CN113308231B - Water shutoff agent, preparation method, experimental method and water shutoff method thereof - Google Patents
Water shutoff agent, preparation method, experimental method and water shutoff method thereof Download PDFInfo
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- CN113308231B CN113308231B CN202010118405.0A CN202010118405A CN113308231B CN 113308231 B CN113308231 B CN 113308231B CN 202010118405 A CN202010118405 A CN 202010118405A CN 113308231 B CN113308231 B CN 113308231B
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- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 title claims abstract description 269
- 239000003795 chemical substances by application Substances 0.000 title claims abstract description 173
- 238000002474 experimental method Methods 0.000 title claims abstract description 26
- 238000002360 preparation method Methods 0.000 title claims abstract description 24
- 238000000034 method Methods 0.000 title claims abstract description 20
- 239000000243 solution Substances 0.000 claims abstract description 87
- 239000012295 chemical reaction liquid Substances 0.000 claims abstract description 79
- 238000006243 chemical reaction Methods 0.000 claims abstract description 66
- BPQQTUXANYXVAA-UHFFFAOYSA-N Orthosilicate Chemical compound [O-][Si]([O-])([O-])[O-] BPQQTUXANYXVAA-UHFFFAOYSA-N 0.000 claims abstract description 29
- 159000000007 calcium salts Chemical class 0.000 claims abstract description 28
- 239000012744 reinforcing agent Substances 0.000 claims abstract description 19
- 230000018044 dehydration Effects 0.000 claims description 26
- 238000006297 dehydration reaction Methods 0.000 claims description 26
- 230000015784 hyperosmotic salinity response Effects 0.000 claims description 19
- 230000015572 biosynthetic process Effects 0.000 claims description 13
- 238000012360 testing method Methods 0.000 claims description 13
- UXVMQQNJUSDDNG-UHFFFAOYSA-L Calcium chloride Chemical group [Cl-].[Cl-].[Ca+2] UXVMQQNJUSDDNG-UHFFFAOYSA-L 0.000 claims description 11
- 150000003839 salts Chemical class 0.000 claims description 11
- 239000011734 sodium Substances 0.000 claims description 11
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 claims description 10
- 239000001110 calcium chloride Substances 0.000 claims description 9
- 229910001628 calcium chloride Inorganic materials 0.000 claims description 9
- ZCCIPPOKBCJFDN-UHFFFAOYSA-N calcium nitrate Chemical compound [Ca+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O ZCCIPPOKBCJFDN-UHFFFAOYSA-N 0.000 claims description 8
- 238000002156 mixing Methods 0.000 claims description 7
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Natural products NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 claims description 6
- 239000007864 aqueous solution Substances 0.000 claims description 6
- 239000000203 mixture Substances 0.000 claims description 6
- 239000011780 sodium chloride Substances 0.000 claims description 5
- NKWPZUCBCARRDP-UHFFFAOYSA-L calcium bicarbonate Chemical compound [Ca+2].OC([O-])=O.OC([O-])=O NKWPZUCBCARRDP-UHFFFAOYSA-L 0.000 claims description 4
- 229910000020 calcium bicarbonate Inorganic materials 0.000 claims description 4
- YYRMJZQKEFZXMX-UHFFFAOYSA-L calcium bis(dihydrogenphosphate) Chemical compound [Ca+2].OP(O)([O-])=O.OP(O)([O-])=O YYRMJZQKEFZXMX-UHFFFAOYSA-L 0.000 claims description 4
- 229940062672 calcium dihydrogen phosphate Drugs 0.000 claims description 4
- 229910000389 calcium phosphate Inorganic materials 0.000 claims description 4
- 235000013877 carbamide Nutrition 0.000 claims description 4
- 239000004202 carbamide Substances 0.000 claims description 4
- 235000019691 monocalcium phosphate Nutrition 0.000 claims description 4
- 238000007789 sealing Methods 0.000 claims description 4
- 150000003672 ureas Chemical group 0.000 claims description 2
- 239000011148 porous material Substances 0.000 abstract description 19
- 239000003623 enhancer Substances 0.000 abstract description 6
- 239000007787 solid Substances 0.000 description 10
- 229920000620 organic polymer Polymers 0.000 description 9
- 238000010586 diagram Methods 0.000 description 6
- 238000011835 investigation Methods 0.000 description 6
- 239000000126 substance Substances 0.000 description 6
- BHPQYMZQTOCNFJ-UHFFFAOYSA-N Calcium cation Chemical compound [Ca+2] BHPQYMZQTOCNFJ-UHFFFAOYSA-N 0.000 description 5
- 229910001424 calcium ion Inorganic materials 0.000 description 5
- 230000000694 effects Effects 0.000 description 5
- 239000000378 calcium silicate Substances 0.000 description 4
- 229910052918 calcium silicate Inorganic materials 0.000 description 4
- OYACROKNLOSFPA-UHFFFAOYSA-N calcium;dioxido(oxo)silane Chemical compound [Ca+2].[O-][Si]([O-])=O OYACROKNLOSFPA-UHFFFAOYSA-N 0.000 description 4
- 230000008569 process Effects 0.000 description 4
- -1 silicate ions Chemical class 0.000 description 4
- HRPVXLWXLXDGHG-UHFFFAOYSA-N Acrylamide Chemical compound NC(=O)C=C HRPVXLWXLXDGHG-UHFFFAOYSA-N 0.000 description 3
- 239000004115 Sodium Silicate Substances 0.000 description 3
- 230000005465 channeling Effects 0.000 description 3
- 238000005516 engineering process Methods 0.000 description 3
