CN116083067A - Viscoelastic self-regulating and flooding agent for polyacrylamide fracturing and preparation method thereof - Google Patents

Viscoelastic self-regulating and flooding agent for polyacrylamide fracturing and preparation method thereof Download PDF

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CN116083067A
CN116083067A CN202310382324.5A CN202310382324A CN116083067A CN 116083067 A CN116083067 A CN 116083067A CN 202310382324 A CN202310382324 A CN 202310382324A CN 116083067 A CN116083067 A CN 116083067A
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CN116083067B (en
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李宇超
崔长海
李振华
杨建峰
许志强
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Shandong Kexing Chemical Co ltd
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Abstract

The invention belongs to the technical field of petroleum exploitation, and particularly relates to a viscoelastic self-regulating and flooding agent for polyacrylamide fracturing and a preparation method thereof. The preparation method comprises the following steps: sequentially adding acrylamide, p-styrenesulfonic acid, allylpentafluorobenzene, dimethyl diallyl ammonium chloride, natural latex, OP-10, K12, diammonium hydrogen phosphate and deionized water into a reaction kettle, and uniformly stirring to form emulsion; adding an initiator aqueous solution into a first elevated tank, adding a reducing agent aqueous solution into a second elevated tank, slowly dripping the initiator of the first elevated tank into a reaction kettle, dripping the reducing agent aqueous solution of the second elevated tank into the reaction kettle, and heating, stirring and cooling the reaction kettle to obtain a product emulsion; granulating the product emulsion by using a granulator to obtain the product profile control agent. The invention has the advantages of simple synthesis process and no byproducts; meanwhile, the invention has the characteristics of high viscosity, high drag reduction rate and high plugging strength.

Description

Viscoelastic self-regulating and flooding agent for polyacrylamide fracturing and preparation method thereof
Technical Field
The invention belongs to the technical field of petroleum exploitation, and particularly relates to a viscoelastic self-regulating and flooding agent for polyacrylamide fracturing and a preparation method thereof.
Background
The low-permeability and ultra-low-permeability reservoir contains rich oil and gas resources, is the key point of water flooding development in China at present, and because the low-permeability and ultra-low-permeability reservoir is influenced by water flooding for a long time, the heterogeneity of the low-permeability and ultra-low-permeability reservoir is enhanced, the pore permeability is poor, a high-permeability channel is formed, injected water is easy to break through along the high-permeability layer, so that a great amount of water is discharged from an oil well, the productivity of an oil field is influenced, and the economic benefit is poor.
In order to uniformly push injected water, reduce the water outlet of an oil well and improve the oil recovery ratio, the most effective method is to inject a chemical profile control agent from a water injection well to plug a high permeable layer, press a new crack into a stratum, extend the crack so as to adjust the water absorption profile of the water well to improve the recovery ratio, namely, perform fracturing operation.
Polyacrylamide flooding agent is widely applied in the aspect of oil field production increase, but the polyacrylamide is easy to hydrolyze in formation water and is sensitive to some ions in the formation water, so that the viscosity of a polymer can be quickly reduced, and polymer molecular chains of the polymer solution can be deformed and broken after the polymer solution is subjected to strong shearing in pores of a reservoir, so that the viscosity of the polymer solution is quickly reduced, the polymer solution can flow along large pore channels of the reservoir, and the sweep coefficient of the flooding polymer is reduced.
Many fracturing fluids are transported by pumps to boreholes at depths of about 500 meters to 6000 meters or more at high pressure and high flow rates, and the fracturing fluid is transported in the tubing as the pressure from the pumps causes turbulence which causes drag to occur, which consumes more energy.
Therefore, the development of a plurality of high molecular weight post-hydrolysis viscoelasticity profile-control polymers with excellent self-salt tolerance, higher apparent viscosity, good shearing resistance and higher plugging strength becomes the pursuing direction of a plurality of scientific researchers.
Disclosure of Invention
The invention provides a viscoelastic self-regulating and flooding agent for polyacrylamide fracturing and a preparation method thereof. The invention has the advantages of simple synthesis process and no byproducts; meanwhile, the invention has the characteristics of high viscosity, high drag reduction rate and high plugging strength.
