CN118995187B - A kind of non-flowback acidification working fluid and its preparation method and construction process - Google Patents
A kind of non-flowback acidification working fluid and its preparation method and construction process Download PDFInfo
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- 239000012530 fluid Substances 0.000 title claims abstract description 28
- 238000002360 preparation method Methods 0.000 title claims abstract description 27
- 238000000034 method Methods 0.000 title claims abstract description 15
- 230000008569 process Effects 0.000 title claims abstract description 11
- 238000010276 construction Methods 0.000 title claims abstract description 10
- 230000020477 pH reduction Effects 0.000 title claims description 31
- 239000002253 acid Substances 0.000 claims abstract description 77
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims abstract description 50
- 239000002131 composite material Substances 0.000 claims abstract description 40
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 37
- 239000004094 surface-active agent Substances 0.000 claims abstract description 30
- 125000002091 cationic group Chemical group 0.000 claims abstract description 27
- 150000007524 organic acids Chemical class 0.000 claims abstract description 10
- 239000003129 oil well Substances 0.000 claims abstract description 5
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 claims description 68
- JVTAAEKCZFNVCJ-UHFFFAOYSA-N lactic acid Chemical compound CC(O)C(O)=O JVTAAEKCZFNVCJ-UHFFFAOYSA-N 0.000 claims description 54
- 239000000243 solution Substances 0.000 claims description 52
- RGHNJXZEOKUKBD-SQOUGZDYSA-N D-gluconic acid Chemical compound OC[C@@H](O)[C@@H](O)[C@H](O)[C@@H](O)C(O)=O RGHNJXZEOKUKBD-SQOUGZDYSA-N 0.000 claims description 44
- 229910000147 aluminium phosphate Inorganic materials 0.000 claims description 34
- 229920000642 polymer Polymers 0.000 claims description 34
- RGHNJXZEOKUKBD-UHFFFAOYSA-N D-gluconic acid Natural products OCC(O)C(O)C(O)C(O)C(O)=O RGHNJXZEOKUKBD-UHFFFAOYSA-N 0.000 claims description 27
- 239000000174 gluconic acid Substances 0.000 claims description 27
- 235000012208 gluconic acid Nutrition 0.000 claims description 27
- 239000004310 lactic acid Substances 0.000 claims description 27
- 235000014655 lactic acid Nutrition 0.000 claims description 27
- 238000003756 stirring Methods 0.000 claims description 26
- 239000007788 liquid Substances 0.000 claims description 25
- ROOXNKNUYICQNP-UHFFFAOYSA-N ammonium persulfate Chemical compound [NH4+].[NH4+].[O-]S(=O)(=O)OOS([O-])(=O)=O ROOXNKNUYICQNP-UHFFFAOYSA-N 0.000 claims description 24
- 239000000178 monomer Substances 0.000 claims description 21
- SMZOUWXMTYCWNB-UHFFFAOYSA-N 2-(2-methoxy-5-methylphenyl)ethanamine Chemical compound COC1=CC=C(C)C=C1CCN SMZOUWXMTYCWNB-UHFFFAOYSA-N 0.000 claims description 20
- NIXOWILDQLNWCW-UHFFFAOYSA-N 2-Propenoic acid Natural products OC(=O)C=C NIXOWILDQLNWCW-UHFFFAOYSA-N 0.000 claims description 20
- YOKDQEBPBYOXHX-UHFFFAOYSA-N prop-1-en-2-ylphosphonic acid Chemical compound CC(=C)P(O)(O)=O YOKDQEBPBYOXHX-UHFFFAOYSA-N 0.000 claims description 19
- 239000012224 working solution Substances 0.000 claims description 17
- AEQDJSLRWYMAQI-UHFFFAOYSA-N 2,3,9,10-tetramethoxy-6,8,13,13a-tetrahydro-5H-isoquinolino[2,1-b]isoquinoline Chemical compound C1CN2CC(C(=C(OC)C=C3)OC)=C3CC2C2=C1C=C(OC)C(OC)=C2 AEQDJSLRWYMAQI-UHFFFAOYSA-N 0.000 claims description 14
- DUIOKRXOKLLURE-UHFFFAOYSA-N 2-octylphenol Chemical compound CCCCCCCCC1=CC=CC=C1O DUIOKRXOKLLURE-UHFFFAOYSA-N 0.000 claims description 14
- 238000006243 chemical reaction Methods 0.000 claims description 14
- 239000000203 mixture Substances 0.000 claims description 14
- 229940051841 polyoxyethylene ether Drugs 0.000 claims description 14
- 229920000056 polyoxyethylene ether Polymers 0.000 claims description 14
- 239000000176 sodium gluconate Substances 0.000 claims description 14
- 235000012207 sodium gluconate Nutrition 0.000 claims description 14
- 229940005574 sodium gluconate Drugs 0.000 claims description 14
- 229910001870 ammonium persulfate Inorganic materials 0.000 claims description 12
- 239000007864 aqueous solution Substances 0.000 claims description 12
- 238000001816 cooling Methods 0.000 claims description 12
- 238000010438 heat treatment Methods 0.000 claims description 12
- 150000001875 compounds Chemical class 0.000 claims description 9
- 238000007865 diluting Methods 0.000 claims description 6
- 238000012360 testing method Methods 0.000 claims description 2
