CN116892387B - Preparation method of radioactive isotope tracer for oilfield gas flooding monitoring - Google Patents
Preparation method of radioactive isotope tracer for oilfield gas flooding monitoring Download PDFInfo
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- 239000000700 radioactive tracer Substances 0.000 title claims abstract description 87
- 238000012544 monitoring process Methods 0.000 title claims abstract description 42
- 238000002360 preparation method Methods 0.000 title claims abstract description 30
- 230000002285 radioactive effect Effects 0.000 title abstract description 17
- 239000007788 liquid Substances 0.000 claims abstract description 38
- 238000000034 method Methods 0.000 claims abstract description 36
- BRPQOXSCLDDYGP-UHFFFAOYSA-N calcium oxide Chemical compound [O-2].[Ca+2] BRPQOXSCLDDYGP-UHFFFAOYSA-N 0.000 claims abstract description 31
- 239000000292 calcium oxide Substances 0.000 claims abstract description 28
- ODINCKMPIJJUCX-UHFFFAOYSA-N calcium oxide Inorganic materials [Ca]=O ODINCKMPIJJUCX-UHFFFAOYSA-N 0.000 claims abstract description 28
- IIZPXYDJLKNOIY-JXPKJXOSSA-N 1-palmitoyl-2-arachidonoyl-sn-glycero-3-phosphocholine Chemical compound CCCCCCCCCCCCCCCC(=O)OC[C@H](COP([O-])(=O)OCC[N+](C)(C)C)OC(=O)CCC\C=C/C\C=C/C\C=C/C\C=C/CCCCC IIZPXYDJLKNOIY-JXPKJXOSSA-N 0.000 claims abstract description 25
- 239000000787 lecithin Substances 0.000 claims abstract description 25
- 229940067606 lecithin Drugs 0.000 claims abstract description 25
- 235000010445 lecithin Nutrition 0.000 claims abstract description 25
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 claims abstract description 20
- IJOOHPMOJXWVHK-UHFFFAOYSA-N chlorotrimethylsilane Chemical compound C[Si](C)(C)Cl IJOOHPMOJXWVHK-UHFFFAOYSA-N 0.000 claims abstract description 14
- 229910000147 aluminium phosphate Inorganic materials 0.000 claims abstract description 10
- 239000002253 acid Substances 0.000 claims abstract description 9
- 238000001914 filtration Methods 0.000 claims abstract description 7
- 239000005051 trimethylchlorosilane Substances 0.000 claims abstract description 7
- XXDAXUSYDPWTPK-UHFFFAOYSA-N 2-(oxo-lambda5-phosphanylidyne)acetic acid Chemical compound P(=O)#CC(=O)O XXDAXUSYDPWTPK-UHFFFAOYSA-N 0.000 claims abstract description 6
- 239000011259 mixed solution Substances 0.000 claims description 33
- 238000003756 stirring Methods 0.000 claims description 33
- 230000000694 effects Effects 0.000 claims description 23
- 239000011148 porous material Substances 0.000 claims description 23
- 239000011734 sodium Substances 0.000 claims description 23
- 239000000243 solution Substances 0.000 claims description 22
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 19
- OFBQJSOFQDEBGM-UHFFFAOYSA-N Pentane Chemical compound CCCCC OFBQJSOFQDEBGM-UHFFFAOYSA-N 0.000 claims description 16
- VLKZOEOYAKHREP-UHFFFAOYSA-N n-Hexane Chemical compound CCCCCC VLKZOEOYAKHREP-UHFFFAOYSA-N 0.000 claims description 16
- 239000011521 glass Substances 0.000 claims description 15
- ZCYVEMRRCGMTRW-UHFFFAOYSA-N 7553-56-2 Chemical compound [I] ZCYVEMRRCGMTRW-UHFFFAOYSA-N 0.000 claims description 12
- 239000000706 filtrate Substances 0.000 claims description 12
- 238000002347 injection Methods 0.000 claims description 12
- 239000007924 injection Substances 0.000 claims description 12
- 229910052740 iodine Inorganic materials 0.000 claims description 12
- 239000011630 iodine Substances 0.000 claims description 12
- 230000008569 process Effects 0.000 claims description 12
- 230000009471 action Effects 0.000 claims description 11
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 9
- -1 polytetrafluoroethylene Polymers 0.000 claims description 9
- 229920001343 polytetrafluoroethylene Polymers 0.000 claims description 9
- 239000004810 polytetrafluoroethylene Substances 0.000 claims description 9
- 238000006243 chemical reaction Methods 0.000 claims description 8
- 238000007789 sealing Methods 0.000 claims description 8
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 6
- 239000000741 silica gel Substances 0.000 claims description 6
- 229910002027 silica gel Inorganic materials 0.000 claims description 6
- 238000003760 magnetic stirring Methods 0.000 claims description 5
- 230000002378 acidificating effect Effects 0.000 claims description 4
- 238000009792 diffusion process Methods 0.000 claims description 4
- 230000005012 migration Effects 0.000 claims description 4
- 238000013508 migration Methods 0.000 claims description 4
- 230000004888 barrier function Effects 0.000 claims description 3
- 150000001875 compounds Chemical class 0.000 claims description 3
- 125000001165 hydrophobic group Chemical group 0.000 claims description 3
- 238000006386 neutralization reaction Methods 0.000 claims description 3
- VIKNJXKGJWUCNN-XGXHKTLJSA-N norethisterone Chemical compound O=C1CC[C@@H]2[C@H]3CC[C@](C)([C@](CC4)(O)C#C)[C@@H]4[C@@H]3CCC2=C1 VIKNJXKGJWUCNN-XGXHKTLJSA-N 0.000 claims description 3
- 238000004806 packaging method and process Methods 0.000 claims description 3
- 239000000047 product Substances 0.000 claims description 3
- 238000003904 radioactive pollution Methods 0.000 claims description 3
- 238000003860 storage Methods 0.000 claims description 3
- 239000000725 suspension Substances 0.000 claims description 3
- 102100036790 Tubulin beta-3 chain Human genes 0.000 claims 3
- 239000002994 raw material Substances 0.000 abstract description 7
- 239000000443 aerosol Substances 0.000 abstract description 5