In order to achieve the above purpose, one of the purposes of the invention discloses a viscoelastic self-regulating and flooding agent for polyacrylamide fracturing, which has the following molecular structural formula:
Figure SMS_1
wherein:
a=2000-40000;
b=20000-200000;
c=1000-20000;
d=4000-80000;
e=20000-200000;
f=1000-20000;
g=4000-80000。
the self-adjusting and flooding agent has the viscosity average molecular weight of: 10000000-40000000.
The invention further discloses a preparation method of the viscoelastic self-regulating and flooding agent for polyacrylamide fracturing, which comprises the following specific steps:
(1) And (3) purging the reaction kettle and the pipeline with nitrogen for 10-15min, wherein the nitrogen introducing speed is 1000-1200mL/min during purging, and the nitrogen introducing speed is adjusted to be 200-250mL/min in the later synthesis process.
(2) Sequentially adding acrylamide, p-styrenesulfonic acid, allylpentafluorobenzene, dimethyl diallyl ammonium chloride, natural latex, OP-10 (dodecylphenol polyoxyethylene ether), K12 (sodium dodecyl sulfate), diammonium hydrogen phosphate and deionized water into a reaction kettle, stirring at a low speed of 250-300rpm for 5-10min, and regulating pH to 7-8 with 2mol of sodium hydroxide solution; the stirring speed was adjusted to 2000-2200rpm and stirring was continued for 20-30min until all the raw materials had completely become a homogeneous emulsion.
(3) The stirring speed of the reaction kettle is reduced to 250-300rpm, the temperature is slowly raised, and after the temperature reaches 35-40 ℃, the temperature is stopped to be raised, and stirring is continued; adding 10wt% of aqueous solution of an initiator into a first elevated tank, adding 10wt% of aqueous solution of a reducing agent into a second elevated tank, slowly dripping the initiator of the first elevated tank into a reaction kettle for 15min, dripping the aqueous solution of the reducing agent into the reaction kettle for the second elevated tank, controlling the dripping time of the initiator to be 60-90min, controlling the dripping time of the aqueous solution of the reducing agent to be 60-90min, delaying the dripping ending time of the aqueous solution of the reducing agent by 10-20min than the ending time of the initiator, heating the reaction kettle to 70-80 ℃ after dripping, continuously stirring for 40-60min, and cooling to below 40 ℃ to obtain the product emulsion.
(4) Granulating the product emulsion into particles with the diameter of 0.5-2mm by using a granulator to obtain the product profile control agent.
Preferably, the p-styrenesulfonic acid, allylpentafluorobenzene, dimethyldiallylammonium chloride are used in an amount of 0.05 to 0.1 molar part, 0.2 to 0.4 molar part, 0.1 to 0.2 molar part, respectively, based on 1 molar part of acrylamide.
Preferably, in the step (2), the weight ratio of the natural latex, OP-10, K12, diammonium phosphate, deionized water and acrylamide is 0.2-0.3:0.05-0.1:0.05-0.1:0.02-0.05:8-10:1.
preferably, in the step (3), the initiator is one of potassium persulfate, sodium persulfate and ammonium persulfate, and the weight ratio of the initiator to the acrylamide is 0.02-0.04:1.
preferably, in the step (3), the reducing agent is sodium formaldehyde sulfoxylate, and the weight ratio of the reducing agent to the acrylamide is 0.01-0.02:1.