- 230000007613 environmental effect Effects 0.000 description 3
- 238000004519 manufacturing process Methods 0.000 description 3
- 238000005259 measurement Methods 0.000 description 3
- NTHWMYGWWRZVTN-UHFFFAOYSA-N sodium silicate Chemical compound [Na+].[Na+].[O-][Si]([O-])=O NTHWMYGWWRZVTN-UHFFFAOYSA-N 0.000 description 3
- 229910052911 sodium silicate Inorganic materials 0.000 description 3
- 238000003756 stirring Methods 0.000 description 3
- ISXSCDLOGDJUNJ-UHFFFAOYSA-N tert-butyl prop-2-enoate Chemical compound CC(C)(C)OC(=O)C=C ISXSCDLOGDJUNJ-UHFFFAOYSA-N 0.000 description 3
- 238000004090 dissolution Methods 0.000 description 2
- 238000002347 injection Methods 0.000 description 2
- 239000007924 injection Substances 0.000 description 2
- 229910010272 inorganic material Inorganic materials 0.000 description 2
- 239000011147 inorganic material Substances 0.000 description 2
- 229910003480 inorganic solid Inorganic materials 0.000 description 2
- 150000002500 ions Chemical class 0.000 description 2
- 239000007788 liquid Substances 0.000 description 2
- 230000000737 periodic effect Effects 0.000 description 2
- 238000011084 recovery Methods 0.000 description 2
- 150000004760 silicates Chemical class 0.000 description 2
- 235000020681 well water Nutrition 0.000 description 2
- 239000002349 well water Substances 0.000 description 2
- XFXPMWWXUTWYJX-UHFFFAOYSA-N Cyanide Chemical compound N#[C-] XFXPMWWXUTWYJX-UHFFFAOYSA-N 0.000 description 1
- 229920002873 Polyethylenimine Polymers 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 125000005521 carbonamide group Chemical group 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 238000010276 construction Methods 0.000 description 1
- 229920001577 copolymer Polymers 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 230000002708 enhancing effect Effects 0.000 description 1
- IQPQWNKOIGAROB-UHFFFAOYSA-N isocyanate Chemical compound [N-]=C=O IQPQWNKOIGAROB-UHFFFAOYSA-N 0.000 description 1
- 230000007774 longterm Effects 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 229910052708 sodium Inorganic materials 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
- C09K8/00—Compositions for drilling of boreholes or wells; Compositions for treating boreholes or wells, e.g. for completion or for remedial operations
- C09K8/50—Compositions for plastering borehole walls, i.e. compositions for temporary consolidation of borehole walls
- C09K8/504—Compositions based on water or polar solvents
- C09K8/5045—Compositions based on water or polar solvents containing inorganic compounds
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
- C09K8/00—Compositions for drilling of boreholes or wells; Compositions for treating boreholes or wells, e.g. for completion or for remedial operations
- C09K8/50—Compositions for plastering borehole walls, i.e. compositions for temporary consolidation of borehole walls
- C09K8/504—Compositions based on water or polar solvents
- C09K8/506—Compositions based on water or polar solvents containing organic compounds
-
- E—FIXED CONSTRUCTIONS
- E21—EARTH OR ROCK DRILLING; MINING
- E21B—EARTH OR ROCK DRILLING; OBTAINING OIL, GAS, WATER, SOLUBLE OR MELTABLE MATERIALS OR A SLURRY OF MINERALS FROM WELLS
- E21B33/00—Sealing or packing boreholes or wells
- E21B33/10—Sealing or packing boreholes or wells in the borehole
- E21B33/13—Methods or devices for cementing, for plugging holes, crevices or the like
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- Life Sciences & Earth Sciences (AREA)
- Chemical & Material Sciences (AREA)
- General Life Sciences & Earth Sciences (AREA)
- Engineering & Computer Science (AREA)
- Organic Chemistry (AREA)
- Materials Engineering (AREA)
- Geology (AREA)
- Mining & Mineral Resources (AREA)
- Geochemistry & Mineralogy (AREA)
- Physics & Mathematics (AREA)
- Fluid Mechanics (AREA)
- Environmental & Geological Engineering (AREA)
- Inorganic Chemistry (AREA)
- Solid-Sorbent Or Filter-Aiding Compositions (AREA)
- Soil Conditioners And Soil-Stabilizing Materials (AREA)
- Silicates, Zeolites, And Molecular Sieves (AREA)
Abstract
The invention provides a water shutoff agent, a preparation method, an experimental method and a water shutoff method thereof, wherein the water shutoff agent comprises the following components: the water shutoff agent comprises: a first reaction liquid comprising: silicate solution, enhancer and water; a second reaction solution comprising: water-soluble calcium salt and water; in the first reaction liquid, the silicate solution is 36 to 48 mass%, the reinforcing agent is 2 to 4 mass%, and the balance is water, and in the second reaction liquid, the water-soluble calcium salt is 1 to 2 mass%, and the balance is water. The water shutoff agent provided by the disclosure has the advantages that the reaction condition for forming gel is simple, inorganic gel can be quickly generated, the water shutoff agent is high-temperature resistant, the viscosity of reaction liquid is low, the reaction liquid can easily enter stratum cracks or pores, meanwhile, the reinforcing agent is added into the water shutoff agent, the strength of the generated gel can be improved, and the water shutoff reliability is high.
