the Isosorbide-5-Nitrae-phenylene bis- (thiocarbamides) is 1:0.72;The carboxylate
Gemini surface active agent includes carboxylate gemini surfactant A and carboxylate gemini surfactant B, the carboxylate gemini
It includes 1,3-propane sultone, absolute ethyl alcohol, p-phenylenediamine, methanol, Anhydrous potassium carbonate, bromo that surfactant A, which prepares raw material,
Dodecane, acetone;It includes 1,3-propane sultone, absolute ethyl alcohol, to benzene that the carboxylate gemini surfactant B, which prepares raw material,
Diamines, methanol, Anhydrous potassium carbonate, hexyl bromide 1 bromohexane, acetone;The carboxylate gemini surfactant A and carboxylate gemini surface
The weight ratio of activating agent B is 1:0.1;
The increasing injection agent prepare raw material include double 32 parts of octyl alkyl dimethyl ammonium chlorides, 4 parts of fluorine carbon FC-4430,
3 parts of ethoxylated dodecyl alcohol, 7 parts of ethylene diamine tetra methylene phosphonic acid sodium, (Z) -3,3 parts of 3,4- trimethyls-piperazine ketoxime, deionization
50 parts of water;
The raw material for preparing of the particle blocking agent includes 35 parts of acrylamide, 21 parts of acrylic acid, 5 parts of sodium hydroxide, acrylic acid
5 parts of modified zeolite, 0.3 part of ammonium persulfate, 0.1 part, N of sodium hydrogensulfite, 0.25 part of N- methylene-bisacrylamides, metering system
3 parts of sour dodecane ester, 50 parts of water;
The preparation method of the surfactant type sealing agent, the preparation method of the increasing injection agent, the particle are stifled
The preparation method of agent is the same as embodiment 7.
Embodiment 11
A kind of compound profile control agent, calculates by weight, and the compound profile control agent includes surfactant type sealing agent
35 parts, 55 parts of increasing injection agent, 10 parts of particle blocking agent;
Wherein, it includes polyacrylamide, multiple crosslinking agent, modified ring paste that the surfactant type sealing agent, which prepares raw material,
Essence, m-phenylene diamine (MPD), oxygen scavenger, carboxylate gemini surfactant, the polyacrylamide are the partial hydrolysis of degree of hydrolysis 18%
Polyacrylamide, molecular weight are 14,000,000;The modified cyclodextrin is citric acid-modified beta-cyclodextrin;The multiple crosslinking agent is
Benzaldehyde, hydroquinone, the weight ratio 1 of the benzaldehyde and the hydroquinone:0.4;The oxygen scavenger is semicarbazides, Isosorbide-5-Nitrae-
Phenylene is bis- (thiocarbamide), and the weight ratio of the semicarbazides and the Isosorbide-5-Nitrae-phenylene bis- (thiocarbamides) is 1:0.72;The carboxylate
Gemini surface active agent includes carboxylate gemini surfactant A and carboxylate gemini surfactant B, the carboxylate gemini
It includes 1,3-propane sultone, absolute ethyl alcohol, p-phenylenediamine, methanol, Anhydrous potassium carbonate, bromo that surfactant A, which prepares raw material,
Dodecane, acetone;It includes 1,3-propane sultone, absolute ethyl alcohol, to benzene that the carboxylate gemini surfactant B, which prepares raw material,
Diamines, methanol, Anhydrous potassium carbonate, hexyl bromide 1 bromohexane, acetone;The carboxylate gemini surfactant A and carboxylate gemini surface
The weight ratio of activating agent B is 1:0.7;
The increasing injection agent prepare raw material include double 32 parts of octyl alkyl dimethyl ammonium chlorides, 4 parts of fluorine carbon FC-4430,
3 parts of ethoxylated dodecyl alcohol, 7 parts of ethylene diamine tetra methylene phosphonic acid sodium, (Z) -3,3 parts of 3,4- trimethyls-piperazine ketoxime, deionization
50 parts of water;
The raw material for preparing of the particle blocking agent includes 35 parts of acrylamide, 21 parts of acrylic acid, 5 parts of sodium hydroxide, acrylic acid
5 parts of modified zeolite, 0.3 part of ammonium persulfate, 0.1 part, N of sodium hydrogensulfite, 0.25 part of N- methylene-bisacrylamides, metering system
3 parts of sour dodecane ester, 50 parts of water;
The preparation method of the surfactant type sealing agent, the preparation method of the increasing injection agent, the particle are stifled
The preparation method of agent is the same as embodiment 7.
Embodiment 12
A kind of compound profile control agent, calculates by weight, and the compound profile control agent includes surfactant type sealing agent
35 parts, 55 parts of increasing injection agent, 10 parts of particle blocking agent;
Wherein, it includes polyacrylamide, multiple crosslinking agent, modified ring paste that the surfactant type sealing agent, which prepares raw material,
Essence, m-phenylene diamine (MPD), oxygen scavenger, carboxylate gemini surfactant, the polyacrylamide are the partial hydrolysis of degree of hydrolysis 18%
Polyacrylamide, molecular weight are 14,000,000;The modified cyclodextrin is citric acid-modified beta-cyclodextrin;The multiple crosslinking agent is
Benzaldehyde, hydroquinone, the weight ratio 1 of the benzaldehyde and the hydroquinone:0.4;The oxygen scavenger is semicarbazides, Isosorbide-5-Nitrae-
Phenylene is bis- (thiocarbamide), and the weight ratio of the semicarbazides and the Isosorbide-5-Nitrae-phenylene bis- (thiocarbamides) is 1:0.5;The carboxylate is double
Sub- surfactant includes carboxylate gemini surfactant A and carboxylate gemini surfactant B, the carboxylate gemini table
It includes 1,3-propane sultone, absolute ethyl alcohol, p-phenylenediamine, methanol, Anhydrous potassium carbonate, bromo ten that face activating agent A, which prepares raw material,
Dioxane, acetone;It includes 1,3-propane sultone, absolute ethyl alcohol, to benzene two that the carboxylate gemini surfactant B, which prepares raw material,
Amine, methanol, Anhydrous potassium carbonate, hexyl bromide 1 bromohexane, acetone;The carboxylate gemini surfactant A lives with carboxylate gemini surface
Property agent B weight ratio be 1:0.24;
The increasing injection agent prepare raw material include double 32 parts of octyl alkyl dimethyl ammonium chlorides, 4 parts of fluorine carbon FC-4430,
3 parts of ethoxylated dodecyl alcohol, 7 parts of ethylene diamine tetra methylene phosphonic acid sodium, (Z) -3,3 parts of 3,4- trimethyls-piperazine ketoxime, deionization
50 parts of water;
The raw material for preparing of the particle blocking agent includes 35 parts of acrylamide, 21 parts of acrylic acid, 5 parts of sodium hydroxide, acrylic acid
5 parts of modified zeolite, 0.3 part of ammonium persulfate, 0.1 part, N of sodium hydrogensulfite, 0.25 part of N- methylene-bisacrylamides, metering system
3 parts of sour dodecane ester, 50 parts of water;
The preparation method of the surfactant type sealing agent, the preparation method of the increasing injection agent, the particle are stifled
The preparation method of agent is the same as embodiment 7.
