CN117468920A - Preparation method of slow-release DNA tracer - Google Patents
Preparation method of slow-release DNA tracer Download PDFInfo
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- CN117468920A CN117468920A CN202311182281.2A CN202311182281A CN117468920A CN 117468920 A CN117468920 A CN 117468920A CN 202311182281 A CN202311182281 A CN 202311182281A CN 117468920 A CN117468920 A CN 117468920A
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- 239000000700 radioactive tracer Substances 0.000 title claims abstract description 101
- 238000002360 preparation method Methods 0.000 title claims abstract description 11
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims abstract description 133
- 235000012239 silicon dioxide Nutrition 0.000 claims abstract description 38
- 239000000377 silicon dioxide Substances 0.000 claims abstract description 35
- 239000002245 particle Substances 0.000 claims abstract description 34
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 30
- 239000005543 nano-size silicon particle Substances 0.000 claims abstract description 29
- 229920000642 polymer Polymers 0.000 claims abstract description 20
- 239000012634 fragment Substances 0.000 claims abstract description 12
- 238000001035 drying Methods 0.000 claims abstract description 7
- 239000007787 solid Substances 0.000 claims abstract description 7
- 238000012986 modification Methods 0.000 claims abstract description 5
- 230000004048 modification Effects 0.000 claims abstract description 5
- 238000012258 culturing Methods 0.000 claims abstract description 4
- 238000006116 polymerization reaction Methods 0.000 claims abstract description 4
- 238000007711 solidification Methods 0.000 claims abstract description 4
- 230000008023 solidification Effects 0.000 claims abstract description 4
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 claims description 27
- 239000002244 precipitate Substances 0.000 claims description 16
- 238000000034 method Methods 0.000 claims description 15
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 11
- 239000000203 mixture Substances 0.000 claims description 10
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims description 9
- 238000002156 mixing Methods 0.000 claims description 6
- 239000006228 supernatant Substances 0.000 claims description 6
- 229920000371 poly(diallyldimethylammonium chloride) polymer Polymers 0.000 claims description 5
- 229920000036 polyvinylpyrrolidone Polymers 0.000 claims description 5
- 239000001267 polyvinylpyrrolidone Substances 0.000 claims description 5
- 235000013855 polyvinylpyrrolidone Nutrition 0.000 claims description 5
- BOTDANWDWHJENH-UHFFFAOYSA-N Tetraethyl orthosilicate Chemical compound CCO[Si](OCC)(OCC)OCC BOTDANWDWHJENH-UHFFFAOYSA-N 0.000 claims description 4
- 239000007788 liquid Substances 0.000 claims description 4
- 239000002105 nanoparticle Substances 0.000 claims description 4
- 238000003260 vortexing Methods 0.000 claims description 4
- NLXLAEXVIDQMFP-UHFFFAOYSA-N Ammonium chloride Substances [NH4+].[Cl-] NLXLAEXVIDQMFP-UHFFFAOYSA-N 0.000 claims description 3
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 claims description 3
- 235000011114 ammonium hydroxide Nutrition 0.000 claims description 3
- 238000006243 chemical reaction Methods 0.000 claims description 3
- 238000002715 modification method Methods 0.000 claims description 3
- 239000011241 protective layer Substances 0.000 claims description 3
- 238000003756 stirring Methods 0.000 claims description 3
- 238000013268 sustained release Methods 0.000 claims 2
- 239000012730 sustained-release form Substances 0.000 claims 2
- 239000003054 catalyst Substances 0.000 claims 1
- 238000004519 manufacturing process Methods 0.000 abstract description 7
- 238000012544 monitoring process Methods 0.000 abstract description 4
- 230000009286 beneficial effect Effects 0.000 abstract description 2
- 239000011248 coating agent Substances 0.000 abstract 1
- 238000000576 coating method Methods 0.000 abstract 1
- 108020004414 DNA Proteins 0.000 description 58
- 239000000243 solution Substances 0.000 description 15
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 description 13
- 238000011161 development Methods 0.000 description 6