Description
Technical Field
The disclosure relates to the technical field of gas well water plugging, in particular to a water plugging agent, a preparation method, an experiment method and a water plugging method thereof.
Background
In the water injection development process of a gas field, the water shutoff agent is usually used for chemical water shutoff to eliminate or reduce water flooding phenomena such as water layer channeling, bottom water coning, side water inrush and the like caused by long-term water injection, so that the recovery efficiency is improved. The water shutoff agent has the advantages of low concentration, low cost, simple process, easy control, obvious effect and the like because the water shutoff agent has large using amount and needs to be injected into a gas well on site for construction.
The water shutoff agent provided in the related technology comprises binary copolymer of acrylamide and tert-butyl acrylate and polyethyleneimine, and can enter formation cracks or pores after being injected into a gas well, and organic polymer cross-linked bodies are formed in the formation cracks or pores to block the formation cracks and prevent water channeling.
However, in the related art, the plugging substance generated by the water shutoff agent at the formation cracks or pores is an organic polymer cross-linked body, the conditions for forming the organic polymer cross-linked body by reaction are harsh, the formed organic polymer cross-linked body has high viscosity, is not easy to enter the formation cracks or pores, and the water shutoff reliability of the water shutoff agent is poor.
Disclosure of Invention
The embodiment of the disclosure provides a water shutoff agent, a preparation method, an experimental method and a water shutoff method thereof, which can quickly generate inorganic gel, have low viscosity of reaction liquid, can easily enter stratum cracks or pores, have high water shutoff reliability and have simple reaction conditions for generating the gel. The technical scheme is as follows:
the embodiment of the present disclosure provides a water shutoff agent, the water shutoff agent includes: a first reaction liquid comprising: silicate solution, reinforcing agent and water; a second reaction solution comprising: water-soluble calcium salt and water; in the first reaction liquid, the silicate solution accounts for 36-48% by mass, the reinforcing agent accounts for 2-4% by mass, and the balance is water, and in the second reaction liquid, the water-soluble calcium salt accounts for 1-2% by mass, and the balance is water.
In one implementation of the disclosed embodiment, the silicate solution is 42.8% by mass, the reinforcing agent is 3% by mass, and the water-soluble calcium salt is 1.36% by mass in the first reaction liquid.
In another implementation of an embodiment of the disclosure, the silicate solution is Na 2 SiO 3 The percentage of solute in the aqueous solution of (1) is 35%.
In another implementation of an embodiment of the disclosure, the enhancer is carbamide.
In another implementation of the disclosed embodiment, the water-soluble calcium salt is calcium chloride, calcium bicarbonate, calcium nitrate, or calcium dihydrogen phosphate.
The embodiment of the present disclosure discloses a preparation method of a water shutoff agent, which is suitable for preparing the water shutoff agent, and the preparation method includes: adding water, 36-48% of silicate solution and 2-4% of reinforcing agent into a first reaction vessel according to the mass percentage to obtain a first reaction solution; and adding water and 1-2% of water-soluble calcium salt into a second reaction vessel according to the mass percentage to obtain a second reaction solution.
The embodiment of the disclosure discloses an experimental method of a water shutoff agent, which is suitable for carrying out an experiment on the water shutoff agent, and the experimental method comprises the following steps: carrying out a high temperature resistance test on the water shutoff agent, and periodically measuring the dehydration amount of gel generated by the water shutoff agent within a set period; determining the high-temperature resistance of the water shutoff agent according to the dehydration amount; carrying out salt tolerance test on the water shutoff agent, and regularly observing the gel character generated by the water shutoff agent within a set period; and determining the salt resistance of the water shutoff agent according to the gel character.
In another implementation manner of the embodiment of the present disclosure, performing a high temperature resistance test on the water shutoff agent includes: sequentially adding the first reaction solution and the second reaction solution into a high-temperature tank, sealing the high-temperature tank, and placing the high-temperature tank in an environment with a set temperature to perform a high-temperature resistance test, wherein the set temperature is not lower than 145 ℃; measuring the dehydration amount of the gel generated by the water shutoff agent within the set time limit, wherein the set time limit is not less than 6 months; the determining the high temperature resistance of the water shutoff agent according to the dehydration amount comprises the following steps: and if the dehydration amount is not more than 4% within the set time limit, determining that the high-temperature resistance of the water shutoff agent can reach the set temperature.
In another implementation manner of the embodiment of the present disclosure, performing a salt tolerance test on the water shutoff agent includes: mixing the first reaction solution and the second reaction solution to obtain a mixture, and adding a sodium chloride solution into the mixture; observing a water-gel interface of gel generated by the water shutoff agent within a set period of not less than 6 months; the salt tolerance of the water shutoff agent is determined according to the gel character, and the method comprises the following steps: and if the water-gel interface is always clear within the set time limit and the shape and the volume of the gel generated by the water shutoff agent are not changed, determining that the salt resistance of the water shutoff agent meets the use requirement.
The embodiment of the disclosure discloses a water plugging method, which is suitable for plugging water by adopting the water plugging agent, and the water plugging method comprises the following steps: injecting a first reaction liquid into the well; and injecting a second reaction liquid into the well, wherein the volume or the mass of the first reaction liquid and the second reaction liquid injected into the well are the same.
