CN108412487B - High-pressure-resistant radioactive isotope tracer and preparation method thereof - Google Patents
High-pressure-resistant radioactive isotope tracer and preparation method thereof Download PDFInfo
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Abstract
本发明公开了一种耐高压放射性同位素示踪剂及其制备方法，包括如下步骤：步骤1：制备含放射性同位素的溶液；步骤2：将多孔吸附材料浸入溶液，吸附放射性同位素离子，干燥；步骤3：加入沉淀剂溶液，用沉淀剂固定放射性同位素离子，干燥；步骤4：置于匣钵中，在一定温度下保温1～2小时，自然冷却；步骤5：用树脂胶、防静电剂、耐温剂、表面活性剂依次处理载体表面。本发明在多孔材料载体吸附、固定放射性同位素后，对其进行高温处理，使得吸附放射性同位素后的多孔材料孔隙明显变小，并收缩成更为致密的多孔小球，进而导致其耐压指标有显著的提升，使得同位素示踪剂耐压指标显著提升。The invention discloses a high-pressure radioisotope tracer and a preparation method thereof, comprising the following steps: step 1: preparing a solution containing radioisotopes; step 2: immersing a porous adsorption material in the solution, adsorbing radioisotope ions, and drying; 3: Add the precipitant solution, fix the radioisotope ions with the precipitant, and dry; Step 4: Put it in a sagger, keep it at a certain temperature for 1-2 hours, and cool it naturally; Step 5: Use resin glue, antistatic agent, The temperature resistant agent and the surfactant treat the surface of the carrier in turn. In the present invention, after the porous material carrier adsorbs and fixes the radioisotope, it is subjected to high temperature treatment, so that the pores of the porous material after adsorbing the radioisotope are obviously reduced, and shrink into a more dense porous ball, which leads to the pressure resistance index of Significant improvement, so that the isotope tracer withstand voltage index is significantly improved.
Description
Technical Field
The invention relates to a preparation method of a radioactive isotope tracer, in particular to a preparation method of a high-pressure-resistant radioactive isotope tracer for water absorption profile logging.
Background
As onshore oil fields in China enter the later stage of high water content development, the pressure of an oil layer is gradually reduced, and in order to realize long-term stable development, energy needs to be supplemented to the stratum and the pressure of the oil layer needs to be maintained, so that the aim of improving the yield of crude oil by 'displacing oil with water' is fulfilled. Therefore, in oil field development, a lot of water injection wells are drilled in addition to a lot of oil production wells, and individual wells with high water content are changed to water injection wells after a period of production. And injecting water into the underground oil layer through the water injection well to maintain the pressure of the oil layer, so that the recovery ratio of the crude oil is improved. Water injection monitoring is the key of 'displacement of reservoir oil with water' failure, and the monitoring uncertainty can influence the utilization of petroleum resources and even can cause major accidents, such as 'Kangfei oil leakage' accident of Bohai sea. In addition, after the oil field enters the middle and later stages, the water injection cost is greatly increased along with the multiple increase of the water injection quantity. Therefore, the waterflood indexes play more and more important roles in measuring the oil reservoir development effect. However, due to the differences in the geological conditions of the various fields, the formation conditions of even the same reservoir are quite complex. How to inject water can achieve the best development effect is always one of the focus problems concerned by oil field logging.