- 239000003921 oil Substances 0.000 description 6
- 239000011780 sodium chloride Substances 0.000 description 6
- 239000010410 layer Substances 0.000 description 5
- 229910021642 ultra pure water Inorganic materials 0.000 description 4
- 239000012498 ultrapure water Substances 0.000 description 4
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 description 3
- 229910004298 SiO 2 Inorganic materials 0.000 description 3
- 230000005465 channeling Effects 0.000 description 3
- 239000011521 glass Substances 0.000 description 3
- 239000000725 suspension Substances 0.000 description 3
- 239000003795 chemical substances by application Substances 0.000 description 2
- 230000007423 decrease Effects 0.000 description 2
- 238000009826 distribution Methods 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 235000019441 ethanol Nutrition 0.000 description 2
- 238000011156 evaluation Methods 0.000 description 2
- 230000001965 increasing effect Effects 0.000 description 2
- 210000002445 nipple Anatomy 0.000 description 2
- 239000012071 phase Substances 0.000 description 2
- 238000005070 sampling Methods 0.000 description 2
- 239000012085 test solution Substances 0.000 description 2
- 238000005406 washing Methods 0.000 description 2
- QGZKDVFQNNGYKY-UHFFFAOYSA-O Ammonium Chemical compound [NH4+] QGZKDVFQNNGYKY-UHFFFAOYSA-O 0.000 description 1
- 108091026890 Coding region Proteins 0.000 description 1
- 238000007171 acid catalysis Methods 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 239000008346 aqueous phase Substances 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 230000000903 blocking effect Effects 0.000 description 1
- 238000006555 catalytic reaction Methods 0.000 description 1
- 238000012512 characterization method Methods 0.000 description 1
- 229910052681 coesite Inorganic materials 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- 229910052906 cristobalite Inorganic materials 0.000 description 1
- 239000010779 crude oil Substances 0.000 description 1
- 238000005520 cutting process Methods 0.000 description 1
- 238000007405 data analysis Methods 0.000 description 1
- 239000008367 deionised water Substances 0.000 description 1
- 229910021641 deionized water Inorganic materials 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000006073 displacement reaction Methods 0.000 description 1
- 238000005553 drilling Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 230000002708 enhancing effect Effects 0.000 description 1
- 231100000584 environmental toxicity Toxicity 0.000 description 1
- 239000012530 fluid Substances 0.000 description 1
- JEGUKCSWCFPDGT-UHFFFAOYSA-N h2o hydrate Chemical compound O.O JEGUKCSWCFPDGT-UHFFFAOYSA-N 0.000 description 1
- 230000015784 hyperosmotic salinity response Effects 0.000 description 1
- 238000002347 injection Methods 0.000 description 1
- 239000007924 injection Substances 0.000 description 1
- 238000013508 migration Methods 0.000 description 1
- 230000005012 migration Effects 0.000 description 1
- 239000003960 organic solvent Substances 0.000 description 1
- 238000004806 packaging method and process Methods 0.000 description 1
- 230000035699 permeability Effects 0.000 description 1
- 230000000379 polymerizing effect Effects 0.000 description 1
- 229920000193 polymethacrylate Polymers 0.000 description 1
- -1 polytetrafluoroethylene Polymers 0.000 description 1
- 229920001343 polytetrafluoroethylene Polymers 0.000 description 1
- 239000004810 polytetrafluoroethylene Substances 0.000 description 1
- 230000008569 process Effects 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
- 230000035945 sensitivity Effects 0.000 description 1
- 229910052682 stishovite Inorganic materials 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 229910052905 tridymite Inorganic materials 0.000 description 1
- 229920002554 vinyl polymer Polymers 0.000 description 1
- 229920003169 water-soluble polymer Polymers 0.000 description 1
Classifications
-
- 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
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01V—GEOPHYSICS; GRAVITATIONAL MEASUREMENTS; DETECTING MASSES OR OBJECTS; TAGS
- G01V9/00—Prospecting or detecting by methods not provided for in groups G01V1/00 - G01V8/00
