WO2024066592A1 - Test method and device for the adaptability of water-based completion fluid in crude oil containing hydrogen sulfide - Google Patents

Test method and device for the adaptability of water-based completion fluid in crude oil containing hydrogen sulfide Download PDF

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WO2024066592A1
WO2024066592A1 PCT/CN2023/104395 CN2023104395W WO2024066592A1 WO 2024066592 A1 WO2024066592 A1 WO 2024066592A1 CN 2023104395 W CN2023104395 W CN 2023104395W WO 2024066592 A1 WO2024066592 A1 WO 2024066592A1
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Prior art keywords
completion fluid
hydrogen sulfide
temperature
crude oil
pressure
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PCT/CN2023/104395
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French (fr)
Chinese (zh)
Inventor
刘会锋
陈怀龙
柴辉
文光耀
巴勒塔别克巴合达尔
程维恒
李万军
顾亦新
周海秋
张玮
Original Assignee
中国石油天然气集团有限公司
中国石油集团工程技术研究院有限公司
中国石油国际勘探开发有限公司
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Publication of WO2024066592A1 publication Critical patent/WO2024066592A1/en

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    • EFIXED CONSTRUCTIONS
    • E21EARTH OR ROCK DRILLING; MINING
    • E21BEARTH OR ROCK DRILLING; OBTAINING OIL, GAS, WATER, SOLUBLE OR MELTABLE MATERIALS OR A SLURRY OF MINERALS FROM WELLS
    • E21B34/00Valve arrangements for boreholes or wells
    • E21B34/06Valve arrangements for boreholes or wells in wells
    • EFIXED CONSTRUCTIONS
    • E21EARTH OR ROCK DRILLING; MINING
    • E21BEARTH OR ROCK DRILLING; OBTAINING OIL, GAS, WATER, SOLUBLE OR MELTABLE MATERIALS OR A SLURRY OF MINERALS FROM WELLS
    • E21B34/00Valve arrangements for boreholes or wells
    • E21B34/06Valve arrangements for boreholes or wells in wells
    • E21B34/10Valve arrangements for boreholes or wells in wells operated by control fluid supplied from outside the borehole
    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N33/00Investigating or analysing materials by specific methods not covered by groups G01N1/00 - G01N31/00

Definitions

  • the invention relates to a method and equipment for testing the adaptability of a water-based completion fluid in crude oil containing hydrogen sulfide, and belongs to the technical field of petroleum engineering.
  • the industry generally uses two methods to evaluate the hydrogen sulfide resistance of completion fluids: one is to first prepare a dilute solution of hydrogen sulfide (i.e., hydrosulfuric acid) and mix it with the completion fluid to test its hydrogen sulfide resistance; the other is to put the completion fluid in a high-temperature and high-pressure reactor and then pass hydrogen sulfide gas into the completion fluid to test its hydrogen sulfide resistance. Both methods cannot simulate the real interface reaction state and cannot simulate the actual concentration of hydrogen sulfide. Testing the hydrogen sulfide resistance of completion fluids has always been one of the problems that need to be solved in this field.
  • a dilute solution of hydrogen sulfide i.e., hydrosulfuric acid
  • the purpose of the present invention is to provide a method and equipment for testing the adaptability of water-based completion fluid in crude oil containing hydrogen sulfide.
  • the testing method provided by the present invention can simulate the interface reaction between the completion fluid and the crude oil containing hydrogen sulfide in the formation when the completion fluid is in a well-killing state, and accurately judge the adaptability of the water-based completion fluid in crude oil containing hydrogen sulfide.
  • the first aspect of the present invention provides a method for testing the adaptability of a water-based completion fluid in hydrogen sulfide-containing crude oil, which comprises the following steps:
  • testing the completion fluid to be tested wherein the testing at least includes testing the basic properties of the completion fluid to be tested, and the basic properties testing of the completion fluid to be tested at least includes density testing;
  • testing the completion fluid after the reaction wherein the testing at least includes testing the basic properties of the completion fluid after the reaction, and the basic properties of the completion fluid after the reaction at least includes density testing;
  • step (7) Based at least on the test result of the completion fluid to be tested obtained in step (1) and the test result of the completion fluid after reaction obtained in step (6), determine whether the completion fluid is suitable for use in crude oil containing hydrogen sulfide.
  • the test method further comprises a preliminary screening after step (1), wherein the preliminary screening comprises:
  • (a)-3 Heat the high-temperature and high-pressure reactor to a set temperature, adjust its pressure to normal pressure as the set pressure, and then keep it stable; measure the temperature of the high-temperature and high-pressure reactor at regular intervals, and if the temperature is different from the set temperature, adjust the temperature of the high-temperature and high-pressure reactor to make it the same as the set temperature;
  • testing at least includes testing the basic properties of the completion fluid after the reaction, and the basic properties of the completion fluid after the reaction at least includes density testing;
  • (a)-6 Preliminarily determine whether the completion fluid is suitable for crude oil containing hydrogen sulfide based at least on the test results of the completion fluid to be tested and the test results of the completion fluid after the reaction, and perform steps (2) to (7) on the completion fluid that is preliminarily determined to be suitable for crude oil containing hydrogen sulfide to finally determine whether the completion fluid is suitable for crude oil containing hydrogen sulfide.
  • step (1) since the above step (1) has already carried out basic performance testing on the completion fluid to be tested, it is not necessary to repeat the basic performance testing on the completion fluid to be tested during the preliminary screening process.
  • the basic property test of the completion fluid to be tested also includes one or a combination of pH value detection, viscosity detection, crystallization temperature detection and turbidity detection.
  • the detection of the completion fluid to be tested also includes detecting the ion content of the completion fluid to be tested.
  • step (2) and step (a)-1 the amount of crude oil pumped into the high temperature and high pressure reactor is 1000 to 3000 mL.
  • step (2) and step (a)-1 the time for introducing hydrogen sulfide gas is 1.5 to 2.5 hours, so that the crude oil is saturated with hydrogen sulfide, that is, the crude oil is dissolved with as much hydrogen sulfide as possible, while the influence of other residual gases in the reactor is eliminated to the greatest extent possible.
  • step (2) and step (a)-1 further include: introducing carbon dioxide gas into the high temperature and high pressure reactor for a period of time until the crude oil is saturated with hydrogen sulfide and carbon dioxide.
  • the time for introducing hydrogen sulfide gas and carbon dioxide gas can be 1.5 to 2.5 hours.
  • the deoxygenation method of the completion fluid to be tested can be a conventional completion fluid deoxygenation method in the art, preferably, the deoxygenation method can be activated carbon deoxygenation.
  • the specific operation method of the activated carbon deoxygenation and the dosage ratio of the activated carbon and the completion fluid to be tested can be conventionally adjusted by those skilled in the art.
  • step (3) and step (a)-2 the amount of the deoxygenated completion fluid to be tested introduced into the high temperature and high pressure reactor is 1000-3000 mL.
  • the amount of crude oil pumped into the high-temperature and high-pressure reactor is the same as the amount of the deoxygenated completion fluid to be tested introduced into the high-temperature and high-pressure reactor.
  • step (4) the fugacity of hydrogen sulfide is calculated according to the following formula (1):
  • the partial pressure of hydrogen sulfide is the partial pressure of hydrogen sulfide in the crude oil containing hydrogen sulfide.
  • the specific calculation method is conventional in the art. Generally speaking, it is obtained by multiplying the total system pressure (that is, the formation pressure of the crude oil containing hydrogen sulfide) by the molar fraction of hydrogen sulfide in the gas phase. The calculation can also be performed using conventional methods in the art.
  • the calculation can be performed according to the formula for calculating the fugacity coefficient of components in a mixture obtained by combining the SRK equation with the one-parameter van der Waals mixing rule disclosed on pages 6 to 8 of "Improvement of the SRK equation and its application in phase equilibrium calculations" (Luo Mingjian, master's thesis of Tianjin University, December 2005), that is, formula (2-34).
  • the set temperature is the crude oil temperature of the completion fluid working formation to be tested, and more preferably can be 80-120°C.
  • step (4) the temperature and pressure of the high temperature and high pressure reactor are measured every 60 to 80 hours.
  • step (a)-3 the temperature of the high temperature and high pressure reactor is measured once every 24 to 80 hours. More preferably, the temperature of the high temperature and high pressure reactor is measured once every 60 to 80 hours.
  • the temperature of the high-temperature and high-pressure reactor is adjusted by the intensity of heating, and the pressure of the high-temperature and high-pressure reactor is adjusted by passing hydrogen sulfide gas.
  • hydrogen sulfide gas is passed into the high-temperature and high-pressure reactor to supplement the pressure to the set pressure.
  • the flow rate of the hydrogen sulfide gas is less than 10mm/min, and the flow rate is 150-250mL/min (especially preferably 200mL/min).
  • step (2) also includes: passing carbon dioxide gas into the high-temperature and high-pressure reactor for a period of time until the crude oil is saturated with hydrogen sulfide and carbon dioxide
  • the pressure of the high-temperature and high-pressure reactor can be adjusted by passing hydrogen sulfide gas and carbon dioxide gas.
  • the flow rates of hydrogen sulfide gas and carbon dioxide gas are both less than 10mm/min, and the flow rates are both 150-250mL/min (more preferably 200mL/min).
  • the gas flow rate and flow rate specified in the present application are used to avoid disturbance and flow shock at the outlet of the gas in the reactor, thereby avoiding convection at the interface between the crude oil and the completion fluid.
  • step (a)-3 the temperature of the high temperature and high pressure reactor is adjusted by the intensity of heating.
  • the set reaction time is 6-8 days.
  • step (a)-4 the set reaction time is 1 day to 2 months. More preferably, the set reaction time is 1 month to 2 months.
  • the basic performance test of the completion fluid after the reaction also includes one or a combination of pH value detection, viscosity detection, crystallization temperature detection and turbidity detection.
  • the detection of the completion fluid after the reaction also includes detecting the ion content of the completion fluid after the reaction.
  • step (7) judging whether the completion fluid is suitable for crude oil containing hydrogen sulfide includes the following manner: if the density change of the completion fluid before and after the reaction is greater than 0.2SG or there is obvious precipitation in the completion fluid after the reaction, then the completion fluid is not suitable for crude oil containing hydrogen sulfide. More preferably, the obvious precipitation is the amount of precipitation after passing through a filter screen of 300 to 400 mesh (more preferably 400 mesh) of 100g/1000mL (the amount of completion fluid after the reaction) or more. Wherein, SG (specific gravity) is the ratio of the density of the completion fluid to the density of water under the conditions of standard atmospheric pressure and 3.98°C.
  • step (7) it is determined whether the completion fluid is suitable for use in a well containing hydrogen sulfide.
