CN104099076A - Fluorescent silica nano particle composite foam system for oil-gas field - Google Patents
Fluorescent silica nano particle composite foam system for oil-gas field Download PDFInfo
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- CN104099076A CN104099076A CN201410327864.4A CN201410327864A CN104099076A CN 104099076 A CN104099076 A CN 104099076A CN 201410327864 A CN201410327864 A CN 201410327864A CN 104099076 A CN104099076 A CN 104099076A
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- composite foam
- modified silica
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- silica nanoparticle
- fluorescent dye
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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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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
- G01N21/62—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light
- G01N21/63—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light optically excited
- G01N21/64—Fluorescence; Phosphorescence
Abstract
The invention provides a fluorescent silica nano particle composite foam system which comprises modified silica nano particles, a surfactant and fluorescent dye, wherein a mass ratio of the modified silica nano particles to the surfactant to the fluorescent dye is (0.05-0.5):(0.5-2):(0.001-0.005). According to the composite foam system, the bonding time of the fluorescent dye on the surfaces of the particles is longer; distribution of the composite foam system can be seen clearly under microscopes such as a fluorescent microscope; the longest drainage half-life period of the composite foam system is about 45min; the stability is excellent; and the composite foam system is very suitable for fundamental research in a laboratory. When the prepared composite foam system is observed under the microscopes such as the fluorescent microscope, the foam form does not have too large change within the observation period, and the stability is good.
Description
Technical field
The invention belongs to oil production preparation technique field, be specifically related to a kind of oil-gas field research fluorescent silicon dioxide nano particle composite foam system.
Background technology
At present, aerated fluid all demonstrates very large application potential in all respects such as the drilling well of petroleum industry, well production increment, well workover, raising recovery ratio.But also there is the limitation such as half foam life period is shorter, poor stability in foam flooding, has greatly restricted its using value and widespread popularity as the tertiary oil recovery technology that has application prospect.Therefore, the suds-stabilizing agents that add go the stability of reinforced foam more at present, but are that organic polymer or the suds-stabilizing agent of biomacromolecule all can stop up stratum, cause damage layer not recoverablely; The stability of nano SiO 2 particle energy reinforced foam, and because diameter own can not stop up stratum than the little order of magnitude of stratum pore throat, demonstrate very large advantage.But be a difficult problem to nano SiO 2 particle with the mechanism research of tensio-active agent acting in conjunction stable foam always, application fluorescence technique and composite go out a kind of foam of good stability contribute to study nano SiO 2 particle with Action of Surfactant mechanism, thereby be better applied to petroleum industry field.
Summary of the invention
The invention provides a kind of oil-gas field fluorescent silicon dioxide nano particle composite foam system and preparation method thereof, can characterize for a long time the form that exists of foam surface nano SiO 2 particle, and be difficult for the composite foam system from particle surface wash-out, thereby provide possibility for study foam system under laser co-focusing inverted microscope, thereby made up the deficiencies in the prior art.
Fluorescent silicon dioxide nano particle composite foam of the present invention, includes modified silica nanoparticle, tensio-active agent, fluorescence dye; Wherein the mass ratio of modified silica nanoparticle, tensio-active agent, fluorescence dye be 0.05 ?0.5:0.5 ?2:0.001 ?0.005;
Composite foam preparation method of the present invention, is that modified silica nanoparticle is joined to ultrasonic in fluorescent dye solution, stirring, centrifugal wash-out, adds water and makes dispersion liquid, then complete preparation after adding tensio-active agent to stir to bubble after cleaning.
Wherein the preparation method of modified silica nanoparticle is as follows: nano SiO 2 particle is warmed up in reactor to 160 DEG C of preheating 2h activation, to after polydimethylsiloxane, 300 DEG C of vaporizations of hexamethyl dichloro azane Rhometal, enter in reactor again, after reaction 30min ?60min, make.
Wherein a kind of concrete preparation process is as follows:
1) preparation of fluorescent dye solution:
Get fluorescence dye and join in the water that resistivity is 18.2M Ω cm, warming-in-water to 40 DEG C, magnetic agitation rotating speed 200rpm1h, makes fluorescent dye solution;
2) modification of nano SiO 2 particle:
Nano SiO 2 particle is warmed up in reactor to 160 DEG C of preheating 2h activation, then will after polydimethylsiloxane, 300 DEG C of vaporizations of hexamethyl dichloro azane Rhometal, enters in reactor, after reaction 30min ?60min, make;
3) dyeing of modified silica nanoparticle:
In fluorescent dye solution, add modified silica nanoparticle 0.5 ?2 parts, ultrasonic 1 ?3h modified silica nanoparticle is combined with fluorescent dye solution, 400rpm rotating speed stirs 4h, makes dispersion liquid even.8000rpm Centrifugal dispersion liquid 15 ?30min, remove supernatant liquor, repeat 3 ?5 times, after cleaning, water is dissolved to 100 parts again, makes dispersion liquid;
3) preparation of composite foam:
Getting tensio-active agent joins in dispersion liquid, to stir after bubbling and makes nano SiO 2 particle composite foam system.