Landscapes
- Physics & Mathematics (AREA)
- Life Sciences & Earth Sciences (AREA)
- Geophysics (AREA)
- Engineering & Computer Science (AREA)
- Geology (AREA)
- Mining & Mineral Resources (AREA)
- General Life Sciences & Earth Sciences (AREA)
- Environmental & Geological Engineering (AREA)
- Fluid Mechanics (AREA)
- Geochemistry & Mineralogy (AREA)
- General Physics & Mathematics (AREA)
- Measuring Or Testing Involving Enzymes Or Micro-Organisms (AREA)
Abstract
The invention discloses a preparation method of a slow-release DNA tracer, which comprises the following steps: s1, preparing nano silicon dioxide particles; s2, carrying out surface positive charge modification on the prepared nano silicon dioxide particles; s3, binding the DNA fragments to the surfaces of the modified nano silicon dioxide particles; s4, attaching a polymer on the surface of the nano silicon dioxide particles combined with the DNA fragments; s5, culturing a silica nano protection layer on the surface of the nano silica particles with the DNA fragments attached with the polymer to obtain a silica coated DNA tracer; s6, carrying out polymerization, solidification and drying treatment on the DNA tracer to obtain a solid DNA tracer, coating the DNA tracer in silicon dioxide and encapsulating the solid DNA tracer in a high polymer skeleton, and realizing slow release and controllable release of the DNA tracer in water phase flow by changing the types, the temperatures and the salinity of the polymer, thereby being beneficial to the use of well sites and being capable of meeting the actual requirements of multi-layer section water production fine monitoring.
Description
Technical Field
The invention relates to the field of horizontal well drilling development devices, in particular to a preparation method of a slow-release DNA tracer.
Background
With the vigorous development of horizontal well development technology, more and more researches focus on the method for improving quality and enhancing efficiency of low-permeability oil reservoirs, hydraulic fracturing is changed into a core development means for improving the productivity of oil and gas wells due to the problems of low permeability, poor fluidity and the like of low-permeability oil fields, and a complex fracture system is formed by fracturing artificial fractures in stratum so as to obtain larger oil and gas migration channels.
However, due to factors such as wellbore pressure and formation heterogeneity, the channeling phenomenon of injected water in a reservoir is serious, so that the water-taking time of a production well is early, the water content is high, crude oil in a part of dense matrixes is difficult to be swept and extracted, the development effect of the reservoir is low, a series of water shutoff water and water terrorism measures are used for preventing the channeling and the channeling phenomenon of the injected water so as to improve the water injection exploitation efficiency, however, how to effectively identify the water outlet position of a horizontal section is critical to the development effect of the horizontal well, the current common method is a tracer monitoring method, the horizontal section is divided into a plurality of units for separate exploitation, the tracer is installed in a groove of a horizontal section completion pipe string, the concentration of the tracer is analyzed through sampling after well production, the data analysis is carried out on the production condition, the water outlet characteristics of the production section are judged, the water outlet amount is low, but the current tracer is mostly chemical tracer or isotope tracer, the quantity in the water is small, the stability is poor, and uncontrollable, and the detection efficiency is low.
Disclosure of Invention
Aiming at the problems, the invention provides a preparation method of a slow-release DNA tracer, which has the advantages that a water-soluble polymer can be encapsulated on the outer layer of a silica coated DNA tracer, so that a functional tracer which is slowly released in a water phase is obtained, and the controllable release of the tracer in the water-finding monitoring application of a horizontal well is realized.