  • the oil further includes the following manner: if the pH value of the completion fluid to be tested is above 2, or if the viscosity of the completion fluid before and after the reaction changes by more than 10 mPa.s, or if the crystallization temperature of the completion fluid before and after the reaction changes by more than 5°C, or if the turbidity of the completion fluid before and after the reaction changes by more than 10 NTU, then the completion fluid is not suitable for crude oil containing hydrogen sulfide.
  • judging whether the completion fluid is suitable for crude oil containing hydrogen sulfide further includes the following manner: if the change in the main ion content of the completion fluid before and after the reaction is greater than 0.05 kg/L, the completion fluid is not suitable for crude oil containing hydrogen sulfide.
  • the main ions include calcium ions, zinc ions, etc., which are mainly derived from inorganic salts commonly used in completion fluids.
  • step (7) if the density change of the completion fluid before and after the reaction is less than 0.2SG and there is no obvious precipitation in the completion fluid after the reaction, and if the pH value, viscosity, crystallization temperature, turbidity and ion content of the completion fluid before and after the reaction are also tested, then they all do not meet the above-mentioned index conditions for completion fluid not suitable for hydrogen sulfide crude oil, then the completion fluid is suitable for hydrogen sulfide crude oil.
  • the preliminary judgment of whether the completion fluid is suitable for crude oil containing hydrogen sulfide includes the following manner: if the density change of the completion fluid before and after the reaction is greater than 0.2SG or there is obvious precipitation in the completion fluid after the reaction, the completion fluid is not suitable for crude oil containing hydrogen sulfide; if the density change of the completion fluid before and after the reaction is less than 0.2SG and there is no obvious precipitation in the completion fluid after the reaction, it is preliminarily judged that the completion fluid is suitable for crude oil containing hydrogen sulfide.
  • the obvious precipitation is the amount of precipitation after passing through a filter screen of 300 to 400 mesh (more preferably 400 mesh) of 100g/1000mL (the amount of completion fluid after the reaction) or more.
  • the completion fluid that is suitable for crude oil containing hydrogen sulfide after preliminary screening is subjected to the above steps (2) to (7) to finally judge whether the completion fluid is suitable for crude oil containing hydrogen sulfide.
  • the preliminary judgment of whether the completion fluid is suitable for crude oil containing hydrogen sulfide further includes the following manner: if the pH value of the completion fluid to be tested is above 2, or if the viscosity of the completion fluid before and after the reaction changes by more than 10 mPa.s, or if the crystallization temperature of the completion fluid before and after the reaction changes by more than 5°C, or if the turbidity of the completion fluid before and after the reaction changes by more than 10 NTU, then the completion fluid is not suitable for crude oil containing hydrogen sulfide.
  • step (a)-6 the preliminary judgment on whether the completion fluid is suitable for crude oil containing hydrogen sulfide further includes the following manner: if the change in the main ion content of the completion fluid before and after the reaction is greater than 0.05 kg/L, the completion fluid is not suitable for crude oil containing hydrogen sulfide.
  • step (a)-6 during the preliminary screening process, if the pH value, viscosity, crystallization temperature, turbidity, and ion content of the completion fluid before and after the reaction are also tested, then if they all do not meet the above-mentioned index conditions for completion fluid that is not suitable for hydrogen sulfide-containing crude oil, then it is preliminarily determined that the completion fluid is suitable for hydrogen sulfide-containing crude oil.
  • step (a)-6 also includes: for the completion fluid that is initially judged to be unsuitable for crude oil containing hydrogen sulfide, steps (2) to (7) may also be performed to finally judge whether the completion fluid is suitable for crude oil containing hydrogen sulfide.
  • the test method for the adaptability of water-based completion fluid in hydrogen sulfide-containing crude oil is a test method for the hydrogen sulfide resistance of water-based completion fluid for oil and gas wells, which can simulate the interface reaction between the completion fluid and the hydrogen sulfide-containing crude oil in the formation when the completion fluid is in a well-killing state, and accurately judge the adaptability of the water-based completion fluid in the hydrogen sulfide-containing crude oil.
  • the method has at least the following technological advances:
  • the present invention uses the fugacity of hydrogen sulfide in crude oil under a specific temperature and pressure environment to simulate the experimental pressure conditions. On the one hand, it is more realistic and effective (fugacity represents the effective pressure of an actual gas in chemical thermodynamics); on the other hand, it is lower than the value of partial pressure, which is easier to implement in the laboratory than using partial pressure to simulate the experimental pressure, and has less experimental risks.
  • the present invention utilizes the density difference and gravity differentiation between water-based completion fluid and crude oil to simulate the interfacial reaction between completion fluid and crude oil containing hydrogen sulfide.
  • Crude oil is first placed in a reactor, and then hydrogen sulfide is introduced to saturation, and then the deoxygenated completion fluid is pumped into the reactor. Due to its high density, the completion fluid will gather below the crude oil containing hydrogen sulfide, thereby ensuring that hydrogen sulfide reacts with the completion fluid only through mass transfer to the crude oil interface during the reaction.
  • the completion fluid and crude oil are both stationary, and hydrogen sulfide is also in a dissolved, stationary liquid phase. There is no convection, and only mass transfer affects the reaction rate.
  • the crude oil is first saturated with hydrogen sulfide, and then it is contacted with the completion fluid in a stationary state for reaction. It can completely simulate the working state of completion fluid, which is an innovative progress in the industry.
  • the order of introducing each fluid is also crucial. If the completion fluid is introduced first and then the crude oil, the crude oil cannot be saturated with hydrogen sulfide, and it cannot be guaranteed that the completion fluid and hydrogen sulfide do not undergo convection reaction.
  • the method of the present invention is to first introduce crude oil, saturate hydrogen sulfide, and then introduce the completion fluid; the static state is maintained during the entire reaction process, and the mass transfer reaction of the interface is truly simulated.
  • the present invention ensures constant experimental pressure conditions during the entire reaction process by compensating the pressure.
  • hydrogen sulfide gas is introduced to compensate the pressure to ensure that the pressure value during the entire reaction process is equal to the set fugacity value.
  • the second aspect of the present invention provides a testing device for the adaptability of a water-based completion fluid in a hydrogen sulfide-containing crude oil, the device being used to implement the above-mentioned testing method for the adaptability of a water-based completion fluid in a hydrogen sulfide-containing crude oil, the device comprising at least: a high-temperature and high-pressure reactor, a hydrogen sulfide tank, a completion fluid inlet pipeline, a gas outlet pipeline, a pressure measuring device, and a temperature control device; the temperature control device comprising a heating unit, a temperature measuring unit, and a regulating unit;
  • the hydrogen sulfide tank is connected to the high-temperature and high-pressure reactor through a pipeline; the completion fluid inlet pipeline is connected to the high-temperature and high-pressure reactor; the gas exhaust pipeline is connected to the high-temperature and high-pressure reactor; the pressure measuring device is arranged on the gas exhaust pipeline through a tee; the heating unit is arranged inside the high-temperature and high-pressure reactor; the temperature measuring unit is connected to the high-temperature and high-pressure reactor; after the regulating unit collects the temperature measured by the temperature measuring unit, it controls the heating intensity of the heating unit to adjust the temperature of the high-temperature and high-pressure reactor.
  • the tank mouth of the hydrogen sulfide tank is provided with a pressure reducing regulator.
  • a pressure-boosting valve is provided at the tank mouth of the hydrogen sulfide tank, and the pressure-boosting valve controls a needle valve and a one-way valve.
  • the pressure-boosting valve is arranged at a position closer to the tank mouth of the hydrogen sulfide tank than the needle valve. More preferably, the nominal diameter of the needle valve is 5 mm.
  • the pressure-boosting valve used in the present invention includes a needle valve capable of accurately controlling the flow rate and a one-way valve to prevent backflow.
  • the present invention preferably uses a needle valve with a nominal diameter of 5 mm.
  • the testing equipment for the adaptability of the water-based completion fluid in hydrogen sulfide-containing crude oil also includes a carbon dioxide tank, which is connected to the pipeline connecting the hydrogen sulfide tank and the high-temperature and high-pressure reactor through a tee.
  • the carbon dioxide tank and the tank port are provided with a pressure reducing regulator.
  • the tank opening of the carbon dioxide tank is provided with a one-way valve, and a needle valve is provided on the pipeline connecting the three-way valve and the high-temperature and high-pressure reactor. More preferably, the nominal diameter of the needle valve is 5mm.
  • the test equipment for the adaptability of the water-based completion fluid in hydrogen sulfide-containing crude oil further includes a hydrogen sulfide absorption device, one end of the gas discharge pipeline is connected to the high-temperature and high-pressure reactor, and the other end is connected to the hydrogen sulfide absorption device. More preferably, the hydrogen sulfide absorption device is filled with sodium hydroxide solution.
  • the testing equipment for the adaptability of the water-based completion fluid in hydrogen sulfide-containing crude oil also includes a completion fluid storage device, one end of the completion fluid inlet pipeline is connected to the high-temperature and high-pressure reactor, and the other end is connected to the completion fluid storage device.
  • the present invention provides a testing method and equipment for the adaptability of a water-based completion fluid in hydrogen sulfide-containing crude oil, which can simulate the interface reaction between the completion fluid and the hydrogen sulfide-containing crude oil in the formation when the completion fluid is in a well-killing state, and at the same time, the fugacity of hydrogen sulfide in the crude oil is used to express the experimental pressure.
  • the hydrogen sulfide gas introduction method is designed, and the gravity differentiation principle is used to simulate the reaction between the completion fluid and the crude oil at the contact interface, which can more closely simulate the actual reaction state of the formation.
  • the test result can provide a basis for whether the completion fluid can be used in a hydrogen sulfide-containing crude oil environment, thereby providing an experimental basis for the optimization of the completion fluid for high-pressure sulfur-containing oil and gas wells.
  • FIG1 is a schematic diagram of the structure of a testing device for the adaptability of a water-based completion fluid in hydrogen sulfide-containing crude oil provided in Example 1.
  • FIG. 2 is a schematic diagram of the structure of a testing device for the adaptability of a water-based completion fluid in hydrogen sulfide-containing crude oil provided in Example 2.
  • High temperature and high pressure reactor 1 hydrogen sulfide tank 2, completion fluid inlet pipeline 3, completion fluid storage device 4, gas discharge pipeline 5, pressure measuring device 6, hydrogen sulfide absorption device 7, heating unit 8, temperature measuring unit 9, regulating unit 10, pressure reducing regulator 11, needle valve 12, one-way valve 13, carbon dioxide tank 14, first three-way 15, second three-way 16.
