CN114736664B - Nanometer titanium dioxide solid particle emulsifier and preparation method thereof - Google Patents
Nanometer titanium dioxide solid particle emulsifier and preparation method thereof Download PDFInfo
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Abstract
The invention provides a nano titanium dioxide solid particle emulsifier and a preparation method thereof, and the nano titanium dioxide solid particle emulsifier is prepared by the method comprising the following steps: dissolving titanium dioxide in absolute ethyl alcohol, and performing ultrasonic treatment to obtain dispersion; adding a phthalate coupling agent into the dispersion liquid for chemical grafting; heating and stirring to react for a period of time, adding a certain amount of bromoalkane, and heating and stirring for a certain period of time; and after heating and stirring are finished, carrying out suction filtration and drying to obtain the nano oleophylic titanium dioxide solid particle emulsifier. The nano-emulsifier can form stable water-in-oil emulsion through the shearing action of stratum under the condition of 10-80% of water saturation of oil deposit, the viscosity of the emulsion is 1.5-22 times of the viscosity of crude oil, the viscosity of the emulsion is in direct proportion to the water saturation of oil deposit in the water saturation range of oil deposit, and the high-viscosity emulsion formed under the high water content condition can block the dominant channel so as to achieve the purposes of controlling the fluidity and stabilizing the drainage and driving front edge and improve the recovery ratio of crude oil.
Description
Technical Field
The invention relates to the technical field of oilfield chemistry, in particular to a nano titanium dioxide solid particle emulsifier capable of forming high internal phase high viscosity emulsion in a high permeability area of an oil reservoir and a preparation method thereof.
Background
In heterogeneous reservoirs, water flooding can lead to severe fingering, i.e., the seepage velocity of injected water is far faster than that of crude oil due to in-situ heterogeneity and oil-water viscosity differences, forming a dominant channel between the injection well and the production well, ultimately resulting in the majority of the reservoir area after water flooding not being affected by water waves and [ ALMANSOUR a O, alqurashi a, alhulsinan S N, et al efficiency pf Enhanced Oil Recovery Using Polymer-ugmented Low Salinity Flooding [ J ] Journal of Petroleum Exploration & Production Technology,2017,7 (1): 1149-1158 ]. The conventional polymer oil displacement agent has the problems that the viscosity of the conventional polymer oil displacement agent is reduced too fast and the conventional polymer oil displacement agent needs to be added for use in high-salinity oil reservoirs, so that the cost is increased, and degradation failure and the like can occur in high-temperature oil reservoirs; the surfactant is easily adsorbed on the surface of oil reservoir rock, and meanwhile, under the influence of high-temperature and high-salt oil reservoir conditions, the stability of emulsion formed by the surfactant is greatly reduced, so that the fluidity control capability of the emulsion has a certain degree of limitation (Zhao Fangjian, wang Lijuan, xia ran.
In recent years, researchers focus on the research of newer nano materials, and the nano materials can be adsorbed on an oil-water interface to form Pickering emulsion through modification treatment. Indoor and field tests prove that Pickering emulsion can be injected for a long time, can be kept stable in the flowing process, and can remarkably improve the recovery ratio (Kaminsky R D, wattenberger R C, lederhos J P, et al, visual oil recovery using solids-stabilized emulsions [ C ]// SPE Annual Technical Conference and Exhibition. Florence: SPE,2010:SPE No.135284.). Shalma et al validated Pickering emulsions formulated using a thickened aqueous phase, with a 5% increase in cumulative recovery. (Shalma T, velmurugan N, patel P, et al use of oil-in-water Pickering emulsion stabilized by nanoparticles in combination with polymer flood for enhanced oil recovery [ J ]. Hat Sci technology, 2015, 33 (17/18): 1959-1604.) nanoparticle stabilized emulsion types are primarily affected by nanoparticle wettability, when θ < 90 °, the nanoparticles appear hydrophilic, forming O/W type emulsions; when θ > 90 °, nanoparticle wettability appears to be lipophilic, forming W/O emulsions (Binks B P, lumsdon s.langmuir, 2000, 16 (23), 862.). However, the type of emulsion is not only related to the emulsifier but also to the oil-water ratio, even if the lipophilic nanoparticles are too high in water content, they are still capable of forming O/W type emulsions, and therefore, a higher phase transition point of the corresponding emulsifier is required.