The technical scheme of the invention is as follows:
a preparation method of a slow-release DNA tracer comprises the following steps:
s1, preparing nano silicon dioxide particles;
s2, carrying out surface positive charge modification on the prepared nano silicon dioxide particles;
s3, binding the DNA fragments to the surfaces of the modified nano silicon dioxide particles;
s4, attaching a polymer on the surface of the nano silicon dioxide particles combined with the DNA fragments;
s5, culturing a silica nano protection layer on the surface of the nano silica particles with the DNA fragments attached with the polymer to obtain a silica coated DNA tracer;
and S6, performing polymerization, solidification and drying treatment on the DNA tracer to obtain the solid DNA tracer.
The preparation method of the nano silicon dioxide particles in the step S1 is as follows:
1) Ethanol, TEOS, milli-Q H 2 Mixing O and ammonia solution, shaking and uniformly mixing, and keeping the room temperature for 4-8 hours;
2) Centrifuging the mixture to remove supernatant to obtain precipitate;
3) Suspending the precipitate with isopropanol;
4) Repeating the step 2) and the step 3), and concentrating to obtain the nano silicon dioxide particles.
The step 3) suspension of the precipitate with isopropanol requires vortexing the tube and sonicating in a water bath.
The step S2 is characterized in that the surface modification method of the nano silicon dioxide particles comprises the following steps:
a. adding TMAPS (50 wt% methanol solution) solution into the nano silicon dioxide particles, oscillating, mixing and stirring for 10-14h;
b. centrifuging the mixture to remove supernatant to obtain precipitate;
c. suspending the precipitate with isopropanol;
d. and c, repeating the step b and the step c, and concentrating to obtain the modified nano silicon dioxide particles.
The suspension of the precipitate with isopropanol in step c requires vortexing the tube and sonicating in a water bath.
In the step S4, the polymer is polydiallyl dimethyl ammonium chloride and polyvinylpyrrolidone.
The concentration of the polydiallyl dimethyl ammonium chloride solution is 1.0mg/mL, and the concentration of the polyvinylpyrrolidone solution is 0.1mg/mL.
The step S5, the silica nano-protective layer is formed by dispersing polymer-attached nano-particles in the catalysisThe reaction solution is formed.
And step S6, mixing the nano silicon dioxide coated DNA tracer prepared in the step S5 with a high molecular polymer, polymerizing the nano silicon dioxide coated DNA tracer into liquid, and drying and solidifying to obtain the solid DNA tracer.
The beneficial effects of the invention are as follows:
by the method, the DNA tracer is coated in the silicon dioxide and encapsulated in the high polymer skeleton, the slow release and controllable release of the DNA tracer in the water phase flow can be realized by changing the types, the temperature and the salinity of the polymer, the quantity of the tracer can be amplified by utilizing the advantages of DNA coding, the composition and the structural characteristics of the DNA, the problems of small quantity, large consumption, low sensitivity, large environmental toxicity and the like of the conventional tracer can be solved, the use of a well site is facilitated, and the actual requirements of multi-layer section water production fine monitoring can be met.
Drawings
FIG. 1 is a schematic diagram of the overall structure of a slow-release DNA tracer according to an embodiment of the invention;
FIG. 2 is a graph showing concentration versus time of a slow-release DNA tracer according to an embodiment of the invention when it is left in pure water;
FIG. 3 is a graph showing the concentration versus time of a slow-release DNA tracer added to a NaCl solution according to an embodiment of the present invention.
Detailed Description
Embodiments of the present invention are further described below with reference to the accompanying drawings.
As shown in fig. 1, a preparation method of the slow-release DNA tracer comprises the following steps:
s1, preparing nano silicon dioxide particles;
s2, carrying out surface positive charge modification on the prepared nano silicon dioxide particles;
s3, binding the DNA fragments to the surfaces of the modified nano silicon dioxide particles;
s4, attaching a polymer on the surface of the nano silicon dioxide particles combined with the DNA fragments;
s5, culturing a silica nano protection layer on the surface of the nano silica particles with the DNA fragments attached with the polymer to obtain a silica coated DNA tracer;
and S6, performing polymerization, solidification and drying treatment on the DNA tracer to obtain the solid DNA tracer.
