CN111087998A - Slow-expansion particles and preparation method thereof - Google Patents
Slow-expansion particles and preparation method thereof Download PDFInfo
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Abstract
The application provides a preparation method of slow-swelling particles, which comprises the following steps: 1) obtaining reaction raw materials, wherein the reaction raw materials comprise a graftable copolymer, acrylic acid, acrylamide, a cross-linking agent, an initiator and water; 2) dissolving acrylic acid and acrylamide in water, adding the graft copolymer, fully dissolving, and introducing N2Then adding the initiator and the cross-linking agent, mixing uniformly, and continuously introducing N during mixing2Obtaining a mixture system; 3) reacting the mixed system under the heating condition to obtain a slow swelling gel block; 4) drying and powdering the slow swelling gel blockCrushing and sieving to obtain the slow swelling granule.
Description
Technical Field
The application provides a slow-swelling particle and a preparation method thereof.
Background
The proven reserves of the carbonate hydrocarbon reservoir account for more than 50% of the total amount of oil and gas resources, wherein more than 30% of the carbonate hydrocarbon reservoir is a fracture-cavity type hydrocarbon reservoir, and the development potential is huge. The Tahe oil field Ordovician reservoir is a typical representative of carbonate rock oil and gas reservoirs discovered in China, and has become the second largest oil and gas production area of medium petrochemicals except for the victory oil field due to large reserves.
The reservoir body of the oil reservoir is influenced by a plurality of functions such as tectonic movement, karst superposition transformation, multi-phase reservoir formation and the like, the reservoir body is generally a composite medium and comprises karst caves, cracks and dissolved pores, discontinuity exists in spatial distribution, a matrix does not have the capacity of storing and permeating, the heterogeneity of the reservoir layer is strong, and the relation of oil and water is complex. Leading to difficulties in the development of such reservoirs. Particularly in recent years, with the pressure attenuation and the water content increase in the middle and later stages of development, the water invasion of the bottom water of some oil wells is serious year by year, and the number of high-water-content oil wells increases year by year and reaches about 320; the water injection and water flooding efficiency shows a trend of deterioration, the water injection effect of a well group is deteriorated, the failure proportion is increased, the water flooding response degree is only 33.6 percent, the unidirectional effect and water channeling become main development contradictions, and the tower and river recovery ratio is only 14.8 percent and is far lower than the average level at home and abroad.
The large-area water outlet of the oil field causes the overall effect of oil field development to be poor, and great economic loss is caused, so that oil-stabilizing and water-controlling measures must be carried out to reduce the water content. On the premise of meeting the production requirements of oil fields, the water plugging technology is the best measure for reducing water outlet.
However, the water plugging of the carbonate fracture-cave type reservoir in the tower river oil field faces a plurality of technical difficulties, such as strong reservoir heterogeneity, complex underground oil-water relationship, difficult determination of water outlet layer sections and the like, so that the adaptability of the conventional water plugging process is poor; the effective application of the conventional high-strength or selective plugging agent is severely restricted by the characteristics of strong flow conductivity of a flow channel of a fracture-cavity reservoir, low stratum pressure gradient, easiness in leakage after production and vacancy, ultra-deep reservoir, high-temperature and high-salinity (the burial depth is 5400-6600 m, the temperature is 120-140 ℃, and the mineralization degree is 210-240 g/L) and the like.
Patent CN 102618232B (plugging agent for fracture-cavity type oil reservoir) reports a method for plugging water in fracture-cavity type oil reservoir, and is especially suitable for high salinity fracture-cavity type oil reservoir. The method comprises the steps of preparing a mixed solution from cement, micro-silicon, sodium bentonite, a polymer dispersant, a retarder and a sodium carbonate aqueous solution, injecting the mixed solution into an oil well, closing the well for a period of time, and then opening the well for production. Due to the fact that the density difference of the plugging agent and oil and water is utilized, the plugging agent can effectively reside between oil and water interfaces in the water plugging process of the fracture-cavity oil reservoir to plug a water outlet channel, oil and water in the water plugging agent are high in selectivity and strength, high-strength selective water plugging is achieved, and the on-site water control and oil increasing effects are obvious.
The patent CN 102587858B (method for water plugging of fracture-cavity reservoir) reports the use of CN 102618232B (plugging agent for fracture-cavity reservoir).
Patent CN 102746835B (carbonate oil well density selective water shutoff agent and preparation process thereof) reports a carbonate oil well density selective water shutoff agent and preparation process thereof. The invention prepares cement, fly ash, clay, micro-silicon, early strength agent and fluid loss agent into aqueous solution according to a certain proportion. By utilizing the density selectivity of the water plugging agent, the water plugging partition plate is easy to stay between oil-water interfaces, and plays a role in precipitation and oil increase.