Embodiment 13
A kind of compound profile control agent, calculates by weight, and the compound profile control agent includes surfactant type sealing agent
35 parts, 55 parts of increasing injection agent, 10 parts of particle blocking agent;
Wherein, it includes polyacrylamide, multiple crosslinking agent, modified ring paste that the surfactant type sealing agent, which prepares raw material,
Essence, m-phenylene diamine (MPD), oxygen scavenger, carboxylate gemini surfactant, the polyacrylamide are the partial hydrolysis of degree of hydrolysis 18%
Polyacrylamide, molecular weight are 14,000,000;The modified cyclodextrin is citric acid-modified beta-cyclodextrin;The multiple crosslinking agent is
Benzaldehyde, hydroquinone, the weight ratio 1 of the benzaldehyde and the hydroquinone:0.4;The oxygen scavenger is semicarbazides, Isosorbide-5-Nitrae-
Phenylene is bis- (thiocarbamide), and the weight ratio of the semicarbazides and the Isosorbide-5-Nitrae-phenylene bis- (thiocarbamides) is 1:1.2;The carboxylate is double
Sub- surfactant includes carboxylate gemini surfactant A and carboxylate gemini surfactant B, the carboxylate gemini table
It includes 1,3-propane sultone, absolute ethyl alcohol, p-phenylenediamine, methanol, Anhydrous potassium carbonate, bromo ten that face activating agent A, which prepares raw material,
Dioxane, acetone;It includes 1,3-propane sultone, absolute ethyl alcohol, to benzene two that the carboxylate gemini surfactant B, which prepares raw material,
Amine, methanol, Anhydrous potassium carbonate, hexyl bromide 1 bromohexane, acetone;The carboxylate gemini surfactant A lives with carboxylate gemini surface
Property agent B weight ratio be 1:0.24;
The increasing injection agent prepare raw material include double 32 parts of octyl alkyl dimethyl ammonium chlorides, 4 parts of fluorine carbon FC-4430,
3 parts of ethoxylated dodecyl alcohol, 7 parts of ethylene diamine tetra methylene phosphonic acid sodium, (Z) -3,3 parts of 3,4- trimethyls-piperazine ketoxime, deionization
50 parts of water;
The raw material for preparing of the particle blocking agent includes 35 parts of acrylamide, 21 parts of acrylic acid, 5 parts of sodium hydroxide, acrylic acid
5 parts of modified zeolite, 0.3 part of ammonium persulfate, 0.1 part, N of sodium hydrogensulfite, 0.25 part of N- methylene-bisacrylamides, metering system
3 parts of sour dodecane ester, 50 parts of water;
The preparation method of the surfactant type sealing agent, the preparation method of the increasing injection agent, the particle are stifled
The preparation method of agent is the same as embodiment 7.
Embodiment 14 (comparative example 1)
A kind of compound profile control agent, calculates by weight, and the compound profile control agent includes surfactant type sealing agent
35 parts, 55 parts of increasing injection agent, 10 parts of particle blocking agent;
Wherein, it includes polyacrylamide, multiple crosslinking agent, β-ring paste that the surfactant type sealing agent, which prepares raw material,
Essence, m-phenylene diamine (MPD), oxygen scavenger, carboxylate gemini surfactant, the polyacrylamide are the partial hydrolysis of degree of hydrolysis 18%
Polyacrylamide, molecular weight are 14,000,000;The multiple crosslinking agent be benzaldehyde, hydroquinone, the benzaldehyde with it is described right
The weight ratio 1 of benzenediol:0.4;It includes 1,3-propane sultone, to benzene that the carboxylate gemini surfactant A, which prepares raw material,
Diamines, bromododecane;The carboxylate gemini surfactant A prepare raw material include 1,3-propane sultone, p-phenylenediamine,
Hexyl bromide 1 bromohexane;The weight ratio of the carboxylate gemini surfactant A and carboxylate gemini surfactant B is 1:
0.24;The oxygen scavenger is semicarbazides, Isosorbide-5-Nitrae-phenylene is bis- (thiocarbamide), and the semicarbazides and the Isosorbide-5-Nitrae-phenylene are bis- (thiocarbamide)
Weight ratio be 1:0.72;
The raw material for preparing of the increasing injection agent includes double 32 parts of octyl alkyl dimethyl ammonium chlorides, fluorocarbon surfactant 4
Part, 3 parts of nonionic surfactant, 7 parts of ethylene diamine tetra methylene phosphonic acid sodium, (Z) -3,3 parts of 3,4- trimethyls-piperazine ketoxime are gone
50 parts of ionized water;The fluorocarbon surfactant is fluorine carbon FC-4430, and the nonionic surfactant is laruyl alcohol polyoxy second
Alkene ether;
The raw material for preparing of the particle blocking agent includes 35 parts of acrylamide, 21 parts of acrylic acid, 5 parts of sodium hydroxide, modified boiling
5 parts of stone, 0.3 part of ammonium persulfate, 0.1 part, N of sodium hydrogensulfite, 0.25 part of N- methylene-bisacrylamides, methacrylic acid 12
3 parts of alkyl ester, 50 parts of water;The modified zeolite is acrylic acid modified zeolite;
The surfactant type sealing agent by polyacrylamide, water, multiple crosslinking agent, beta-cyclodextrin, m-phenylene diamine (MPD), remove
Oxygen agent, carboxylate gemini surfactant are by weight 1:120:0.1:0.5:0.2:0.1:0.6 ratio is prepared;It is described
The preparation method of surfactant type sealing agent includes the following steps:
It is 14,000,000 that molecular weight is added into reactor, the partially hydrolyzed polyacrylamide (PHPA) of degree of hydrolysis 18%, and salinity is
The water of 125520mg/L is 5.0 with careless acid for adjusting pH value after stirring and dissolving, places 2 hours fully to cure, then successively plus
Oxygen scavenger, multiple crosslinking agent, beta-cyclodextrin, the m-phenylene diamine (MPD) for entering formula ratio after stirring evenly, are warming up to 88 DEG C, keep the temperature 30h,
60 DEG C are cooled to, the carboxylate gemini surfactant of formula ratio is added, 1h is stirred, is cooled to room temperature, the surface is obtained and lives
Property dosage form sealing agent.
The carboxylate gemini surfactant A is by 1,3-propane sultone, absolute ethyl alcohol, p-phenylenediamine, methanol, anhydrous
Potassium carbonate, bromododecane, acetone are by weight 1:6:0.5:10:1.2:1:4 ratio is prepared;The carboxylate gemini
The preparation method of surfactant A includes the following steps:
The 1,3-propane sultone of formula ratio, absolute ethyl alcohol, p-phenylenediamine are sequentially added into reactor, are stirred, heating
To 60 DEG C, insulation reaction 20h is concentrated to dryness, and sequentially adds the methanol, Anhydrous potassium carbonate, bromododecane of formula ratio,
70 DEG C, insulation reaction 30h are warming up to, filtering, filtrate decompression is concentrated to dryness, and the acetone that formula ratio is added is recrystallized, 60 DEG C
It is dried under reduced pressure 10h, obtains the carboxylate gemini surfactant A;1,3-propane sultone described in the present embodiment, anhydrous second
Alcohol, p-phenylenediamine, methanol, Anhydrous potassium carbonate, bromododecane, acetone weight ratio be 1:6:0.5:10:1.2:1:4.
The carboxylate gemini surfactant B is by 1,3-propane sultone, absolute ethyl alcohol, p-phenylenediamine, methanol, anhydrous
Potassium carbonate, hexyl bromide 1 bromohexane, acetone are by weight 1:6:0.5:10:1.2:1:4 ratios are prepared;The carboxylate gemini surface
The preparation method of activating agent B includes the following steps:
The 1,3-propane sultone of formula ratio, absolute ethyl alcohol, p-phenylenediamine are sequentially added into reactor, are stirred, heating
To 60 DEG C, insulation reaction 20h is concentrated to dryness, and sequentially adds the methanol, Anhydrous potassium carbonate, hexyl bromide 1 bromohexane of formula ratio, is risen
Temperature is to 70 DEG C, insulation reaction 30h, and filtering, filtrate decompression is concentrated to dryness, and the acetone that formula ratio is added is recrystallized, and 60 DEG C subtract
Dry 10h is pressed dry, the carboxylate gemini surfactant B is obtained.
