CN109456745A - A kind of nanometer of wetting agent and its preparation method and application - Google Patents
A kind of nanometer of wetting agent and its preparation method and application Download PDFInfo
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- CN109456745A CN109456745A CN201710797057.2A CN201710797057A CN109456745A CN 109456745 A CN109456745 A CN 109456745A CN 201710797057 A CN201710797057 A CN 201710797057A CN 109456745 A CN109456745 A CN 109456745A
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
- C09K8/00—Compositions for drilling of boreholes or wells; Compositions for treating boreholes or wells, e.g. for completion or for remedial operations
- C09K8/58—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
Abstract
The invention discloses a kind of nanometer of wetting agent and its preparation method and application, this nanometer of wetting agent is the nano silica aggregate for being grafted with surfactant, and the nano silica aggregate is coupling agent modified nano silica aggregate.Preparation method includes: to prepare coupling agent modified nanometer aggregate；Link surfactant；Separating-purifying.Nanometer wetting agent of the invention is the link by surfactant in the nanometer aggregate surface of coupling modifier, make its dilute aqueous solution that there is the ability for improving reservoir wettability, can make the performance of the improvement reservoir wettability of the aqueous solution of surface finish nano wetting agent of the invention adjustable by using different surfactant and concentration.Nanometer wetting agent of the invention can be configured to surfactant displacement liquid, be used for waterflooding reservoir, and provided wetting agent can be effectively improved reservoir wettability, to play the effect for improving recovery ratio.
Description
Technical field
The invention belongs to field of oil development, more particularly, to a kind of nanometer of wetting agent and its preparation method and application.
Background technique
The medium to high permeable rate old filed of China's major part waterflooding extraction has entered High water cut, " the double height " of high recovery percent of reserves is opened
The hair stage.Under China's background increasing to oil demand, increasing is particularly important the exploitation of remaining oil.It is general next
It says, remaining oil can be divided into two kinds of fundamental types: macroscopical and microcosmic.Macroscopical remaining oil, which refers to, not to be arrived by water-driven still
Reserves, and the reserves in zone of stagnation and lithologic lens.Microscopic remaining oil refers to be arrived by water-driven, but Analysis of Water-drive Energy is still
It is not enough to be produced, is in remanent state, in adsorption-like and fetter shape such as the petroleum of filminess, and on pore surface
Petroleum, such as the residual oil that capillary force fetters, it, which remains in, injects the area that fluid passes through, and the quilt completely in tiny hole
Capillary force constraint etc..This kind of oil distribution is microcosmic, and mostly discontinuous.
Microscopic remaining oil occupies larger proportion in current petroleum reserves, how to improve its recovery percent of reserves, becomes pendulum in oil
Major issue in face of the developer of field.
Reservoir wettability is a key factor for controlling formation fluid regional location, distribution and flow behavior.Storage
The wetability of layer pore surface is to capillary pressure, remaining oil-containing or water saturation, relative permeability, electrical property feature and water filling
Development features have the influence of essence.Studies have shown that water-wet stratum is changed to generally make oleic permeability after oil wet formation
15~85% are reduced, averagely reduces by 40%, the percentage of permeability reduction is bigger in tight rock.Therefore reservoir wettability
Variation it is in close relations related to oil recovery factor.Therefore, by changing reservoir wettability, adopting for the type crude oil can be improved
Degree out.
For reservoir wettability, researcher is adjusted by changing injection fluid pH value, surfactant and phase permeability
The means such as agent realize the change to reservoir wettability, to improve crude oil recovery percent of reserves.
Nano particle is due to unique small-size effect itself and skin effect, in the exploration and development process of petroleum industry
In more and more paid attention to.As report by wettability modification improves recovery ratio, water injection well increasing injection, prevents stratum
Injure and prevent scale deposition etc..
104449631 B of Chinese patent CN (strong gas wetability nano silica Xie Shui lock agent, preparation method and rock
The method of stone moistened surface reversion) a kind of gas wetting nano silica Xie Shui lock agent is reported, the system is by modified Nano two
Silica, emulsifier op-10, lauryl sodium sulfate, ethyl alcohol and water compound to be formed, and show good super-hydrophobic oleophobic property
Energy.