The radioactive isotope tracing method is the most common method for acquiring water absorption profile information at present in an oil field. During logging, the radioactive isotope tracer is released at a specified depth, the tracer and the borehole injection form an activated suspension, and when the selected tracer diameter is equal to the pore diameter of the formation, the injection in the suspension enters the formation, and the tracer is filtered and deposited on the borehole wall. The injection amount of the stratum, the tracer amount accumulated on the section of stratum well wall and the radioactive intensity of the tracer are in a direct proportion relation, and water injection information can be calculated and obtained by comparing gamma logging curves measured before and after the formation accumulation by the tracer. Compared with other well logging methods, the radioactive isotope tracing well logging method has the advantages of high sensitivity, simplicity and convenience in method, accuracy in positioning and quantification and the like. However, the existing isotope tracer products have a prominent problem that the pressure resistance is low (less than or equal to 60 MPa). At present, as onshore oil fields in China successively enter the middle and later periods of exploitation, oil production wells become deeper and deeper, geological environments become more and more complex, and higher requirements are put forward on the pressure resistance of isotope tracers. The existing isotope tracer agent can be broken due to low pressure resistance when in use, so that the problems of easy desorption of the isotope, small particle size of the tracer agent and the like are caused, and when the particle size of the tracer agent is smaller than the pore of a stratum, the tracer agent can enter the stratum along with water instead of being accumulated on a well wall, so that finally, the acquired logging information is inaccurate or even wrong.
Disclosure of Invention
The invention aims to provide a high-pressure resistant radioactive isotope tracer and a preparation method thereof aiming at the defects of the prior art.
A preparation method of a high pressure resistant radioactive isotope tracer agent comprises the following steps:
step 1: preparing a solution containing a radioisotope;
step 2: immersing the porous adsorption material into the solution, adsorbing radioactive isotope ions, and drying;
and step 3: adding precipitant solution, fixing radioisotope ions with precipitant, and drying;
and 4, step 4: placing the mixture in a sagger, preserving heat for 1-2 hours at high temperature, and naturally cooling;
and 5: and sequentially treating the surface of the carrier by using a resin adhesive, an antistatic agent, a temperature resistant agent and a surfactant, and drying to obtain the high-pressure resistant radioisotope tracer for water absorption profile logging.
The method, the radioactive isotope in the step (1) is barium-131; the preparation method of the solution containing the radioactive isotope comprises the steps of directly dissolving carbonate containing barium-131 by acid;
in the method, the concentration of acid used for dissolving carbonate is 40-70% of perchloric acid or 10-20% of nitric acid.
In the method, the porous adsorption material in the step (2) is coarse-pore silica gel; the particle size of the coarse-pore silica gel is 200-400 μm.
In the method, the precipitating agent in the step (3) is soluble salt which can form a difficultly soluble substance with radioactive isotope ions, and the soluble salt comprises carbonate or sulfate.
The method comprises the steps that in the step (2) and the step (3), the drying temperature is 100-300 ℃;
in the method, the sagger in the step (4) is a corundum sagger, a silicon carbide sagger, a mullite sagger or other high-temperature saggers with the highest temperature resistance higher than 1500 ℃.
In the method, the heat preservation temperature in the step (4) is 1000-1400 ℃.
According to the method, the specific radioactivity of the high-pressure resistant radioisotope tracer prepared in the step (5) is 0.15-6.32 (E +6 Bq)/g.
A radioisotope tracer prepared according to any one of the methods.
In order to better utilize the adsorbability of a porous material to adsorb radioactive isotopes, the conventional preparation process of the radioactive isotope tracer mainly adopts a porous material with high porosity and large specific surface area, and the pressure resistance of the porous material with stronger adsorption performance is lower, so that the pressure resistance of a porous material carrier is generally sacrificed in the conventional process. Compared with the existing preparation process of the radioactive isotope tracer, the preparation process disclosed by the invention has the advantages that after the radioactive isotope is adsorbed and fixed by the porous material carrier, the porous material is subjected to high-temperature treatment, so that the pores of the porous material after the radioactive isotope is adsorbed are obviously reduced and are contracted into more compact porous small balls, and further the pressure resistance index of the porous material is obviously improved, the problem that the adsorbability and the pressure resistance of the porous adsorbing material carrier in the existing preparation process of the radioactive isotope tracer cannot be simultaneously solved, and finally, the pressure resistance index of the isotope tracer is obviously improved, so that the preparation process is more suitable for oil and gas exploitation in medium-deep wells and complex geological exploitation environments.
Detailed Description
The technical solution of the present invention is further described in detail with reference to the following embodiments, but the scope of the present invention is not limited thereto.