According to the technical scheme, an oil-water interface low-density selective plugging agent system is developed indoors by optimizing different component ratios of superfine cement, a permeation enhancer, a framework bridging agent, a density regulator, a suspension dispersant, a water reducer, a retarder and the like in the document (evaluation of the performance of the Wexue oil-water interface low-density selective plugging agent [ J ]. development of fine petrochemical industry, 2015,16(4): 21-24).
The literature (Wu civilization, Tahe oilfield carbonate fracture-vug type reservoir water plugging technology [ J ] oil gas geology and recovery ratio, 2013,20(6): 104-.
In summary, the water plugging method for the fracture-cavity carbonate reservoir reported in the prior art is only suitable for reservoirs with obvious oil-water interfaces, and the related plugging agent and construction method can utilize the characteristic of density difference of fluid under the reservoir condition to play a role in water plugging; however, for water outflow of a fractured reservoir in a fractured-vuggy reservoir, fractures are not only seepage channels but also reservoir spaces, and reservoir fluids have no obvious oil-water interface, so that the existing method is difficult to meet the field requirements.
The better the fracture connectivity, the higher the fracture permeability and the lower the reservoir mobility. In the reservoir body of the type, oil and water have no obvious interface, and the existing plugging agent product depending on density selectivity is difficult to meet the requirement; meanwhile, due to the development of cracks, particularly the development of vertical large cracks, a single component cannot fill large crack channels, so that a large amount of plugging agent is leaked from the cracks, and finally the formed plugging agent cannot meet the field requirements.
Therefore, the existing plugging agent still has great room for improvement in technology and performance. The research and development of the water plugging agent with excellent performance aiming at the water plugging of the fractured reservoir body undoubtedly can generate positive effects on the development of the existing fractured-vuggy carbonate rock oil reservoir and finally show economic benefits which all have important influences.
Disclosure of Invention
One of the applications provides a preparation method of slow-swelling particles, which comprises the following steps:
1) obtaining reaction raw materials, wherein the reaction raw materials comprise a graftable copolymer, acrylic acid, acrylamide, a cross-linking agent, an initiator and water;
2) dissolving acrylic acid and acrylamide in water, adding the graft copolymer, fully dissolving, and introducing N2Then adding the initiator and the cross-linking agent, mixing uniformly, and continuously introducing N during mixing2Obtaining a mixture system;
3) reacting the mixed system under the heating condition to obtain a slow swelling gel block;
4) and drying, crushing and sieving the slow swelling gel block to obtain the slow swelling granules.
In one embodiment, the graftable copolymer comprises 10% to 55%, the acrylamide comprises 5% to 10%, the acrylic acid comprises 3% to 5%, the crosslinking agent comprises 0.03% to 0.5%, the initiator comprises 0.02% to 0.15%, and the water comprises 29.35% to 81.95%, based on 100% of the total mass of the mixture system.
In one embodiment, in step 2), N is introduced for the first time2For 10 to 30 minutes, and introducing N for the second time2For a period of 5 to 15 minutes.
In one embodiment, in step 3), the reaction is heated to 50 to 55 ℃ for 4 to 6 hours.
In one embodiment, the graftable copolymer is selected from at least one of chitin, chitosan, soluble starch, carboxymethylcellulose, guar gum and fenugreek gum.
In one embodiment, the crosslinking agent is an organotitanium crosslinking agent.
In one embodiment, the organotitanium crosslinking agent is prepared as follows: mixing triethanolamine and ethanol, adding tetraisopropyl titanate under the condition of stirring, heating and continuously stirring for reaction, thereby obtaining the organic titanium crosslinking agent.
In one embodiment, in the process of preparing the organic titanium crosslinking agent, the mass ratio of the triethanolamine, the ethanol and the tetraisopropyl titanate is (1-2): 0.8: (0.8-0.4).
In one embodiment, during the preparation of the organotitanium crosslinking agent, the temperature is raised to 45 to 65 ℃ for reaction for 3 to 6 hours.
In a specific embodiment, in the preparing of the organic titanium crosslinking agent, the initiator is at least one of ammonium persulfate, potassium persulfate, sodium sulfite, and sodium bisulfite.
In one embodiment, in step 3), the temperature of drying is 80 to 95 ℃, and the time of drying is 5 to 12 hours; the granularity after crushing and sieving is 100 to 120 meshes.
The second application provides slow-swelling particles prepared by the preparation method in the first application.
The third application provides the application of the slow-swelling particles prepared by the preparation method in the third application in profile control and water shutoff.