- 238000005259 measurement Methods 0.000 abstract description 5
- 231100000252 nontoxic Toxicity 0.000 abstract description 5
- 230000003000 nontoxic effect Effects 0.000 abstract description 5
- 239000003795 chemical substances by application Substances 0.000 abstract description 4
- 239000000126 substance Substances 0.000 abstract description 4
- 238000006297 dehydration reaction Methods 0.000 abstract description 3
- 241000237858 Gastropoda Species 0.000 abstract 1
- 239000012535 impurity Substances 0.000 abstract 1
- 238000007670 refining Methods 0.000 abstract 1
- 238000001179 sorption measurement Methods 0.000 abstract 1
- 239000007789 gas Substances 0.000 description 56
- 239000003921 oil Substances 0.000 description 24
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 7
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 description 6
- 238000006073 displacement reaction Methods 0.000 description 6
- 230000015572 biosynthetic process Effects 0.000 description 5
- 238000011161 development Methods 0.000 description 5
- 238000004519 manufacturing process Methods 0.000 description 5
- 238000011084 recovery Methods 0.000 description 5
- 239000001569 carbon dioxide Substances 0.000 description 3
- 229910002092 carbon dioxide Inorganic materials 0.000 description 3
- 238000005516 engineering process Methods 0.000 description 3
- 239000012530 fluid Substances 0.000 description 3
- 229910052757 nitrogen Inorganic materials 0.000 description 3
- 239000003513 alkali Substances 0.000 description 2
- GZUXJHMPEANEGY-UHFFFAOYSA-N bromomethane Chemical compound BrC GZUXJHMPEANEGY-UHFFFAOYSA-N 0.000 description 2
- 238000000605 extraction Methods 0.000 description 2
- 231100000053 low toxicity Toxicity 0.000 description 2
- 239000010413 mother solution Substances 0.000 description 2
- 150000002894 organic compounds Chemical class 0.000 description 2
- 230000035699 permeability Effects 0.000 description 2
- 230000001105 regulatory effect Effects 0.000 description 2
- 239000002699 waste material Substances 0.000 description 2
- OYPRJOBELJOOCE-UHFFFAOYSA-N Calcium Chemical compound [Ca] OYPRJOBELJOOCE-UHFFFAOYSA-N 0.000 description 1
- UGFAIRIUMAVXCW-UHFFFAOYSA-N Carbon monoxide Chemical compound [O+]#[C-] UGFAIRIUMAVXCW-UHFFFAOYSA-N 0.000 description 1
- 244000292411 Excoecaria agallocha Species 0.000 description 1
- 150000001335 aliphatic alkanes Chemical class 0.000 description 1
- 238000000889 atomisation Methods 0.000 description 1
- 239000011575 calcium Substances 0.000 description 1
- 229910052791 calcium Inorganic materials 0.000 description 1
- 239000000969 carrier Substances 0.000 description 1
- 239000010779 crude oil Substances 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 230000008021 deposition Effects 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000004090 dissolution Methods 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 239000003546 flue gas Substances 0.000 description 1
- 239000004088 foaming agent Substances 0.000 description 1
- 239000007943 implant Substances 0.000 description 1
- 229940102396 methyl bromide Drugs 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000007935 neutral effect Effects 0.000 description 1
- JCXJVPUVTGWSNB-UHFFFAOYSA-N nitrogen dioxide Inorganic materials O=[N]=O JCXJVPUVTGWSNB-UHFFFAOYSA-N 0.000 description 1
- 238000011160 research Methods 0.000 description 1
Classifications
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01V—GEOPHYSICS; GRAVITATIONAL MEASUREMENTS; DETECTING MASSES OR OBJECTS; TAGS
- G01V5/00—Prospecting or detecting by the use of ionising radiation, e.g. of natural or induced radioactivity
- G01V5/04—Prospecting or detecting by the use of ionising radiation, e.g. of natural or induced radioactivity specially adapted for well-logging
-
- 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
- E21B43/16—Enhanced recovery methods for obtaining hydrocarbons
- E21B43/166—Injecting a gaseous medium; Injecting a gaseous medium and a liquid medium
- E21B43/168—Injecting a gaseous medium
-
- 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
- E21B47/00—Survey of boreholes or wells
- E21B47/10—Locating fluid leaks, intrusions or movements
- E21B47/11—Locating fluid leaks, intrusions or movements using tracers; using radioactivity
- E21B47/111—Locating fluid leaks, intrusions or movements using tracers; using radioactivity using radioactivity
Landscapes
- Life Sciences & Earth Sciences (AREA)
- Physics & Mathematics (AREA)
- Geology (AREA)
- Engineering & Computer Science (AREA)
- Mining & Mineral Resources (AREA)
- General Life Sciences & Earth Sciences (AREA)
- Geophysics (AREA)
- Environmental & Geological Engineering (AREA)
- Fluid Mechanics (AREA)
- Geochemistry & Mineralogy (AREA)
- General Physics & Mathematics (AREA)
- High Energy & Nuclear Physics (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The invention discloses a method for preparing a radioisotope tracer for oilfield gas flooding monitoring. Firstly adding a radioisotope tracing carrier liquid at a controlled temperature, then adding a porous calcium oxide adsorption Na 131 I solution to realize chemical dehydration, then adding phosphoric acid to make the mixed liquid become weak acid, then adding trimethylchlorosilane and trimethyl phosphorylacetate to obtain a CH 3 131 I mixed liquid, then adding lecithin to reduce 131 I escape, and finally filtering, refining and removing impurities to obtain the finished product. Compared with the same type of substances, the tracer has lower density under the condition of high-pressure logging, is easy to form stable aerosol, and can form more stable radioactive slugs after being released by a releaser. The preparation method has the advantages of mild and controllable conditions, safe and nontoxic trace carrier, wide source of common liquid releaser and radioactive isotope 131 I raw materials of the trace agent, suitability for relevant flow tracing well logging, support of a radioactive isotope tracing method to replace a turbine flowmeter, and realization of gas flooding quantitative measurement.