Embodiment 1:
step 1: dissolving barium carbonate with activity of 7.16(E +8Bq) and containing radioactive isotope barium-131 in 25ml of 10% nitric acid, and diluting to 500 ml;
step 2: then weighing 400g of coarse-pore silica gel with the particle size of 200-400 mu m, adding the coarse-pore silica gel into the solution in the step (1), stirring the mixture for 3 hours at the temperature of 100-300 ℃, and drying the mixture;
and step 3: adding 150ml of 5% sodium carbonate solution, stirring at the temperature of 100-300 ℃ for 2 hours, and drying;
and 4, step 4: placing a porous silica gel carrier for absorbing the radioactive isotope in a corundum sagger, then placing the corundum sagger in a KSL-1700X-A4 box-type furnace, and preserving heat for 2 hours at 1100 ℃;
and 5: and sequentially treating the surface of the porous silica gel carrier by using resin adhesive, an antistatic agent, temperature-resistant resin and a surfactant. The resin adhesive is used for plugging holes on the surface of the porous silica gel, and is used for regulating the specific gravity of the tracer together with the precipitator and preventing the desorption of the tracer; the antistatic agent is used for removing static electricity generated by mutual friction of the tracers; the temperature-resistant resin can enhance the high-temperature stability of the tracer; surfactants are used to enhance the hydrophilicity of the tracer surface.
For example, the following treatments are performed in order: adding 400ml of resin adhesive, rotating at 60 ℃ for 20min-1Stirring for 9 hours; ② antistatic agent 1g, 80 ℃, rotating speed 20min-1Stirring for 2 hours; ③ 400ml of temperature-resistant resin, 100 ℃ and 30min of rotating speed-1Stirring for 8 hours; fourthly, 60ml of surface active agent with the rotating speed of 25min at 75 DEG C-1Stirring for 6 h.
After the surface treatment is carried out on the porous silica gel carrier absorbing the radioactive isotope, the high-pressure resistant radioactive isotope tracer for water absorption profile logging is prepared.
The obtained radioisotope tracer is soaked in distilled water for 2 hr to obtain specific gravity of 1.03g/cm3(ii) a After being put into a polyester textile bag, the tracer is put into a hydrostatic test device, the pressure is increased to 90MPa, and the breaking rate is 4.8%; specific activity of 1.01(E +6Bq)/cm3(ii) a Taking 20mCi tracer, measuring the activity change of the tracer before and after soaking in normal temperature distilled water for 24h by using an activity meter, wherein the static desorption rate is 4.8%; the 20mCi tracer is taken, the activity change of the tracer in water flow at 75 ℃ for 24 hours is measured by an activity meter, and the dynamic desorption rate is 9.3%. The same porous silica gel carrier, without high temperature heat treatment, was crushed at 60MPa according to the same test methodThe rate is 5%, the static desorption rate is 5.2%, and the dynamic desorption rate is 10.5%. The comparison of the test results shows that the porous silica gel carrier is heated at high temperature after adsorbing and fixing the radioactive isotope, so that the pressure resistance index of the radioactive isotope tracer can be obviously improved without influencing the adsorption performance of the isotope, and the porous silica gel carrier is more suitable for oil gas exploitation in medium-deep wells and complex geological exploitation environments.
Embodiment 2:
step 1: barium carbonate with activity 8.59(E +8Bq) containing the radioisotope barium-131 was dissolved in 30ml of 40% perchloric acid and diluted to 500 ml;
step 2: then weighing 400g of coarse-pore silica gel with the particle size of 200-400 mu m, adding the coarse-pore silica gel into the solution in the step (1), stirring the mixture at the temperature of 100-300 ℃ for 2 hours, and drying the mixture;
and step 3: adding 250ml of 2% sodium sulfate solution, stirring at the temperature of 100-300 ℃ for 2 hours, and drying;
and 4, step 4: placing a porous silica gel carrier for absorbing the radioactive isotope in a corundum sagger, then placing the corundum sagger in a KSL-1700X-A4 box-type furnace, and keeping the temperature at 1200 ℃ for 1.5 h;
and 5: and sequentially treating the surface of the porous silica gel carrier by using resin adhesive, an antistatic agent, temperature-resistant resin and a surfactant. The resin adhesive is used for plugging holes on the surface of the porous silica gel, and is used for regulating the specific gravity of the tracer together with the precipitator and preventing the desorption of the tracer; the antistatic agent is used for removing static electricity generated by mutual friction of the tracers; the temperature-resistant resin can enhance the high-temperature stability of the tracer; surfactants are used to enhance the hydrophilicity of the tracer surface. After the surface treatment is carried out on the porous silica gel carrier absorbing the radioactive isotope, the high-pressure resistant radioactive isotope tracer for water absorption profile logging is prepared.
