CN112321777B - Nano composite microsphere plugging agent for water plugging and profile control of low-permeability oil field and preparation method thereof - Google Patents
Nano composite microsphere plugging agent for water plugging and profile control of low-permeability oil field and preparation method thereof Download PDFInfo
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Abstract
The invention discloses a nano composite microsphere plugging agent for water plugging and profile control of a low-permeability oil field and a preparation method thereof, and relates to the technical field of oil field chemicals. A nano composite microsphere plugging agent for water shutoff and profile control of a low-permeability oilfield is mainly prepared from the following profile control agent raw materials in parts by weight: 20-46 parts of sodium acrylate, 3-6 parts of acrylamide, 0.2-0.8 part of cross-linking agent, 1-8 parts of nano Beta molecular sieve, 0.1-0.9 part of initiator and 60-80 parts of deionized water; the profile control agent raw material also comprises an auxiliary agent, wherein the auxiliary agent comprises 1-4 parts by weight of phosphate starch. The nano composite microsphere plugging agent for water shutoff and profile control of the low-permeability oil field has the advantage of good strength performance. The preparation method comprises the following steps: mixing materials, polymerization reaction and the like. The preparation method of the nano composite microsphere plugging agent for water shutoff and profile control of the low-permeability oilfield has the advantage of improving the strength performance of the product.
Description
Technical Field
The invention relates to the technical field of oilfield chemicals, in particular to a nano composite microsphere plugging agent for water plugging and profile control of a low-permeability oilfield and a preparation method thereof.
Background
The oil field generally adopts a water flooding development process, after the oil field is developed by long-term water flooding, the physical properties of an oil reservoir layer are greatly changed, the interlayer and in-layer heterogeneity is serious, a high-permeability and large-pore-passage stratum is generated, the permeability of a water-flooded stratum is changed, water flow advances along a high-permeability layer in the stratum and bypasses a low-permeability layer, and therefore the swept volume coefficient of water flooding injection fluid is reduced, the water flooding effect is poor, and the oil field exploitation efficiency is reduced. In order to improve the exploitation efficiency, the oil field generally uses the nano composite microsphere plugging agent to solve the problem of flow bypassing, and people are increasingly researching the nano composite microsphere plugging agent.
CN106675540A discloses a temperature-resistant and salt-resistant profile control water shutoff agent and a preparation method thereof, which are composed of the following raw materials in parts by weight: 1-3 parts of temperature-resistant and salt-resistant polyacrylamide, 0.15-1.2 parts of cross-linking agent A, 0.03-0.1 part of cross-linking agent B, 0.01-0.1 part of retarder, 1-7.5 parts of pH regulator and 988-997 parts of water; the preparation method comprises the following steps: adding a pH regulator into water, fully dissolving, adding temperature-resistant and salt-resistant polyacrylamide, stirring for 2-4 hours, adding a retarder and a cross-linking agent B, stirring for 1-2 hours at normal temperature, adding a cross-linking agent A, uniformly stirring, and keeping the temperature at 70-90 ℃ for 3-5 days. Wherein the temperature-resistant and salt-resistant polyacrylamide is polymerized by raw materials such as acrylamide and the like. According to the technical scheme, the profile control water shutoff agent is prepared by polymerizing acrylamide, so that the problem of oil field flow bypassing is solved, and the exploitation efficiency is improved.
In view of the above-mentioned related technologies, the inventors believe that the hardness of polyacrylamide is not high, which is not favorable for improving the strength of the profile control water shutoff agent, and is not favorable for better exerting the profile control water shutoff effect of the profile control water shutoff agent product.
Disclosure of Invention
In order to improve the strength performance of the profile control water shutoff agent, the application provides a nano composite microsphere water shutoff agent for water shutoff and profile control of a low-permeability oilfield and a preparation method thereof.
In a first aspect, the application provides a nano composite microsphere plugging agent for water shutoff and profile control of a low permeability oilfield, which adopts the following technical scheme:
a nano composite microsphere plugging agent for water shutoff and profile control of a low-permeability oilfield is mainly prepared from the following profile control agent raw materials in parts by weight: 20-46 parts of sodium acrylate, 3-6 parts of acrylamide, 0.2-0.8 part of cross-linking agent, 1-8 parts of nano Beta molecular sieve, 0.1-0.9 part of initiator and 60-80 parts of deionized water; the profile control agent raw material also comprises an auxiliary agent, wherein the auxiliary agent comprises 1-4 parts by weight of phosphate starch.
