CN106590577A - Foam composition and preparation method of the same - Google Patents
Foam composition and preparation method of the same Download PDFInfo
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- CN106590577A CN106590577A CN201510683608.3A CN201510683608A CN106590577A CN 106590577 A CN106590577 A CN 106590577A CN 201510683608 A CN201510683608 A CN 201510683608A CN 106590577 A CN106590577 A CN 106590577A
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- 238000002360 preparation method Methods 0.000 title claims abstract description 46
- 239000006260 foam Substances 0.000 title claims abstract description 36
- 239000000203 mixture Substances 0.000 title claims abstract description 13
- 239000004721 Polyphenylene oxide Substances 0.000 claims abstract description 40
- 229920000570 polyether Polymers 0.000 claims abstract description 40
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 17
- 125000000217 alkyl group Chemical group 0.000 claims abstract description 8
- 239000004094 surface-active agent Substances 0.000 claims abstract description 5
- 125000000129 anionic group Chemical group 0.000 claims abstract description 4
- -1 nitrogen-containing compound Chemical class 0.000 claims description 55
- 238000006243 chemical reaction Methods 0.000 claims description 54
- 239000004088 foaming agent Substances 0.000 claims description 41
- 230000015572 biosynthetic process Effects 0.000 claims description 29
- 238000003786 synthesis reaction Methods 0.000 claims description 29
- FYSNRJHAOHDILO-UHFFFAOYSA-N thionyl chloride Chemical compound ClS(Cl)=O FYSNRJHAOHDILO-UHFFFAOYSA-N 0.000 claims description 13
- 239000002585 base Substances 0.000 claims description 9
- 239000000126 substance Substances 0.000 claims description 8
- 238000012545 processing Methods 0.000 claims description 6
- QGZKDVFQNNGYKY-UHFFFAOYSA-O Ammonium Chemical compound [NH4+] QGZKDVFQNNGYKY-UHFFFAOYSA-O 0.000 claims description 4
- 229910001413 alkali metal ion Inorganic materials 0.000 claims description 4
- 229910001420 alkaline earth metal ion Inorganic materials 0.000 claims description 4
- 125000002947 alkylene group Chemical group 0.000 claims description 4
- 239000003054 catalyst Substances 0.000 claims description 4
- YCWSUKQGVSGXJO-NTUHNPAUSA-N nifuroxazide Chemical group C1=CC(O)=CC=C1C(=O)N\N=C\C1=CC=C([N+]([O-])=O)O1 YCWSUKQGVSGXJO-NTUHNPAUSA-N 0.000 claims description 4
- 239000002904 solvent Substances 0.000 claims description 4
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 claims description 2
- IAYPIBMASNFSPL-UHFFFAOYSA-N Ethylene oxide Chemical compound C1CO1 IAYPIBMASNFSPL-UHFFFAOYSA-N 0.000 claims description 2
- GOOHAUXETOMSMM-UHFFFAOYSA-N Propylene oxide Chemical compound CC1CO1 GOOHAUXETOMSMM-UHFFFAOYSA-N 0.000 claims description 2
- 150000004996 alkyl benzenes Chemical class 0.000 claims description 2
- 229910052760 oxygen Inorganic materials 0.000 claims description 2
- 229910052717 sulfur Inorganic materials 0.000 claims description 2
- QJGQUHMNIGDVPM-UHFFFAOYSA-N nitrogen group Chemical group [N] QJGQUHMNIGDVPM-UHFFFAOYSA-N 0.000 claims 2
- 229940126062 Compound A Drugs 0.000 claims 1
- NLDMNSXOCDLTTB-UHFFFAOYSA-N Heterophylliin A Natural products O1C2COC(=O)C3=CC(O)=C(O)C(O)=C3C3=C(O)C(O)=C(O)C=C3C(=O)OC2C(OC(=O)C=2C=C(O)C(O)=C(O)C=2)C(O)C1OC(=O)C1=CC(O)=C(O)C(O)=C1 NLDMNSXOCDLTTB-UHFFFAOYSA-N 0.000 claims 1
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 abstract description 34
- 229910052757 nitrogen Inorganic materials 0.000 abstract description 17
- 238000010795 Steam Flooding Methods 0.000 abstract description 7
- 238000007789 sealing Methods 0.000 abstract description 4
- 150000002500 ions Chemical class 0.000 abstract description 2
- 238000004519 manufacturing process Methods 0.000 abstract description 2
- 150000001875 compounds Chemical class 0.000 abstract 3
- 125000001118 alkylidene group Chemical group 0.000 abstract 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 47
- 239000000243 solution Substances 0.000 description 46
- 238000010992 reflux Methods 0.000 description 31
- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical compound [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 description 30
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 27
- 239000000460 chlorine Substances 0.000 description 24
- 238000009835 boiling Methods 0.000 description 23
- ATUOYWHBWRKTHZ-UHFFFAOYSA-N Propane Chemical compound CCC ATUOYWHBWRKTHZ-UHFFFAOYSA-N 0.000 description 22
- 238000005292 vacuum distillation Methods 0.000 description 22
- JUJWROOIHBZHMG-UHFFFAOYSA-N Pyridine Chemical compound C1=CC=NC=C1 JUJWROOIHBZHMG-UHFFFAOYSA-N 0.000 description 20
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical class [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 description 20
- 238000005406 washing Methods 0.000 description 20
- 239000000047 product Substances 0.000 description 19
- 238000001816 cooling Methods 0.000 description 17
- 238000006073 displacement reaction Methods 0.000 description 13
- 235000020679 tap water Nutrition 0.000 description 13
- 239000008399 tap water Substances 0.000 description 12
- JECYNCQXXKQDJN-UHFFFAOYSA-N 2-(2-methylhexan-2-yloxymethyl)oxirane Chemical compound CCCCC(C)(C)OCC1CO1 JECYNCQXXKQDJN-UHFFFAOYSA-N 0.000 description 11
- 238000004090 dissolution Methods 0.000 description 11
- 239000012467 final product Substances 0.000 description 11
- 239000007789 gas Substances 0.000 description 11
- 238000004128 high performance liquid chromatography Methods 0.000 description 11
- 239000001294 propane Substances 0.000 description 11
- 239000011734 sodium Substances 0.000 description 11
- 238000003756 stirring Methods 0.000 description 11
- 230000018044 dehydration Effects 0.000 description 10
- 238000006297 dehydration reaction Methods 0.000 description 10
- 238000001035 drying Methods 0.000 description 10
- UMJSCPRVCHMLSP-UHFFFAOYSA-N pyridine Natural products COC1=CC=CN=C1 UMJSCPRVCHMLSP-UHFFFAOYSA-N 0.000 description 10
- 239000000376 reactant Substances 0.000 description 10
- 238000013517 stratification Methods 0.000 description 10
- 238000010792 warming Methods 0.000 description 10
- 238000004458 analytical method Methods 0.000 description 9
- 238000006386 neutralization reaction Methods 0.000 description 9
- 239000003921 oil Substances 0.000 description 9
- 125000002572 propoxy group Chemical group [*]OC([H])([H])C(C([H])([H])[H])([H])[H] 0.000 description 8
- 229910052799 carbon Inorganic materials 0.000 description 7
- 238000009833 condensation Methods 0.000 description 7
- 230000005494 condensation Effects 0.000 description 7
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical group [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 6
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 description 6
- 230000000052 comparative effect Effects 0.000 description 6
- 239000007791 liquid phase Substances 0.000 description 6
- 150000002028 dodecanols Chemical class 0.000 description 5
- 125000003438 dodecyl group Chemical group [H]C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])* 0.000 description 5
- 238000005187 foaming Methods 0.000 description 5
- 239000003086 colorant Substances 0.000 description 4
- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 4
- 238000002347 injection Methods 0.000 description 4
- 239000007924 injection Substances 0.000 description 4
- 229910052500 inorganic mineral Inorganic materials 0.000 description 4
- 239000007788 liquid Substances 0.000 description 4
- 238000004088 simulation Methods 0.000 description 4
- 238000001228 spectrum Methods 0.000 description 4
- 238000012360 testing method Methods 0.000 description 4
- 125000002252 acyl group Chemical group 0.000 description 3
- 125000002915 carbonyl group Chemical group [*:2]C([*:1])=O 0.000 description 3
- 239000013067 intermediate product Substances 0.000 description 3
- 150000003839 salts Chemical class 0.000 description 3
- 235000002639 sodium chloride Nutrition 0.000 description 3
- BHPQYMZQTOCNFJ-UHFFFAOYSA-N Calcium cation Chemical compound [Ca+2] BHPQYMZQTOCNFJ-UHFFFAOYSA-N 0.000 description 2
- 238000010793 Steam injection (oil industry) Methods 0.000 description 2
- 229910001424 calcium ion Inorganic materials 0.000 description 2
- DIOQZVSQGTUSAI-UHFFFAOYSA-N decane Chemical compound CCCCCCCCCC DIOQZVSQGTUSAI-UHFFFAOYSA-N 0.000 description 2
- 239000008367 deionised water Substances 0.000 description 2