The obtained radioisotope tracer is soaked in distilled water for 2 hr to obtain specific gravity of 1.04g/cm3(ii) a After being put into a polyester textile bag, the tracer is put into a hydrostatic test device, the pressure is increased to 90MPa, and the breaking rate is 4.3%; the specific activity of the radioactivity is 1.21(E +6Bq)/cm3(ii) a Taking 20mCi tracer, measuring activity change of tracer before and after soaking in distilled water at normal temperature for 24h by using activity meterThe static desorption rate is 4.5%; the activity change of 20mCi tracer in water flow at 75 deg.c for 24 hr is measured with activity meter and the dynamic desorption rate is 8.7%. The same porous silica gel carrier, without high temperature heat treatment, was directly subjected to the above steps to obtain the radioisotope tracer, according to the same test method, at 60MPa, the breakage rate was 5%, the static desorption rate was 5.2%, and the dynamic desorption rate was 10.5%. The comparison of the test results shows that the porous silica gel carrier is heated at high temperature after adsorbing and fixing the radioactive isotope, so that the pressure resistance index of the radioactive isotope tracer can be obviously improved without influencing the adsorption performance of the isotope, and the porous silica gel carrier is more suitable for oil gas exploitation in medium-deep wells and complex geological exploitation environments.
Embodiment 3:
step 1: barium carbonate with activity 8.33(E +8Bq) containing the radioisotope barium-131 was dissolved in 30ml of 70% perchloric acid and diluted to 500 ml;
step 2: then weighing 400g of coarse-pore silica gel with the particle size of 200-400 mu m, adding the coarse-pore silica gel into the solution in the step (1), stirring the mixture at the temperature of 100-300 ℃ for 2 hours, and drying the mixture;
and step 3: adding 200ml of 2% sodium sulfate solution, stirring at the temperature of 100-300 ℃ for 2 hours, and drying;
and 4, step 4: placing a porous silica gel carrier for absorbing the radioactive isotope in a corundum sagger, then placing the corundum sagger in a KSL-1700X-A4 box-type furnace, and preserving heat for 1h at 1300 ℃;
and 5: and sequentially treating the surface of the porous silica gel carrier by using resin adhesive, an antistatic agent, temperature-resistant resin and a surfactant. The resin adhesive is used for plugging holes on the surface of the porous silica gel, and is used for regulating the specific gravity of the tracer together with the precipitator and preventing the desorption of the tracer; the antistatic agent is used for removing static electricity generated by mutual friction of the tracers; the temperature-resistant resin can enhance the high-temperature stability of the tracer; surfactants are used to enhance the hydrophilicity of the tracer surface. After the surface treatment is carried out on the porous silica gel carrier absorbing the radioactive isotope, the high-pressure resistant radioactive isotope tracer for water absorption profile logging is prepared.