  • This embodiment provides a test device for the adaptability of a water-based completion fluid in hydrogen sulfide-containing crude oil, as shown in FIG1 , the device comprises: a high-temperature and high-pressure reactor 1, a hydrogen sulfide tank 2, a completion fluid inlet pipeline 3, a completion fluid storage device 4, Gas discharge pipeline 5, pressure measuring device 6, temperature control device, hydrogen sulfide absorption device 7; the temperature control device includes a heating unit 8, a temperature measuring unit 9 and a regulating unit 10;
  • the hydrogen sulfide tank 2 is connected to the high-temperature and high-pressure reactor 1 through a pipeline; one end of the completion fluid inlet pipeline 3 is connected to the high-temperature and high-pressure reactor 1, and the other end is connected to the completion fluid storage device 4; one end of the gas discharge pipeline 5 is connected to the high-temperature and high-pressure reactor 1, and the other end is connected to the hydrogen sulfide absorption device 7, and the hydrogen sulfide absorption device 7 is filled with sodium hydroxide solution; the pressure measuring device 6 is arranged on the gas discharge pipeline 5 through the first three-way 15; the heating unit 8 is arranged inside the high-temperature and high-pressure reactor 1; the temperature measuring unit 9 is connected to the high-temperature and high-pressure reactor; the regulating unit 10 controls the heating intensity of the heating unit 8 after collecting the temperature measured by the temperature measuring unit 9 to adjust the temperature of the high-temperature and high-pressure reactor 1;
  • the tank mouth of the hydrogen sulfide tank 2 is provided with a pressure reducing regulator 11;
  • the tank mouth of the hydrogen sulfide tank 2 is also provided with a pressure compensation valve, which includes a needle valve 12 and a one-way valve 13; the nominal diameter of the needle valve is 5 mm.
  • the model of the high temperature and high pressure autoclave is FCZ3-31/325C276, and the remaining devices and units are conventional devices and units in the art.
  • This embodiment provides a testing device for the adaptability of a water-based completion fluid in hydrogen sulfide-containing crude oil, as shown in FIG2 , the device comprises: a high-temperature and high-pressure reactor 1, a hydrogen sulfide tank 2, a carbon dioxide tank 14, a completion fluid inlet pipeline 3, a completion fluid storage device 4, a gas discharge pipeline 5, a pressure measuring device 6, a temperature control device, and a hydrogen sulfide absorption device 7; the temperature control device comprises a heating unit 8, a temperature measuring unit 9 and a regulating unit 10;
  • the hydrogen sulfide tank 2 is connected to the high-temperature and high-pressure reactor 1 through a pipeline;
  • the carbon dioxide tank 14 is connected to the pipeline connecting the hydrogen sulfide tank 2 and the high-temperature and high-pressure reactor 1 through a second tee 16;
  • one end of the completion fluid inlet pipeline 3 is connected to the high-temperature and high-pressure reactor 1, and the other end is connected to the completion fluid storage device 4;
  • one end of the gas discharge pipeline 5 is connected to the high-temperature and high-pressure reactor 1, and the other end is connected to the hydrogen sulfide absorption device 7, and the hydrogen sulfide absorption device 7 is filled with sodium hydroxide solution;
  • the pressure measuring device 6 is arranged on the gas discharge pipeline 5 through a first tee 15;
  • the heating unit 8 is arranged inside the high-temperature and high-pressure reactor 1;
  • the temperature measuring unit 9 is connected to the high-temperature and high-pressure reactor; after the regulating unit 10 collects the temperature
  • the tank opening of the hydrogen sulfide tank 2 is provided with a pressure reducing regulator 11, and the tank opening of the hydrogen sulfide tank 2 is also provided with a one-way valve 13;
  • the tank opening of the carbon dioxide tank 14 is provided with a pressure reducing regulator 11, and the tank opening of the carbon dioxide tank 14 is also provided with a one-way valve 13;
  • a needle valve 12 is provided on the pipeline connecting the second three-way valve 16 and the high-temperature and high-pressure reactor 1 , and the nominal diameter of the needle valve 12 is 5 mm.
  • the model of the high temperature and high pressure autoclave is FCZ3-31/325C276, and the remaining devices and units are conventional devices and units in the art.
  • This embodiment provides a method for testing the adaptability of a water-based completion fluid in crude oil containing hydrogen sulfide, which is performed using the testing equipment provided in Example 1.
  • the method tests the adaptability of a CaBr 2 /ZnCl 2 completion fluid in crude oil containing hydrogen sulfide.
  • the method comprises the following steps:
  • the basic properties and main ion content of the completion fluid to be tested were tested at 24°C, -28°C, and 100°C, respectively.
  • the basic properties include density, turbidity, pH value, viscosity, and crystallization temperature.
  • the density tester model SY-1/3
  • pH tester model STARTER 300
  • turbidity tester model 1900C
  • other equipment and instruments used are all conventional in the art. The results are shown in Tables 1 to 4.
  • (a)-2 Use activated carbon to deoxygenate the completion fluid to be tested, and then pass 1000 mL of the deoxygenated completion fluid to be tested into a high-temperature and high-pressure reactor;
  • the completion fluid is still subjected to the following steps (2) to (8) to ultimately determine whether the completion fluid is suitable for crude oil containing hydrogen sulfide;
  • the partial pressure of hydrogen sulfide is the partial pressure of hydrogen sulfide in the hydrogen sulfide-containing crude oil.
  • the specific calculation method is conventional in the art. Generally speaking, it is obtained by multiplying the total system pressure (that is, the formation pressure of the hydrogen sulfide-containing crude oil) by the molar fraction of hydrogen sulfide in the gas phase.
  • the fugacity coefficient According to the calculation formula for the fugacity coefficient of the components in the mixture obtained by combining the SRK equation with the one-parameter van der Waals mixing rule disclosed on pages 6 to 8 in "Improvement of the SRK equation and its application in phase equilibrium calculation" (Luo Mingjian, master's degree thesis of Tianjin University, December 2005), that is, formula (2-34), the fugacity of hydrogen sulfide is calculated to be 5.8 MPa;
  • step (2) heating the high-temperature and high-pressure reactor to a set temperature of 100° C., and adjusting its pressure to the set pressure obtained in step (2), i.e., 5.8 MPa, and then keeping it stable; measuring the temperature and pressure of the high-temperature and high-pressure reactor every 3 days, and if the temperature and/or pressure are different from the set temperature and/or set pressure, adjusting the temperature and/or pressure of the high-temperature and high-pressure reactor to make them the same as the set temperature and set pressure;
  • the temperature of the high-temperature and high-pressure reactor is adjusted by the intensity of heating, and the pressure of the high-temperature and high-pressure reactor is adjusted by introducing hydrogen sulfide gas.
  • hydrogen sulfide gas is introduced into the high-temperature and high-pressure reactor to supplement the pressure to the set pressure.
  • the flow rate of the hydrogen sulfide gas is less than 10 mm/min, and the flow rate is 200 mL/min.
  • the pH value of the completion fluid to be tested is less than 2, and the density change of the completion fluid before and after the reaction is less than 0.2SG.
  • the amount of precipitation of the completion fluid after the reaction after passing through a 400-mesh filter is more than 100 g/1000 mL, and there is obvious precipitation. Therefore, the completion fluid is not suitable for crude oil containing hydrogen sulfide.

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Abstract

The present invention provides a test method and device for the adaptability of a water-based completion fluid in crude oil containing hydrogen sulfide. The test method comprises: testing a completion fluid to be tested; pumping crude oil into a high-temperature and high-pressure reactor, and then introducing hydrogen sulfide gas until the crude oil is saturated with hydrogen sulfide; introducing the deoxygenated completion fluid to be tested into the reactor; heating the reactor to a set temperature and making adjustment to a set pressure, the set pressure being the fugacity of hydrogen sulfide; after a set reaction time is reached, performing pressure relief, and stopping heating; and performing comparison to obtain a change of the completion fluid before and after the reaction, and determining whether the completion fluid is adaptive to the crude oil containing hydrogen sulfide. The device comprises the high-temperature and high-pressure reactor, a hydrogen sulfide tank, a completion fluid introduction pipeline, a gas discharge pipeline, a pressure measurement apparatus and a temperature control apparatus. According to the test method provided by the present invention, interfacial reaction between a completion fluid and crude oil containing hydrogen sulfide in the stratum can be simulated when the completion fluid is in a well-kill state, and the adaptability of the water-based completion fluid in the crude oil containing hydrogen sulfide is accurately determined.

Description

一种水基完井液在含硫化氢原油中适应性的测试方法及设备A test method and device for the adaptability of water-based completion fluid in crude oil containing hydrogen sulfide 技术领域Technical Field
本发明涉及一种水基完井液在含硫化氢原油中适应性的测试方法及设备,属于石油工程技术领域。The invention relates to a method and equipment for testing the adaptability of a water-based completion fluid in crude oil containing hydrogen sulfide, and belongs to the technical field of petroleum engineering.
背景技术Background technique
很多油藏原油中含硫化氢,因此完井过程中所用到的工作液都必须考虑抗硫化氢的要求。尤其是完井液,如果与硫化氢反应,一方面容易生成沉淀堵塞井筒或储层;更为重要的是,另一方面,完井液密度可能发生变化,进而引发井控风险。因此,含硫化氢的油气井所用的完井液需要进行抗硫化氢性能测试,以确保它在含硫化氢的井筒环境中的稳定性。Many reservoirs contain hydrogen sulfide in the crude oil, so the working fluid used in the completion process must take into account the requirements for hydrogen sulfide resistance. In particular, if the completion fluid reacts with hydrogen sulfide, it is easy to generate precipitation and block the wellbore or reservoir; more importantly, on the other hand, the density of the completion fluid may change, thereby causing well control risks. Therefore, the completion fluid used in oil and gas wells containing hydrogen sulfide needs to be tested for hydrogen sulfide resistance to ensure its stability in the wellbore environment containing hydrogen sulfide.
然而,完井液与含硫化氢原油的反应的实验设计一直是业界的一个瓶颈问题。完井液在井筒中静置时,主要起到压井的作用。它和含硫化氢原油的反应仅发生在完井液-原油接触的界面上。所以直接将完井液与原油混合进行反应是不合理的。同时,硫化氢是剧毒气体,混合反应容易造成泄漏,危害实验人员的人身安全。However, the experimental design of the reaction between completion fluid and crude oil containing hydrogen sulfide has always been a bottleneck problem in the industry. When the completion fluid is stationary in the wellbore, it mainly plays the role of well killing. Its reaction with crude oil containing hydrogen sulfide only occurs at the interface between the completion fluid and crude oil. Therefore, it is unreasonable to directly mix the completion fluid with crude oil for reaction. At the same time, hydrogen sulfide is a highly toxic gas, and the mixed reaction is prone to leakage, endangering the personal safety of the experimenters.
