CN109667574B - Metal ion tracer for multi-section fracturing and application thereof - Google Patents
Metal ion tracer for multi-section fracturing and application thereof Download PDFInfo
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- E—FIXED CONSTRUCTIONS
- E21—EARTH DRILLING; MINING
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Abstract
The invention discloses a metal ion tracer for multistage fracturing, which consists of 28 complex aqueous solutions formed by mixing 28 metal ion compounds with high-temperature complexing agents respectively, wherein the metal ion compounds are chlorides of the following metal elements: scandium, yttrium, vanadium, niobium, tantalum, molybdenum, tungsten, manganese, rhenium, ruthenium, osmium, cobalt, rhodium, iridium, nickel, palladium, platinum, silver, gold, zinc, cadmium, mercury, germanium, tin, lead, antimony, bismuth, and selenium; the high-temperature complexing agent is selected from hydroxyethylidene phosphoric acid, amino trimethylene phosphoric acid, hydroxyethylidene diphosphonic acid, amino trimethylene phosphoric acid, 2, 4-tricarboxylic acid-2-phosphonic butane, diethylenetriamine pentamethylene phosphonic acid or ethylene diamine tetramethylene phosphonic acid. The metal ion tracer for multistage fracturing has good compatibility with hydroxypropyl guar gum and boron gel fracturing fluid, good compatibility with formation water, no precipitation under the formation temperature condition, and the advantages of multiple types, simple preparation, high detection precision, small mutual interference and the like.
Description
Technical Field
The invention relates to a metal ion tracer for multistage fracturing and application thereof, which are used for hydraulic fracturing yield-increasing measures in oilfield development.
Background
In hydraulic fracturing, a high-viscosity liquid (fracturing fluid) is pumped into a well by a ground high-pressure pump set at a discharge capacity exceeding the absorption capacity of a stratum, high pressure is suppressed at the bottom of the well, and when the pressure overcomes the stress near the wall of the well and reaches the tensile strength of a rock, a crack is generated at the bottom of the well. And continuously injecting the fracturing fluid with the proppant, continuously extending the fracture, and filling the proppant in the fracture. After the pump is stopped, a sand filling fracture which is long enough and has certain flow conductivity can be formed in the stratum due to the supporting effect of the propping agent on the fracture. The hydraulic fracturing yield increasing technology for oil and gas well is an effective method for reforming oil and gas layer and an effective measure for increasing yield and injection of oil and gas well and water well. The technology has accumulated over 50 years of experience and is widely applied to oil field exploration and development.
In multi-section fracturing of a vertical inclined well and a horizontal well, due to the fact that the stratum of each measure well section has heterogeneous difference, yield of each section after fracturing construction is greatly different, and monitoring of the yield of fracturing flowback fluid becomes an important work for evaluating fracturing effect. Flowback after frac can be followed up with an aqueous phase tracer. In a method for monitoring a fracturing flow-back fluid by using a tracer, the requirements on the tracer are as follows: good compatibility with fracturing fluid and formation water, small adsorption amount in the formation, high detection precision and the like. Although the types of the tracers in the prior art are many, a plurality of tracers which simultaneously meet the requirements of good compatibility with fracturing fluid, small adsorption quantity in stratum, good stability and high analysis precision and do not mutually interfere with each other cannot be found out.
Chinese patent application publication No. CN103946336A discloses a method of using a controlled release tracer, which is proposed to be immobilized on porous particles or emulsions and slowly released in the formation for the detection of produced hydrocarbons and produced water. The tracer may be a dye, gas, isotope, ionic compound, radioactive material, gene, microorganism, synthetic or natural polymer, fluorine-containing compound, or the like. If an ionic compound, it may form a chelate with a chelating agent (e.g., ethylenediaminetetraacetic acid).