Description
Technical Field
The invention is mainly applied to the field of oilfield gas flooding monitoring, relates to a preparation method of a radioactive isotope tracer, and particularly relates to a preparation method of a radioactive isotope tracer for oilfield gas flooding monitoring.
Background
The Oil field is developed by gas Oil displacement (GAS ENHANCED Oil Recovery, GEOR) and is an Oil field exploitation technology appearing in the mid seventies of the last century, the principle is that high-pressure gas is injected into an Oil layer to push crude Oil to flow to a wellhead, so that the Oil at the upper part of the middle part of the Oil field can be directionally displaced, in addition, the gas Oil displacement can reduce the viscosity and the adhesion of the Oil through the dissolution and diffusion effects of the gas, so that the Oil which is difficult to collect originally can be exploited, and the micro and macro Oil displacement efficiency is improved. Compared with the traditional oil extraction method, the gas flooding method can effectively improve the recovery ratio of the oil field, so that more oil can be extracted, the energy consumption of the gas flooding is lower, and the oil extraction cost can be reduced. In addition, the gas displacement can prolong the production life of the oil field, reduce the later exploitation difficulty and cost and improve the development efficiency of the oil field. The development of the gas oil displacement exploitation technology in China is relatively late, the experimental preparation work of nitrogen injection exploitation occurs in the last eighties of the last century, and the experimental preparation work is in the research and preparation stage for a long time afterwards. In recent years, the related technology is mature continuously, and the gas displacement is used for entering the high-speed development period. The injection gases used internationally are mainly nitrogen (deoxidized air), carbon dioxide and flue gas, and nitrogen and carbon dioxide are mainly used in China. Compared with carbon dioxide, nitrogen has the advantages of sufficient resources, no limitation of geographical conditions, no corrosiveness, low cost and the like, and has more popularization value.
The monitoring data is an important basis for adjusting the gas drive recovery scheme. Currently, the first turbine flowmeter used for gas drive monitoring is based on the principle that the flow rate is calculated by measuring the rotation of fluid passing through turbine blades, the rotation speed of the turbine blades is approximately proportional to the volume flow rate, and the volume indication of the fluid passing through the flowmeter is based on the rotation number of the turbine impeller. However, the foaming agent added during gas injection exploitation can adhere to turbine blades, so that the turbine is difficult to rotate, the measurement result is distorted, and an accurate quantitative result cannot be provided, which is a difficult problem that a turbine continuous flowmeter cannot overcome, so that the conventional turbine flowmeter can only obtain a qualitative result.
The most widely applied, economical and reliable technique in dynamic monitoring of water injection development is a radioisotope tracing method, the principle is that a radioisotope tracer is added into water injection liquid, the migration and distribution condition of the injected liquid in the ground is tracked by utilizing the characteristic of radioisotope, and the logging technique is not affected by a pipe column, has obvious layering and is widely used by various oil fields. The lack of tracers makes isotope tracers difficult to implant into gas injection monitoring, and some challenges may be encountered if existing water-flooding tracers are still used, for example, tracers used in water-flooding typically have a high density and are compatible with water and migrate downwards with the injected water liquid, and the gas rises faster during gas injection, and the tracers are difficult to rise with the gas, and may sink quickly to the bottom of the formation, fail to rise, and are difficult to accurately filter at the surface of the gas-intake formation. In addition, tracers in water flooding typically have some adsorptivity, and can filter out and maintain some stability in the formation pores. However, during gas injection, the gas flow rate in the formation pores is relatively high, and the tracer is difficult to accurately filter and remain stable on the surface of the intake formation. If the relative flow method is used for monitoring, the sinking speed is too high, the tracking of the detector is difficult, and the correlation between the tracer moving speed and the gas flowing speed is poor.