Document (Jin Jiafeng air humidity Nano-meter SiO_22Particle to rock core wettability reversal and solution water lock machine reason [J] drilling fluid with
Completion fluid, 2015,32 (6): 5-11), use ethyl orthosilicate and ammonium hydroxide to prepare nano silica for raw material, and by from
The absorption of subtype fluorocarbon surfactant is modified, and the nano particle wetting agent for having air humidity reverse function is prepared.
It is prepared in conclusion the nano silica wetting agent of report is modified using directly compounding or absorption, to oil
It hides in injection process, similar products inevitably will lead to chromatographic isolation or unstable quality phenomenon occurs, in addition, report
Nanometer wetting agent technology is directed to gas reservoir solution liquid lock, there is no for the nanometer wetting agent technology for changing reservoir wettability.Therefore, existing
Some nanometer wetting agents still have biggish improvement to promote leeway in technology and performance.And the nanometer wetting agent of function admirable is ground
Hair all undoubtedly can generate positive effect, and the economy and environmental benefit that finally show to existing waterflooding reservoir, all
It will have an important influence on.
Reservoir wettability is a key factor for controlling formation fluid regional location, distribution and flow behavior, special
Oil recovery factor is not improved by changing reservoir wettability there are in the case where a large amount of remaining oils in current waterflooding reservoir,
It is of great significance.
Summary of the invention
Existing nanometer wetting agent there are aiming at the problem that, the purpose of the present invention is to provide a kind of nanometer of wetting agent and its systems
Preparation Method and application prepare structure by grafting respective surfaces active group after nano-silica surface coupling modifier
Stable nanometer wetting agent, can effectively improve reservoir wettability, finally play the effect for improving recovery ratio.
To achieve the above object, the first aspect of the present invention provides a kind of nanometer of wetting agent, this nanometer of wetting agent is grafting
There is the nano silica aggregate of surfactant, the nano silica aggregate is coupling agent modified nano silica
Aggregate.
A preferred embodiment according to the present invention, the particle size of the nano silica aggregate are 10-
10000nm, preferably 10-100nm.
A preferred embodiment according to the present invention, the coupling agent are amino silicane coupling agent, preferably include γ-ammonia
Propyl-triethoxysilicane, γ-aminopropyltrimethoxysilane, N- β-aminoethyl-γ-aminopropyltriethoxy dimethoxysilane,
N- β-aminoethyl-γ-aminopropyltrimethoxysilane, γ-aminopropyltriethoxy diethoxy silane and γ-divinyl triammonium propyl
At least one of methyl dimethoxysilane.
The surfactant in the present invention can for anionic surfactant, nonionic surface active agent and
At least one of cationic surface active agent.A preferred embodiment according to the present invention, the surfactant are
Anionic surfactant, preferably sulfonate type anionic surfactant, sulfuric ester salt form anionic surfactant
At least one of with alkyl phosphate salt form anionic surfactant.
Sulfonate type anionic surfactant, such as alkylbenzene sulfonate, alpha-alkene sulfonate, alkylsulfonate, α-sulphur
Base monocarboxylate, fatty acid sulfoalkyl ester, sulphosuccinates, alkylnaphthalene sulfonate, petroleum sulfonate, lignin sulfonic acid
Salt, alkyl glyceryl ether sulfonate etc.；Sulfuric ester salt form anionic surfactant, as polyoxyethylene alkyl ether sulfate salt,
Polyoxypropylene sulfuric acid；Alkyl phosphate salt form anionic surfactant, such as the single, double ester salt of alkyl phosphoric acid, poly alkyl alcohol
The phosphate mono-ester/diester salt of ethylene oxide ether and mono phosphoric acid ester, the dibasic acid esters salt of alkyl phenol polyoxyethylene ether.The surfactant is above-mentioned
The combination of one or more of surfactant can be with when the surfactant includes the above two above substance
Arbitrary proportion mixing.
A preferred embodiment according to the present invention, wherein the molar ratio of surfactant and coupling agent is 1:0.5-
3；The molar ratio of nanometer aggregate and coupling agent is 1:0.5-6.