目前业界在评价完井液的抗硫化氢性能时,一般用两种方法:一种是先制备硫化氢的稀溶液(即,氢硫酸),将其与完井液混合来测试其抗硫化氢性能;另一种是在高温高压反应釜中放入完井液,然后在完井液中通入硫化氢气体,来测试其抗硫化氢性能。这两种方法都不能模拟真实的界面反应状态,并且不能模拟硫化氢的实际浓度。完井液的抗硫化氢性能测试一直以来都是本领域亟待解决的问题之一。At present, the industry generally uses two methods to evaluate the hydrogen sulfide resistance of completion fluids: one is to first prepare a dilute solution of hydrogen sulfide (i.e., hydrosulfuric acid) and mix it with the completion fluid to test its hydrogen sulfide resistance; the other is to put the completion fluid in a high-temperature and high-pressure reactor and then pass hydrogen sulfide gas into the completion fluid to test its hydrogen sulfide resistance. Both methods cannot simulate the real interface reaction state and cannot simulate the actual concentration of hydrogen sulfide. Testing the hydrogen sulfide resistance of completion fluids has always been one of the problems that need to be solved in this field.
发明内容Summary of the invention
为解决上述技术问题,本发明的目的在于提供一种水基完井液在含硫化氢原油中适应性的测试方法及设备。本发明提供的测试方法可以模拟完井液处于压井状态时与地层含硫化氢原油的界面反应,准确判断水基完井液在含硫化氢原油中的适应性。In order to solve the above technical problems, the purpose of the present invention is to provide a method and equipment for testing the adaptability of water-based completion fluid in crude oil containing hydrogen sulfide. The testing method provided by the present invention can simulate the interface reaction between the completion fluid and the crude oil containing hydrogen sulfide in the formation when the completion fluid is in a well-killing state, and accurately judge the adaptability of the water-based completion fluid in crude oil containing hydrogen sulfide.
为了实现上述目的,本发明第一方面提供了一种水基完井液在含硫化氢原油中适应性的测试方法,其包括以下步骤:In order to achieve the above object, the first aspect of the present invention provides a method for testing the adaptability of a water-based completion fluid in hydrogen sulfide-containing crude oil, which comprises the following steps:
(1)对待测完井液进行检测,所述检测至少包括对所述待测完井液的基本性能的检测,所述待测完井液的基本性能检测至少包括密度检测;(1) testing the completion fluid to be tested, wherein the testing at least includes testing the basic properties of the completion fluid to be tested, and the basic properties testing of the completion fluid to be tested at least includes density testing;
(2)将原油泵入高温高压反应釜,然后向高温高压反应釜中通入硫化氢气体一段时间直至原油饱和硫化氢; (2) pumping crude oil into a high-temperature and high-pressure reactor, and then introducing hydrogen sulfide gas into the high-temperature and high-pressure reactor for a period of time until the crude oil is saturated with hydrogen sulfide;
(3)对待测完井液进行除氧,然后向高温高压反应釜中通入除过氧的待测完井液;(3) deoxygenating the completion fluid to be tested, and then introducing the deoxygenated completion fluid to be tested into a high-temperature and high-pressure reactor;
(4)将高温高压反应釜加热至设定温度,并调整其压力至设定压力,所述设定压力为硫化氢的逸度,然后使之保持稳定;每隔一段时间测量一次高温高压反应釜的温度和压力,如果温度和/或压力与设定温度和/或设定压力不同,则调整高温高压反应釜的温度和/或压力,使它们与设定温度和设定压力相同;(4) heating the high-temperature and high-pressure reactor to a set temperature, adjusting its pressure to a set pressure, wherein the set pressure is the fugacity of hydrogen sulfide, and then keeping it stable; measuring the temperature and pressure of the high-temperature and high-pressure reactor at regular intervals, and if the temperature and/or pressure are different from the set temperature and/or set pressure, adjusting the temperature and/or pressure of the high-temperature and high-pressure reactor to make them the same as the set temperature and set pressure;
(5)达到设定的反应时间后,卸掉压力,停止加热并使高温高压反应釜冷却至室温,排出其中的流体;(5) After the set reaction time is reached, the pressure is released, the heating is stopped, the high temperature and high pressure reactor is cooled to room temperature, and the fluid therein is discharged;
(6)对反应后的完井液进行检测,所述检测至少包括对所述反应后的完井液的基本性能的检测,所述反应后的完井液的基本性能检测至少包括密度检测;(6) testing the completion fluid after the reaction, wherein the testing at least includes testing the basic properties of the completion fluid after the reaction, and the basic properties of the completion fluid after the reaction at least includes density testing;
(7)至少基于步骤(1)得到的待测完井液的检测结果以及步骤(6)得到的反应后完井液的检测结果,判断所述完井液是否适用于含硫化氢原油。(7) Based at least on the test result of the completion fluid to be tested obtained in step (1) and the test result of the completion fluid after reaction obtained in step (6), determine whether the completion fluid is suitable for use in crude oil containing hydrogen sulfide.
根据本发明的具体实施方式,优选地,所述测试方法在步骤(1)之后还包括初步筛选,所述初步筛选包括:According to a specific embodiment of the present invention, preferably, the test method further comprises a preliminary screening after step (1), wherein the preliminary screening comprises:
(a)-1将原油泵入高温高压反应釜,然后向高温高压反应釜中通入硫化氢气体一段时间直至原油饱和硫化氢;(a)-1 Pump crude oil into a high temperature and high pressure reactor, and then introduce hydrogen sulfide gas into the high temperature and high pressure reactor for a period of time until the crude oil is saturated with hydrogen sulfide;
(a)-2对待测完井液进行除氧,然后向高温高压反应釜中通入除过氧的待测完井液;(a)-2 Deoxygenate the completion fluid to be tested, and then introduce the deoxygenated completion fluid to be tested into a high-temperature and high-pressure reactor;
(a)-3将高温高压反应釜加热至设定温度,并调整其压力至常压作为设定压力,然后使之保持稳定;每隔一段时间测量一次高温高压反应釜的温度,如果温度与设定温度不同,则调整高温高压反应釜的温度,使其与设定温度相同;(a)-3 Heat the high-temperature and high-pressure reactor to a set temperature, adjust its pressure to normal pressure as the set pressure, and then keep it stable; measure the temperature of the high-temperature and high-pressure reactor at regular intervals, and if the temperature is different from the set temperature, adjust the temperature of the high-temperature and high-pressure reactor to make it the same as the set temperature;
(a)-4达到设定的反应时间后,停止加热,并使高温高压反应釜冷却至室温,排出其中的流体;(a)-4 After reaching the set reaction time, stop heating, cool the high temperature and high pressure reactor to room temperature, and discharge the fluid therein;
(a)-5对反应后的完井液进行检测,所述检测至少包括对所述反应后的完井液的基本性能的检测,所述反应后的完井液的基本性能检测至少包括密度检测;(a)-5 testing the completion fluid after the reaction, wherein the testing at least includes testing the basic properties of the completion fluid after the reaction, and the basic properties of the completion fluid after the reaction at least includes density testing;
(a)-6至少基于待测完井液的检测结果以及反应后完井液的检测结果,初步判断所述完井液是否适用于含硫化氢原油,将初步判断结果为适用于含硫化氢原油的完井液进行步骤(2)~(7),以最终判断所述完井液是否适用于含硫化氢原油。(a)-6 Preliminarily determine whether the completion fluid is suitable for crude oil containing hydrogen sulfide based at least on the test results of the completion fluid to be tested and the test results of the completion fluid after the reaction, and perform steps (2) to (7) on the completion fluid that is preliminarily determined to be suitable for crude oil containing hydrogen sulfide to finally determine whether the completion fluid is suitable for crude oil containing hydrogen sulfide.
本领域技术人员应当理解,由于上述的步骤(1)已经对待测完井液进行了基本性能检测,因此在初步筛选的过程中可以无需重复对待测完井液进行基本性能检测。Those skilled in the art should understand that since the above step (1) has already carried out basic performance testing on the completion fluid to be tested, it is not necessary to repeat the basic performance testing on the completion fluid to be tested during the preliminary screening process.
在上述方法中,优选地,在步骤(1)中,所述待测完井液的基本性能检测还包括pH值检测、粘度检测、结晶温度检测以及浊度检测等中的一种或几种的组合。 In the above method, preferably, in step (1), the basic property test of the completion fluid to be tested also includes one or a combination of pH value detection, viscosity detection, crystallization temperature detection and turbidity detection.
在上述方法中,优选地,在步骤(1)中,对待测完井液进行的检测还包括检测所述待测完井液的离子含量。In the above method, preferably, in step (1), the detection of the completion fluid to be tested also includes detecting the ion content of the completion fluid to be tested.
在上述方法中,优选地,在步骤(2)和步骤(a)-1中,泵入高温高压反应釜的原油的量为1000~3000mL。In the above method, preferably, in step (2) and step (a)-1, the amount of crude oil pumped into the high temperature and high pressure reactor is 1000 to 3000 mL.
在上述方法中,优选地,在步骤(2)和步骤(a)-1中,通入硫化氢气体的时间为1.5~2.5小时,使原油饱和硫化氢,也就是使原油溶解尽可能多的硫化氢,同时最大限度地排除反应釜中其它残留气体的影响。In the above method, preferably, in step (2) and step (a)-1, the time for introducing hydrogen sulfide gas is 1.5 to 2.5 hours, so that the crude oil is saturated with hydrogen sulfide, that is, the crude oil is dissolved with as much hydrogen sulfide as possible, while the influence of other residual gases in the reactor is eliminated to the greatest extent possible.
在上述方法中,优选地,步骤(2)和步骤(a)-1还包括:向高温高压反应釜中通入二氧化碳气体一段时间直至原油饱和硫化氢和二氧化碳。通入硫化氢气体和二氧化碳气体的时间可以为1.5~2.5小时。In the above method, preferably, step (2) and step (a)-1 further include: introducing carbon dioxide gas into the high temperature and high pressure reactor for a period of time until the crude oil is saturated with hydrogen sulfide and carbon dioxide. The time for introducing hydrogen sulfide gas and carbon dioxide gas can be 1.5 to 2.5 hours.
在上述方法中,在步骤(3)和步骤(a)-2中,对所述待测完井液进行除氧的方式可以采用本领域常规的完井液除氧方式,优选地,所述除氧的方式可以为活性炭除氧。所述活性炭除氧的具体操作方法以及活性炭和待测完井液的用量比例均可以由本领域技术人员进行常规调节。In the above method, in step (3) and step (a)-2, the deoxygenation method of the completion fluid to be tested can be a conventional completion fluid deoxygenation method in the art, preferably, the deoxygenation method can be activated carbon deoxygenation. The specific operation method of the activated carbon deoxygenation and the dosage ratio of the activated carbon and the completion fluid to be tested can be conventionally adjusted by those skilled in the art.
在上述方法中,优选地,在步骤(3)和步骤(a)-2中,向高温高压反应釜中通入的除过氧的待测完井液的量为1000~3000mL。In the above method, preferably, in step (3) and step (a)-2, the amount of the deoxygenated completion fluid to be tested introduced into the high temperature and high pressure reactor is 1000-3000 mL.