The emulsion formed by the nano particles solves the problem of poor stability of the emulsion formed by the traditional surfactant, can still keep stable under some severe oil reservoir conditions, and has strong fluidity control capability, so that the emulsion has very good application potential in the field of improving the recovery rate of crude oil. At present, few researches on forming emulsion by single nano particles are carried out, and the emulsion is mostly generated by adopting the synergistic effect of a surfactant and nano particles. Meanwhile, the phase change point of the finally formed emulsion is low, and the application range is relatively narrow.
Disclosure of Invention
The invention provides a preparation method of a nano titanium dioxide solid particle emulsifier, which is simple and can be industrialized, and the prepared nano solid particle emulsifier can form emulsion with viscosity in proportion to water saturation under the condition of a certain water saturation of an oil reservoir, so that the purpose of plugging a dominant channel and improving recovery ratio is achieved.
In order to achieve the above object, the technical scheme of the present invention is as follows: the preparation method of the nano titanium dioxide solid particle emulsifier comprises the following steps:
(1) Adding nano titanium dioxide into absolute ethyl alcohol and performing ultrasonic dispersion to obtain a dispersion liquid;
(2) Adding a phthalate coupling agent into the dispersion liquid and enabling the phthalate coupling agent to perform a coupling reaction with the titanium dioxide, wherein the coupling agent is 0.08-0.15 times of the mass of the nano titanium dioxide in percentage by mass;
(3) Dripping the lengthened bromoalkane into the reaction liquid obtained in the step (2), maintaining stirring in the dripping process, and reacting for 10-12 h at 60-70 ℃ under the condition of continuous stirring after the dripping is finished; the long-chain bromoalkane is obtained by separating and purifying the nano titanium dioxide after the reaction is completed, wherein the adding amount of the long-chain bromoalkane is 1-2 times of the adding amount of the nano titanium dioxide.
In one embodiment of the present invention, in the step (1), the titanium dioxide is hydrophilic titanium dioxide having a diameter of 20 to 100nm, and the amount of the titanium dioxide added is 0.02 to 0.05 times that of the absolute ethyl alcohol in terms of mass percent.
In one embodiment of the present invention, in the step (1), the preparation time of the dispersion liquid is 20 to 40 minutes.
In one embodiment of the present invention, in the step (2), the reaction temperature is 60 to 70 ℃ and the reaction time is 10 to 12 hours.
One embodiment of the invention is that in the step (2), the titanate coupling agent is one or more of isopropyl tri (dioctyl pyrophosphoryl oxy) titanate, bis (dioctyl pyrophosphoryl oxy) ethylene titanate and isopropoxydioic acid acyloxy (dioctyl phosphoric acid acyloxy) titanate;
one embodiment of the present invention is that in step (3), the long-chain bromoalkane is at least one of bromododecane, bromotetradecane, or bromohexadecane.
One embodiment of the invention is characterized in that the specific operation of separation and purification is as follows: filtering the reacted product, washing with absolute ethyl alcohol for several times, vacuum drying the filter cake after separation, and crushing after drying.
Another object of the present invention is to disclose a nano-solid particle emulsifier, which is prepared by any of the above methods. The emulsifier can form water-in-oil emulsion with high viscosity and high internal phase, and can improve oil displacement efficiency.
The beneficial effects are that: the invention introduces long-chain alkane on the surface of titanium dioxide through a coupling agent, thereby synthesizing a nano solid particle emulsifier. As an emulsifier, a high internal phase emulsion of high viscosity can be formed relative to conventional surfactant emulsifiers; meanwhile, the synthesis method is simple and has strong industrialization.
