CN106634923B - The nano silica and oil recovering nano-fluid of surface modification - Google Patents
The nano silica and oil recovering nano-fluid of surface modification Download PDFInfo
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- CN106634923B CN106634923B CN201610853302.2A CN201610853302A CN106634923B CN 106634923 B CN106634923 B CN 106634923B CN 201610853302 A CN201610853302 A CN 201610853302A CN 106634923 B CN106634923 B CN 106634923B
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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
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07F—ACYCLIC, CARBOCYCLIC OR HETEROCYCLIC COMPOUNDS CONTAINING ELEMENTS OTHER THAN CARBON, HYDROGEN, HALOGEN, OXYGEN, NITROGEN, SULFUR, SELENIUM OR TELLURIUM
- C07F7/00—Compounds containing elements of Groups 4 or 14 of the Periodic System
- C07F7/02—Silicon compounds
- C07F7/025—Silicon compounds without C-silicon linkages
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
- C09K2208/00—Aspects relating to compositions of drilling or well treatment fluids
- C09K2208/10—Nanoparticle-containing well treatment fluids
Abstract
The invention discloses a kind of nano silica of surface modification and oil recovering nano-fluids.The nano silica of surface modification, preparation method include the following steps: that 1) nano silica is reacted with hydrosulphonyl silane, obtain sulfhydrylation nano silica；2) sulfhydrylation nano silica made from step 1) and monounsaturated fatty acids is taken to carry out click-reaction to get the nano silica of monounsaturated fatty acids surface modification.Oil recovering nano-fluid: being dispersed in water to obtain dispersion liquid for the nano silica of the surface modification, adjust dispersion liquid pH value to 8 ~ 12 to get.The nanometer silicon dioxide particle of monounsaturated fatty acids surface modification of the invention can not add dispersing agent self-dispersing Yu Shuizhong.Nano-fluid preparation process of the invention is simple, dispersion is uniform, stability is good, is easy to extemporaneous preparation and large-scale application, can be improved Oil in Super-low Permeability Reservoirs recovery ratio.
Description
Technical field
The invention belongs to nano-functional materials and oil field chemical technical field, and in particular to a kind of nanometer of surface modification
Silica and oil recovering nano-fluid, the nano-fluid can be improved Oil in Super-low Permeability oil deposil erude petroleum recovery ratio.
Background technique
Petroleum has irreplaceable role as a kind of high efficient energy sources in national economy.With Chinese national economy
It increases rapidly, oil demand is continuously improved.With going deep into for oil-gas exploration and development, the ratio of Low Permeability Oil/gas resources exploration
Again will be increasing, the reserves for especially newly verifying extra-low-permeability reservoir in recent years are especially abundant, and such as middle petroleum Changqing oilfields are super
Nearly 1,000,000,000 tons of low-permeability oil deposit proved reserves, account for the 70% of Changqing oilfields petroleum proven reserve.But extra-low-permeability reservoir reservoir
Micro-nano pore throat is developed, the effective use rate of reserves is improved and faces the challenge.
In recent years, with the increase of the development of nanotechnology and oil-gas field development difficulty, nanotechnology is gradually applied to oil
Gas field development field.The nano-fluid displacement of reservoir oil is a kind of emerging oil recovery technique, it is formed in water using aqueous solution as transfer medium
Several hundred to tens even several nanometers of little particle has very big specific surface area and surface energy, greatly reduces grease
Interfacial tension, so that injection fluid during washing away hole, makes crude oil be easy to peel off into small oil droplet, and driven liquid displacement
Out.Nano-fluid drive has the characteristics that using concentration is lower, small investment, quick, oil displacement efficiency is obvious, will become has hair
" the improving water drive " of exhibition prospect improves the new technology of oil recovery factor and increasing injection.
