CN114736664A - Nano titanium dioxide solid particle emulsifier and preparation method thereof - Google Patents
Nano 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 following steps: dissolving titanium dioxide in absolute ethyl alcohol, and performing ultrasonic treatment to obtain a dispersion liquid; adding a phthalate ester coupling agent into the dispersion liquid for chemical grafting; heating, stirring and reacting for a period of time, adding a certain amount of bromoalkane, heating and stirring for a period of time; after heating and stirring, carrying out suction filtration and drying to obtain the nano lipophilic titanium dioxide solid particle emulsifier. The nano emulsifier can form a stable water-in-oil emulsion under the condition that the water saturation of an oil reservoir is 10-80%, the viscosity of the emulsion is 1.5-22 times that of crude oil, the viscosity of the emulsion is in direct proportion to the water saturation of the oil reservoir within the range of the water saturation of the oil reservoir, and the high-viscosity emulsion formed under the high water-containing condition can block an advantageous channel so as to achieve the purposes of controlling the fluidity and stabilizing the drainage front edge and improve the recovery ratio of the 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 a high internal phase and high viscosity emulsion in a high permeability zone of an oil reservoir and a preparation method thereof.
Background
In heterogeneous reservoirs, water Flooding causes severe fingering, i.e., affected by the heterogeneity in the formation and the Oil-water viscosity difference, the seepage velocity of injected water is much faster than that of crude Oil, and a dominant channel is formed between the injection well and the Production well, resulting in most areas of the reservoir after water Flooding not being flooded by water waves and [ ALMANSOUR A O, ALQURAISHI A A, ALHUSSINAN S N, ethylene. efficiency pf Enhanced Oil Recovery Using Polymer-augmented Low sales flow [ J ]. Journal of Petroleum expansion & Production Technology,2017,7(1): 1149. 1158 ]. The conventional polymer oil displacement agent has the problems that the viscosity is reduced too fast and the dosage is required to be used in a high-salinity oil reservoir, so that the cost is increased, and the conditions of degradation failure and the like can occur in a high-temperature oil reservoir; and the surfactant is easy to be adsorbed on the surface of oil reservoir rock, and simultaneously, under the influence of high-temperature and high-salt oil reservoir conditions, the stability of the surfactant forming emulsion is greatly reduced, so that the fluidity control capability of the surfactant is limited to a certain extent (Zhao, Wang Li Juan, Xia 26206ran. Petroleum geology and engineering [ J ], 2014, 28(2):100 + 103.).
In recent years, researchers focus on research and turn to 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 and can be kept stable in the flowing process, and the recovery ratio is obviously improved (Kaminsky R D, Wattenbarger R C, Lederhos J P, et al. Sharma et al demonstrated that the cumulative recovery could be increased by 5% using Pickering emulsions formulated with a thickened aqueous phase. (Sharma T, Velmurugan N, Patel P, et al. use of oil-in-water stabilized by nanoparticles in combination with a polymer flow for enhanced oil recovery [ J ]. Pet Sci Technol, 2015, 33 (17/18): 1959-1604.) the type of emulsion stabilized by nanoparticles is mainly affected by the wettability of the nanoparticles, and when θ < 90 °, the nanoparticles appear hydrophilic, forming an O/W type emulsion; when θ > 90 °, the nanoparticle wetting behavior appears lipophilic, forming a W/O type emulsion (Binks B P, Lumsdon S O. langmuir, 2000, 16(23), 8622.). However, the type of emulsion is not only related to the emulsifier, but also to the oil-water ratio, and even lipophilic nanoparticles, even if the water content is too high, can still form an O/W type emulsion, and thus, the corresponding emulsifier is required to have a high phase transition point.
The emulsion formed by the nanoparticles solves the problem of poor stability of the emulsion formed by the traditional surfactant, can still keep stable under some harsh 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, the research on the formation of the emulsion by single nano-particles is less, and the emulsion is mostly generated by adopting the synergistic action of 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 strongly, and the prepared nano solid particle emulsifier can form an emulsion with the viscosity in direct proportion to the water saturation under the condition of certain water saturation of an oil reservoir, so that the aim of plugging a dominant channel and improving the recovery ratio is fulfilled.