Methyl bromide (CH 3-82 Br) is a radioactive gas with a short half-life (T 1/2 =36 h) and moderate radiant energy (92 keV), and is used for pipeline gas tracing and underground pipeline leakage positioning in foreign countries. From the physical characteristics, CH 3-82 Br is very suitable for gas-driven logging, but the technical introduction has the following limitations: 82 The Br nuclide needs to be imported, and the raw material supply cannot be ensured; the application and approval of the new nuclide are difficult; the logging equipment and the tracer production equipment have higher requirements, large investment and long fund recovery period. In order to solve the problems, the isotope tracer for gas flooding monitoring, which has low density and is easy to form aerosol, is used for tracking and quantitatively measuring the flow of gas, improving the monitoring and control capability of a gas flooding process and further optimizing the oil reservoir development and production effect, and is a problem to be solved urgently.
Disclosure of Invention
Object of the invention
Aiming at the defects and shortcomings of the prior art, the invention provides a preparation method of a gas-driven radioactive isotope tracer capable of quantitatively monitoring, which is needed by isotope tracing monitoring in an oil field, and is a 131 I marked isotope tracer for gas-driven monitoring, which is liquid at normal temperature and pressure, has the trace carrier of alkane, is safe and nontoxic, can still use a common liquid releaser, and is easy to log, construct, transport, store and protect, in order to overcome the limitations and challenges of unstable raw material supply, high equipment requirement, long fund recovery period and the like faced by the existing available nuclides in the technical introduction and application processes. The density of the tracer agent is between 0.6 and 0.7g/ml under the high pressure of the gas drive, the density of the same type of substances under the same temperature and the same pressure is lower, the tracer agent is sprayed out by a releaser during well logging, and the tracer agent enters the high pressure gas in the form of small liquid drops, and aerosol is obtained through atomization, so that a relatively stable radioactive slug is formed. The adopted radioisotope 131 I is a medical domestic isotope, the source of raw materials is wide, the source of goods is stable, and almost all oilfield logging units have permission, so the method is easy to popularize and apply. The tracer is suitable for relevant flow tracing logging, and supports a radioactive isotope tracing method to replace a turbine flowmeter so as to realize gas flooding quantitative measurement.
(II) technical scheme
The technical scheme adopted by the invention for solving the technical problems is as follows:
the preparation method of the radioisotope tracer for oilfield gas flooding monitoring is characterized by at least comprising the following steps:
SS1, placing a preparation container added with a stirring device in a constant-temperature water bath, and maintaining the temperature of the constant-temperature water bath within the range of 10-30 ℃;
SS2. Adding a set amount of radio-isotope labeled carrier liquid into the preparation container, adding a set amount of porous calcium oxide or porous material loaded with calcium oxide into the radio-isotope labeled carrier liquid, and then starting the stirring device to stir so that the porous calcium oxide or porous material loaded with calcium oxide and the radio-isotope labeled carrier liquid form a uniform mixed liquid in a suspension state and rotate along with the uniform mixed liquid;
SS3, slowly dripping a set amount of Na 131 I solution with a set activity into the uniform mixed solution prepared in the step SS2, and stirring for 10-20 minutes under the action of a stirring device, so that the porous calcium oxide or the porous material loaded with the calcium oxide forms an anhydrous Na 131 I mixed solution environment after fully absorbing the moisture in the Na 131 I solution;
SS4 adding a set amount of phosphoric acid into the Na 131 I mixed solution prepared in the step SS3, and stirring for 5-10 minutes under the action of a stirring device, so that the phosphoric acid and sodium hydroxide in the Na 131 I mixed solution undergo a neutralization reaction to form a weak acid mixed solution;
SS5 adding a set amount of trimethylchlorosilane and trimethyl phosphorylacetate into the weakly acidic mixed solution prepared in the step SS4, stirring for 40-80 minutes under the action of a stirring device, and fully reacting according to a chemical reaction formula CH3OCOCH2PO(OCH3)2+2Me3SiCl+2Na131I→CH3OCOCH2PO(OSiMe3)2+2CH3 131I+2NaCl to generate CH 3 131 I mixed solution;
SS6 adding a set amount of lecithin tracer carrier solution into the CH 3 131 I mixed solution prepared in the step SS5, stirring for 5-10 minutes under the action of a stirring device to form a lecithin tracer carrier mixed solution, preventing radioactive pollution caused by escape of iodine molecules possibly separated out of CH 3 131 I into the air in the process of storage and use by utilizing the characteristic that lecithin is easy to react with iodine molecules to form stable coordination compounds, and increasing the viscosity of the CH 3 131 I mixed solution by utilizing hydrophobic groups in the lecithin molecules so as to increase diffusion barrier of iodine and reduce migration rate and escape amount of iodine;
SS7, finely filtering the lecithin tracer carrier mixed solution prepared in the step SS6 by using a micron-sized filter screen, wherein the filter screen filtrate is a radioisotope tracer product for monitoring oilfield gas flooding;
SS8 measuring the activity of the filtrate obtained in the step SS7, and sub-packaging the filtrate meeting the activity requirement according to the specification and storing the filtrate in a low-temperature sealing way.