- 125000001449 isopropyl group Chemical group [H]C([H])([H])C([H])(*)C([H])([H])[H] 0.000 claims 1
- 230000000694 effects Effects 0.000 abstract description 15
- 230000000979 retarding effect Effects 0.000 abstract description 7
- 239000000693 micelle Substances 0.000 abstract description 4
- 239000010779 crude oil Substances 0.000 abstract description 3
- 238000004519 manufacturing process Methods 0.000 abstract description 3
- 238000005516 engineering process Methods 0.000 abstract 1
- 239000000126 substance Substances 0.000 abstract 1
- 230000000052 comparative effect Effects 0.000 description 10
- 230000001965 increasing effect Effects 0.000 description 5
- KRHYYFGTRYWZRS-UHFFFAOYSA-N Fluorane Chemical compound F KRHYYFGTRYWZRS-UHFFFAOYSA-N 0.000 description 4
- 238000011156 evaluation Methods 0.000 description 4
- -1 hydrogen ions Chemical class 0.000 description 4
- 239000003921 oil Substances 0.000 description 4
- 239000002994 raw material Substances 0.000 description 4
- IHBVNSPHKMCPST-UHFFFAOYSA-N 3-bromopropanoyl chloride Chemical compound ClC(=O)CCBr IHBVNSPHKMCPST-UHFFFAOYSA-N 0.000 description 3
- XEKOWRVHYACXOJ-UHFFFAOYSA-N Ethyl acetate Chemical compound CCOC(C)=O XEKOWRVHYACXOJ-UHFFFAOYSA-N 0.000 description 3
- 230000007797 corrosion Effects 0.000 description 3
- 238000005260 corrosion Methods 0.000 description 3
- 229910052739 hydrogen Inorganic materials 0.000 description 3
- 239000001257 hydrogen Substances 0.000 description 3
- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 3
- 238000002347 injection Methods 0.000 description 3
- 239000007924 injection Substances 0.000 description 3
- 239000000463 material Substances 0.000 description 3
- 238000001556 precipitation Methods 0.000 description 3
- 239000000047 product Substances 0.000 description 3
- LXAHHHIGZXPRKQ-UHFFFAOYSA-N 5-fluoro-2-methylpyridine Chemical compound CC1=CC=C(F)C=N1 LXAHHHIGZXPRKQ-UHFFFAOYSA-N 0.000 description 2
- BVKZGUZCCUSVTD-UHFFFAOYSA-L Carbonate Chemical compound [O-]C([O-])=O BVKZGUZCCUSVTD-UHFFFAOYSA-L 0.000 description 2
- 102000004190 Enzymes Human genes 0.000 description 2
- 108090000790 Enzymes Proteins 0.000 description 2
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 2
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 description 2
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 description 2
- 150000007513 acids Chemical class 0.000 description 2
- 230000009471 action Effects 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 2
- 150000001768 cations Chemical class 0.000 description 2
- 238000004140 cleaning Methods 0.000 description 2
- 230000001276 controlling effect Effects 0.000 description 2
- 230000003628 erosive effect Effects 0.000 description 2
- 238000002474 experimental method Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 239000002245 particle Substances 0.000 description 2
- 230000035699 permeability Effects 0.000 description 2
- 239000011148 porous material Substances 0.000 description 2
- 230000001105 regulatory effect Effects 0.000 description 2
- 239000011435 rock Substances 0.000 description 2
- 239000002904 solvent Substances 0.000 description 2
- 239000012086 standard solution Substances 0.000 description 2
- BHPQYMZQTOCNFJ-UHFFFAOYSA-N Calcium cation Chemical compound [Ca+2] BHPQYMZQTOCNFJ-UHFFFAOYSA-N 0.000 description 1
- DBMJMQXJHONAFJ-UHFFFAOYSA-M Sodium laurylsulphate Chemical group [Na+].CCCCCCCCCCCCOS([O-])(=O)=O DBMJMQXJHONAFJ-UHFFFAOYSA-M 0.000 description 1
- 150000001408 amides Chemical class 0.000 description 1
- 229910001424 calcium ion Inorganic materials 0.000 description 1
- 229940041131 calcium lactate gluconate Drugs 0.000 description 1
- PWKNEBQRTUXXLT-ZBHRUSISSA-L calcium lactate gluconate Chemical compound [Ca+2].CC(O)C([O-])=O.OC[C@@H](O)[C@@H](O)[C@H](O)[C@@H](O)C([O-])=O PWKNEBQRTUXXLT-ZBHRUSISSA-L 0.000 description 1
- 125000005587 carbonate group Chemical group 0.000 description 1
- 150000007942 carboxylates Chemical class 0.000 description 1
- 125000002843 carboxylic acid group Chemical group 0.000 description 1
- 239000007795 chemical reaction product Substances 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- OEYIOHPDSNJKLS-UHFFFAOYSA-N choline Chemical compound C[N+](C)(C)CCO OEYIOHPDSNJKLS-UHFFFAOYSA-N 0.000 description 1
- 229960001231 choline Drugs 0.000 description 1
- 239000004927 clay Substances 0.000 description 1
- 239000008139 complexing agent Substances 0.000 description 1
- 235000014113 dietary fatty acids Nutrition 0.000 description 1
