CN112195023A - Design method of acidizing fluid - Google Patents
Design method of acidizing fluid Download PDFInfo
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- CN112195023A CN112195023A CN201910533160.5A CN201910533160A CN112195023A CN 112195023 A CN112195023 A CN 112195023A CN 201910533160 A CN201910533160 A CN 201910533160A CN 112195023 A CN112195023 A CN 112195023A
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- 239000012530 fluid Substances 0.000 title claims abstract description 129
- 238000000034 method Methods 0.000 title claims abstract description 50
- 238000013461 design Methods 0.000 title claims abstract description 25
- 239000002253 acid Substances 0.000 claims abstract description 103
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims abstract description 76
- 239000011435 rock Substances 0.000 claims abstract description 46
- 239000000126 substance Substances 0.000 claims abstract description 40
- 238000006243 chemical reaction Methods 0.000 claims abstract description 33
- KRHYYFGTRYWZRS-UHFFFAOYSA-N Fluorane Chemical compound F KRHYYFGTRYWZRS-UHFFFAOYSA-N 0.000 claims abstract description 30
- 239000002244 precipitate Substances 0.000 claims abstract description 28
- 239000011343 solid material Substances 0.000 claims abstract description 26
- 239000007788 liquid Substances 0.000 claims abstract description 16
- 238000001035 drying Methods 0.000 claims abstract description 10
- 238000005406 washing Methods 0.000 claims abstract description 10
- 230000007935 neutral effect Effects 0.000 claims abstract description 9
- 239000007787 solid Substances 0.000 claims abstract description 7
- 238000000926 separation method Methods 0.000 claims abstract description 4
- XEEYBQQBJWHFJM-UHFFFAOYSA-N iron Substances [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims description 27
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 claims description 24
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 claims description 24
- 229910052742 iron Inorganic materials 0.000 claims description 24
- 239000003381 stabilizer Substances 0.000 claims description 22
- 238000012360 testing method Methods 0.000 claims description 21
- 239000003112 inhibitor Substances 0.000 claims description 19
- 239000004094 surface-active agent Substances 0.000 claims description 19
- 230000007797 corrosion Effects 0.000 claims description 18
- 238000005260 corrosion Methods 0.000 claims description 18
- 230000002579 anti-swelling effect Effects 0.000 claims description 17
- 239000003795 chemical substances by application Substances 0.000 claims description 17
- 239000000843 powder Substances 0.000 claims description 15
- 239000000654 additive Substances 0.000 claims description 12
- 229910000147 aluminium phosphate Inorganic materials 0.000 claims description 12
- 238000002441 X-ray diffraction Methods 0.000 claims description 10
- BDAGIHXWWSANSR-UHFFFAOYSA-N methanoic acid Natural products OC=O BDAGIHXWWSANSR-UHFFFAOYSA-N 0.000 claims description 10
- 230000000996 additive effect Effects 0.000 claims description 8
- OSWFIVFLDKOXQC-UHFFFAOYSA-N 4-(3-methoxyphenyl)aniline Chemical compound COC1=CC=CC(C=2C=CC(N)=CC=2)=C1 OSWFIVFLDKOXQC-UHFFFAOYSA-N 0.000 claims description 5
- 235000019253 formic acid Nutrition 0.000 claims description 5
- 239000013049 sediment Substances 0.000 claims description 5
- 239000002245 particle Substances 0.000 claims description 3
- 238000003825 pressing Methods 0.000 claims description 3
- 230000001965 increasing effect Effects 0.000 abstract description 12
- 230000000694 effects Effects 0.000 abstract description 4
- 238000002347 injection Methods 0.000 abstract description 4
- 239000007924 injection Substances 0.000 abstract description 4
- 238000004519 manufacturing process Methods 0.000 abstract description 3
- 238000001556 precipitation Methods 0.000 description 43
- -1 iron ion Chemical class 0.000 description 30
- 239000003921 oil Substances 0.000 description 19
- 230000020477 pH reduction Effects 0.000 description 17
- 238000005259 measurement Methods 0.000 description 13
- 230000035699 permeability Effects 0.000 description 12
- 239000000243 solution Substances 0.000 description 11
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 10
- 239000010703 silicon Substances 0.000 description 10
- 229910052710 silicon Inorganic materials 0.000 description 10
- IEECXTSVVFWGSE-UHFFFAOYSA-M iron(3+);oxygen(2-);hydroxide Chemical compound [OH-].[O-2].[Fe+3] IEECXTSVVFWGSE-UHFFFAOYSA-M 0.000 description 9
- 229960004887 ferric hydroxide Drugs 0.000 description 8
- XJKVPKYVPCWHFO-UHFFFAOYSA-N silicon;hydrate Chemical compound O.[Si] XJKVPKYVPCWHFO-UHFFFAOYSA-N 0.000 description 8
- NLXLAEXVIDQMFP-UHFFFAOYSA-N Ammonia chloride Chemical compound [NH4+].[Cl-] NLXLAEXVIDQMFP-UHFFFAOYSA-N 0.000 description 7
- 230000006872 improvement Effects 0.000 description 7
- 239000011734 sodium Substances 0.000 description 7
- 229910052708 sodium Inorganic materials 0.000 description 7
- ZLMJMSJWJFRBEC-UHFFFAOYSA-N Potassium Chemical compound [K] ZLMJMSJWJFRBEC-UHFFFAOYSA-N 0.000 description 6
- KRKNYBCHXYNGOX-UHFFFAOYSA-N citric acid Chemical compound OC(=O)CC(O)(C(O)=O)CC(O)=O KRKNYBCHXYNGOX-UHFFFAOYSA-N 0.000 description 6