The preparation method comprises the following steps:
the preparation method of the nano silicon dioxide particles comprises the following steps:
(1) 18mL of ethanol, 0.8mL of TEOS and 0.5mL of Milli-Q H O were mixed in a 50mL conical tube, and 0.8mL (25 wt.%) ammonia solution was added. The mixture was shaken at 900rpm/min and kept at room temperature (25 ℃) for 6h;
(2) Centrifuging the mixture at room temperature for 20min, discarding supernatant, taking 5mL, and packaging in a tube;
(3) The precipitate was suspended with 2mL of isopropanol (the tube was vortexed for several seconds and sonicated in a water bath for 5 min);
(4) Repeating the steps (2) and (3), centrifuging the tube at 15,000g for 6min at room temperature;
(5) The precipitate was suspended in 1mL of isopropanol to give nanosilica (50 mg/mL).
The surface modification method of the nano silicon dioxide particles comprises the following steps:
(1) To 1mL (50 mg/mL) of the nanosilica prepared above was added 40. Mu.L of TMAPS (50 wt.% methanol solution);
(2) The mixture was stirred at 900rpm/min at room temperature for 12h;
(3) The tube was centrifuged at 18,930g for 4min at room temperature and the supernatant was discarded; (washing twice)
(4) The precipitate was suspended in 2mL of isopropanol (the tube was vortexed for a few seconds and sonicated in the bath for 3 min);
(5) Repeating the steps (3) and (4), suspending the precipitate in 1mL of isopropanol, and preserving at room temperature. The surface potential of the modified nano silicon dioxide is about +25mV to +35mV.
Add 250. Mu.L, 50mg/L DNA solution to 110. Mu.L, 50mg/mL positive charge modified SiO 2 The nanoparticle suspension is shaken for 5min on a mini-mixer, and centrifugally and ultrasonically cleaned; the DNA is a coding sequence, and the number of bases is more than or equal to 80.
To 500. Mu.L of a 1.0mg/mL polydiallyl dimethyl ammonium chloride solution was added, and after shaking at 900rpm for 20min at room temperature, the particles were washed twice with ultrapure water. The particles were then dispersed in 1.0mL of a 0.1mg/mL polyvinylpyrrolidone solution, shaken at 900rpm for 20min at room temperature, and then washed once with ultrapure water and then with absolute ethanol.
Dispersing the washed nanoparticles in acid catalysisThe mixture was shaken at 900rpm for 10 hours in a reaction solution (500. Mu.L of absolute ethanol, 125. Mu.L of ultrapure water, 44. Mu.L of ethyl orthosilicate, 10M, 10. Mu.L of acetic acid) to grow a SiO2 layer. And then washing the DNA tracer with absolute ethyl alcohol, ultrapure water and isopropanol once respectively to obtain the silica coated DNA tracer.
The ammonium polymethacrylate, vinyl polymer and silica coated DNA tracer are filled into Schott bottles and put into a drying oven to be softened for 30min and then become low-viscosity liquid. Stirring the low-viscosity liquid uniformly, pouring the mixture into a polytetrafluoroethylene mould, putting the mould into a drying oven at 120 ℃, solidifying for 1h, and cooling to room temperature. Taking out the solidified tracer, cutting into small blocks to obtain the slow-release silicon dioxide coated DNA tracer
The use method of the slow-release silica coated DNA tracer comprises the following steps:
simulating an oil pipe string nipple by using core holders, wherein the inlet end of each core holder is independently connected with a constant flow pump, the outlet section is connected with a glass column branch, and one end of the glass column is closed and the other end of the glass column is connected with a sampling container;
different slow-release silica coated DNA tracer sample blocks are fixed on the corresponding core holder cylinder wall by means of embedding, pasting, punching, binding, magnetic attraction and the like, a screen pipe is added outside the tracer wire belt, the type and the mark number of the tracer belt installed in each unit nipple are marked, the screen pipe provided with the tracer belt is connected with an oil pipe, and the screen pipe is arranged on a corresponding horizontal section; displacing the aqueous phase fluid into different core holders through each constant flow pump, stopping displacement after the core holders are filled with injected water, and closing the outlet valve of the core holders; the tracer samples discharged by the core holder are obtained at fixed time, and the content of each silicon dioxide coated DNA tracer in the tracer samples is measured; and acquiring the water production contribution rate in a unit time period according to the content and the discharge time of the silica coated DNA tracer, so that a series of water blocking and controlling measures are developed, and the recovery ratio is improved. .