In order to achieve the above object, the technical solution of the present invention is as follows: a preparation method of a nano titanium dioxide solid particle emulsifier comprises the following steps:
(1) adding nano titanium dioxide into absolute ethyl alcohol and performing ultrasonic dispersion on the nano titanium dioxide to obtain a dispersion liquid;
(2) adding a phthalate ester coupling agent into the dispersion liquid, and performing coupling reaction on the phthalate ester coupling agent and titanium dioxide, wherein the coupling agent accounts for 0.08-0.15 times of the mass of the nano titanium dioxide in percentage by mass;
(3) dropwise adding long-chain alkyl bromide into the reaction liquid obtained in the step (2), maintaining stirring in the dropwise adding process, and reacting for 10-12 hours at 60-70 ℃ under the condition of continuous stirring after dropwise adding; and (3) the addition of the long-chain brominated alkane is 1-2 times of the addition of the nano titanium dioxide in parts by mass, and after the reaction is finished, the long-chain brominated alkane is separated and purified to obtain the nano titanium dioxide.
One embodiment of the invention is that in the step (1), the titanium dioxide is hydrophilic titanium dioxide with the diameter of 20-100 nm, and the addition amount of the titanium dioxide is 0.02-0.05 times of that of the absolute ethyl alcohol in percentage by mass.
One embodiment of the present invention is that, in the step (1), the preparation time of the dispersion is 20 to 40 min.
One embodiment of the invention is that, in the step (2), the reaction temperature is 60-70 ℃ and the reaction time is 10-12 h.
One embodiment of the present invention is that, in the step (2), the titanate coupling agent is one or more of isopropyl tris (dioctyl pyrophosphato acyloxy) titanate, bis (dioctyl pyrophosphato acyloxy) ethylene titanate, isopropoxy dioleate acyloxy (dioctyl phosphato) titanate;
one embodiment of the present invention is that, in the step (3), the long-chain alkyl bromide is at least one of dodecane bromide, tetradecane bromide or hexadecane bromide.
One embodiment of the present invention is that the specific operations of the separation and purification are: and filtering the product after the reaction, washing the product for a plurality of times by using absolute ethyl alcohol, after the separation is finished, drying the filter cake in vacuum, and crushing the filter cake after the drying is finished.
The invention also aims to disclose a nano solid particle emulsifier which is prepared by adopting any one of the methods. The emulsifier can form a water-in-oil emulsion with high viscosity and high internal phase, and can improve the oil displacement efficiency.
Has the advantages that: the invention introduces long-chain alkane on the surface of titanium dioxide by a coupling agent, thereby synthesizing the nano solid particle emulsifier. As an emulsifier, a high internal phase emulsion can be formed with high viscosity relative to conventional surfactant emulsifiers; meanwhile, the synthetic method is simple and can be industrialized strongly.
Drawings
Fig. 1 is a graph of the oil-water-solid three phase contact angle of the modified nanoparticle emulsified particles;
FIG. 2 is a microscopic view of the nanoemulsion formed into a water-in-oil Pickering emulsion;
Detailed Description
The present invention will now be described more fully hereinafter with reference to the accompanying examples, in which some, but not all embodiments of the invention are shown.
The invention is further described below with reference to the following examples:
example 1
(1) 100g of absolute ethanol and 3g of hydrophilic titanium dioxide were added to a reagent bottle, and the dispersion was prepared by sonication for 30 minutes.
(2) 0.3g of isopropyl tris (dioctyl pyrophosphato) titanate (available from Nanjing England New Material technology Co., Ltd.) was added to the dispersion, and the mixture was heated and stirred in a 65 ℃ oil bath for 12 hours.
(3) Dropwise adding 3g of bromododecane into the dispersion liquid obtained in the step 2, and shaking a reagent bottle in the dropwise adding process to ensure that a reaction system is uniformly mixed; and (3) putting the mixture into an oil bath kettle at 65 ℃ for heating and stirring for 12 hours, after the reaction is finished, carrying out suction filtration and washing treatment on the product, and drying and grinding the product to obtain the nano solid particle emulsifier S1.
Example 2
(1) 100g of absolute ethanol and 3g of hydrophilic titanium dioxide were added to a reagent bottle, and the dispersion was prepared by sonication for 30 minutes.
(2) 0.3g of bis (dioctylphosphato acyloxy) ethylene titanate (commercially available from Nanjing England New Material technology Co., Ltd.) was added to the dispersion, and the mixture was heated and stirred in a 65 ℃ oil bath for 12 hours.
(3) Dropwise adding 3g of bromododecane into the dispersion liquid obtained in the step 2, and shaking a reagent bottle in the dropwise adding process to ensure that a reaction system is uniformly mixed; put into an oil bath pan at 65 ℃ to be heated and stirred 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 S2.