Described fluorescence dye be fluorescein isothiocyanate (FITC) (maximum absorption optical wavelength 490 ?495nm, emission maximum optical wavelength 520 ?530nm) or rhodamine B (maximum absorption optical wavelength 552nm, emission maximum optical wavelength 610nm).
Described tensio-active agent is preferably Sodium dodecylbenzene sulfonate (SDBS);
Composite foam system fluorescence dye of the present invention is longer at particle surface binding time, can under the microscopes such as fluorescent microscope, clearly see its distribution, and composite foam system to analyse the liquid transformation period the longest about 45 minutes, stability is splendid, is applicable to very much use for laboratory fundamental research.The composite foam system of preparation is placed under the microscopes such as fluorescent microscope and is observed, and within the observation phase, can there is not too large variation in the form of foam, and stability is good.
Embodiment
The present invention uses nano SiO 2 particle as foam suds-stabilizing agent, has good stable foam ability; And in to the research of the nano SiO 2 particle mechanism of action, foaming system of the present invention can better mark out the position of nano particle, contributes to the research to mechanism.
Nano SiO 2 particle used in the present invention is that particle diameter is between 10 to 18nm, through the particle of surperficial polydimethylsiloxane and the modification of hexamethyl dichloro azane surface hydrophobicity, silanol alkyl density 0.1/nm
2– 0.6/nm
2, 70 °～130 ° of water contact angles, strong with the binding ability of fluorescence dye, can long storage time not come off from particle surface.Before modification, nano SiO 2 particle water contact angle is less than 20 °, and silanol alkyl density is 2/nm
2, foaming property is general, analyses the liquid transformation period to be less than 10min.
Below in conjunction with embodiment, fluorescent silicon dioxide nano particle composite foam of the present invention is described in detail.
Embodiment 1:
1) configuration of fluorescent dye solution
The water of getting resistivity that FITC0.1mg is placed in 100ml and be 18.2M Ω cm dissolves, warming-in-water to 40 DEG C, and magnetic agitation rotating speed 200rpm, time 1h, makes 100ml fluorescent dye solution.
2) preparation of modified silica nanoparticle
By 100g nano SiO 2 particle (silanol alkyl density 2/nm
2) in reactor, be warmed up to 160 DEG C of preheating 2h activation, add polydimethylsiloxane 30g and hexamethyl dichloro azane 25g, and add catalyzer Rhometal, by entering in reactor after 300 DEG C of vaporizations of vapourizing unit, with discharging after silicon dioxde reaction 45min, the 0.3/nm of density of silica particles silanol alkyl after modification
2, 120 ° of contact angles.
3) dyeing of modified silica nanoparticle:
Get modified silica nanoparticle 1g and be dissolved in above-mentioned 100ml fluorescent dye solution, ultrasonic 1h, 400rpm magnetic agitation 4h.8000rpm Centrifugal dispersion liquid, removes supernatant liquor, repeats 5 times, and after cleaning, water is dissolved to 100 parts again, makes dispersion liquid.
4) preparation of composite foam
Add SDBS0.5g in above-mentioned dispersion liquid, magnetic agitation 300rpm stirs 5 minutes.Solution is placed in to homogenizer and stirs 3min, rotating speed 8000rpm.Make stable dyeing inorganic nanoparticles composite foam system.
5) stability test of foam:
Foam is placed in to graduated cylinder, seals graduated cylinder with sealed membrane.In the time separating out liquid volume and reach 50ml, the time of consumption thinks to analyse the liquid transformation period, and the time of survey is 40min.When lather volume become firm foaming complete 50% time, the time of consumption is thought half foam life period, the time of survey is 15h.
Embodiment 2:
1) configuration of fluorescent dye solution
The water of getting resistivity that rhodamine B 0.1mg is placed in 100ml and be 18.2M Ω cm dissolves, warming-in-water to 40 DEG C, and magnetic agitation rotating speed 200rpm, time 1h, makes 100ml fluorescent dye solution.
2) preparation of modified silica nanoparticle
100g nano SiO 2 particle (silanol alkyl density 2/nm2) is warmed up to 160 DEG C of preheating 2h activation in reactor, add polydimethylsiloxane 15g and hexamethyl dichloro azane 25g, and add catalyzer Rhometal, by entering in reactor after 300 DEG C of vaporizations of vapourizing unit, with discharging after silicon dioxde reaction 30min, 0.5/the nm2 of density of silica particles silanol alkyl after modification, 85 ° of contact angles.