- JRBPAEWTRLWTQC-UHFFFAOYSA-N dodecylamine Chemical compound CCCCCCCCCCCCN JRBPAEWTRLWTQC-UHFFFAOYSA-N 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 238000001704 evaporation Methods 0.000 description 1
- 238000000605 extraction Methods 0.000 description 1
- 239000000194 fatty acid Substances 0.000 description 1
- 229930195729 fatty acid Natural products 0.000 description 1
- 150000004665 fatty acids Chemical class 0.000 description 1
- 125000001153 fluoro group Chemical class F* 0.000 description 1
- 238000005213 imbibition Methods 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 229910052500 inorganic mineral Inorganic materials 0.000 description 1
- 239000013067 intermediate product Substances 0.000 description 1
- 230000007246 mechanism Effects 0.000 description 1
- 229910021645 metal ion Inorganic materials 0.000 description 1
- 230000000813 microbial effect Effects 0.000 description 1
- 235000010755 mineral Nutrition 0.000 description 1
- 239000011707 mineral Substances 0.000 description 1
- 239000012046 mixed solvent Substances 0.000 description 1
- 231100000252 nontoxic Toxicity 0.000 description 1
- 230000003000 nontoxic effect Effects 0.000 description 1
- FATBGEAMYMYZAF-KTKRTIGZSA-N oleamide Chemical compound CCCCCCCC\C=C/CCCCCCCC(N)=O FATBGEAMYMYZAF-KTKRTIGZSA-N 0.000 description 1
- FATBGEAMYMYZAF-UHFFFAOYSA-N oleicacidamide-heptaglycolether Natural products CCCCCCCCC=CCCCCCCCC(N)=O FATBGEAMYMYZAF-UHFFFAOYSA-N 0.000 description 1
- 238000004080 punching Methods 0.000 description 1
- 238000011084 recovery Methods 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 229910000029 sodium carbonate Inorganic materials 0.000 description 1
- 230000000638 stimulation Effects 0.000 description 1
- 230000002195 synergetic effect Effects 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
- C09K8/60—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
- C09K8/74—Eroding chemicals, e.g. acids combined with additives added for specific purposes
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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
- C09K8/58—Compositions for enhanced recovery methods for obtaining hydrocarbons, i.e. for improving the mobility of the oil, e.g. displacing fluids
- C09K8/588—Compositions for enhanced recovery methods for obtaining hydrocarbons, i.e. for improving the mobility of the oil, e.g. displacing fluids characterised by the use of specific polymers
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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
- E21B43/25—Methods for stimulating production
- E21B43/26—Methods for stimulating production by forming crevices or fractures
- E21B43/27—Methods for stimulating production by forming crevices or fractures by use of eroding chemicals, e.g. acids
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- Materials Engineering (AREA)
- Organic Chemistry (AREA)
- Physics & Mathematics (AREA)
- Environmental & Geological Engineering (AREA)
- Fluid Mechanics (AREA)
- Geochemistry & Mineralogy (AREA)
- Oil, Petroleum & Natural Gas (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
本申请公开了一种无返排酸化工作液及其制备方法与施工工艺，属于油田化学技术领域。该无返排酸化工作液包括前处理液和复合酸液，前处理液与复合酸液的体积比为1：（2~10）；复合酸液包括有机酸、盐酸和阳离子双子表面活性剂；按照重量百分比，复合酸液包括15~25%的有机酸、1%~3%的盐酸、0.2%~1%的阳离子双子表面活性剂，余量为水。前处理液对油井的套管进行清洗和保护，溶解储层表面的原油和有机垢；将有机酸、盐酸和阳离子双子表面活性剂复配得到复合酸液，将有机酸与盐酸配合作用，提高缓速性能，配合阳离子双子表面活性剂，其具备更强的表面活性和界面活性，更容易形成胶束，增产效果好。The present application discloses a non-flowback acidizing working fluid and its preparation method and construction process, which belongs to the field of oilfield chemical technology. The non-flowback acidizing working fluid includes a pretreatment fluid and a composite acid fluid, and the volume ratio of the pretreatment fluid to the composite acid fluid is 1: (2~10); the composite acid fluid includes an organic acid, hydrochloric acid and a cationic gemini surfactant; in terms of weight percentage, the composite acid fluid includes 15~25% of an organic acid, 1%~3% of hydrochloric acid, 0.2%~1% of a cationic gemini surfactant, and the remainder is water. The pretreatment fluid cleans and protects the casing of the oil well, dissolves the crude oil and organic scale on the surface of the reservoir; the organic acid, hydrochloric acid and the cationic gemini surfactant are compounded to obtain the composite acid fluid, and the organic acid is combined with the hydrochloric acid to improve the retarding performance, and the cationic gemini surfactant is combined, so that it has stronger surface activity and interfacial activity, is easier to form micelles, and has a good production increase effect.