The beneficial effects brought by the technical scheme provided by the embodiment of the disclosure at least comprise:
according to the embodiment of the disclosure, the silicate in the first reaction liquid and the water-soluble calcium chloride in the second reaction liquid are both inorganic substances, so that the gel formed by mixing the first reaction liquid and the second reaction liquid is also inorganic, and meanwhile, the generated gel can be tightly combined together by using the reinforcing agent, so that the mechanical property of the gel is improved, and the water shutoff agent has a good water shutoff effect. In the using process, the first reaction liquid and the second reaction liquid can be injected into the well in sequence, the silicate and the calcium chloride in the first reaction liquid and the second reaction liquid can react quickly to generate gel after being mixed under an alkaline condition, the silicate solution and the calcium chloride solution have low viscosity and can enter stratum pores or cracks more easily, the gel produced by reaction is completely filled in the stratum cracks and a flow channel formed by the pores, and the inorganic solid gel does not flow and has certain strength, so that the water plugging function can be realized. The reaction condition for generating the gel by the water shutoff agent is simple, the inorganic gel can be quickly generated, the viscosity of the reaction liquid is low, the reaction liquid can easily enter stratum cracks or pores, and the water shutoff reliability is high.
Drawings
In order to more clearly illustrate the technical solutions in the embodiments of the present disclosure, the drawings required to be used in the description of the embodiments are briefly introduced below, and it is apparent that the drawings in the description below are only some embodiments of the present disclosure, and it is obvious for those skilled in the art that other drawings may be obtained according to the drawings without creative efforts.
Fig. 1 is a temperature-resistant investigation experimental data diagram of a water shutoff agent provided by an embodiment of the disclosure;
fig. 2 is a temperature-resistant investigation experiment data diagram of the water shutoff agent provided by the embodiment of the disclosure;
fig. 3 is a temperature-resistant investigation experiment data diagram of the water shutoff agent provided by the embodiment of the disclosure;
fig. 4 is a flow chart of a method of preparing a water shutoff agent according to an embodiment of the disclosure;
fig. 5 is a flowchart of an experimental method for providing a water shutoff agent according to an embodiment of the present disclosure.
Detailed Description
To make the objects, technical solutions and advantages of the present disclosure more apparent, embodiments of the present disclosure will be described in detail with reference to the accompanying drawings.
The gas reservoir of the Longwanggao group with the gas reserves of 4065.76 billions cubic meters in the MX block of the Sichuan Anyue gas field is an oversize gas reservoir, the average temperature of the middle part of the gas reservoir can reach 142.26 ℃, the pressure of the middle part can reach 76.02Mpa, and the pressure coefficient is 1.63, thus belonging to a high-temperature and high-pressure gas reservoir.
For the super-huge gas reservoir, if bottom water coning, side water inrush and the like occur, water can flow out of the gas well, the normal production of the gas well is seriously influenced, and the recovery ratio of the gas reservoir is greatly reduced. Thus, gas fields typically require the implementation of gas well water shutoff.
In the related technology, a large amount of water shutoff agents are generally injected into a gas well, the water shutoff agents mostly adopt an organic polymer system, and the water shutoff agents enter formation cracks or pores after being injected into the gas well to form organic polymer crosslinked gel so as to block the formation cracks and prevent water channeling.
However, in the case of a high-temperature gas reservoir in which the average temperature in the middle of the gas reservoir reaches 142.26 ℃, the organic polymer crosslinked body of the related art is not heat-resistant and is easily decomposed at an excessively high temperature, and therefore, the water shutoff layer formed by the water shutoff agent of the related art is easily deteriorated in a short period of time.
In addition, in the related technology, the conditions for forming the organic polymer cross-linked body by the water shutoff agent reaction are harsh, the formed organic polymer cross-linked body has high viscosity, is not easy to enter stratum cracks or pores, and the water shutoff reliability of the water shutoff agent is poor.
Therefore, the embodiment of the present disclosure provides a water shutoff agent, which includes: a first reaction solution and a second reaction solution. The first reaction solution includes: silicate solution, reinforcing agent and clear water; a second reaction solution comprising: water-soluble calcium salt and clear water. In the first reaction liquid, the silicate solution accounts for 36-48% by mass, the reinforcing agent accounts for 2-4% by mass, and the balance is water, and in the second reaction liquid, the water-soluble calcium salt accounts for 1-2% by mass, and the balance is water.
According to the embodiment of the disclosure, the silicate in the first reaction liquid and the water-soluble calcium chloride in the second reaction liquid are both inorganic substances, so that the gel formed by mixing the first reaction liquid and the second reaction liquid is also an inorganic gel, and meanwhile, the generated gel can be tightly combined together by using the reinforcing agent, so that the mechanical property of the gel is improved, and the water shutoff agent has a good water shutoff effect. In the using process, the first reaction liquid and the second reaction liquid can be injected into the well in sequence, the silicate and the calcium chloride in the first reaction liquid and the second reaction liquid can react quickly to generate gel after being mixed under an alkaline condition, the silicate solution and the calcium chloride solution have low viscosity and can enter stratum pores or cracks more easily, the gel produced by reaction is completely filled in the stratum cracks and a flow channel formed by the pores, and the inorganic solid gel does not flow and has certain strength, so that the water plugging function can be realized. The reaction condition for generating the gel by the water shutoff agent is simple, the inorganic gel can be quickly generated, the viscosity of the reaction liquid is low, the reaction liquid can easily enter stratum cracks or pores, and the water shutoff reliability is high. Compared with the prior art in which organic matters are used as the water shutoff agent, the preparation cost of the water shutoff agent is higher due to the high price of the organic matters such as acrylamide, tert-butyl acrylate and the like. The components used in the water shutoff agent in the embodiment are inorganic materials, so that the water shutoff agent is cheap and easy to obtain and has good economical efficiency.