Drawings
FIG. 1 is an oil-water-solid three-phase contact angle plot of modified nanoparticle emulsified particles;
FIG. 2 is a microscopic view of nanoemulsions forming a water-in-oil Pickering emulsion;
Detailed Description
The following detailed description of the invention will be clearly and fully described in connection with the examples which are set forth to illustrate, but are not necessarily all embodiments of the invention.
The invention is further described below with reference to examples:
example 1
(1) To the reagent bottle were added 100g of absolute ethanol and 3g of hydrophilic titanium dioxide, and the mixture was sonicated for 30 minutes to prepare a dispersion.
(2) 0.3g of isopropyl tri (dioctyl pyrophosphoryloxy) titanate (commercially available from Nanjing Netherlands New Material Co., ltd.) was added to the dispersion, and the mixture was heated and stirred in an oil bath at 65℃for 12 hours.
(3) 3g of bromododecane is dripped into the dispersion liquid in the step 2, and a reagent bottle is rocked in the dripping process, so that the uniform mixing of a reaction system is ensured; heating and stirring in an oil bath at 65 ℃ for 12 hours, and after the reaction is finished, carrying out suction filtration and washing treatment on the product, and drying and grinding to obtain the nano solid particle emulsifier S1.
Example 2
(1) To the reagent bottle were added 100g of absolute ethanol and 3g of hydrophilic titanium dioxide, and the mixture was sonicated for 30 minutes to prepare a dispersion.
(2) 0.3g of bis (dioctyl pyrophosphoryloxy) ethylene titanate (commercially available from Nanjing New Material technology Co., ltd.) was added to the dispersion, and the mixture was heated in an oil bath at 65℃and stirred for 12 hours.
(3) 3g of bromododecane is dripped into the dispersion liquid in the step 2, and a reagent bottle is rocked in the dripping process, so that the uniform mixing of a reaction system is ensured; heating in 65 deg.C oil bath, and stirring for 12 hr. And after the reaction is finished, carrying out suction filtration, washing treatment, drying and grinding on the product to obtain the nano solid particle emulsifier S2.
Example 3
(1) To the reagent bottle were added 100g of absolute ethanol and 3g of hydrophilic titanium dioxide, and the mixture was sonicated for 30 minutes to prepare a dispersion.
(2) 0.3g of isopropoxydioxydioleate (dioctyl phosphoryloxy) titanate (available from Nanjing Netherlands materials technology Co., ltd.) was added to the dispersion, and the mixture was heated in an oil bath at 65℃and stirred for 12 hours.
(3) 3g of bromohexadecane is dripped into the dispersion liquid in the step 2, and the reagent bottle is rocked in the dripping process, so that the uniform mixing of the reaction system is ensured; heating in 65 deg.C oil bath, and stirring for 12 hr. And after the reaction is finished, carrying out suction filtration, washing treatment, drying and grinding on the product to obtain the nano solid particle emulsifier S3.
Comparative example 1
As a comparison with the grafting of long chains on nanosilica by means of silane coupling agents, this was added as a control.
(1) To the flask, 100g of absolute ethanol and 3g of hydrophilic silica were added, and the mixture was sonicated for 30 minutes to prepare a dispersion.
(2) 0.3g of a silane coupling agent KH-570 was added to the dispersion, and the mixture was heated in an oil bath at 65℃and stirred for 12 hours.
(3) 3g of bromotetradecane is dripped into the dispersion liquid in the step 2, and a reagent bottle is rocked in the dripping process, so that the uniform mixing of a reaction system is ensured; heating in 65 deg.C oil bath, and stirring for 12 hr. And after the reaction is finished, carrying out suction filtration, washing treatment, drying and grinding on the product to obtain the nano solid particle emulsifier D1.