the reaction equation for synthesizing the self-adjusting flooding agent is as follows:
Figure SMS_2
Figure SMS_3
the self-regulating and flooding agent is a quaternary high polymer taking acrylamide, p-styrenesulfonic acid, allylpentafluorobenzene and dimethyldiallylammonium chloride as monomers, has the functions of fracturing, water shutoff, profile control and resistance reduction, and can improve the oil displacement effect. Wherein, acrylamide is a polymer main body; the styrene sulfonic acid is hydrophilic anions, so that the oil-water interfacial tension can be reduced during oil displacement, the viscosity of crude oil can be reduced, the oil displacement effect can be improved, and the shearing resistance of the whole molecule can be enhanced through a benzene ring structure; the allylpentafluorobenzene is a fluorine-containing lipophilic surfactant, so that the surface tension and interfacial tension can be greatly reduced, the oil displacement effect is improved, the structure of the pentafluorobenzene ring greatly improves the shearing resistance of molecules, the viscosity of the polymer is kept not to be reduced in the stratum migration process, and meanwhile, the lipophilic characteristic can enable the polymer to be better combined with natural latex; on one hand, the dimethyl diallyl ammonium chloride is used as a cross-linking agent, so that the whole molecule is changed into a two-dimensional and three-dimensional network structure from a one-dimensional linear structure, the molecular weight is greatly increased, the swept volume is increased during oil displacement, and meanwhile, the structure of the dimethyl diallyl ammonium chloride belongs to a hydrophilic surfactant and has a certain oil displacement effect; the natural latex has the characteristics of high elasticity and good film forming property, and the adding proportion of the natural latex can be adjusted to control the molecular elasticity in the synthesis process. OP-10 and K12 can improve the polymerization quality and uniformity and increase the molecular weight of the polymer, and can strengthen the oil displacement effect because of being a surfactant.
Compared with the prior art, the invention has the following advantages and beneficial effects:
(1) The profile control agent has the characteristic of high apparent viscosity, and the apparent viscosity of 0.2 weight percent concentration reaches more than 110 mPa.s.
(2) The profile control agent has good drag reduction effect, and the drag reduction rate of 0.2wt% concentration can reach more than 65%.
(3) The high-permeability core has higher plugging strength, and the breakthrough pressure gradient of the high-permeability core reaches more than 110MPa/m at the concentration of 0.2 wt%.
Detailed Description
The endpoints and any values of the ranges disclosed herein are not limited to the precise range or value, and are understood to encompass values approaching those ranges or values. For numerical ranges, one or more new numerical ranges may be found between the endpoints of each range, between the endpoint of each range and the individual point value, and between the individual point value, in combination with each other, and are to be considered as specifically disclosed herein.
The invention will be further illustrated with reference to specific examples.
Example 1 (1) the reactor and the pipeline were purged with nitrogen for 10min at a nitrogen introduction rate of 1200mL/min, and the nitrogen introduction rate was adjusted to 250mL/min in the post synthesis process.
(2) 2mol of acrylamide, 0.2mol of p-styrenesulfonic acid, 0.8mol of allylpentafluorobenzene, 0.2mol of dimethyldiallylammonium chloride, 28.4g of natural latex, 7.1g of OP-10, 14.2g of K12, 2.84g of diammonium hydrogen phosphate and 1420g of deionized water are sequentially added into a reaction kettle, and the mixture is stirred at a low speed for 5 minutes, the stirring speed is 270rpm, and the pH value is regulated to 7-8 by using 2mol of sodium hydroxide solution; the stirring speed was adjusted to 2000rpm and stirring was continued for 25min until all the raw materials had completely become a homogeneous emulsion.
(3) Regulating the stirring speed of the reaction kettle to 250rpm, slowly heating, stopping heating after the temperature reaches 35 ℃, and continuing stirring; adding 10wt% of an aqueous initiator solution containing 2.84g of potassium persulfate into a first upper tank, and adding 10wt% of an aqueous reducing agent solution containing 1.42g of formaldehyde sodium bisulfate into a second upper tank; slowly dripping the first overhead tank initiator into the reaction kettle for 15min, slowly dripping the second overhead tank reducer aqueous solution into the reaction kettle, controlling the dripping time of the initiator at 90min, controlling the dripping time of the reducer aqueous solution at 90min, delaying the dripping end time of the reducer aqueous solution by 15min than the ending time of the initiator, heating the reaction kettle to 78 ℃ after dripping, continuously stirring for 40min, and cooling to below 40 ℃ to obtain the product emulsion.
(4) Granulating the product emulsion into particles with the diameter of 0.5-2mm by using a granulator to obtain the product profile control agent A.
Example 2 (1) the reactor and the pipeline were purged with nitrogen for 15min at a nitrogen introduction rate of 1000mL/min, and the post synthesis procedure was adjusted to a nitrogen introduction rate of 200mL/min.