3) configuration of modified silica nanoparticle solution
Get modified silica nanoparticle 1.5g and be dissolved in above-mentioned 100ml dispersion liquid, ultrasonic 1.5h, 400rpm magnetic agitation 4h.8000rpm Centrifugal dispersion liquid, removes supernatant liquor, repeats 3 times, and after cleaning, water is dissolved to 100 parts again, makes dispersion liquid.
4) preparation of foam
Add SDBS0.2g in above-mentioned dispersion liquid, magnetic agitation 300rpm stirs 5 minutes.Solution is placed in to homogenizer and stirs 3min, rotating speed 8000rpm.Make stable dyeing inorganic nanoparticles composite foam system.
5) stability test of foam
Foam is placed in to graduated cylinder, seals graduated cylinder with sealed membrane, analysing the liquid transformation period is 28min, and half foam life period is 12h.
Embodiment 3:
1) configuration of fluorescent dye solution
The water of getting resistivity that FITC0.1mg is placed in 100ml and be 18.2M Ω cm dissolves, warming-in-water to 40 DEG C, and magnetic agitation rotating speed 200rpm1h, makes 100ml fluorescent dye solution.
2) preparation of modified silica nanoparticle
100g nano SiO 2 particle (silanol alkyl density 2/nm2) is warmed up to 160 DEG C of preheating 2h activation in reactor, add polydimethylsiloxane 30g and hexamethyl dichloro azane 25g, and add catalyzer Rhometal, by entering in reactor after 300 DEG C of vaporizations of vapourizing unit, with discharging after silicon dioxde reaction 45min, 0.3/the nm2 of density of silica particles silanol alkyl after modification, 120 ° of contact angles.
3) configuration of modified silica nanoparticle solution
Get modified silica nanoparticle 1.5g and be dissolved in above-mentioned 100ml fluorescent dye solution, ultrasonic 1h, ultrasonic 1h, 400rpm rotating speed stirs 4h.8000rpm Centrifugal dispersion liquid, removes supernatant liquor, repeats 5 times, and after cleaning, water is dissolved to 100 parts again, makes dispersion liquid.
4) preparation of foam
Add SDBS0.2g in above-mentioned dispersion liquid, magnetic agitation 300rpm stirs 5 minutes.Solution is placed in to homogenizer and stirs 3min, rotating speed 8000rpm.Make stable dyeing inorganic nanoparticles composite foam system.
5) stability test of foam
Foam is placed in to graduated cylinder, seals graduated cylinder with sealed membrane, analysing the liquid transformation period is 50min, and half foam life period is 17h.
Embodiment 4:
1) configuration of fluorescent dye solution
The water of getting resistivity that rhodamine B 0.1mg is placed in 100ml and be 18.2M Ω cm dissolves, warming-in-water to 40 DEG C, and magnetic agitation rotating speed 200rpm1h, makes 100ml fluorescent dye solution.
2) dyeing of nano SiO 2 particle solution
Before getting modification, (water contact angle is 20 ° to nano SiO 2 particle, silanol alkyl density 2/nm
2) 1.5g is dissolved in above-mentioned 100ml fluorescent dye solution, ultrasonic 1h, 400rpm rotating speed stirs 4h.8000rpm Centrifugal dispersion liquid, removes supernatant liquor, repeats 5 times, and after cleaning, water is dissolved to 100 parts again, makes dispersion liquid.
3) preparation of composite foam
Add SDBS0.2g in above-mentioned dispersion liquid, magnetic agitation 300rpm stirs 5 minutes.Solution is placed in to homogenizer and stirs 3min, rotating speed 8000rpm.Make dyeing nano SiO 2 particle composite foam system
4) stability test of foam
Foam is placed in to graduated cylinder, seals graduated cylinder with sealed membrane, analysing the liquid transformation period is 8min, and half foam life period is 10h.
The composite foam system solution that the present invention knows, fluorescence intensity is high, easily observation; And storage period is long, be difficult for cancellation.The foam of having manufactured, in the time that laser is inverted under Laser Scanning Confocal Microscope experiment Analysis, foam coalescence speed is very slow, substantially can reach a static equilibrium, thus the time period is analyzed and tests greatly.In addition, particle is very clear in experimental observation in the distribution situation of foam surface, and the tracking that can fix a point, for research silica dioxide granule provides strong technical support with the mechanism research of the collaborative steady bubble of tensio-active agent.
Claims (7)
1. a fluorescent silicon dioxide nano particle composite foam, is characterized in that, described composite foam includes modified silica nanoparticle, tensio-active agent, fluorescence dye.