Characterization analysis:
dispersing the silica-coated DNA tracer in an organic solvent, and analyzing the morphology of the tracer by using an electron microscope to determine that the silica-coated DNA tracer particles are spherical.
Evaluation of performance:
the silica-coated DNA tracer was prepared as a 20. Mu.g/mL solution, 500. Mu.L of the solution was stored under a sealed condition at 30℃and 60℃and 90℃for 7 days, and the temperature stability of the silica-coated DNA tracer was evaluated by comparing the variation of the hydrated particle size of the silica-coated DNA tracer at different temperatures, and the results are shown in Table 1.
TABLE 1 DNA@SiO 2 Hydrated particle size distribution of tracers at different temperatures
Further, naCl solutions with concentrations of 0, 10000mg/L, 30000mg/L and 50000mg/L were prepared, 4mL of each was added with 10. Mu.L of a 5.4mg/L silica-coated DNA tracer, each tube was allowed to stand at room temperature for 48 hours, and the salt tolerance of the silica-coated DNA tracer was evaluated by comparing the variation in the hydrated particle size of the silica-coated DNA tracer under different salinity, and the results are shown in Table 2.
TABLE 2 DNA@SiO 2 Hydrated particle size distribution of tracers at different salinity
Release behavior evaluation:
the slow-release silica coated DNA tracer is placed in pure water and placed in water baths with the temperature of 30 ℃, 60 ℃ and 90 ℃ respectively. The concentration of the DNA tracer in the test solution environment was sampled at 0min, 5min, 15min, 20min, 30min, 45min, 60min, 90min and 120min, respectively, and the concentration-time curves were plotted as shown in FIG. 2.
From this graph, it can be seen that the polymer-encapsulated DNA tracer strip released faster within 30min, after which the release process was slower within 90 min. At 30 ℃, the polymer releases the DNA tracer at a slower rate, the concentration of the tracer being only about 30% of the total concentration of the tracer in 120 min. When the temperature is 60 ℃, the release amount of the tracer is obviously improved, 80% of the total amount is released within 60min, and about 90% of the total amount is released within 120 min. When the temperature continues to rise to 90 ℃ and above, the tracer is released rapidly from the polymer and can be released completely within 60 minutes only. The results show that an increase in temperature favors the release of the tracer and that the concentration of tracer released tends to be constant with the release time.
Preparing NaCl solution to replace stratum water, preparing mineralized water and deionized water blank groups with mineralized degrees of 10000mg/L, 30000mg/L and 50000mg/L respectively, adding a slow-release silica coated DNA tracer agent with a certain mass, and standing in a constant temperature environment (20 ℃) to enable the DNA tracer agent to be released stably. The release behavior was evaluated over 48h, the concentration of the DNA tracer in the test solution environment was sampled at 5min, 30min, 1h, 2h, 3h, 6h, 8h, 12h, 34h, 38h and 48h, respectively, and the concentration-time curves were plotted as shown in fig. 3.
From this graph, it can be seen that when the NaCl concentration is 0, the tracer concentration becomes larger with the increase in time. Within 24 hours, about 80% of the DNA tracer coated in the polymer is released, and within 48 hours the DNA tracer can be completely released. When the NaCl concentration is 10000mg/L, 60% of the tracer is released within 24 hours, and the tracer is not completely released after 48 hours. When the NaCl concentration is 30000mg/L, the release amount of the tracer is greatly reduced, and the tracer is only released by about 50% within 24 hours. When the NaCl concentration is increased to 50000mg/L, the tracer release amount in the same time gradually decreases along with the extension of time, and the tracer release amount only accounts for about 60% of the total tracer after 48 hours. The results show that with increasing salinity, the tracer release amount decreases significantly, revealing that salinity can be an effective parameter for controlling DNA tracer release in the polymer.