Recovery efficiency technique is improved compared to traditional chemical displacement of reservoir oil, modified dispersions of nanoparticles has for oil field development
There is good effect of increasing production.2010, the Saudi Arabia tip A Mei company EXPEC research center utilized the fluid for carrying nanometer robot
Chemicals is sent into oil reservoir depths and carries out the displacement of reservoir oil, ASP flooding test is as a result, it has been found that the fluid has good stability and mobility.
" Energy fuels " the 1st phase " Enhanced Heavy Oil Recovery in Sandstone of volume 28 in 2014
Cores Using TiO2A Nanofluids " text reports a kind of nano titanium oxide dispersion and adopts for heavy oil raising
Yield, the results showed that recovery ratio can be increased to 80% from 49% by nano particle, and main function mechanism is wetability conversion, nanometer
Oil wet surface is converted to water-wet surface by titanium dioxide, and oil is stripped from wall surface, nano material interaction and adsorption mechanism pair
Wetability conversion plays key effect." Langmuir " " Dynamic Spreading of Nanofluids of volume 28 in 2012
On Solids. Part I:Experimental " and " Dynamic Spreading of Nanofluids on Solids
Two articles of Part II:Modeling " are reported respectively through laboratory experiment and sunykatuib analysis to dispersions of nanoparticles
The research for improving recovery ratio, since there are Brownian movements and interparticle electrostatic repulsion forces for nano particle, when particle size is enough
It is small, when quantity is enough, a stronger extension will be generated, and the electrostatic repulsion of the surface of solids exist it is uneven, thus
A wedge structure is self-assembly of in three-phase contact zone, the forward thrust that this wedge structure generates, what articulated system generated
It reduces capillary pressure, wettability reversal and mutually seeps and change the booster actions such as hysteresis effect, it can be by oil under rock surface removing
Come.
Chinese patent CN104531118A reports " a kind of preparation method of intelligent nano oil displacement agent ", by responsive to temperature type
Polymer and hydrophilic polymer, hydrophobic polymer are grafted to nanoparticle surface by covalent bond, prepare with temperature
The composite nanoparticle of sensitivity characteristic obtains the intelligent nano with temperature response characteristics then with alkali, surfactant compound
Oil displacement agent.
At present nanometer technology of reservoir sweep be mainly used for middle and high infiltration reservoir improve recovery ratio, and it is small by Oil in Super-low Permeability Reservoirs pore throat,
The limitation of the factors such as nano-fluid dispersion stabilization, there are no the nanometer streams that can be improved Oil in Super-low Permeability Reservoirs recovery ratio in the prior art
Body.
Summary of the invention
In order to solve the above-mentioned technical problem, a kind of nano silica of surface modification and containing its oil recovering with receiving
Meter Liu Ti, the nano-fluid can be improved Oil in Super-low Permeability oil deposil erude petroleum recovery ratio.
The nano-fluid is made of the nanometer silicon dioxide particle and alkaline aqueous solution of monounsaturated fatty acids surface modification.
The nano silica of monounsaturated fatty acids surface modification of the invention is successively repaired by hydrosulphonyl silane and monounsaturated fatty acids
It adorns nanometer silicon dioxide particle and is made.Monounsaturated fatty acids modification nanometer silicon dioxide particle is dispersed in water, 50 ~
At 100 DEG C, dispersion liquid pH value is adjusted to 8 ~ 12 with sodium hydroxide or potassium hydroxide solution, it is saturating that well dispersed clarification can be obtained
Bright shape nano-fluid.Monounsaturated fatty acids modifies nanometer silicon dioxide particle, and there are Brownian movements and interparticle electrostatic repulsion
Power, reduction capillary pressure that articulated system generates, wettability reversal and mutually seeps and changes the booster actions such as hysteresis effect, can will be oily
It is stripped down from rock surface, to improve Oil in Super-low Permeability oil recovery.The nano-fluid preparation process is simple, dispersion is uniform,
Stability is good, is easy to extemporaneous preparation and large-scale application.
