CN108410441A - Based on the strengthening foam system and preparation method thereof that the collaboration of graphite oxide particle is stable - Google Patents
Based on the strengthening foam system and preparation method thereof that the collaboration of graphite oxide particle is stable Download PDFInfo
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- 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
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- 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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- 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
- C09K8/594—Compositions used in combination with injected gas, e.g. CO2 orcarbonated gas
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Abstract
The invention discloses a kind of strengthening foam systems and preparation method thereof stable based on the collaboration of graphite oxide particle, belong to Oil-Gas Field Development Engineering technical field.The strengthening foam system stable based on the collaboration of graphite oxide particle is made of following parts by weight of component：0.3~0.7 part of cationic surfactant, 0.1~0.3 part of stabilizer, 0.2~0.5 part of graphite oxide particle, 100 parts of water；Wherein, cationic surfactant is cetyl trimethylammonium bromide.The strengthening foam system stable based on the collaboration of graphite oxide particle provided by the invention, stability is excellent, environment friendly and pollution-free, and preparation process is simple, can significantly improve oil recovery rate.
Description
Technical field
The present invention relates to Oil-Gas Field Development Engineering technical fields, particularly relate to a kind of based on graphite oxide particle collaboration stabilization
Strengthening foam system and preparation method thereof.
Background technology
Foam flooding is widely used as a kind of technological means improving oil recovery factor, has there is nearly application in 60 years so far
History.Foam can cause the reduction of gas phase relative permeability, delay gas fingering.Foam quality is to determine foam flooding efficiency
Key factor, however foam, as a kind of thermodynamically unstable dispersion, this unstability applies band to foam
Tremendous influence is carried out.Scholars both domestic and external have carried out numerous studies around how improving foam stability, it was also proposed that many
Method.
It is a kind of important method to research and develop novel foaming agent.Surface-active is concentrated mainly on to the research and development of foaming agent at present
The synthesis of agent or compounding.Research before finds that the alkyl chain appropriate that extends helps to increase the stability of foam.Since surface is lived
The limitation of property agent itself chemical characteristic, although enough foaming volumes can be generated, its stability is poor.In order to increase gas
The polymer such as polyacrylamide, albumen, polypeptide are added in the stability of bubble in foaming agent, by improving the viscosity of base fluid, reduce
Bubble mobility, to achieve the effect that foam stabilizing.
Chinese patent document ZL201210223060.0 discloses a kind of composite foam of oil gas field addition nano particle
System and preparation method thereof.Composite foam system is by anion surfactant, modified silica nanoparticle, counter ion salt
And water composition.The foam generated using the composite foam system, blistering longer than the half foam life period that conventional surfactants are stablized
Volume is big；But nano particle preparation process used is complicated in the system, involves great expense, it can not be in the big rule in oil-gas field development field
Mould application.
Chinese patent document ZL201510600689.6 discloses a kind of oil gas field novel inorganic subparticle enhanced foam
Foam system and preparation method thereof.Novel inorganic subparticle used in this method is that the μ of the grain size that screens≤2.5 is trapped in air
The fine particle of m, the surfactant compound formed with sasanguasaponin and sodium lauroyl glutamate form stable foam system.
Such subparticle derives from a wealth of sources, mostly coal-burning power plant's solid waste, it can be realized by being applied to agent for improving oilfield recovery
Recycling, but such subparticle is influenced more apparent, ingredient by each batch coal kind, ingredient and burning degree
It forms complex changeable so that it cooperates with the effect of stable foam to be difficult to control with surfactant compound.
Invention content
The technical problem to be solved in the present invention is to provide it is a kind of it is at low cost, performance is stable, preparation method is simply based on oxygen
The stable strengthening foam system and preparation method thereof of graphite particle collaboration.
In order to solve the above technical problems, present invention offer technical solution is as follows：
On the one hand, a kind of strengthening foam system stable based on the collaboration of graphite oxide particle is provided, by following parts by weight
Group is grouped as：0.3~0.7 part of cationic surfactant, 0.1~0.3 part of dispersant, 0.2~0.5 part of graphite oxide particle,
100 parts of water；
Wherein, cationic surfactant is cetyl trimethylammonium bromide, and graphite oxide particle is through ultrasonication point
It dissipates for the smaller oxidized graphite flake of scale, uniform and stable is dispersed in water, and surface is negatively charged, cetyl trimethylammonium bromide
It is positively charged in aqueous solution, cetyl trimethylammonium bromide is adsorbed onto by graphite oxide particle surface by electrostatic interaction；Ten
The hydrophobic segment of six alkyl trimethyl ammonium bromides stretches to aqueous solution, increases oxidized graphite flake hydrophobic properties of the surface.