- 238000001816 cooling Methods 0.000 description 6
- 238000001914 filtration Methods 0.000 description 6
- 239000011591 potassium Substances 0.000 description 6
- 229910052700 potassium Inorganic materials 0.000 description 6
- IRPGOXJVTQTAAN-UHFFFAOYSA-N 2,2,3,3,3-pentafluoropropanal Chemical compound FC(F)(F)C(F)(F)C=O IRPGOXJVTQTAAN-UHFFFAOYSA-N 0.000 description 5
- KLZUFWVZNOTSEM-UHFFFAOYSA-K Aluminum fluoride Inorganic materials F[Al](F)F KLZUFWVZNOTSEM-UHFFFAOYSA-K 0.000 description 5
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 description 5
- 238000004458 analytical method Methods 0.000 description 5
- WUKWITHWXAAZEY-UHFFFAOYSA-L calcium difluoride Chemical compound [F-].[F-].[Ca+2] WUKWITHWXAAZEY-UHFFFAOYSA-L 0.000 description 5
- 229910001634 calcium fluoride Inorganic materials 0.000 description 5
- 229910001919 chlorite Inorganic materials 0.000 description 5
- 229910052619 chlorite group Inorganic materials 0.000 description 5
- QBWCMBCROVPCKQ-UHFFFAOYSA-N chlorous acid Chemical compound OCl=O QBWCMBCROVPCKQ-UHFFFAOYSA-N 0.000 description 5
- 150000001875 compounds Chemical class 0.000 description 5
- BVKZGUZCCUSVTD-UHFFFAOYSA-L Carbonate Chemical compound [O-]C([O-])=O BVKZGUZCCUSVTD-UHFFFAOYSA-L 0.000 description 4
- WCUXLLCKKVVCTQ-UHFFFAOYSA-M Potassium chloride Chemical compound [Cl-].[K+] WCUXLLCKKVVCTQ-UHFFFAOYSA-M 0.000 description 4
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 4
- BAERPNBPLZWCES-UHFFFAOYSA-N (2-hydroxy-1-phosphonoethyl)phosphonic acid Chemical compound OCC(P(O)(O)=O)P(O)(O)=O BAERPNBPLZWCES-UHFFFAOYSA-N 0.000 description 3
- VTLYFUHAOXGGBS-UHFFFAOYSA-N Fe3+ Chemical compound [Fe+3] VTLYFUHAOXGGBS-UHFFFAOYSA-N 0.000 description 3
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 3
- WNROFYMDJYEPJX-UHFFFAOYSA-K aluminium hydroxide Chemical compound [OH-].[OH-].[OH-].[Al+3] WNROFYMDJYEPJX-UHFFFAOYSA-K 0.000 description 3
- 235000019270 ammonium chloride Nutrition 0.000 description 3
- 230000008859 change Effects 0.000 description 3
- 238000011156 evaluation Methods 0.000 description 3
- 229910001447 ferric ion Inorganic materials 0.000 description 3
- 239000004570 mortar (masonry) Substances 0.000 description 3
- RRRXPPIDPYTNJG-UHFFFAOYSA-N perfluorooctanesulfonamide Chemical compound NS(=O)(=O)C(F)(F)C(F)(F)C(F)(F)C(F)(F)C(F)(F)C(F)(F)C(F)(F)C(F)(F)F RRRXPPIDPYTNJG-UHFFFAOYSA-N 0.000 description 3
- 230000035945 sensitivity Effects 0.000 description 3
- 230000000087 stabilizing effect Effects 0.000 description 3
- 235000020985 whole grains Nutrition 0.000 description 3
- SJPVZEOHRLQKQN-UHFFFAOYSA-N 2-benzylpyridine;hydrochloride Chemical compound Cl.C=1C=CC=NC=1CC1=CC=CC=C1 SJPVZEOHRLQKQN-UHFFFAOYSA-N 0.000 description 2
- ABJVAXXYHSSYLK-UHFFFAOYSA-N 2-dodecylpyridine;hydrobromide Chemical compound Br.CCCCCCCCCCCCC1=CC=CC=N1 ABJVAXXYHSSYLK-UHFFFAOYSA-N 0.000 description 2
- 239000005995 Aluminium silicate Substances 0.000 description 2
- KCXVZYZYPLLWCC-UHFFFAOYSA-N EDTA Chemical compound OC(=O)CN(CC(O)=O)CCN(CC(O)=O)CC(O)=O KCXVZYZYPLLWCC-UHFFFAOYSA-N 0.000 description 2
- 238000004847 absorption spectroscopy Methods 0.000 description 2
- 235000012211 aluminium silicate Nutrition 0.000 description 2
- VSCWAEJMTAWNJL-UHFFFAOYSA-K aluminium trichloride Chemical compound Cl[Al](Cl)Cl VSCWAEJMTAWNJL-UHFFFAOYSA-K 0.000 description 2
- 229940077388 benzenesulfonate Drugs 0.000 description 2
- 239000004927 clay Substances 0.000 description 2
- 239000002131 composite material Substances 0.000 description 2
- 229960001484 edetic acid Drugs 0.000 description 2
- VKYKSIONXSXAKP-UHFFFAOYSA-N hexamethylenetetramine Chemical compound C1N(C2)CN3CN1CN2C3 VKYKSIONXSXAKP-UHFFFAOYSA-N 0.000 description 2
- 229910052500 inorganic mineral Inorganic materials 0.000 description 2
- NLYAJNPCOHFWQQ-UHFFFAOYSA-N kaolin Chemical compound O.O.O=[Al]O[Si](=O)O[Si](=O)O[Al]=O NLYAJNPCOHFWQQ-UHFFFAOYSA-N 0.000 description 2
- ORUIBWPALBXDOA-UHFFFAOYSA-L magnesium fluoride Chemical compound [F-].[F-].[Mg+2] ORUIBWPALBXDOA-UHFFFAOYSA-L 0.000 description 2
- 229910001635 magnesium fluoride Inorganic materials 0.000 description 2
- 239000011707 mineral Substances 0.000 description 2
- 235000010755 mineral Nutrition 0.000 description 2
- MGFYIUFZLHCRTH-UHFFFAOYSA-N nitrilotriacetic acid Chemical compound OC(=O)CN(CC(O)=O)CC(O)=O MGFYIUFZLHCRTH-UHFFFAOYSA-N 0.000 description 2
- 239000011148 porous material Substances 0.000 description 2
- 239000001103 potassium chloride Substances 0.000 description 2
- 235000011164 potassium chloride Nutrition 0.000 description 2
- 238000011158 quantitative evaluation Methods 0.000 description 2
- PNGBYKXZVCIZRN-UHFFFAOYSA-M sodium;hexadecane-1-sulfonate Chemical compound [Na+].CCCCCCCCCCCCCCCCS([O-])(=O)=O PNGBYKXZVCIZRN-UHFFFAOYSA-M 0.000 description 2
- RILZRCJGXSFXNE-UHFFFAOYSA-N 2-[4-(trifluoromethoxy)phenyl]ethanol Chemical compound OCCC1=CC=C(OC(F)(F)F)C=C1 RILZRCJGXSFXNE-UHFFFAOYSA-N 0.000 description 1
- LLVHFJHCODIQJH-UHFFFAOYSA-N 2-benzylquinoline Chemical compound C=1C=C2C=CC=CC2=NC=1CC1=CC=CC=C1 LLVHFJHCODIQJH-UHFFFAOYSA-N 0.000 description 1
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 description 1