The fourth application provides a method for blocking water in an oil reservoir and an oil well, which comprises the following steps:
I) injecting a first plugging agent into the oil well at the front section plug, wherein the first plugging agent is a first mixture comprising expansion-slowing particles and water; wherein, the slow swelling particles are prepared by the preparation method in any one of the application;
II) injecting a second plugging agent into the well at the body slug, the second plugging agent being a second mixture comprising polyacrylamide and an organic cross-linking agent (e.g., polyethyleneimine) with water; wherein the polyacrylamide has a degree of hydrolysis of 15% to 30% and a molecular weight of 500 to 2000 ten thousand;
II) injecting a third plugging agent into the oil well at the sealing section plug, wherein the third plugging agent is a third mixture comprising sodium soil, cement, a retarder and water.
In a specific embodiment, the content of the slow swelling particles in the first mixture is 0.2% to 2% by mass.
In a specific embodiment, the content of the polyacrylamide in the second mixture is 0.5% to 1.5% by mass; the polyethyleneimine is present in the second mixture in an amount of 0.15% to 0.35%.
In a specific embodiment, the content of the sodium soil in the third mixture is 5 to 10% by mass; the content of the cement in the third mixture is 20% to 40%; the retarder is present in the third mixture in an amount of 0.01% to 1%.
In a particular embodiment, the total amount of said first, second and third plugging agent does not exceed 500m3。
In a specific embodiment, the concentration of the water solution of the slow swelling particle of the front slug is not particularly limited, and preferably, the amount of the first plugging agent is 10 to 25 percent of the total amount by volume percentage.
In a specific embodiment, the concentration of the system in the bulk slug is not particularly limited, and preferably, the second plugging agent is used in an amount of 60 to 75 volume percent of the total amount.
In a specific embodiment, the concentration of the system for sealing the slug is not particularly limited, and preferably, the third plugging agent is used in an amount of 10 to 15% by volume of the total amount.
In one embodiment, the injection speed of the plugging agent in step I), step II) and step III) is 3-15m independently3/h。
In one embodiment, the injection rate of the plugging agent in step I), step II) and step III) is preferably 9 to 10m, independently of each other3H is used as the reference value. However, the injection speed in the actual use process needs to be determined according to the field situation, and can be controlled to be any value within a certain range.
In a specific embodiment, the cement is a grade G cement.
In one embodiment, the set retarder is a borate and/or silicate. Such as sodium borate.
"graftable copolymer" as used herein refers to a copolymer that has not undergone a grafting reaction, wherein the backbone units of the "copolymer" are capable of incorporating other monomer units to form new branches.
The beneficial effect of this application:
(1) the slow expansion particles can be prepared into particles with proper particle size according to the on-site requirement, so the particle size is adjustable, the preparation and on-site pump injection are facilitated, and meanwhile, the slow expansion particles have good high temperature resistance, high calcium magnesium resistance and high mineralization degree resistance;
(2) the slow expansion particles slowly absorb water and expand, so that the slow expansion particles can be injected into deep parts in the stratum, and after the slow expansion particles completely absorb water, gel particles with high strength and certain toughness are formed;
(3) the slow expansion particles can be used under the conditions of high temperature, high calcium and magnesium and high mineralization degree, can effectively block cracks, block water outlet channels and finally achieve the purposes of oil increasing and water controlling.
(4) The method for blocking water in the oil reservoir oil well has wide application range of stratum conditions, and the temperature of the stratum needing water blocking is preferably less than or equal to 150 ℃, and more preferably 90-140 ℃; the degree of mineralization of the groundwater is preferably less than or equal to 250,000 mg/L. The method can realize effective plugging of the fractured carbonate reservoir, inhibit water invasion of the oil well, improve the production effect of the oil well, improve the overall production effect of the block and have good application prospect.
Detailed Description
The present invention is further illustrated by the following examples, which are intended to be purely exemplary of the invention and are not to be construed as limiting the invention in any way.
The starting materials used in the present application are commercially available unless otherwise specified.
Example 1
Preparation of organic titanium crosslinking agent
Weighing triethanolamine, industrial alcohol and tetraisopropyl titanate in sequence according to the mass ratio of 1.2:0.6:1, mixing the triethanolamine and the alcohol, adding the tetraisopropyl titanate under the stirring condition, heating to 55 ℃, continuously stirring for reaction for 5 hours, sampling, dripping into water to be completely dissolved, and stopping the reaction to obtain the organic titanium crosslinking agent No. 1, wherein the liquid color is orange brown. Used in the next step without purification.
Example 2
Preparation of organic titanium crosslinking agent
Weighing triethanolamine, industrial alcohol and tetraisopropyl titanate in sequence according to the mass ratio of 1:0.8:0.8, mixing the triethanolamine and the alcohol, adding the tetraisopropyl titanate under the stirring condition, heating to 45 ℃, reacting for 6 hours, sampling, dripping into water to be completely dissolved, and stopping the reaction to obtain the organic titanium crosslinking agent No. 2, wherein the liquid color is orange brown. Used in the next step without purification.