Description
Technical Field
The application relates to a flowback-free acidification working solution and a preparation method and a construction process thereof, belonging to the technical field of oilfield chemistry.
Background
Acidification is one of the main measures of increasing production and injection of an oil-water well at present, and acid liquor is injected into a reservoir, so that the acid liquor, reservoir minerals and clay undergo corrosion reaction, the damage of the reservoir is relieved, the permeability of the reservoir is recovered, and the injection capacity and the liquid production capacity are improved. The conventional earth acid liquid system is mixed acid of hydrochloric acid and hydrofluoric acid, the acid liquid and sandstone react at an excessively high speed, so that the acidification effect is poor, the conventional acidification also has the problem that the effect is poor year by year, the residual acid is easy to form secondary precipitation, the reservoir is seriously damaged, and the acidification effect is limited to a great extent.
In order to obtain the acid liquor with excellent performance, retarded acid systems such as fluorine salt autogenous acid, fluoboric acid, organic earth acid, phosphoric acid, polyhydrogen acid and the like are developed from the viewpoint of reducing the acid liquor reaction rate, and chelating acid systems are developed from the viewpoint of reducing the precipitation damage of reaction products. However, in the acidification construction, the residual acid of the acid solution is not environment-friendly and can not be degraded.
Chinese patent CN 112143479A discloses a low permeability oil reservoir water injection well no-flowback punching acidification system and a preparation method, wherein a metal ion complexing agent is adopted, no flowback is required after acidification, but the main acid liquor is not environment-friendly enough and has the problem of too fast reaction rate due to the adoption of traditional hydrochloric acid and hydrofluoric acid, and the acid liquor can not keep the acid liquor activity for a long time.
Disclosure of Invention
In order to solve the problems, the flowback-free acidification working solution, the preparation method and the construction process thereof are provided, wherein the pretreatment solution and the composite acid solution are arranged, the pretreatment solution is used for cleaning and protecting a sleeve of an oil well, crude oil and organic scale on the surface of a reservoir are dissolved, the organic acid, hydrochloric acid and a cationic gemini surfactant are compounded to obtain the composite acid solution, the reaction rate is further regulated and controlled, the retarding performance is improved, the cationic gemini surfactant is matched, the composite acid solution has stronger surface activity and interfacial activity, micelles are easier to form, the composite acid solution firstly enters a hypertonic zone or a crack, the cationic gemini surfactant becomes viscous to prevent the acid solution from continuously entering a hypertonic pore canal along with the progress of the reaction, and the fresh acid continuously penetrates to the deep part and turns to a hypotonic layer to perform yield increasing treatment.
According to one aspect of the application, the flowback-free acidification working solution comprises a pretreatment solution and a compound acid solution, wherein the volume ratio of the pretreatment solution to the compound acid solution is 1 (2-10), the compound acid solution comprises organic acid, hydrochloric acid and cationic gemini surfactant, and the compound acid solution comprises, by weight, 15-25% of organic acid, 1-3% of hydrochloric acid, 0.2-1% of cationic gemini surfactant and the balance of water.
Optionally, according to weight percentage, the organic acid comprises a mixture of lactic acid and gluconic acid and an organic phosphoric acid polymer, wherein the mixture of lactic acid and gluconic acid accounts for 10-15% of the composite acid liquid, the organic phosphoric acid polymer accounts for 5-10% of the composite acid liquid, the pretreatment liquid comprises 5-12% of octyl phenol polyoxyethylene ether, 2-7% of sodium gluconate and the balance of water.
Optionally, the volume ratio of the pretreatment liquid to the composite acid liquid is 1:2-4.
Optionally, the molar ratio of the lactic acid to the gluconic acid is 1-2:1-1.5.
Optionally, the organic phosphoric acid polymer is polymerized by isopropenyl phosphonic acid monomer and acrylic acid.