- 229910000323 aluminium silicate Inorganic materials 0.000 description 1
- 239000004568 cement Substances 0.000 description 1
- 239000002734 clay mineral Substances 0.000 description 1
- 230000000052 comparative effect Effects 0.000 description 1
- HNPSIPDUKPIQMN-UHFFFAOYSA-N dioxosilane;oxo(oxoalumanyloxy)alumane Chemical compound O=[Si]=O.O=[Al]O[Al]=O HNPSIPDUKPIQMN-UHFFFAOYSA-N 0.000 description 1
- 229940104869 fluorosilicate Drugs 0.000 description 1
- 235000010299 hexamethylene tetramine Nutrition 0.000 description 1
- 229910052909 inorganic silicate Inorganic materials 0.000 description 1
- 235000014413 iron hydroxide Nutrition 0.000 description 1
- NCNCGGDMXMBVIA-UHFFFAOYSA-L iron(ii) hydroxide Chemical compound [OH-].[OH-].[Fe+2] NCNCGGDMXMBVIA-UHFFFAOYSA-L 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 229910017604 nitric acid Inorganic materials 0.000 description 1
- 230000001590 oxidative effect Effects 0.000 description 1
- 230000008569 process Effects 0.000 description 1
- 239000000047 product Substances 0.000 description 1
- 230000036632 reaction speed Effects 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 238000004062 sedimentation Methods 0.000 description 1
- 238000001228 spectrum Methods 0.000 description 1
- 230000008961 swelling Effects 0.000 description 1
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- 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
- C09K8/60—Compositions for stimulating production by acting on the underground formation
- C09K8/62—Compositions for forming crevices or fractures
- C09K8/72—Eroding chemicals, e.g. acids
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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
- C09K8/60—Compositions for stimulating production by acting on the underground formation
- C09K8/62—Compositions for forming crevices or fractures
- C09K8/66—Compositions based on water or polar solvents
- C09K8/665—Compositions based on water or polar solvents containing inorganic compounds
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- 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
- E21B43/00—Methods or apparatus for obtaining oil, gas, water, soluble or meltable materials or a slurry of minerals from wells
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Abstract
The invention relates to a design method of acidizing fluid, and belongs to the technical field of oilfield exploitation. The design method of the acidizing fluid comprises the following steps: 1) fully reacting a conventional earth acid basic acidizing fluid consisting of hydrochloric acid and hydrofluoric acid with a natural rock core at an oil reservoir temperature, carrying out solid-liquid separation, washing a solid to be neutral, and drying at the temperature of not higher than 60 ℃ to obtain an acid rock reaction residual solid material; 2) measuring secondary precipitated substances and content in the obtained acid rock reaction residual solid material; 3) and analyzing the reason of generating the precipitate according to the determined secondary precipitate substances and content, and designing the acidizing fluid on the basis of the basic acidizing fluid. The design method of the acidizing fluid provided by the invention can be used for directly measuring the type and the content of the secondary precipitated substances in the residual solid materials of the acid rock reaction, and designing the acidizing fluid in a targeted manner, so that the types and the quantity of the secondary precipitated substances can be effectively reduced, the acidizing effect is improved, and the design method of the acidizing fluid has important significance for the acidizing, production increasing and injection increasing of the oil field.
Description
Technical Field
The invention relates to a design method of acidizing fluid, and belongs to the technical field of oilfield exploitation.
Background
Acidification is one of the main measures for increasing the production and injection of oil fields, and the main function of the acidification is to improve the seepage capability of oil reservoirs by dissolving cement, clay minerals filled in pores or plugs through an acidification fluid. After the acidizing fluid reacts with oil reservoir rocks, the residual acidizing fluid is precipitated by compounds such as iron, silicon and the like due to the reduction of the pH value, and the precipitates are called secondary precipitates, and the common secondary precipitates mainly comprise: hydrated silicon, calcium fluoride, fluorosilicate, fluoroaluminate, aluminum fluoride, aluminum hydroxide, ferric hydroxide and the like, secondary precipitation can block pores of the oil reservoir, the yield increasing and injection increasing effects of acidification measures are reduced, and secondary pollution even to the oil reservoir can be seriously caused. Therefore, the control of the reaction of the acidizing fluid and the rock of the oil and gas reservoir to avoid secondary precipitation is an important technical content of acidizing fluid design in the acidizing process and an important guarantee of the success of the acidizing.