Example 3
Preparation of organic titanium crosslinking agent
Weighing triethanolamine, industrial alcohol and tetraisopropyl titanate in sequence according to the mass ratio of 2:0.8:0.4, mixing the triethanolamine and the alcohol, adding the tetraisopropyl titanate under the stirring condition, heating to 60 ℃, reacting for 3 hours, sampling, dripping into water to be completely dissolved, and stopping the reaction to obtain the organic titanium crosslinking agent No. 3, wherein the liquid color of the organic titanium crosslinking agent is orange brown. Used in the next step without purification.
Example 4
Preparation of slow swelling granules
Taking 10 parts by mass of chitin, 5 parts by mass of acrylamide monomer, 3 parts by mass of acrylic acid monomer, 0.03 part by mass of organic phthalein cross-linking agent 1# and 0.02 part by mass of potassium persulfate, and the balance of water, wherein the total mass is 100 parts by mass.
Adding weighed acrylic acid and acrylamide into a four-mouth bottle, adding water to dissolve, adding chitin, continuously stirring to fully dissolve, and introducing N2After 10 minutes, adding weighed potassium persulfate and organic phthalein cross-linking agent No. 1, fully and uniformly stirring, and continuously introducing N during the period25 minutes, a mixture system was obtained. Sealing the prepared mixture system, putting the mixture system into a thermostat (BINDER ED115) at 50 ℃, and reacting for 4 hours under a heating condition to obtain a slow swelling gel block; and (3) putting the prepared slow swelling gel block into an oven (BINDER ED115) at 85 ℃ for drying, and crushing into 100-mesh and 120-mesh particles by using a crusher (ZT-600 type), thereby obtaining the slow swelling particles 4 #.
Example 5
Preparation of slow swelling granules
Based on 100 parts by mass of the total amount, 55 parts by mass of chitin, 10 parts by mass of an acrylamide monomer, 5 parts by mass of an acrylic acid monomer, 0.5 part by mass of an organic phthalein cross-linking agent 1#, 0.15 part by mass of potassium persulfate and the balance of water are taken.
Adding weighed acrylic acid and acrylamide into a four-mouth bottle, adding water to dissolve, adding chitin, continuously stirring to fully dissolve, and introducing N2After 15 minutes, adding weighed potassium persulfate and organic phthalein cross-linking agent No. 1, fully and uniformly stirring, and continuously introducing N during the period215 minutes, a mixture system was obtained. Sealing the prepared mixture system, putting the mixture system into a thermostat (BINDER ED115) at 75 ℃, and reacting for 6 hours under a heating condition to obtain a slow swelling gel block; and (3) putting the prepared slow swelling gel block into an oven (BINDER ED115) at 85 ℃ for drying, and crushing into 100-mesh and 120-mesh particles by using a crusher (ZT-600 type), thereby obtaining the slow swelling particles 5 #.
Example 6
Preparation of slow swelling granules
Taking 25 parts by mass of chitin, 8 parts by mass of acrylamide monomer, 5 parts by mass of acrylic acid monomer, 0.15 part by mass of organic phthalein cross-linking agent 1# and 0.1 part by mass of potassium persulfate, and the balance of water, wherein the total mass is 100 parts by mass.
Adding weighed acrylic acid and acrylamide into a four-mouth bottle, adding water to dissolve, adding chitin, continuously stirring to fully dissolve, and introducing N2After 10 minutes, adding weighed potassium persulfate and organic phthalein cross-linking agent No. 1, fully and uniformly stirring, and continuously introducing N during the period215 minutes, a mixture system was obtained. Sealing the prepared mixture system, putting the mixture system into a thermostat (BINDER ED115) at 75 ℃, and reacting for 5 hours under a heating condition to obtain a slow swelling gel block; and (3) putting the prepared slow swelling gel block into an oven (BINDER ED115) at 85 ℃ for drying, and crushing into 100-mesh and 120-mesh particles by using a crusher (ZT-600 type), thereby obtaining the slow swelling particles 6 #.
Example 7
Preparation of slow swelling granules
According to the total amount of 100 parts, 10 parts by mass of chitosan, 5 parts by mass of acrylamide monomer, 3 parts by mass of acrylic acid monomer, 0.03 part by mass of organic phthalein cross-linking agent 2#, 0.02 part by mass of ammonium persulfate and the balance of water are taken.