Example 3
(1) 100g of absolute ethanol and 3g of hydrophilic titanium dioxide were added to a reagent bottle, and the dispersion was prepared by sonication for 30 minutes.
(2) 0.3g of isopropoxydioleato acyloxy (dioctylphosphonato) titanate (commercially available from Nanjing England New Material technology Co., Ltd.) was added to the dispersion, and the mixture was heated and stirred in a 65 ℃ oil bath for 12 hours.
(3) Dropwise adding 3g of bromohexadecane into the dispersion liquid obtained in the step 2, and shaking a reagent bottle in the dropwise adding process to ensure that a reaction system is uniformly mixed; put into an oil bath pan at 65 ℃ to be heated and stirred 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 S3.
Comparative example 1
This was used as a control in comparison with the conventional method of grafting a long chain onto a nanosilicon dioxide by a silane coupling agent.
(1) 100g of absolute ethanol and 3g of hydrophilic silica were added to a reagent bottle, and a dispersion was prepared by sonication for 30 minutes.
(2) 0.3g of silane coupling agent KH-570 was added to the dispersion, and the mixture was put into a 65 ℃ oil bath and heated with stirring for 12 hours.
(3) Dropwise adding 3g of bromotetradecane into the dispersion liquid obtained in the step 2, and shaking a reagent bottle in the dropwise adding process to ensure that a reaction system is uniformly mixed; placed in an oil bath pan at 65 ℃ and heated and stirred 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 D1.
In order to illustrate the effect of the nano solid particle emulsifier prepared in the embodiment of the present invention, the performance test thereof is performed as follows.
1. Wettability test
The nano-emulsifiers synthesized in examples 1 to 4 were uniformly spread on a quartz slide glass, and the oil-water-solid three-phase contact angle of the nano-emulsifiers was measured with a HARHE-SPCA contact angle measuring instrument (Haako, china) in a kerosene environment, as shown in fig. 1. The contact angles of the nano-emulsifier in the embodiments 1-3 are 135.5 degrees, 132.3 degrees and 139.7 degrees respectively, and the hydrophobicity of the nano-emulsifier is proved. Example 4 as a control had a contact angle of 109.8 deg., and was slightly less hydrophobic than the nanoemulsifiers of the present invention.
2. Ability of nano-emulsion dispersion to emulsify crude oil (different oil-water ratio)
The nano-emulsifier synthesized in the example 1-4 is respectively added into formation water (the formation water type is NaHCO3, and the mineralization degree is 5054mg/L) to prepare the nano-emulsifier with the mass concentration of 0.06%, and the nano-emulsifier is ultrasonically dissolved for 10 minutes to obtain the nano-emulsifier dispersion liquid. In a specially prepared measuring cylinder with a measuring range of 50mL, the nano-emulsion dispersion and degassed crude oil (the viscosity under the conditions of 30 ℃, the shear rate of 7.336s < -1 > is 84.2mPa & s) are mixed according to the volume ratio of water to oil of 1: 9. 2:8, 3:7, 4:6, 5:5, 6:4, 7:3, 8:2 and 9:1 are mixed and sealed, and the total volume is 20 mL; then stirring for 30 minutes in a water bath condition at 30 ℃, observing the emulsification condition, and calculating the water content of the emulsion to obtain the water content shown in table 1. The nano-emulsifier in the embodiment 1-3 still has good emulsifying property under the condition of 90% water content, and the water content of the formed emulsion is more than 80%. The water content of the emulsion formed by grafting the long-chain nano-silica through the silane coupling agent in the embodiment 4 can only reach 70%, which shows that the effect of the emulsified crude oil of the nano-solid particle emulsifier is better than that of the long-chain nano-silica grafted through the silane coupling agent.