The acidizing fluid design includes the type of acidizing fluid, the concentration and the preference of various additives. The types of the current common acidizing fluid for sandstone oil reservoirs are conventional earth acid, authigenic earth acid, fluoroboric acid, organic retarded earth acid, earth acidizing fluid containing strong oxidizing nitric acid, retarded earth acid containing aluminum chloride, low-damage acid containing phosphoric acid, underground generated organic weak acid and the like; common types of additives are clay stabilizers, iron ion stabilizers, corrosion inhibitors, surfactants, demulsifiers, acid residue inhibitors, and the like. If the type, concentration and additive of the acidizing fluid are not properly selected in the design of the acidizing fluid, the type and quantity of secondary precipitation can be greatly increased, and the acidizing effect is influenced.
At present, because the evaluation of secondary precipitation is generally qualitative evaluation, and no method capable of quickly, simply and conveniently evaluating all secondary precipitation and contents exists, most of acidizing fluid and additives are designed according to the characteristics of minerals contained in an oil reservoir, the sensitivity characteristics of water sensitivity, acid sensitivity and the like, reservoir damage factors and the like, and the method cannot completely ensure that less secondary precipitation is generated after acid rock reaction. In addition, there is no patent for quantitatively evaluating the secondary precipitation, and there is no document for quantitatively evaluating the acidification liquid and additives by quantitatively evaluating various secondary precipitations generated by the acid rock reaction. Quantitative evaluation is carried out on secondary precipitation of the hydrated silicon by using a plasma absorption spectrometry in the analysis of influencing factors of the hydrated silicon precipitation in sandstone acidification (23 th volume of 25.12.2006 in oilfield chemistry), the design of the acidizing fluid is guided by an evaluation result, the method for designing the acidizing fluid only singly evaluates the precipitation amount of the hydrated silicon, does not carry out quantitative evaluation on other secondary precipitation, simultaneously evaluates that kaolin reacts with the acidizing fluid during secondary precipitation instead of a natural core, and obtains the conclusion that the concentration of hydrofluoric acid should be reduced in the design of the acidizing fluid, and the method for designing the acidizing fluid has one-sidedness and cannot ensure that various secondary precipitates generated in the reaction of the acidizing fluid and the natural core of the oil reservoir are reduced.
Disclosure of Invention
The invention aims to provide a design method capable of effectively reducing acidizing fluid generated by secondary precipitation.
In order to achieve the above purpose, the technical scheme adopted by the invention is as follows:
a design method of acidizing fluid comprises the following steps:
1) fully reacting a conventional earth acid basic acidizing fluid consisting of hydrochloric acid and hydrofluoric acid with a natural rock core at an oil reservoir temperature, carrying out solid-liquid separation, washing a solid to be neutral, and drying at the temperature of not higher than 60 ℃ to obtain an acid rock reaction residual solid material;
2) determining the type and content of secondary precipitated substances in the obtained acid rock reaction residual solid material;
3) and analyzing the reason of generating the precipitate according to the type and the content of the measured secondary precipitate substances, and designing the acidizing fluid on the basis of the conventional alkaline earth acid basic acidizing fluid.
The design method of the acidizing fluid provided by the invention can be used for directly measuring the type and the content of the secondary precipitated substances in the residual solid materials of the acid rock reaction, and designing the acidizing fluid in a targeted manner, so that the types and the quantity of the secondary precipitated substances can be effectively reduced, the acidizing effect is improved, and the design method of the acidizing fluid has important significance for the acidizing, production increasing and injection increasing of the oil field.
Preferably, in step 3), the method for designing the acidizing fluid comprises: and (3) replacing the conventional alkaline earth acid basic acidizing fluid in the step 1) after adjusting the mass ratio of HCl to HF in the conventional alkaline earth acid basic acidizing fluid, and repeating the step 1) and the step 2) to determine the concentrations of HCl and HF meeting the acidizing requirements. The generation of secondary precipitation can be reduced by adjusting the mass ratio of HCl to HF in the conventional alkaline earth acid basic acidizing fluid.
Preferably, in step 3), the method for designing the acidizing fluid further comprises: adding complex acid after adjusting the mass ratio of HCl to HF in the conventional alkaline earth acid basic acidizing fluid; the complex acid is at least one of formic acid, acetic acid, phosphoric acid and organic phosphoric acid. The pH value of the acidification liquid can be ensured to be less than or equal to 2 by adding the complex acid so as to prevent the generation of ferric hydroxide precipitate.
Preferably, in step 3), the method for designing the acidizing fluid further comprises: adding an additive after adjusting the mass ratio of HCl to HF in the conventional alkaline earth acid basic acidizing fluid; the additive comprises an iron ion stabilizer, an anti-swelling agent, a surfactant and a corrosion inhibitor. The iron ion stabilizer is added to prevent the generation of ferric hydroxide precipitate; the addition of the anti-swelling agent can prevent the oil reservoir permeability from being reduced due to clay swelling caused by acidizing fluid; the surface tension of the acidizing fluid can be reduced by adding the surfactant, so that the residual acid is favorably drained back; the corrosion inhibitor is added to prevent the acidizing fluid from corroding metal equipment. The additive is added into the conventional alkaline earth acid basic acidizing fluid according to the type and the content of the secondary precipitation substances, so that the type and the content of the secondary precipitation substances after acidizing can be further reduced.
Preferably, in the step 2), the method for measuring the secondary precipitated substances and the content of the secondary precipitated substances in the obtained solid comprises the following steps: and preparing the obtained solid material into powder, pressing the powder into a measuring test piece, and measuring secondary sediment substances and content in the measuring test piece by adopting an X-ray diffraction method. The content of each secondary precipitate can be more simply, conveniently and accurately determined by adopting an X-ray diffraction method.
In order to make the measurement result more accurate, it is preferable that the particle size of the powder is not more than 40 μm.
Drawings
FIG. 1 is an X-ray diffraction pattern of a test piece measured in step 2) of example 1 of the present invention;
FIG. 2 is an X-ray diffraction pattern of the test piece measured in step 2) of example 2 of the present invention;
FIG. 3 is an X-ray diffraction pattern of the test piece measured in step 2) of example 3 of the present invention.