在上述方法中,优选地,泵入高温高压反应釜的原油的量与向高温高压反应釜中通入的除过氧的待测完井液的量相同。In the above method, preferably, the amount of crude oil pumped into the high-temperature and high-pressure reactor is the same as the amount of the deoxygenated completion fluid to be tested introduced into the high-temperature and high-pressure reactor.
在上述方法中,优选地,在步骤(4)中,所述的硫化氢的逸度是按照以下公式(1)计算得到的:
In the above method, preferably, in step (4), the fugacity of hydrogen sulfide is calculated according to the following formula (1):
公式(1)中,为硫化氢的逸度,单位为MPa;为硫化氢的分压,单位为MPa;为逸度系数。In formula (1), is the fugacity of hydrogen sulfide, in MPa; is the partial pressure of hydrogen sulfide, in MPa; is the fugacity coefficient.
其中,硫化氢的分压为在含硫化氢原油中硫化氢的分压,其具体计算方法为本领域常规的,一般而言是用系统总压力(也就是含硫化氢原油的地层压力)乘硫化氢在气相中的摩尔分数得到。逸度系数也可以采用本领域常规的方法进行计算,例如,可以按照《SRK方程的改进及其在相平衡计算中的应用》(罗明检,天津大学硕士学位论文,2005年12月)中第6~8页公开的对SRK方程结合1参数van der Waals混合规则得到的混合物中组分的逸度系数计算公式进行计算,即,式(2-34)。The partial pressure of hydrogen sulfide is the partial pressure of hydrogen sulfide in the crude oil containing hydrogen sulfide. The specific calculation method is conventional in the art. Generally speaking, it is obtained by multiplying the total system pressure (that is, the formation pressure of the crude oil containing hydrogen sulfide) by the molar fraction of hydrogen sulfide in the gas phase. The calculation can also be performed using conventional methods in the art. For example, the calculation can be performed according to the formula for calculating the fugacity coefficient of components in a mixture obtained by combining the SRK equation with the one-parameter van der Waals mixing rule disclosed on pages 6 to 8 of "Improvement of the SRK equation and its application in phase equilibrium calculations" (Luo Mingjian, master's thesis of Tianjin University, December 2005), that is, formula (2-34).
在上述方法中,优选地,在步骤(4)和步骤(a)-3中,所述设定温度为待测完井液工作地层的原油温度,更优选可以为80~120℃。 In the above method, preferably, in step (4) and step (a)-3, the set temperature is the crude oil temperature of the completion fluid working formation to be tested, and more preferably can be 80-120°C.
在上述方法中,优选地,在步骤(4)中,每60~80小时测量一次高温高压反应釜的温度和压力。In the above method, preferably, in step (4), the temperature and pressure of the high temperature and high pressure reactor are measured every 60 to 80 hours.
在上述方法中,优选地,在步骤(a)-3中,每24~80小时测量一次高温高压反应釜的温度。更优选地,每60~80小时测量一次高温高压反应釜的温度。In the above method, preferably, in step (a)-3, the temperature of the high temperature and high pressure reactor is measured once every 24 to 80 hours. More preferably, the temperature of the high temperature and high pressure reactor is measured once every 60 to 80 hours.
在上述方法中,优选地,在步骤(4)中,高温高压反应釜的温度是通过加热的强度进行调整的,高温高压反应釜的压力是通过通入硫化氢气体进行调整的。其中,更优选地,当测量的高温高压反应釜的压力低于所述设定压力0.5MPa以上时,则向高温高压反应釜中通过通入硫化氢气体,补充压力至设定压力。更优选地,在进行压力调整时,硫化氢气体的流速为10mm/min以下,流量为150~250mL/min(尤为优选为200mL/min)。或者,如果步骤(2)还包括:向高温高压反应釜中通入二氧化碳气体一段时间直至原油饱和硫化氢和二氧化碳,则可以通过通入硫化氢气体和二氧化碳气体调整高温高压反应釜的压力,优选地,硫化氢气体和二氧化碳气体的流速均为10mm/min以下,流量均为150~250mL/min(更优选为200mL/min)。补压时,采用本申请所限定的气体的流速和流量,能够避免反应釜中气体的出口处形成扰动、流动冲击,进而避免在原油和完井液界面上形成对流。In the above method, preferably, in step (4), the temperature of the high-temperature and high-pressure reactor is adjusted by the intensity of heating, and the pressure of the high-temperature and high-pressure reactor is adjusted by passing hydrogen sulfide gas. Among them, more preferably, when the measured pressure of the high-temperature and high-pressure reactor is lower than the set pressure by more than 0.5MPa, hydrogen sulfide gas is passed into the high-temperature and high-pressure reactor to supplement the pressure to the set pressure. More preferably, when the pressure is adjusted, the flow rate of the hydrogen sulfide gas is less than 10mm/min, and the flow rate is 150-250mL/min (especially preferably 200mL/min). Alternatively, if step (2) also includes: passing carbon dioxide gas into the high-temperature and high-pressure reactor for a period of time until the crude oil is saturated with hydrogen sulfide and carbon dioxide, the pressure of the high-temperature and high-pressure reactor can be adjusted by passing hydrogen sulfide gas and carbon dioxide gas. Preferably, the flow rates of hydrogen sulfide gas and carbon dioxide gas are both less than 10mm/min, and the flow rates are both 150-250mL/min (more preferably 200mL/min). When replenishing the pressure, the gas flow rate and flow rate specified in the present application are used to avoid disturbance and flow shock at the outlet of the gas in the reactor, thereby avoiding convection at the interface between the crude oil and the completion fluid.
在上述方法中,优选地,在步骤(a)-3中,高温高压反应釜的温度是通过加热的强度进行调整的。In the above method, preferably, in step (a)-3, the temperature of the high temperature and high pressure reactor is adjusted by the intensity of heating.
在上述方法中,优选地,在步骤(5)中,所述设定的反应时间为6-8天。In the above method, preferably, in step (5), the set reaction time is 6-8 days.
在上述方法中,优选地,在步骤(a)-4中,所述设定的反应时间为1天-2个月。更优选地,所述设定的反应时间为1个月-2个月。In the above method, preferably, in step (a)-4, the set reaction time is 1 day to 2 months. More preferably, the set reaction time is 1 month to 2 months.
在上述方法中,优选地,在步骤(6)和步骤(a)-5中,所述反应后的完井液的基本性能检测还包括pH值检测、粘度检测、结晶温度检测以及浊度检测等中的一种或几种的组合。In the above method, preferably, in step (6) and step (a)-5, the basic performance test of the completion fluid after the reaction also includes one or a combination of pH value detection, viscosity detection, crystallization temperature detection and turbidity detection.
在上述方法中,优选地,在步骤(6)和步骤(a)-5中,对反应后的完井液进行的检测还包括检测所述反应后的完井液的离子含量。In the above method, preferably, in step (6) and step (a)-5, the detection of the completion fluid after the reaction also includes detecting the ion content of the completion fluid after the reaction.
在上述方法中,优选地,在步骤(7)中,判断所述完井液是否适用于含硫化氢原油包括以下方式:如果反应前后完井液的密度变化大于0.2SG或反应后的完井液存在明显沉淀,则所述完井液不适用于含硫化氢原油。更优选地,所述明显沉淀为过300~400目(更优选为400目)的滤网后沉淀的量为100g/1000mL(反应后完井液的量)以上。其中,SG(比重)是在标准大气压、3.98℃的条件下完井液的密度与水的密度之比。In the above method, preferably, in step (7), judging whether the completion fluid is suitable for crude oil containing hydrogen sulfide includes the following manner: if the density change of the completion fluid before and after the reaction is greater than 0.2SG or there is obvious precipitation in the completion fluid after the reaction, then the completion fluid is not suitable for crude oil containing hydrogen sulfide. More preferably, the obvious precipitation is the amount of precipitation after passing through a filter screen of 300 to 400 mesh (more preferably 400 mesh) of 100g/1000mL (the amount of completion fluid after the reaction) or more. Wherein, SG (specific gravity) is the ratio of the density of the completion fluid to the density of water under the conditions of standard atmospheric pressure and 3.98°C.
在上述方法中,优选地,在步骤(7)中,判断所述完井液是否适用于含硫化氢原 油进一步包括以下方式:如果待测完井液的pH值为2以上,或者如果反应前后完井液的粘度变化为10mPa.s以上,或者如果反应前后完井液的结晶温度变化为5℃以上,或者如果反应前后完井液的浊度变化为10NTU以上,则所述完井液不适用于含硫化氢原油。In the above method, preferably, in step (7), it is determined whether the completion fluid is suitable for use in a well containing hydrogen sulfide. The oil further includes the following manner: if the pH value of the completion fluid to be tested is above 2, or if the viscosity of the completion fluid before and after the reaction changes by more than 10 mPa.s, or if the crystallization temperature of the completion fluid before and after the reaction changes by more than 5°C, or if the turbidity of the completion fluid before and after the reaction changes by more than 10 NTU, then the completion fluid is not suitable for crude oil containing hydrogen sulfide.
在上述方法中,优选地,在步骤(7)中,判断所述完井液是否适用于含硫化氢原油进一步包括以下方式:如果反应前后完井液的主要离子含量的变化为0.05kg/L以上,则所述完井液不适用于含硫化氢原油。其中,所述的主要离子包括钙离子、锌离子等,主要来源于完井液中常规使用的无机盐等。In the above method, preferably, in step (7), judging whether the completion fluid is suitable for crude oil containing hydrogen sulfide further includes the following manner: if the change in the main ion content of the completion fluid before and after the reaction is greater than 0.05 kg/L, the completion fluid is not suitable for crude oil containing hydrogen sulfide. The main ions include calcium ions, zinc ions, etc., which are mainly derived from inorganic salts commonly used in completion fluids.
在上述方法中,在步骤(7)中,如果反应前后完井液的密度变化为0.2SG以下且反应后的完井液不存在明显沉淀,并且如果对反应前后的完井液的pH值、粘度、结晶温度、浊度、离子含量也进行了检测的话,那么均需不满足上述的不适用于含硫化氢原油的完井液的指标条件,则所述完井液适用于含硫化氢原油。In the above method, in step (7), if the density change of the completion fluid before and after the reaction is less than 0.2SG and there is no obvious precipitation in the completion fluid after the reaction, and if the pH value, viscosity, crystallization temperature, turbidity and ion content of the completion fluid before and after the reaction are also tested, then they all do not meet the above-mentioned index conditions for completion fluid not suitable for hydrogen sulfide crude oil, then the completion fluid is suitable for hydrogen sulfide crude oil.