Optionally, the preparation process of the organic phosphoric acid polymer comprises the following steps:
(1) Diluting the isopropenyl phosphonic acid monomer with water to 50% aqueous solution, and heating to 70-80 ℃;
(2) And (3) dropwise adding the mixture of ammonium persulfate and acrylic acid into the aqueous solution, and continuing the reaction to obtain the organic phosphoric acid polymer.
Optionally, the mol ratio of the isopropenyl phosphonic acid monomer to the acrylic acid is 1-1.2:1, and the dosage of the ammonium persulfate is 15-20% of the isopropenyl phosphonic acid monomer to the acrylic acid.
Optionally, the cationic gemini surfactant has a formula of formula (1):
formula (1).
According to another aspect of the application, the application also discloses a preparation method of the flowback-free acidification working solution, which comprises the following steps:
(1) The preparation of pretreatment liquid comprises adding sodium gluconate into water, stirring at room temperature for 5-10min, adding octyl phenol polyoxyethylene ether, heating to 35-40deg.C, stirring for 20-25min, and naturally cooling to room temperature to obtain pretreatment liquid;
(2) The preparation method of the composite acid liquor comprises the steps of sequentially adding lactic acid, gluconic acid, organic phosphoric acid polymer and hydrochloric acid into water, stirring for 20-25min at 35-40 ℃, naturally cooling to room temperature, adding a cationic gemini surfactant, and stirring for 10-20min to obtain the composite acid liquor.
According to still another aspect of the application, the application also discloses a construction process of the flowback-free acidification working solution, which comprises the following steps:
(1) Injecting pretreatment liquid into the oil sleeve annulus of the test oil well;
(2) Injecting the compound acid solution after 3-5h, and closing the well after injecting the compound acid solution for 24-72h.
The beneficial effects of the application include, but are not limited to:
1. According to the flowback-free acidification working solution, octyl phenol polyoxyethylene ether, sodium gluconate and water are compounded to obtain a pretreatment solution, the pretreatment solution is used for cleaning and protecting a sleeve of an oil well under the combined action of the octyl phenol polyoxyethylene ether, sodium gluconate and water to dissolve crude oil and organic scale on the surface of a reservoir, lactic acid, gluconic acid, an organic phosphoric acid polymer, hydrochloric acid and a cationic gemini surfactant are compounded to obtain a composite acid solution, the four kinds of coordination effects of lactic acid, gluconic acid, organic phosphoric acid polymer and hydrochloric acid are used for further regulating and controlling the reaction rate, improving the retarding performance, and the cationic gemini surfactant is matched with the pretreatment solution, so that the pretreatment solution has stronger surface activity and interfacial activity and is easier to form micelles, the composite acid solution firstly enters a hypertonic zone or a crack, the cationic gemini surfactant becomes viscous to prevent the acid solution from continuously entering a hypertonic pore canal along with the progress of the reaction, and fresh acid continuously penetrates into a deep part and turns to a low-permeability layer to perform yield increasing treatment.
2. According to the flowback-free acidification working solution, the components of the composite acid solution are compounded according to a specific proportion, lactic acid and gluconic acid are used as main acids, protons of carboxylic acid groups in the lactic acid and the gluconic acid are replaced by cations to generate carboxylate, degradable calcium lactate gluconate with larger solubility is generated in the acidification process, secondary precipitation is avoided, the lactic acid and the gluconic acid are environment-friendly, hydrochloric acid, an organic phosphoric acid polymer and the lactic acid gluconic acid are compounded, the acidification effect is improved, meanwhile, the retarding performance is improved, the hydrochloric acid is a monobasic strong acid, hydrogen ions are in all ionization states, and the hydrogen ions in the organic phosphoric acid polymer are slowly released and have the characteristic of multistage ionization, so that four acids are compounded to realize synergistic effect, the acidification effect, the retarding performance and the environment friendliness.
3. According to the flowback-free acidification working solution, a specific cationic gemini surfactant is adopted, the surfactant contains hydroxyl C3 and single-chain oleamide, hydroxyl functional groups are introduced, electrostatic repulsion between 2 cations can be reduced through hydrogen bonding of the hydroxyl groups, and water solubility of molecules is enhanced, so that the flowback-free acidification working solution has better interfacial activity and is easier to form a compact micelle structure, and the gemini surfactant containing amide has excellent biodegradability and can be hydrolyzed into nontoxic fatty acid and choline by enzymes under the action of environmental microbial enzymes without recovery.
4. According to the preparation method and the construction process of the flowback-free acidification working solution, the preparation method and the construction process are simple, easy to operate, environment-friendly and beneficial to large-scale popularization.
Detailed Description
The present application is described in detail below with reference to examples, but the present application is not limited to these examples.
Unless defined otherwise, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art. The reagents or materials used in the present invention may be purchased in conventional manners, and unless otherwise indicated, they may be used in conventional manners in the art or according to the product specifications. In addition, any methods and materials similar or equivalent to those described herein can be used in the methods of the present invention. The preferred methods and materials described in this patent are illustrative only.