In the embodiment of the present disclosure, the water-soluble silicate may be selected and prepared into a solution, so as to be mixed with the clear water and the enhancing agent to prepare the first reaction solution. The common characteristics of the above silicates are: after being dissolved in water, a large amount of silicate ions can be ionized in the aqueous solution, so that the prepared first reaction liquid is easier to combine with a large amount of calcium ions in the second reaction liquid, calcium silicate is generated by reaction, and a solid gel which is not dissolved in water is formed.
Illustratively, the silicate solution may be Na 2 SiO 3 In aqueous solution of (i.e. Na) 2 SiO 3 Is a solute and is dissolved in clear water to form a solution. And the percentage of solute is 35%.
Wherein, the percentage content of the solute in the solution can be determined by adopting the following formula:
in the formula (1), C is the percentage content of the solute, M is the mass of the solute, and M is the mass of the solvent.
For example, if Na is to be prepared 2 SiO 3 Is a 35% solution, according to preparation of 100g of Na 2 SiO 3 Solution, it was determined that the solution included 35g of Na 2 SiO 3 And 65g of clear water.
Optionally, in the preparation of Na 2 SiO 3 During the solution, instant solid sodium silicate can be selected, and hot water and sodium silicate are required to be mixed in the preparation process so as to accelerate the dissolution of the sodium silicate.
The water-soluble silicate may be Na as exemplified above 2 SiO 3 Besides, the gel can be other water-soluble silicates, as long as the silicate can be ionized into a large number of silicate ions in the water solution after being dissolved in water, and the ionized other ions do not influence the generated solid gel, and the embodiment of the disclosure canAnd are not intended to be limiting.
Alternatively, the reinforcing agent is a substance added to the gel to be tightly bound to the gel and to significantly improve the mechanical properties of the gel. The reinforcing agent is added into the water shutoff agent, so that inorganic gel generated by the reaction in the first reaction liquid and the second reaction liquid can be tightly combined, and the stability of the inorganic gel is improved.
In this example, the enhancer was a carbonyl amide. The reinforcing agent of the carbonamide can react with cyanide ions under the alkaline condition to participate in the formation of bonds in the gel, thereby increasing the strength of the water shutoff agent.
Optionally, after the water-soluble calcium salt is dissolved in clear water, the formed second reaction liquid contains a large amount of calcium ions, the calcium ions can be combined with a large amount of silicate ions in the first reaction liquid to react to generate calcium silicate, and the calcium silicate is a water-insoluble solid gel, so that the purpose of water plugging can be realized.
Illustratively, the water-soluble calcium salt may be calcium chloride, calcium bicarbonate, calcium nitrate, or calcium dihydrogen phosphate. The common characteristics of the calcium salts are as follows: after being dissolved in water, a large amount of calcium ions can be ionized in the aqueous solution, so that the prepared second reaction liquid is more easily combined with a large amount of silicate ions in the first reaction liquid to react to generate calcium silicate so as to form a solid gel which is not dissolved in water.
The water-soluble calcium salt may be calcium chloride, calcium bicarbonate, calcium nitrate, or calcium dihydrogen phosphate, which are exemplified above, or may be other water-soluble calcium salts, as long as the calcium salt is dissolved in water, and then a large amount of calcium ions are ionized in the aqueous solution, and the ionized other ions do not affect the solid gel formed, and the embodiment of the present disclosure is not limited.
In the embodiment of the disclosure, the content of each component in the water shutoff agent has the optimal proportioning relationship, so that the gel formed by the water shutoff agent with the optimal proportioning relationship can have good water shutoff performance and salt tolerance. The optimal content proportion relation of each component in the water shutoff agent comprises the following steps: 42.8 percent of silicate solution, 3 percent of reinforcing agent and 1.36 percent of water-soluble calcium salt.
Fig. 1 is a temperature-resistant investigation experimental data diagram of the water shutoff agent provided by the embodiment of the disclosure. As shown in FIG. 1, the experiment examined a 50mL water shutoff agent pattern and the amount of dehydration of the gel formed by the water shutoff agent at an ambient temperature of 145 ℃. As can be seen from FIG. 1, the amount of water removed by the water shutoff agent is always 0 in 0 to 30 days, and the amount of water removed by the water shutoff agent is maintained within 1.6mL in 30 to 240 days. Therefore, the gel formed by the water shutoff agent with the proportioning relation can keep good water shutoff performance at the environmental temperature of more than 145 ℃.
Meanwhile, salt tolerance experiments are carried out on the water shutoff agent in the proportioning relation, and the gel formed by the water shutoff agent is complete in half a year and clear in water-gel interface. Therefore, the gel formed by the water shutoff agent with the proportioning relation has better salt resistance.
In this embodiment, the content of each component in the water shutoff agent may also be at a critical value, and the content of each component is a critical value, so that the gel formed by the water shutoff agent can have water shutoff performance and salt resistance, so as to satisfy the effect of the gel in realizing water shutoff and plugging in formation cracks or pores.