- 229910021641 deionized water Inorganic materials 0.000 description 2
- 238000011161 development Methods 0.000 description 2
- 235000014113 dietary fatty acids Nutrition 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 238000002474 experimental method Methods 0.000 description 2
- 239000000194 fatty acid Substances 0.000 description 2
- 229930195729 fatty acid Natural products 0.000 description 2
- 239000012530 fluid Substances 0.000 description 2
- 230000015784 hyperosmotic salinity response Effects 0.000 description 2
- 238000000034 method Methods 0.000 description 2
- 125000001424 substituent group Chemical group 0.000 description 2
- QEMHBAGGYKJNSS-UHFFFAOYSA-N 2-icosylphenol Chemical compound CCCCCCCCCCCCCCCCCCCCC1=CC=CC=C1O QEMHBAGGYKJNSS-UHFFFAOYSA-N 0.000 description 1
- JOONSONEBWTBLT-UHFFFAOYSA-N 2-tetradecylphenol Chemical compound CCCCCCCCCCCCCCC1=CC=CC=C1O JOONSONEBWTBLT-UHFFFAOYSA-N 0.000 description 1
- ZAMOUSCENKQFHK-UHFFFAOYSA-N Chlorine atom Chemical compound [Cl] ZAMOUSCENKQFHK-UHFFFAOYSA-N 0.000 description 1
- OTMSDBZUPAUEDD-UHFFFAOYSA-N Ethane Chemical compound CC OTMSDBZUPAUEDD-UHFFFAOYSA-N 0.000 description 1
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 1
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 description 1
- JLVVSXFLKOJNIY-UHFFFAOYSA-N Magnesium ion Chemical compound [Mg+2] JLVVSXFLKOJNIY-UHFFFAOYSA-N 0.000 description 1
- 230000003213 activating effect Effects 0.000 description 1
- 239000004480 active ingredient Substances 0.000 description 1
- 239000003513 alkali Substances 0.000 description 1
- 125000002877 alkyl aryl group Chemical group 0.000 description 1
- 150000008055 alkyl aryl sulfonates Chemical class 0.000 description 1
- 150000001450 anions Chemical class 0.000 description 1
- 239000007864 aqueous solution Substances 0.000 description 1
- 239000012752 auxiliary agent Substances 0.000 description 1
- 230000000903 blocking effect Effects 0.000 description 1
- 239000012267 brine Substances 0.000 description 1
- 125000002091 cationic group Chemical group 0.000 description 1
- 229910052801 chlorine Inorganic materials 0.000 description 1
- 238000013329 compounding Methods 0.000 description 1
- 239000006071 cream Substances 0.000 description 1
- 125000004122 cyclic group Chemical group 0.000 description 1
- 238000009792 diffusion process Methods 0.000 description 1
- 239000003792 electrolyte Substances 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000011049 filling Methods 0.000 description 1
- 239000008398 formation water Substances 0.000 description 1
- 239000012634 fragment Substances 0.000 description 1
- 125000000524 functional group Chemical group 0.000 description 1
- BXWNKGSJHAJOGX-UHFFFAOYSA-N hexadecan-1-ol Chemical class CCCCCCCCCCCCCCCCO BXWNKGSJHAJOGX-UHFFFAOYSA-N 0.000 description 1
- 230000003301 hydrolyzing effect Effects 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-M hydroxide Chemical compound [OH-] XLYOFNOQVPJJNP-UHFFFAOYSA-M 0.000 description 1
- 229910001425 magnesium ion Inorganic materials 0.000 description 1
- 125000001421 myristyl group Chemical group [H]C([*])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])[H] 0.000 description 1
- 229910017464 nitrogen compound Inorganic materials 0.000 description 1
- 150000002830 nitrogen compounds Chemical class 0.000 description 1
- 230000001590 oxidative effect Effects 0.000 description 1
- 125000000913 palmityl group Chemical group [H]C([*])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])[H] 0.000 description 1
- 230000035699 permeability Effects 0.000 description 1
- 239000012071 phase Substances 0.000 description 1
- 229920000642 polymer Polymers 0.000 description 1
- 238000001556 precipitation Methods 0.000 description 1
- 150000003242 quaternary ammonium salts Chemical class 0.000 description 1
- 238000011084 recovery Methods 0.000 description 1
- 239000004576 sand Substances 0.000 description 1
- 229910052708 sodium Inorganic materials 0.000 description 1
- HPALAKNZSZLMCH-UHFFFAOYSA-M sodium;chloride;hydrate Chemical compound O.[Na+].[Cl-] HPALAKNZSZLMCH-UHFFFAOYSA-M 0.000 description 1
- 125000000547 substituted alkyl group Chemical group 0.000 description 1
- 125000000475 sulfinyl group Chemical group [*:2]S([*:1])=O 0.000 description 1
- 239000003784 tall oil Substances 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
- C09K8/00—Compositions for drilling of boreholes or wells; Compositions for treating boreholes or wells, e.g. for completion or for remedial operations
- C09K8/58—Compositions for enhanced recovery methods for obtaining hydrocarbons, i.e. for improving the mobility of the oil, e.g. displacing fluids
- C09K8/584—Compositions for enhanced recovery methods for obtaining hydrocarbons, i.e. for improving the mobility of the oil, e.g. displacing fluids characterised by the use of specific surfactants
-
- 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
- C09K8/58—Compositions for enhanced recovery methods for obtaining hydrocarbons, i.e. for improving the mobility of the oil, e.g. displacing fluids
- C09K8/592—Compositions used in combination with generated heat, e.g. by steam injection
-
- E—FIXED CONSTRUCTIONS
- E21—EARTH OR ROCK DRILLING; MINING
- E21B—EARTH OR ROCK DRILLING; OBTAINING OIL, GAS, WATER, SOLUBLE OR MELTABLE MATERIALS OR A SLURRY OF MINERALS FROM WELLS
- E21B43/00—Methods or apparatus for obtaining oil, gas, water, soluble or meltable materials or a slurry of minerals from wells
- E21B43/16—Enhanced recovery methods for obtaining hydrocarbons
Landscapes
- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Life Sciences & Earth Sciences (AREA)
- General Life Sciences & Earth Sciences (AREA)
- Organic Chemistry (AREA)
- Materials Engineering (AREA)
- Oil, Petroleum & Natural Gas (AREA)
- Geology (AREA)
- Mining & Mineral Resources (AREA)
- Physics & Mathematics (AREA)
- Environmental & Geological Engineering (AREA)
- Fluid Mechanics (AREA)
- Geochemistry & Mineralogy (AREA)
- Polyethers (AREA)
Abstract
The invention relates to a foam composition and a preparation method of the same, mainly solving the current problems of foam agent subsiding when meeting with divalent ions and less capacity of foam sealing ,with oil production of nitrogen high salinity reservoir of steam flooding. The foam composition and the preparation method of the same based on the molecule of the compounds, comprising 1 potion of long-chain polyether compounds with nitrogen and 0.1-50 potions of the surfactant of long-chain diaryl-toluenesulfonate salt, wherein the long-chain polyether compounds with nitrogen has the general molecular formula as (I) and the the long-chain diaryl-toluenesulfonate salt has the general molecular formula as (II). The R1 refers to fatty group C10-C26; R4,R5 alkyl C1-C5 or anyone of alkyl; R6,R7 alkylidene C1-C5 or anyone of alkylidene; and Y selected from the technical scheme of the general molecular formula (I) where molecule in anionic groups is with electric neutrality. And the foam composition and the preparation method of the same solve the problems better and can also be applied to the nitrogen high salinity reservoir of steam flooding.
Description
Technical field
The present invention relates to a kind of foaming agent combination and preparation method, particularly for high salinity reservoir steam nitrogen foam combination flooding
With foaming agent combination and preparation method.
Background technology
China's viscous crude resource is quite enriched.Viscous crude has the characteristics of viscosity is high, density is big, and development difficulty increases, development effectiveness
Difference.Steam drives and cyclic steam injection tech is the Main Means for developing viscous crude at present, but due to density between steam and profit and viscosity
Difference, causes steam onlap flowing and Character of Viscous Finger in oil reservoir, the serious oil reservoir of anisotropism steamchanneling occur.
Foam assisted steam flooding is that foaming agent is added during steam injection, and foam is a kind of compressible non-Newtonian fluid,
Seepage flow has selectivity in the earth formation, and displacement is carried out in the form of aerated fluid, can selectively block high permeability zone, change
The injection profile that kind steam drives, increases sweep efficiency, effectively suppresses onlap and the channelling of steam.
