CN115850678B - Small molecular polysilicone pore throat dredging agent for fracturing and preparation method thereof - Google Patents
Small molecular polysilicone pore throat dredging agent for fracturing and preparation method thereof Download PDFInfo
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Abstract
The invention belongs to the technical field of petroleum exploitation, and particularly relates to a small molecular polysilicone pore throat dredging agent for fracturing and a preparation method thereof. The preparation method comprises the following steps: adding 1, 3-tetramethyl-1, 3-diphenyl disilazane and potassium hydroxide solid into a high-pressure reaction kettle, adding propylene oxide, stirring at a speed of 400-500rpm, heating to 140-145 ℃, and cooling the system by using circulating cooling water after reaction to obtain an intermediate; and (3) introducing ethylene oxide into the intermediate, stirring at a speed of 130-135 ℃, cooling to room temperature after the reaction, and regulating the pH value to obtain the product, namely the small molecular polysilicone pore throat dredging agent for fracturing. The small molecular polysilicone pore throat dredging agent for fracturing has wide raw material sources, simple synthesis and preparation processes, the synthesis method is a one-pot method, no byproducts are generated, and the yield is 100%.
Description
Technical Field
The invention belongs to the technical field of petroleum exploitation, and particularly relates to a small molecular polysilicone pore throat dredging agent for fracturing and a preparation method thereof.
Background
Most of domestic oil fields enter the middle and later stages of water injection development, injected water is easy to break through along a high permeable layer due to the heterogeneity of oil reservoirs, so that the permeability of the high permeable layer is further improved, a large amount of water is discharged from the oil wells, and the productivity is reduced. 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, and adjust the water absorption profile of the well, namely, perform fracturing operation. Cracks are formed in the stratum, and the diversion capacity of the hydrocarbon reservoir is improved, so that the aim of increasing yield is fulfilled.
After the fracturing operation is completed, corresponding joints are formed, the joints are not restored again, in this case, the flow conductivity of the target layer is continuously enhanced, and meanwhile, the permeation effect of the oil and gas field is continuously improved. However, the flowback of the fracturing fluid is difficult, and if no corresponding measures are taken, new damage and pollution can be caused to the stratum, so that the early construction fails.
Cleanup additives are generally added into industrial liquid in the later stage of fracturing, so that capillary resistance is reduced, and stratum blockage is cleared. However, the cleanup additive has limited effect on flowback of the fracturing fluid, so that the fracturing fluid of the low-permeability reservoir small pore throat cannot be cleaned, and the flowback fluid can cause certain pollution to the environment.
Disclosure of Invention
The invention provides a small molecular polysilicone pore throat dredging agent for fracturing and a preparation method thereof aiming at the defects of the prior art. The pore-throat dredging agent has the characteristics of wide raw material sources, simple preparation process, no byproducts, low surface interfacial tension and adjustable cloud point.
The invention discloses a small molecular polysilicone pore throat dredger for fracturing, which has the following molecular structural formula:
wherein: m=2-20;
n=5-100。
the molecular weight of the small molecular polysilicone pore throat dredger for fracturing is 1000-3000.
The invention further discloses a synthesis method of the small molecular polysilicone pore throat dredger for fracturing, which comprises the following specific steps:
(1) Adding 1, 3-tetramethyl-1, 3-diphenyl disilazane and potassium hydroxide solid into a high-pressure reaction kettle, purging a pipeline and the reaction kettle for 2-3min by nitrogen, vacuumizing, purging the pipeline and the reaction kettle for 2-3min by nitrogen again, vacuumizing again, slowly heating to 85-90 ℃ while stirring at a speed of 200-300rpm, stopping vacuumizing, adding propylene oxide at one time, increasing the stirring speed to 400-500rpm, heating to 140-145 ℃, and cooling the system to 85-90 ℃ by circulating cooling water after reaction to obtain an intermediate;
(2) Continuously stirring the intermediate at 80-90 ℃, simultaneously reducing the stirring speed to 200-300rpm, introducing ethylene oxide at the speed of 1.5-2ml/min, after the introduction, increasing the stirring speed to 400-500rpm, heating to 130-135 ℃, cooling the system to room temperature by adopting circulating cooling water after the reaction, and adding 1mol/L hydrochloric acid to adjust the pH value to 6-7 to obtain the small molecular polysilicone pore throat dredge agent for fracturing.