2. composite foam as claimed in claim 1, is characterized in that, the mass ratio of described modified silica nanoparticle, tensio-active agent, fluorescence dye is 0.05-0.5:0.5-2:0.001-0.005.
3. composite foam as claimed in claim 1 or 2, it is characterized in that, the preparation method of described modified silica nanoparticle is as follows: nano SiO 2 particle is warmed up in reactor to 160 DEG C of preheating 2h activation, to after polydimethylsiloxane, 300 DEG C of vaporizations of hexamethyl dichloro azane Rhometal, enter in reactor again, after reaction 30min-60min, make.
4. composite foam as claimed in claim 3, is characterized in that, described fluorescence dye is isosulfocyanic acid fluorescence and/or rhodamine B.
5. composite foam as claimed in claim 3, is characterized in that, described tensio-active agent is Sodium dodecylbenzene sulfonate.
6. the preparation method of composite foam claimed in claim 3, it is characterized in that, described method is that modified silica nanoparticle is joined to ultrasonic in fluorescent dye solution, stirring, centrifugal wash-out, adds water and makes dispersion liquid, then complete preparation after adding tensio-active agent to stir to bubble after cleaning.
7. method as claimed in claim 4, is characterized in that, described method comprises following step:
1) preparation of fluorescent dye solution:
Get fluorescence dye and join in the water that resistivity is 18.2M Ω cm, warming-in-water to 40 DEG C, magnetic agitation rotating speed 200rpm1h, makes fluorescent dye solution;
2) modification of nano SiO 2 particle:
Nano SiO 2 particle is warmed up in reactor to 160 DEG C of preheating 2h activation, then will after polydimethylsiloxane, 300 DEG C of vaporizations of hexamethyl dichloro azane Rhometal, enters in reactor, after reaction 30min-60min, make;
3) dyeing of modified silica nanoparticle:
In fluorescent dye solution, add modified silica nanoparticle 0.5-2 part, ultrasonic 1-3h makes modified silica nanoparticle be combined with fluorescent dye solution, and 400rpm rotating speed stirs 4h, makes dispersion liquid even; 8000rpm Centrifugal dispersion liquid 15-30min, removes supernatant liquor, repeats 3-5 time, and after cleaning, water is dissolved to 100 parts again, makes dispersion liquid;
4) preparation of composite foam:
Getting tensio-active agent joins in dispersion liquid, to stir after bubbling and makes nano SiO 2 particle composite foam system.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201410327864.4A CN104099076B (en) | 2014-07-10 | 2014-07-10 | A kind of oil gas field fluorescent silicon dioxide nano-particles reinforcement foam system |
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|---|---|---|---|
| CN201410327864.4A CN104099076B (en) | 2014-07-10 | 2014-07-10 | A kind of oil gas field fluorescent silicon dioxide nano-particles reinforcement foam system |
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| CN104099076B CN104099076B (en) | 2016-09-28 |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108300447A (en) * | 2018-02-09 | 2018-07-20 | 上海大学 | A kind of nano particle foam system and preparation method thereof improving oil displacement efficiency |
| CN111982763A (en) * | 2020-08-17 | 2020-11-24 | 上海普康药业有限公司 | Method for determining particle size and particle size distribution of coenzyme Q10 |
| CN114352244A (en) * | 2022-01-14 | 2022-04-15 | 中国石油大学(北京) | Method for evaluating capability of nanoparticles with different interface properties for improving crude oil recovery efficiency based on fluorescent tracing |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101280189A (en) * | 2008-05-23 | 2008-10-08 | 上海师范大学 | Preparation of red fluorescent powder Zn2SiO4:Eu3+ |
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Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101280189A (en) * | 2008-05-23 | 2008-10-08 | 上海师范大学 | Preparation of red fluorescent powder Zn2SiO4:Eu3+ |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108300447A (en) * | 2018-02-09 | 2018-07-20 | 上海大学 | A kind of nano particle foam system and preparation method thereof improving oil displacement efficiency |
| CN111982763A (en) * | 2020-08-17 | 2020-11-24 | 上海普康药业有限公司 | Method for determining particle size and particle size distribution of coenzyme Q10 |
| CN114352244A (en) * | 2022-01-14 | 2022-04-15 | 中国石油大学(北京) | Method for evaluating capability of nanoparticles with different interface properties for improving crude oil recovery efficiency based on fluorescent tracing |
| CN114352244B (en) * | 2022-01-14 | 2022-10-18 | 中国石油大学(北京) | Method for evaluating capability of nanoparticles with different interface properties for improving crude oil recovery efficiency based on fluorescent tracing |
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