By adopting the technical scheme, the nano-scale nano Beta molecular sieve is added into the nano composite microsphere plugging agent, the nano Beta molecular sieve contains a large number of nano particles, the nano particles contain micropores, the micropores of the nano particles have a certain adsorption effect on sodium ions on sodium acrylate and drive the acrylic acid radical ions to migrate to the nano particles, under the action of an initiator, the acrylic acid radical is polymerized on the surfaces of the nano particles to form an anion core-shell structure, acrylamide is polymerized on the surfaces of the anion core-shell structure to form a multilayer structure, the nano Beta molecular sieve is added, on one hand, the nano Beta molecular sieve has the effect of a filler, on the other hand, the nano Beta molecular sieve has the effect of an inner core, the addition of phosphate starch is beneficial to improvement of the compatibility among the raw materials such as the nano particles, the sodium acrylate and the acrylamide, and the phosphate starch and the nano Beta molecular sieve are beneficial to improvement of the gel strength of products and is beneficial to better exerting the profile control and water plugging effects of the products.
Preferably, the profile control agent is mainly prepared from the following raw materials in parts by weight: 30-36 parts of sodium acrylate, 3-6 parts of acrylamide, 0.4-0.6 part of cross-linking agent, 3-6 parts of nano Beta molecular sieve, 0.4-0.6 part of initiator, 60-80 parts of deionized water and 2-3 parts of phosphate starch. More preferably, 33 parts of sodium acrylate, 4.5 parts of acrylamide, 0.5 part of cross-linking agent, 4.5 parts of nano Beta molecular sieve, 0.5 part of initiator, 70 parts of deionized water and 2.5 parts of phosphate starch.
By adopting the technical scheme, the better raw material proportion is used, the product performance is favorably optimized, the product quality is improved, and the profile control and water shutoff effects of the product are favorably exerted better.
Preferably, the cross-linking agent is methylene acrylamide or polyethylene glycol diacrylate.
By adopting the technical scheme, methylene acrylamide or polyethylene glycol diacrylate is used as a cross-linking agent, which is beneficial to improving the strength and elasticity of gel, improving the using effect of products and being beneficial to market popularization of the products.
Preferably, the initiator is potassium persulfate or ammonium persulfate.
By adopting the technical scheme, the potassium persulfate or ammonium persulfate initiator is used for inducing monomer polymerization, which is beneficial to shortening polymerization time, improving product yield and reducing cost.
Preferably, the average particle size of the nano Beta molecular sieve is 20-40nm.
By adopting the technical scheme, the nano Beta molecular sieve with the proper particle size is used, the size of the gel is favorably controlled, the product performance is favorably improved, and the product use effect is improved.
Preferably, the auxiliary agent also comprises 0.1-0.4 weight part of ammonium acetate.
By adopting the technical scheme, ammonium acetate is added, so that the polymerization reaction system has a certain pH adjusting function, is carried out in a proper acid-base environment, is beneficial to adjusting the polymerization degree, is beneficial to improving the product performance and improves the product using effect.
In a second aspect, the application provides a preparation method of a nano composite microsphere plugging agent for water plugging and profile control of a low permeability oilfield, which adopts the following technical scheme:
a preparation method of a nano composite microsphere plugging agent for water shutoff and profile control of a low-permeability oilfield comprises the following steps:
s1, mixing materials: adding an auxiliary agent into deionized water, uniformly mixing, cooling to a temperature not higher than 25 ℃, adding sodium acrylate, acrylamide, a nano Beta molecular sieve and a cross-linking agent, and uniformly mixing to obtain a mixed solution;
s2, polymerization reaction: adding an initiator into the mixed solution, stirring at the rotating speed of 100-300 r/min, heating to 50-70 ℃ and reacting for 8-15h to prepare the nano composite microsphere plugging agent for water plugging and profile control of the low-permeability oilfield.
By adopting the technical scheme, materials are mixed at a low temperature, the initiator is added, and then the polymerization reaction is carried out at a proper temperature, so that the polymerization degree is adjusted, the product performance is improved, the product use effect is improved, and the product market popularization is facilitated.
Preferably, in the step S2, the initiator is added into the mixed solution, the mixed solution is stirred at the rotating speed of 100-300 r/min, the temperature is raised to 50-70 ℃ for reaction for 8-15h, ethanol with the weight 0.2-0.4 times that of deionized water is added for demulsification, filtration is carried out, and the filter cake is dried at 65-80 ℃ for 200-300min, so as to prepare the nano composite microsphere plugging agent for water shutoff and profile control of the low permeability oilfield.