The nano silica of surface modification provided by the invention, preparation method include the following steps:
1) nano silica is reacted with hydrosulphonyl silane, obtains sulfhydrylation nano silica；
2) sulfhydrylation nano silica made from step 1) and monounsaturated fatty acids is taken to carry out click-reaction to get list
The nano silica of unsaturated fatty acid surface modification.
Preferably, step 1) is that nano silica is taken to be scattered in organic solvent, addition hydrosulphonyl silane, at 30 ~ 80 DEG C
It is stirred to react, it is cooling, it is separated by solid-liquid separation, solid washing is dry, obtains sulfhydrylation nano silica；Wherein, the organic solvent
For the one of which or combinations thereof of methanol, ethyl alcohol, toluene or N,N-dimethylformamide.It is highly preferred that being stirred to react the time is 2
~8 h；Solid is washed 4 ~ 8 times with ethyl alcohol or N,N-dimethylformamide；24 ~ 48 h are dried in vacuo at 30 ~ 80 DEG C.
Preferably, step 2 is that the sulfhydrylation nano silica for taking step 1) to obtain is scattered in organic solvent, is added
Catalyst is added in monounsaturated fatty acids, stirring, and ultraviolet lighting reaction is separated by solid-liquid separation after completion of the reaction, and solid washing is dry
Obtain the nano silica of monounsaturated fatty acids surface modification；Wherein, the catalyst be styrax, benzoin ethyl ether,
Benzoin isopropyl ether, benzoin isobutyl ether, dimethoxybenzoin, diphenylethan, benzophenone, 2,4 dihydroxyl benzophenone,
Michler's keton or triethylamine one of which or combinations thereof.Preferably, the mass ratio of monounsaturated fatty acids and catalyst are as follows: 1 ~ 40:
0.01~5；The ultraviolet lighting reaction time is 10 ~ 120 min；Solid is washed 4 ~ 8 times with ethyl alcohol or N,N-dimethylformamide；30~
24 ~ 48 h are dried in vacuo at 80 DEG C.
Preferably, the partial size of the nano silica is 7 ~ 15 nm, and specific surface area is 150 ~ 400 m2/g。
Preferably, the weight ratio of the nano silica, hydrosulphonyl silane and monounsaturated fatty acids are as follows: 1 ~ 10:1 ~
40:1 ~ 40(is with this ratio, it is ensured that each nanometer silicon dioxide particle is modified, so that well dispersed single insatiable hunger be made
With fatty acid modifying nanometer silicon dioxide particle).
Preferably, the hydrosulphonyl silane chemical formula is X3Si(CH2)nSH, X CH3O、CH3CH2O, Cl or Br, wherein 1≤
N≤30, n are integer；The monounsaturated fatty acids chemical formula is CH3(CH2)aHC=CH(CH2)bCOOH, wherein 1≤a≤50,
1≤b≤50, a and b are integer.
The present invention also provides a kind of oil recovering nano-fluids of nano silica containing above-mentioned surface modification:
The nano silica of the surface modification is dispersed in water to obtain dispersion liquid, adjust dispersion liquid pH value to 8 ~ 12 to get.
Preferably, the nano silica of surface modification mass percent shared in dispersion liquid be 0.001 ~
1%。
Preferably, pH is adjusted with the aqueous solution of alkali.
Preferably, dispersion liquid pH value is adjusted at 50 ~ 100 DEG C to 8 ~ 12.
Present invention has the advantage that:
The nanometer silicon dioxide particle of monounsaturated fatty acids surface modification of the invention can not add dispersing agent self-dispersing
Yu Shuizhong.
Nano-fluid preparation process of the invention is simple, dispersion is uniform, stability is good, is easy to extemporaneous preparation and answers on a large scale
With.
Nano-fluid of the invention can be improved Oil in Super-low Permeability Reservoirs oil recovery factor.
Detailed description of the invention
Fig. 1 is monounsaturated fatty acids surface finish nano silica dioxide granule preparation process schematic diagram.