在上述方法中,优选地,在步骤(a)-6中,初步判断所述完井液是否适用于含硫化氢原油包括以下方式:如果反应前后完井液的密度变化大于0.2SG或反应后的完井液存在明显沉淀,则所述完井液不适用于含硫化氢原油;如果反应前后完井液的密度变化为0.2SG以下且反应后的完井液不存在明显沉淀,则初步判断所述完井液适用于含硫化氢原油。更优选地,所述明显沉淀为过300~400目(更优选为400目)的滤网后沉淀的量为100g/1000mL(反应后完井液的量)以上。将初步筛选后适用于含硫化氢原油的完井液进行上述的步骤(2)~(7),以最终判断所述完井液是否适用于含硫化氢原油。In the above method, preferably, in step (a)-6, the preliminary judgment of whether the completion fluid is suitable for crude oil containing hydrogen sulfide includes the following manner: if the density change of the completion fluid before and after the reaction is greater than 0.2SG or there is obvious precipitation in the completion fluid after the reaction, the completion fluid is not suitable for crude oil containing hydrogen sulfide; if the density change of the completion fluid before and after the reaction is less than 0.2SG and there is no obvious precipitation in the completion fluid after the reaction, it is preliminarily judged that the completion fluid is suitable for crude oil containing hydrogen sulfide. More preferably, the obvious precipitation is the amount of precipitation after passing through a filter screen of 300 to 400 mesh (more preferably 400 mesh) of 100g/1000mL (the amount of completion fluid after the reaction) or more. The completion fluid that is suitable for crude oil containing hydrogen sulfide after preliminary screening is subjected to the above steps (2) to (7) to finally judge whether the completion fluid is suitable for crude oil containing hydrogen sulfide.
在上述方法中,优选地,在步骤(a)-6中,初步判断所述完井液是否适用于含硫化氢原油进一步包括以下方式:如果待测完井液的pH值为2以上,或者如果反应前后完井液的粘度变化为10mPa.s以上,或者如果反应前后完井液的结晶温度变化为5℃以上,或者如果反应前后完井液的浊度变化为10NTU以上,则所述完井液不适用于含硫化氢原油。In the above method, preferably, in step (a)-6, the preliminary judgment of whether the completion fluid is suitable for crude oil containing hydrogen sulfide further includes the following manner: if the pH value of the completion fluid to be tested is above 2, or if the viscosity of the completion fluid before and after the reaction changes by more than 10 mPa.s, or if the crystallization temperature of the completion fluid before and after the reaction changes by more than 5°C, or if the turbidity of the completion fluid before and after the reaction changes by more than 10 NTU, then the completion fluid is not suitable for crude oil containing hydrogen sulfide.
在上述方法中,优选地,在步骤(a)-6中,初步判断所述完井液是否适用于含硫化氢原油进一步包括以下方式:如果反应前后完井液的主要离子含量的变化为0.05kg/L以上,则所述完井液不适用于含硫化氢原油。In the above method, preferably, in step (a)-6, the preliminary judgment on whether the completion fluid is suitable for crude oil containing hydrogen sulfide further includes the following manner: if the change in the main ion content of the completion fluid before and after the reaction is greater than 0.05 kg/L, the completion fluid is not suitable for crude oil containing hydrogen sulfide.
在上述方法中,在步骤(a)-6中,在初步筛选的过程中,如果对反应前后的完井液的pH值、粘度、结晶温度、浊度、离子含量也进行了检测的话,那么均需不满足上述的不适用于含硫化氢原油的完井液的指标条件,则初步判断所述完井液适用于含硫化氢原油。 In the above method, in step (a)-6, during the preliminary screening process, if the pH value, viscosity, crystallization temperature, turbidity, and ion content of the completion fluid before and after the reaction are also tested, then if they all do not meet the above-mentioned index conditions for completion fluid that is not suitable for hydrogen sulfide-containing crude oil, then it is preliminarily determined that the completion fluid is suitable for hydrogen sulfide-containing crude oil.
在上述方法中,优选地,步骤(a)-6还包括:对于初步判断结果为不适用于含硫化氢原油的完井液也可以进行步骤(2)~(7),以最终判断所述完井液是否适用于含硫化氢原油。In the above method, preferably, step (a)-6 also includes: for the completion fluid that is initially judged to be unsuitable for crude oil containing hydrogen sulfide, steps (2) to (7) may also be performed to finally judge whether the completion fluid is suitable for crude oil containing hydrogen sulfide.
本发明提供的水基完井液在含硫化氢原油中适应性的测试方法是一种用于油气井的水基完井液的抗硫化氢性能的测试方法,可以模拟完井液处于压井状态时与地层含硫化氢原油的界面反应,准确判断水基完井液在含硫化氢原油中的适应性。该方法至少具有以下开创性的进步:The test method for the adaptability of water-based completion fluid in hydrogen sulfide-containing crude oil provided by the present invention is a test method for the hydrogen sulfide resistance of water-based completion fluid for oil and gas wells, which can simulate the interface reaction between the completion fluid and the hydrogen sulfide-containing crude oil in the formation when the completion fluid is in a well-killing state, and accurately judge the adaptability of the water-based completion fluid in the hydrogen sulfide-containing crude oil. The method has at least the following groundbreaking advances:
(1)本发明采用特定温度压力环境下硫化氢在原油中的逸度来模拟实验压力条件,一方面更加真实有效(逸度表示在化学热力学中实际气体的有效压强);另一方面,它比分压的值更低,比用分压来模拟实验压力更容易在实验室实现,并且实验风险更小。(1) The present invention uses the fugacity of hydrogen sulfide in crude oil under a specific temperature and pressure environment to simulate the experimental pressure conditions. On the one hand, it is more realistic and effective (fugacity represents the effective pressure of an actual gas in chemical thermodynamics); on the other hand, it is lower than the value of partial pressure, which is easier to implement in the laboratory than using partial pressure to simulate the experimental pressure, and has less experimental risks.
石油行业中关于硫化氢的实验都是假定硫化氢是气体状态,硫化氢的压力用系统总压力乘硫化氢在气相中摩尔分数得到。业界标准NACE TM0177:Laboratory Testing of Metals for Resistance to Sulfide Stress Cracking and Stress Corrosion Cracking in H2S Environments,也推荐用硫化氢在气体中的分压来模拟含硫化氢的腐蚀环境——将硫化氢与氮气或二氧化碳混合,使之达到需要的分压,然后将混合气体通入反应溶液中。Experiments on hydrogen sulfide in the petroleum industry all assume that hydrogen sulfide is in gaseous state, and the pressure of hydrogen sulfide is obtained by multiplying the total system pressure by the mole fraction of hydrogen sulfide in the gas phase. The industry standard NACE TM0177: Laboratory Testing of Metals for Resistance to Sulfide Stress Cracking and Stress Corrosion Cracking in H 2 S Environments also recommends using the partial pressure of hydrogen sulfide in gas to simulate the corrosive environment containing hydrogen sulfide - mixing hydrogen sulfide with nitrogen or carbon dioxide to reach the required partial pressure, and then passing the mixed gas into the reaction solution.
而在本发明涉及的溶解状态下的硫化氢与完井液的反应中,上述采用分压进行模拟实验是不合理的,因为此时硫化氢的化学反应活性比其在气体状态下要低得多。如果采用分压来表征,硫化氢的反应活性被估计得过高(尤其是在高温高压状况下),不符合实际情况;并且如果反应环境的压力过高,实验室条件下也很难模拟。所以本发明创造性地采用逸度来表征溶解状态下的硫化氢的化学反应活性。In the reaction between hydrogen sulfide in a dissolved state and completion fluid involved in the present invention, the above-mentioned simulation experiment using partial pressure is unreasonable, because the chemical reactivity of hydrogen sulfide is much lower than that in a gas state. If partial pressure is used to characterize, the reactivity of hydrogen sulfide is estimated to be too high (especially under high temperature and high pressure conditions), which does not conform to the actual situation; and if the pressure of the reaction environment is too high, it is also difficult to simulate under laboratory conditions. Therefore, the present invention creatively uses fugacity to characterize the chemical reactivity of hydrogen sulfide in a dissolved state.
(2)本发明利用水基完井液与原油的密度差异和重力分异,模拟完井液与含硫化氢原油的界面反应。先在反应釜中放置原油,然后通入硫化氢至饱和,之后再向反应釜中泵入除过氧的完井液,完井液因为密度大,会聚集在含硫化氢原油的下方,从而保证反应过程中硫化氢仅通过传质到原油界面与完井液发生反应。(2) The present invention utilizes the density difference and gravity differentiation between water-based completion fluid and crude oil to simulate the interfacial reaction between completion fluid and crude oil containing hydrogen sulfide. Crude oil is first placed in a reactor, and then hydrogen sulfide is introduced to saturation, and then the deoxygenated completion fluid is pumped into the reactor. Due to its high density, the completion fluid will gather below the crude oil containing hydrogen sulfide, thereby ensuring that hydrogen sulfide reacts with the completion fluid only through mass transfer to the crude oil interface during the reaction.
而石油行业中,在测试硫化氢与入井流体的反应时,常常采用直接在液相中通入硫化氢气体的方法。但这远远不能模拟含硫化氢的原油与入井流体的接触反应。用这种方法来开展本发明的实验时,一定会发生测取的反应速度远远高于实际反应速度的问题。这是因为溶解有硫化氢的原油与完井液的反应速度取决于两个过程:一是对流,二是传质。所以如何模拟传质控制的反应过程至关重要。而本发明所涉及的应用场景中,完井液和原油都是静止的,硫化氢也是溶解状态的、静置的液相,没有对流发生,影响反应速度的只有传质。本发明先将原油饱和硫化氢,然后在静置状态下和完井液发生接触反 应,完全真实地模拟了完井液的工作状态,这是本行业内的创新性进步。In the oil industry, when testing the reaction between hydrogen sulfide and the fluid entering the well, the method of directly introducing hydrogen sulfide gas into the liquid phase is often used. However, this is far from simulating the contact reaction between crude oil containing hydrogen sulfide and the fluid entering the well. When this method is used to carry out the experiment of the present invention, the problem of the measured reaction rate being much higher than the actual reaction rate will definitely occur. This is because the reaction rate between crude oil dissolved with hydrogen sulfide and completion fluid depends on two processes: one is convection, and the other is mass transfer. Therefore, how to simulate the reaction process controlled by mass transfer is crucial. In the application scenario involved in the present invention, the completion fluid and crude oil are both stationary, and hydrogen sulfide is also in a dissolved, stationary liquid phase. There is no convection, and only mass transfer affects the reaction rate. In the present invention, the crude oil is first saturated with hydrogen sulfide, and then it is contacted with the completion fluid in a stationary state for reaction. It can completely simulate the working state of completion fluid, which is an innovative progress in the industry.
此外,在本发明中,各流体的通入顺序也至关重要。如果先通入完井液、再通入原油,则无法向原油中饱和硫化氢,且不能保证完井液与硫化氢不发生对流反应。而本发明的方法是先通入原油、饱和硫化氢,然后再通入完井液;在整个反应过程中保持静止状态,真实模拟界面的传质反应。In addition, in the present invention, the order of introducing each fluid is also crucial. If the completion fluid is introduced first and then the crude oil, the crude oil cannot be saturated with hydrogen sulfide, and it cannot be guaranteed that the completion fluid and hydrogen sulfide do not undergo convection reaction. The method of the present invention is to first introduce crude oil, saturate hydrogen sulfide, and then introduce the completion fluid; the static state is maintained during the entire reaction process, and the mass transfer reaction of the interface is truly simulated.