(2) 2mol of acrylamide, 0.19mol of p-styrenesulfonic acid, 0.75mol of allylpentafluorobenzene, 0.25mol of dimethyldiallylammonium chloride, 30.6g of natural latex, 8.3g of OP-10, 13.2g of K12, 7.1g of diammonium hydrogen phosphate and 1136g of deionized water are sequentially added into the reaction kettle, and the mixture is stirred at a low speed for 10 minutes, the stirring speed is 260rpm, and the pH value is regulated to 7-8 by using 2mol of sodium hydroxide solution; the stirring speed was adjusted to 2200rpm and stirring was continued for 27min until all the raw materials had completely formed a uniform emulsion.
(3) The stirring speed of the reaction kettle is regulated down to 300rpm, the temperature is slowly raised, and after the temperature reaches 38 ℃, the temperature is stopped to be raised, and stirring is continued. Adding 10wt% of an aqueous initiator solution containing 2.98g of potassium persulfate into a first upper tank, and adding 10wt% of an aqueous reducing agent solution containing 1.51g of formaldehyde sodium bisulfate into a second upper tank; slowly dripping the first overhead tank initiator into the reaction kettle for 15min, slowly dripping the second overhead tank reducer aqueous solution into the reaction kettle, controlling the dripping time of the initiator to be 60min, controlling the dripping time of the reducer aqueous solution to be 60min, delaying the dripping end time of the reducer aqueous solution by 15min than the ending time of the initiator, heating the reaction kettle to 77 ℃ after dripping is finished, continuously stirring for 60min, and cooling to below 40 ℃ to obtain the product emulsion.
(4) Granulating the product emulsion into particles with the diameter of 0.5-2mm by using a granulator to obtain the product profile control agent B.
Example 3 (1) the reactor and the pipeline were purged with nitrogen for 12min at a nitrogen introduction rate of 1100mL/min, and the post synthesis procedure was adjusted to a nitrogen introduction rate of 220mL/min.
(2) 2mol of acrylamide, 0.18mol of p-styrenesulfonic acid, 0.7mol of allylpentafluorobenzene, 0.28mol of dimethyldiallylammonium chloride, 32.5g of natural latex, 9.4g of OP-10, 12.5g of K12, 3.34g of diammonium hydrogen phosphate and 1415g of deionized water are sequentially added into a reaction kettle, stirring is carried out for 6 minutes at a low speed, the stirring speed is 290rpm, and the pH is regulated to 7-8 by using 2mol of sodium hydroxide solution; the stirring speed was adjusted to 2000rpm and stirring was continued for 28min until all the raw materials had completely become a homogeneous emulsion.
(3) Regulating the stirring speed of the reaction kettle to 260rpm, slowly heating, stopping heating after the temperature reaches 37 ℃, and continuing stirring; adding 10wt% of an aqueous initiator solution containing 3.19g of sodium persulfate into a first upper tank, and adding 10wt% of an aqueous reducing agent solution containing 1.62g of formaldehyde sodium bisulfate into a second upper tank; slowly dripping the first overhead tank initiator into the reaction kettle for 15min, slowly dripping the second overhead tank reducer aqueous solution into the reaction kettle, controlling the dripping time of the initiator at 70min, controlling the dripping time of the reducer aqueous solution at 65min, delaying the dripping end time of the reducer aqueous solution by 10min than the ending time of the initiator, heating the reaction kettle to 75 ℃ after dripping, continuously stirring for 500min, and cooling to below 40 ℃ to obtain the product emulsion.
(4) Granulating the product emulsion into particles with the diameter of 0.5-2mm by using a granulator to obtain the product profile control agent C.
Example 4 (1) the reactor and the pipeline were purged with nitrogen for 13min at a nitrogen introduction rate of 1100mL/min, and the post synthesis procedure was adjusted to a nitrogen introduction rate of 230mL/min.
(2) 2mol of acrylamide, 0.17mol of p-styrenesulfonic acid, 0.65mol of allylpentafluorobenzene, 0.3mol of dimethyldiallylammonium chloride, 34.7g of natural latex, 10.2g of OP-10, 11.7g of K12, 6.17g of diammonium hydrogen phosphate and 1275g of deionized water are sequentially added into a reaction kettle, and the mixture is stirred at a low speed for 8 minutes, the stirring speed is 270rpm, and the pH value is regulated to 7-8 by using 2mol of sodium hydroxide solution; the stirring speed was adjusted to 2200rpm and stirring was continued for 22min until all the raw materials had completely formed a uniform emulsion.