The resistant to elevated temperatures foaming agent that the steam of report drives at present mainly has fatty acid sodium salt, alpha-alkene sulfonate, alkylaryl
Sulfonate etc..Such as document《Oilfield chemistry》1000-4092 (2010) 02-0196-04 provides one kind with mass fraction as 0.5%
Tall oil fatty acid sodium-salt based on agent steam drive resistant to elevated temperatures foaming agent, be applied to formation water salinity be 1500m
Gram/L, wherein in the stratum of calcium ions and magnesium ions content 15.16mg/L.For another example document US055148, CN88103174.7 are selected
Mean molecule quantity be at least 400 alkylaryl sulfonatess, alpha-alkene sulfonate, the component such as alpha-alkene sulfonate dimer
In one or more, using the agent as foaming host cause the salt resistant character of system limited, so the system be suitable for model
Enclose to include the water phase of the electrolyte of 100～50,000mg/L.
The content of the invention
One of the technical problem to be solved is that foam salt resistance ability present in existing steam drive oil production process is poor,
A kind of little problem of the foam sweep efficiency of formation, there is provided new foaming agent combination.Said composition is with salinity
Steam nitrogen foam will not be formed there is good stability, resistance with ion precipitation under the stratum water condition of 0～300000mg/L
The advantages of factor is high.
The two of the technical problem to be solved are to provide a kind of foam combination corresponding with technical problem one is solved
The preparation method of thing.
To solve one of above-mentioned technical problem, the technical solution used in the present invention is as follows：A kind of foaming agent combination, with mole
Number meter includes the long-chain diaryl sulfosalt surfactant of 1 part of long-chain polyether nitrogen-containing compound and 0.1～50 part；
Wherein, the long-chain polyether nitrogen-containing compound, with the general molecular formula shown in formula (I)：
Formula (I)；
The long-chain diaryl sulfosalt surfactant, with the general molecular formula shown in formula (II)：
Formula (II)；
In formula (I), the R1For C10～C26Fat-based；Y=0～20, z=0～60；R4、R5For C1～C5Alkyl, take
Any one in substituted alkyl；R6、R7For C1～C5Alkylidene, any one in substituted alkylene；Y is selected from and makes formula
(I) molecule shown in is in electroneutral anionic group；In formula (II), the R2For C10～C26Fat-based；It is described
R3For H or C1～C26Fat-based；N, m are 0～3 integer or decimal and n+m>1；L is O, S ,-(CH2)1-3-、
-OC2H4O-、-OC3H6One kind in O-；X is the one kind in alkali metal ion, alkaline-earth metal ions or ammonium ion, and is worked as
When X is alkali metal ion or ammonium ion, a=n, b=m, when X is alkaline-earth metal ions, a=n/2, b=m/2.
In above-mentioned technical proposal, the R1For C10～C26Fat-based, can be containing acyl group, carbonyl, ether, hydroxyl etc.
Group, can be saturated carbon chains, it is also possible to containing unsaturated carbon chains, as preferred R1Preferred version be C10～C20Alkane
Base, alkylbenzene.
In above-mentioned technical proposal, the R4、R5For C1～C5Alkyl, replace alkyl in any one；R6、R7For
C1～C5Alkylidene, any one in substituted alkylene；Substituent group in wherein described replacement alkyl, substituted alkylene
Can be the substituted radicals such as hydroxyl substituent, halogenic substituent.
In above-mentioned technical proposal, the R7Preferably C2H4Or C3H6。
In above-mentioned technical proposal, as long as the Y makes general molecular formula (I) in electroneutral anionic group, for example
But do not limit Y and preferably be selected from-COO—、-SO3 —、-HPO4 —In at least one, more preferably-COO—、-SO3 —
In at least one.
In above-mentioned technical proposal, the y is preferably greater than 0, z and is preferably greater than 0.
In above-mentioned technical proposal, the preferred version of the z is that 30 are less than or equal to more than 0；The preferred version of y is more than 0.
In above-mentioned technical proposal, the R2For C10～C26Fat-based, can be containing acyl group, carbonyl, ether, hydroxyl etc.
Group, can be saturated carbon chains, it is also possible to containing unsaturated carbon chains, as the preferred R2Preferred version be C12～C20
Alkyl.
In above-mentioned technical proposal, the R3For H or C1～C26Fat-based, acyl group, carbonyl, ether, hydroxyl can be contained
The groups such as base, can be saturated carbon chains, it is also possible to containing unsaturated carbon chains, as preferred R3Preferred version be H or C1～C16
Alkyl.
In above-mentioned technical proposal, the preferred version of the X is K+、Na+、NH4 +In at least one；Long-chain polyether is nitrogenous
Compound is preferably 1 with the mol ratio of long-chain diaryl sulfonate:0.2～10.
Foaming agent combination in the present invention does not have particular/special requirement to water, can be deionized water, can also be when preparing
Water containing inorganic mineral, and the water for containing inorganic mineral can be tap water, oil field stratum water or oilfield injection water.
To solve the two of above-mentioned technical problem, the technical solution used in the present invention is as follows：A kind of preparation side of foaming agent combination
Method, comprises the following steps：
(1) synthesis of long-chain polyether nitrogen-containing compound
A, in the presence of base catalyst, R1OH obtains R with aequum propylene oxide reaction1O(CHCH3CH2O)yH；
B, in the presence of base catalyst, R1O (CHCH3CH2O)yH is obtained with aequum reacting ethylene oxide
R1O(CHCH3CH2O)y(CH2CH2O)z+1H；
C, by R1O(CHCH3CH2O)y(CH2CH2O)z+1H is reacted Jing after processing with thionyl chloride and is obtained
R1O(CHCH3CH2O)y(CH2CH2O)zR7Cl；
D, by R1O(CHCH3CH2O)y(CH2CH2O)zR7Cl and NR4R5In a solvent, in 70～90 DEG C of reaction temperature
Reaction obtains R Jing after processing1O(CHCH3CH2O)y(CH2CH2O)zR7NR4R5；
E, by R1O(CHCH3CH2O)y(CH2CH2O)zR7NR4R5With ClR6Y is in a solvent in reaction temperature 70-90 DEG C
Lower reaction obtains the long-chain polyether nitrogen-containing compound Jing after processing；
(2) preparation of foaming agent combination
The desired amount of long-chain polyether nitrogen-containing compound, long-chain diaryl sulfonate mix homogeneously are obtained into the foaming agent combination.
The key active ingredient of foam of the present invention is long-chain diaryl sulfonate and long-chain polyether nitrogen-containing compound, this area skill
Art personnel know, for the ease of transport and store or onsite application etc. from the aspect of, various supply forms can be adopted, for example
Water-free solid-state form, or aqueous solid-state form, or aqueous cream form, or aqueous solution form；It is water-soluble
Liquid form includes the form that concentrated solution is made into water, is directly made into the foam form of live displacement of reservoir oil desired concn；Wherein, it is right
Water does not have particular/special requirement, can be deionized water, can also be the water containing inorganic mineral, and the water for containing inorganic mineral can
Being tap water, oil field stratum water or oilfield injection water.
Foaming agent combination of the present invention has good compatibility, can also contain other commonly used in the art inorganic agent, such as table
The oil recovery auxiliary agent such as face activating agent, polymer, alkali.
In the foaming agent combination of the present invention, long-chain diaryl sulfonate belongs to Shuangzi type from structure so that its salt tolerance has
Very big raising, the agent can keep clear in the mineralized water of salinity 300000mg/L；Long-chain polyether nitrogen
Compound is due to the functional group simultaneous with yin, yang both sexes, while also non-ionic fragment, it may have preferable salt tolerance；
After two kinds of components compounding, the anionicsite of long-chain diaryl sulfonate and the cationic moiety of long-chain polyether quaternary ammonium salt, due to
Electrostatic attraction effect between anions and canons foam opposite charges polar group so that foam agent molecule adsorbance on the surface
Increase, so as to the incomparable interface arrangement density of single foam, the diffusion of the gas of obstruction by liquid film is allowed to
It is more readily formed and stable foam.And two kinds of components all do not contain the easy group for hydrolyzing so which can apply to high salt oil
During the steam nitrogen displacement of reservoir oil of Tibetan.
The foaming agent combination of the present invention, can effectively macropore plugging, experiment finds, salinity 250000mg/L,
Under conditions of 200 DEG C, the foam resistance factor that said composition is formed achieves preferable technique effect up to 100.
Below by embodiment, the present invention is further elaborated.
Specific embodiment
In order to be better understood from the present invention, present disclosure, but present disclosure are expanded on further with reference to embodiments
It is not limited solely to the following examples.