The preparation method of the surfactant type sealing agent with embodiment 7 difference lies in:Changed with beta-cyclodextrin substitution
Property cyclodextrin;The preparation method of the increasing injection agent, the preparation method of the particle blocking agent are the same as embodiment 7.
Embodiment 15 (comparative example 2)
A kind of compound profile control agent, calculates by weight, and the compound profile control agent includes surfactant type sealing agent
35 parts, 55 parts of increasing injection agent, 10 parts of particle blocking agent;
Wherein, it includes polyacrylamide, multiple crosslinking agent, modified ring paste that the surfactant type sealing agent, which prepares raw material,
Essence, m-phenylene diamine (MPD), oxygen scavenger, carboxylate gemini surfactant, the polyacrylamide are the partial hydrolysis of degree of hydrolysis 18%
Polyacrylamide, molecular weight are 14,000,000;The modified cyclodextrin is citric acid-modified beta-cyclodextrin;The multiple crosslinking agent is
Benzaldehyde, hydroquinone, the weight ratio 1 of the benzaldehyde and the hydroquinone:0.4;The oxygen scavenger is semicarbazides, Isosorbide-5-Nitrae-
Phenylene is bis- (thiocarbamide), and the weight ratio of the semicarbazides and the Isosorbide-5-Nitrae-phenylene bis- (thiocarbamides) is 1:0.72;The carboxylate
Gemini surface active agent includes carboxylate gemini surfactant A and carboxylate gemini surfactant B, the carboxylate gemini
It includes 1,3-propane sultone, absolute ethyl alcohol, p-phenylenediamine, methanol, Anhydrous potassium carbonate, bromo that surfactant A, which prepares raw material,
Dodecane, acetone;It includes 1,3-propane sultone, absolute ethyl alcohol, to benzene that the carboxylate gemini surfactant B, which prepares raw material,
Diamines, methanol, Anhydrous potassium carbonate, hexyl bromide 1 bromohexane, acetone;The carboxylate gemini surfactant A and carboxylate gemini surface
The weight ratio of activating agent B is 1:0.24;
The raw material for preparing of the particle blocking agent includes 35 parts of acrylamide, 21 parts of acrylic acid, 5 parts of sodium hydroxide, acrylic acid
5 parts of modified zeolite, 0.3 part of ammonium persulfate, 0.1 part, N of sodium hydrogensulfite, 0.25 part of N- methylene-bisacrylamides, metering system
3 parts of sour dodecane ester, 50 parts of water;
The increasing injection agent prepare raw material include double 32 parts of octyl alkyl dimethyl ammonium chlorides, 4 parts of fluorine carbon FC-4430,
3 parts of ethoxylated dodecyl alcohol, 7 parts of ethylene diamine tetra methylene phosphonic acid sodium, 3 parts of dimethyl ketone oxime, 50 parts of deionized water;
The preparation method of the increasing injection agent includes the following steps:
Double octyl alkyl dimethyl ammonium chlorides of 32 parts by weight, the fluorine carbon FC- of 4 parts by weight are sequentially added into reactor
4430, the dimethyl ketone of the ethoxylated dodecyl alcohol of 3 parts by weight, the ethylene diamine tetra methylene phosphonic acid sodium of 7 parts by weight, 3 parts by weight
The deionized water of oxime, 50 parts by weight is warming up to 50 DEG C, and insulation reaction 3h is cooled to room temperature, obtains the increasing injection agent.
The preparation method of the surfactant type sealing agent, the preparation method of particle blocking agent are the same as embodiment 7;The decompression
The preparation method of injection agent and embodiment 7 difference lies in:Replace (Z) -3 using dimethyl ketone oxime, 3,4- trimethyls-piperazinones
Oxime.
Embodiment 16 (comparative example 3)
A kind of compound profile control agent, calculates by weight, and the compound profile control agent includes surfactant type sealing agent
35 parts, 55 parts of increasing injection agent, 10 parts of particle blocking agent;
Wherein, it includes polyacrylamide, multiple crosslinking agent, modified ring paste that the surfactant type sealing agent, which prepares raw material,
Essence, m-phenylene diamine (MPD), oxygen scavenger, carboxylate gemini surfactant, the polyacrylamide are the partial hydrolysis of degree of hydrolysis 18%
Polyacrylamide, molecular weight are 14,000,000;The modified cyclodextrin is citric acid-modified beta-cyclodextrin;The multiple crosslinking agent is
Benzaldehyde, hydroquinone, the weight ratio 1 of the benzaldehyde and the hydroquinone:0.4;The oxygen scavenger is semicarbazides, Isosorbide-5-Nitrae-
Phenylene is bis- (thiocarbamide), and the weight ratio of the semicarbazides and the Isosorbide-5-Nitrae-phenylene bis- (thiocarbamides) is 1:0.72;The carboxylate
Gemini surface active agent includes carboxylate gemini surfactant A and carboxylate gemini surfactant B, the carboxylate gemini
It includes 1,3-propane sultone, absolute ethyl alcohol, p-phenylenediamine, methanol, Anhydrous potassium carbonate, bromo that surfactant A, which prepares raw material,
Dodecane, acetone;It includes 1,3-propane sultone, absolute ethyl alcohol, to benzene that the carboxylate gemini surfactant B, which prepares raw material,
Diamines, methanol, Anhydrous potassium carbonate, hexyl bromide 1 bromohexane, acetone;The carboxylate gemini surfactant A and carboxylate gemini surface
The weight ratio of activating agent B is 1:0.24;
The increasing injection agent prepare raw material include double 32 parts of octyl alkyl dimethyl ammonium chlorides, 4 parts of fluorine carbon FC-4430,
3 parts of ethoxylated dodecyl alcohol, 7 parts of ethylene diamine tetra methylene phosphonic acid sodium, (Z) -3,3 parts of 3,4- trimethyls-piperazine ketoxime, deionization
50 parts of water;
The raw material for preparing of the particle blocking agent includes 35 parts of acrylamide, 21 parts of acrylic acid, 5 parts of sodium hydroxide, zeolite 5
Part, 0.3 part of ammonium persulfate, 0.1 part, N of sodium hydrogensulfite, 0.25 part of N- methylene-bisacrylamides, lauryl
3 parts of ester, 50 parts of water;
The preparation method of the particle blocking agent includes the following steps:
The deionized water of 50 parts by weight, the sodium hydroxide of 5 parts by weight are sequentially added into reactor, after stirring evenly, are added
The acrylic acid for entering 21 parts by weight, is sufficiently stirred, and sequentially adds the lauryl esters of 3 parts by weight, 35 parts by weight
The zeolite of acrylamide, 5 parts by weight is warming up to 45 DEG C, and the N of 0.25 parts by weight is added, and N- methylene-bisacrylamides are warming up to
80 DEG C, the sodium hydrogensulfite of 0.1 parts by weight, the ammonium persulfate of 0.3 parts by weight is added, insulation reaction 2h is cooled to room temperature, shreds
Drying, is ground into powder, obtains the particle blocking agent.
The preparation method of the surfactant type sealing agent, the preparation method of increasing injection agent are the same as embodiment 7;Described
Preparation method and the embodiment 7 of grain blocking agent difference lies in:With zeolite substituting modification zeolite.