Preferably, the propylene oxide and the ethylene oxide are used in an amount of 2 to 20 mole parts and 5 to 100 mole parts, respectively, based on 1 mole part of 1, 3-tetramethyl-1, 3-diphenyldisilazane; more preferably, the propylene oxide and ethylene oxide are used in an amount of 5 to 20 mole parts and 20 to 100 mole parts, respectively, based on 1 mole part of 1, 3-tetramethyl-1, 3-diphenyldisilazane.
Preferably, the weight ratio of potassium hydroxide to 1, 3-tetramethyl-1, 3-diphenyldisilazane in step (1) is 0.1-0.3:1.
preferably, the reaction time in step (1) is from 4 to 8 hours; more preferably, the reaction time is 4 to 6 hours.
Preferably, the reaction time in step (2) is 1-2h.
The synthesis reaction equation of the small molecular polysilicone pore throat dredger for fracturing is as follows:
the invention relates to a small molecular polysilicone pore throat dredge agent for fracturing, which belongs to a low molecular surfactant, wherein the cationic property of tertiary amine in molecules is weaker, the whole molecule basically presents nonionic property, the lipophilic comprises benzene ring, silane group and polypropylene ether, and the hydrophilic group is polyvinyl ether. The solubility of the invention is reduced along with the rise of temperature, so emulsion is easy to form in the high-temperature environment of the stratum, the hypertonic oil reservoir can be regulated and controlled, the permeability of the water phase is reduced, and the fracturing effect is improved to a certain extent. The cloud point of the molecules can be regulated by regulating the quantity of propylene oxide and ethylene oxide in the synthesis process, and the fracturing effect is optimized according to the characteristics of different oil reservoirs.
After the pore throat dredging agent is injected into a stratum, the aqueous solution automatically becomes emulsion with the rise of temperature, and the viscosity rises rapidly. The method has the beneficial effects on the following three aspects of oil reservoir development: (1) reducing the oil-water interfacial tension; (2) increasing the water drive wave and volume; (3) decreasing the permeability of the aqueous phase. When water flooding operation is carried out on the oil reservoir in the later period, the pore-throat dredger is automatically converted into an aqueous solution along with the reduction of temperature, and can be automatically discharged from the pore throat of a low-permeability area of the oil reservoir under a lower driving force, so that the effect of dredging the pore throat of the oil reservoir is achieved.
Compared with the prior art, the invention has the following advantages and beneficial effects:
(1) The micromolecular polysilicone pore throat dredging agent for fracturing has wide raw material sources, simple synthesis and preparation processes, the synthesis method is a one-pot method, no byproducts are generated, and the yield is 100 percent
(2) The small molecular polysilicone pore throat dredging agent for fracturing has the characteristics of low surface tension and interfacial tension, the concentration surface tension of 0.5wt% is less than 25mN/m, and the interfacial tension is less than 0.02 mN/m;
(3) The invention can adjust parameters to control the cloud point in the synthesis process according to the requirement, and the cloud point range of 0.5wt% solution is 67-84 ℃.
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.
Example one (1) 0.5mol of 1, 3-tetramethyl-1, 3-diphenyl disilazane and 14.3g of potassium hydroxide solid are added into a high-pressure reaction kettle, a nitrogen purging pipeline and the reaction kettle are used for 2min, vacuum pumping is carried out, the nitrogen purging pipeline and the reaction kettle are used for 2min again, vacuum pumping is carried out again, then the temperature is slowly heated to 85 ℃, meanwhile, stirring is carried out at a speed of 200rpm, vacuum pumping is stopped, 1mol of propylene oxide is added at one time, the stirring speed is increased to 400rpm, the temperature is increased to 140 ℃, and after reaction for 4h, the system is cooled to 90 ℃ by using circulating cooling water, so as to obtain an intermediate;
(2) Continuously stirring the intermediate at 80 ℃ while reducing the stirring speed to 200rpm, introducing 2.5mol of ethylene oxide at the speed of 2ml/min, after the introduction, increasing the stirring speed to 400rpm, heating to 130 ℃, reacting for 1h, cooling the system to room temperature by adopting circulating cooling water, adding 1mol/L of hydrochloric acid, and regulating the pH to 6 to obtain a product J 1 。