【Embodiment 1】
The preparation of compositionss HF-1, preparation process：
(1) long-chain polyether nitrogen-containing compound (C12H25O(CHCH3CH2O)3(CH2CH2O)7CH2CH2N(CH3)2C3H6OSO3)
Synthesis with prepare：
186.0 grams of dodecanols, 5.6 grams of potassium hydroxide are added in the pressure reactor equipped with agitating device, it is heated to 80～
When 90 DEG C, vacuum system is opened, be dehydrated under a high vacuum 1 hour, then with nitrogen displacement 3～4 times, system reacted
Temperature is adjusted to 150 DEG C and is slowly passed through 179.9 grams of expoxy propane, and control pressure≤0.60MPa is cooled to 90 DEG C, is removed in vacuum
System reaction temperature is adjusted to 150 DEG C and is slowly passed through 360.0 grams of oxirane, control pressure≤0.60MPa by low-boiling-point substance, continuation.
After reaction terminates, after cooling, neutralization, dehydration, obtain C12H25O(CHCH3CH2O)3(CH2CH2O)8H, yield 98.8wt%.
339 grams are added in the four round flask equipped with reflux condensate device, thermometer, agitator and gas absorbing device
C12H25O(CHCH3CH2O)3(CH2CH2O)8H and 57 gram of pyridine, is heated to 70 DEG C under stirring, slow with Dropping funnel
85 grams of thionyl chlorides of Deca, react 10 hours after completion of dropping at 90 DEG C.After reaction terminates, reactant stood, cooled down
Upper strata is neutralized to neutrality with sodium hydroxide solution by layering, with saturated common salt water washing 5-6 time of heat, in obtaining after drying
Between product C12H25O(CHCH3CH2O)3(CH2CH2O)7CH2CH2Cl, yield are 88%.
By C12H25O(CHCH3CH2O)3(CH2CH2O)7CH2CH2143 grams of Cl is added with reflux condensate device, temperature
In degree meter, the four-hole boiling flask of agitator, 77 DEG C are heated to, by N (CH3)2Solution Dropping funnel is slowly dripped in flask,
System remains alkalescence, stratification after reacting 10 hours.By the saturated common salt washing after the vacuum distillation of upper strata with heat
Wash 5-6 time, obtain desired intermediate C12H25O(CHCH3CH2O)3(CH2CH2O)7CH2CH2N(CH3)2, yield
For 83%.
By C12H25O(CHCH3CH2O)3(CH2CH2O)7CH2CH2N(CH3)2100 grams are added to reflux condensation mode dress
Put, in the four-hole boiling flask of thermometer, agitator, be heated to 70 DEG C, be slowly added dropwise ClCH2CHOHCH2SO3Na solution
30 grams, after reacting 2 hours at 70 DEG C, it is warming up to 90 DEG C and continues reaction 6 hours, vacuum distillation, Jing high-efficient liquid phase colors
Spectrum (HPLC) analysis, C in product12H25O(CHCH3CH2O)3(CH2CH2O)7CH2CH2N(CH3)2C3H6OSO3
Content is 91.62wt%.
(2) preparation of foaming agent combination：
At normal temperatures and pressures, weigh 93.9 grams of the long-chain polyether nitrogen-containing compound of synthesis gained in previous step in reactor,
Add appropriate local originally water dissolution；138 grams of long-chain diaryl sulfonate is added thereto to again, adds enough sheets
Ground tap water is configured to the solution of 30wt%, is sufficiently stirred for 30min to being completely dissolved, obtains final product foam to 748 grams
Agent compositionss HF-1.
【Embodiment 2】
The preparation of compositionss HF-2, preparation process：
(1) long-chain polyether nitrogen-containing compound (C16H33O(CHCH3CH2O)10(CH2CH2O)20CH2CH2
N(C2H5)(C3H7O)CH2COO synthesis) and preparation：
121 grams of hexadecanols, 3 grams of potassium hydroxide are added in the pressure reactor equipped with agitating device, 80～90 are heated to
DEG C when, open vacuum system, be dehydrated under a high vacuum 1 hour, then with nitrogen displacement 3～4 times, by system reaction temperature
Degree is adjusted to 150 DEG C and is slowly passed through 300 grams of expoxy propane, and control pressure≤0.60MPa is cooled to 90 DEG C, low boiling is removed in vacuum
System reaction temperature is adjusted to 150 DEG C and is slowly passed through 500.0 grams of oxirane, control pressure≤0.60MPa by thing, continuation.Instead
After should terminating, after cooling, neutralization, dehydration, obtain C16H33O(CHCH3CH2O)10(CH2CH2O)21H, yield 98.6wt%.
131 grams are added in the four round flask equipped with reflux condensate device, thermometer, agitator and gas absorbing device
C16H33O(CHCH3CH2O)10(CH2CH2O)21H and 20 gram of pyridine, is heated to 70 DEG C under stirring, slow with Dropping funnel
35 grams of thionyl chlorides of Deca, react 10 hours after completion of dropping at 90 DEG C.After reaction terminates, reactant stood, cooled down
Upper strata is neutralized to neutrality with sodium hydroxide solution by layering, with saturated common salt water washing 5-6 time of heat, in obtaining after drying
Between product C16H33O(CHCH3CH2O)10(CH2CH2O)20CH2CH2Cl, yield are 86.6%.
By C16H33O(CHCH3CH2O)10(CH2CH2O)20CH2CH2135 grams of Cl is added with reflux condensate device, temperature
In degree meter, the four-hole boiling flask of agitator, 77 DEG C are heated to, by N (C2H5)(C3H6OH) solution Dropping funnel is slowly dripped to
In flask, system remains alkalescence, stratification after reacting 10 hours.By the saturation after the vacuum distillation of upper strata with heat
Brine It 5-6 time, obtains desired intermediate C16H33O(CHCH3CH2O)10(CH2CH2O)20CH2CH2
N(C2H5)(C3H7O), yield is 83.3%.
By C16H33O(CHCH3CH2O)10(CH2CH2O)20CH2CH2N(C2H5)(C3H7O) 100 grams are added to and carry
In reflux condensate device, thermometer, the four-hole boiling flask of agitator, 70 DEG C are heated to, ClCH is slowly added dropwise2COONa is molten
30 grams of liquid, after reacting 2 hours, is warming up to 90 DEG C and continues reaction 6 hours, vacuum distillation, Jing efficient liquid phases at 70 DEG C
Chromatograph (HPLC) is analyzed, C in product16H33O(CHCH3CH2O)10(CH2CH2O)20CH2CH2
N(C2H5)(C3H7O)CH2COO contents are 91.32wt%.
(2) preparation of foaming agent combination：
At normal temperatures and pressures, weigh 20.7 grams of the long-chain polyether nitrogen-containing compound of synthesis gained in previous step in reactor,
Add appropriate local originally water dissolution；78.1 grams of long-chain diaryl sulfonate is added thereto to again, adds enough sheets
Ground tap water is configured to the solution of 30wt%, is sufficiently stirred for 30min to being completely dissolved, obtains final product foam to 323 grams
Agent compositionss HF-2.
【Embodiment 3】
The preparation of compositionss HF-3, preparation process：
(1) long-chain polyether nitrogen-containing compound (C14H29OCHCH3CH2O(CH2CH2O)30CH2CH2N(C3H7O)2C5H10SO3)
Synthesis with prepare：
107.0 grams of tetradecanols, 3.0 grams of potassium hydroxide are added in the pressure reactor equipped with agitating device, it is heated to 80～
When 90 DEG C, vacuum system is opened, be dehydrated under a high vacuum 1 hour, then with nitrogen displacement 3～4 times, system reacted
Temperature is adjusted to 150 DEG C and is slowly passed through 60 grams of expoxy propane, and control pressure≤0.60MPa is cooled to 90 DEG C, low boiling is removed in vacuum
System reaction temperature is adjusted to 150 DEG C and is slowly passed through 700.0 grams of oxirane, control pressure≤0.60MPa by thing, continuation.Instead
After should terminating, after cooling, neutralization, dehydration, obtain C14H29OCHCH3CH2O(CH2CH2O)31H, yield 98.7wt%.
327 grams are added in the four round flask equipped with reflux condensate device, thermometer, agitator and gas absorbing device
C14H29OCHCH3CH2O(CH2CH2O)31H and 20 gram of pyridine, is heated to 70 DEG C, is slowly dripped with Dropping funnel under stirring
Plus 35 grams of thionyl chlorides, react 10 hours at 90 DEG C after completion of dropping.After reaction terminates, reactant is stood, cooling divides
Upper strata is neutralized to neutrality with sodium hydroxide solution by layer, with saturated common salt water washing 5-6 time of heat, obtains centre after drying
Product C14H29OCHCH3CH2O(CH2CH2O)30CH2CH2Cl, yield are 87%.