In the following examples and comparative examples, the cationic gemini surfactants involved are prepared by referring to prior art literature Huang Feifei. Dense oil reservoir no-flowback fracturing fluid system and imbibition oil extraction mechanism research [ D ]. Chinese oil university (Huadong), the specific preparation method comprises the following steps:
(1) 20g of laurylamine and 3g of sodium carbonate were dissolved in a three-necked flask containing 300ml of DMF;
(2) 21g of 3-bromopropionyl chloride was diluted with 100 mM LDMF;
(3) Slowly dripping the component (2) into the component (1) under stirring at 150rpm, and controlling the dripping speed to ensure that the temperature of the system is not higher than 45 ℃;
(4) Continuously stirring and reacting for 1h after the 3-bromopropionyl chloride solution is added dropwise, transferring the reacted solution into a rotary evaporator, evaporating in vacuum at 90 ℃ to remove the solvent and the residual bromopropionyl chloride, and separating to obtain an intermediate product 3-bromo-N-dodecylpropionamide (3-bromo-N-dodecylpropanamide);
(5) 300ml of isopropanol is added into a three-neck flask fixed in a water bath kettle, 6.5g of 1, 3-bis (dimethylamino) propanediol and the product obtained in the step (4) are added into the three-neck flask, and the three-neck flask is stirred and refluxed for 15 hours at the rotation speed of 30rpm and the temperature of 60 ℃;
(6) The solvent was removed from the solution after the reaction in (5) in a rotary evaporator at 90℃and the product was recrystallized 2 times from a mixed solvent of ethyl acetate and ethanol (20:1) and dried at 60℃for 24 hours.
Example 1 no flowback acidizing fluid 1#
(1) Preparation of the organic phosphoric acid polymer:
diluting the isopropenyl phosphonic acid monomer with water to 50% aqueous solution, heating to 70 ℃, dripping the mixture of ammonium persulfate and acrylic acid into the aqueous solution, wherein the mol ratio of the isopropenyl phosphonic acid monomer to the acrylic acid is 1:1, the dosage of the ammonium persulfate is 15% of that of the isopropenyl phosphonic acid monomer and the acrylic acid, and continuing to react to obtain the organic phosphoric acid polymer.
(2) Preparing raw materials, namely preparing a mixture of 5% of octyl phenol polyoxyethylene ether, 2% of sodium gluconate, 10% of lactic acid and gluconic acid, and the balance of water according to the weight percentage, wherein the molar ratio of the lactic acid to the gluconic acid is 1:1,5% of organic phosphoric acid polymer, 1% of hydrochloric acid, 0.2% of cationic gemini surfactant and the balance of water;
(3) Preparation of pretreatment liquid:
adding sodium gluconate into water, stirring at normal temperature for 5min, adding octyl phenol polyoxyethylene ether, heating to 35 ℃, stirring for 20min, and naturally cooling to room temperature to obtain pretreatment liquid;
(4) Preparation of composite acid liquor:
Sequentially adding lactic acid, gluconic acid, an organic phosphoric acid polymer and hydrochloric acid into water, stirring for 20min at 35 ℃, naturally cooling to room temperature, adding a cationic gemini surfactant, and stirring for 10min to obtain a composite acid solution, wherein the volume ratio of the pretreatment solution to the composite acid solution is 1:1, and obtaining the flowback-free acidification working solution No. 1.
EXAMPLE 2 no flowback acidizing fluid 2#
(1) Preparation of the organic phosphoric acid polymer:
Diluting the isopropenyl phosphonic acid monomer with water to 50% aqueous solution, heating to 80 ℃, dripping a mixture of ammonium persulfate and acrylic acid into the aqueous solution, wherein the mol ratio of the isopropenyl phosphonic acid monomer to the acrylic acid is 1.2:1, the dosage of the ammonium persulfate is 20% of that of the isopropenyl phosphonic acid monomer and the acrylic acid, and continuously reacting to obtain the organic phosphoric acid polymer.
(2) Preparing raw materials, namely preparing a mixture of 12% of octyl phenol polyoxyethylene ether, 7% of sodium gluconate, 15% of lactic acid and gluconic acid, and the balance of water according to the weight percentage, wherein the molar ratio of the lactic acid to the gluconic acid is 2:1,10% of organic phosphoric acid polymer, 3% of hydrochloric acid, 1% of cationic gemini surfactant and the balance of water;
(3) Preparation of pretreatment liquid:
Adding sodium gluconate into water, stirring at normal temperature for 10min, adding octyl phenol polyoxyethylene ether, heating to 40 ℃, stirring for 25min, and naturally cooling to room temperature to obtain pretreatment liquid;
(4) Preparation of composite acid liquor:
Sequentially adding lactic acid, gluconic acid, an organic phosphoric acid polymer and hydrochloric acid into water, stirring for 25min at 40 ℃, naturally cooling to room temperature, adding a cationic gemini surfactant, and stirring for 20min to obtain a composite acid solution, wherein the volume ratio of the pretreatment solution to the composite acid solution is 1:4, and obtaining the flowback-free acidification working solution No. 2.
