CN107384356B - Preparation method of nano composite material applied to nano oil-displacing agent and nano oil-displacing agent prepared by using preparation method - Google Patents
Preparation method of nano composite material applied to nano oil-displacing agent and nano oil-displacing agent prepared by using preparation method Download PDFInfo
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- CN107384356B CN107384356B CN201710565267.9A CN201710565267A CN107384356B CN 107384356 B CN107384356 B CN 107384356B CN 201710565267 A CN201710565267 A CN 201710565267A CN 107384356 B CN107384356 B CN 107384356B
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- 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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- C09K2208/00—Aspects relating to compositions of drilling or well treatment fluids
- C09K2208/10—Nanoparticle-containing well treatment fluids
Abstract
3 3The invention provides a nano oil displacement agent which comprises 0.1-1 part of a nano composite material and 99-99.9 parts of a NaCl solution by weight, and a preparation method of the nano composite material applied to the oil displacement agent.
Description
Technical Field
The invention relates to the technical field of nano materials, in particular to a preparation method of a nano composite material applied to a nano oil-displacing agent and the nano oil-displacing agent prepared by the method.
background
Currently, global unconventional oil and gas exploration is in a high-speed development stage, and from a strategic and long-term perspective, unconventional oil and gas resources play an increasingly important role. China has huge potential of unconventional oil and gas resources, but oil and gas geological conditions are complex, and great challenges exist in geological theory and exploration technology. The method is a ten-year exploration for pioneering development of Chinese dense gas and dense oil in nearly 10 years. Although China is rich in dense oil resources, the following disadvantages exist: the physical property of the compact oil and gas reservoir is very poor, the matrix permeability is low, and the oil layer pressure coefficient is high; the pore throat radius is small, and the capillary pressure is high; the oil layer sand and mud are interactive, and the heterogeneity is severe; relative development of natural cracks; the oil layer is controlled by lithology and the hydrodynamic connection is poor; single wells generally have no natural production capacity or natural production capacity below the lower limit of industrial oil flow. Generally, measures including acidizing fracturing, multi-stage fracturing, horizontal wells, multi-branch wells and the like can be adopted to obtain industrial petroleum yield, and although the methods achieve certain results, the methods have the defects of difficulty in mining, high cost and low mining efficiency, and the improvement of the recovery rate is difficult to break through.
Nanomaterials are the emerging materials that have received the most attention in the last three decades, and they exhibit many novel properties that are different from conventional materials, since the properties of the elementary particles that constitute the material change after reaching a nanometer size.
Disclosure of Invention
In view of the above, the invention provides a nano oil-displacing agent which is low in price, safe, environment-friendly and high in oil displacement efficiency and is suitable for compact oil reservoirs, and also provides a preparation method of the nano oil-displacing agent with a simple preparation process and a preparation method of a nano composite material applied to the nano oil-displacing agent.
The invention provides a nano oil displacement agent suitable for a compact oil reservoir, which comprises 0.1-1 part of nano composite material and 99-99.9 parts of NaCl solution by weight.
further, the mass fraction of the NaCl solution is 0.3%.
Furthermore, the particle size of the nano composite material is 5-25 nm.
further, the nano composite material is nano TiO 2/PAM, and the preparation method of the nano composite material comprises a hydrothermal synthesis method and an ultrasonic synthesis method.
The invention also provides a preparation method of the nano composite material applied to the nano oil displacement agent, which comprises the following steps:
S501, dropwise adding tetrabutyl titanate into absolute ethyl alcohol, stirring while dropwise adding, and then carrying out ultrasonic treatment for 10min to obtain a first solution;
S502, mixing polyacrylamide with the HNO 3 solution to obtain a second solution;
S503, slowly and dropwisely adding the first solution into the second solution in an ice bath device for ice bath reaction, and then reacting for 4 hours at 80 ℃ to obtain sol;
s504, adding the sol into a reaction kettle for hydrothermal reaction, then separating out a precipitate, repeatedly washing the precipitate with deionized water and absolute ethyl alcohol, centrifuging, and drying to obtain the nano composite material.