Detailed Description
The design method of the acidizing fluid provided by the invention comprises the following steps:
1) fully reacting a conventional earth acid basic acidizing fluid consisting of hydrochloric acid and hydrofluoric acid with a natural rock core at an oil reservoir temperature, carrying out solid-liquid separation, washing a solid to be neutral, and drying at the temperature of not higher than 60 ℃ to obtain an acid rock reaction residual solid material;
2) determining the type and content of secondary precipitated substances in the obtained acid rock reaction residual solid material;
3) and analyzing the reason of generating the precipitate according to the type and the content of the measured secondary precipitate substances, and designing the acidizing fluid on the basis of the conventional alkaline earth acid basic acidizing fluid.
In order to simplify the design of the acidizing fluid on the basis of the conventional alkaline earth acid basic acidizing fluid, it is preferable that, in the step 1), the conventional alkaline earth acid basic acidizing fluid contains HCl and HF, the mass concentration of the HCl is 12%, and the mass concentration of the HF is 3%.
Preferably, in step 3), the method for designing the acidizing fluid comprises: adjusting the mass ratio of HCl and HF in the conventional alkaline earth acid basic acidizing fluid, then replacing the conventional alkaline earth acid basic acidizing fluid in the step 1), and repeating the step 1) and the step 2), and determining the concentrations of HCl and HF which meet the acidizing requirements.
Preferably, the adjusting the mass ratio of the HCl to the HF in the conventional alkaline earth acid basic acidizing fluid comprises: the mass concentration of HCl in the conventional alkaline earth acid basic acidizing fluid is increased, and the mass concentration of HF in the conventional alkaline earth acid basic acidizing fluid is reduced. The reason for increasing the mass concentration of HCl is that when the concentration of hydrochloric acid is higher, the reaction speed of hydrofluoric acid and reservoir rock can be increased, and when the mass percentage of hydrochloric acid to hydrofluoric acid is higher, the precipitation amount of silicon hydrate, aluminum fluoride and aluminum hydroxide is less, and the low-concentration hydrofluoric acid can avoid the generation of a large amount of silicon hydrate precipitates.
Further preferably, the mass ratio of HCl to HF in the conventional alkaline earth acid basic acidizing fluid is adjusted to be not less than 9: 1.
Further preferably, the mass concentration of HF in the conventional alkaline earth acid basic acidizing fluid is adjusted to be not more than 1%.
Preferably, in step 3), the method for designing the acidizing fluid further comprises: adding complex acid after adjusting the mass ratio of HCl to HF in the conventional alkaline earth acid basic acidizing fluid; the complex acid is at least one of formic acid, acetic acid, phosphoric acid and organic phosphoric acid. Further preferably, the mass percentage of the compound acid in the acidizing fluid after the compound acid is added is 5-12%. The organic phosphoric acid is hydroxyethylidene diphosphonic acid.
Preferably, in step 3), the method for designing the acidizing fluid further comprises: adding an additive after adjusting the mass ratio of HCl to HF in the conventional alkaline earth acid basic acidizing fluid; the additive comprises an iron ion stabilizer, an anti-swelling agent, a surfactant and a corrosion inhibitor. Preferably, after the iron ion stabilizer, the anti-swelling agent, the surfactant and the corrosion inhibitor are added, the iron ion stabilizer accounts for 0.5-2% of the acidizing fluid by mass, the anti-swelling agent accounts for 0.8-3% of the acidizing fluid by mass, the surfactant accounts for 0.3-1.5% of the acidizing fluid by mass, and the corrosion inhibitor accounts for 0.3-1.5% of the acidizing fluid by mass.
Preferably, the iron ion stabilizer is at least one of citric acid, ethylene diamine tetraacetic acid and nitrilotriacetic acid.
Preferably, the anti-swelling agent is at least one of ammonium chloride, potassium chloride and organic silicon.
Preferably, the surfactant is at least one of sodium hexadecyl sulfonate, sodium alkyl benzene sulfonate, perfluoroalkyl acrylate and perfluorooctyl sulfonamide (CAS #: 754-91-6).
Preferably, the corrosion inhibitor is at least one of benzyl quinoline quaternary ammonium chloride, dodecyl pyridine bromide, benzyl pyridine chloride and urotropine.
Preferably, when the secondary precipitated substance measured in step 2) includes at least one of calcium fluoride and magnesium fluoride, the method for designing the acidizing fluid in step 3) further includes setting a pre-acid. Preferably, the pre-acid is hydrochloric acid with the mass fraction of 5-15%.
Preferably, when the secondary precipitate measured in the step 2) comprises ferric hydroxide, the method for carrying out acidification design in the step 3) further comprises controlling the pH of the residual acid to be less than or equal to 2, and adding an iron ion stabilizer to ensure that the iron ion stabilizing capacity of the acidification liquid is greater than or equal to 90 mg/L. The residual acid is acid liquor after the acid rock reaction is finished.
Preferably, in the step 2), the method for measuring the secondary precipitated substances and the content of the secondary precipitated substances in the obtained solid comprises the following steps: and preparing the obtained solid material into powder, pressing the powder into a measuring test piece, and measuring secondary sediment substances and content in the measuring test piece by adopting an X-ray diffraction method.
Preferably, the particle size of the powder is not more than 40 μm.
The technical solution of the present invention will be further described with reference to the following embodiments.
The concentration of hydrochloric acid and the concentration of hydrofluoric acid used in each example were 37% and 40%. In the embodiment, when the acidizing fluid is designed, the total amount of the secondary precipitated substances is controlled to be below 0.5 percent (mass percentage), and the product is qualified.