Example 3 no flowback acidizing fluid 3#
(1) Preparation of the organic phosphoric acid polymer:
Diluting the isopropenyl phosphonic acid monomer with water to 50% aqueous solution, heating to 75 ℃, dripping a mixture of ammonium persulfate and acrylic acid into the aqueous solution, wherein the molar ratio of the isopropenyl phosphonic acid monomer to the acrylic acid is 1.1:1, the dosage of the ammonium persulfate is 18% of that of the isopropenyl phosphonic acid monomer and the acrylic acid, and continuously reacting to obtain the organic phosphoric acid polymer.
(2) Preparing raw materials, namely preparing a mixture of 8% of octyl phenol polyoxyethylene ether, 5% of sodium gluconate, 12% of lactic acid and gluconic acid, and the balance of water according to the weight percentage, wherein the molar ratio of the lactic acid to the gluconic acid is 1:1.5,8% of organic phosphoric acid polymer, 2% of hydrochloric acid, 0.5% of cationic gemini surfactant and the balance of water;
(3) Preparation of pretreatment liquid:
Adding sodium gluconate into water, stirring at normal temperature for 8min, adding octyl phenol polyoxyethylene ether, heating to 37 ℃, stirring for 25min, and naturally cooling to room temperature to obtain pretreatment liquid;
(4) Preparation of composite acid liquor:
sequentially adding lactic acid, gluconic acid, an organic phosphoric acid polymer and hydrochloric acid into water, stirring for 20min at 35 ℃, naturally cooling to room temperature, adding a cationic gemini surfactant, and stirring for 15min to obtain a composite acid solution, wherein the volume ratio of the pretreatment solution to the composite acid solution is 1:2, and obtaining the flowback-free acidification working solution 3#.
EXAMPLE 4 non-flowback acidizing fluid 4#
(1) Preparation of the organic phosphoric acid polymer:
diluting the isopropenyl phosphonic acid monomer with water to 50% aqueous solution, heating to 70 ℃, dripping the mixture of ammonium persulfate and acrylic acid into the aqueous solution, wherein the mol ratio of the isopropenyl phosphonic acid monomer to the acrylic acid is 1:1, the dosage of the ammonium persulfate is 15% of that of the isopropenyl phosphonic acid monomer and the acrylic acid, and continuing to react to obtain the organic phosphoric acid polymer.
(2) Preparing raw materials, namely preparing a mixture of 12% of octyl phenol polyoxyethylene ether, 7% of sodium gluconate, 15% of lactic acid and gluconic acid according to the weight percentage, and the balance of water, wherein the molar ratio of the lactic acid to the gluconic acid is 1:1,8% of organic phosphoric acid polymer, 1% of hydrochloric acid, 0.5% of cationic gemini surfactant and the balance of water;
(3) Preparation of pretreatment liquid:
Adding sodium gluconate into water, stirring at normal temperature for 10min, adding octyl phenol polyoxyethylene ether, heating to 35 ℃, stirring for 20min, and naturally cooling to room temperature to obtain pretreatment liquid;
(4) Preparation of composite acid liquor:
Sequentially adding lactic acid, gluconic acid, an organic phosphoric acid polymer and hydrochloric acid into water, stirring for 20min at 35 ℃, naturally cooling to room temperature, adding a cationic gemini surfactant, and stirring for 15min to obtain a composite acid solution, wherein the volume ratio of the pretreatment solution to the composite acid solution is 1:1, and obtaining the flowback-free acidification working solution No. 4.
Example 5 no flowback acidizing fluid 5#
Example 5 differs from example 4 in that the molar ratio of lactic acid to gluconic acid is 3:1, the remainder being identical.
EXAMPLE 6 no flowback acidizing fluid 6#
Example 6 is different from example 4 in that the volume ratio of the pretreatment liquid to the composite acid liquid is 1:10, and the rest are the same.
Comparative example 1 no-flowback acidizing fluid D1#
Comparative example 1 differs from example 4 in that the organic phosphoric acid polymer was not included by 8% and the weight percentage of hydrochloric acid was 9%.
Comparative example 2 flowback-free acidified working fluid D2#
Comparative example 2 is compared to example 4, except that the surfactant is sodium dodecyl sulfate, and the rest are the same.
Comparative example 3 no flowback acidizing fluid D3#
Comparative example 3 is different from example 4 in that the pretreatment liquid is not included, and the rest is the same.