(3)本发明通过补压来保证整个反应过程中实验压力条件的恒定。实验反应过程中,如果检测到系统压力降低值大于0.5MPa,则通入硫化氢气体进行补压,确保整个反应过程中的压力值等于设定的逸度值。(3) The present invention ensures constant experimental pressure conditions during the entire reaction process by compensating the pressure. During the experimental reaction, if the system pressure drop is detected to be greater than 0.5 MPa, hydrogen sulfide gas is introduced to compensate the pressure to ensure that the pressure value during the entire reaction process is equal to the set fugacity value.
本发明第二方面提供了一种水基完井液在含硫化氢原油中适应性的测试设备,所述设备用于实现上述的水基完井液在含硫化氢原油中适应性的测试方法,所述设备至少包括:高温高压反应釜、硫化氢罐、完井液通入管线、气体排出管线、测压装置以及温度控制装置;所述温度控制装置包括加热单元、测温单元和调节单元;The second aspect of the present invention provides a testing device for the adaptability of a water-based completion fluid in a hydrogen sulfide-containing crude oil, the device being used to implement the above-mentioned testing method for the adaptability of a water-based completion fluid in a hydrogen sulfide-containing crude oil, the device comprising at least: a high-temperature and high-pressure reactor, a hydrogen sulfide tank, a completion fluid inlet pipeline, a gas outlet pipeline, a pressure measuring device, and a temperature control device; the temperature control device comprising a heating unit, a temperature measuring unit, and a regulating unit;
其中,所述硫化氢罐通过管线连接于所述高温高压反应釜;所述完井液通入管线连接于所述高温高压反应釜;所述气体排出管线连接于所述高温高压反应釜;所述测压装置通过三通设置于所述气体排出管线上;所述加热单元设置于所述高温高压反应釜的内部;所述测温单元连接于所述高温高压反应釜;所述调节单元收集所述测温单元测定的温度后,控制所述加热单元的加热强度以实现对所述高温高压反应釜的温度的调整。Wherein, the hydrogen sulfide tank is connected to the high-temperature and high-pressure reactor through a pipeline; the completion fluid inlet pipeline is connected to the high-temperature and high-pressure reactor; the gas exhaust pipeline is connected to the high-temperature and high-pressure reactor; the pressure measuring device is arranged on the gas exhaust pipeline through a tee; the heating unit is arranged inside the high-temperature and high-pressure reactor; the temperature measuring unit is connected to the high-temperature and high-pressure reactor; after the regulating unit collects the temperature measured by the temperature measuring unit, it controls the heating intensity of the heating unit to adjust the temperature of the high-temperature and high-pressure reactor.
在上述设备中,优选地,所述硫化氢罐的罐口设置有减压调节器。In the above equipment, preferably, the tank mouth of the hydrogen sulfide tank is provided with a pressure reducing regulator.
在上述设备中,优选地,所述硫化氢罐的罐口设置有补压阀,所述补压阀控制针阀和单向阀。所述补压阀相较于所述针阀设置于更为靠近所述硫化氢罐的罐口的位置。更优选地,所述针阀的公称直径为5mm。本发明所采用的补压阀包括能够进行流量精准控制的针阀和防止倒流的单向阀。如果检测到系统压力降低值大于0.5MPa时,则打开单向阀和针阀进行补压,但针阀的开度应较低,以确保补压的硫化氢气体的流速较低,以避免反应釜中硫化氢气体的出口处形成扰动、流动冲击,进而避免在原油和完井液界面上形成对流。因此,本发明优选采用公称直径为5mm的针阀。In the above-mentioned equipment, preferably, a pressure-boosting valve is provided at the tank mouth of the hydrogen sulfide tank, and the pressure-boosting valve controls a needle valve and a one-way valve. The pressure-boosting valve is arranged at a position closer to the tank mouth of the hydrogen sulfide tank than the needle valve. More preferably, the nominal diameter of the needle valve is 5 mm. The pressure-boosting valve used in the present invention includes a needle valve capable of accurately controlling the flow rate and a one-way valve to prevent backflow. If it is detected that the system pressure drop value is greater than 0.5 MPa, the one-way valve and the needle valve are opened for pressure boosting, but the opening of the needle valve should be relatively low to ensure that the flow rate of the pressure-boosting hydrogen sulfide gas is relatively low, so as to avoid disturbance and flow shock at the outlet of the hydrogen sulfide gas in the reactor, thereby avoiding convection at the interface between crude oil and completion fluid. Therefore, the present invention preferably uses a needle valve with a nominal diameter of 5 mm.
根据本发明的具体实施方式,优选地,所述水基完井液在含硫化氢原油中适应性的测试设备还包括二氧化碳罐,所述二氧化碳罐通过三通连接于所述硫化氢罐与所述高温高压反应釜相连接的管线。According to a specific embodiment of the present invention, preferably, the testing equipment for the adaptability of the water-based completion fluid in hydrogen sulfide-containing crude oil also includes a carbon dioxide tank, which is connected to the pipeline connecting the hydrogen sulfide tank and the high-temperature and high-pressure reactor through a tee.
在上述设备中,优选地,所述二氧化碳罐与的罐口设置有减压调节器。In the above device, preferably, the carbon dioxide tank and the tank port are provided with a pressure reducing regulator.
在上述设备中,优选地,所述二氧化碳罐的罐口设置有单向阀,并且在所述三通与所述高温高压反应釜相连接的管线上设置有针阀。更优选地,所述针阀的公称直径为 5mm。In the above device, preferably, the tank opening of the carbon dioxide tank is provided with a one-way valve, and a needle valve is provided on the pipeline connecting the three-way valve and the high-temperature and high-pressure reactor. More preferably, the nominal diameter of the needle valve is 5mm.
根据本发明的具体实施方式,优选地,所述水基完井液在含硫化氢原油中适应性的测试设备还包括硫化氢吸收装置,所述气体排出管线的一端连接于所述高温高压反应釜,另一端连接于所述硫化氢吸收装置。其中,更优选地,所述硫化氢吸收装置中装有氢氧化钠溶液。According to a specific embodiment of the present invention, preferably, the test equipment for the adaptability of the water-based completion fluid in hydrogen sulfide-containing crude oil further includes a hydrogen sulfide absorption device, one end of the gas discharge pipeline is connected to the high-temperature and high-pressure reactor, and the other end is connected to the hydrogen sulfide absorption device. More preferably, the hydrogen sulfide absorption device is filled with sodium hydroxide solution.
根据本发明的具体实施方式,优选地,所述水基完井液在含硫化氢原油中适应性的测试设备还包括完井液储存装置,所述完井液通入管线的一端连接于所述高温高压反应釜,另一端连接于所述完井液储存装置。According to a specific embodiment of the present invention, preferably, the testing equipment for the adaptability of the water-based completion fluid in hydrogen sulfide-containing crude oil also includes a completion fluid storage device, one end of the completion fluid inlet pipeline is connected to the high-temperature and high-pressure reactor, and the other end is connected to the completion fluid storage device.
本发明提供了一种水基完井液在含硫化氢原油中适应性的测试方法及设备,可以模拟完井液处于压井状态时与地层含硫化氢原油的界面反应,同时采用硫化氢在原油中的逸度来表现实验压力,并通过硫化氢气体通入方式的设计,利用重力分异原理模拟完井液与原油在接触界面上的反应,能够更加贴切地模拟地层实际反应状态,测试结果可以为完井液是否能够在含硫化氢原油环境中使用提供依据,从而为高压含硫油气井完井液的优选提供实验依据。The present invention provides a testing method and equipment for the adaptability of a water-based completion fluid in hydrogen sulfide-containing crude oil, which can simulate the interface reaction between the completion fluid and the hydrogen sulfide-containing crude oil in the formation when the completion fluid is in a well-killing state, and at the same time, the fugacity of hydrogen sulfide in the crude oil is used to express the experimental pressure. The hydrogen sulfide gas introduction method is designed, and the gravity differentiation principle is used to simulate the reaction between the completion fluid and the crude oil at the contact interface, which can more closely simulate the actual reaction state of the formation. The test result can provide a basis for whether the completion fluid can be used in a hydrogen sulfide-containing crude oil environment, thereby providing an experimental basis for the optimization of the completion fluid for high-pressure sulfur-containing oil and gas wells.
附图说明BRIEF DESCRIPTION OF THE DRAWINGS
图1为实施例1提供的水基完井液在含硫化氢原油中适应性的测试设备的结构示意图。FIG1 is a schematic diagram of the structure of a testing device for the adaptability of a water-based completion fluid in hydrogen sulfide-containing crude oil provided in Example 1.
图2为实施例2提供的水基完井液在含硫化氢原油中适应性的测试设备的结构示意图。FIG. 2 is a schematic diagram of the structure of a testing device for the adaptability of a water-based completion fluid in hydrogen sulfide-containing crude oil provided in Example 2.
附图标号说明:Description of Figure Numbers:
高温高压反应釜1、硫化氢罐2、完井液通入管线3、完井液储存装置4、气体排出管线5、测压装置6、硫化氢吸收装置7、加热单元8、测温单元9、调节单元10、减压调节器11、针阀12、单向阀13、二氧化碳罐14、第一三通15、第二三通16。High temperature and high pressure reactor 1, hydrogen sulfide tank 2, completion fluid inlet pipeline 3, completion fluid storage device 4, gas discharge pipeline 5, pressure measuring device 6, hydrogen sulfide absorption device 7, heating unit 8, temperature measuring unit 9, regulating unit 10, pressure reducing regulator 11, needle valve 12, one-way valve 13, carbon dioxide tank 14, first three-way 15, second three-way 16.
具体实施方式Detailed ways
为了对本发明的技术特征、目的和有益效果有更加清楚的理解,现对本发明的技术方案进行以下详细说明,但不能理解为对本发明的可实施范围的限定。In order to have a clearer understanding of the technical features, purposes and beneficial effects of the present invention, the technical solution of the present invention is now described in detail below, but it should not be construed as limiting the applicable scope of the present invention.