Preferably, in step SS1, the preparation container is a glass container disposed in a radiation-proof glove box, and the glass container is provided with a magnetic stirring device and is installed in a thermostatic water bath, and the setting temperature of the thermostatic water bath is 10-30 ℃.
Further, the glass container is characterized in that the glass container is a flat bottom or round bottom flask, a straight pipe-shaped outlet extending along the height direction is arranged at the top of the flask, a bent tip pipe is connected to the upper part of the straight pipe-shaped outlet through a clamp ring-shaped joint, a filter screen is arranged in the middle of the ring-shaped joint, a double-sided polytetrafluoroethylene silica gel pad is arranged on the upper outer edge and the lower outer edge of the filter screen for sealing, a side pipe for injection feeding is arranged on the straight pipe-shaped outlet, the side pipe is sealed by a single-sided polytetrafluoroethylene silica gel sheet, and the polytetrafluoroethylene surface faces inwards.
Preferably, in step SS2 above, the radioisotope labelled carrier fluid added to the preparation vessel is n-pentane or n-hexane.
Further, in the above step SS2, the amount of n-pentane or n-hexane added is 0.5 to 20ml per milligram, and the amount of porous calcium oxide or a porous material loaded with calcium oxide added is 0.05 to 0.5g per milligram.
Preferably, in the above step SS3, the activity of Na 131 I is in the range of 5 to 800mCi/ml.
Preferably, in the above step SS4, the phosphoric acid is added in an amount of 3 to 20. Mu.l per milli-meter.
Preferably, in the above step SS5, the addition amount of the trimethylchlorosilane is 1 to 20. Mu.l per milli-house, and the addition amount of the trimethyl phosphorylacetate is 0.5 to 10. Mu.l per milli-house.
Preferably, in the step SS6, the mass concentration of the lecithin tracer carrier solution is 1-10 per mill, and the addition amount is 0.5-5 ml of the tracer carrier per 100 ml.
Preferably, in the step SS7, the filter is a small pore glass filter, and the mesh size of the filter is between 5 μm and 15 μm.
(III) technical effects
Compared with the prior art, the preparation method of the radioisotope tracer for oilfield gas flooding monitoring has the following outstanding technical advantages:
(1) The adopted radioisotope 131 I is a medical domestic isotope, the source of raw materials is wide, and almost all oilfield logging units have permission, so the method is easy to popularize and apply;
(2) The tracer carrier solution is safe and nontoxic: the raw materials such as the tracer carrier n-pentane or n-hexane, lecithin and the like which are sequentially used in the process of preparing the radioisotope tracer for oilfield gas flooding monitoring have low toxicity from the safety point of view, are relatively safe and nontoxic in general cases, and have small influence on human bodies and environment;
(3) The prepared tracer can still use a common liquid releaser: the tracer is in a liquid state although being used for gas tracing, and can be released by using a common liquid releaser, and meanwhile, the finally generated tracer is slightly acidic, so that the acid resistance requirement on the liquid releaser is not high, and the logging cost of an oil field can be saved. In addition, lecithin is added in the preparation process of the tracer to prevent 131 I from escaping, the lecithin belongs to a soluble organic compound, and has good permeability for a liquid releaser, and the prepared tracer can still use a common liquid releaser due to the characteristics of acid and alkali, fluidity and the like, so that the tracer is easy to log, construct, transport, store and protect;
(4) The density of the prepared tracer is kept between 0.6 and 0.7g/ml in a high-pressure logging environment, compared with substances of the same type under the same temperature and the same pressure, the density is lower, when logging, the tracer is atomized and released by a releaser and then enters high-pressure gas in the form of small liquid drops, aerosol is easy to form, a relatively stable radioactive slug is formed, and gas flooding quantitative measurement can be carried out by a relevant flow tracing method;
(5) In the process of preparing the radioisotope tracer for oilfield gas flooding monitoring, porous calcium oxide or a porous material loaded with the calcium oxide is adopted to absorb water in Na 131 I solution, so that chemical dehydration is realized, an anhydrous environment is ensured, and the calcium oxide is a porous material or is loaded on the porous material and is easy to separate;
(6) In the process of preparing the radioisotope tracer for oilfield gas flooding monitoring, na 131 I solution can be flexibly added according to actual production requirements, so that the specific activity of the prepared tracer can be flexibly regulated and controlled, the required specific activity can be achieved at one time, and the mother solution with high specific activity can be prepared first and then diluted according to requirements;
(7) In the process of preparing the radioisotope tracer for monitoring the oilfield gas flooding, the reaction condition is mild and easy to control, the equipment is simple and efficient and easy to prepare, and the radioisotope conversion rate is ensured;
(8) In the process of preparing the radioisotope tracer for oilfield gas flooding monitoring, the tracer carrier is added first, and the reaction occurs in the continuous phase of the tracer carrier, so that the waste of the radioisotope caused by incapability of reacting due to the sinking of Na 131 I solution is avoided, and the post-treatment protection difficulty is reduced.