By adopting the technical scheme, the ethanol is added for demulsification and then is dried, and the product is stored in a solid form, which is beneficial to prolonging the shelf life of the product.
In summary, the invention includes at least one of the following beneficial technical effects:
1. according to the application, a nano-scale nano Beta molecular sieve is added into a nano composite microsphere plugging agent, the nano Beta molecular sieve contains a large number of nano particles, the nano particles contain micropores, the micropores of the nano particles have a certain adsorption effect on sodium ions on sodium acrylate to drive the migration of acrylic acid radical ions to the nano particles, under the action of an initiator, acrylic acid radicals are polymerized on the surfaces of the nano particles to form an anion core-shell structure, acrylamide is polymerized on the surfaces of the anion core-shell structure to form a multilayer structure, the nano Beta molecular sieve is added, one side has the effect of a filler, the other side has the effect of an inner core, the addition of phosphate starch is beneficial to improvement of the compatibility among the raw materials such as the nano particles, the sodium acrylate and the acrylamide, the phosphate starch and the nano Beta molecular sieve are beneficial to improvement of the gel strength of a product, and the profile control and water plugging effects of the product are better exerted;
2. the polymerization degree is adjusted, product performance is improved, product using effect is improved, and product market popularization is facilitated.
Detailed Description
The oil field generally uses nano composite microsphere plugging agent to solve the problems of flow-around, etc., and the production method of the commonly used nano composite microsphere plugging agent uses raw materials of acrylamide, acrylate, etc. as monomers to prepare gel through polymerization, and has the functions of water plugging and profile control. In view of the above-mentioned related technologies, the inventors believe that the gel strength after polymerization of acrylate or acrylamide is not good, which is not good for better performing the water-plugging and profile-controlling function of the water-plugging and profile-controlling agent product. According to the application, a nano-scale nano Beta molecular sieve is added into a nano composite microsphere plugging agent, the nano Beta molecular sieve contains a large number of nano particles, the nano particles contain micropores, the micropores of the nano particles have a certain adsorption effect on sodium ions on sodium acrylate to drive the migration of acrylic acid radical ions to the nano particles, under the action of an initiator, acrylic acid radicals are polymerized on the surfaces of the nano particles to form an anion core-shell structure, acrylamide is polymerized on the surfaces of the anion core-shell structure to form a multilayer structure, the nano Beta molecular sieve is added, one side has the effect of a filler, the other side has the effect of an inner core, the addition of phosphate starch is beneficial to improvement of the compatibility among the raw materials such as the nano particles, the sodium acrylate and the acrylamide, the phosphate starch and the nano Beta molecular sieve are beneficial to improvement of the gel strength of a product, and the profile control and water plugging effects of the product are better exerted.
Examples
The raw materials related to the invention are all commercially available, and the types and sources of the raw materials are shown in table 1.
TABLE 1 Specification, type and origin of the raw materials
The product is preserved in the form of emulsion or solid in actual production. The solid form has a long storage period, is suitable for occasions where the solid form cannot be used as soon as possible, and the product stored in the solid form can be used after being ground to a required size according to the requirement. In the actual production, the product which is not subjected to the ethanol demulsification and drying processes can be stored in the form of emulsion, and the method is suitable for occasions where the product can be used as soon as possible (for example, the product can be used only after being placed for 0-5 days).
Example 1: a preparation method of a nano composite microsphere plugging agent for water shutoff and profile control of a low-permeability oilfield comprises the following steps:
s1, mixing materials: taking 70kg of deionized water (the conductivity is 18 mu s/cm), adding 2.5kg of phosphate starch and 0.25kg of ammonium acetate auxiliary agent, stirring at the rotating speed of 100 r/min, cooling to 20 ℃, adding 33kg of sodium acrylate, 4.5kg of acrylamide, 4.5kg of nano Beta molecular sieve and 0.5kg of cross-linking agent, and continuously stirring for 10min to obtain a mixed solution.
S2, polymerization reaction: adding 0.5kg of potassium persulfate into the mixed solution, stirring at the rotating speed of 200 revolutions per minute, heating to 60 ℃ for reaction for 12 hours, adding 21kg of ethanol for demulsification, uniformly mixing, stopping stirring, standing for 40min, precipitating out a large amount of precipitate, filtering, and drying the filter cake at 70 ℃ for 270min to obtain the nano composite microsphere plugging agent for water shutoff and profile control of the low-permeability oilfield.