Embodiment 17 (comparative example 4)
A kind of compound profile control agent, calculates by weight, and the compound profile control agent includes surfactant type sealing agent
35 parts, 55 parts of increasing injection agent, 10 parts of particle blocking agent;
20-50 parts, 30-70 parts of increasing injection agent, 5-20 parts of particle blocking agent
A kind of compound profile control agent, by weight, the compound profile control agent include surfactant type sealing agent 35
Part, 55 parts of increasing injection agent, 10 parts of particle blocking agent;
Wherein, it includes polyacrylamide, multiple crosslinking agent, β-ring paste that the surfactant type sealing agent, which prepares raw material,
Essence, m-phenylene diamine (MPD), oxygen scavenger, carboxylate gemini surfactant, the polyacrylamide are the partial hydrolysis of degree of hydrolysis 18%
Polyacrylamide, molecular weight are 14,000,000;The multiple crosslinking agent be benzaldehyde, hydroquinone, the benzaldehyde with it is described right
The weight ratio 1 of benzenediol:0.4;The oxygen scavenger is semicarbazides, Isosorbide-5-Nitrae-phenylene is bis- (thiocarbamide), the semicarbazides and described 1,
The weight ratio of 4- phenylenes bis- (thiocarbamides) is 1:0.72;The carboxylate gemini surfactant includes that carboxylate gemini surface is lived
Property agent A and carboxylate gemini surfactant B, the carboxylate gemini surfactant A prepare raw material include 1,3-N-morpholinopropanesulfonic acid
Lactone, absolute ethyl alcohol, p-phenylenediamine, methanol, Anhydrous potassium carbonate, bromododecane, acetone;The carboxylate gemini surface-active
It includes 1,3-propane sultone, absolute ethyl alcohol, p-phenylenediamine, methanol, Anhydrous potassium carbonate, hexyl bromide 1 bromohexane, third that agent B, which prepares raw material,
Ketone;The weight ratio of the carboxylate gemini surfactant A and carboxylate gemini surfactant B is 1:0.24;
The surfactant type sealing agent by polyacrylamide, water, multiple crosslinking agent, beta-cyclodextrin, m-phenylene diamine (MPD), remove
Oxygen agent, carboxylate gemini surfactant are by weight 1:120:0.1:0.5:0.2:0.1:0.6 ratio is prepared;It is described
The preparation method of surfactant type sealing agent includes the following steps:
It is 14,000,000 that molecular weight is added into reactor, the partially hydrolyzed polyacrylamide (PHPA) of degree of hydrolysis 18%, and salinity is
The water of 125520mg/L is 5.0 with careless acid for adjusting pH value after stirring and dissolving, places 2 hours fully to cure, then successively plus
Oxygen scavenger, multiple crosslinking agent, beta-cyclodextrin, the m-phenylene diamine (MPD) for entering formula ratio after stirring evenly, are warming up to 88 DEG C, keep the temperature 30h,
60 DEG C are cooled to, the carboxylate gemini surfactant of formula ratio is added, 1h is stirred, is cooled to room temperature, the surface is obtained and lives
Property dosage form sealing agent.
Preparation method, the preparation method of carboxylate gemini surfactant B of the carboxylate gemini surfactant A is same
Embodiment 7.
The increasing injection agent prepare raw material include double 32 parts of octyl alkyl dimethyl ammonium chlorides, 4 parts of fluorine carbon FC-4430,
3 parts of ethoxylated dodecyl alcohol, 7 parts of ethylene diamine tetra methylene phosphonic acid sodium, 3 parts of dimethyl ketone oxime, 50 parts of deionized water;
The preparation method of the increasing injection agent includes the following steps:
Double octyl alkyl dimethyl ammonium chlorides of 32 parts by weight, the fluorine carbon FC- of 4 parts by weight are sequentially added into reactor
4430, the dimethyl ketone of the ethoxylated dodecyl alcohol of 3 parts by weight, the ethylene diamine tetra methylene phosphonic acid sodium of 7 parts by weight, 3 parts by weight
The deionized water of oxime, 50 parts by weight is warming up to 50 DEG C, and insulation reaction 3h is cooled to room temperature, obtains the increasing injection agent.
The raw material for preparing of the particle blocking agent includes 35 parts of acrylamide, 21 parts of acrylic acid, 5 parts of sodium hydroxide, zeolite 5
Part, 0.3 part of ammonium persulfate, 0.1 part, N of sodium hydrogensulfite, 0.25 part of N- methylene-bisacrylamides, lauryl
3 parts of ester, 50 parts of water;
The preparation method of the particle blocking agent includes the following steps:
The deionized water of 50 parts by weight, the sodium hydroxide of 5 parts by weight are sequentially added into reactor, after stirring evenly, are added
The acrylic acid for entering 21 parts by weight, is sufficiently stirred, and sequentially adds the lauryl esters of 3 parts by weight, 35 parts by weight
The zeolite of acrylamide, 5 parts by weight is warming up to 45 DEG C, and the N of 0.25 parts by weight is added, and N- methylene-bisacrylamides are warming up to
80 DEG C, the sodium hydrogensulfite of 0.1 parts by weight, the ammonium persulfate of 0.3 parts by weight is added, insulation reaction 2h is cooled to room temperature, shreds
Drying, is ground into powder, obtains the particle blocking agent.
The preparation method of the surfactant type sealing agent, the preparation method of the increasing injection agent, the particle are stifled
The preparation method of agent with embodiment 7, difference lies in beta-cyclodextrin substituting modification cyclodextrin, dimethyl ketone oxime replaces (Z)-
3,3,4- trimethyls-piperazine ketoxime, zeolite substituting modification zeolite.
Performance test:
1, thermodynamic stability measures:The compound profile control agent system that embodiment 7-17 is prepared is respectively placed in 90 DEG C of perseverance
In tepidarium, the layering and precipitating and homogeneous transparent situation of system are observed;
Thermodynamic stability is good:Uniformly, transparent, be not layered;
Thermodynamic stability is general:Uniformly, there is some muddiness, be not layered;
Thermodynamic stability is poor:Uneven, opaque, layering.
2, increasing injection ability measurement:Water drive before and after injecting the compound profile control agent slugs of 0.2PV is measured using core experiment
Injection pressure after pressure stability.
3, oil recovery factor ability measurement is improved:It is continuously injected into compound profile control agent and injection using core experiment measurement
The compound profile control agent slugs of 0.2PV improve recovery ratio ability.
1 the performance test results of table
It is seen from the above data that the present invention provides a kind of compound profile control agent, carry out water plugging and profiling technology and decompression
Increase water injection technology has combination, has preferable thermodynamic stability, realizes that the water blockoff in water logging crack is adjusted, improves matrix reservoirs
Water injection rate improves the oil displacement efficiency of heterogeneous reservoir.
Embodiment 18
A kind of compound profile control agent, by weight, the compound profile control agent include surfactant type sealing agent 40
Part, 50 parts of increasing injection agent, 20 parts of particle blocking agent;
Wherein, it includes polyacrylamide, multiple crosslinking agent, modified ring paste that the surfactant type sealing agent, which prepares raw material,
Essence, m-phenylene diamine (MPD), oxygen scavenger, carboxylate gemini surfactant, the polyacrylamide, water, multiple crosslinking agent, citric acid
Modified beta-cyclodextrin, m-phenylene diamine (MPD), oxygen scavenger, carboxylate gemini surfactant weight ratio be 1:110:0.12:0.8:
0.3:0.2:1.0.