Adding weighed acrylic acid and acrylamide into a four-mouth bottle, adding water to dissolve, adding chitosan, continuously stirring to fully dissolve, and introducing N2After 10 minutes, adding weighed ammonium persulfate and organic phthalein cross-linking agent No. 2, fully and uniformly stirring, and continuously introducing N during the period2For 5 minutes. Sealing the prepared mixture system, putting the mixture system into a thermostat (BINDERED115) at 50 ℃, and reacting for 4 hours under a heating condition to obtain a slow swelling gel block; and (3) putting the prepared slow swelling gel block into an oven (BINDER ED115) at 85 ℃ for drying, and crushing into 100-mesh and 120-mesh particles by using a crusher (ZT-600 type), thereby obtaining the slow swelling particles 7 #.
Example 8
Preparation of slow swelling granules
According to the total amount of 100 parts by mass, 55 parts by mass of chitosan, 10 parts by mass of acrylamide monomer, 5 parts by mass of acrylic acid monomer, 0.5 part by mass of organic phthalein cross-linking agent 3#, 0.15 part by mass of ammonium persulfate and the balance of water are taken.
Adding weighed acrylic acid and acrylamide into a four-mouth bottle, adding water to dissolve, adding chitosan, continuously stirring to fully dissolve, and introducing N215 minutes later, then adding weighed ammonium persulfate and organic phthalein cross-linking agent No. 3, fully and uniformly stirring, and continuously introducing N during the period2For 15 minutes. Sealing the prepared mixture system, putting the mixture system into a thermostat (BINDERED115) at 75 ℃, and reacting for 6 hours under a heating condition to obtain a slow swelling gel block; and (3) putting the prepared slow swelling gel block into an oven (BINDER ED115) at 85 ℃ for drying, and crushing into 100-mesh and 120-mesh particles by using a crusher (ZT-600 type), thereby obtaining the slow swelling particles 8 #.
Example 9
Preparation of slow swelling granules
According to the total amount of 100 parts by mass, 25 parts by mass of carboxymethyl cellulose, 8 parts by mass of acrylamide monomer, 5 parts by mass of acrylic acid monomer, 0.15 part by mass of organic phthalein cross-linking agent 1#, 0.1 part by mass of sodium persulfate and the balance of water are taken.
Adding weighed acrylic acid and acrylamide into a four-mouth bottle, adding water to dissolve, adding chitosan, continuously stirring to fully dissolve, and introducing N2After 10 minutes, adding weighed sodium persulfate and organic phthalein cross-linking agent No. 1, fully and uniformly stirring, and continuously introducing N during the period2For 15 minutes. Sealing the prepared mixture system, putting the mixture system into a thermostat (BINDERED115) at 75 ℃, and reacting for 5 hours under a heating condition to obtain a slow swelling gel block; and (3) putting the prepared slow swelling gel block into an oven (BINDER ED115) at 85 ℃ for drying, and crushing into 100-mesh and 120-mesh particles by using a crusher (ZT-600 type), thereby obtaining the slow swelling particles 9 #.
Example 10
Preparation of slow swelling granules
According to the total amount of 100 parts by mass, 10 parts by mass of soluble starch, 5 parts by mass of acrylamide monomer, 3 parts by mass of acrylic acid monomer, 0.03 part by mass of organic phthalein cross-linking agent 1#, 0.02 part by mass of ammonium persulfate and the balance of water are taken.
Adding weighed acrylic acid and acrylamide into a four-mouth bottle, adding water to dissolve, adding soluble starch, and continuously stirring to fully stirDissolving, introducing N2After 10 minutes, adding weighed ammonium persulfate and organic phthalein cross-linking agent No. 1, fully and uniformly stirring, and continuously introducing N during the period2For 5 minutes. Sealing the prepared mixture system, putting the mixture system into a thermostat (BINDER ED115) at 50 ℃, and reacting for 4 hours under a heating condition to obtain a slow swelling gel block; and (3) putting the prepared slow swelling gel block into an oven (BINDER ED115) at 85 ℃ for drying, and crushing into 100-mesh and 120-mesh particles by using a crusher (ZT-600 type), thereby obtaining the slow swelling particles of 10 #.
Example 11
Preparation of slow swelling granules
According to the total amount of 100 parts by mass, 55 parts by mass of soluble starch, 10 parts by mass of acrylamide monomer, 5 parts by mass of acrylic acid monomer, 0.5 part by mass of organic phthalein cross-linking agent 1#, 0.15 part by mass of ammonium persulfate and the balance of water are taken.
Adding weighed acrylic acid and acrylamide into a four-mouth bottle, adding water to dissolve, adding soluble starch, continuously stirring to fully dissolve, and introducing N215 minutes later, then adding weighed ammonium persulfate and organic phthalein cross-linking agent No. 1, fully and uniformly stirring, and continuously introducing N during the period2For 15 minutes. Sealing the prepared mixture system, putting the mixture system into a thermostat (BINDER ED115) at 75 ℃, and reacting for 6 hours under a heating condition to obtain a slow swelling gel block; and (3) putting the prepared slow swelling gel block into an oven (BINDER ED115) at 85 ℃ for drying, and crushing into 100-mesh and 120-mesh particles by using a crusher (ZT-600 type), thereby obtaining the slow swelling particles 11 #.