Distillation of the prepared radiotracerAfter soaking in water for 2h, the specific gravity was measured to be 1.05g/cm3(ii) a After being put into a polyester textile bag, the tracer is put into a hydrostatic test device, the pressure is increased to 90MPa, and the breaking rate is 4.0%; the specific activity of the radioactivity is 1.17(E +6Bq)/cm3(ii) a Taking 20mCi tracer, measuring the activity change of the tracer before and after soaking in normal temperature distilled water for 24h by using an activity meter, wherein the static desorption rate is 4.3%; the activity change of 20mCi tracer in water flow at 75 deg.c for 24 hr is measured with activity meter and the dynamic desorption rate is 8.1%. The same porous silica gel carrier, without high temperature heat treatment, was directly subjected to the above steps to obtain the radioisotope tracer, according to the same test method, at 60MPa, the breakage rate was 5%, the static desorption rate was 5.2%, and the dynamic desorption rate was 10.5%. The comparison of the test results shows that the porous silica gel carrier is heated at high temperature after adsorbing and fixing the radioactive isotope, so that the pressure resistance index of the radioactive isotope tracer can be obviously improved without influencing the adsorption performance of the isotope, and the porous silica gel carrier is more suitable for oil gas exploitation in medium-deep wells and complex geological exploitation environments.
It will be understood that modifications and variations can be made by persons skilled in the art in light of the above teachings and all such modifications and variations are intended to be included within the scope of the invention as defined in the appended claims.
Claims (11)
1. A preparation method of a high pressure resistant radioactive isotope tracer agent is characterized by comprising the following steps:
step 1: preparing a solution containing a radioisotope;
step 2: immersing the porous material into the solution obtained in the step (1), adsorbing radioactive isotope ions, and drying;
and step 3: adding a precipitant solution into the dried product obtained in the step (2), fixing radioisotope ions by using the precipitant, and drying to obtain a porous material for adsorbing the radioisotope;
and 4, step 4: placing the porous material for adsorbing the radioactive isotope in a sagger, preserving heat for 1-2 hours at high temperature, and naturally cooling to obviously reduce the pores of the porous material for adsorbing the radioactive isotope;
and 5: and sequentially treating the surface of the porous material by using a resin adhesive, an antistatic agent, a temperature resistant agent and a surfactant, and drying to obtain the high-pressure resistant radioactive isotope tracer for water absorption profile logging.
2. The method of claim 1, wherein: the radioactive isotope in the step (1) is barium-131; the preparation method of the solution containing the radioactive isotope is to directly dissolve carbonate containing barium-131 by acid.
3. The method of claim 2, wherein: the acid used for dissolving the carbonate has the concentration of 40-70% perchloric acid or 10-20% nitric acid.
4. The method of claim 1, wherein: the porous adsorption material in the step (2) is coarse-pore silica gel; the particle size of the coarse-pore silica gel is 200-400 μm.
5. The method of claim 1, wherein: the precipitant in the step (3) is soluble salt which can form insoluble matters with radioactive isotope ions, and comprises carbonate or sulfate.
6. The method of claim 1, wherein: and (3) drying at 100-300 ℃.
7. The method of claim 1, wherein: and (4) the sagger is a high-temperature sagger with the highest temperature resistance higher than 1500 ℃.
8. The method of claim 7, wherein: the high-temperature sagger is a corundum sagger, a silicon carbide sagger or a mullite sagger.
9. The method according to claim 1 or 4, characterized in that: and (4) keeping the temperature of 1000-1400 ℃.
10. The method of claim 1, wherein: the radioactive specific activity of the high-pressure resistant radioactive isotope tracer prepared in the step (5) is 0.15-6.32 (E +6 Bq)/g.
11. A radiotracer prepared according to the method of any one of claims 1 to 10.
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| CN113803058B (en) * | 2021-09-28 | 2024-03-15 | 河南工业大学 | Radioisotope tracer for thick oil steam injection well logging and preparation method thereof |
| CN114233282A (en) * | 2021-12-22 | 2022-03-25 | 河南省科学院同位素研究所有限责任公司 | High-efficient zero radioactivity emission well logging tracer preparation system |
| CN114837656A (en) * | 2022-05-23 | 2022-08-02 | 河南省科学院同位素研究所有限责任公司 | Preparation method of density controllable isotope carrier |
| CN117072144B (en) * | 2023-06-27 | 2024-05-28 | 河南省科学院同位素研究所有限责任公司 | Preparation device and method of radioactive isotope tracer for injection profile logging |
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| CN108412487A (en) | 2018-08-17 |
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