The polyacrylamide is the partially hydrolyzed polyacrylamide (PHPA) of degree of hydrolysis 18%, and molecular weight is 14,000,000;It is described to change
Property cyclodextrin be citric acid-modified beta-cyclodextrin;The multiple crosslinking agent is benzaldehyde, hydroquinone by weight 1:0.3 ratio
Example mixes;The oxygen scavenger is that semicarbazides, Isosorbide-5-Nitrae-phenylene bis- (thiocarbamides) are 1 by weight:0.3 ratio mixing and
At;The carboxylate gemini surfactant includes carboxylate gemini surfactant A and carboxylate gemini surfactant B,
It includes 1,3-propane sultone, absolute ethyl alcohol, p-phenylenediamine, methanol, nothing that the carboxylate gemini surfactant A, which prepares raw material,
Aqueous carbonate potassium, bromododecane, acetone;The carboxylate gemini surfactant B prepare raw material include 1,3-propane sultone,
Absolute ethyl alcohol, p-phenylenediamine, methanol, Anhydrous potassium carbonate, hexyl bromide 1 bromohexane, acetone;The carboxylate gemini surfactant A and carboxylic
The weight ratio of hydrochlorate Gemini surface active agent B is 1:0.4;
The preparation method of the surfactant type sealing agent includes the following steps:
It is 14,000,000 that molecular weight is added into reactor, the partially hydrolyzed polyacrylamide (PHPA) of degree of hydrolysis 18%, and salinity is
The water of 125520mg/L is 5.0 with careless acid for adjusting pH value after stirring and dissolving, places 2 hours fully to cure, then successively plus
Oxygen scavenger, multiple crosslinking agent, citric acid-modified beta-cyclodextrin, the m-phenylene diamine (MPD) for entering formula ratio, after stirring evenly, are warming up to 88
DEG C, 30h is kept the temperature, is cooled to 60 DEG C, the carboxylate gemini surfactant of formula ratio is added, 1h is stirred, is cooled to room temperature, obtains
The surfactant type sealing agent.
The citric acid-modified beta-cyclodextrin is by citric acid, sodium hypophosphite, deionized water, beta-cyclodextrin, absolute ethyl alcohol
By weight 1:0.1:1:0.8:3 compositions;The preparation method of the citric acid-modified beta-cyclodextrin includes the following steps:To reaction
The citric acid of formula ratio, sodium hypophosphite, deionized water are sequentially added in device, beta-cyclodextrin is added after being completely dissolved in stirring, rises
Temperature is warming up to 110 DEG C to 80 DEG C, insulation reaction 2h, and insulation reaction 6h is cooled to room temperature, is slowly dropped to the anhydrous of formula ratio
In ethyl alcohol, after being added dropwise, 2h is stirred, filtering, 60 DEG C are dried under reduced pressure 16h.
The carboxylate gemini surfactant A is by 1,3-propane sultone, absolute ethyl alcohol, p-phenylenediamine, methanol, anhydrous
Potassium carbonate, bromododecane, acetone are by weight 1:4:0.4:8:1:0.8:3 ratio is prepared;The carboxylate gemini
The preparation method of surfactant A includes the following steps:
The 1,3-propane sultone of formula ratio, absolute ethyl alcohol, p-phenylenediamine are sequentially added into reactor, are stirred, heating
To 60 DEG C, insulation reaction 20h is concentrated to dryness, and sequentially adds the methanol, Anhydrous potassium carbonate, bromododecane of formula ratio,
70 DEG C, insulation reaction 30h are warming up to, filtering, filtrate decompression is concentrated to dryness, and the acetone that formula ratio is added is recrystallized, 60 DEG C
It is dried under reduced pressure 10h, obtains the carboxylate gemini surfactant A.
The carboxylate gemini surfactant B is by 1,3-propane sultone, absolute ethyl alcohol, p-phenylenediamine, methanol, anhydrous
Potassium carbonate, hexyl bromide 1 bromohexane, acetone are 1 by weight:7:0.6:12:1.3:1.1:6 ratio is prepared;The carboxylate is double
The preparation method of sub- surfactant B includes the following steps:
The 1,3-propane sultone of formula ratio, absolute ethyl alcohol, p-phenylenediamine are sequentially added into reactor, are stirred, heating
To 60 DEG C, insulation reaction 20h is concentrated to dryness, and sequentially adds the methanol, Anhydrous potassium carbonate, hexyl bromide 1 bromohexane of formula ratio, is risen
Temperature is to 70 DEG C, insulation reaction 30h, and filtering, filtrate decompression is concentrated to dryness, and the acetone that formula ratio is added is recrystallized, and 60 DEG C subtract
Dry 10h is pressed dry, the carboxylate gemini surfactant B is obtained.
The increasing injection agent prepare raw material include double 35 parts of octyl alkyl dimethyl ammonium chlorides, 7 parts of fluorine carbon FC-4430,
5 parts of ethoxylated dodecyl alcohol, 10 parts of ethylene diamine tetra methylene phosphonic acid sodium, (Z) -3,5 parts of 3,4- trimethyls-piperazine ketoxime, go from
57 parts of sub- water;
The preparation method of the increasing injection agent includes the following steps:
Double octyl alkyl dimethyl ammonium chlorides of 35 parts by weight, the fluorine carbon FC- of 7 parts by weight are sequentially added into reactor
4430, the ethoxylated dodecyl alcohol of 5 parts by weight, the ethylene diamine tetra methylene phosphonic acid sodium of 10 parts by weight, 5 parts by weight (Z) -3,3,
The deionized water of 4- trimethyls-piperazine ketoxime, 57 parts by weight is warming up to 50 DEG C, and insulation reaction 3h is cooled to room temperature, obtains institute
State increasing injection agent.
The raw material for preparing of the particle blocking agent includes 50 parts of acrylamide, 20 parts of acrylic acid, 10 parts of sodium hydroxide, acrylic acid
8 parts of modified zeolite, 0.5 part of ammonium persulfate, 0.2 part, N of sodium hydrogensulfite, 0.4 part of N- methylene-bisacrylamides, metering system
5 parts of sour dodecane ester, 60 parts of water;
The preparation method of the particle blocking agent includes the following steps:
The deionized water of 60 parts by weight, the sodium hydroxide of 10 parts by weight are sequentially added into reactor, after stirring evenly, are added
The acrylic acid for entering 20 parts by weight, is sufficiently stirred, and sequentially adds the lauryl esters of 5 parts by weight, 50 parts by weight
The acrylic acid modified zeolite of acrylamide, 8 parts by weight is warming up to 45 DEG C, and the N of 0.4 parts by weight, N- methylene bisacrylamide acyls is added
Amine is warming up to 80 DEG C, and the sodium hydrogensulfite of 0.2 parts by weight, the ammonium persulfate of 0.5 parts by weight is added, and insulation reaction 2h is cooled to
Room temperature shreds drying, is ground into powder, obtains the particle blocking agent.
The acrylic acid modified zeolite is 100 by weight by zeolite powder, acrylic acid and dibenzoyl peroxide (BPO):
20:0.2 ratio is prepared;The preparation method of the acrylic acid modified zeolite includes the following steps:
It is in 60 DEG C of mixing machines, by weight addition acrylic acid and dibenzoyl peroxide that barrel temperature, which is added, in zeolite powder
(BPO), after stirring 2h, discharging after mixing machine barrel temperature is risen to 120 DEG C, above-mentioned material is refunded in mixing machine, high-speed stirring
It discharges after mixing 1h, obtains acrylic acid modified zeolite.
Embodiment 19
A kind of compound profile control agent, by weight, the compound profile control agent include surfactant type sealing agent 30
Part, 40 parts of increasing injection agent, 5 parts of particle blocking agent;
Wherein, it includes polyacrylamide, multiple crosslinking agent, modified ring paste that the surfactant type sealing agent, which prepares raw material,
Essence, m-phenylene diamine (MPD), oxygen scavenger, carboxylate gemini surfactant, the polyacrylamide, water, multiple crosslinking agent, citric acid change
Property beta-cyclodextrin, m-phenylene diamine (MPD), oxygen scavenger, carboxylate gemini surfactant weight ratio be 1:131:0.09:0.6:0.25:
0.15:0.95.