Preferably, the dispersant is sodium lignin sulfonate；Sodium lignin sulfonate as a kind of high molecular polymer skeleton,
The surrounding graphene particles of tridimensional network is formed, the drain of foam is further decreased, to improve the stability of foam.
Preferably, the water is distilled water.
Preferably, the graphite oxide particle is 100 mesh flaky graphites, and grain size is 3-5 μm, and the angle of wetting to water is
30 °~50 °.
Graphite oxide particle used in the present invention can be commercial product, can also be prepared through Hummers methods,
The specific method is as follows：
Step 1：It is put into large beaker in ice-water bath, the 110mL concentrated sulfuric acids are added, is stirred on magnetic stirring apparatus, is put into temperature
Degree meter allows its temperature to be down to 4 DEG C or so；
Step 2：Add 100 mesh flaky graphite 5g, adds 2.5g sodium nitrate, be then slowly added into 15g potassium permanganate, add
When complete postscript, 90min is stirred to react on magnetic stirring apparatus, solution changes tepidarium, temperature control into purple green, by ice-water bath
At 32 DEG C~40 DEG C, 30min is reacted, solution is in purple green；
Step 3：After reaction terminates, 220mL deionized waters are slowly added to, heating keeps 70~100 DEG C or so of temperature, delays
The slow mass concentration that is added is that 5% hydrogen peroxide is reacted, and reaction solution color becomes golden yellow；
Step 4：Solution after reaction repeatedly centrifuges in centrifuge, is washed with water, until sulfate radical-free ion in solution,
Drying graphite oxide particle at a temperature of 40~50 DEG C.
On the other hand, the present invention also provides the above-mentioned preparations based on the stable strengthening foam system of graphite oxide particle collaboration
Method, including：
Step 1：Graphite oxide particle is added to the water and carries out ultrasonic disperse, obtains sheet graphite oxide dispersion；
Step 2：Cetyl trimethylammonium bromide and lignosulfonates are added to the graphite oxide point that step 1 obtains
In dispersion liquid, stirring obtains compounding dispersion liquid；
Step 3：Compounding dispersion liquid is stirred with Waring Blender methods, after generation foam to obtain the final product.
Preferably, in the step 1, graphite oxide particle uses 100 mesh flaky graphites, 3-5 μm of grain size, to the profit of water
Wet angle is 30 °~50 °；The mass concentration of graphite oxide is 0.2~0.5wt.%；The sheet that step 1 is prepared aoxidizes stone
Black preferable particle size is 0.5-2 μm, thickness in monolayer 1-3nm.Graphite oxide has outstanding heat resistance, so the present invention provides
Strengthening foam system have stronger temperature tolerance.
Preferably, in the step 1, the condition of ultrasonic disperse is time 2h, ultrasonic power 500-1000W.
Preferably, in the step 2, when the mass concentration of cetyl trimethylammonium bromide is 0.3~0.7wt.%, oxygen
The contact angle of fossil ink sheet and water is 80 °~90 °, and this graphite oxide thin slice with certain hydrophobic property can be irreversible
Be adsorbed onto on bubble interface liquid film, and by flocculation reaction, form one layer of compacted zone on interface, increase bubble film
Viscoplasticity, reduce drain and the gas diffusion of foam.
Preferably, the mass concentration of lignosulfonates is 0.1~0.3wt.%.
Preferably, in the step 2, the condition of stirring is 25 DEG C -30 DEG C of temperature, time 0.5-1h.
Preferably, in the step 2, it is 80 °~90 ° to compound the contact angle of sheet graphite oxide and water in dispersion liquid.
Preferably, it in the step 3, is stirred 3 minutes with the speed of 8000rpm in Waring Blender methods, air source is
Air, nitrogen or carbon dioxide gas.
The invention has the advantages that：
In said program, the present invention obtains stabilization using cationic surfactant and graphite oxide particle preparation for the first time
Foam system increases the hydrophobic performance of graphite oxide particle, irreversible can be adsorbed onto on bubble interface liquid film, and lead to
Cross flocculation reaction, on interface formed one layer of compacted zone, increase the viscoplasticity of bubble film, reduce foam drain and
Gas diffusion；With the use of lignosulfonates, graphite oxide particle is set to form tridimensional network in solution phase, further
The drain for reducing foam, to improve the stability of foam；And the present invention is at low cost, preparation process is simple, indoor simulation can be shown
It writes and improves recovery ratio.