(3) Regulating the stirring speed of the reaction kettle to 270rpm, slowly heating, stopping heating after the temperature reaches 36 ℃, and continuing stirring; adding 10wt% of an aqueous initiator solution containing 3.47g of sodium persulfate into a first upper tank, and adding 10wt% of an aqueous reducing agent solution containing 1.75g of formaldehyde sodium bisulfate into a second upper tank; slowly dripping the first overhead tank initiator into the reaction kettle for 15min, slowly dripping the second overhead tank reducer aqueous solution into the reaction kettle, controlling the dripping time of the initiator to be 80min, controlling the dripping time of the reducer aqueous solution to be 85min, delaying the dripping end time of the reducer aqueous solution by 20min than the ending time of the initiator, heating the reaction kettle to 76 ℃ after dripping is finished, continuously stirring for 50min, and cooling to below 40 ℃ to obtain the product emulsion.
(4) Granulating the product emulsion into particles with the diameter of 0.5-2mm by using a granulator to obtain the product profile control agent D.
Example 5 (1) the reactor and the pipeline were purged with nitrogen for 12min at a nitrogen introduction rate of 1200mL/min, and the post synthesis procedure was adjusted to a nitrogen introduction rate of 210mL/min.
(2) 2mol of acrylamide, 0.15mol of p-styrenesulfonic acid, 0.6mol of allylpentafluorobenzene, 0.33mol of dimethyldiallylammonium chloride, 36.6g of natural latex, 11.7g of OP-10, 10.8g of K12, 4.86g of diammonium hydrogen phosphate and 1333g of deionized water are sequentially added into a reaction kettle, and the mixture is stirred at a low speed for 7 minutes, the stirring speed is 280rpm, and the pH value is regulated to 7-8 by using 2mol of sodium hydroxide solution; the stirring speed was adjusted to 2100rpm and stirring was continued for 25min until all the raw materials had completely become a homogeneous emulsion.
(3) The stirring speed of the reaction kettle is reduced to 280rpm, the temperature is slowly increased, and after the temperature reaches 35 ℃, the temperature is stopped to be increased, and stirring is continued. Adding 10wt% of an aqueous initiator solution containing 4.25g of ammonium persulfate into a first upper tank, and adding 10wt% of an aqueous reducing agent solution containing 2.18g of sodium formaldehyde sulfoxylate into a second upper tank; slowly dripping the first overhead tank initiator into the reaction kettle for 15min, slowly dripping the second overhead tank reducer aqueous solution into the reaction kettle, controlling the dripping time of the initiator at 90min, controlling the dripping time of the reducer aqueous solution at 85min, delaying the dripping end time of the reducer aqueous solution by 10min than the ending time of the initiator, heating the reaction kettle to 72 ℃ after dripping, continuously stirring for 45min, and cooling to below 40 ℃ to obtain the product emulsion.
(4) Granulating the product emulsion into particles with the diameter of 0.5-2mm by using a granulator to obtain the product profile control agent E.
Example 6 (1) the reactor and the pipeline were purged with nitrogen for 10 minutes at a nitrogen introduction rate of 1000mL/min, and the post synthesis procedure was adjusted to a nitrogen introduction rate of 240mL/min.
(2) 2mol of acrylamide, 0.13mol of p-styrenesulfonic acid, 0.55mol of allylpentafluorobenzene, 0.35mol of dimethyldiallylammonium chloride, 38.1g of natural latex, 12.6g of OP-10, 9.6g of K12, 5.12g of diammonium hydrogen phosphate and 1380g of deionized water are sequentially added into a reaction kettle, and the mixture is stirred at a low speed for 8 minutes, the stirring speed is 260rpm, and the pH value is regulated to 7-8 by using 2mol of sodium hydroxide solution; the stirring speed was adjusted to 2050rpm and stirring was continued for 25min until all the raw materials had completely become a homogeneous emulsion.