Experimental example 1 evaluation of erosion Property
Firstly preparing an EDTA disodium standard solution with the concentration of 0.01 mol/L, respectively preparing 100 mL composite acid solutions in examples 1-5 and comparative examples 1-2, then adding carbonate particles of 6 g into the composite acid solution, titrating the solution with the EDTA disodium standard solution after a certain time of reaction to determine the calcium ion concentration after a certain time of reaction, and calculating the corrosion rate of the composite acid solution on the carbonate particles. The calculation results are shown in Table 1.
TABLE 1 evaluation results of erosion Properties
Experimental example 2 evaluation of retarding Performance
The polished and dried carbonate core column (phi 2.5X1 cm) is fixed on a rotating shaft in a ZDJ-1 acid rock reaction rotating rock disk instrument reaction kettle, and the corrosion rates of cores in the compound acid solutions in examples 1-5 and comparative example 1 for 1h, 3h, 8h and 16h are tested under the conditions of 80 ℃ and 7 MPa, and the results are shown in table 2.
TABLE 2 evaluation results of retarding Performance
Experimental example 3 stimulation experiment
The flowback-free acidizing fluid of examples 4 to 6 and comparative examples 1 to 3 was applied to wells, and the yield increasing effect was as shown in table 3.
TABLE 3 results of yield increasing experiments
The above description is only an example of the present application, and the scope of the present application is not limited to the specific examples, but is defined by the claims of the present application. Various modifications and variations of the present application will be apparent to those skilled in the art. Any modification, equivalent replacement, improvement, etc. made within the technical idea and principle of the present application should be included in the protection scope of the present application.
Claims (6)
1. The flowback-free acidification working solution is characterized by comprising 1 (2-10) of a pretreatment solution and a composite acid solution, wherein the composite acid solution comprises 15-25% of an organic acid, 1-3% of hydrochloric acid, 0.2-1% of a cationic gemini surfactant and the balance of water in percentage by weight, the organic acid comprises 10-15% of a mixture of lactic acid and gluconic acid and an organic phosphoric acid polymer in percentage by weight, the mixture of lactic acid and gluconic acid accounts for 5-10% of the composite acid solution, the organic phosphoric acid polymer accounts for 5-12% of the composite acid solution, the pretreatment solution comprises 5-12% of octyl phenol polyoxyethylene ether, 2-7% of sodium gluconate and the balance of water in percentage by weight, the molar ratio of lactic acid to gluconic acid is (1-1.5), the organic phosphoric acid polymer is an isopropyl acid monomer and acrylic acid monomer in percentage by weight, and the organic phosphoric acid polymer accounts for 1-1.5% of the cationic gemini surfactant is represented by the formula:
formula (1).
2. The flowback-free acidification working fluid according to claim 1, wherein the volume ratio of the pretreatment fluid to the composite acid fluid is 1 (2-4).
3. The flowback-free acidified working fluid of claim 1 wherein the process of preparing the organophosphate polymer comprises the steps of:
(1) Diluting the isopropenyl phosphonic acid monomer with water to 50% aqueous solution, and heating to 70-80 ℃;
(2) And (3) dropwise adding the mixture of ammonium persulfate and acrylic acid into the aqueous solution, and continuing the reaction to obtain the organic phosphoric acid polymer.
4. The flowback-free acidification working solution according to claim 3, wherein the molar ratio of the isopropenyl phosphonic acid monomer to the acrylic acid is 1-1.2:1, and the dosage of ammonium persulfate is 15-20% of the isopropenyl phosphonic acid monomer to the acrylic acid.
5. The method for preparing the flowback-free acidification working fluid according to any one of claims 1 to 4, which is characterized by comprising the following steps:
(1) The preparation of pretreatment liquid comprises adding sodium gluconate into water, stirring at room temperature for 5-10min, adding octyl phenol polyoxyethylene ether, heating to 35-40deg.C, stirring for 20-25min, and naturally cooling to room temperature to obtain pretreatment liquid;
(2) The preparation method of the composite acid liquor comprises the steps of sequentially adding lactic acid, gluconic acid, organic phosphoric acid polymer and hydrochloric acid into water, stirring for 20-25min at 35-40 ℃, naturally cooling to room temperature, adding a cationic gemini surfactant, and stirring for 10-20min to obtain the composite acid liquor.
6. The construction process of the flowback-free acidification working fluid according to any one of claims 1 to 4, which is characterized by comprising the following steps:
(1) Injecting pretreatment liquid into the oil sleeve annulus of the test oil well;
(2) Injecting the compound acid solution after 3-5h, and closing the well after injecting the compound acid solution for 24-72h.
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| CN103013489A (en) * | 2012-12-17 | 2013-04-03 | 中国石油天然气股份有限公司 | Acidizing blocking remover and preparation method thereof |
| US10428265B2 (en) * | 2014-05-07 | 2019-10-01 | Halliburton Energy Services, Inc. | Selective acidizing of a subterranean formation |
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