Example 12
Preparation of slow swelling granules
According to the total amount of 100 parts by mass, 25 parts by mass of soluble starch, 8 parts by mass of acrylamide monomer, 5 parts by mass of acrylic acid monomer, 0.15 part by mass of organic phthalein cross-linking agent 1#, 0.1 part by mass of ammonium persulfate and the balance of water are taken.
Adding weighed acrylic acid and acrylamide into a four-mouth bottle, adding water to dissolve, adding soluble starch, continuously stirring to fully dissolve, and introducing N2After 10 minutes, the weighed ammonium persulfate and the organic phthalein cross-linking agent No. 1 are added and fully stirred uniformlyDuring the period of homogenizing, continuously introducing N2For 15 minutes. Sealing the prepared mixture system, putting the mixture system into a thermostat (BINDER ED115) at 75 ℃, and reacting for 5 hours under a heating condition to obtain a slow swelling gel block; and (3) putting the prepared slow swelling gel block into an oven (BINDER ED115) at 85 ℃ for drying, and crushing into 100-mesh and 120-mesh particles by using a crusher (ZT-600 type), thereby obtaining the slow swelling particles 12 #.
Example 13
Preparation of slow swelling granules
According to the total amount of 100 parts by mass, 25 parts by mass of guar gum, 8 parts by mass of acrylamide monomer, 5 parts by mass of acrylic acid monomer, 0.15 part by mass of organic phthalein cross-linking agent 1#, 0.1 part by mass of ammonium persulfate and the balance of water are taken.
Adding weighed acrylic acid and acrylamide into a four-mouth bottle, adding water to dissolve, adding fenugreek gum, continuously stirring to fully dissolve, and introducing N2After 10 minutes, adding weighed ammonium persulfate and organic phthalein cross-linking agent No. 1, fully and uniformly stirring, and continuously introducing N during the period2For 15 minutes. Sealing the prepared mixture system, putting the mixture system into a thermostat (BINDERED115) at 75 ℃, and reacting for 5 hours under a heating condition to obtain a slow swelling gel block; and (3) putting the prepared slow swelling gel block into an oven (BINDER ED115) at 85 ℃ for drying, and crushing into 100-mesh and 120-mesh particles by using a crusher (ZT-600 type), thereby obtaining the slow swelling particles 13 #.
Example 14
Preparation of slow swelling granules
According to the total amount of 100 parts by mass, 25 parts by mass of fenugreek gum, 8 parts by mass of acrylamide monomer, 5 parts by mass of acrylic acid monomer, 0.15 part by mass of organic phthalein cross-linking agent 1#, 0.1 part by mass of ammonium persulfate and the balance of water are taken.
Adding weighed acrylic acid and acrylamide into a four-mouth bottle, adding water to dissolve, adding fenugreek gum, continuously stirring to fully dissolve, and introducing N2After 10 minutes, adding weighed ammonium persulfate and organic phthalein cross-linking agent No. 1, fully and uniformly stirring, and continuously introducing N during the period2For 15 minutes. Sealing the prepared mixture, placing into 75 deg.C incubator (BINDERED115), and reacting under heating5 hours, preparing the slow swelling gel block; and (3) putting the prepared slow swelling gel block into an oven (BINDER ED115) at 85 ℃ for drying, and crushing into 100-mesh and 120-mesh particles by using a crusher (ZT-600 type), thereby obtaining the slow swelling particles 14 #.
Example 15
Evaluation of Properties of Slow swelling particles
The experimental method comprises the following steps: 0.5g of the slow swelling granules prepared in each example was weighed, respectively, and filled in an ampoule bottle, 30mL of simulated water (total degree of mineralization 230000mg/L, Ca) was added2+、Mg2+13000mg/L), sealing the ampoule bottle, putting the ampoule bottle into an aging tank, and putting the aging tank with the ampoule bottle into an oven at 80 ℃, 120 ℃ and 140 ℃. Wherein, 30 parallel samples, namely 30 samples at 80 ℃, 120 ℃ and 140 ℃, are respectively made in the performance evaluation experiment corresponding to the slow-swelling particles prepared in each example. The particles were weighed at intervals according to table 1, filtered to remove free water, and the expansion factor was calculated according to the formula. The expansion factor is calculated as follows:
expansion factor (mass of expanded particles-mass of initial particles)/mass of initial particles
The results are shown in Table 1.