To illustrate the effect of the nano-solid particle emulsifier prepared in the examples of the present invention, performance tests were performed as follows.
1. Wettability test
The nanoemulsions synthesized in examples 1 to 4 were uniformly spread on a quartz glass slide, and the oil-water-solid three-phase contact angle of the nanoemulsions was measured using a HARHE-SPCA contact angle meter (Haako, china) under kerosene environment, as shown in fig. 1. Nanoemulsion examples 1-3 demonstrated the hydrophobicity of nanoemulsions with contact angles of 135.5 °, 132.3 °, and 139.7 °, respectively. Example 4, which is a control group, had a contact angle of 109.8 deg., and was slightly less hydrophobic than the nanoemulsion of the present invention.
2. Ability of nanoemulsifier dispersions to emulsify crude oil (different oil to water ratios)
The nanoemulsions synthesized in examples 1 to 4 are respectively added into formation water (the formation water is NaHCO3 and the mineralization degree is 5054 mg/L) to prepare the nanoemulsion with the mass concentration of 0.06%, and the nanoemulsion dispersion is obtained after ultrasonic dissolution for 10 minutes. In a special measuring cylinder with a measuring range of 50mL, the nano-emulsifier dispersion liquid and the de-aerated crude oil (viscosity of 84.2 mPa.s under the conditions of 30 ℃ and a shear rate of 7.336s < -1 >) are mixed according to a water-oil volume ratio of 1: 9. 2:8, 3:7, 4:6, 5:5, 6:4, 7:3, 8:2, 9:1 total volume of 20mL mixing, sealing; then, the mixture was stirred in a water bath at 30℃for 30 minutes, the emulsification was observed, and the water content of the emulsion was calculated as shown in Table 1. It can be observed that the nanoemulsions of examples 1 to 3 still have good emulsifying properties under 90% aqueous conditions, the resulting emulsion having a water content of more than 80%. While the emulsion water content of the long-chain nano-silica grafted by the silane coupling agent in the example 4 can only reach 70%, the effect of the nano-solid particle emulsifier for emulsifying crude oil is better than that of the long-chain nano-silica grafted by the silane coupling agent.
The inventor analyses that the phenomenon is mainly caused by the fact that the nano silicon dioxide has low density relative to nano titanium dioxide, and even if a hydrophobic long chain is grafted, the nano silicon dioxide still has slight agglomeration phenomenon, so that the effect of the nano silicon dioxide is poor; meanwhile, the titanate coupling agent is provided with a plurality of hydrophobic groups, so that after long-chain hydrophobic alkane is grafted, the hydrophobic effect is enhanced, and the final effect is better.
TABLE 1 Water/oil ratio of emulsion Water ratio of Water, nanoemulsifier Dispersion and crude oil
3. The nanometer emulsifier dispersion liquid and crude oil form the viscosity of emulsion (different oil-water ratio)
The nanoemulsions synthesized in examples 1 to 4 are respectively added into stratum water to prepare nanoemulsions with mass concentration of 0.06%, and the nanoemulsions are dissolved for 10 minutes by ultrasonic to obtain nanoemulsion dispersion liquid. In a special measuring cylinder with a measuring range of 50mL, the nano-emulsifier dispersion liquid and the de-aerated crude oil (viscosity of 84.2 mPa.s under the conditions of 30 ℃ and a shear rate of 7.336s < -1 >) are mixed according to a water-oil volume ratio of 1: 9. 2:8, 3:7, 4:6, 5:5, 6:4, 7:3, 8:2, 9:1 total volume of 20mL mixing, sealing; then stirring for 30 minutes at 30 ℃ in a water bath condition, observing the emulsification condition, and measuring the apparent viscosity of the emulsion by a viscosimeter at 30 ℃ and a shearing rate of 7.336s-1 after the stirring is finished, wherein the apparent viscosity is shown in table 2. It can be observed that the high internal phase emulsion viscosity formed by the nano-solid particle emulsifiers of examples 1 to 3 is higher than the emulsion viscosity of crude oil and water, whereas the emulsion viscosity formed by grafting long chain nano-silica with the silane coupling agent in comparative example 1 is lower than the emulsion viscosity formed by examples 1 to 3 at a water content of 70% or more. And the emulsion viscosity formed in example 4 is less than the nano-solid particle emulsifier of the present invention.