Example two (1) adding 0.5mol of 1, 3-tetramethyl-1, 3-diphenyl disilazane and 42.8g of potassium hydroxide solid into a high-pressure reaction kettle, purging a pipeline and the reaction kettle with nitrogen for 2min, vacuumizing, purging the pipeline and the reaction kettle with nitrogen again for 3min, vacuumizing again, then slowly heating to 90 ℃ while stirring at the speed of 250rpm, stopping vacuumizing, adding 10mol of propylene oxide at one time, increasing the stirring speed to 500rpm, heating to 145 ℃, and cooling the system to 89 ℃ with circulating cooling water after reacting for 8h to obtain an intermediate;
(2) Continuously stirring the intermediate at 85 ℃ while reducing the stirring speed to 270rpm, introducing 5mol of ethylene oxide at a speed of 1.5ml/min, after the introduction, increasing the stirring speed to 430rpm, heating to 132 ℃, reacting for 1.2h, cooling the system to room temperature by adopting circulating cooling water, adding 1mol/L of hydrochloric acid, and regulating the pH to 6 to obtain a product J 2 。
Example III (1) 0.5mol of 1, 3-tetramethyl-1, 3-diphenyl disilazane and 18.2g of potassium hydroxide solid are added into a high-pressure reaction kettle, a nitrogen purging pipeline and the reaction kettle are used for 3min, vacuum pumping is carried out again, the nitrogen purging pipeline and the reaction kettle are used for 3min, vacuum pumping is carried out again, then the temperature is slowly heated to 86 ℃ while stirring is carried out at a speed of 220rpm, vacuum pumping is stopped, 2.5mol of propylene oxide is added at one time, the stirring speed is increased to 450rpm, the temperature is increased to 142 ℃, and after the reaction is carried out for 6h, the system is cooled to 85 ℃ by using circulating cooling water, so as to obtain an intermediate;
(2) Continuously stirring the intermediate at 90 ℃ while reducing the stirring speed to 280rpm, introducing 20mol of ethylene oxide at a speed of 2ml/min, after the introduction, increasing the stirring speed to 470rpm, heating to 135 ℃, reacting for 1.4h, cooling the system to room temperature by adopting circulating cooling water, adding 1mol/L of hydrochloric acid, and regulating the pH to 6 to obtain a product J 3 。
Example four (1) 0.5mol of 1, 3-tetramethyl-1, 3-diphenyl disilazane and 38.8g of potassium hydroxide solid are added into a high-pressure reaction kettle, a nitrogen purging pipeline and the reaction kettle are used for 2min, vacuum pumping is carried out, the nitrogen purging pipeline and the reaction kettle are used for 3min again, vacuum pumping is carried out again, then the temperature is slowly heated to 87 ℃ while stirring is carried out at a speed of 260rpm, vacuum pumping is stopped, 8mol of propylene oxide is added at one time, the stirring speed is increased to 420rpm, the temperature is increased to 143 ℃, and after reaction is carried out for 4h, the system is cooled to 87 ℃ by circulating cooling water, so as to obtain an intermediate;
(2) Continuously stirring the intermediate at 88 ℃ while reducing the stirring speed to 260rpm, introducing 30mol of ethylene oxide at a speed of 1.6ml/min, after the introduction, increasing the stirring speed to 480rpm, heating to 133 ℃, reacting for 1.5h, cooling the system to room temperature by adopting circulating cooling water, adding 1mol/L of hydrochloric acid, and regulating the pH to 6 to obtain a product J 4 。
Example five (1) 0.5mol of 1, 3-tetramethyl-1, 3-diphenyl disilazane and 21.4g of potassium hydroxide solid are added into a high-pressure reaction kettle, a nitrogen purging pipeline and the reaction kettle are used for 3min, vacuum pumping is carried out, the nitrogen purging pipeline and the reaction kettle are used for 2min again, the vacuum pumping is carried out again, then the temperature is slowly heated to 88 ℃ while stirring is carried out at a speed of 280rpm, the vacuum pumping is stopped, 3mol of propylene oxide is added at one time, the stirring speed is increased to 460rpm, the temperature is increased to 145 ℃, and after the reaction is carried out for 5h, the system is cooled to 88 ℃ by using circulating cooling water, so as to obtain an intermediate;
(2) Continuously stirring the intermediate at 86 ℃ while reducing the stirring speed to 220rpm, introducing 40mol of ethylene oxide at a speed of 1.5ml/min, after the introduction, increasing the stirring speed to 420rpm, heating to 134 ℃, reacting for 1.8h, cooling the system to room temperature by adopting circulating cooling water, adding 1mol/L of hydrochloric acid, and regulating the pH to 7 to obtain a product J 5 。