Fig. 2 is monounsaturated fatty acids surface finish nano silica dioxide granule grain size distribution in nano-fluid.
Specific embodiment
The present invention will be further explained below with reference to the attached drawings and specific examples, so that those skilled in the art can be with
It better understands the present invention and can be practiced, but illustrated embodiment is not as a limitation of the invention.
As shown in Figure 1, the nano silica of monounsaturated fatty acids surface modification of the invention is by hydrosulphonyl silane and list
Unsaturated fatty acid is successively modified nanometer silicon dioxide particle and is made.Monounsaturated fatty acids surface modification of the invention is received
Rice silica is since the monounsaturated fatty acids on surface can form steric effect and electrostatic repulsion effect, so as to repair surface
The nanometer silicon dioxide particle of decorations is well dispersed in the nano-fluid.
The nano silica of surface modification of the invention is prepared via a method which:
(1) by 1 ~ 10 g partial size, 7 ~ 15 nm, 150 ~ 400 m of specific surface area2The nanometer silicon dioxide particle of/g is scattered in
In 100 ~ 1000 mL organic solvents, 1 ~ 40 g hydrosulphonyl silane is added, is stirred to react 2 ~ 8 h at 30 ~ 80 DEG C, is cooled to room temperature, from
The heart or filtering reaction product wash 24 ~ 48 h of vacuum drying at 4 ~ 8 times, 30 ~ 80 DEG C with ethyl alcohol or n,N-Dimethylformamide,
Obtain sulfhydrylation nanometer silicon dioxide particle；The organic solvent is its of methanol, ethyl alcohol, toluene or N,N-dimethylformamide
Middle one kind or combinations thereof can be such that nano silica is dispersed in wherein；
(2) it disperses above-mentioned sulfhydrylation nanometer silicon dioxide particle in 100 ~ 1000 mL organic solvents, 1 ~ 40 g is added
Monounsaturated fatty acids stirs 5 ~ 30 min, adds 0.01 ~ 5 g catalyst, 10 ~ 120 min, centrifugation are reacted under ultraviolet lighting
Or filtering reaction product, 24 ~ 48 h of vacuum drying at 4 ~ 8 times, 30 ~ 80 DEG C are washed with ethyl alcohol or n,N-Dimethylformamide, are obtained
Nanometer silicon dioxide particle is modified to monounsaturated fatty acids；
The organic solvent is methanol, ethyl alcohol, toluene or one of which of N,N-dimethylformamide or combinations thereof；It is described
Catalyst is styrax, benzoin ethyl ether, benzoin isopropyl ether, benzoin isobutyl ether, dimethoxybenzoin, diphenylethan, two
Benzophenone, 2,4 dihydroxyl benzophenone, Michler's keton or one of which of triethylamine or combinations thereof.
Several embodiments are exemplified below so that invention is further explained:
Embodiment 1
By 2 g partial size, 10 nm, 200 m of specific surface area2The nanometer silicon dioxide particle of/g is scattered in 100 mL ethyl alcohol,
2 g (CH are added3CH2O)3SiCH2CH2SH is stirred to react 3 h at 60 DEG C, is cooled to room temperature, is centrifuged or filters reaction product, uses
24 h are dried in vacuo at ethanol washing 4 times, 50 DEG C, obtain sulfhydrylation nanometer silicon dioxide particle.
It disperses above-mentioned sulfhydrylation nanometer silicon dioxide particle in 100 mL ethyl alcohol, 2 g CH is added3(CH2)4HC=CH
(CH2)4COOH stirs 30 min, and 0.01 g dimethoxybenzoin is added as catalyst, reacts 20 min under ultraviolet lighting, from
The heart or filtering reaction product, are dried in vacuo 24 h at ethanol washing 4 times, 50 DEG C, obtain monounsaturated fatty acids surface modification
Nanometer silicon dioxide particle.