The second aspect of the present invention provides the preparation method of above-mentioned nanometer wetting agent, method includes the following steps:
Step 1: preparing coupling agent modified nanometer aggregate
Under conditions of inert gas shielding and stirring, by washing to neutral nanometer aggregate, coupling agent and organic solvent
Aqueous solution contact and react, obtain coupling agent modified nanometer aggregate solution；
Step 2: link surfactant
Under conditions of inert gas shielding and stirring, by coupling agent modified the nanometer aggregate solution and surface-active
Agent is contacted and is reacted, and obtains the nanometer wetting agent mixed liquor of surface modification；
Step 3: separating-purifying
The nanometer wetting agent mixed liquor of the surface modification is centrifuged, the nanometer wetting of surface modification is obtained
Agent.
A preferred embodiment according to the present invention, the weight of the aqueous solution of nanometer aggregate and organic solvent in step 1
Than for 1:10-30；The organic solvent preferably includes ethyl alcohol and/or isopropanol.When the organic solvent include it is above two with
When upper solvent, it can be mixed with arbitrary proportion.The aqueous solution of the organic solvent be preferably organic solvent and deionized water according to
Volume ratio is the solution that the ratio of 1:1 is formulated.
In the present invention, the reaction condition of step 1 includes: that temperature is preferably 50-80 DEG C, and the time is preferably 1-2h；Step 2
Reaction condition includes: that temperature is preferably 50-80 DEG C, and the time is preferably 2-4h.
Heretofore described method further include: after mixing nanometer aggregate with the aqueous solution of organic solvent, stir 20-
30min, then ultrasonic vibration 20-30min, is uniformly mixed the two.Wherein, it is highly preferred that the revolving speed of stirring is 400-500
Turn/min.
In the preparation process in accordance with the present invention, the cleaning solution and washing times washed to lower part nano material can be by this
Skilled person carries out conventional selection and regulation.Preferably, successively surface is repaired with dehydrated alcohol and deionized water
Lower part nano material after decorations magnetic Nano material mixed liquor is centrifuged respectively is washed three times, be then dried in vacuo (such as
80 DEG C), obtain the surface finish nano wetting agent.
The third aspect of the present invention provides the wetting of nanometer made from the nanometer wetting agent and/or the preparation method
Agent is improving the application in oil recovery rate.
Beneficial effects of the present invention:
1, nanometer wetting agent of the invention is to be made by surfactant in the link of the nanometer aggregate surface of coupling modifier
Its dilute aqueous solution has the ability for improving reservoir wettability, can make the present invention by using different surfactant and concentration
Surface finish nano wetting agent aqueous solution improvement reservoir wettability performance it is adjustable.
2, nanometer wetting agent of the invention can be configured to surfactant displacement liquid.The displacing fluid is of the invention receives
The aqueous solution of rice wetting agent can be nanometer wetting agent-aqueous dispersion of mass concentration 0.2-1%, be used for filling the water
Oil reservoir is developed, provided wetting agent can be effectively improved reservoir wettability, to play the effect for improving recovery ratio.
Other features and advantages of the present invention will then part of the detailed description can be specified.
Specific embodiment
The preferred embodiment of the present invention is described in more detail below.Although the following describe preferred implementations of the invention
Mode, however, it is to be appreciated that may be realized in various forms the present invention without that should be limited by the embodiments set forth herein.Phase
Instead, these embodiments are provided so that the present invention is more thorough and complete, and can be by the scope of the present invention completely
It is communicated to those skilled in the art.
Embodiment 1:
(1) the silica aggregate 5g of 50nm is taken, deionized water is spare after washing to neutrality.
(2) 100mL ethanol water (volume ratio of ethyl alcohol and deionized water is 1:1) is packed into beaker, it then will be quasi-
The silica got ready is added in beaker, is put into ultrasonator, sonic oscillation 30min.It is transferred into three necks burning again
It in bottle, is put on the magnetic stirring apparatus with water bath with thermostatic control, leads to nitrogen protection, be added under the conditions of being stirred at room temperature into three-necked bottle
The gamma-aminopropyl-triethoxy-silane of 18.25g is warming up to 70 DEG C and isothermal reaction 2h under continuous stirring, obtains surface link
The nano silica mixed liquor of coupling agent.