Example 1
The design method of the acidizing fluid comprises the following steps:
1) respectively measuring 57.8mL of hydrochloric acid, 13.4mL of hydrofluoric acid and water, and mixing to prepare 200mL of conventional basic earth acid acidizing fluid; the mass concentration of HCl in the conventional alkaline earth acid basic acidizing fluid is 12 percent, and the mass concentration of HF is 3 percent;
then adding 40g of a natural rock core sample (the chlorite content is less than 5%) into a conventional basic earth acid acidizing fluid, fully reacting for 5 hours at the oil reservoir temperature, filtering, washing to be neutral, drying at 60 ℃, and cooling to room temperature to obtain a residual solid material of acid rock reaction;
2) putting the residual solid material of the acid rock reaction into an agate mortar to be ground into powder with the whole grain diameter less than 40 mu m, putting the powder into a sample frame, vertically and uniformly compacting and forming to prepare a measuring test piece, putting the measuring test piece into an X-ray diffractometer, obtaining an X-ray diffraction pattern (shown in figure 1) through measurement, and determining secondary precipitated substances existing in the measuring test piece to be silicon hydrate, aluminum fluoride, potassium fluoroaluminate, sodium fluosilicate and ferric hydroxide which sequentially account for 2.6%, 0.8%, 1.3% and 0.1% of the mass of the measuring test piece;
3) analyzing the reasons of the secondary precipitation substances according to specific substances and contents of the secondary precipitation, and designing the acidification liquid on the basis of the basic acidification liquid:
the amount of the secondary precipitated iron hydroxide generated by the reaction of the basic acidizing fluid and the core sample is very small, the secondary precipitated silicon hydrate, aluminum fluoride, potassium fluoroaluminate and sodium fluosilicate are mainly considered, and the precipitates are generated by the reaction of HF and aluminosilicate, so that the concentration of the HF is reduced and the ratio of the HCl to the HF is increased during the design of the acidizing fluid;
respectively designing 200mL of different acidizing solutions according to the analysis, wherein the mass fractions of HCl and HF in each acidizing solution are respectively 9% HCl + 3% HF, 10% HCl + 2% HF, 10.5% HCl + 1.5% HF, 9% HCl + 1% HF and 12% HCl + 1% HF, namely the mass ratios of HCl to HF in each acidizing solution are respectively 3:1, 5:1, 7:1, 9:1 and 12:1, and complex acid, an anti-swelling agent, an iron ion stabilizer, a surfactant and a corrosion inhibitor are added into each acidizing solution; the mass fraction of the composite acid in the acidizing fluid can be 5-12%, the mass fraction of the anti-swelling agent can be 0.8-3%, the mass fraction of the iron ion stabilizer can be 0.5-2%, the mass fraction of the surfactant can be 0.3-1.5%, and the mass fraction of the corrosion inhibitor can be 0.3-1.5%; specifically, in the embodiment, the compound acid in the acidizing fluid is selected to be acetic acid, the mass fraction of the compound acid is 6%, the anti-swelling agent is ammonium chloride, the mass fraction of the anti-swelling agent is 0.8%, the iron ion stabilizer is citric acid, the mass fraction of the iron ion stabilizer is 0.5%, the surfactant is sodium hexadecyl sulfonate, the mass fraction of the surfactant is 0.7%, and the corrosion inhibitor is benzyl quinoline quaternary ammonium salt, and the mass fraction of the corrosion inhibitor is 0.6%.
Adding 40g of natural rock core into prepared different acidizing fluids, fully reacting for 5h at the oil reservoir temperature, filtering, washing to be neutral, drying at 60 ℃, cooling to room temperature to obtain acid rock reaction residual solid materials corroded by each acidizing fluid, measuring secondary sediment substances and content of each acid rock reaction residual solid material according to the step 2), and determining the type and content of secondary sediment and the change of permeability of the rock core, wherein the change is shown in table 1.
TABLE 1 type, content and effect of secondary precipitation of acidified solutions with different HCl to HF mass ratios
As can be seen from table 1, the larger the mass ratio of HCl to HF and the smaller the HF mass fraction, the smaller the type and content of the secondary precipitated matter, and the greater the improvement in the core permeability. When the mass ratio of HCl to HF is less than 9:1, the total amount of secondary precipitation exceeds 0.5%, the improvement of the permeability of the rock core by acidification is not obvious, the maximum permeability improvement rate is only 18.63%, and the index is lower than the index that the field acidification blockage removal permeability improvement rate is more than or equal to 20%; when the mass ratio of HCl to HF is more than or equal to 9:1, the variety and quantity change of the precipitates tends to be smooth, the variety and quantity of the secondary precipitates are not reduced any more, at the moment, the amount of the precipitates can be controlled to be 0.2 percent, the types of the precipitates are 1, the permeability of the rock core is improved by 146.54 percent, and the permeability is improved obviously; when the mass fraction of HF is more than 1%, the total amount of secondary precipitation is more than 0.5%, and when the mass fraction of HF is 1%, the total amount of secondary precipitation is only 0.2%.
The acidification liquid designed according to the indexes reduces the types of the total precipitation substances from 5 to 1, reduces the total precipitation amount from 6.1% to 0.2%, and better controls the types and the content of secondary precipitation.
Example 2
The design method of the acidizing fluid comprises the following steps:
1) 57.8mL of hydrochloric acid and 13.4mL of hydrofluoric acid are respectively measured and mixed with water to prepare 200mL of conventional basic acidizing fluid of the earth acid.
And then adding 40g of a natural rock core sample (the content of carbonate is more than 10 percent and the content of chlorite is less than 5 percent) into a conventional basic acidizing fluid of the earth acid, fully reacting for 5 hours at the temperature of an oil reservoir, filtering, washing to be neutral, drying at 60 ℃, and cooling to room temperature to obtain the residual solid material of the acid rock reaction.
2) And (2) putting the residual solid material of the acid rock reaction into an agate mortar to be ground into powder with the whole grain diameter of less than 40 mu m, putting the powder into a sample frame, vertically and uniformly compacting and forming to prepare a measurement test piece, putting the measurement test piece into an X-ray diffractometer, and obtaining an X-ray diffraction pattern (shown in figure 2) through measurement to determine that secondary precipitated substances existing in the measurement test piece are calcium fluoride, silicon hydrate, potassium fluoroaluminate and sodium fluosilicate and sequentially account for 1.8%, 2.1%, 1.0% and 1.0% of the mass of the measurement test piece.