Drawings
FIG. 1 is a schematic illustration of a process flow for preparing a radioisotope tracer for oilfield gas flooding monitoring of the present invention;
Fig. 2 is a schematic diagram of a preparation vessel for a radioisotope tracer for oilfield gas flooding monitoring in accordance with the present invention.
Reference numerals illustrate:
1-filter screen, 2-injection charging side pipe.
Detailed Description
For a better understanding of the present invention, the following examples are set forth to illustrate the present invention. In the drawings, the same or similar reference numerals denote the same or similar elements or elements having the same or similar functions throughout. The described embodiments are some, but not all, embodiments of the invention. The embodiments described below by referring to the drawings are illustrative and intended to explain the present invention and should not be construed as limiting the invention. All other embodiments, which can be made by those skilled in the art based on the embodiments of the invention without making any inventive effort, are intended to be within the scope of the invention. The following describes the structure and technical scheme of the present invention in detail with reference to the accompanying drawings, and an embodiment of the present invention is given.
As shown in fig. 1, when the radioisotope tracer for monitoring the oilfield gas flooding is prepared, the method mainly comprises the following process steps:
SS1. Placing a preparation container with a stirring device in a constant-temperature water bath, and maintaining the temperature of the constant-temperature water bath within the range of 10-30 ℃.
In a preferred embodiment of the present invention, the preparation vessel is shown in fig. 2, the preparation vessel is a glass vessel arranged in a radiation-proof glove box, a magnetic stirring device is arranged in the glass vessel and is arranged in a constant-temperature water bath, and the set temperature of the constant-temperature water bath is 10-30 ℃. The glass container is characterized in that the glass container is a flat bottom or round bottom flask, a straight pipe-shaped outlet extending along the height direction is arranged at the top of the flask, the upper part of the straight pipe-shaped outlet is connected with a bent tip pipe through a clamp ring-shaped joint, a filter screen 1 is arranged in the middle of the ring-shaped joint, double-sided polytetrafluoroethylene silica gel pads are arranged on the upper outer edge and the lower outer edge of the filter screen for sealing, a side pipe 2 for injection feeding is arranged on the straight pipe-shaped outlet, the side pipe is sealed by a single-sided polytetrafluoroethylene silica gel sheet, and the polytetrafluoroethylene surface faces inwards.
SS2 adding a set amount of a radioactive isotope labeled carrier liquid, preferably n-pentane or n-hexane, into a preparation container, adding a set amount of porous calcium oxide or a porous material loaded with calcium oxide into the radioactive isotope labeled carrier liquid, and then starting a stirring device to stir so that the porous calcium oxide or the porous material loaded with calcium oxide and the radioactive isotope labeled carrier liquid form a uniform mixed liquid in a suspension state and rotate along with the uniform mixed liquid. In this step, the amount of n-pentane or n-hexane added is preferably 0.5 to 20ml per milli-house, and the amount of porous calcium oxide or a porous material loaded with calcium oxide added is preferably 0.05 to 0.5g per milli-house.
And SS3, slowly adding a set amount of Na 131 I solution with the activity range of 5-800 mCi/ml into the uniform mixed solution prepared in the step SS2, and stirring for 10-20 minutes under the action of a stirring device, so that the porous calcium oxide or the porous material loaded with the calcium oxide forms an anhydrous Na 131 I mixed solution environment after fully absorbing the moisture in the Na 131 I solution.
And S4, adding 3-20 mu l of phosphoric acid per millilitre into the Na 131 I mixed solution prepared in the step S3, and stirring for 5-10 minutes under the action of a stirring device, so that the phosphoric acid and sodium hydroxide in the Na 131 I mixed solution are subjected to neutralization reaction to form a weak acid mixed solution.
SS5 adding 1-20 mu l of trimethylchlorosilane and 0.5-10 mu l of trimethyl phosphorylacetate per milli into the weakly acidic mixed solution prepared in the step SS4, stirring for 40-80 minutes, and fully reacting according to CH3OCOCH2PO(OCH3)2+2Me3SiCl+2Na131I→CH3OCOCH2PO(OSiMe3)2+2CH3 131I+2NaCl to obtain CH 3 131 I mixed solution.
SS6 adding a set amount of lecithin tracer carrier solution into the CH 3 131 I mixed solution prepared in the step SS5, stirring for 5-10 minutes under the action of a stirring device to form a lecithin tracer carrier mixed solution, preventing radioactive pollution caused by escape of iodine molecules possibly separated out of CH 3 131 I into the air in the process of storage and use by utilizing the characteristic that lecithin is easy to react with iodine molecules to form stable coordination compounds, and increasing the viscosity of the CH 3 131 I mixed solution by utilizing hydrophobic groups in the lecithin molecules so as to increase diffusion barrier of iodine and reduce migration rate and escape amount of iodine;
SS7, finely filtering the lecithin tracer carrier mixed solution prepared in the step SS6 by using a micron-sized filter screen, wherein the filter screen filtrate is a radioisotope tracer product for monitoring oilfield gas flooding;
SS8 measuring the activity of the filtrate obtained in the step SS7, and sub-packaging the filtrate meeting the activity requirement according to the specification and storing the filtrate in a low-temperature sealing way.