Embodiment 2
By 4 g partial size, 7 nm, 300 m of specific surface area2The nanometer silicon dioxide particle of/g is scattered in 200 mL N, N- diformazans
In base formamide, 4 g (CH are added3O)3SiCH2CH2SH is stirred to react 3 h at 60 DEG C, is cooled to room temperature, and is centrifuged or filters and is anti-
Product is answered, 24 h is dried in vacuo at ethanol washing 4 times, 50 DEG C, obtains sulfhydrylation nanometer silicon dioxide particle.
It disperses above-mentioned sulfhydrylation nanometer silicon dioxide particle in 200 mL n,N-Dimethylformamide, 2 g is added
CH3(CH2)10HC=CH(CH2)10COOH stirs 30 min, and 0.01 g diphenylethan is added as catalyst, under ultraviolet lighting
20 min, centrifugation or filtering reaction product are reacted, 24 h is dried in vacuo at ethanol washing 4 times, 50 DEG C, obtains single unsaturated lipid
Fat acid modifies nanometer silicon dioxide particle.
Embodiment 3
By 2 g partial size, 10 nm, 250 m of specific surface area2The nanometer silicon dioxide particle of/g is scattered in 200 mL N, N- bis-
In methylformamide, 2 g Cl are added3SiCH2CH2SH is stirred to react 3 h at 60 DEG C, is cooled to room temperature, is centrifuged or filters reaction
Product is dried in vacuo 24 h at ethanol washing 4 times, 50 DEG C, obtains sulfhydrylation nanometer silicon dioxide particle.
It disperses above-mentioned sulfhydrylation nanometer silicon dioxide particle in 200 mL n,N-Dimethylformamide, 2 g is added
CH3(CH2)15HC=CH(CH2)15COOH stirs 20 min, and 0.01 g triethylamine is added as catalyst, reacts under ultraviolet lighting
30 min, centrifugation or filtering reaction product, are dried in vacuo 24 h at ethanol washing 4 times, 50 DEG C, obtain monounsaturated fatty acids
Modify nanometer silicon dioxide particle.
Embodiment 4
Monounsaturated fatty acids surface finish nano silica dioxide granule made from 0.01 g embodiment 1 is weighed to be scattered in
It in 99.99 g water, is stirred under the conditions of 80 DEG C, dispersion liquid pH value is adjusted to 10, until list is not with 1 mol/L sodium hydroxide solution
Saturated fatty acid modification nanometer silicon dioxide particle clear shape is evenly dispersed, and the nano-fluid can be obtained.
Embodiment 5
It weighs the modification nanometer silicon dioxide particle of monounsaturated fatty acids made from 0.1 g embodiment 2 and is scattered in 99.9 g
It in water, is stirred under the conditions of 100 DEG C, dispersion liquid pH value is adjusted to 9, until single unsaturated lipid with 1 mol/L potassium hydroxide solution
Fat acid modification nanometer silicon dioxide particle clear shape is evenly dispersed, and the nano-fluid can be obtained.
Embodiment 6
It weighs the modification nanometer silicon dioxide particle of monounsaturated fatty acids made from 0.1 g embodiment 3 and is scattered in 99.9 g
It in water, is stirred under the conditions of 100 DEG C, dispersion liquid pH value is adjusted to 9, until single unsaturated lipid with 1 mol/L potassium hydroxide solution
Fat acid modification nanometer silicon dioxide particle clear shape is evenly dispersed, and the nano-fluid can be obtained.
Embodiment 7
Using nanometer silicon dioxide particle particle diameter distribution in laser particle size analyzer measurement nano-fluid, as shown in Figure 2: real
In the nano-fluid for applying example 4 ~ 6,7 ~ 25 nm of nanometer silicon dioxide particle particle size distribution range.