Description of the drawings
Fig. 1 is that the graphite oxide particle ultrasonic disperse of the present invention is lamella layered graphite oxide schematic diagram；
Fig. 2 is the scanning electron microscope image of the graphite oxide particle used in the embodiment of the present invention 2；
Fig. 3 is the images of transmissive electron microscope of the sheet graphite oxide obtained in 2 preparation method step 1 of the embodiment of the present invention.
Specific implementation mode
To keep the technical problem to be solved in the present invention, technical solution and advantage clearer, below in conjunction with attached drawing and tool
Body embodiment is described in detail.
The present invention is directed to problem of high cost in the prior art and foam system stability difference, provides a kind of based on oxygen
The stable strengthening foam system and preparation method thereof of graphite particle collaboration.
Embodiment 1
The preparation method of graphite oxide particle, including：
Step 1：It is put into large beaker in ice-water bath, the 110mL concentrated sulfuric acids are added, is stirred on magnetic stirring apparatus, is put into temperature
Degree meter allows its temperature to be down to 4 DEG C or so；
Step 2：Add 100 mesh flaky graphite 5g, adds 2.5g sodium nitrate, be then slowly added into 15g potassium permanganate, add
When complete postscript, 90min is stirred to react on magnetic stirring apparatus, solution changes tepidarium, temperature control into purple green, by ice-water bath
At 32 DEG C~40 DEG C, 30min is reacted, solution is in purple green；
Step 3：After reaction terminates, 220mL deionized waters are slowly added to, heating keeps 70~100 DEG C or so of temperature, delays
The slow mass concentration that is added is that 5% hydrogen peroxide is reacted, and reaction solution color becomes golden yellow；
Step 4：Solution after reaction repeatedly centrifuges in centrifuge, is washed with water, until sulfate radical-free ion in solution,
Drying graphite oxide particle at a temperature of 40~50 DEG C.
It is 3.5 μm by the graphite oxide mean particle size that SEM is measured, its profit to water is measured based on sessile drop method
Wet angle is 35 °.
It should be noted that inventor is by verification, preferred 3-5 μm of the grain size of graphite oxide particle, to the angle of wetting of water
For within the scope of 30 °~50 °, self-control graphite oxide particle is with commercially available graphite oxide particle (3-5 μm of grain size, 45 ° of angle of wetting) to strong
The influence difference for changing foam system is small, and cost, the graphite oxide particle that the present invention uses are purchased from Nanjing in order to save time
Xian Feng Nanosolutions GmbH.
Embodiment 2
Based on the strengthening foam system that the collaboration of graphite oxide particle is stable, it is grouped as by the group of following parts by weight：Hexadecane
0.7 part of base trimethylammonium bromide, 0.1 part of lignosulfonates, 0.3 part of graphite oxide particle, 100 parts of water.
Based on the preparation method of the stable strengthening foam system of graphite oxide particle collaboration, including：
Step 1：It it is 3-5 μm by grain size, the graphite oxide particle 0.3g that the angle of wetting to water is 30 °~50 ° is added to
In 100g water, ultrasonic disperse 2h, ultrasonic power 800W are carried out at 30 DEG C, it is 0.5-2 μm to obtain grain size, thickness in monolayer 1-
The sheet graphite oxide dispersion of 3nm；
Step 2：By 0.7g cetyl trimethylammonium bromides and 0.1g
Lignosulfonates are added in the graphite oxide dispersion that step 1 obtains, and 1h is stirred at 30 DEG C, are stood
10min obtains compounding dispersion liquid, and it is about 85 ° to compound the contact angle of sheet graphite oxide and water in dispersion liquid；
Step 3：Dispersion liquid will be compounded to be prepared within 3 minutes surely with the speed stirring of 8000rpm with Waring Blender methods
Fixed air foam to get.
Embodiment 3
Based on the strengthening foam system that the collaboration of graphite oxide particle is stable, it is grouped as by the group of following parts by weight：Hexadecane
0.7 part of base trimethylammonium bromide, 0.1 part of lignosulfonates, 0.3 part of graphite oxide particle, 100 parts of water.
Preparation method based on the stable strengthening foam system of graphite oxide particle collaboration, which is removed, uses Waring Blender
It is nitrogen that air source, which uses, in method whipping process, other steps are identical with embodiment 2.