In the preparation process of the radioisotope tracer for oilfield gas flooding monitoring, tracer carriers such as n-pentane or n-hexane, lecithin and the like are sequentially used, so that the radioisotope tracer has low toxicity from the safety point of view, is relatively safe and nontoxic in general, and has small influence on human bodies and environment. The reaction condition is mild and controllable, the equipment is simple and efficient and easy to prepare, the adopted radioisotope 131 I is medical domestic isotope, the raw material source is wide, and almost all oilfield logging units have permission and are easy to popularize and apply. Meanwhile, the tracer is in a liquid state although being used for gas tracing, and can be released by using a common liquid releaser, and meanwhile, the finally generated tracer is weak acid or neutral, so that the acid resistance requirement on the releaser is not high, and the logging cost of an oil field can be saved. In addition, a lecithin tracer carrier solution is added in the preparation process of the tracer to prevent 131 I from escaping, the lecithin belongs to a soluble organic compound, and has good permeability for a liquid releaser, and the prepared tracer can still use a common liquid releaser due to the characteristics of acid and alkali, fluidity and the like, so that the tracer is easy to log, construct, transport, store and protect. In addition, the density of the prepared tracer is kept between 0.6 and 0.7g/ml in a high-pressure logging environment, compared with substances of the same type under the same temperature and the same pressure, the tracer has lower density, and when in logging, the tracer is atomized and released by a releaser and then enters high-pressure gas in the form of small liquid drops, aerosol is easy to form, a relatively stable radioactive slug is easy to form, and gas flooding quantitative measurement can be carried out by using a related flow tracing method. It should be noted that in the process of preparing the radioisotope tracer for monitoring the oilfield gas flooding, porous calcium oxide or a porous material loaded with the calcium oxide is adopted to absorb the moisture in the Na 131 I solution, so that chemical dehydration is realized, the anhydrous environment is ensured, and the calcium oxide is a porous material or is loaded on the porous material, and is easy to separate; in the preparation process, na 131 I solution can be flexibly added according to actual production requirements, so that the specific activity of the prepared tracer can be flexibly regulated and controlled, the required specific activity can be achieved at one time, and the mother solution with high specific activity can be prepared first and then diluted as required; in addition, in the preparation process, the tracer carrier is added first, and the reaction occurs in the continuous phase of the tracer carrier, so that the waste of radioactive isotopes caused by incapacity of reacting due to the deposition of Na 131 I solution is avoided, and the post-treatment protection difficulty is reduced.
Example 1
In a radiation-proof glove box, a flat bottom glass container as shown in fig. 1 is fixed in a constant temperature water bath with magnetic stirring at a set temperature of 20 ℃ and a magnet with proper size is placed. 200ml of the tracer carrier was added, 5g of the calcium oxide-supported porous material was added, and the magnetic stirring was turned on to suspend the porous material in the tracer carrier and rotate therewith. 30mCi of Na 131 I solution was added and stirred for 15 minutes. After that, 300. Mu.l of phosphoric acid was added thereto and stirred for 10 minutes. After that, 360. Mu.l of trimethylchlorosilane and 230. Mu.l of trimethylphosphorylacetate were added and stirred for 50 minutes. And adding 10ml of lecithin tracer carrier solution with the concentration of 1 per mill, stirring for 5 minutes, and filtering and pouring out through a small-hole glass filter screen to obtain the oil field gas flooding monitoring isotope tracer. Measuring activity, and storing in a low-temperature sealing way. Sealing and standing the filtering matter of the filtering net.
Examples 2 to 5
The procedure was essentially the same as in example 1, except that the reaction temperature was 10℃and 15℃and 25℃and the activity of the Na 131 I solution added was 200mci, 120mci, 80mci and 300mci, respectively, and the other parameters were the same. The data on the yield, density and specific activity of the radioisotope tracers for oilfield gas flooding monitoring prepared in examples 1 to 5 are shown in table 1.
Table 1 data relating to examples 1 to 5
The object of the present invention is fully effectively achieved by the above-described embodiments. Those skilled in the art will appreciate that the present invention includes, but is not limited to, those illustrated in the drawings and described in the foregoing detailed description. While the invention has been described in connection with what is presently considered to be the most practical and preferred embodiment, it is to be understood that the invention is not limited to the disclosed embodiment, but on the contrary, is intended to cover various modifications and equivalent arrangements included within the scope of the appended claims.