By C14H29OCHCH3CH2O(CH2CH2O)30CH2CH2165 grams of Cl is added with reflux condensate device, temperature
In meter, the four-hole boiling flask of agitator, 77 DEG C are heated to, by N (C3H6OH)2Solution Dropping funnel is slowly dripped in flask,
System remains alkalescence, stratification after reacting 10 hours.By the saturated common salt washing after the vacuum distillation of upper strata with heat
Wash 5-6 time, obtain desired intermediate C14H29OCHCH3CH2O(CH2CH2O)30CH2CH2N(C3H7O)2, yield
For 83.3%.
By C14H29OCHCH3CH2O(CH2CH2O)30CH2CH2N(C3H7O)2100 grams are added to reflux condensation mode dress
Put, in the four-hole boiling flask of thermometer, agitator, be heated to 70 DEG C, be slowly added dropwise ClC5H10SO340 grams of Na solution,
After reacting 2 hours at 70 DEG C, it is warming up to 90 DEG C and continues reaction 6 hours, vacuum distillation, Jing high performance liquid chromatography (HPLC)
Analysis, C in product14H29OCHCH3CH2O(CH2CH2O)30CH2CH2N(C3H7O)2C5H10SO3Content is 91.71
Wt%.
(2) preparation of foaming agent combination：
At normal temperatures and pressures, weigh 207 grams of the long-chain polyether nitrogen-containing compound of synthesis gained in previous step in reactor,
Add appropriate local originally water dissolution；15.5 grams of long-chain diaryl sulfonate is added thereto to again, adds enough sheets
Ground tap water is configured to the solution of 30wt%, is sufficiently stirred for 30min to being completely dissolved, obtains final product foam to 685 grams
Agent compositionss HF-3.
【Embodiment 4】
The preparation of compositionss HF-4, preparation process：
(1) long-chain polyether nitrogen-containing compound (C20H33OCHCH3CH2OCH2CH2OCH2CH2N(C3H7)(C5H11)CH2SO3)
Synthesis with prepare：
145.0 grams of myristyl phenol, 2.0 grams of potassium hydroxide are added in the pressure reactor equipped with agitating device, is heated to
When 80～90 DEG C, vacuum system is opened, be dehydrated under a high vacuum 1 hour, then with nitrogen displacement 3～4 times, by system
Reaction temperature is adjusted to 150 DEG C and is slowly passed through 60 grams of expoxy propane, and control pressure≤0.60MPa is cooled to 90 DEG C, and vacuum is removed
Low-boiling-point substance, continuation is gone system reaction temperature to be adjusted to 150 DEG C and is slowly passed through 90.0 grams of oxirane, control pressure≤0.60MPa.
After reaction terminates, after cooling, neutralization, dehydration, obtain C20H33OCHCH3CH2O(CH2CH2O)2H, yield 99.6wt%.
218 grams are added in the four round flask equipped with reflux condensate device, thermometer, agitator and gas absorbing device
C20H33OCHCH3CH2O(CH2CH2O)2H and 20 gram of pyridine, is heated to 70 DEG C, is slowly added dropwise with Dropping funnel under stirring
35 grams of thionyl chlorides, react 10 hours after completion of dropping at 90 DEG C.After reaction terminates, reactant is stood, cooling is layered,
Upper strata is neutralized to into neutrality with sodium hydroxide solution, with saturated common salt water washing 5-6 time of heat, after drying, intermediate product is obtained
C20H33OCHCH3CH2O CH2CH2OCH2CH2Cl, yield are 87.1%.
By C20H33OCHCH3CH2OCH2CH2OCH2CH296 grams of Cl add with reflux condensate device, thermometer,
In the four-hole boiling flask of agitator, 77 DEG C are heated to, by N (C3H7)(C5H11) solution Dropping funnel slowly dripped in flask,
System remains alkalescence, stratification after reacting 10 hours.By the saturated common salt washing after the vacuum distillation of upper strata with heat
Wash 5-6 time, obtain desired intermediate C20H33OCHCH3CH2OCH2CH2OCH2CH2N(C3H7)(C5H11), yield
For 83.7%.
By C20H33OCHCH3CH2OCH2CH2OCH2CH2N(C3H7)(C5H11) 100 grams be added to reflux condensation mode
In device, thermometer, the four-hole boiling flask of agitator, 70 DEG C are heated to, ClCH is slowly added dropwise2SO3100 grams of Na solution,
After reacting 2 hours at 70 DEG C, it is warming up to 90 DEG C and continues reaction 6 hours, after vacuum distillation, Jing high performance liquid chromatography (HPLC)
Analysis, C in product20H33OCHCH3CH2OCH2CH2OCH2CH2N(C3H7)(C5H11)CH2SO3Content is 91.61
Wt%.
(2) preparation of foaming agent combination：
At normal temperatures and pressures, weigh 70 grams of the long-chain polyether nitrogen-containing compound of synthesis gained in previous step in reactor,
Add appropriate local originally water dissolution；98 grams of long-chain diaryl sulfonate is added thereto to again, adds enough sheets
Ground tap water is configured to the solution of 30wt%, is sufficiently stirred for 30min to being completely dissolved, obtains final product foam to 560 grams
Agent compositionss HF-4.
【Embodiment 5】
The preparation of compositionss HF-5, preparation process：
(1) long-chain polyether nitrogen-containing compound (C12H25O(CHCH3CH2O)20CH2CH2OCH2CH2
N(CH3)(C2H5)C2H4SO3) synthesis with prepare：
93.0 grams of dodecanols, 5.6 grams of potassium hydroxide are added in the pressure reactor equipped with agitating device, it is heated to 80～
When 90 DEG C, vacuum system is opened, be dehydrated under a high vacuum 1 hour, then with nitrogen displacement 3～4 times, system reacted
Temperature is adjusted to 150 DEG C and is slowly passed through 600 grams of expoxy propane, and control pressure≤0.60MPa is cooled to 90 DEG C, is removed in vacuum
System reaction temperature is adjusted to 150 DEG C and is slowly passed through 90 grams of oxirane, control pressure≤0.60MPa by low-boiling-point substance, continuation.
After reaction terminates, after cooling, neutralization, dehydration, obtain C12H25O(CHCH3CH2O)20(CH2CH2O)2H, yield 98.6wt%.
287 grams are added in the four round flask equipped with reflux condensate device, thermometer, agitator and gas absorbing device
C12H25O(CHCH3CH2O)20(CH2CH2O)2H and 30 gram of pyridine, is heated to 70 DEG C, is slowly dripped with Dropping funnel under stirring
Plus 35 grams of thionyl chlorides, react 10 hours at 90 DEG C after completion of dropping.After reaction terminates, reactant is stood, cooling divides
Upper strata is neutralized to neutrality with sodium hydroxide solution by layer, with saturated common salt water washing 5-6 time of heat, obtains centre after drying
Product C12H25O(CHCH3CH2O)20CH2CH2OCH2CH2Cl, yield are 88%.
By C12H25O(CHCH3CH2O)20CH2CH2OCH2CH2146 grams of Cl is added with reflux condensate device, temperature
In meter, the four-hole boiling flask of agitator, 77 DEG C are heated to, by N (CH3)(C2H5) solution Dropping funnel slowly drips to flask
In, system remains alkalescence, stratification after reacting 10 hours.By the saturated common salt after the vacuum distillation of upper strata with heat
Water washing 5-6 time, obtains desired intermediate C12H25O(CHCH3CH2O)20CH2CH2OCH2CH2N(CH3)(C2H5),
Yield is 83.3%.
By C12H25O(CHCH3CH2O)20CH2CH2OCH2CH2N(CH3)(C2H5) 100 grams be added to returned cold
In solidifying device, thermometer, the four-hole boiling flask of agitator, 70 DEG C are heated to, ClC is slowly added dropwise2H4SO330 grams of Na solution,
After reacting 2 hours at 70 DEG C, it is warming up to 90 DEG C and continues reaction 6 hours, vacuum distillation, Jing high performance liquid chromatography (HPLC)
Analysis, C in product12H25O(CHCH3CH2O)20CH2CH2OCH2CH2N(CH3)(C2H5)C2H4SO3Content is 90.97
Wt%.
(2) preparation of foaming agent combination：
At normal temperatures and pressures, weigh 174 grams of the long-chain polyether nitrogen-containing compound of synthesis gained in previous step in reactor,
Add appropriate local originally water dissolution；32.5 grams of long-chain diaryl sulfonate is added thereto to again, adds enough sheets
Ground tap water is configured to the solution of 30wt%, is sufficiently stirred for 30min to being completely dissolved, obtains final product foam to 688 grams
Compositionss HF-5.