(3) The stirring speed of the reaction kettle is regulated down to 290rpm, the temperature is slowly raised, and after the temperature reaches 35 ℃, the temperature is stopped to be raised, and stirring is continued. Adding 10wt% of an aqueous initiator solution containing 3.47g of sodium persulfate into a first upper tank, and adding 10wt% of an aqueous reducing agent solution containing 1.75g of formaldehyde sodium bisulfate into a second upper tank; slowly dripping the first overhead tank initiator into the reaction kettle for 15min, slowly dripping the second overhead tank reducer aqueous solution into the reaction kettle, controlling the dripping time of the initiator at 70min, controlling the dripping time of the reducer aqueous solution at 70min, delaying the dripping end time of the reducer aqueous solution by 15min compared with the ending time of the initiator, heating the reaction kettle to 75 ℃ after dripping, continuously stirring for 52min, and cooling to below 40 ℃ to obtain the product emulsion.
(4) Granulating the product emulsion into particles with the diameter of 0.5-2mm by using a granulator to obtain the product profile control agent F.
Example 7 (1) the reactor and the pipeline were purged with nitrogen for 15min at a nitrogen introduction rate of 1100mL/min, and the post synthesis procedure was adjusted to a nitrogen introduction rate of 210mL/min.
(2) 2mol of acrylamide, 0.11mol of p-styrenesulfonic acid, 0.5mol of allylpentafluorobenzene, 0.38mol of dimethyldiallylammonium chloride, 41.4g of natural latex, 13.3g of OP-10, 8.4g of K12, 5.66g of diammonium hydrogen phosphate and 1395g of deionized water are sequentially added into a reaction kettle, and the mixture is stirred at a low speed for 5 minutes, the stirring speed is 300rpm, and the pH value is regulated to 7-8 by using 2mol of sodium hydroxide solution; the stirring speed was adjusted to 2150rpm and stirring was continued for 20min until all the raw materials had completely formed a homogeneous emulsion.
(3) Regulating the stirring speed of the reaction kettle to 270rpm, slowly heating, stopping heating after the temperature reaches 40 ℃, and continuing stirring; adding 10wt% of an aqueous initiator solution containing 5.17g of ammonium persulfate into a first upper tank, and adding 10wt% of an aqueous reducing agent solution containing 2.59g of sodium formaldehyde sulfoxylate into a second upper tank; slowly dripping the first overhead tank initiator into the reaction kettle for 15min, slowly dripping the second overhead tank reducer aqueous solution into the reaction kettle, controlling the dripping time of the initiator to be 60min, controlling the dripping time of the reducer aqueous solution to be 65min, delaying the dripping end time of the reducer aqueous solution by 20min than the ending time of the initiator, heating the reaction kettle to 70 ℃ after dripping, continuously stirring for 55min, and cooling to below 40 ℃ to obtain the product emulsion.
(4) Granulating the product emulsion into particles with the diameter of 0.5-2mm by using a granulator to obtain the product profile control agent G.
Example 8 (1) the reactor and the pipeline were purged with nitrogen for 12min at a nitrogen introduction rate of 1200mL/min, and the post synthesis procedure was adjusted to a nitrogen introduction rate of 230mL/min.
(2) 2mol of acrylamide, 0.1mol of p-styrenesulfonic acid, 0.4mol of allylpentafluorobenzene, 0.4mol of dimethyldiallylammonium chloride, 42.6g of natural latex, 14.2g of OP-10, 7.1g of K12, 6.45g of diammonium hydrogen phosphate and 1414g of deionized water are sequentially added into a reaction kettle, and the mixture is stirred at a low speed for 10 minutes, the stirring speed is 250rpm, and the pH value is regulated to 7-8 by using 2mol of sodium hydroxide solution; the stirring speed was adjusted to 2100rpm and stirring was continued for 30min until all the raw materials had completely become a homogeneous emulsion.
(3) Regulating the stirring speed of the reaction kettle to 260rpm, slowly heating, stopping heating after the temperature reaches 40 ℃, and continuing stirring; adding 10wt% of an aqueous initiator solution containing 5.68g of ammonium persulfate into a first upper tank, and adding 10wt% of an aqueous reducing agent solution containing 2.84g of sodium formaldehyde sulfoxylate into a second upper tank; slowly dripping the first overhead tank initiator into the reaction kettle for 15min, slowly dripping the second overhead tank reducer aqueous solution into the reaction kettle, controlling the dripping time of the initiator at 90min, controlling the dripping time of the reducer aqueous solution at 85min, delaying the dripping ending time of the reducer aqueous solution by 10min than the ending time of the initiator, heating the reaction kettle to 80 ℃ after dripping is finished, continuously stirring for 47min, and cooling to below 40 ℃ to obtain the product emulsion.