Illustratively, the silicate solution may be 36% by weight, the enhancer 2% by weight, and the water-soluble calcium salt 1% by weight. The content of each component in the water shutoff agent is the lowest value in the critical values, the water shutoff agent can also have water shutoff performance and salt tolerance, and the water shutoff performance and the salt tolerance are slightly poor compared with the water shutoff agent with the content of each component in the optimal proportioning relation, but the content of each component in the water shutoff agent is reduced, so the cost for manufacturing the water shutoff agent can be saved during mass production.
Fig. 2 is a temperature-resistant investigation experimental data diagram of the water shutoff agent provided by the embodiment of the disclosure. As shown in FIG. 2, the experiment examined the 50mL water shutoff agent pattern and the amount of dehydration of the gel formed by the water shutoff agent at an ambient temperature of 145 ℃. As can be seen from FIG. 1, the amount of water removed by the water shutoff agent is always 0 in 0 to 25 days, and the water shutoff agent starts to remove water only in 25 to 240 days, and the amount of water removed is maintained within 1.9 mL. Therefore, the gel formed by the water shutoff agent with the proportioning relation can keep good water shutoff performance at the environmental temperature of more than 145 ℃.
Meanwhile, salt tolerance experiments are carried out on the water shutoff agent in the proportioning relation, and the gel formed by the water shutoff agent is complete in half a year and clear in water-gel interface. Therefore, the gel formed by the water shutoff agent with the proportioning relation has better salt resistance.
Illustratively, the silicate solution may be 48% by mass, the enhancer 4% by mass, and the water-soluble calcium salt 2% by mass. The water shutoff agent has certain water shutoff performance and salt tolerance, and the water shutoff agent has the water shutoff performance and salt tolerance equivalent to those of the water shutoff agent with the optimal proportion relation of the content of each component in the water shutoff agent.
Fig. 3 is a temperature-resistant investigation experiment data diagram of the water shutoff agent provided by the embodiment of the disclosure. As shown in fig. 3, the experiment examined the 50mL water shutoff agent pattern, and the amount of dehydration of the gel formed by the water shutoff agent at an ambient temperature of 145 ℃. As can be seen from FIG. 1, the dehydration amount of the water shutoff agent is always 0 in 0 to 28 days, and the dehydration amount of the water shutoff agent is maintained within 1.7mL in 28 to 240 days. Therefore, the gel formed by the water shutoff agent with the proportioning relation can keep good water shutoff performance at the environmental temperature of more than 145 ℃.
Meanwhile, salt tolerance experiments are carried out on the water shutoff agent in the proportioning relation, and the gel formed by the water shutoff agent is complete in half a year and clear in water-gel interface. Therefore, the gel formed by the water shutoff agent with the proportioning relation has better salt resistance.
In addition, in the embodiment, if the content of each component in the water shutoff agent is at the critical value, the content of each component may also be different from the minimum critical value or the maximum critical value.
Illustratively, the silicate solution may be 48% by weight, the enhancer 2% by weight, and the water-soluble calcium salt 1% by weight. The water shutoff agent with the proportioning relation can also have certain water shutoff performance and salt tolerance, and the water shutoff performance and the salt tolerance of the water shutoff agent with the proportioning relation are equivalent to those of the water shutoff agent with the optimal proportioning relation of the contents of the components in the water shutoff agent, so that the effect of water shutoff and leakage stoppage of gel formed by the water shutoff agent in bottom cracks or pores can be realized.
Fig. 4 is a flowchart of a method for preparing a water shutoff agent according to an embodiment of the present disclosure. As shown in fig. 4, the preparation method is suitable for preparing the water shutoff agent, and the preparation method comprises the following steps:
step 101: according to the mass percent, adding water, 36 to 48 percent of silicate solution and 2 to 4 percent of reinforcing agent into a first reaction vessel to obtain first reaction liquid.
Taking the best proportion of the contents of the components in the water shutoff agent preparation as an example for illustration, 54.2 percent of clear water and 42.8 percent of Na are sequentially added into a beaker according to the mass percentage 2 SiO 3 The solution (solute percentage content is 35 percent) and 3 percent carbamide are fully stirred to prepare a first reaction liquid.
Illustratively, taking the preparation of 25g of the first reaction solution as an example, the preparation process may be: adding 13.55g of clear water into a 50mL beaker, then adding 0.75g of carbamide, stirring for complete dissolution, and then adding 10.7g of Na 2 SiO 3 The solution (solute content of 35%) is stirred uniformly. 25g of the first reaction solution was prepared.
Step 102: and adding water and 1-2% of water-soluble calcium salt into a second reaction vessel according to the mass percentage to obtain a second reaction solution.
Taking the best proportion of the components in the water shutoff agent preparation as an example for illustration, 98.64 percent of clear water and 1.36 percent of water-soluble calcium salt (CaCl) are sequentially added into a beaker according to the mass percentage 2 ) And fully stirring to prepare a second reaction solution.
Illustratively, taking the preparation of 25g of the second reaction solution as an example, the preparation process may be: adding 24.66g of clear water into a 50mL beaker, and adding 0.34g of water-soluble calcium salt (CaCl) 2 ) And stirring uniformly. 25g of the second reaction solution was prepared.
In this embodiment, the solid gel is obtained by mixing the first reaction solution and the second reaction solution, and therefore, after the first reaction solution and the second reaction solution are prepared, the first reaction solution and the second reaction solution are mixed when a water shutoff agent is required.