Example 2
Example 2 differs from example 1 in that example 2 replaces methylene acrylamide with an equal mass of polyethylene glycol diacrylate, all otherwise in accordance with example 1.
Example 3
Example 3 differs from example 1 in that example 3 uses an equal mass of ammonium persulfate in place of potassium persulfate, all otherwise in accordance with example 1.
Example 4
Example 4 differs from example 1 in that no ammonium acetate was added to example 4, all else remaining the same as in example 1.
Example 5
The difference between the example 5 and the example 1 is that the ethanol is not used for demulsification in the example 5, the stirring is stopped after the reaction at 60 ℃ in the example 5 is finished, the mixture is kept stand for 40min, and the material is dried at 70 ℃ for 270min to prepare the nano composite microsphere plugging agent for water shutoff and profile control of the low permeability oilfield, and the rest is consistent with that in the example 1.
Examples 6 to 13
Examples 6 to 13 are different from example 1 in that the amounts of the respective raw materials of examples 6 to 13 were different from each other and were identical to example 1, and the amounts of the respective raw materials of examples 6 to 13 were shown in Table 2.
TABLE 2 addition amounts of the respective raw materials of examples 6 to 13
Examples 14 to 17
Examples 14-17 differ from example 1 in that the process parameters for each step of examples 14-17 are different and are otherwise identical to example 1, and the process parameters for each step of examples 14-17 are shown in Table 3.
TABLE 3 parameters in the various steps of examples 14-17
Comparative example
Comparative example 1
Comparative example 1 differs from example 1 in that comparative example 1 does not incorporate the nano Beta molecular sieve and the phosphate starch, all of which are otherwise identical to example 1.
Performance detection
1. Expansion factor: weighing 20g of product, measuring and recording the volume of 20g of product by using a measuring cylinder, adding water into the product according to the ratio of the product to the water of 1 (mass ratio) to 20 (mass ratio), uniformly mixing, standing for 24h, filtering the swelling substance by using a filter screen with the aperture of 150 mu m, sucking excess water on the surface of the swelling substance by using filter paper, measuring and recording the volume of the swelling substance by using the measuring cylinder, and dividing the volume of the swelling substance by the volume of 20g of product to obtain the expansion multiple, wherein the experimental result is shown in Table 4.
2. Gel strength: placing the gel product into gel strength tester, and loading the lower end face (diameter 5.3mm, cross-sectional area 0.22 cm) of the glass rod 2 ) Contacting the gel, adding weight into the tray above the glass rod, and calculating the total mass (g/cm) of the glass rod in unit area when the glass rod is 10cm deep into the gel 2 ) I.e., gel strength, the results are shown in table 4.
TABLE 4 comparison table of different product performance test results
| Sample numbering | Expansion factor | Gel Strength (g/cm) 2 ) |
| Example 1 | 4.51 | 816 |
| Example 2 | 4.17 | 793 |
| Example 3 | 4.05 | 824 |
| Example 4 | 3.72 | 812 |
| Example 5 | 3.14 | 738 |
| Example 6 | 3.98 | 831 |
| Example 7 | 4.76 | 587 |
| Example 8 | 4.65 | 635 |
| Example 9 | 3.43 | 856 |
| Example 10 | 4.24 | 795 |
| Example 11 | 4.17 | 802 |
| Example 12 | 4.28 | 807 |
| Example 13 | 4.56 | 812 |
| Example 14 | 4.47 | 819 |
| Example 15 | 4.42 | 821 |
| Example 16 | 4.61 | 798 |
| Example 17 | 4.54 | 804 |
| Comparative example 1 | 4.78 | 173 |
Comparative example 1 no nano Beta molecular sieve and phosphate starch were added, and the prepared product had good swelling properties, but poor gel strength, and was not good for better exerting the water shutoff profile control effect of the product, and not good for product market promotion.
Comparing the experimental results of example 1 and comparative example 1, it can be seen that, in the process of preparing the nano composite microsphere plugging agent for water shutoff and profile control in low permeability oil field, the nano Beta molecular sieve and the phosphate starch are added, and the prepared nano composite microsphere plugging agent for water shutoff and profile control in low permeability oil field has good expansion performance and excellent gel strength performance, is beneficial to better exerting the water shutoff and profile control effect of the product, and is beneficial to market popularization of the product.