(4) Granulating the product emulsion into particles with the diameter of 0.5-2mm by using a granulator to obtain the product profile control agent H.
Example 9 apparent viscosity test
The polymer drag reducer (comparative sample) of the present invention and the Puyang sea source chemical industry Co., ltd was prepared to a concentration of 0.2wt% with 10000mg/L sodium chloride solution, and apparent viscosity was measured by referring to the method of 7.1 in SY/T6376-2008 general technical Condition for fracturing fluids, and the measurement results are shown in Table 1.
As can be seen from table 1: the profile control agent A, B, C, D, E, F, G, H of the present invention has an apparent viscosity of greater than 110mpa.s at a concentration of 0.2wt%, wherein G is up to 1599mpa.s; the apparent viscosity of the comparative sample is larger than 92mPa.s, which is obviously lower than that of the invention, and the profile control agent of the invention has good apparent viscosity.
Example 10 drag reduction rate test
The drag reduction ratio of the polymer drag reducer (comparative sample) of the present invention and the Puyang sea source chemical industry Co., ltd was tested by using 10000mg/L sodium chloride solution to prepare 0.1wt% and 0.2wt% concentration, referring to the method of 7.13 in SY/T6376-2008 general technical Condition for fracturing fluids, and the test results are shown in Table 1.
TABLE 1 apparent viscosity, drag reduction test results
Figure SMS_4
As can be seen from table 1: (1) The drag reduction rate of the profile control agent A, B, C, D, E, F, G, H is more than 50% and reaches 60% at most when the concentration is 0.1 wt%; the drag reduction rate of the comparison sample is 40%, which is obviously lower than that of the invention; (2) The drag reduction rate of the profile control agent A, B, C, D, E, F, G, H is more than 65% and reaches 80% at most when the concentration is 0.2 wt%; the drag reduction rate of the comparative sample is 53%, which is significantly lower than that of the present invention. The profile control agent has good resistance reducing capability.
Example 11 test of blocking Strength
The polymer drag reducer (comparative sample) of the present invention and the Puyang sea source chemical industry limited company is prepared into 0.2wt% concentration with 10000mg/L sodium chloride solution, artificial seal cores with different permeabilities are adopted at 90 ℃, wherein the length of the low permeability core is 6.6cm, the length of the high permeability core is 6.7cm, and 1PV solution is extruded, and the seal strength, breakthrough pressure and breakthrough pressure gradient test results of the present invention are shown in Table 2.
Table 2 results of breakthrough pressure and breakthrough pressure gradient tests for different cores
Figure SMS_5
As can be seen from table 2:
(1) For hypotonic cores (0.048, mum 2 ) The breakthrough pressure of the profile control agent A, B, C, D, E, F, G, H is more than 10MPa, the highest breakthrough pressure reaches 11.6MPa, and the breakthrough pressure of a comparison sample is 7.2MPa; the breakthrough pressure gradient of the profile control agent A, B, C, D, E, F, G, H is more than 150MPa/m and is up to 175.8MPa/m, and the breakthrough pressure gradient of a comparison sample is 109.1MPa/m and is obviously lower than that of the profile control agent A, B, C, D, E, F, G, H;
(2) For hypertonic cores (0.278, mum 2 ) The breakthrough pressure of the profile control agent A, B, C, D, E, F, G, H is more than 7MPa and reaches 9.0MPa at the highest, and the breakthrough pressure of a comparison sample is 5.8MPa; the breakthrough pressure gradient of the profile control agent A, B, C, D, E, F, G, H is more than 115MPa/m and is up to 134.3MPa/m, and the breakthrough pressure gradient of a comparison sample is 86.6MPa/m, which is obviously lower than that of the profile control agent A, B, C, D, E, F, G, H.
The profile control agent has good blocking strength.