【Embodiment 6】
The preparation of compositionss HF-6, preparation process：
(1) long-chain polyether nitrogen-containing compound (C12H25O(CH2CH2O)7CH2CH2N(CH3)2C3H6OSO3) synthesis with system
It is standby：
186.0 grams of dodecanols, 5.6 grams of potassium hydroxide are added in the pressure reactor equipped with agitating device, it is heated to 80～
When 90 DEG C, vacuum system is opened, be dehydrated under a high vacuum 1 hour, then with nitrogen displacement 3～4 times, system reacted
Temperature is adjusted to 150 DEG C and is slowly passed through 360.0 grams of oxirane, control pressure≤0.60MPa, after reaction terminates, after cooling in
With, dehydration, obtain C12H25O(CH2CH2O)8H, yield 99.3wt%.
269 grams are added in the four round flask equipped with reflux condensate device, thermometer, agitator and gas absorbing device
C12H25O(CH2CH2O)8H and 57 gram of pyridine, is heated to 70 DEG C under stirring, be slowly added dropwise 85 grams of thionyl with Dropping funnel
Chlorine, reacts 10 hours after completion of dropping at 90 DEG C.After reaction terminates, reactant is stood, cooling is layered, and uses hydroxide
Upper strata is neutralized to neutrality by sodium solution, with saturated common salt water washing 5-6 time of heat, obtains intermediate product C after drying12H25O
(CH2CH2O)7CH2CH2Cl, yield are 88.3%.
By C12H25O(CH2CH2O)7CH2CH2115 grams of Cl add with reflux condensate device, thermometer, the four of agitator
In mouth flask, 77 DEG C are heated to, by N (CH3)2Solution Dropping funnel is slowly dripped in flask, and system remains weak base
Property, stratification after reacting 10 hours.After the vacuum distillation of upper strata with saturated common salt water washing 5-6 time of heat, mesh will be obtained
Mark intermediate product C12H25O(CH2CH2O)7CH2CH2N(CH3)2, yield is 83.8%.
By C12H25O(CH2CH2O)7CH2CH2N(CH3)2100 grams are added to reflux condensate device, thermometer, stir
Mix in the four-hole boiling flask of device, be heated to 70 DEG C, be slowly added dropwise ClCH2CHOHCH2SO330 grams of Na solution, at 70 DEG C
After lower reaction 2 hours, it is warming up to 90 DEG C and continues reaction 6 hours, vacuum distillation, Jing high performance liquid chromatography (HPLC) point
Analysis, C in product12H25O(CH2CH2O)7CH2CH2N(CH3)2C3H6OSO3Content is 91.32wt%.
(2) preparation of foaming agent combination：
At normal temperatures and pressures, weigh 75.2 grams of the long-chain polyether nitrogen-containing compound of synthesis gained in previous step in reactor,
Add appropriate local originally water dissolution；129.6 grams of long-chain diaryl sulfonate is added thereto to again, is added enough
Local tap water is configured to the solution of 30wt%, is sufficiently stirred for 30min to being completely dissolved, obtains final product foam to 661 grams
Agent compositionss HF-6.
【Embodiment 7】
The preparation of compositionss HF-7, preparation process：
(1) long-chain polyether nitrogen-containing compound (C12H25O(CHCH3CH2O)3(CH2CH2O)7CH2CH2
N(CH3)2C3H6OSO3) synthesis with prepare：
186.0 grams of dodecanols, 5.6 grams of potassium hydroxide are added in the pressure reactor equipped with agitating device, it is heated to 80～
When 90 DEG C, vacuum system is opened, be dehydrated under a high vacuum 1 hour, then with nitrogen displacement 3～4 times, system reacted
Temperature is adjusted to 150 DEG C and is slowly passed through 179.9 grams of expoxy propane, and control pressure≤0.60MPa is cooled to 90 DEG C, is removed in vacuum
System reaction temperature is adjusted to 150 DEG C and is slowly passed through 360.0 grams of oxirane, control pressure≤0.60MPa by low-boiling-point substance, continuation.
After reaction terminates, after cooling, neutralization, dehydration, obtain C12H25O(CHCH3CH2O)3(CH2CH2O)8H, yield 98.8wt%.
339 grams are added in the four round flask equipped with reflux condensate device, thermometer, agitator and gas absorbing device
C12H25O(CHCH3CH2O)3(CH2CH2O)8H and 57 gram of pyridine, is heated to 70 DEG C under stirring, slow with Dropping funnel
85 grams of thionyl chlorides of Deca, react 10 hours after completion of dropping at 90 DEG C.After reaction terminates, reactant stood, cooled down
Upper strata is neutralized to neutrality with sodium hydroxide solution by layering, with saturated common salt water washing 5-6 time of heat, in obtaining after drying
Between product C12H25O(CHCH3CH2O)3(CH2CH2O)7CH2CH2Cl, yield are 88%.
By C12H25O(CHCH3CH2O)3(CH2CH2O)7CH2CH2143 grams of Cl is added with reflux condensate device, temperature
In degree meter, the four-hole boiling flask of agitator, 77 DEG C are heated to, by N (CH3)2Solution Dropping funnel is slowly dripped in flask,
System remains alkalescence, stratification after reacting 10 hours.By the saturated common salt washing after the vacuum distillation of upper strata with heat
Wash 5-6 time, obtain desired intermediate C12H25O(CHCH3CH2O)3(CH2CH2O)7CH2CH2N(CH3)2, yield
For 83%.
By C12H25O(CHCH3CH2O)3(CH2CH2O)7CH2CH2N(CH3)2100 grams are added to reflux condensation mode dress
Put, in the four-hole boiling flask of thermometer, agitator, be heated to 70 DEG C, be slowly added dropwise ClCH2CHOHCH2SO3Na solution
30 grams, after reacting 2 hours at 70 DEG C, it is warming up to 90 DEG C and continues reaction 6 hours, vacuum distillation, Jing high-efficient liquid phase colors
Spectrum (HPLC) analysis, C in product12H25O(CHCH3CH2O)3(CH2CH2O)7CH2CH2N(CH3)2C3H6OSO3
Content is 91.62wt%.
(2) preparation of foaming agent combination：
At normal temperatures and pressures, weigh 6.4 grams of the long-chain polyether nitrogen-containing compound of synthesis gained in previous step in reactor,
Add appropriate local originally water dissolution；353 grams of long-chain diaryl sulfonate is added thereto to again, adds enough sheets
Ground tap water is configured to the solution of 30wt%, is sufficiently stirred for 30min to being completely dissolved, obtains final product foam to 1198 grams
Agent compositionss HF-7.
【Embodiment 8】
The preparation of compositionss HF-8, preparation process：
(1) long-chain polyether nitrogen-containing compound (C26H45O(CHCH3CH2O)3(CH2CH2O)7CH2CH2N(CH3)2C3H6OSO3)
Synthesis with prepare：
373.0 grams of eicosyl phenol, 5.6 grams of potassium hydroxide are added in the pressure reactor equipped with agitating device, is heated to
When 80～90 DEG C, vacuum system is opened, be dehydrated under a high vacuum 1 hour, then with nitrogen displacement 3～4 times, by system
Reaction temperature is adjusted to 150 DEG C and is slowly passed through 179.9 grams of expoxy propane, and control pressure≤0.60MPa is cooled to 90 DEG C, vacuum
Low-boiling-point substance is removed, system reaction temperature is adjusted to 150 DEG C and is slowly passed through 360.0 grams of oxirane, control pressure by continuation
≤0.60MPa.After reaction terminates, after cooling, neutralization, dehydration, obtain C26H45O(CHCH3CH2O)3(CH2CH2O)8H,
Yield 98.6wt%.
437 grams are added in the four round flask equipped with reflux condensate device, thermometer, agitator and gas absorbing device
C26H45O(CHCH3CH2O)3(CH2CH2O)8H and 57 gram of pyridine, is heated to 70 DEG C, is slowly dripped with Dropping funnel under stirring
Plus 85 grams of thionyl chlorides, react 10 hours at 90 DEG C after completion of dropping.After reaction terminates, reactant is stood, cooling divides
Upper strata is neutralized to neutrality with sodium hydroxide solution by layer, with saturated common salt water washing 5-6 time of heat, obtains centre after drying
Product C26H45O(CHCH3CH2O)3(CH2CH2O)7CH2CH2Cl, yield are 87.8%.
By C26H45O(CHCH3CH2O)3(CH2CH2O)7CH2CH2183 grams of Cl is added with reflux condensate device, temperature
In meter, the four-hole boiling flask of agitator, 77 DEG C are heated to, by N (CH3)2Solution Dropping funnel is slowly dripped in flask, body
System remains alkalescence, stratification after reacting 10 hours.By the saturated common salt water washing after the vacuum distillation of upper strata with heat
5-6 time, obtain desired intermediate C26H45O(CHCH3CH2O)3(CH2CH2O)7CH2CH2N(CH3)2, yield is
83%.