(3) to the nano silica mixed liquor for holding the surface link coupling agent at 70 DEG C and under conditions of stirring
The lauryl sodium sulfate of 20.55g is added in three-necked bottle, isothermal reaction 4h, obtains the nano-silica of surface modification under stiring
SiClx mixed liquor.
(4) the surface finish nano wetting agent mixed liquor is transferred in centrifugal bottle and is centrifuged, it is clear to discard top
Liquid, after lower part nano material is successively respectively washed three times with dehydrated alcohol and deionized water, then 80 DEG C of vacuum drying, obtain institute
State surface finish nano wetting agent NWSD-1.
Embodiment 2:
(1) the silica aggregate 10g of 80nm is taken, deionized water is spare after washing to neutrality.
(2) 300mL ethanol water (ethyl alcohol is 1:1 with water volume ratio) is packed into beaker, then by ready two
Silica is put into ultrasonator in being added to beaker, sonic oscillation 30min.It is transferred into three-neck flask, puts again
Onto the magnetic stirring apparatus with water bath with thermostatic control, leads to nitrogen protection, 26.75g is added under the conditions of being stirred at room temperature into three-necked bottle
γ-aminopropyltrimethoxysilane, be warming up to 70 DEG C and isothermal reaction 2h under continuous stirring, obtain surface link coupling agent
Nano silica mixed liquor.
(3) to the nano silica mixed liquor for holding the surface link coupling agent at 70 DEG C and under conditions of stirring
The neopelex of 48.50g is added in three-necked bottle, isothermal reaction 4h, obtains the nanometer two of surface modification under stiring
Silica mixed liquor.
(4) the surface finish nano wetting agent mixed liquor is transferred in centrifugal bottle and is centrifuged, it is clear to discard top
Liquid, after lower part nano material is successively respectively washed three times with dehydrated alcohol and deionized water, then 80 DEG C of vacuum drying, obtain institute
State surface finish nano wetting agent NWSD-2.
Embodiment 3:
(1) the silica aggregate 5g of 50nm is taken, deionized water is spare after washing to neutrality.
(2) 300mL ethanol water (ethyl alcohol is 1:1 with water volume ratio) is packed into beaker, then by ready two
Silica is added in beaker, is put into ultrasonator, sonic oscillation 30min.It is transferred into three-neck flask, is put into again
On magnetic stirring apparatus with water bath with thermostatic control, lead to nitrogen protection, is added 17.25g's under the conditions of being stirred at room temperature into three-necked bottle
γ-aminopropyltriethoxy diethoxy silane is warming up to 70 DEG C and isothermal reaction 2h under continuous stirring, obtains surface link coupling
The nano silica mixed liquor of agent.
(3) to the nano silica mixed liquor for holding the surface link coupling agent at 70 DEG C and under conditions of stirring
Three sodium sulfonate of ethoxylated of myristyl of 52.25g is added in three-necked bottle, isothermal reaction 4h, obtains to surface and repair under stiring
Adorn nano silica mixed liquor.
(4) the surface finish nano wetting agent mixed liquor is transferred in centrifugal bottle and is centrifuged, it is clear to discard top
Liquid, after lower part nano material is successively respectively washed three times with dehydrated alcohol and deionized water, then 80 DEG C of vacuum drying, obtain institute
State surface finish nano wetting agent NWSD-3.
Test case 1:
The nanometer wetting agent-of mass concentration 0.5% is respectively configured using nanometer wetting agent sample obtained by embodiment 1-3
Then aqueous dispersion carries out surface tension test and contact angle test to it.
Nanometer displacement agent-aqueous dispersion preparation method of the mass concentration 0.5% is the following steps are included: sample is claimed
It takes required amount in beaker, the desired amount of water is then added, be put into magnetic stir bar stirring (200 revs/min of revolving speed) 30min
Afterwards, beaker is moved into ultrasonator, sonic oscillation 30min obtains this nanometer of wetting agent-aqueous dispersion.
Surface tension test: it is carried out using the K100 type surface and interface tension measuring device of German KRUSS company to above-mentioned NWSD-
1, nanometer wetting agent-aqueous dispersion of the mass concentration 0.5% of NWSD-2, NWSD-3 configuration carries out the survey of surface tension performance
Examination, the results are shown in Table 1 (room temperature condition).