When the first reaction solution and the second reaction solution are mixed, the first reaction solution and the second reaction solution may be mixed in equal volumes. Because the proportion of each component in the first reaction liquid and the second reaction liquid is determined during preparation, when the solid gel is used on site, the solid gel can be generated by equal mass or equal volume, and the equal volume is adopted for mixing the first reaction liquid and the second reaction liquid, because the first reaction liquid and the second reaction liquid are both in liquid state, the volume is used as a metering unit, and the measurement and the use are easier.
The silicate of the first reaction liquid and the water-soluble calcium chloride of the second reaction liquid in the water plugging agent prepared by the preparation method are inorganic substances, so that the gel formed by mixing the first reaction liquid and the second reaction liquid is also inorganic gel, and meanwhile, the inorganic gel generated by the water plugging agent has simple reaction conditions, can quickly generate the inorganic gel, has low viscosity of the reaction liquid, can easily enter stratum cracks or pores, and has high water plugging reliability. Compared with the prior art in which organic matters are used as the water shutoff agent, the preparation cost of the water shutoff agent is higher due to the high price of the organic matters such as acrylamide, tert-butyl acrylate and the like. The components used in the water shutoff agent in the embodiment are inorganic materials, so that the water shutoff agent is cheap and easy to obtain and has good economical efficiency.
Fig. 5 is a flowchart of an experimental method for providing a water shutoff agent according to an embodiment of the present disclosure. As shown in fig. 5, the experimental method is suitable for performing the experiment on the water shutoff agent, and the experimental method comprises the following steps:
step 201: and (3) carrying out a high-temperature resistance test on the water shutoff agent, and periodically measuring the dehydration amount of the gel generated by the water shutoff agent within a set period.
Wherein, step 201 may include: and (3) sequentially adding the first reaction solution and the second reaction solution with equal volumes into a high-temperature tank, sealing the high-temperature tank, and placing the high-temperature tank in an environment with a set temperature for high-temperature resistance test, wherein the set temperature is not lower than 145 ℃.
Illustratively, 25mL of the first reaction solution may be transferred into a 60mL high temperature tank, and 25mL of the second reaction solution may be added and stirred uniformly to prepare a 50g sample of the water shutoff agent. Sealing the high-temperature tank, putting the high-temperature tank into an oven at 145 ℃, periodically measuring the dehydration amount of the gel within half a year, and observing the gel property.
The periodic measurement or observation may be performed in a plurality of periodic manners such as every 1 day and every 2 days, and this embodiment is not limited.
Step 202: and determining the high temperature resistance of the water shutoff agent according to the dehydration amount.
Step 202 may include: measuring the dehydration amount of the gel generated by the water shutoff agent within a set period of not less than 6 months; and if the dehydration amount is not more than 4% within the set time limit, determining that the high-temperature resistance of the water shutoff agent can reach the set temperature.
As can be seen from fig. 1, the dehydration amount of the water shutoff agent is 1.6ml within 6 months, and the dehydration amount is less than 4% (50 ml × 4% =2 ml) of the volume of the water shutoff agent, that is, the dehydration amount is not greater than 4%, so that it can be determined that the high temperature resistance of the water shutoff agent can reach 145 ℃.
Step 203: and (3) carrying out salt tolerance test on the water shutoff agent, and regularly observing the gel character generated by the water shutoff agent within a set period.
Wherein, step 203 may comprise: the first reaction solution and the second reaction solution were mixed to obtain a mixture, and a sodium chloride solution was added to the mixture.
Illustratively, 2 × 10 is added to the water shutoff agent 5 And (3) measuring the gel property periodically in half a year by using mg/L sodium chloride solution to investigate the salt resistance of the water shutoff agent. The gel property can be the integrity of the gel, such as the change degree of the shape and volume of the gel, and the clearness of the water-gel interface.
Step 204: and determining the salt resistance of the water shutoff agent according to the gel property.
Step 204 may include: observing a water-gel interface of gel generated by the water shutoff agent within a set period of not less than 6 months; and if the water-gel interface is always clear within a set period of time and the shape and the volume of the gel generated by the water shutoff agent are not changed, determining that the salt resistance of the water shutoff agent meets the use requirement.
In this embodiment, 2X 10 5 The salt tolerance of the water shutoff agent is inspected in mg/L sodium chloride solution, the experimental result is that the shape and the volume of the gel are not changed all the time within 6 months, and the water-gel interface is clear, so that the salt tolerance of the water shutoff agent can be determined to meet the use requirement.
The embodiment provides a water shutoff method, which is suitable for water shutoff by using the water shutoff agent, and the water shutoff method comprises the following steps: and injecting a first reaction liquid into the well, injecting a second reaction liquid into the well after the first reaction liquid enters the well and flows to the formation cracks or pores, converging the second reaction liquid into the formation cracks to mix with the first reaction liquid after the second reaction liquid enters the well, reacting to generate inorganic gel, and filling the gel into flow channels in the formation cracks and pores so as to realize the water plugging function.
Wherein, the volumes or the masses of the first reaction liquid and the second reaction liquid injected into the well are the same. When the first reaction solution and the second reaction solution are mixed, the first reaction solution and the second reaction solution may be mixed in equal volumes. Because the proportion of each component in the first reaction liquid and the second reaction liquid is determined well during preparation, when water is blocked for on-site use, solid gel can be generated at equal mass or equal volume.