By C26H45O(CHCH3CH2O)3(CH2CH2O)7CH2CH2N(CH3)2100 grams are added to reflux condensation mode dress
Put, in the four-hole boiling flask of thermometer, agitator, be heated to 70 DEG C, be slowly added dropwise ClCH2CHOHCH2SO3Na solution
30 grams, after reacting 2 hours at 70 DEG C, it is warming up to 90 DEG C and continues reaction 6 hours, vacuum distillation, Jing high-efficient liquid phase colors
Spectrum (HPLC) analysis, C in product26H45O(CHCH3CH2O)3(CH2CH2O)7CH2CH2N(CH3)2C3H6OSO3
Content is 91.12wt%.
(2) preparation of foaming agent combination：
At normal temperatures and pressures, weigh 116.9 grams of the long-chain polyether nitrogen-containing compound of synthesis gained in previous step in reactor,
Add appropriate local originally water dissolution；115 grams of long-chain diaryl sulfonate is added thereto to again, adds enough sheets
Ground tap water is configured to the solution of 30wt%, is sufficiently stirred for 30min to being completely dissolved, obtains final product foam to 738 grams
Agent compositionss HF-8.
【Embodiment 9】
The preparation of compositionss HF-9, preparation process：
(1) long-chain polyether nitrogen-containing compound (C10H21O(CHCH3CH2O)3(CH2CH2O)7CH2CH2N(CH3)2C3H6OSO3)
Synthesis with prepare：
172.0 grams of decane alcohol, 5.6 grams of potassium hydroxide are added in the pressure reactor equipped with agitating device, it is heated to 80～
When 90 DEG C, vacuum system is opened, be dehydrated under a high vacuum 1 hour, then with nitrogen displacement 3～4 times, system reacted
Temperature is adjusted to 150 DEG C and is slowly passed through 179.9 grams of expoxy propane, and control pressure≤0.60MPa is cooled to 90 DEG C, is removed in vacuum
System reaction temperature is adjusted to 150 DEG C and is slowly passed through 360.0 grams of oxirane, control pressure≤0.60MPa by low-boiling-point substance, continuation.
After reaction terminates, after cooling, neutralization, dehydration, obtain C10H21O(CHCH3CH2O)3(CH2CH2O)8H, yield 98.7wt%.
325 grams are added in the four round flask equipped with reflux condensate device, thermometer, agitator and gas absorbing device
C10H21O(CHCH3CH2O)3(CH2CH2O)8H and 57 gram of pyridine, is heated to 70 DEG C, is slowly dripped with Dropping funnel under stirring
Plus 85 grams of thionyl chlorides, react 10 hours at 90 DEG C after completion of dropping.After reaction terminates, reactant is stood, cooling divides
Upper strata is neutralized to neutrality with sodium hydroxide solution by layer, with saturated common salt water washing 5-6 time of heat, obtains centre after drying
Product C10H21O(CHCH3CH2O)3(CH2CH2O)7CH2CH2Cl, yield are 88.1%.
By C10H21O(CHCH3CH2O)3(CH2CH2O)7CH2CH2137 grams of Cl is added with reflux condensate device, temperature
In meter, the four-hole boiling flask of agitator, 77 DEG C are heated to, by N (CH3)2Solution Dropping funnel is slowly dripped in flask, body
System remains alkalescence, stratification after reacting 10 hours.By the saturated common salt water washing after the vacuum distillation of upper strata with heat
5-6 time, obtain desired intermediate C10H21O(CHCH3CH2O)3(CH2CH2O)7CH2CH2N(CH3)2, yield is
83.7%.
By C10H21O(CHCH3CH2O)3(CH2CH2O)7CH2CH2N(CH3)2100 grams are added to reflux condensation mode dress
Put, in the four-hole boiling flask of thermometer, agitator, be heated to 70 DEG C, be slowly added dropwise ClCH2CHOHCH2SO3Na solution
30 grams, after reacting 2 hours at 70 DEG C, it is warming up to 90 DEG C and continues reaction 6 hours, vacuum distillation, Jing high-efficient liquid phase colors
Spectrum (HPLC) analysis, C in product10H21O(CHCH3CH2O)3(CH2CH2O)7CH2CH2N(CH3)2C3H6OSO3
Content is 91.33wt%.
(2) preparation of foaming agent combination：
At normal temperatures and pressures, weigh 91.2 grams of the long-chain polyether nitrogen-containing compound of synthesis gained in previous step in reactor,
Add appropriate local originally water dissolution；129.6 grams of long-chain diaryl sulfonate is added thereto to again, is added enough
Local tap water is configured to the solution of 30wt%, is sufficiently stirred for 30min to being completely dissolved, obtain final product bubble to 710 grams
Foam agent compositionss HF-9.
【Embodiment 10】
The preparation of compositionss HF-10, preparation process：
(1) long-chain polyether nitrogen-containing compound (C14H29N(CH3)2C3H6OSO3) synthesis with prepare：
By C14H29During 143 grams of Cl is added with reflux condensate device, thermometer, the four-hole boiling flask of agitator, 77 DEG C are heated to,
By N (CH3)2Solution Dropping funnel is slowly dripped in flask, and system remains alkalescence, and reaction was stood after 10 hours
Layering.After the vacuum distillation of upper strata with saturated common salt water washing 5-6 time of heat, desired intermediate C will be obtained14H29N(CH3)2,
Yield is 88.7%.
By C14H29N(CH3)2During 100 grams are added to reflux condensate device, thermometer, the four-hole boiling flask of agitator,
70 DEG C are heated to, ClCH is slowly added dropwise2CHOHCH2SO3100 grams of Na solution, after reacting 2 hours, rises at 70 DEG C
Temperature continues reaction 6 hours, vacuum distillation, Jing high performance liquid chromatography (HPLC) analysis, C in product to 90 DEG C14H29
N(CH3)2C3H6OSO3Content is 91.69wt%.
(2) preparation of foaming agent combination：
At normal temperatures and pressures, weigh 41.3 grams of the long-chain polyether nitrogen-containing compound of synthesis gained in previous step in reactor,
Add appropriate local originally water dissolution；129.6 grams of long-chain diaryl sulfonate is added thereto to again, is added enough
Local tap water is configured to the solution of 30wt%, is sufficiently stirred for 30min to being completely dissolved, obtain final product bubble to 570 grams
Foam agent compositionss HF-10.
【Embodiment 11】
Prepare calcium ion concentration 6000mg/L, the simulation water of total salinity 250000mg/L, by a certain amount of foam
HF-1～HF-10 dissolves, and is configured to the solution of 0.15wt%.
Combinations of the above thing solution is taken under the conditions of 200 DEG C, be 100 centimetres in length, a diameter of 3.8 centimetres are filled out in sand tube
Row foam blocking ability determination experiment, the resistance formed after record injection foam balance form the ratio of resistance with water filling, as
Resistance factor, the results are shown in Table shown in 2.
【Comparative example 1】
Use【Embodiment 1】The C of middle synthesis12H25O(CHCH3CH2O)3(CH2CH2O)7CH2CH2
N(CH3)2C3H6OSO3,【Embodiment 2】The C of middle synthesis16H33O(CHCH3CH2O)10(CH2CH2O)20CH2CH2
N(C2H5)(C3H7O)CH2COO,【Embodiment 3】Middle synthesis
C14H29OCHCH3CH2O(CH2CH2O)30CH2CH2N(C3H7O)2C5H10SO3,【Embodiment 4】Middle synthesis
C20H33OCHCH3CH2OCH2CH2OCH2CH2N(C3H7)(C5H11)CH2SO3,【Embodiment 5】Middle synthesis
C12H25O(CHCH3CH2O)20CH2CH2OCH2CH2N(CH3)(C2H5)C2H4SO3Single dose, be added without subsequent component
Foaming agent combination is prepared into, together【Embodiment 11】Foaming properties test is carried out, be the results are shown in Table shown in 3.
【Comparative example 2】
Use【Embodiment 1-5】In long-chain diaryl sulfonate, be added without subsequent component and be prepared into foaming agent combination,
Together【Embodiment 11】Foaming properties test is carried out, be the results are shown in Table shown in 4.
【Comparative example 3】
Together【Embodiment 1】, difference is successively not reacted step by step with expoxy propane and oxirane,
But both are mixed into the reaction of later stepping row.179.9 gram expoxy propane and 360.0 gram rings are slowly passed through at 140～150 DEG C
Oxidative ethane mixture, control pressure≤0.60MPa, remaining is identical, obtains long-chain polyether nitrogen-containing compound, and together【Embodiment
1】The foaming agent combination LF-1 of corresponding proportion is prepared into, together【Embodiment 11】Foaming properties determination test result is carried out,
Foam resistance factor only has 30.