Embodiment 4
Based on the strengthening foam system that the collaboration of graphite oxide particle is stable, it is grouped as by the group of following parts by weight：Hexadecane
0.5 part of base trimethylammonium bromide, 0.3 part of lignosulfonates, 0.3 part of graphite oxide particle, 100 parts of water.
Preparation method based on the stable strengthening foam system of graphite oxide particle collaboration is identical with embodiment 3.
Since length is limited, the advantageous effect obtained in order to further illustrate the present invention, only by taking embodiment 3 as an example, setting
Relevant comparative example carries out performance verification.Can it be led to unless otherwise specified using reagent and material in embodiment and comparative example
Commercial sources are crossed to obtain.It should be pointed out that for those skilled in the art, in the premise for not departing from principle of the present invention
Under, it can also make several improvements and retouch, these improvements and modifications also should be regarded as protection scope of the present invention.
Comparative example 1
Foam system is grouped as by the group of following parts by weight：0.7 part of cetyl trimethylammonium bromide, graphite oxide
0.3 part of grain, 100 parts of water.
The preparation method of foam system includes：
Step 1：It it is 3-5 μm by grain size, the graphite oxide particle 0.3g that the angle of wetting to water is 30 °~50 ° is added to
In 100g water, ultrasonic disperse 2h, ultrasonic power 800W are carried out at 30 DEG C, it is 0.5-2 μm to obtain grain size, thickness in monolayer 1-
The sheet graphite oxide dispersion of 3nm；
Step 2：0.7g cetyl trimethylammonium bromides are added in the graphite oxide dispersion that step 1 obtains,
1h is stirred at 30 DEG C, stands 10min, is obtained compounding dispersion liquid, is compounded the contact angle of sheet graphite oxide and water in dispersion liquid
About 85 °；
Step 3：Dispersion liquid will be compounded to be stirred 3 minutes with the speed of 8000rpm with Waring Blender methods, whipping process
The middle nitrogen that is continually fed into tank body is to get stable nitrogen foam.
Comparative example 2
Foam system is grouped as by the group of following parts by weight：0.1 part of lignosulfonates, 0.3 part of graphite oxide particle,
100 parts of water.
The preparation method of foam system includes：
Step 1：It it is 3-5 μm by grain size, the graphite oxide particle 0.3g that the angle of wetting to water is 30 °~50 ° is added to
In 100g water, ultrasonic disperse 2h is carried out at 30 DEG C, ultrasonic power 800W obtains graphite oxide dispersion；
Step 2：0.1g lignosulfonates are added in the graphite oxide dispersion that step 1 obtains, are stirred at 30 DEG C
1h is mixed, 10min is stood, obtains compounding dispersion liquid, it is about 45 ° to compound the contact angle of sheet graphite oxide and water in dispersion liquid；
Step 3：Dispersion liquid will be compounded to be stirred 3 minutes with the speed of 8000rpm with Waring Blender methods, whipping process
The middle nitrogen that is continually fed into tank body is to get stable nitrogen foam.
Comparative example 3
Foam system is grouped as by the group of following parts by weight：0.7 part of cetyl trimethylammonium bromide, lignin sulfonic acid
0.1 part of salt, 100 parts of water.
Step 1：0.7g cetyl trimethylammonium bromides and 0.1g lignosulfonates are added in 100g water, 30
1h is stirred at DEG C, stands 10min；
Step 3：It is stirred 3 minutes with the speed of 8000rpm with Waring Blender methods, is held into tank body in whipping process
It is continuous to be passed through nitrogen to get stable nitrogen foam.
Comparative example 4
Foam system is grouped as by the group of following parts by weight：0.7 part of cetyl trimethylammonium bromide, lignin sulfonic acid
0.1 part of salt, 100 0.3 part of mesh flaky graphites, 100 parts of water.
The preparation method of foam system, it is same as Example 3.
Comparative example 5
Foam system is grouped as by the group of following parts by weight：0.7 part of neopelex, lignosulfonates 0.1
Part, 100 0.3 part of mesh flaky graphites, 100 parts of water.
The preparation method of foam system, it is same as Example 3.
The foaming characteristic of product and estimation of stability use conventional laboratory methods Waring in embodiment and comparative example
Blender methods measure.