Claims (10)
1. The preparation method of the radioisotope tracer for oilfield gas flooding monitoring is characterized by at least comprising the following steps:
SS1, placing a preparation container added with a stirring device in a constant-temperature water bath, and maintaining the temperature of the constant-temperature water bath within the range of 10-30 ℃;
SS2. Adding a set amount of radio-isotope labeled carrier liquid into the preparation container, adding a set amount of porous calcium oxide or porous material loaded with calcium oxide into the radio-isotope labeled carrier liquid, and then starting the stirring device to stir so that the porous calcium oxide or porous material loaded with calcium oxide and the radio-isotope labeled carrier liquid form a uniform mixed liquid in a suspension state and rotate along with the uniform mixed liquid;
SS3, slowly dripping a set amount of Na 131 I solution with a set activity into the uniform mixed solution prepared in the step SS2, and stirring for 10-20 minutes under the action of a stirring device, so that the porous calcium oxide or the porous material loaded with the calcium oxide forms an anhydrous Na 131 I mixed solution environment after fully absorbing the moisture in the Na 131 I solution;
SS4 adding a set amount of phosphoric acid into the Na 131 I mixed solution prepared in the step SS3, and stirring for 5-10 minutes under the action of a stirring device, so that the phosphoric acid and sodium hydroxide in the Na 131 I mixed solution undergo a neutralization reaction to form a weak acid mixed solution;
SS5 adding a set amount of trimethylchlorosilane and trimethyl phosphorylacetate into the weakly acidic mixed solution prepared in the step SS4, stirring for 40-80 minutes under the action of a stirring device, and fully reacting according to a chemical reaction formula CH3OCOCH2PO(OCH3)2+2Me3SiCl+2Na131I→CH3OCOCH2PO(OSiMe3)2+2CH3 131I+2NaCl to generate CH 3 131 I mixed solution;
SS6 adding a set amount of lecithin tracer carrier solution into the CH 3 131 I mixed solution prepared in the step SS5, stirring for 5-10 minutes under the action of a stirring device to form a lecithin tracer carrier mixed solution, preventing radioactive pollution caused by escape of iodine molecules possibly separated out of CH 3 131 I into the air in the process of storage and use by utilizing the characteristic that lecithin is easy to react with iodine molecules to form stable coordination compounds, and increasing the viscosity of the CH 3 131 I mixed solution by utilizing hydrophobic groups in the lecithin molecules so as to increase diffusion barrier of iodine and reduce migration rate and escape amount of iodine;
SS7, finely filtering the lecithin tracer carrier mixed solution prepared in the step SS6 by using a micron-sized filter screen, wherein the filter screen filtrate is a radioisotope tracer product for monitoring oilfield gas flooding;
SS8 measuring the activity of the filtrate obtained in the step SS7, and sub-packaging the filtrate meeting the activity requirement according to the specification and storing the filtrate in a low-temperature sealing way.
2. The method for preparing a radioisotope tracer for oilfield gas flooding monitoring as claimed in claim 1, wherein in the step SS1, the preparation container is a glass container arranged in a radiation-proof glove box, a magnetic stirring device is arranged in the glass container and is arranged in a thermostatic water bath, and the setting temperature of the thermostatic water bath is 10-30 ℃.
3. The method for preparing the radioisotope tracer for oilfield gas flooding monitoring according to claim 2, wherein the glass container is a flat bottom or round bottom flask, the top of the flask is a straight tubular outlet extending along the height direction, the upper part of the straight tubular outlet is connected with a bent tip tube through a clamp type annular joint, the filter screen is arranged in the middle of the annular joint, double-sided polytetrafluoroethylene silica gel pads are arranged on the upper outer edge and the lower outer edge of the filter screen for sealing, a side tube for injection feeding is arranged on the straight tubular outlet, the side tube is sealed by a single-sided polytetrafluoroethylene silica gel sheet, and the polytetrafluoroethylene faces inwards.
4. The method for preparing a radioisotope tracer for oilfield gas flooding monitoring as recited in claim 1, wherein the radioisotope tracer carrier liquid added to the preparation vessel in the step SS2 is n-pentane or n-hexane.
5. The method for preparing a radioisotope tracer for oilfield gas flooding monitoring as claimed in claim 4, wherein in the step SS2, the amount of n-pentane or n-hexane added is 0.5-20 ml per milli-house, and the amount of porous calcium oxide or porous material loaded with calcium oxide added is 0.05-0.5 g per milli-house.
6. The method for preparing a radioisotope tracer for oilfield gas flooding monitoring as claimed in claim 1, wherein in the step SS3, the Na 131 I has an activity range of 5-800 mCi/ml.
7. The method for preparing a radioisotope tracer for oilfield gas flooding monitoring as claimed in claim 1, wherein the phosphoric acid is added in an amount of 3-20 μl/milli-meter in the step SS 4.
8. The method for preparing a radioisotope tracer for oilfield gas flooding monitoring as claimed in claim 1, wherein in the step SS5, the addition amount of the trimethylchlorosilane is 1-20 μl/milli, and the addition amount of the trimethyl phosphorylacetate is 0.5-10 μl/milli.
9. The method for preparing a radioisotope tracer for oilfield gas flooding monitoring as claimed in claim 1, wherein in the step SS6, the mass concentration of the lecithin tracer carrier solution is 1-10 per mill, and the addition amount is 0.5-5 ml per 100ml of tracer carrier.
10. The method for preparing a radioisotope tracer for oilfield gas flooding monitoring as claimed in claim 1, wherein in the step SS7, the filter is a small-hole glass filter with a mesh size of 5-15 μm.
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