As can be seen from Table 1, each of the examples exhibited better swelling retarding properties. The lower the temperature, the slower the expansion rate; the higher the temperature, the higher the expansion rate. But shows better delayed expansion performance and stability in the temperature range.
TABLE 1 evaluation of expansion retarding Properties of granules
Example 16
Evaluation of plugging performance of expansion-retarding particles
The experimental method comprises the following steps: 100-1 prepared in examples 7, 10 and 11 were randomly selected from examples 1 to 14 and weighed20 mesh slow swelling granule, simulated formation water (total mineralization 230000mg/L, Ca)2+、Mg2+13000mg/L) as the preparation solution, and respectively preparing the suspension into the slow swelling particle with the mass concentration of 0.20 percent. The sand-packed tubes (2.5 cm. times.30 cm) were saturated with the simulated water and their permeability was measured with a displacement apparatus (model HV-III). Then 0.05PV of slow swelling particle suspension is respectively injected into the sand-packed pipe at the injection speed of 0.3mL/min, and then the sand-packed pipe is placed at the constant temperature of 120 ℃ for 5 days, and then simulated water is respectively injected at the injection speed of 0.3mL/min to displace different water for measuring the permeability (K)b) The measured permeability K of the sand-filled pipe at the moment is calculatedfAccording to the formula η ═ 1-Kf/Kb) The plugging rate η of the slow swelling granules was calculated at 100%, and the results are shown in Table 2.
As can be seen from Table 2, the slow swelling particles still have strong plugging capability under the conditions of high temperature and high mineralization, and the plugging rate is as high as more than 95%.
TABLE 2 Slow expansion particle plugging Properties
Example 17
Implementation in situ
The site implementation is to inject three slugs into the formation by using a cement truck according to the following steps (the total volume is prepared to be 300 m)3)：
Injecting a front-mounted slug into simulated water (total mineralization is 230000mg/L, Ca) according to mass percentage concentration2+、Mg2+13000mg/L) is added with 0.8 percent of plugging agent prepared by slow swelling particles to prepare 45m3(15% of the total) is injected into the formation. Wherein, no sedimentation occurs in the preparation process.
Injecting a main body slug, adding 1.0 percent of polyacrylamide with the molecular weight of 1100 ten thousand and the hydrolysis degree of 25 percent and 0.25 percent of polyethyleneimine organic cross-linking agent into water according to the mass percentage concentration, and preparing 225m3(75% of the total), injecting into the formation;
step three, injecting a sealing slug according toAdding 5 percent of sodium soil, 20 percent of G-grade cement and 0.1 percent of retarder (sodium borate) into water according to mass percentage concentration to prepare 30m3(10% of the total) is injected into the formation.
During the injection process, the injection speed of each slug is kept at 10m3/h。
After the oil field oil well of the embodiment is subjected to water plugging, 2214t of oil production and 7862t of water production are periodically carried out, and the comprehensive water content is 78.03%. The well wheel adopts conventional gel water plugging, 150t of oil production, 3152t of water production and 95.45 percent of comprehensive water content. Compared with the conventional water plugging method, the water plugging method of the embodiment has the advantages that the comprehensive water content is reduced by 17.42 percent compared with the conventional water plugging method in which oil is periodically increased by 2064t, and the oil increasing and water controlling effects are outstanding.
Example 18
Implementation in situ
The field implementation is that a cement truck is utilized to inject three slugs into the stratum according to the following steps:
injecting a front-mounted slug into simulated water (total mineralization is 230000mg/L, Ca) according to mass percentage concentration2+、Mg2+13000mg/L) is added with 0.2 percent of plugging agent prepared by slow swelling particles to prepare 30m3(10% of the total) is injected into the formation. Wherein, no sedimentation occurs in the preparation process.
Injecting a main body slug, adding 0.5 percent of polyacrylamide (molecular weight of 2000 ten thousand and hydrolysis degree of 30 percent) and 0.15 percent of polyethyleneimine organic cross-linking agent into water according to mass percentage concentration, and preparing 225m3(75% of the total), injecting into the formation;
step three, injecting a sealing slug, adding 5 percent of sodium soil, 20 percent of G-grade cement and 0.01 percent of retarder (sodium borate) into water according to the mass percentage concentration, and preparing 45m3(15% of the total) is injected into the formation.
During the injection process, the injection speed of each slug is kept at 9m3/h。
After the oil field oil well of the embodiment is subjected to water plugging, 1876t of oil production, 6528t of water production and 77.67% of comprehensive water content are periodically produced. The well-logging wheel adopts conventional gel water plugging, oil production 102t, water production 4427t and comprehensive water content 97.75 percent. Compared with the conventional water plugging method, the water plugging method of the embodiment has the advantages that the comprehensive water content is reduced by 20.08 percent compared with the conventional water plugging method which increases oil at 1774t periodically, and the oil increasing and water controlling effects are outstanding.