Contact angle test: oil-wet core (water survey contact angle: 85 °) is polished smooth with sand paper, is placed in embodiment 1-3 system
In standby 0.5% NWSD-1, NWSD-2, NWSD-3 nanometer-aqueous dispersion, impregnates 24 hours, place 3 in 50 DEG C of baking ovens
A hour, the rock core that obtains that treated after drying use German dataphysics OCA50AF contact angle instrument to measure water phase
In the contact angle of core surface, it the results are shown in Table 2 (room temperature conditions).
The surface tension (room temperature condition) of 1 nanometer of wetting agent of table
As can be seen from Table 1, nanometer wetting agent made from embodiment 1-3 has lower surface tension.
The water of 2 nanometers of wetting agents of table surveys contact angle (room temperature condition)
As can be seen from Table 2, nanometer wetting agent made from embodiment 1-3 has the hydrophilic energy for significantly reducing hydrophobic rock core
Power.
Various embodiments of the present invention are described above, above description is exemplary, and non-exclusive, and
It is not limited to disclosed each embodiment.Without departing from the scope and spirit of illustrated each embodiment, for this skill
Many modifications and changes are obvious for the those of ordinary skill in art field.
Claims (10)
1. a kind of nanometer of wetting agent, which is characterized in that this nanometer of wetting agent is the nano silica for being grafted with surfactant
Aggregate, the nano silica aggregate are coupling agent modified nano silica aggregate.
2. according to claim 1 nanometer of wetting agent, wherein the particle size of the nano silica aggregate is 10-
10000nm, preferably 10-100nm.
3. according to claim 1 nanometer of wetting agent, wherein the coupling agent is amino silicane coupling agent, is preferably included
Gamma-aminopropyl-triethoxy-silane, γ-aminopropyltrimethoxysilane, N- β-aminoethyl-γ-aminopropyltriethoxy dimethoxy
Silane, N- β-aminoethyl-γ-aminopropyltrimethoxysilane, γ-aminopropyltriethoxy diethoxy silane and γ-divinyl three
At least one of aminopropyltriethoxy dimethoxysilane.
4. according to claim 1 nanometer of wetting agent, wherein the surfactant is anionic surfactant, excellent
It is selected as sulfonate type anionic surfactant, sulfuric ester salt form anionic surfactant and alkyl phosphate salt form anion
At least one of surfactant.
5. according to claim 1 nanometer of wetting agent, wherein the molar ratio of surfactant and coupling agent is 1:0.5-3；
The molar ratio of nanometer aggregate and coupling agent is 1:0.5-6.
6. the preparation method of nanometer wetting agent described in any one of claim 1-5, which is characterized in that this method include with
Lower step:
Step 1: preparing coupling agent modified nanometer aggregate
Under conditions of inert gas shielding and stirring, by washing to neutral nanometer aggregate, the water of coupling agent and organic solvent
Solution is contacted and is reacted, and obtains coupling agent modified nanometer aggregate solution；
Step 2: link surfactant
Under conditions of inert gas shielding and stirring, the coupling agent modified nanometer aggregate solution is connect with surfactant
It touches and reacts, obtain the nanometer wetting agent mixed liquor of surface modification；
Step 3: separating-purifying
The nanometer wetting agent mixed liquor of the surface modification is centrifuged, the nanometer wetting agent of surface modification is obtained.
7. preparation method according to claim 6, wherein the weight of the aqueous solution of nanometer aggregate and organic solvent in step 1
Amount is than being 1:10-30；The organic solvent includes ethyl alcohol and/or isopropanol.
8. preparation method according to claim 6, wherein the reaction condition of step 1 includes: that temperature is 50-80 DEG C, the time
For 1-2h；The reaction condition of step 2 includes: that temperature is 50-80 DEG C, time 2-4h.
9. preparation method according to claim 6, wherein this method further include: by the water of nanometer aggregate and organic solvent
After solution mixing, 20-30min is stirred, then ultrasonic vibration 20-30min, is uniformly mixed the two.
10. described in any one of nanometer wetting agent and/or claim 6-9 described in any one of claim 1-5
Nanometer wetting agent made from preparation method is improving the application in oil recovery rate.
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