Further, in the step S502, the concentration of the HNO 3 solution is 0.1mol/L, the mass concentration of the second solution is 0.6%, in the step S503, the time of ice-bath reaction is 0.5-1 h, and in the step S504, the reaction temperature of hydrothermal reaction is 180 ℃, and the reaction time of hydrothermal reaction is 6-8 h.
The invention also provides a preparation method of the nano composite material applied to the nano oil displacement agent, which comprises the following steps:
s701, adding titanium dioxide particles into deionized water to obtain a suspension;
S702, mixing polyacrylamide with the HNO 3 solution to obtain a third solution;
and S703, slowly dripping the suspension into the third solution, performing ultrasonic treatment for 2 hours, stirring by using a magnetic stirrer, and drying to obtain the nano composite material.
further, in step S702, the concentration of the HNO 3 solution is 0.1mol/L, the mass concentration of the third solution is 0.6%, and in step S703, drying is performed at 60 ℃.
The invention also provides a preparation method of the nano oil displacement agent suitable for the compact oil reservoir, which comprises the following steps: and adding the nano composite material into a NaCl solution, and performing ultrasonic dispersion to obtain the nano oil displacement agent.
Further, the time of ultrasonic dispersion is 15-30 min.
The technical scheme provided by the invention has the beneficial effects that:
1. The polymer of the nano composite material is bonded with the nano titanium dioxide through a covalent bond, so that the water interfacial tension can be reduced, the nano composite material has good thermal stability and dispersibility, and can be widely applied to complex stratum environments;
2. the particle size of the nano composite material is suitable for a compact oil reservoir throat, so that the blockage of a stratum can not be caused;
3. The preparation method of the nano oil displacement agent provided by the invention is simple, low in production cost, less in process flow and easy to realize large-scale production;
4. the nano oil displacement agent provided by the invention has a good oil displacement effect, and can improve the oil displacement efficiency by 5-15%.
drawings
FIG. 1 is an X-ray diffraction pattern of TiO 2 and the nanocomposite material of example 1 of the invention.
FIG. 2 is a transmission electron micrograph of the nanocomposite obtained in example 1 of the present invention.
FIG. 3 is a transmission electron microscope image of a nanocomposite prepared by the ultrasonic synthesis method according to an embodiment of the present invention.
FIG. 4 is a graph of the contact angle of a sample of the nanocomposite obtained in example 1 of the present invention.
FIG. 5 is an IR spectrum of a nanocomposite prepared in an example of the invention.
Fig. 6 is a schematic view of a drive unit for use with the present invention.
Fig. 7 is a schematic diagram of the change of the recovery degree after the dynamic displacement of the nano oil displacement agent.
Fig. 8 is a schematic diagram of the dynamic displacement pressure change of the nano oil displacement agent of the invention.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, embodiments of the present invention will be further described with reference to the accompanying drawings.
The embodiment of the invention provides a nano oil displacement agent suitable for a compact oil reservoir, which comprises 0.1-1 part of a nano composite material and 99-99.9 parts of a NaCl solution by weight, wherein the mass fraction of the NaCl solution is 0.3%, and the particle size of the nano composite material is 5-25 nm.
The nano composite material is nano TiO 2/PAM, and the preparation method comprises a hydrothermal synthesis method and an ultrasonic synthesis method.