The citric acid-modified beta-cyclodextrin is by citric acid, sodium hypophosphite, deionized water, beta-cyclodextrin, absolute ethyl alcohol
By weight 1:0.2:2:0.95:5 compositions;The polyacrylamide is the partially hydrolyzed polyacrylamide (PHPA) of degree of hydrolysis 18%, point
Son amount is 14,000,000;The modified cyclodextrin is citric acid-modified beta-cyclodextrin;The multiple crosslinking agent is benzaldehyde, to benzene two
Phenol is by weight 1:0.45 ratio mixes;The oxygen scavenger be semicarbazides, Isosorbide-5-Nitrae-phenylene bis- (thiocarbamides) by weight
It is 1:1.3 ratio mixes;The carboxylate gemini surfactant includes carboxylate gemini surfactant A and carboxylic acid
Salt Gemini surface active agent B, it includes 1,3-propane sultone, anhydrous second that the carboxylate gemini surfactant A, which prepares raw material,
Alcohol, p-phenylenediamine, methanol, Anhydrous potassium carbonate, bromododecane, acetone;The carboxylate gemini surfactant B prepares raw material
Including 1,3-propane sultone, absolute ethyl alcohol, p-phenylenediamine, methanol, Anhydrous potassium carbonate, hexyl bromide 1 bromohexane, acetone;The carboxylate
The weight ratio of Gemini surface active agent A and carboxylate gemini surfactant B is 1:0.5;
The preparation method of the surfactant type sealing agent includes the following steps:
It is 14,000,000 that molecular weight is added into reactor, the partially hydrolyzed polyacrylamide (PHPA) of degree of hydrolysis 18%, and salinity is
The water of 125520mg/L is 5.0 with careless acid for adjusting pH value after stirring and dissolving, places 2 hours fully to cure, then successively plus
Oxygen scavenger, multiple crosslinking agent, citric acid-modified beta-cyclodextrin, the m-phenylene diamine (MPD) for entering formula ratio, after stirring evenly, are warming up to 88
DEG C, 30h is kept the temperature, is cooled to 60 DEG C, the carboxylate gemini surfactant of formula ratio is added, 1h is stirred, is cooled to room temperature, obtains
The surfactant type sealing agent.
The citric acid-modified beta-cyclodextrin is by citric acid, sodium hypophosphite, deionized water, beta-cyclodextrin, absolute ethyl alcohol
By weight 1:0.3:3:1:6 compositions;The preparation method of the citric acid-modified beta-cyclodextrin includes the following steps:
The citric acid of formula ratio, sodium hypophosphite, deionized water are sequentially added into reactor, after stirring is completely dissolved plus
Enter beta-cyclodextrin, be warming up to 80 DEG C, insulation reaction 2h, be warming up to 110 DEG C, insulation reaction 6h is cooled to room temperature, is slowly dropped to
In the absolute ethyl alcohol of formula ratio, after being added dropwise, 2h is stirred, filtering, 60 DEG C are dried under reduced pressure 16h, obtain the citric acid-modified
Beta-cyclodextrin.
The carboxylate gemini surfactant A is by 1,3-propane sultone, absolute ethyl alcohol, p-phenylenediamine, methanol, anhydrous
Potassium carbonate, bromododecane, acetone are by weight 1:8:0.7:12:1.3:1.2:6 ratio is prepared;The carboxylate is double
The preparation method of sub- surfactant A includes the following steps:
The 1,3-propane sultone of formula ratio, absolute ethyl alcohol, p-phenylenediamine are sequentially added into reactor, are stirred, heating
To 60 DEG C, insulation reaction 20h is concentrated to dryness, and sequentially adds the methanol, Anhydrous potassium carbonate, bromododecane of formula ratio,
70 DEG C, insulation reaction 30h are warming up to, filtering, filtrate decompression is concentrated to dryness, and the acetone that formula ratio is added is recrystallized, 60 DEG C
It is dried under reduced pressure 10h, obtains the carboxylate gemini surfactant A.
The carboxylate gemini surfactant B is by 1,3-propane sultone, absolute ethyl alcohol, p-phenylenediamine, methanol, anhydrous
Potassium carbonate, hexyl bromide 1 bromohexane, acetone are 1 by weight:4:0.4:9:1:0.9:3 ratio is prepared;The carboxylate gemini
The preparation method of surfactant B includes the following steps:
The 1,3-propane sultone of formula ratio, absolute ethyl alcohol, p-phenylenediamine are sequentially added into reactor, are stirred, heating
To 60 DEG C, insulation reaction 20h is concentrated to dryness, and sequentially adds the methanol, Anhydrous potassium carbonate, hexyl bromide 1 bromohexane of formula ratio, is risen
Temperature is to 70 DEG C, insulation reaction 30h, and filtering, filtrate decompression is concentrated to dryness, and the acetone that formula ratio is added is recrystallized, and 60 DEG C subtract
Dry 10h is pressed dry, the carboxylate gemini surfactant B is obtained.
The increasing injection agent prepare raw material include double 30 parts of octyl alkyl dimethyl ammonium chlorides, 3 parts of fluorine carbon FC-4430,
3 parts of ethoxylated dodecyl alcohol, 5 parts of ethylene diamine tetra methylene phosphonic acid sodium, (Z) -3,2 parts of 3,4- trimethyls-piperazine ketoxime, deionization
38 parts of water;
The preparation method of the increasing injection agent includes the following steps:
Double octyl alkyl dimethyl ammonium chlorides of 30 parts by weight, the fluorine carbon FC- of 3 parts by weight are sequentially added into reactor
4430, the ethoxylated dodecyl alcohol of 3 parts by weight, the ethylene diamine tetra methylene phosphonic acid sodium of 5 parts by weight, 2 parts by weight (Z) -3,3,
The deionized water of 4- trimethyls-piperazine ketoxime, 38 parts by weight is warming up to 50 DEG C, and insulation reaction 3h is cooled to room temperature, obtains institute
State increasing injection agent.
The raw material for preparing of the particle blocking agent includes 20 parts of acrylamide, 35 parts of acrylic acid, 8 parts of sodium hydroxide, acrylic acid
2 parts of modified zeolite, 0.1 part of ammonium persulfate, 0.05 part, N of sodium hydrogensulfite, 0.1 part of N- methylene-bisacrylamides, metering system
2 parts of sour dodecane ester, 40 parts of water;
The preparation method of the particle blocking agent includes the following steps:
The deionized water of 40 parts by weight, the sodium hydroxide of 8 parts by weight are sequentially added into reactor, after stirring evenly, are added
The acrylic acid for entering 35 parts by weight, is sufficiently stirred, and sequentially adds the lauryl esters of 2 parts by weight, 20 parts by weight
The acrylic acid modified zeolite of acrylamide, 2 parts by weight is warming up to 45 DEG C, and the N of 0.1 parts by weight, N- methylene bisacrylamide acyls is added
Amine is warming up to 80 DEG C, and the sodium hydrogensulfite of 0.05 parts by weight, the ammonium persulfate of 0.1 parts by weight, insulation reaction 2h, cooling is added
To room temperature, drying is shredded, powder is ground into, obtains the particle blocking agent.
The acrylic acid modified zeolite is 100 by weight by zeolite powder, acrylic acid and dibenzoyl peroxide (BPO):
12:0.13 ratio is prepared;The preparation method of the acrylic acid modified zeolite includes the following steps:Zeolite powder is added and is expected
Barrel temperature is, by weight acrylic acid and dibenzoyl peroxide (BPO) is added, after stirring 2h, to discharge in 60 DEG C of mixing machines,
After mixing machine barrel temperature rises to 120 DEG C, above-mentioned material is refunded in mixing machine, discharges after high-speed stirred 1h, obtains acrylic acid
Modified zeolite.
Embodiment 20
A kind of compound profile control agent, by weight, the compound profile control agent include surfactant type sealing agent 55
Part, 60 parts of increasing injection agent, 8 parts of particle blocking agent;
Wherein, it includes polyacrylamide, multiple crosslinking agent, modified ring paste that the surfactant type sealing agent, which prepares raw material,
Essence, m-phenylene diamine (MPD), oxygen scavenger, carboxylate gemini surfactant, the polyacrylamide, water, multiple crosslinking agent, citric acid change
Property beta-cyclodextrin, m-phenylene diamine (MPD), oxygen scavenger, carboxylate gemini surfactant weight ratio be 1:115:0.05:0.2:0.1:
0.05:0.3.