Embodiment 8
Taking a block length is 6 cm, diameter is 2.5 cm Oil in Super-low Permeability natural cores, cleans rock core, is dried in vacuo 24 at 90 DEG C
After h, gas permeability is 2.3 mD, saturation simulation oil (viscosity 3 mPas, 25 DEG C), after 24 h of aging, record saturation oil mass,
With the speed of 0.1 mL/min with 3% potassium chloride brine displacements rock core until outlet end is not fuel-displaced, record cumulative oil production, meter
Calculating primary recovery rate is 35.69%；Nano-fluid made from 0.3 PV embodiment 4 is injected to rock core with the speed of 0.1 mL/min
Slug records oil production；It is not fuel-displaced that secondary water is driven to rock core outlet end, records cumulative oil production, calculates secondary waterflood recovery efficiency factor
It is 45.78%, nano-fluid improves recovery ratio 10.09%.
Embodiment 9
Taking a block length is 6 cm, diameter is 2.5 cm Oil in Super-low Permeability natural cores, cleans rock core, is dried in vacuo 24 at 90 DEG C
After h, gas permeability is 1.9 mD, saturation simulation oil (viscosity 3 mPas, 25 DEG C), after 24 h of aging, record saturation oil mass,
With the speed of 0.1 mL/min with 3% potassium chloride brine displacements rock core until outlet end is not fuel-displaced, record cumulative oil production, meter
Calculating primary recovery rate is 32.18%；Nano-fluid made from 0.3 PV embodiment 5 is injected to rock core with the speed of 0.1 mL/min
Slug records oil production；It is not fuel-displaced that secondary water is driven to rock core outlet end, records cumulative oil production, calculates secondary waterflood recovery efficiency factor
It is 45.29%, nano-fluid improves recovery ratio 13.11%.
Embodiment 10
Taking a block length is 6 cm, diameter is 2.5 cm Oil in Super-low Permeability natural cores, cleans rock core, is dried in vacuo 24 at 90 DEG C
After h, gas permeability is 2.5 mD, saturation simulation oil (viscosity 3 mPas, 25 DEG C), after 24 h of aging, record saturation oil mass,
With the speed of 0.1 mL/min with 3% potassium chloride brine displacements rock core until outlet end is not fuel-displaced, record cumulative oil production, meter
Calculating primary recovery rate is 34.26%；Nano-fluid made from 0.3 PV embodiment 6 is injected to rock core with the speed of 0.1 mL/min
Slug records oil production；It is not fuel-displaced that secondary water is driven to rock core outlet end, records cumulative oil production, calculates secondary waterflood recovery efficiency factor
It is 44.29%, nano-fluid improves recovery ratio 10.03%.
Embodiment 11
Taking 5 block lengths is 6 cm, diameter is the similar Oil in Super-low Permeability natural core of 2.5 cm permeabilities, cleaning rock core, 90 DEG C
After 24 h of lower vacuum drying, gas permeability is divided into 3.3 mD, 3.1 mD, 3.4 mD, 2.9 mD and 3.7 mD, saturation simulation oil
(viscosity 3 mPas, 25 DEG C), after 24 h of aging, record saturation oil mass；Above-mentioned 5 blocks of rock cores are put into imbibition bottle, are soaked respectively
Bubble is concentration is 3wt% potassium chloride salt water, concentration is 0.1wt% neopelex surfactant solution, embodiment 4
In the nano-fluid of nano-fluid, the nano-fluid of embodiment 5 and embodiment 6,5 blocks of rock cores are recorded in different imbibition liquid at any time
Between oil drain quantity record final oil drain quantity until oil drain quantity no longer changes, the recovery ratio for calculating separately 5 kinds of imbibition liquid is respectively
13.2%, 18.6%, 30.1%, 30.0% and 29.8%, nano-fluid improves 10% or more compared to surfactant solution.
Embodiment described above is only to absolutely prove preferred embodiment that is of the invention and being lifted, protection model of the invention
It encloses without being limited thereto.Those skilled in the art's made equivalent substitute or transformation on the basis of the present invention, in the present invention
Protection scope within.Protection scope of the present invention is subject to claims.