TABLE 2 viscosity of emulsion formed by Water and nanoemulsifier Dispersion and crude oil under different Water-oil ratio conditions
4. Microcosmic morphology of high inward water-in-oil emulsion with 80% water content
The nano-emulsifier is adsorbed on an oil-water interface under the induction of shear, and the oil-water interface is reversely bent due to the hydrophobicity of the nano-emulsifier to form water-in-oil emulsion, so that the emulsion has higher viscosity than crude oil, has no phase change under the condition of 10-80% of water content, has the viscosity proportional to the water content and inversely proportional to the oil content, and has the self-adaptive control fluidity, stable displacement front and intelligent displacement characteristics under the oil reservoir condition. The microstructure of the emulsion with a water content of 80% (volume ratio of nano solid particle emulsifier 1 dispersion to crude oil 8:2) is shown in fig. 2, which demonstrates that the water-in-oil emulsion can still form a water-in-oil emulsion under very high water content conditions.
The present invention has been disclosed in the foregoing description of preferred embodiments, but it will be understood by those skilled in the art that these embodiments are merely for the purpose of describing the present invention and should not be construed as limiting the scope of the present invention. Further modifications are possible without departing from the principles of the invention, and such modifications should be considered as protecting the invention.
Claims (6)
1. The preparation method of the nano titanium dioxide solid particle emulsifier is characterized by comprising the following steps of:
(1) Adding hydrophilic nano titanium dioxide into absolute ethyl alcohol and dispersing the hydrophilic nano titanium dioxide to obtain a dispersion liquid;
(2) Adding a phthalate coupling agent into the dispersion liquid and enabling the phthalate coupling agent to perform a coupling reaction with the titanium dioxide, wherein the phthalate coupling agent accounts for 8-15% of the mass of the nano titanium dioxide in percentage by mass;
(3) Dripping the lengthened bromoalkane into the reaction liquid obtained in the step (2), maintaining stirring in the dripping process, and reacting for 10-12 h at 60-70 ℃ under the condition of continuous stirring after the dripping is finished; the method comprises the steps of (1) separating and purifying the long-chain bromoalkane after the reaction is finished, wherein the adding amount of the long-chain bromoalkane is 1-2 times that of the nano titanium dioxide;
the titanate coupling agent is one or more of isopropyl tri (dioctyl pyrophosphoryl oxy) titanate, di (dioctyl pyrophosphoryl oxy) ethylene titanate and isopropyl dioleoyl (dioctyl phosphoric acyloxy) titanate; the long-chain bromoalkane is at least one of bromododecane, bromotetradecane or bromohexadecane.
2. The method according to claim 1, characterized in that: in the step (1), the titanium dioxide is hydrophilic titanium dioxide with the diameter of 20-100 nm, and the adding amount of the titanium dioxide is 0.02-0.05 times of that of the absolute ethyl alcohol according to mass percentage.
3. The method according to claim 1, characterized in that: in the step (1), the preparation time of the dispersion liquid is 20-40 min.
4. The method according to claim 1, wherein in the step (2), the reaction temperature is 60 to 70 ℃ and the reaction time is 10 to 12 hours.
5. The method according to claim 1, characterized in that: the specific operation of separation and purification is as follows: filtering the reacted product, washing with absolute ethyl alcohol for several times, vacuum drying the filter cake after separation, and crushing after drying.
6. A nano titanium dioxide solid particle emulsifier prepared by the method of any one of claims 1-5.
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