【Comparative example 4】
The preparation of compositionss LF-2, preparation process：
(1) long-chain polyether nitrogen-containing compound (C12H25O(CH2CH2O)8(CHCH3CH2O)2CHCH3CH2
N(CH3)2C3H6OSO3) synthesis with prepare：
186.0 grams of dodecanols, 5.6 grams of potassium hydroxide are added in the pressure reactor equipped with agitating device, it is heated to 80～
When 90 DEG C, vacuum system is opened, be dehydrated under a high vacuum 1 hour, then with nitrogen displacement 3～4 times, system reacted
Temperature is adjusted to 150 DEG C and is slowly passed through 360.0 grams of oxirane, and control pressure≤0.60MPa is cooled to 90 DEG C, is removed in vacuum
System reaction temperature is adjusted to 150 DEG C and is slowly passed through 179.9 grams of expoxy propane, control pressure≤0.60MPa by low-boiling-point substance, continuation.
After reaction terminates, after cooling, neutralization, dehydration, obtain C12H25O(CH2CH2O)8(CHCH3CH2O)3H, yield 98.8wt%.
339 grams are added in the four round flask equipped with reflux condensate device, thermometer, agitator and gas absorbing device
C12H25O(CH2CH2O)8(CHCH3CH2O)3H and 57 gram of pyridine, is heated to 70 DEG C, is slowly dripped with Dropping funnel under stirring
Plus 85 grams of thionyl chlorides, react 10 hours at 90 DEG C after completion of dropping.After reaction terminates, reactant is stood, cooling divides
Upper strata is neutralized to neutrality with sodium hydroxide solution by layer, with saturated common salt water washing 5-6 time of heat, obtains centre after drying
Product C12H25O(CH2CH2O)8(CHCH3CH2O)2CHCH3CH2Cl, yield are 88%.
By C12H25O(CH2CH2O)8(CHCH3CH2O)2CHCH3CH2143 grams of Cl is added with reflux condensate device, temperature
In degree meter, the four-hole boiling flask of agitator, 77 DEG C are heated to, by N (CH3)2Solution Dropping funnel is slowly dripped in flask,
System remains alkalescence, stratification after reacting 10 hours.By the saturated common salt washing after the vacuum distillation of upper strata with heat
Wash 5-6 time, obtain desired intermediate C12H25O(CH2CH2O)8(CHCH3CH2O)2CHCH3CH2N(CH3)2, receive
Rate is 83%.
By C12H25O(CH2CH2O)8(CHCH3CH2O)2CHCH3CH2N(CH3)2100 grams are added to reflux condensation mode
In device, thermometer, the four-hole boiling flask of agitator, 70 DEG C are heated to, ClCH is slowly added dropwise2CHOHCH2SO3Na is molten
30 grams of liquid, after reacting 2 hours, is warming up to 90 DEG C and continues reaction 6 hours, vacuum distillation, Jing efficient liquid phases at 70 DEG C
Chromatograph (HPLC) is analyzed, in product
C12H25O(CH2CH2O)8(CHCH3CH2O)2CHCH3CH2N(CH3)2C3H6OSO3Content is 91.62wt%.
(2) preparation of foaming agent combination：
At normal temperatures and pressures, weigh 93.9 grams of the long-chain polyether nitrogen-containing compound of synthesis gained in previous step in reactor,
Add appropriate local originally water dissolution；Identical long-chain diaryl sulfonate in 129.6 grams of HF-1 is added thereto to again,
Enough local tap waters are added to 719 grams, the solution of 30wt% is configured to, and 30min are sufficiently stirred for being completely dissolved
Till, obtain final product foaming agent combination LF-2.
Said composition is same【Embodiment 11】Foaming properties test is carried out, as a result resistance factor only has 20.
Composition component structure in table 1 (continued) embodiment
| Foam | R1 | y | z | R4 | R5 | R6 | R7 | Y |
| HF-1 | C12H25 | 3 | 7 | CH3 | CH3 | C3H6O | C2H4 | SO3 - |
| HF-2 | C16H33 | 10 | 20 | C2H5 | C3H7O | CH2 | C2H4 | COO- |
| HF-3 | C14H29 | 1 | 30 | C3H7O | C3H7O | C5H10 | C2H4 | SO3 - |
| HF-4 | C20H33 | 1 | 1 | C3H7 | C5H11 | CH2 | C2H4 | SO3 - |
| HF-5 | C12H25 | 20 | 1 | C2H5 | CH3 | C2H4 | C2H4 | SO3 - |
| HF-6 | C12H25 | 0 | 7 | CH3 | CH3 | C3H6O | C2H4 | SO3 - |
| HF-7 | C12H25 | 3 | 7 | CH3 | CH3 | C3H6O | C3H6 | SO3 - |
| HF-8 | C26H45 | 3 | 7 | CH3 | CH3 | C3H6O | C2H4 | SO3 - |
| HF-9 | C10H21 | 3 | 7 | CH3 | CH3 | C3H6O | C2H4 | SO3 - |
| HF-10 | C12H25 | 0 | 0 | CH3 | CH3 | C3H6O | C2H4 | SO3 - |
Composition component structure in 1 (Continued) embodiment of table
Sealing characteristics of the compositionss in 2 embodiment of table in simulation water
Sealing characteristics of the compositionss in 3 comparative example 1 of table in simulation water
Sealing characteristics of the compositionss in 4 comparative example 2 of table in simulation water
Claims (10)
1. a kind of foaming agent combination, long-chain polyether nitrogen-containing compound in terms of molfraction including 1 part and
0.1～50 part of long-chain diaryl sulfosalt surfactant；
Wherein, the long-chain polyether nitrogen-containing compound, with the general molecular formula shown in formula (I)：
The long-chain diaryl sulfosalt surfactant, with the general molecular formula shown in formula (II)：
In formula (I), the R1For C10～C26Fat-based；Y=0～20, z=0～60；R4、R5For C1～C5's
Any one in alkyl, replacement alkyl；R6、R7For C1～C5Alkylidene, appointing in substituted alkylene
Meaning is a kind of；Y is in electroneutral anionic group selected from molecule shown in formula (I) is made；It is in formula (II), described
R2For C10～C26Fat-based；The R3For H or C1～C26Fat-based；N, m are 0～3 integer
Or decimal and n+m>1；L is O, S ,-(CH2)1-3-、-OC2H4O-、-OC3H6One kind in O-；X
For the one kind in alkali metal ion, alkaline-earth metal ions or ammonium ion, and when X be alkali metal ion or ammonium from
The period of the day from 11 p.m. to 1 a.m, a=n, b=m, when X is alkaline-earth metal ions, a=n/2, b=m/2.
2. foaming agent combination according to claim 1, it is characterised in that the R1For C10～C20Alkane
Base, alkylbenzene.
3. foaming agent combination according to claim 1, it is characterised in that the R2For C12～C20Alkane
Any one in base.
4. foaming agent combination according to claim 1, it is characterised in that the R3For H or C1～C16
Alkyl in any one.
5. foaming agent combination according to claim 1, it is characterised in that the X is K+、Na+、NH4 +
In at least one.
6. foaming agent combination according to claim 1, it is characterised in that the y is more than 0, the z
More than 0.
7. foaming agent combination according to claim 1, it is characterised in that the nitrogenous chemical combination of the long-chain polyether
Thing is 1 with the mol ratio of long-chain diaryl sulfonate:0.2～10.
8. foaming agent combination according to claim 1, it is characterised in that the Y is selected from-COO—、
-SO3 —、-HPO4 —In at least one.
9. foaming agent combination according to claim 1, it is characterised in that the R7Preferably C2H4Or
C3H6。
10. the preparation method of foaming agent combination described in claim 1, comprises the following steps：
(1) synthesis of long-chain polyether nitrogen-containing compound
A, in the presence of base catalyst, R1OH obtains R with aequum propylene oxide reaction1O
(CHCH3CH2O)yH；
B, in the presence of base catalyst, R1O(CHCH3CH2O)yH is obtained with aequum reacting ethylene oxide
R1O(CHCH3CH2O)y(CH2CH2O)z+1H；
C, by R1O(CHCH3CH2O)y(CH2CH2O)z+1H is reacted Jing after processing with thionyl chloride and is obtained
R1O(CHCH3CH2O)y(CH2CH2O)zR7Cl；
D, by R1O(CHCH3CH2O)y(CH2CH2O)zR7Cl and NR4R5In a solvent, in reaction temperature
70～90 DEG C of reactions obtain R Jing after processing1O(CHCH3CH2O)y(CH2CH2O)zR7NR4R5；
E, by R1O(CHCH3CH2O)y(CH2CH2O)zR7NR4R5With ClR6Y is in a solvent in reaction temperature
Reaction at 70-90 DEG C of degree obtains long-chain polyether nitrogen-containing compound Jing after processing；
(2) preparation of foaming agent combination
The desired amount of long-chain polyether nitrogen-containing compound, long-chain diaryl sulfonate mix homogeneously are obtained into described bubble
Foam agent compositionss.
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Application publication date: 20170426 |