Claims (7)
1. a kind of nano silica of surface modification, which is characterized in that preparation method includes the following steps:
1) it takes nano silica to be scattered in organic solvent, hydrosulphonyl silane is added, is stirred to react at 30 ~ 80 DEG C, cooling, solid-liquid
Separation, solid washing is dry, obtains sulfhydrylation nano silica；Wherein, the organic solvent be methanol, ethyl alcohol, toluene or
One of which of N,N-dimethylformamide or combinations thereof；
2) the sulfhydrylation nano silica for taking step 1) to obtain is scattered in organic solvent, and monounsaturated fatty acids is added, stirs
It mixes, catalyst is added, ultraviolet lighting reaction is separated by solid-liquid separation after completion of the reaction, and solid washing is dried to obtain monounsaturated fatty acids
The nano silica of surface modification；Wherein, the catalyst is styrax, benzoin ethyl ether, benzoin isopropyl ether, styrax
Butyl ether, dimethoxybenzoin, diphenylethan, benzophenone, 2,4 dihydroxyl benzophenone, Michler's keton or triethylamine wherein one
Kind or combinations thereof；
The hydrosulphonyl silane chemical formula is X3Si(CH2)nSH, X CH3O、CH3CH2O, Cl or Br, wherein 1≤n≤30, n are whole
Number；The monounsaturated fatty acids chemical formula is CH3(CH2)aHC=CH(CH2)bCOOH, wherein 1≤a≤15,1≤b≤15, a
It is integer and equal with b.
2. the nano silica of surface modification according to claim 1, which is characterized in that the nano silica
Partial size is 7 ~ 15 nm, and specific surface area is 150 ~ 400 m2/g。
3. the nano silica of surface modification according to claim 1, which is characterized in that the nano silica,
The weight ratio of hydrosulphonyl silane and monounsaturated fatty acids are as follows: 1 ~ 10:1 ~ 40:1 ~ 40.
4. the oil recovering of nano silica of the one kind containing the described in any item surface modifications of claim 1 ~ 3 is flowed with nanometer
Body, which is characterized in that be dispersed in water to obtain dispersion liquid for the nano silica of the surface modification, adjust dispersion liquid pH value
To 8 ~ 12 to get.
5. oil recovering nano-fluid according to claim 4, which is characterized in that the nano-silica of the surface modification
SiClx mass percent shared in dispersion liquid is 0.001 ~ 1%.
6. oil recovering nano-fluid according to claim 4, which is characterized in that adjust pH with the aqueous solution of alkali.
7. oil recovering nano-fluid according to claim 4, which is characterized in that adjust dispersion liquid at 50 ~ 100 DEG C
PH value is to 8 ~ 12.
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| CN108410440B (en) * | 2018-03-07 | 2020-09-15 | 中国石油大学(华东) | Surface modified nano-silica nanofluid for improving recovery ratio |
| CN112745987B (en) * | 2019-10-31 | 2022-07-08 | 中国石油化工股份有限公司 | Saturated fatty acid crystallization aid and preparation method thereof |
| CN116023916A (en) * | 2021-10-25 | 2023-04-28 | 中国石油化工股份有限公司 | Nanometer self-adaptive profile control and flooding agent and preparation method thereof |
| CN113881415B (en) * | 2021-11-05 | 2022-07-26 | 清华大学 | Nanoparticle oil displacement agent and method for improving recovery ratio |
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Application publication date: 20170510 Assignee: KARAMAY XINKEAO PETROLEUM TECHNOLOGICAL Co.,Ltd. Assignor: China University of Petroleum (East China) Contract record no.: X2020370010013 Denomination of invention: Surface-modified nano-silica and nano fluid for crude oil recovery Granted publication date: 20190607 License type: Exclusive License Record date: 20200721 |
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