Through the analysis of the inventor, the phenomenon is mainly caused because the density of the nano silicon dioxide relative to the nano titanium dioxide is low, and even though the hydrophobic long chain is grafted, the nano silicon dioxide still has a slight agglomeration phenomenon, so the effect is inferior to that of the nano titanium dioxide; meanwhile, the titanate coupling agent has 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 content of emulsion formed by water, nano-emulsion dispersion and crude oil under different water-oil ratio conditions
3. The viscosity (different oil-water ratio) of the emulsion formed by the nano-emulsion dispersion and the crude oil
And (3) respectively adding the nano-emulsifier synthesized in the examples 1-4 into the formation water to prepare a nano-emulsifier with the mass concentration of 0.06%, and ultrasonically dissolving for 10 minutes to obtain a nano-emulsifier dispersion liquid. In a specially prepared measuring cylinder with a measuring range of 50mL, the nano-emulsion dispersion and degassed crude oil (the viscosity under the conditions of 30 ℃, the shear rate of 7.336s < -1 > is 84.2mPa & s) are mixed according to the volume ratio of water to oil of 1: 9. 2:8, 3:7, 4:6, 5:5, 6:4, 7:3, 8:2 and 9:1 are mixed and sealed, and the total volume is 20 mL; and then stirring for 30 minutes in a water bath condition at the temperature of 30 ℃, observing the emulsification condition, and after the stirring is finished, testing the apparent viscosity of the emulsion by using a viscosity instrument at the temperature of 30 ℃ and at the shear rate of 7.336s-1, wherein the apparent viscosity is shown in table 2. It can be observed that the viscosity of the high internal phase emulsion formed by the nano solid particle emulsifier in the examples 1-3 is higher than that of the emulsion formed by crude oil and water, and when the water content is more than 70%, the viscosity of the emulsion formed by grafting long-chain nano silicon dioxide by the silane coupling agent in the comparative example 1 is lower than that of the emulsion formed in the examples 1-3. And example 4 the viscosity of the resulting emulsion was lower than the nano-solid particle emulsifier of the present invention.
TABLE 2 viscosity of emulsions formed from water, nanoemulsion dispersions and crude oil at different water-to-oil ratios
4. Micro-morphology of high inward water-in-oil emulsion with water content of 80%
The nano emulsifier is adsorbed on an oil-water interface under the shearing induction, the oil-water interface is reversely bent due to the hydrophobicity of the nano emulsifier to form a water-in-oil emulsion, the viscosity of the emulsion is higher than that of crude oil, the emulsion has no phase change under the condition that the water content is 10-80%, the viscosity of the emulsion is in direct proportion to the water content and in inverse proportion to the oil content, and the characteristics of self-adaptive control of the flow, stable displacement front edge and intelligent displacement of the emulsion under the oil reservoir condition are reflected. The micro-morphology of the emulsion with the water content of 80% (volume ratio of nano solid particle emulsifier 1 dispersion to crude oil 8:2) is shown in fig. 2, and the water-in-oil emulsion can still be formed under the condition of very high water content.
The present invention has been disclosed in the foregoing in terms of preferred embodiments, but it will be understood by those skilled in the art that these embodiments are merely illustrative of the present invention and should not be construed to limit the scope of the present invention. Further modifications are possible without departing from the principles of the invention and these modifications are to be considered as protection of the invention.
Claims (8)
1. The preparation method of the nano titanium dioxide solid particle emulsifier is characterized by comprising the following steps:
(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 ester coupling agent into the dispersion liquid and enabling the phthalate ester coupling agent and titanium dioxide to have a coupling reaction, wherein the mass percentage of the phthalate ester coupling agent is 8-15% of that of the nano titanium dioxide;
(3) dropwise adding long-chain alkyl bromide into the reaction liquid obtained in the step (2), maintaining stirring in the dropwise adding process, and reacting for 10-12 hours at 60-70 ℃ under the condition of continuous stirring after dropwise adding; and (3) the addition of the long-chain brominated alkane is 1-2 times of the addition of the nano titanium dioxide in parts by mass, and after the reaction is finished, the long-chain brominated alkane is separated and purified to obtain the nano titanium dioxide.
2. The method of claim 1, wherein: in the step (1), the titanium dioxide is hydrophilic titanium dioxide with the diameter of 20-100 nm, and the addition amount of the titanium dioxide is 0.02-0.05 times of that of the absolute ethyl alcohol in percentage by mass.
3. The method of claim 1, wherein: 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 60-70 ℃ and the reaction time is 10-12 h.
5. The method of claim 1, wherein: in the step (2), the titanate coupling agent is one or more of isopropyl tri (dioctyl pyrophosphato acyloxy) titanate, bis (dioctyl pyrophosphato acyloxy) ethylene titanate, and isopropoxy dioleate acyloxy (dioctyl phosphato) titanate.
6. The method of claim 1, wherein: in the step (3), the long-chain alkyl bromide is at least one of dodecane bromide, tetradecane bromide or hexadecane bromide.
7. The method of claim 1, wherein: the specific operation of separation and purification is as follows: and filtering the product after the reaction, washing the product for a plurality of times by using absolute ethyl alcohol, after the separation is finished, drying the filter cake in vacuum, and crushing the filter cake after the drying is finished.
8. A nano titanium dioxide solid particle emulsifier, which is prepared by the method of any one of claims 1 to 7.
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