Chinese patent publication No. CN103132986A discloses a method for measuring liquid production rates of different reservoirs of a coal-bed gas well, and provides a method for measuring liquid production rates of different reservoirs of the coal-bed gas well by using a tracer, wherein the used tracer is NaNO3、NH4SCN、NH4NO3、KNO3、KI。
Chinese patent publication No. CN103603655A discloses a tracer for monitoring multi-stage fracturing flow-back fluid and a monitoring method, and proposes a tracer for monitoring multi-stage fracturing flow-back fluid, which includes a tracer element and a complexing agent, wherein the tracer element is praseodymium, neodymium, samarium, europium, gadolinium, terbium, dysprosium, holmium, erbium, thulium, ytterbium and lutetium, the complexing agent is hydroxylamine chloride, and a molar ratio of the two is 1: 8.
At present, no report related to a tracer agent compounded by a metal ion compound and a high-temperature complexing agent is seen.
Disclosure of Invention
Aiming at the prior art, the invention provides a metal ion tracer for multi-stage fracturing and application thereof in monitoring fracturing flowback fluid.
The invention is realized by the following technical scheme:
the metal ion tracer for multistage fracturing consists of 28 kinds of complex aqueous solutions formed by mixing 28 kinds of metal ion compounds with high-temperature complexing agents respectively, wherein the metal ion compounds comprise chlorides of the following metal elements: scandium, yttrium, vanadium, niobium, tantalum, molybdenum, tungsten, manganese, rhenium, ruthenium, osmium, cobalt, rhodium, iridium, nickel, palladium, platinum, silver, gold, zinc, cadmium, mercury, germanium, tin, lead, antimony, bismuth, and selenium; the high-temperature complexing agent is selected from any one or the combination of more than two of hydroxyethylidene phosphoric acid, amino trimethylene phosphoric acid, hydroxyethylidene diphosphonic acid, amino trimethylene phosphoric acid, 2, 4-tricarboxylic acid-2-phosphonic butane, diethylenetriamine pentamethylene phosphonic acid or ethylene diamine tetramethylene phosphonic acid; in each complex aqueous solution, the molar ratio of the metal elements to the high-temperature complexing agent is 1: 3-5; the mass concentration of the metal ion compound is 1% to 5%, preferably 2%.
In the metal ion tracer for multistage fracturing, 28 complex aqueous solutions can be independently prepared and are added into a corresponding fractured stratum one by one when in use, and the dosage of each tracer element complex can be determined according to the specific condition of injection into the stratum.
The preparation method of the metal ion tracer for multi-section fracturing comprises the following steps: adding high-temperature complexing agent into water, stirring uniformly, adding metal ion compound, and continuously stirring for 10min to obtain complex water solution.
The metal ion tracer for multistage fracturing has good compatibility with hydroxypropyl guar gum boron gel fracturing fluid, and the addition amount of the metal ion tracer is 0.001-1%. Good compatibility with formation water and no precipitation under the condition of formation temperature. The method can be used for monitoring the yield and the output speed of the fracturing flow-back fluid, and the specific application method comprises the following steps: adding the metal ion tracer layering section for multistage fracturing into an oil well (added with fracturing fluid) for implementing multistage fracturing measures, and adding different complex aqueous solutions into each layer section; after fracturing construction is finished, in the fracturing fluid flowback process, continuous sampling is carried out on the fracturing flowback fluid, the content of metal ions in the fluid is detected (the concentration of the metal ions can be detected by adopting a liquid chromatography-plasma emission spectrometry), and the yield and the output speed of each stage of the fracturing flowback fluid can be obtained through further calculation, so that the monitoring on the multistage fracturing flowback fluid is realized.
The metal ion tracer for multi-section fracturing has the advantages of multiple types, simplicity in preparation, high detection precision, small mutual interference and the like, and can be used for continuously monitoring the yield and the output speed of multi-section fracturing flow-back fluid.
Drawings
FIG. 1: tracer aging test results schematic, wherein, left beaker: aging the liquid in an oil bath at 120 ℃ for 3 days; right beaker: the liquid was aged in an oil bath at 150 ℃ for 3 days.