It should be noted that, because the first reaction solution and the second reaction solution are both in liquid state, the first reaction solution and the second reaction solution are easier to measure and take by using the volume as a measurement unit, so as to complete the water plugging operation quickly.
The above description is meant to be illustrative of the principles of the present disclosure and not to be taken in a limiting sense, and any modifications, equivalents, improvements and the like that are within the spirit and scope of the present disclosure are intended to be included therein.
Claims (9)
1. A water shutoff agent suitable for use in plugging formation fractures in gas fields, the water shutoff agent comprising:
a first reaction liquid comprising: silicate solution, reinforcing agent and water;
a second reaction solution comprising: water-soluble calcium salt and water;
in the first reaction liquid, the silicate solution is 42.8% by mass, the reinforcing agent is 3% by mass, and the balance is water;
in the second reaction liquid, the mass percent of the water-soluble calcium salt is 1.36 percent, and the balance is water;
when the water plugging agent is used for plugging water, the first reaction liquid and the second reaction liquid are injected into the well in sequence, and after the first reaction liquid enters the well, the second reaction liquid is added;
50mL of the water shutoff agent sample, the dehydration amount of the gel formed by the water shutoff agent is 0 within 0 to 30 days at the ambient temperature of 145 ℃, the dehydration of the water shutoff agent starts within 30 to 240 days, and the dehydration amount of the water shutoff agent is maintained within 1.6 mL.
2. The plugging agent of claim 1, wherein the silicate solution is Na 2 SiO 3 The percentage of solute in the aqueous solution of (1) is 35%.
3. The water shutoff agent of claim 1 wherein the reinforcing agent is carbamide.
4. The water shutoff agent according to claim 1, wherein the water-soluble calcium salt is calcium chloride, calcium bicarbonate, calcium nitrate or calcium dihydrogen phosphate.
5. A method of preparing a water shutoff agent suitable for use in the preparation of the water shutoff agent of any of claims 1 to 4, comprising:
adding water, 42.8% of silicate solution and 3% of reinforcing agent into a first reaction vessel according to the mass percentage to obtain first reaction liquid;
and adding water and 1.36% of water-soluble calcium salt into the second reaction vessel according to the mass percentage to obtain a second reaction solution.
6. An experimental method for water shutoff agents, which is suitable for the experiment of the water shutoff agent according to any one of claims 1 to 4, and which comprises:
carrying out a high temperature resistance test on the water shutoff agent, and periodically measuring the dehydration amount of gel generated by the water shutoff agent within a set time limit;
determining the high-temperature resistance of the water shutoff agent according to the dehydration amount;
carrying out salt tolerance test on the water shutoff agent, and regularly observing the gel character generated by the water shutoff agent within a set period;
and determining the salt resistance of the water shutoff agent according to the gel character.
7. The experimental method of a water shutoff agent according to claim 6, wherein the performing a high temperature resistance test on the water shutoff agent comprises:
sequentially adding the first reaction solution and the second reaction solution into a high-temperature tank, sealing the high-temperature tank, and placing the high-temperature tank in an environment with a set temperature for high-temperature resistance test, wherein the set temperature is not lower than 145 ℃;
measuring the dehydration amount of the gel generated by the water shutoff agent within the set time limit, wherein the set time limit is not less than 6 months;
the determining the high temperature resistance of the water shutoff agent according to the dehydration amount comprises the following steps:
and if the dehydration amount is not more than 4% within the set time limit, determining that the high-temperature resistance of the water shutoff agent can reach the set temperature.
8. The experimental method of water shutoff agent according to claim 6, wherein the salt tolerance test of the water shutoff agent comprises:
mixing the first reaction solution and the second reaction solution to obtain a mixture, and adding a sodium chloride solution into the mixture;
observing a water-gel interface of gel generated by the water shutoff agent within a set period of not less than 6 months;
the salt tolerance of the water shutoff agent is determined according to the gel character, and the method comprises the following steps:
and if the water-gel interface is clear all the time within the set time limit and the shape and the volume of the gel generated by the water shutoff agent are not changed, determining that the salt resistance of the water shutoff agent meets the use requirement.
9. A water shutoff method suitable for water shutoff using the water shutoff agent according to any one of claims 1 to 4, comprising:
injecting a first reaction liquid into the well; and injecting a second reaction liquid into the well, wherein the volume or the mass of the first reaction liquid and the second reaction liquid injected into the well are the same.
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| CN1563259A (en) * | 2004-03-30 | 2005-01-12 | 中国石油化工股份有限公司河南油田分公司石油工程技术研究院 | Inorganic delay silicic acid gel plugging regulator |
| CN106566503A (en) * | 2016-11-10 | 2017-04-19 | 中国石油化工股份有限公司 | Compound profile control agent for plugging large pore path of oil layer and preparation method thereof |
| CN109868126A (en) * | 2017-12-01 | 2019-06-11 | 中国石油天然气股份有限公司 | Water plugging agent and preparation method and application thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN1563259A (en) * | 2004-03-30 | 2005-01-12 | 中国石油化工股份有限公司河南油田分公司石油工程技术研究院 | Inorganic delay silicic acid gel plugging regulator |
| CN106566503A (en) * | 2016-11-10 | 2017-04-19 | 中国石油化工股份有限公司 | Compound profile control agent for plugging large pore path of oil layer and preparation method thereof |
| CN109868126A (en) * | 2017-12-01 | 2019-06-11 | 中国石油天然气股份有限公司 | Water plugging agent and preparation method and application thereof |
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