The foregoing examples merely illustrate specific embodiments of the invention, which are described in greater detail and are not to be construed as limiting the scope of the invention. It should be noted that it will be apparent to those skilled in the art that several variations and modifications can be made without departing from the spirit of the invention, which are all within the scope of the invention.
Claims (9)
1. The preparation method of the slow-release DNA tracer is characterized by comprising the following steps of:
s1, preparing nano silicon dioxide particles;
s2, carrying out surface positive charge modification on the prepared nano silicon dioxide particles;
s3, binding the DNA fragments to the surfaces of the modified nano silicon dioxide particles;
s4, attaching a polymer on the surface of the nano silicon dioxide particles combined with the DNA fragments;
s5, culturing silicon dioxide (SiO) on the surface of the nanometer silicon dioxide particles with the DNA fragments attached with the polymer 2 ) A nano protective layer is used for obtaining the DNA tracer coated with silicon dioxide;
and S6, performing polymerization, solidification and drying treatment on the DNA tracer to obtain the solid DNA tracer.
2. The method for preparing a slow release DNA tracer according to claim 1, wherein in the step S1, the method for preparing nano silica particles comprises the following steps:
1) Ethanol, TEOS, milli-QH 2 Mixing O and ammonia solution, shaking and uniformly mixing, and keeping the room temperature for 4-8 hours;
2) Centrifuging the mixture to remove supernatant to obtain precipitate;
3) Suspending the precipitate with isopropanol;
4) Repeating the step 2) and the step 3), and concentrating to obtain the nano silicon dioxide particles.
3. A method of preparing a slow release DNA tracer according to claim 2, wherein in step 3), the precipitate is suspended with isopropanol by vortexing the tube and sonicating it in a water bath.
4. The method for preparing a slow release DNA tracer according to claim 1, wherein in the step S2, the surface modification method of the nano silica particles is as follows:
a. adding TMAPS (50 wt.% methanol solution) solution into the nano silicon dioxide particles, and stirring and shaking for 10-14h;
b. centrifuging the mixture to remove supernatant to obtain precipitate;
c. suspending the precipitate with isopropanol;
d. and c, repeating the step b and the step c, and concentrating to obtain the modified nano silicon dioxide particles.
5. The method of preparing a slow release DNA tracer according to claim 4, wherein in step c, the precipitate is suspended with isopropyl alcohol by vortexing the tube and sonicating it in a water bath.
6. The method for preparing a sustained-release DNA tracer according to claim 1, wherein in the step S4, the polymer is polydiallyl dimethyl ammonium chloride or polyvinylpyrrolidone.
7. The method for preparing a sustained-release DNA tracer according to claim 6, wherein the concentration of the polydiallyl dimethyl ammonium chloride solution is 1.0mg/mL, and the concentration of the polyvinylpyrrolidone solution is 0.1mg/mL.
8. The method for preparing a slow release DNA tracer according to claim 1, wherein in the step S5, the silica nano-protective layer is prepared by dispersing polymer-attached nano-particles in a catalystThe reaction solution is formed.
9. The method for preparing a slow release DNA tracer according to claim 1, wherein in step S6, the DNA tracer coated with nano silica prepared in step S5 is mixed with a high molecular polymer, and the DNA tracer coated with nano silica is polymerized into a liquid and dried and solidified to obtain a solid DNA tracer.
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| CN202311182281.2A CN117468920A (en) | 2023-09-14 | 2023-09-14 | Preparation method of slow-release DNA tracer |
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| CN202311182281.2A CN117468920A (en) | 2023-09-14 | 2023-09-14 | Preparation method of slow-release DNA tracer |
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