Comparing the experimental results of example 1 and example 2, in example 2, methylene acrylamide is replaced by polyethylene glycol diacrylate, and the expansion performance and the strength performance of the prepared nano composite microsphere plugging agent product for water plugging and profile control of low permeability oilfield have no obvious change. Comparing the experimental results of example 1 and example 3, example 3 uses ammonium persulfate instead of potassium persulfate, and the expansion performance and strength performance of the prepared nano composite microsphere plugging agent product for water plugging and profile control of low permeability oilfield have no obvious change. Comparing the experimental results of example 1 and example 4, in example 4, no ammonium acetate was added, and the swelling performance of the prepared nanocomposite microsphere plugging agent product for water plugging and profile control in low permeability oilfield was slightly reduced. Comparing the experimental results of example 1 and example 5, in example 5, ethanol is not used for demulsification, and the expansion performance of the prepared nano composite microsphere plugging agent product for water plugging and profile control of the low permeability oilfield is reduced, which is not beneficial to market popularization.
Compared with the embodiment 1, the addition amount of each raw material in the embodiments 6 to 13 is different, the process parameters in the steps of the embodiments 14 to 17 are different, and the prepared nano composite microsphere plugging agent product for water shutoff and profile control of the low-permeability oilfield has excellent expansion performance and strength performance, is favorable for better exerting the water shutoff and profile control effect of the product, and is favorable for market popularization of the product.
The embodiments of the present invention are all preferred embodiments of the present invention, and the scope of the present invention is not limited thereby, so: all equivalent changes made according to the structure, shape and principle of the invention are covered by the protection scope of the invention.
Claims (5)
1. The nano composite microsphere plugging agent for water shutoff and profile control of the low-permeability oilfield is characterized by mainly comprising the following profile control agent raw materials in parts by weight: 20-46 parts of sodium acrylate, 3-6 parts of acrylamide, 0.2-0.8 part of cross-linking agent, 1-8 parts of nano Beta molecular sieve, 0.1-0.9 part of initiator and 60-80 parts of deionized water; the profile control agent raw material also comprises an auxiliary agent, wherein the auxiliary agent comprises 1-4 parts by weight of phosphate ester starch and 0.1-0.4 part by weight of ammonium acetate;
the preparation method of the nano composite microsphere plugging agent for water plugging and profile control of the low-permeability oilfield comprises the following steps:
s1, mixing materials: adding an auxiliary agent into deionized water, uniformly mixing, cooling to a temperature not higher than 25 ℃, adding sodium acrylate, acrylamide, a nano Beta molecular sieve and a cross-linking agent, and uniformly mixing to obtain a mixed solution;
s2, polymerization reaction: adding an initiator into the mixed solution, stirring at the rotating speed of 100-300 r/min, heating to 50-70 ℃ for reacting for 8-15h, adding ethanol with the weight 0.2-0.4 time that of deionized water for demulsification, filtering, and drying the filter cake at 65-80 ℃ for 200-300min to prepare the nano composite microsphere plugging agent for water shutoff and profile control of the low-permeability oilfield.
2. The nano-composite microsphere plugging agent for water shutoff and profile control of low permeability oilfield according to claim 1, which is characterized by being mainly prepared from the following profile control agent raw materials in parts by weight: 30-36 parts of sodium acrylate, 3-6 parts of acrylamide, 0.4-0.6 part of cross-linking agent, 3-6 parts of nano Beta molecular sieve, 0.4-0.6 part of initiator, 60-80 parts of deionized water and 2-3 parts of phosphate starch.
3. The nanocomposite microsphere plugging agent for water shutoff and profile control of low permeability oilfield according to claim 1, wherein the nanocomposite microsphere plugging agent comprises: the cross-linking agent is N, N-methylene diacrylamide or polyethylene glycol diacrylate.
4. The nanocomposite microsphere plugging agent for water shutoff and profile control of low permeability oilfield according to claim 2, wherein the nanocomposite microsphere plugging agent comprises: the initiator is potassium persulfate or ammonium persulfate.
5. The nanocomposite microsphere plugging agent for water shutoff and profile control of low permeability oilfield according to claim 1, wherein the nanocomposite microsphere plugging agent comprises: the average grain diameter of the nano Beta molecular sieve is 20-40nm.
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