FIG. 2: schematic diagram of shear results of fracturing fluid without addition of tracer (at shear rate: 170S)-1Namely: viscosity profile at 170 revolutions per second under shear).
FIG. 3: schematic diagram of shear results of fracturing fluid with tracer (at shear rate of 170S)-1Namely: viscosity profile at 170 revolutions per second under shear).
FIG. 4: the stability result of the tracer under acid-base conditions is shown in a schematic diagram (which shows that if the tracer is not stable in complexation, turbidity and precipitation phenomena can occur, the solution is clear and transparent, and the complexation is stable, and the judgment can be directly carried out through observation).
FIG. 5: the flowback rate of each layer section is shown schematically.
FIG. 6: section 3 returns concentration change schematic diagram.
Detailed Description
The present invention will be further described with reference to the following examples.
The instruments, reagents, materials and the like used in the following examples are conventional instruments, reagents, materials and the like in the prior art and are commercially available in a normal manner unless otherwise specified. Unless otherwise specified, the experimental methods, detection methods, and the like in the following examples are all conventional experimental methods, detection methods, and the like in the prior art.
Example 1
Adding 9.0g of hydroxyethylidene phosphoric acid 206 into 89g of water, stirring uniformly, adding 2.0g of scandium trichloride, and continuously stirring for 10min to obtain a product, wherein the scandium trichloride is contained in the product by 2%.
Example 2
Adding 10.0g of amino trimethylene phosphoric acid 299 into 88g of water, stirring uniformly, adding 2.0g of yttrium trichloride, and continuously stirring for 10min to obtain a product, wherein the product contains 2% of yttrium trichloride.
Example 3
Adding 10.0g of hydroxyethylidene diphosphonic acid into 88g of water, stirring uniformly, adding 2.0g of niobium pentachloride, and continuously stirring for 10min to obtain a product, wherein the niobium pentachloride is 2 percent in the product.
Example 4
Adding 12.0g of hydroxyethylidene diphosphonic acid into 86g of water, stirring uniformly, adding 2.0g of vanadium trichloride, and continuously stirring for 10min to obtain a product, wherein the vanadium trichloride is 2 percent in the product.
Example 5
Adding 12.0g of hydroxyethylidene diphosphonic acid into 86g of water, stirring uniformly, adding 2.0g of molybdenum trichloride, and continuously stirring for 10min to obtain a product, wherein the product contains 2% of molybdenum trichloride.
Example 6
Adding 12.0g of hydroxyethylidene diphosphonic acid into 86g of water, stirring uniformly, adding 2.0g of tantalum pentachloride, and continuously stirring for 10min to obtain a product, wherein the tantalum pentachloride is 2 percent.
Example 7
Adding 13.0g of hydroxyethylidene diphosphonic acid into 85g of water, uniformly stirring, adding 2.0g of tungsten dichloride, and continuously stirring for 10min to obtain the product, wherein the tungsten dichloride is 2 percent in the product.
Example 8
Adding 13.0g of hydroxyethylidene diphosphonic acid into 85g of water, uniformly stirring, adding 2.0g of manganese dichloride, and continuously stirring for 10min to obtain a product, wherein the manganese dichloride is 2 percent in the product.
Example 9
Adding 13.0g of hydroxyethylidene diphosphonic acid into 85g of water, stirring uniformly, adding 2.0g of rhenium trichloride, and continuously stirring for 10min to obtain a product, wherein the rhenium trichloride is 2 percent in the product.
Example 10
Adding 13.0g of hydroxyethylidene diphosphonic acid into 85g of water, stirring uniformly, adding 2.0g of ruthenium trichloride, and continuously stirring for 10min to obtain a product, wherein the ruthenium trichloride is 2 percent in the product.
Example 11
Adding 13.0g of hydroxy ethylidene diphosphonic acid into 85g of water, stirring uniformly, adding 2.0g of osmium trichloride, and continuously stirring for 10min to obtain a product, wherein the osmium trichloride is 2%.