Example six (1) 0.5mol of 1, 3-tetramethyl-1, 3-diphenyl disilazane and 28.8g of potassium hydroxide solid are added into a high-pressure reaction kettle, a nitrogen purging pipeline and the reaction kettle are used for 2min, vacuum pumping is carried out, the nitrogen purging pipeline and the reaction kettle are used for 2min again, vacuum pumping is carried out again, then the temperature is slowly heated to 90 ℃ while stirring at the speed of 300rpm, vacuum pumping is stopped, 6.5mol of propylene oxide is added at one time, the stirring speed is increased to 480rpm, the temperature is increased to 144 ℃, and after the reaction is carried out for 6.4h, the system is cooled to 86 ℃ by using circulating cooling water, so as to obtain an intermediate;
(2) Continuously stirring the intermediate at 83 ℃ while reducing the stirring speed to 300rpm, introducing 40mol of ethylene oxide at a speed of 1.8ml/min, after the introduction, increasing the stirring speed to 450rpm, heating to 135 ℃, reacting for 1.8h, cooling the system to room temperature by adopting circulating cooling water, adding 1mol/L of hydrochloric acid, and regulating the pH to 7 to obtain a product J 6 。
In the seventh embodiment (1), 0.5mol of 1, 3-tetramethyl-1, 3-diphenyl disilazane and 34.5g of potassium hydroxide solid are added into a high-pressure reaction kettle, a nitrogen purging pipeline and the reaction kettle are used for 3min, vacuum pumping is performed again, the nitrogen purging pipeline and the reaction kettle are used for 3min, vacuum pumping is performed again, then the temperature is slowly heated to 85 ℃, meanwhile, stirring is performed at the speed of 250rpm, vacuum pumping is stopped, 4mol of propylene oxide is added at one time, the stirring speed is increased to 430rpm, the temperature is increased to 140 ℃, and after the reaction is performed for 6.5h, the system is cooled to 85 ℃ by using circulating cooling water, so as to obtain an intermediate;
(2) Stirring the intermediate at 85deg.C while reducing stirring speed to 250rpm, introducing 45mol of ethylene oxide at a rate of 1.6ml/minAfter that, the stirring speed is increased to 500rpm, the temperature is increased to 130 ℃, after 2 hours of reaction, the system is cooled to room temperature by adopting circulating cooling water, and 1mol/L hydrochloric acid is added to adjust the pH value to 7, thus obtaining the product J 7 。
Example eight (1) 0.5mol of 1, 3-tetramethyl-1, 3-diphenyl disilazane and 36.6g of potassium hydroxide solid are added into a high-pressure reaction kettle, a nitrogen purging pipeline and the reaction kettle are used for 2min, vacuum pumping is carried out, the nitrogen purging pipeline and the reaction kettle are used for 2min again, vacuum pumping is carried out again, then the temperature is slowly heated to 87 ℃ while stirring is carried out at a speed of 260rpm, vacuum pumping is stopped, 4mol of propylene oxide is added at one time, the stirring speed is increased to 450rpm, the temperature is increased to 145 ℃, and after 7h of reaction, the system is cooled to 90 ℃ by using circulating cooling water, so as to obtain an intermediate;
(2) Continuously stirring the intermediate at 81 ℃, simultaneously reducing the stirring speed to 200rpm, introducing 50mol of ethylene oxide at a speed of 2.8ml/min, after the introduction, increasing the stirring speed to 400rpm, heating to 132 ℃, reacting for 2 hours, cooling the system to room temperature by adopting circulating cooling water, adding 1mol/L of hydrochloric acid, and regulating the pH to 6 to obtain a product J 8 。
Example 9 testing of surface tension and interfacial tension
The small molecular polysilicone pore throat dredge agent of the invention is prepared into 0.5% solution, and the surface tension and the interfacial tension are measured according to the method in SY/T5370-2018 surface and interfacial tension measuring method, and the result is shown in Table 1.
As can be seen from table 1: small molecular polysilicone pore throat dredging agent J for fracturing 1 -J 8 The surface tension test values are all less than 25mN/m, wherein J 8 A minimum value of 23.8mN/m; interfacial tension is less than 0.02mN/m, J 8 Minimum 0.015mN/m. The small molecular polysilicone pore throat dredging agent for fracturing has the characteristics of low surface tension and interface tension.