The polyacrylamide is the partially hydrolyzed polyacrylamide (PHPA) of degree of hydrolysis 18%, and molecular weight is 14,000,000;It is described to change
Property cyclodextrin be citric acid-modified beta-cyclodextrin;The multiple crosslinking agent is benzaldehyde, hydroquinone by weight 1:0.6 ratio
Example mixes;The oxygen scavenger is that semicarbazides, Isosorbide-5-Nitrae-phenylene bis- (thiocarbamides) are 1 by weight:2 ratio mixes;
The carboxylate gemini surfactant includes carboxylate gemini surfactant A and carboxylate gemini surfactant B, described
It includes 1,3-propane sultone, absolute ethyl alcohol, p-phenylenediamine, methanol, anhydrous carbon that carboxylate gemini surfactant A, which prepares raw material,
Sour potassium, bromododecane, acetone;The carboxylate gemini surfactant B prepare raw material include 1,3-propane sultone, it is anhydrous
Ethyl alcohol, p-phenylenediamine, methanol, Anhydrous potassium carbonate, hexyl bromide 1 bromohexane, acetone;The carboxylate gemini surfactant A and carboxylate
The weight ratio of Gemini surface active agent B is 1:0.7;
The preparation method of the surfactant type sealing agent includes the following steps:
It is 14,000,000 that molecular weight is added into reactor, the partially hydrolyzed polyacrylamide (PHPA) of degree of hydrolysis 18%, and salinity is
The water of 125520mg/L is 5.0 with careless acid for adjusting pH value after stirring and dissolving, places 2 hours fully to cure, then successively plus
Oxygen scavenger, multiple crosslinking agent, citric acid-modified beta-cyclodextrin, the m-phenylene diamine (MPD) for entering formula ratio, after stirring evenly, are warming up to 88
DEG C, 30h is kept the temperature, is cooled to 60 DEG C, the carboxylate gemini surfactant of formula ratio is added, 1h is stirred, is cooled to room temperature, obtains
The surfactant type sealing agent.
The citric acid-modified beta-cyclodextrin is by citric acid, sodium hypophosphite, deionized water, beta-cyclodextrin, absolute ethyl alcohol
By weight 1:0.15:2:0.5:4 compositions;The preparation method of the citric acid-modified beta-cyclodextrin includes the following steps:
The citric acid of formula ratio, sodium hypophosphite, deionized water are sequentially added into reactor, after stirring is completely dissolved plus
Enter beta-cyclodextrin, be warming up to 80 DEG C, insulation reaction 2h, be warming up to 110 DEG C, insulation reaction 6h is cooled to room temperature, is slowly dropped to
In the absolute ethyl alcohol of formula ratio, after being added dropwise, 2h is stirred, filtering, 60 DEG C are dried under reduced pressure 16h, obtain the citric acid-modified
Beta-cyclodextrin.
The carboxylate gemini surfactant A is by 1,3-propane sultone, absolute ethyl alcohol, p-phenylenediamine, methanol, anhydrous
Potassium carbonate, bromododecane, acetone are by weight 1:5:0.3:9:1.1:0.9:5 ratio is prepared;The carboxylate is double
The preparation method of sub- surfactant A includes the following steps:
The 1,3-propane sultone of formula ratio, absolute ethyl alcohol, p-phenylenediamine are sequentially added into reactor, are stirred, heating
To 60 DEG C, insulation reaction 20h is concentrated to dryness, and sequentially adds the methanol, Anhydrous potassium carbonate, bromododecane of formula ratio,
70 DEG C, insulation reaction 30h are warming up to, filtering, filtrate decompression is concentrated to dryness, and the acetone that formula ratio is added is recrystallized, 60 DEG C
It is dried under reduced pressure 10h, obtains the carboxylate gemini surfactant A.
The carboxylate gemini surfactant B is by 1,3-propane sultone, absolute ethyl alcohol, p-phenylenediamine, methanol, anhydrous
Potassium carbonate, hexyl bromide 1 bromohexane, acetone are 1 by weight:5:0.5:10:1.1:1.0:5 ratio is prepared;The carboxylate is double
The preparation method of sub- surfactant B includes the following steps:
The 1,3-propane sultone of formula ratio, absolute ethyl alcohol, p-phenylenediamine are sequentially added into reactor, are stirred, heating
To 60 DEG C, insulation reaction 20h is concentrated to dryness, and sequentially adds the methanol, Anhydrous potassium carbonate, hexyl bromide 1 bromohexane of formula ratio, is risen
Temperature is to 70 DEG C, insulation reaction 30h, and filtering, filtrate decompression is concentrated to dryness, and the acetone that formula ratio is added is recrystallized, and 60 DEG C subtract
Dry 10h is pressed dry, the carboxylate gemini surfactant B is obtained.
The increasing injection agent prepare raw material include double 33 parts of octyl alkyl dimethyl ammonium chlorides, 5 parts of fluorine carbon FC-4430,
4 parts of ethoxylated dodecyl alcohol, 8 parts of ethylene diamine tetra methylene phosphonic acid sodium, (Z) -3,2 parts of 3,4- trimethyls-piperazine ketoxime, deionization
47 parts of water;
The preparation method of the increasing injection agent includes the following steps:
The fluorine carbon FC- of double 57 parts by weight of octyl alkyl dimethyl ammonium chloride of 33 parts by weight is sequentially added into reactor
4430, the ethoxylated dodecyl alcohol of 4 parts by weight, the ethylene diamine tetra methylene phosphonic acid sodium of 8 parts by weight, 2 parts by weight (Z) -3,3,
The deionized water of 4- trimethyls-piperazine ketoxime, 47 parts by weight is warming up to 50 DEG C, and insulation reaction 3h is cooled to room temperature, obtains institute
State increasing injection agent.
The raw material for preparing of the particle blocking agent includes 30 parts of acrylamide, 50 parts of acrylic acid, 4 parts of sodium hydroxide, acrylic acid
10 parts of modified zeolite, 0.4 part of ammonium persulfate, 0.15 part, N of sodium hydrogensulfite, 0.3 part of N- methylene-bisacrylamides, methyl-prop
4 parts of olefin(e) acid dodecane ester, 55 parts of water;
The preparation method of the particle blocking agent includes the following steps:
The deionized water of 55 parts by weight, the sodium hydroxide of 4 parts by weight are sequentially added into reactor, after stirring evenly, are added
The acrylic acid for entering 50 parts by weight, is sufficiently stirred, and sequentially adds the lauryl esters of 4 parts by weight, 30 parts by weight
The acrylic acid modified zeolite of acrylamide, 10 parts by weight is warming up to 45 DEG C, and the N of 0.3 parts by weight, N- methylene bisacrylamides is added
Amide is warming up to 80 DEG C, and the sodium hydrogensulfite of 0.15 parts by weight, the ammonium persulfate of 0.4 parts by weight, insulation reaction 2h, drop is added
It warms to room temperature, shreds drying, be ground into powder, obtain the particle blocking agent.
The acrylic acid modified zeolite is 100 by weight by zeolite powder, acrylic acid and dibenzoyl peroxide (BPO):
15:0.16 ratio is prepared;The preparation method of the acrylic acid modified zeolite includes the following steps:Zeolite powder is added and is expected
Barrel temperature is, by weight acrylic acid and dibenzoyl peroxide (BPO) is added, after stirring 2h, to discharge in 60 DEG C of mixing machines,
After mixing machine barrel temperature rises to 120 DEG C, above-mentioned material is refunded in mixing machine, discharges after high-speed stirred 1h, obtains acrylic acid
Modified zeolite.