Waring Blender paddling process is one of common stirring means, and the bubble of foaming agent is measured frequently with the method
Ability and the stability for forming foam, paddling process measure foaming agent performance using high speed agitator.Quantitative foaming agent solution is fallen
Enter in graduated cylinder, certain speed stirs the regular hour, and record stops foam volume V when stirring0(mL) and half is precipitated in foam
Time (becoming half-life period) t when liquid0.5(s), V is used0It indicates bubbling ability, uses t0.5Indicate foam stability.
Take 100ml foam liquids that Waring Blender methods is used to be stirred 3 minutes with the speed of 8000rpm, stirring is completed
Foam is poured into 1000mL graduated cylinders afterwards, liquid in the initial volume and foam of foam is recorded at normal temperatures and pressures and 50mL institutes is precipitated
Time, it may be verified that the stability of foam.
The foaming volume of foam system prepared by above-described embodiment 2-4 and comparative example 1-5 and the performance number for analysing liquid half-life period
According to being shown in Table 1.
Table 1
As seen from the above table, the strengthening foam system stable based on the collaboration of graphite oxide particle for inventing offer, has excellent
Frothing capacity and half-life it is long, bubble stability can good feature.
The above is the preferred embodiment of the present invention, it is noted that for those skilled in the art
For, without departing from the principles of the present invention, it can also make several improvements and retouch, these improvements and modifications
It should be regarded as protection scope of the present invention.
Claims (10)
1. a kind of strengthening foam system stable based on the collaboration of graphite oxide particle, which is characterized in that by the group of following parts by weight
It is grouped as：0.3~0.7 part of cationic surfactant, 0.1~0.3 part of dispersant, 0.2~0.5 part of graphite oxide particle, water
100 parts；
Wherein, cationic surfactant is cetyl trimethylammonium bromide.
2. the strengthening foam system stable based on the collaboration of graphite oxide particle according to claim 1, which is characterized in that institute
It is sodium lignin sulfonate to state dispersant；The water is distilled water.
3. the strengthening foam system stable based on the collaboration of graphite oxide particle according to claim 1, which is characterized in that institute
It is 100 mesh flaky graphites to state graphite oxide particle, and grain size is 3-5 μm, and the angle of wetting to water is 30 °~50 °.
4. any preparation methods based on the stable strengthening foam system of graphite oxide particle collaboration of claim 1-3,
It is characterised in that it includes：
Step 1：Graphite oxide particle is added to the water and carries out ultrasonic disperse, obtains sheet graphite oxide dispersion；
Step 2：Cetyl trimethylammonium bromide and sodium lignin sulfonate are added to the graphite oxide dispersion that step 1 obtains
In, stirring obtains compounding dispersion liquid；
Step 3：Compounding dispersion liquid is stirred with Waring Blender methods, after generation foam to obtain the final product.
5. the preparation method according to claim 4 based on the stable strengthening foam system of graphite oxide particle collaboration,
It is characterized in that, in the step 1, the mass concentration of graphite oxide is 0.2~0.5wt.%.
6. the preparation method according to claim 4 based on the stable strengthening foam system of graphite oxide particle collaboration,
It is characterized in that, in the step 1, the condition of ultrasonic disperse is time 2h, ultrasonic power 500-1000W.
7. the preparation method according to claim 4 based on the stable strengthening foam system of graphite oxide particle collaboration,
It is characterized in that, in the step 2, the mass concentration of cetyl trimethylammonium bromide is 0.3~0.7wt.%；Lignin sulfonic acid
The mass concentration of sodium is 0.1~0.3wt.%.
8. the preparation method according to claim 4 based on the stable strengthening foam system of graphite oxide particle collaboration,
It is characterized in that, in the step 2, the condition of stirring is 25 DEG C -30 DEG C of temperature, time 0.5-1h.
9. the preparation method according to claim 4 based on the stable strengthening foam system of graphite oxide particle collaboration,
It is characterized in that, in the step 2, it is 80 °~90 ° to compound the contact angle of sheet graphite oxide and water in dispersion liquid.
10. the preparation method according to claim 4 based on the stable strengthening foam system of graphite oxide particle collaboration,
It is characterized in that, in the step 3, stirred 3 minutes with the speed of 8000rpm in Waring Blender methods, air source is air, nitrogen
Gas or carbon dioxide gas.
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| CN109456747A (en) * | 2018-10-29 | 2019-03-12 | 中国石油大学(华东) | The production system and method for the high stability foam of graphitiferous particle |
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| CN116102335A (en) * | 2023-04-13 | 2023-05-12 | 天津冶建特种材料有限公司 | Foaming composition, purple clay pug and preparation method thereof |
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