Example 19
Implementation in situ
The field implementation is that a cement truck is utilized to inject three slugs into the stratum according to the following steps:
injecting a front-mounted slug into simulated water (total mineralization is 230000mg/L, Ca) according to mass percentage concentration2+、Mg2+13000mg/L) is added with the plugging agent prepared by 2.0 percent of slow swelling particles to prepare 75m3(20% of the total) is injected into the formation. Wherein, no sedimentation occurs in the preparation process.
Injecting a main body slug, adding 1.5 percent of polyacrylamide with the molecular weight of 500 ten thousand and the hydrolysis degree of 15 percent and 0.35 percent of polyethyleneimine organic cross-linking agent into water according to the mass percentage concentration, and preparing 180m3(60% of the total), injecting into the formation;
step three, injecting a sealing slug, adding 10% of sodium soil, 40% of G-grade cement and 1% of retarder (sodium borate) into water according to the mass percentage concentration, and preparing 45m3(15% of the total) is injected into the formation.
During the injection process, the injection speed of each slug is kept at 9m3/h。
After the oil field oil well of the embodiment is subjected to water plugging, 3581t of oil production, 11253t of water production and 75.86% of comprehensive water content are obtained periodically. The well wheel adopts conventional gel water plugging, oil production is 280t, water production is 5632t, and comprehensive water content is 95.26%. Compared with the conventional water plugging method, the water plugging method of the embodiment has the advantages that the comprehensive water content is reduced by 19.4 percent compared with the conventional water plugging method in which oil is added for 3301t periodically, and the oil-adding and water-controlling effects are outstanding.
While the present application has been described with reference to specific embodiments, those skilled in the art will appreciate that various changes can be made without departing from the true spirit and scope of the present application. In addition, many modifications may be made to adapt a particular situation, material, composition of matter, and method to the objective, spirit and scope of the present application. All such modifications are intended to be included within the scope of the claims of this application.
Claims (10)
1. A preparation method of slow swelling particles comprises the following steps:
1) obtaining reaction raw materials, wherein the reaction raw materials comprise a graftable copolymer, acrylic acid, acrylamide, a cross-linking agent, an initiator and water;
2) dissolving acrylic acid and acrylamide in water, adding the graft copolymer, fully dissolving, and introducing N2Then adding the initiator and the cross-linking agent, mixing uniformly, and continuously introducing N during mixing2Obtaining a mixture system;
3) reacting the mixed system under the heating condition to obtain a slow swelling gel block;
4) and drying, crushing and sieving the slow swelling gel block to obtain the slow swelling granules.
2. The method of claim 1, wherein the graftable copolymer comprises 10% to 55%, the acrylamide comprises 5% to 10%, the acrylic acid comprises 3% to 5%, the crosslinking agent comprises 0.03% to 0.5%, the initiator comprises 0.02% to 0.15%, and the water comprises 29.35% to 81.95%, based on 100% of the total mass of the mixture system.
3. The production method according to claim 1 or 2, wherein in step 2), N is introduced for the first time2For 10 to 30 minutes, and introducing N for the second time2For a period of 5 to 15 minutes.
4. The production method according to any one of claims 1 to 3, wherein in step 3), the reaction is carried out by heating to 50 to 75 ℃ for 4 to 6 hours.
5. The method according to any one of claims 1 to 4, wherein the graftable copolymer is at least one selected from the group consisting of chitin, chitosan, soluble starch, carboxymethyl cellulose, guar gum and fenugreek gum.
6. The production method according to any one of claims 1 to 5, characterized in that the crosslinking agent is an organic titanium crosslinking agent;
preferably, the organic titanium crosslinking agent is prepared as follows: mixing triethanolamine and ethanol, adding tetraisopropyl titanate under the stirring condition, heating and continuously stirring for reaction to obtain the organic titanium crosslinking agent;
more preferably, the mass ratio of the triethanolamine to the ethanol to the tetraisopropyl titanate is (1-2): 0.8: (0.8-0.4);
more preferably, the temperature is raised to 45 to 65 ℃ for 3 to 6 hours.
7. The production method according to any one of claims 1 to 6, characterized in that the initiator is at least one of ammonium persulfate, potassium persulfate, sodium sulfite, and sodium bisulfite.
8. The production method according to any one of claims 1 to 7, wherein in step 3), the temperature of the drying is 80 to 95 ℃ and the time of the drying is 5 to 12 hours; the granularity after crushing and sieving is 100 to 120 meshes.
9. The slow-swelling granules prepared by the preparation method according to any one of claims 1 to 8.
10. Use of the swelling-slowing particles prepared by the preparation method according to any one of claims 1 to 8 in profile control and water shutoff.
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