Example 12
Adding 13.0g of hydroxyethylidene diphosphonic acid into 85g of water, stirring uniformly, adding 2.0g of cobalt chloride, and continuously stirring for 10min to obtain a product, wherein the cobalt chloride is 2 percent in the product.
Example 13
Adding 10.0g of amino trimethylene phosphoric acid 299 into 88g of water, stirring uniformly, adding 2.0g of rhodium trichloride 232, and continuously stirring for 10min to obtain a product, wherein the product contains 2% of rhodium trichloride.
Example 14
Adding 10.0g of amino trimethylene phosphoric acid 299 into 88g of water, stirring uniformly, adding 2.0g of iridium trichloride 232, and continuously stirring for 10min to obtain a product, wherein the product contains 2% of iridium trichloride.
Example 15
Adding 10.0g of hydroxyethylidene diphosphonic acid into 88g of water, stirring uniformly, adding 2.0g of nickel chloride, and continuously stirring for 10min to obtain a product, wherein the nickel chloride in the product is 2%.
Example 16
Adding 10.0g of hydroxyethylidene diphosphonic acid into 88g of water, stirring uniformly, adding 2.0g of palladium chloride, and continuously stirring for 10min to obtain a product, wherein the palladium chloride in the product is 2%.
Example 17
Adding 10.0g of hydroxyethylidene diphosphonic acid into 88g of water, stirring uniformly, adding 2.0g of platinum tetrachloride, and continuously stirring for 10min to obtain a product, wherein the product contains 2% of platinum tetrachloride.
Example 18
Adding 10.0g of hydroxyethylidene diphosphonic acid into 88g of water, stirring uniformly, adding 2.0g of silver chloride, and continuously stirring for 10min to obtain a product, wherein the silver chloride in the product is 2%.
Example 19
Adding 10.0g of hydroxyethylidene diphosphonic acid into 88g of water, stirring uniformly, adding 2.0g of gold chloride, and continuously stirring for 10min to obtain a product, wherein the gold chloride is 2 percent in the product.
Example 20
Adding 10.0g of hydroxyethylidene diphosphonic acid into 88g of water, stirring uniformly, adding 2.0g of zinc chloride, and continuously stirring for 10min to obtain a product, wherein the zinc chloride in the product is 2%.
Example 21
Adding 12.0g of hydroxyethylidene diphosphonic acid into 86g of water, stirring uniformly, adding 2.0g of cadmium chloride, and continuously stirring for 10min to obtain a product, wherein the cadmium chloride in the product is 2%.
Example 22
Adding 12.0g of hydroxyethylidene diphosphonic acid into 86g of water, stirring uniformly, adding 2.0g of mercuric chloride, and continuously stirring for 10min to obtain a product, wherein the mercuric chloride in the product is 2%.
Example 23
Adding 10.0g of hydroxyethylidene diphosphonic acid into 88g of water, stirring uniformly, adding 2.0g of germanium dichloride, and continuously stirring for 10min to obtain a product, wherein the content of the germanium dichloride in the product is 2%.
Example 24
Adding 10.0g of hydroxyethylidene diphosphonic acid into 88g of water, stirring uniformly, adding 2.0g of tin chloride, and continuously stirring for 10min to obtain a product, wherein the tin chloride in the product is 2%.
Example 25
Adding 10.0g of hydroxyethylidene diphosphonic acid into 88g of water, stirring uniformly, adding 2.0g of lead chloride, and continuously stirring for 10min to obtain a product, wherein the lead chloride is 2 percent in the product.
Example 26
Adding 10.0g of hydroxyethylidene diphosphonic acid into 88g of water, stirring uniformly, adding 2.0g of antimony chloride, and continuously stirring for 10min to obtain a product, wherein the content of antimony chloride in the product is 2%.
Example 27
Adding 10.0g of hydroxyethylidene diphosphonic acid into 88g of water, stirring uniformly, adding 2.0g of bismuth chloride, and continuously stirring for 10min to obtain a product, wherein the product contains 2% of bismuth chloride.