Example 10 cloud Point testing
The small molecular polysilicone pore throat dredge agent of the invention is prepared into 0.5% solution by using 5% sodium chloride aqueous solution by weight, the solution is placed in a cylinder with a plug, the cylinder is placed in an oil bath for heating, and the temperature at which turbidity appears in the solution, namely the cloud point of the invention, is tested, and the result is shown in Table 1.
TABLE 1 results of surface tension, interfacial tension, contact Angle test
Cloud point analysis: the cloud point is mainly determined by the ratio of lipophilic groups to hydrophilic groups, and generally, the larger the adding amount of propylene oxide is, the smaller the adding amount of ethylene oxide is, and the lower the cloud point is. The test results approximately compound the conclusion, so the invention can adjust the synthesis parameters to meet different oil reservoir requirements.
As can be seen from table 1: 0.5wt% of small molecule polysilicone pore throat dredger J for fracturing 1 -J 8 The cloud point is between 67 and 84 ℃.
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 (9)
1. The small molecular polysilicone pore throat dredger for fracturing is characterized by comprising the following molecular structural formula:
wherein: m=2-20;
n=5-100。
2. the small molecular polysilicone pore throat dredger for fracturing according to claim 1, wherein the molecular weight of the small molecular polysilicone pore throat dredger for fracturing is 1000-3000.
3. The preparation method of the small molecule polysilicone pore throat dredger for fracturing according to claim 1 or 2, which is characterized in that the preparation method comprises the following steps:
(1) Adding 1, 3-tetramethyl-1, 3-diphenyl disilazane and potassium hydroxide solid into a high-pressure reaction kettle, purging a pipeline and the reaction kettle for 2-3min by nitrogen, vacuumizing, purging the pipeline and the reaction kettle for 2-3min by nitrogen again, vacuumizing again, slowly heating to 85-90 ℃ while stirring at a speed of 200-300rpm, stopping vacuumizing, adding propylene oxide at one time, increasing the stirring speed to 400-500rpm, heating to 140-145 ℃, and cooling the system to 85-90 ℃ by circulating cooling water after reaction to obtain an intermediate;
(2) Continuously stirring the intermediate at 80-90 ℃, simultaneously reducing the stirring speed to 200-300rpm, introducing ethylene oxide at the speed of 1.5-2ml/min, after the introduction, increasing the stirring speed to 400-500rpm, heating to 130-135 ℃, cooling the system to room temperature by adopting circulating cooling water after the reaction, and adding 1mol/L hydrochloric acid to adjust the pH value to 6-7 to obtain the small molecular polysilicone pore throat dredge agent for fracturing.
4. The method for preparing a small molecular weight polysilicone pore throat dredge agent for fracturing according to claim 3, wherein the amount of propylene oxide and ethylene oxide is 2-20 mol parts and 5-100 mol parts respectively based on 1mol part of 1, 3-tetramethyl-1, 3-diphenyl disilazane.
5. The method for preparing a small molecular polysilicone pore throat dredge agent for fracturing according to claim 4, wherein the amount of propylene oxide and ethylene oxide is 5 to 20mol parts and 20 to 100 mol parts respectively based on 1mol part of 1, 3-tetramethyl-1, 3-diphenyl disilazane.
6. The method for preparing a small molecular polysilicone pore throat dredging agent for fracturing according to claim 3, wherein the weight ratio of potassium hydroxide to 1, 3-tetramethyl-1, 3-diphenyl disilazane in the step (1) is 0.1-0.3:1.
7. the method for preparing a small molecular polysilicone pore throat dredger for fracturing according to claim 3, wherein the reaction time in the step (1) is 4-8h.
8. The method for preparing a small molecular polysilicone pore throat dredger for fracturing according to claim 7, wherein the reaction time in the step (1) is 4-6h.
9. The method for preparing a small molecular polysilicone pore throat dredger for fracturing according to claim 3, wherein the reaction time in the step (2) is 1-2h.
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| CN106582809A (en) * | 2016-12-22 | 2017-04-26 | 红宝丽集团股份有限公司 | Catalyst for epoxidation of olefin and preparation method thereof |
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| CN110591679B (en) * | 2019-10-16 | 2020-09-18 | 西南石油大学 | Granular profile control agent adaptive to size of pore throat of stratum and preparation method thereof |
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| CN106582809A (en) * | 2016-12-22 | 2017-04-26 | 红宝丽集团股份有限公司 | Catalyst for epoxidation of olefin and preparation method thereof |
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