3) Analyzing the reasons of the secondary precipitation substances according to specific substances and contents of the secondary precipitation, and designing the acidification liquid on the basis of the basic acidification liquid:
calcium fluoride precipitate in the secondary precipitation of the reaction of the basic acidizing fluid and the natural rock core sample is mainly generated by the reaction of carbonate rock and HF, 5-15% hydrochloric acid can be used as a front acid to pretreat the stratum, dissolve the carbonate rock and prevent the precipitate from being generated.
Respectively designing different acidizing fluids as main acidizing fluids according to the analysis, wherein the mass fractions of HCl and HF in the acidizing fluids are respectively 9% HCl + 3% HF, 10% HCl + 2% HF, 10.5% HCl + 1.5% HF, 9% HCl + 1% HF and 12% HCl + 1% HF, namely the mass ratios of HCl and HF in the acidizing fluids are respectively 3:1, 5:1, 7:1, 9:1 and 12:1, and complex acid, an anti-swelling agent, an iron ion stabilizer, a surfactant and a corrosion inhibitor are added into the acidizing fluids; in each acidizing fluid, the mass fraction of the composite acid is 5-12%, the mass fraction of the anti-swelling agent is 0.8-3%, the mass fraction of the iron ion stabilizer is 0.5-2%, the mass fraction of the surfactant is 0.3-1.5%, and the mass fraction of the corrosion inhibitor is 0.3-1.5%. In this embodiment, the specifically selected complex acid is acetic acid and organic phosphoric acid, the mass fraction of acetic acid is 4%, the mass fraction of organic phosphoric acid is hydroxyethylidene diphosphonic acid (HEDP), and the mass fraction is 1.5%; the anti-swelling agent is potassium chloride, and the mass fraction is 1.2%; the iron ion stabilizer is ethylenediamine tetraacetic acid, and the mass fraction is 0.9%; the surfactant is perfluorooctyl sulfonamide, and the mass fraction is 0.6%; the corrosion inhibitor is benzyl pyridine chloride, and the mass fraction is 0.7%.
Preparing 10% hydrochloric acid according to the above requirements, pretreating a natural rock core sample with high carbonate content (Tg > 10%) and low chlorite content (Tg < 5%), taking 200mL of prepared main acidizing fluid, adding the pretreated natural rock core sample into each main acidizing fluid, fully reacting for 5h at the oil reservoir temperature, filtering, washing to neutrality, drying at the temperature of not higher than 60 ℃, and cooling to room temperature to obtain the acid rock reaction residual solid material.
And then measuring secondary precipitation substances and contents in the obtained residual solid materials of the acid rock reaction according to the step 2), determining that the secondary precipitation type is potassium fluoroaluminate when the mass ratio of HCl to HF in the acidizing fluid is 9:1 and the mass fraction of HF is not more than 1%, reducing the types of the precipitation substances from 4 to 1, reducing the total precipitation amount from 5.9% to 0.2%, and changing the core permeability improvement rate from-62.43% to 157.65%.
Example 3
The method of designing an acidizing fluid of embodiment 3 includes the steps of:
1) 57.8mL of hydrofluoric acid and 13.4mL of hydrofluoric acid are respectively weighed and mixed with water to prepare 200mL of conventional alkaline earth acid basic acidizing fluid.
And then adding 40g of a natural core sample (the chlorite content is more than or equal to 5%) into the conventional earth acid basic acidizing fluid, fully reacting for 5 hours at the oil reservoir temperature, filtering, washing to be neutral, drying at 60 ℃, and cooling to room temperature to obtain the residual solid material of the acid-rock reaction.
2) And (2) putting the residual solid material of the acid rock reaction into an agate mortar to be ground into powder with the whole grain diameter of less than 40 mu m, putting the powder into a sample frame, vertically and uniformly compacting and forming to prepare a measurement test piece, putting the measurement test piece into an X-ray diffractometer, and obtaining an X-ray diffraction spectrum (shown in figure 3) through measurement to determine that secondary precipitated substances existing in the measurement test piece are silicon hydrate, potassium fluoroaluminate, sodium fluosilicate and ferric hydroxide and sequentially account for 2.5%, 1.4% and 0.7% of the mass of the measurement test piece.
3) Analyzing the reason for the generation of the precipitate according to the specific substance and content of the secondary precipitate, wherein the ferric hydroxide is mainly dissolved in iron-containing minerals such as chlorite and the like in the stratum, and when the acidizing fluid is consumed to have a pH value of more than 2, ferric ions are precipitated in a ferric hydroxide form, so that the pH value of residual acid is controlled to be less than or equal to 2 by adding complex acid during the design of the acidizing fluid, and the generation of the residual acid is controlled by adding a ferric ion stabilizer to ensure that the capacity of stabilizing the ferric ions is greater than or equal to 90 mg/L.
Different acidizing solutions are designed according to the analysis, the mass fractions of HCl and HF in each acidizing solution are respectively 9% HCl + 3% HF, 10% HCl + 2% HF, 10.5% HCl + 1.5% HF, 9% HCl + 1% HF and 12% HCl + 1% HF, a complex acid, an anti-swelling agent, an iron ion stabilizer, a surfactant and a corrosion inhibitor are added into each acidizing solution, the complex acid in each acidizing solution is controlled to be acetic acid and phosphoric acid, the mass fraction of the acetic acid is 4.5%, the mass fraction of the phosphoric acid is 3%, the iron ion stabilizer is nitrilotriacetic acid, the mass fraction is 0.5%, the anti-swelling agent is ammonium chloride, the mass fraction is 1.5%, the corrosion inhibitor is dodecyl pyridine bromide, the mass fraction is 1.0%, the surfactant is perfluoroalkyl acrylate, and the mass fraction is 0.3%.