Above-mentioned example is merely illustrative, some features for explaining the method for the invention.Appended right is wanted
The range as wide as possible for being intended to require to be contemplated that is sought, and embodiments as presented herein is only according to all possible implementation
The explanation of the embodiment of the selection of the combination of example.Therefore, the purpose of applicant is that the attached claims are not illustrated this hair
The exemplary selectional restriction of bright feature.Some numberical ranges used also include sub- model in the claims
It encloses, the variation in these ranges should also be construed to be covered by the attached claims in the conceived case.
Claims (10)
1. a kind of compound profile control agent, it is characterised in that:By weight, the compound profile control agent includes surfactant type
20-50 parts of sealing agent, 30-70 parts of increasing injection agent, 5-20 parts of particle blocking agent;Wherein, the surfactant type sealing agent by
Polyacrylamide, water, multiple crosslinking agent, modified cyclodextrin, m-phenylene diamine (MPD), oxygen scavenger and carboxylate gemini surfactant are by weight
Measure ratio 1:(110-131):(0.05-0.12):(0.2-0.8):(0.1-0.3):(0.05-0.2):It is prepared by the ratio of (0.3-1)
It forms.
2. a kind of compound profile control agent according to claim 1, it is characterised in that:The raw material group of the increasing injection agent
At, by weight, including 30-35 parts of double octyl alkyl dimethyl ammonium chlorides, 3-7 parts of fluorocarbon surfactant, non-ionic surface
3-5 parts of activating agent, 5-10 parts of ethylene diamine tetra methylene phosphonic acid sodium, (Z) -3,2-5 parts of 3,4- trimethyls-piperazine ketoxime, deionized water
38-57 parts;Wherein, the fluorocarbon surfactant is fluorine carbon FC-4430, and the nonionic surfactant is laruyl alcohol polyoxy
Vinethene.
3. a kind of compound profile control agent according to claim 1, it is characterised in that:The raw material of the particle blocking agent forms,
By weight, including 20-50 parts of acrylamide, 20-50 parts of acrylic acid, 1-15 parts of sodium hydroxide, 2-10 parts of modified zeolite, mistake
0.1-0.5 parts of ammonium sulfate, 0.05-0.25 parts, N of sodium hydrogensulfite, 0.1-0.5 parts of N- methylene-bisacrylamides, metering system
1-5 parts of sour dodecane ester, 40-60 parts of water;
The modified zeolite is acrylic acid modified zeolite, and the acrylic acid modified zeolite is by zeolite powder, acrylic acid, diphenyl peroxide
Formyl is by weight 100:(12-20):(0.13-0.2) is formed, and preparation method includes the following steps:Zeolite powder is added and is expected
Barrel temperature is, by weight acrylic acid and dibenzoyl peroxide is added, after stirring 2-3h, to discharge in 50-70 DEG C of mixing machine,
After mixing machine barrel temperature rises to 110-120 DEG C, above-mentioned material is refunded in mixing machine, discharges, obtains after high-speed stirred 1-2h
Acrylic acid modified zeolite.
4. a kind of compound profile control agent according to claim 1, it is characterised in that:The surfactant type sealing agent
Preparation method includes the following steps:The polyacrylamide and water of formula ratio are added first into reactor, after stirring and dissolving, with grass
Acid for adjusting pH value is 5.0, places 1-3h fully to cure;Then the oxygen scavenger, multiple crosslinking agent, modification of formula ratio are sequentially added
Cyclodextrin, m-phenylene diamine (MPD) after stirring evenly, are warming up to 80-90 DEG C, after keeping the temperature 20-40h, then are cooled to 55-60 DEG C, addition is matched
The carboxylate gemini surfactant just measured stirs 1-2h, is cooled to room temperature to get the surfactant type sealing agent.
5. a kind of compound profile control agent according to claim 1, it is characterised in that:The modified cyclodextrin changes for citric acid
Property beta-cyclodextrin, the citric acid-modified beta-cyclodextrin is by citric acid, sodium hypophosphite, deionized water, beta-cyclodextrin and anhydrous
Ethyl alcohol is by weight 1:(0.1-0.3):(1-3):(0.5-1):(3-6) is formed;The preparation of the citric acid-modified beta-cyclodextrin
Method includes the following steps:By weight citric acid, sodium hypophosphite and deionized water is sequentially added into reactor, stir
After fully dissolved, the beta-cyclodextrin of formula ratio is added, is warming up to 70-80 DEG C, insulation reaction 2-3h, then be warming up to 100-110 DEG C, protects
Temperature reaction 4-6h, is then cooled to room temperature, is slowly dropped in the absolute ethyl alcohol of formula ratio, after being added dropwise, stirs 1-2h, mistake
Filter, 60 DEG C are dried under reduced pressure 16-20h, obtain the citric acid-modified beta-cyclodextrin.
6. a kind of compound profile control agent according to claim 1, it is characterised in that:The carboxylate gemini surfactant
By carboxylate gemini surfactant A and carboxylate gemini surfactant B by weight 1:The ratio of (0.1-0.7) mix and
At.
7. a kind of compound profile control agent according to claim 6, it is characterised in that:The carboxylate gemini surfactant
A is by 1,3-propane sultone, absolute ethyl alcohol, p-phenylenediamine, methanol, Anhydrous potassium carbonate, bromododecane, acetone by weight 1:
(4-8):(0.3-0.7):(8-12):(1-1.3):(0.8-1.2):The ratio of (3-6) is prepared;
The preparation method of the carboxylate gemini surfactant A includes the following steps:It sequentially adds and matches into reactor first
The 1,3-propane sultone just measured, absolute ethyl alcohol, p-phenylenediamine, stirring are warming up to 55-60 DEG C, insulation reaction 20-25h, decompression
It is concentrated to dryness;Then the methanol, Anhydrous potassium carbonate, bromododecane for sequentially adding formula ratio are warming up to 60-70 DEG C, and heat preservation is anti-
30-35h is answered, is filtered, filtrate decompression is concentrated to dryness;The acetone for being eventually adding formula ratio is recrystallized, and 60 DEG C are dried under reduced pressure 10-
12h obtains the carboxylate gemini surfactant A.
8. a kind of compound profile control agent according to claim 6, it is characterised in that:The carboxylate gemini surfactant
B prepare raw material include 1,3-propane sultone, absolute ethyl alcohol, p-phenylenediamine, methanol, Anhydrous potassium carbonate, hexyl bromide 1 bromohexane, acetone by
Weight ratio 1:(4-7):(0.4-0.6):(9-12):(1-1.3):(0.9-1.1):The ratio of (3-6) is prepared;
The preparation method of the carboxylate gemini surfactant B includes the following steps:It sequentially adds and matches into reactor first
The 1,3-propane sultone just measured, absolute ethyl alcohol, p-phenylenediamine, stirring are warming up to 55-60 DEG C, insulation reaction 20-25h, decompression
It is concentrated to dryness;Then the methanol, Anhydrous potassium carbonate, hexyl bromide 1 bromohexane for sequentially adding formula ratio, are warming up to 60-70 DEG C, insulation reaction
30-35h, filtering, filtrate decompression are concentrated to dryness;The acetone for being eventually adding formula ratio is recrystallized, and 60 DEG C are dried under reduced pressure 10-
12h obtains the carboxylate gemini surfactant B.
9. a kind of compound profile control agent according to claim 1, it is characterised in that:The multiple crosslinking agent by benzaldehyde and
Benzenediol is by weight 1:The ratio of (0.3-0.6) mixes.
10. a kind of compound profile control agent according to claim 1, it is characterised in that:The oxygen scavenger includes thiocarbamide, 2,4-
It is one or more in dithiobiuret, semicarbazides, thiosemicarbazide, Isosorbide-5-Nitrae-phenylene bis- (thiocarbamides).
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