The preparation of the nano composite material by using the hydrothermal synthesis method comprises the following steps:
S501, dropwise adding tetrabutyl titanate into absolute ethyl alcohol, stirring while dropwise adding, and performing ultrasonic treatment for 10min to obtain a first solution;
S502, mixing Polyacrylamide (PAM) with 0.1mol/L HNO 3 solution to obtain a second solution with the mass concentration of 0.6%;
S503, slowly and dropwise adding the first solution into the second solution in an ice bath device to perform ice bath reaction for 0.5-1 h, and then reacting for 4h at 80 ℃ to obtain sol;
s504, adding the sol into a reaction kettle to perform hydrothermal reaction, reacting at 180 ℃ for 6-8 hours to separate out a precipitate, repeatedly washing the precipitate with deionized water and absolute ethyl alcohol, centrifuging, and drying to obtain the nano composite material.
The preparation of the nano composite material by using the ultrasonic synthesis method comprises the following steps:
S701, adding titanium dioxide particles into deionized water to obtain a suspension;
S702, mixing polyacrylamide with 0.1mol/L HNO 3 solution to obtain a third solution with the mass concentration of 0.6%;
And S703, slowly dripping the suspension into the third solution, performing ultrasonic treatment for 2 hours, stirring by using a magnetic stirrer, and drying at 60 ℃ to obtain the nano composite material.
the embodiment of the invention also provides a preparation method of the nano oil displacement agent suitable for the compact oil reservoir, which comprises the following steps: and adding the nano composite material into a NaCl solution, and performing ultrasonic dispersion for 15-30 min to obtain the nano oil displacement agent.
The nanometer oil displacement agent can generate wedge-shaped pressure action in a micro channel of a reservoir during flowing, and then crude oil attached to the surface of reservoir rock is stripped and carried out, so that the oil displacement effect is generated.
the following provides an example of the preparation method of the nano oil-displacing agent and the preparation method of the nano composite material applied to the nano oil-displacing agent, and the preparation method is exemplified by combining the example.
Example 1
Measuring 4ml of tetrabutyl titanate, dropwise adding the tetrabutyl titanate into 60ml of absolute ethyl alcohol, stirring while dropwise adding, and performing ultrasonic treatment for 10min to obtain a first solution, weighing 0.0606g of PAM, dissolving the PAM in 0.1mol/L of HNO 3 solution to obtain a second solution, slowly dropwise adding the first solution into the second solution in an ice bath device to perform ice bath reaction for 1h, then performing reaction for 4h at 80 ℃ to obtain sol, adding the sol into a reaction kettle to perform hydrothermal reaction for 8h at 180 ℃ to precipitate, repeatedly washing the precipitate by using deionized water and absolute ethyl alcohol, centrifuging and drying to obtain a nano composite material, weighing 0.1g of the nano composite material, adding into 33g of 0.3% NaCl aqueous solution, and performing ultrasonic dispersion for 10min to obtain the nano oil displacement agent.
FIG. 1 is an X-ray diffraction (XRD) pattern of TiO 2 and the nanocomposite prepared in example 1. from FIG. 1, it can be seen that the particle size of TiO 2 is reduced from 9.67nm to 7.57nm under the modification of PAM.
Fig. 2 is a transmission electron microscope image of the nanocomposite obtained in example 1, fig. 3 is a transmission electron microscope image of the nanocomposite obtained in example by the ultrasonic synthesis method, and it can be seen from fig. 2 and 3 that PAM in the nanocomposite is modified on the surface of TiO 2, inhibiting the growth of TiO 2 and agglomeration between particles.
fig. 4 is a contact angle graph of a sample of the nanocomposite obtained using example 1, and as can be seen from fig. 4, the nanocomposite has a contact angle of 25.5 °, indicating that it has good hydrophilicity.
fig. 5 is an infrared spectrum of the nanocomposite obtained in one example, and it can be seen from fig. 5 that PAM is partially hydrolyzed during the reaction and interacts with TiO 2.
The performance of the nano oil displacement agent of the invention is illustrated by an oil displacement test.
The principle of the oil repellency test is as follows: in order to simulate the oil displacement process, an artificial core or a natural core is used for representing a stratum, the oil extraction process of periodic water injection is simulated, and the oil displacement effect is evaluated by monitoring the change of water content, recovery ratio and displacement pressure.