Adding 40g of natural rock core into prepared different acidizing fluids, fully reacting for 5h at the oil reservoir temperature, filtering, washing to be neutral, drying at 60 ℃, cooling to room temperature to obtain acid rock reaction residual solid materials corroded by each acidizing fluid, and then determining secondary precipitate substances and content of each acid rock reaction residual solid material according to the step 2). When the mass ratio of HCl to HF in the acidizing fluid is 9:1 and the mass fraction of HF is not more than 1%, the secondary precipitation type is hydrated silicon, the content is 0.2%, the types of precipitation substances are reduced from 4 to 1, the total precipitation amount is reduced from 6.0% to 0.2%, and the increase rate of the permeability of the core is changed from-47.93% to 153.26%.
With reference to examples 1 to 3, when the secondary precipitate contains at least one of silicon hydrate, aluminum hydroxide, aluminum fluoride, sodium fluorosilicate, potassium fluorosilicate, calcium fluorosilicate, sodium fluoroaluminate and potassium fluoroaluminate, the mass ratio of HCl to HF in the acidizing fluid needs to be controlled to be not less than 9:1, and the mass fraction of HF is not more than 1%; when the secondary precipitation contains at least one of calcium fluoride and magnesium fluoride, a pre-acid is required to be arranged, and the pre-acid is hydrochloric acid with the mass fraction of 5-15%; when the secondary precipitation contains ferric hydroxide, complex acid is added into acidizing fluid (when pre-acid is needed, the acidizing fluid is main acid) to control the pH value of residual acid to be less than or equal to 2, and an iron ion stabilizing agent is added to ensure that the iron ion stabilizing capacity is greater than or equal to 90 mg/mL.
In example 4 of the method for designing an acidified liquid of the present invention, only the differences from example 3 were: the added complex acid is formic acid, and the mass fraction of the formic acid in the acidizing fluid is 5%; the added anti-swelling agent is organic silicon, and the mass fraction is 3%; the mass fraction of the added iron ion stabilizer is 2 percent; the added surfactant is sodium alkyl benzene sulfonate, and the mass fraction is 1.5%; the added corrosion inhibitor is urotropin with the mass fraction of 1.5%.
In other embodiments of the method for designing an acidified liquid according to the invention, the difference from embodiment 3 is only that: the mass fraction of the added surfactant was 0.3%.
The acidified liquid designed in the embodiment 4 and other embodiments of the method for designing acidified liquid can also effectively reduce the types and the amount of secondary precipitated substances.
Comparative example
According to the article of 'analysis of influence factors of hydrated silicon precipitation in sandstone acidification', 10g of kaolin is added into a 9.0% hydrochloric acid + 3.0% hydrofluoric acid system at 60 ℃, and the concentration of soluble silicon in each solution is measured by using a plasma absorption spectrometry method to obtain the productThe secondary precipitation type after 5h of reaction is silicon hydrate, the content is 2.3 percent, and the design method of the acidizing fluid is to reduce the concentration of hydrofluoric acid. Designing acidizing fluid according to a method in the literature, adopting a rock core which is the same as that in the example 3 to fully react with the acidizing fluid for 5 hours, treating a sample, putting the treated sample into an X-ray diffractometer, and determining that the type of the secondary sedimentation is H through measurement4SiO4And Fe (OH)3The secondary precipitation amounts were 0.2% and 0.6%, respectively, the permeability improvement rate of the acid rock reaction residual solid material was 17.83%, the secondary precipitation amount was higher than 0.2% in example 3, and the permeability improvement rate was much lower than 153.26% in example 3.
Claims (6)
1. A design method of acidizing fluid is characterized by comprising the following steps: the method comprises the following steps:
1) fully reacting a conventional earth acid basic acidizing fluid consisting of hydrochloric acid and hydrofluoric acid with a natural rock core at an oil reservoir temperature, carrying out solid-liquid separation, washing a solid to be neutral, and drying at the temperature of not higher than 60 ℃ to obtain an acid rock reaction residual solid material;
2) determining the type and content of secondary precipitated substances in the obtained acid rock reaction residual solid material;
3) and analyzing the reason of generating the precipitate according to the type and the content of the measured secondary precipitate substances, and designing the acidizing fluid on the basis of the conventional alkaline earth acid basic acidizing fluid.
2. The method of designing an acidizing fluid, as recited in claim 1 wherein: in step 3), the method for designing the acidizing fluid comprises the following steps: and (3) replacing the conventional alkaline earth acid basic acidizing fluid in the step 1) after adjusting the mass ratio of HCl to HF in the conventional alkaline earth acid basic acidizing fluid, and repeating the step 1) and the step 2) to determine the concentrations of HCl and HF meeting the acidizing requirements.
3. The method of designing an acidizing fluid, as set forth in claim 2, characterized in that: in step 3), the method for designing the acidizing fluid further comprises the following steps: adding complex acid after adjusting the mass ratio of HCl to HF in the conventional alkaline earth acid basic acidizing fluid; the complex acid is at least one of formic acid, acetic acid, phosphoric acid and organic phosphoric acid.
4. The method of designing an acidizing fluid, as set forth in claim 2, characterized in that: in step 3), the method for designing the acidizing fluid further comprises the following steps: adding an additive after adjusting the mass ratio of HCl to HF in the conventional alkaline earth acid basic acidizing fluid; the additive comprises an iron ion stabilizer, an anti-swelling agent, a surfactant and a corrosion inhibitor.
5. The method for designing an acidizing fluid according to any one of the claims 1 to 4, which is characterized by comprising the following steps: in the step 2), the method for measuring the secondary precipitated substances and the content of the secondary precipitated substances in the obtained solid comprises the following steps: and preparing the obtained solid material into powder, pressing the powder into a measuring test piece, and measuring secondary sediment substances and content in the measuring test piece by adopting an X-ray diffraction method.
6. The method of designing an acidizing fluid, as recited in claim 5 wherein: the particle size of the powder is not more than 40 μm.
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