Example 28
Adding 10.0g of hydroxyethylidene diphosphonic acid into 88g of water, stirring uniformly, adding 2.0g of selenium tetrachloride, and continuously stirring for 10min to obtain a product, wherein the selenium tetrachloride is 2 percent in the product.
Experiment 1: stability of tracer at high temperature conditions of formation
The ion analysis was performed on the formation water of a gas well, and the results are shown in table 1.
TABLE 1 analysis of water ions in formation of a gas well
The well formation water is of calcium chloride water type.
500mL of the formation water was taken, 2.0mL of each of the tracers prepared in examples 1 to 28 was added, the mixture was stirred uniformly and placed in a closed aging tank, the aging tank was heated in an oil bath at 120 ℃ and 150 ℃ for 3 days, the mixture was taken out and poured into a beaker for observation, and no obvious precipitate was found, and the experimental results are shown in FIG. 1. And (4) conclusion: the tracer is stable at formation conditions with a temperature of 150 ℃.
Experiment 2: compatibility of tracer and hydroxypropyl guar gum boron gel fracturing fluid
Preparing a fracturing fluid: 1000g of water, 4.5g of guar gum, 2g of soda ash and 4g of cross-linking agent.
Tracers were prepared according to the methods of examples 1 to 28, 0.5mL each was taken and added to the fracturing fluid.
At a temperature of 110 ℃ and a rate of 170S-1In the shear test, the viscosity of the fracturing fluid after shearing was stabilized at about 60mpa.s and satisfied the predetermined requirement of not less than 50mpa.s, as shown in FIGS. 2 and 3, with respect to the fracturing fluid to which no tracer was added.
Experiment 3: stability of the tracer under acid-base conditions
2.0mL of each of the tracers prepared in examples 1 to 28 was mixed and poured into cups having pHs of 1, 3, 5, 7, 9, 11 and 12. After 24 hours of standing, the solution was still clear and bright, and no precipitate was generated, as shown in FIG. 4.
Experiment 4: adsorption test of tracer
In examples 1 to 28, 100ml of each tracer was prepared, 0.5ml of each tracer was mixed, diluted to 1000ml with water (the concentrations of the metal elements in the tracer are shown in table 2) (the concentrations are mass concentrations), and then the core chips were put into the core chips and left for 24 hours, and the change in concentration was detected, and as a result, as shown in table 2, no significant adsorption phenomenon was observed (data slightly floated due to the apparatus itself).
TABLE 2 detection results of concentrations of metal elements before and after adsorption
| Name (R) | Scandium (Sc) | Yttrium (III) | Vanadium oxide | Niobium (Nb) | Tantalum alloy | Molybdenum (Mo) | Tungsten (W) |
| Concentration (1.0E-5) | 1.077 | 0.921 | 1.049 | 0.944 | 0.987 | 1.006 | 0.913 |
| Post-adsorption concentration (1.0E-5) | 0.935 | 0.97 | 1.058 | 1.033 | 1.018 | 1.045 | 1.041 |
| Name(s) | Manganese oxide | Rhenium | Selenium | Ruthenium (II) | Osmium (III) | Cobalt | Rhodium |
| Concentration (1.0E-5) | 1.053 | 0.967 | 1.065 | 0.928 | 0.93 | 0.973 | 1.062 |
| Concentration after adsorption (1.0E-5) | 0.954 | 1.068 | 1.067 | 0.972 | 0.933 | 1.075 | 1.095 |
| Name(s) | Iridium (III) | Nickel (II) | Palladium (II) | Platinum (II) | Silver (Ag) | Gold (Au) | Zinc |
| Concentration (1.0E-5) | 1.039 | 0.94 | 0.99 | 0.916 | 0.961 | 1.064 | 0.94 |
| Concentration after adsorption (1.0E-5) | 1.09 | 1.018 | 1.046 | 0.995 | 1.012 | 1.035 | 1.081 |
| Name (R) | Cadmium (Cd) | Mercury | Germanium (Ge) | Tin (Sn) | Lead (II) | Antimony (Sb) | Bismuth (III) |
| Concentration (1.0E-5) | 0.918 | 0.957 | 1.049 | 0.943 | 1.064 | 0.937 | 0.91 |
| Concentration after adsorption (1.0E-5) | 1.069 | 1.088 | 1.024 | 0.957 | 1.083 | 0.988 | 1.018 |
Examples of the applications
The specific data of 9 sections of fracturing of a certain well are shown in a table 3.