The preferred embodiments of the present invention have been described in detail above, but the present invention is not limited thereto. Within the scope of the technical idea of the invention, a number of simple variants of the technical solution of the invention are possible, including combinations of the individual technical features in any other suitable way, which simple variants and combinations should likewise be regarded as being disclosed by the invention, all falling within the scope of protection of the invention.

Claims (7)

1. The preparation method of the viscoelastic self-regulating and flooding agent for the polyacrylamide fracturing is characterized by comprising the following specific steps of:
(1) Purging the reaction kettle and the pipeline with nitrogen for 10-15min, wherein the nitrogen introducing speed is 1000-1200mL/min during purging, and the nitrogen introducing speed is adjusted to be 200-250mL/min in the later synthesis process;
(2) Sequentially adding acrylamide, p-styrenesulfonic acid, allylpentafluorobenzene, dimethyl diallyl ammonium chloride, natural latex, dodecylphenol polyoxyethylene ether, sodium dodecyl sulfate, diammonium hydrogen phosphate and deionized water into a reaction kettle, stirring at a low speed of 250-300rpm for 5-10min, and regulating pH to 7-8 with 2mol of sodium hydroxide solution; regulating stirring speed to 2000-2200rpm, and continuing stirring for 20-30min until all the raw materials completely become uniform emulsion;
(3) The stirring speed of the reaction kettle is reduced to 250-300rpm, the temperature is slowly raised, and after the temperature reaches 35-40 ℃, the temperature is stopped to be raised, and stirring is continued; adding 10wt% of aqueous solution of an initiator into a first elevated tank, adding 10wt% of aqueous solution of a reducing agent into a second elevated tank, slowly dripping the initiator of the first elevated tank into a reaction kettle, dripping the aqueous solution of the reducing agent into the reaction kettle after 15min, controlling the dripping time of the initiator to be 60-90min, controlling the dripping time of the aqueous solution of the reducing agent to be 60-90min, delaying the dripping ending time of the aqueous solution of the reducing agent by 10-20min than the ending time of the initiator, heating the reaction kettle to 70-80 ℃ after dripping, continuously stirring for 40-60min, and cooling to below 40 ℃ to obtain a product emulsion;
(4) Granulating the product emulsion into particles with the diameter of 0.5-2mm by using a granulator to obtain the product profile control agent.
2. The method for preparing the viscoelastic self-regulating and flooding agent for the polyacrylamide fracturing according to claim 1, wherein the dosage of the p-styrenesulfonic acid, the allylpentafluorobenzene and the dimethyldiallylammonium chloride is 0.05-0.1 part by mole, 0.2-0.4 part by mole and 0.1-0.2 part by mole respectively based on 1 part by mole of acrylamide.
3. The preparation method of the viscoelastic self-regulating and flooding agent for the polyacrylamide fracturing according to claim 1, wherein in the step (2), the weight ratio of the natural latex, the dodecylphenol polyoxyethylene ether, the sodium dodecyl sulfate, the diammonium hydrogen phosphate, the deionized water and the acrylamide is 0.2-0.3:0.05-0.1:0.05-0.1:0.02-0.05:8-10:1.
4. the preparation method of the viscoelastic self-regulating and flooding agent for the polyacrylamide fracturing is characterized in that in the step (3), the initiator is one of potassium persulfate, sodium persulfate and ammonium persulfate, and the weight ratio of the initiator to the acrylamide is 0.02-0.04:1.
5. the preparation method of the viscoelastic self-regulating and flooding agent for the polyacrylamide fracturing is characterized in that in the step (3), the reducing agent is sodium formaldehyde sulfoxylate, and the weight ratio of the reducing agent to the acrylamide is 0.01-0.02:1.
6. the viscoelastic self-regulating and flooding agent for the polyacrylamide fracturing is characterized by comprising the following molecular structural formula:
Figure QLYQS_1
wherein:
a=2000-40000;
b=20000-200000;
c=1000-20000;
d=4000-80000;
e=20000-200000;
f=1000-20000;
g=4000-80000。
7. the viscoelastic self-regulating and flooding agent for polyacrylamide fracturing according to claim 6, wherein the self-regulating and flooding agent has a viscosity-average molecular weight of: 10000000-40000000.
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