Referring to fig. 6, the oil displacement device used in the oil displacement test comprises a high-pressure advection pump 1, a manual metering pump 2, a six-way valve 3, a water container 4, an oil displacement agent container 5, a pressure gauge 6, a core holder 7, an effluent receiver 8, a pressure sensor 9, a pressure display instrument 10, a pressure recorder 11 and a thermostat 12, wherein the pressure gauge 6 is arranged on the water container 4 and the oil displacement agent container 5, the water container 4, the oil displacement agent container 5, the core holder 7 and the effluent receiver 8 are all located in the thermostat 12, the water container 4 and the oil displacement agent container 5 are respectively connected with the core holder 7, and the core holder 7 is further connected with the manual metering pump 2.
test one:
The oil repellency test specifically comprises the following steps:
The rock core is an artificial columnar rock core, the height and the diameter of the rock core are measured by a caliper, and then the gas logging permeability of the rock core is measured.
Weighing the original mass m 0 of the rock core by using an analytical balance, putting the rock core into a filter flask, pumping the rock core into the filter flask by using a manual metering pump 2 until the pressure in the filter flask is 0.1kPa, continuously pumping for 8 hours under the pressure of 0.1kPa, then closing the manual metering pump 2, sucking formation water into the filter flask, continuously pumping for 4 hours by using the manual metering pump 2 until no bubble exists in the filter flask, then taking out the processed rock core, and calling the final mass m of the rock core, calculating the pore volume V p by using a formula, wherein the calculation formula of the pore volume V p of the rock core is as follows:
Vp＝(m-m0)/ρ，
in the formula, V p is the pore volume of the core, V p is expressed in cm 3, rho is the density of water, and rho is expressed in g/cm 3.
And (3) installing the rock core on a rock core holder 7, recording the displacement pressure and the displacement flow rate, and calculating the water drive permeability by using a Darcy formula.
saturating the core with oil by using a saturated water flow until the oil output is twice of the saturated oil quantity; and (3) loading the saturated oil core into a core holder 7, carrying out saturated oil flow again in the slotted core, and carrying out oil displacement after 24 h.
in the first test of the invention, water is selected as a comparative experiment:
the periodic water injection process of the water flooding is as follows:
1.1, adding water into a water container 4, and injecting water and displacing oil through a water displacement oil flow until the water content of produced liquid reaches 98%;
After 1.224 h, step 1.1 was repeated, repeatedly until no more oil appeared.
The periodic water injection process of the nano oil displacement agent for oil displacement is as follows:
2.1 adding a nano oil displacement agent into an oil displacement agent container 5, injecting the nano oil displacement agent through the oil displacement agent process to displace oil until the water content of produced fluid reaches 98%;
2.224 h, repeating step 2.1 repeatedly until no oil is produced.
table 1 shows the results of the core dynamic displacement experiment performed by using water and the nano oil displacement agent respectively in the first experiment, and it can be seen from table 1 that the oil displacement recovery ratio is significantly improved by using the nano oil displacement agent, and the oil displacement effect is good.
Table 1 results of core dynamic displacement experiments using water and nano-oil displacement agent
And (2) test II:
and in the second test, a low-permeability core of the Changqing oil field is selected for carrying out a core dynamic displacement test, the temperature of the thermostat 12 is set to be 70 ℃, and the oil displacement process of the second test is as follows: firstly, water flooding is carried out, and then a displacement test is carried out by adopting the nano oil displacement agent prepared by the invention.
The recovery degree of crude oil obtained by the second test is shown in fig. 7, and fig. 7 shows that the recovery degree of crude oil is 46% after water flooding is injected, and the recovery degree of crude oil is 58% after the nano oil displacement agent of the present invention is injected for displacement after the test is ended, which indicates that the recovery ratio can be effectively improved by using the nano oil displacement agent of the present invention compared with the injection of water flooding.
fig. 8 is a schematic diagram of pressure change in the displacement process of test two, and it can be seen from fig. 8 that the pressure slightly changes when the nano oil-displacing agent of the present invention is displaced after water flooding is injected, which illustrates that no blocking damage is caused to the formation when the nano oil-displacing agent of the present invention is used for displacement.