TABLE 3
1. Preparing corresponding tracers according to the number of the fracturing sections and the liquid amount in the table 3;
2. when in fracturing, the auxiliary agent is injected with an injection pump of a fracturing truck;
3. sampling, testing and analyzing the flow-back liquid.
After the construction is finished, open blowing is carried out on day 1 of 7 months, sampling and testing are carried out from the open blowing, and the construction is finished on day 18 of 10 months.
The results are shown in Table 4 (unit: ppb, i.e., 1.0E-9), FIGS. 5 and 6.
TABLE 4
The following points can be concluded from table 4, fig. 5 and fig. 6:
1) the difference of the flowback rate of each layer section after fracturing is large, which indicates that the energy physical properties of each layer are different;
2) the flowback condition of the 6 th section is poor, and the characteristic layer section can be considered to be abandoned in the subsequent fracturing;
3) the 3 rd stage flowback concentration has 3 wide-interval changes along with time, which indicates that 3 large cracks are formed in the stage of fracturing, and simultaneously, micro cracks are associated, the SRV volume is large, and the fracturing modification effect is good;
4) and more information can be provided for further analysis by matching with the change of production system, logging information and the like.
Although the specific embodiments of the present invention have been described with reference to the examples, the scope of the present invention is not limited thereto, and those skilled in the art will appreciate that various modifications and variations can be made without inventive effort by those skilled in the art based on the technical solution of the present invention.
Claims (1)
1. The application of the metal ion tracer for multi-section fracturing in monitoring fracturing flow-back fluid is characterized in that:
the metal ion tracer for multistage fracturing consists of 28 complex aqueous solutions formed by mixing 28 metal ion compounds with high-temperature complexing agents respectively, wherein the metal ion compounds are chlorides of the following metal elements: scandium, yttrium, vanadium, niobium, tantalum, molybdenum, tungsten, manganese, rhenium, ruthenium, osmium, cobalt, rhodium, iridium, nickel, palladium, platinum, silver, gold, zinc, cadmium, mercury, germanium, tin, lead, antimony, bismuth, and selenium; the high-temperature complexing agent is selected from any one or the combination of more than two of hydroxyethylidene phosphoric acid, amino trimethylene phosphoric acid, hydroxyethylidene diphosphonic acid, amino trimethylene phosphoric acid, 2, 4-tricarboxylic acid-2-phosphonic butane, diethylenetriamine pentamethylene phosphonic acid or ethylene diamine tetramethylene phosphonic acid; in each complex aqueous solution, the molar ratio of the metal element to the high-temperature complexing agent is 1: 3-5; detecting the content of metal ions by adopting a liquid chromatography-plasma emission spectrometry method, wherein the mass concentration of a metal ion compound is 2%; the preparation method of the metal ion tracer for multi-section fracturing comprises the following steps: adding high-temperature complexing agent into water, stirring uniformly, adding metal ion compound, and continuously stirring for 10min to obtain complex water solution;
the application method comprises the following steps: adding the multi-section metal ion tracer for fracturing into an oil well for implementing multi-stage fracturing measures in a layered manner, and adding different complex aqueous solutions into each layer section; after fracturing construction is finished, in the fracturing fluid flowback process, continuous sampling is carried out on the fracturing flowback fluid, the metal ion content in the fluid is detected, the output and the output speed of each section of fracturing flowback fluid are further calculated, and therefore monitoring on the multistage fracturing flowback fluid is achieved.
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