The polymer of the nano composite material is bonded with the nano titanium dioxide through a covalent bond, so that the water interfacial tension can be reduced, the nano composite material has good thermal stability and dispersibility, and can be widely applied to complex stratum environments; the particle size of the nano composite material is suitable for a compact oil reservoir throat, so that the blockage of a stratum can not be caused; the preparation method of the nano oil displacement agent provided by the invention is simple, low in production cost, less in process flow and easy to realize large-scale production; the nano oil displacement agent provided by the invention has a good oil displacement effect, and can improve the oil displacement efficiency by 5-15%.
The features of the embodiments and embodiments described herein above may be combined with each other without conflict.
the above description is only for the purpose of illustrating the preferred embodiments of the present invention and is not to be construed as limiting the invention, and any modifications, equivalents, improvements and the like that fall within the spirit and principle of the present invention are intended to be included therein.
Claims (9)
1. A method for preparing a nano composite material applied to a nano oil displacement agent is characterized by comprising the following steps: the preparation method comprises the following steps:
s501, dropwise adding tetrabutyl titanate into absolute ethyl alcohol, stirring while dropwise adding, and then carrying out ultrasonic treatment for 10min to obtain a first solution;
S502, mixing polyacrylamide with the HNO 3 solution to obtain a second solution;
S503, slowly and dropwisely adding the first solution into the second solution in an ice bath device for ice bath reaction, and then reacting for 4 hours at 80 ℃ to obtain sol;
S504, adding the sol into a reaction kettle, carrying out hydrothermal reaction for 6-8 hours at 180 ℃, then separating out a precipitate, repeatedly washing the precipitate with deionized water and absolute ethyl alcohol, centrifuging, and drying to obtain the nano composite material.
2. The method for preparing the nanocomposite material according to claim 1, wherein in the step S502, the concentration of the HNO 3 solution is 0.1mol/L, the mass concentration of the second solution is 0.6%, and in the step S503, the ice-bath reaction time is 0.5-1 h.
3. A method for preparing a nano composite material applied to a nano oil displacement agent is characterized by comprising the following steps: the preparation method comprises the following steps:
S701, adding titanium dioxide particles into deionized water to obtain a suspension;
s702, mixing polyacrylamide with the HNO 3 solution to obtain a third solution;
And S703, slowly dripping the suspension into the third solution, performing ultrasonic treatment for 2 hours, stirring by using a magnetic stirrer, and drying to obtain the nano composite material.
4. the method of claim 3, wherein the HNO 3 solution has a concentration of 0.1mol/L and the third solution has a mass concentration of 0.6% in step S702, and the drying is performed at 60 ℃ in step S703.
5. The nano oil displacement agent suitable for the tight oil reservoir is characterized by comprising 0.1-1 part by weight of nano composite material and 99-99.9 parts by weight of NaCl solution, wherein the nano composite material is nano TiO 2/PAM and is prepared by the preparation method of claim 1 or claim 3.
6. The nano oil displacement agent suitable for tight oil reservoirs according to claim 5, wherein the mass fraction of the NaCl solution is 0.3%.
7. the nano oil displacement agent suitable for tight oil reservoirs according to claim 5, wherein the particle size of the nano composite material is 5-25 nm.
8. the preparation method of the nano oil displacement agent suitable for the tight oil reservoir, which is characterized by comprising the following steps: and adding the nano composite material into a NaCl solution, and performing ultrasonic dispersion to obtain the nano oil displacement agent.
9. The preparation method of the nano oil displacement agent suitable for the tight oil reservoir according to claim 8, wherein the time of ultrasonic dispersion is 15-30 min.
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