实施例1Example 1
本实施例提供一种水基完井液在含硫化氢原油中适应性的测试设备,如图1所示,所述设备包括:高温高压反应釜1、硫化氢罐2、完井液通入管线3、完井液储存装置4、 气体排出管线5、测压装置6、温度控制装置、硫化氢吸收装置7;所述温度控制装置包括加热单元8、测温单元9和调节单元10;This embodiment provides a test device for the adaptability of a water-based completion fluid in hydrogen sulfide-containing crude oil, as shown in FIG1 , the device comprises: a high-temperature and high-pressure reactor 1, a hydrogen sulfide tank 2, a completion fluid inlet pipeline 3, a completion fluid storage device 4, Gas discharge pipeline 5, pressure measuring device 6, temperature control device, hydrogen sulfide absorption device 7; the temperature control device includes a heating unit 8, a temperature measuring unit 9 and a regulating unit 10;
其中,所述硫化氢罐2通过管线连接于所述高温高压反应釜1;所述完井液通入管线3的一端连接于所述高温高压反应釜1,另一端连接于所述完井液储存装置4;所述气体排出管线5的一端连接于所述高温高压反应釜1,另一端连接于所述硫化氢吸收装置7,所述硫化氢吸收装7中装有氢氧化钠溶液;所述测压装置6通过第一三通15设置于所述气体排出管线5上;所述加热单元8设置于所述高温高压反应釜1的内部;所述测温单元9连接于所述高温高压反应釜;所述调节单元10收集所述测温单元9测定的温度后,控制所述加热单元8的加热强度以实现对所述高温高压反应釜1的温度的调整;Wherein, the hydrogen sulfide tank 2 is connected to the high-temperature and high-pressure reactor 1 through a pipeline; one end of the completion fluid inlet pipeline 3 is connected to the high-temperature and high-pressure reactor 1, and the other end is connected to the completion fluid storage device 4; one end of the gas discharge pipeline 5 is connected to the high-temperature and high-pressure reactor 1, and the other end is connected to the hydrogen sulfide absorption device 7, and the hydrogen sulfide absorption device 7 is filled with sodium hydroxide solution; the pressure measuring device 6 is arranged on the gas discharge pipeline 5 through the first three-way 15; the heating unit 8 is arranged inside the high-temperature and high-pressure reactor 1; the temperature measuring unit 9 is connected to the high-temperature and high-pressure reactor; the regulating unit 10 controls the heating intensity of the heating unit 8 after collecting the temperature measured by the temperature measuring unit 9 to adjust the temperature of the high-temperature and high-pressure reactor 1;
所述硫化氢罐2的罐口设置有减压调节器11;The tank mouth of the hydrogen sulfide tank 2 is provided with a pressure reducing regulator 11;
所述硫化氢罐2的罐口还设置有补压阀,所述补压阀包括针阀12和单向阀13;所述针阀的公称直径为5mm。The tank mouth of the hydrogen sulfide tank 2 is also provided with a pressure compensation valve, which includes a needle valve 12 and a one-way valve 13; the nominal diameter of the needle valve is 5 mm.
在本实施例中,所述高温高压釜的型号为FCZ3-31/325C276,其余装置与单元均为本领域常规装置与单元。In this embodiment, the model of the high temperature and high pressure autoclave is FCZ3-31/325C276, and the remaining devices and units are conventional devices and units in the art.
实施例2Example 2
本实施例提供一种水基完井液在含硫化氢原油中适应性的测试设备,如图2所示,所述设备包括:高温高压反应釜1、硫化氢罐2、二氧化碳罐14、完井液通入管线3、完井液储存装置4、气体排出管线5、测压装置6、温度控制装置、硫化氢吸收装置7;所述温度控制装置包括加热单元8、测温单元9和调节单元10;This embodiment provides a testing device for the adaptability of a water-based completion fluid in hydrogen sulfide-containing crude oil, as shown in FIG2 , the device comprises: a high-temperature and high-pressure reactor 1, a hydrogen sulfide tank 2, a carbon dioxide tank 14, a completion fluid inlet pipeline 3, a completion fluid storage device 4, a gas discharge pipeline 5, a pressure measuring device 6, a temperature control device, and a hydrogen sulfide absorption device 7; the temperature control device comprises a heating unit 8, a temperature measuring unit 9 and a regulating unit 10;
其中,所述硫化氢罐2通过管线连接于所述高温高压反应釜1;所述二氧化碳罐14通过第二三通16连接于所述硫化氢罐2与所述高温高压反应釜1相连接的管线;所述完井液通入管线3的一端连接于所述高温高压反应釜1,另一端连接于所述完井液储存装置4;所述气体排出管线5的一端连接于所述高温高压反应釜1,另一端连接于所述硫化氢吸收装置7,所述硫化氢吸收装7中装有氢氧化钠溶液;所述测压装置6通过第一三通15设置于所述气体排出管线5上;所述加热单元8设置于所述高温高压反应釜1的内部;所述测温单元9连接于所述高温高压反应釜;所述调节单元10收集所述测温单元9测定的温度后,控制所述加热单元8的加热强度以实现对所述高温高压反应釜1的温度的调整;Wherein, the hydrogen sulfide tank 2 is connected to the high-temperature and high-pressure reactor 1 through a pipeline; the carbon dioxide tank 14 is connected to the pipeline connecting the hydrogen sulfide tank 2 and the high-temperature and high-pressure reactor 1 through a second tee 16; one end of the completion fluid inlet pipeline 3 is connected to the high-temperature and high-pressure reactor 1, and the other end is connected to the completion fluid storage device 4; one end of the gas discharge pipeline 5 is connected to the high-temperature and high-pressure reactor 1, and the other end is connected to the hydrogen sulfide absorption device 7, and the hydrogen sulfide absorption device 7 is filled with sodium hydroxide solution; the pressure measuring device 6 is arranged on the gas discharge pipeline 5 through a first tee 15; the heating unit 8 is arranged inside the high-temperature and high-pressure reactor 1; the temperature measuring unit 9 is connected to the high-temperature and high-pressure reactor; after the regulating unit 10 collects the temperature measured by the temperature measuring unit 9, it controls the heating intensity of the heating unit 8 to adjust the temperature of the high-temperature and high-pressure reactor 1;
所述硫化氢罐2的罐口设置有减压调节器11,所述硫化氢罐2的罐口还设置有单向阀13; The tank opening of the hydrogen sulfide tank 2 is provided with a pressure reducing regulator 11, and the tank opening of the hydrogen sulfide tank 2 is also provided with a one-way valve 13;
所述二氧化碳罐14的罐口设置有减压调节器11,所述述二氧化碳罐14的罐口还设置有单向阀13;The tank opening of the carbon dioxide tank 14 is provided with a pressure reducing regulator 11, and the tank opening of the carbon dioxide tank 14 is also provided with a one-way valve 13;
在所述第二三通16与所述高温高压反应釜1相连接的管线上设置有针阀12,所述针阀12的公称直径为5mm。A needle valve 12 is provided on the pipeline connecting the second three-way valve 16 and the high-temperature and high-pressure reactor 1 , and the nominal diameter of the needle valve 12 is 5 mm.
在本实施例中,所述高温高压釜的型号为FCZ3-31/325C276,其余装置与单元均为本领域常规装置与单元。In this embodiment, the model of the high temperature and high pressure autoclave is FCZ3-31/325C276, and the remaining devices and units are conventional devices and units in the art.
实施例3Example 3
本实施例提供一种水基完井液在含硫化氢原油中适应性的测试方法,其采用实施例1提供的测试设备进行,该方法对CaBr2/ZnCl2完井液在含硫化氢原油中适应性进行测试。This embodiment provides a method for testing the adaptability of a water-based completion fluid in crude oil containing hydrogen sulfide, which is performed using the testing equipment provided in Example 1. The method tests the adaptability of a CaBr 2 /ZnCl 2 completion fluid in crude oil containing hydrogen sulfide.
该方法包括以下步骤:The method comprises the following steps:
(1)分别在24℃、-28℃、100℃条件下检测待测完井液(即,CaBr2/ZnCl2完井液)的基本性能和主离子含量,基本性能包括密度、浊度、pH值、粘度和结晶温度等,所采用的密度测试仪(型号SY-1/3)、pH测试仪(型号STARTER 300)、浊度测试仪(型号1900C)等设备仪器均为本领域常规的,结果如表1~表4所示;(1) The basic properties and main ion content of the completion fluid to be tested (i.e., CaBr 2 /ZnCl 2 completion fluid) were tested at 24°C, -28°C, and 100°C, respectively. The basic properties include density, turbidity, pH value, viscosity, and crystallization temperature. The density tester (model SY-1/3), pH tester (model STARTER 300), turbidity tester (model 1900C), and other equipment and instruments used are all conventional in the art. The results are shown in Tables 1 to 4.
表1 CaBr2/ZnCl2完井液在不同温度下的基础性能检测结果
Table 1 Basic performance test results of CaBr 2 /ZnCl 2 completion fluid at different temperatures
初步筛选:Initial screening:
(a)-1将1000mL原油泵入高温高压反应釜,然后向高温高压反应釜中通入硫化氢气体2小时直至原油饱和硫化氢;(a)-1 Pump 1000 mL of crude oil into a high temperature and high pressure reactor, and then introduce hydrogen sulfide gas into the high temperature and high pressure reactor for 2 hours until the crude oil is saturated with hydrogen sulfide;
(a)-2采用活性炭对待测完井液进行除氧,然后向高温高压反应釜中通入除过氧的待测完井液1000mL;(a)-2 Use activated carbon to deoxygenate the completion fluid to be tested, and then pass 1000 mL of the deoxygenated completion fluid to be tested into a high-temperature and high-pressure reactor;
(a)-3将高温高压反应釜加热至设定温度,所述设定温度为100℃,并调整其压力至常压作为设定压力,然后使之保持稳定;每3天测量一次高温高压反应釜的温度,如果温度与设定温度不同,则调整高温高压反应釜的温度,使其与设定温度相同;其中,高温高压反应釜的温度是通过加热的强度进行调整的;(a)-3 heating the high temperature and high pressure reactor to a set temperature of 100°C, adjusting its pressure to normal pressure as the set pressure, and then keeping it stable; measuring the temperature of the high temperature and high pressure reactor every 3 days, and if the temperature is different from the set temperature, adjusting the temperature of the high temperature and high pressure reactor to make it the same as the set temperature; wherein the temperature of the high temperature and high pressure reactor is adjusted by the intensity of heating;
(a)-4达到设定的反应时间后,停止加热,并使高温高压反应釜冷却至室温,排 出其中的流体;其中,设定的反应时间分别为1天、3天、7天、15天、30天;(a)-4 After reaching the set reaction time, stop heating and cool the high temperature and high pressure reactor to room temperature. out the fluid therein; wherein the set reaction times are 1 day, 3 days, 7 days, 15 days, and 30 days respectively;
(a)-5在1天、3天、7天、15天、30天时,分别在常温常压下检测反应后的完井液的基本性能和主离子含量,所述反应后的完井液的基本性能检测至少包括密度检测、pH值检测,结果如表3和表4所示;(a)-5 At 1 day, 3 days, 7 days, 15 days and 30 days, the basic properties and main ion content of the completion fluid after the reaction were tested at room temperature and pressure, respectively. The basic properties test of the completion fluid after the reaction at least includes density test and pH value test. The results are shown in Tables 3 and 4;
(a)-6初步判断所述完井液是否适用于含硫化氢原油:由表3和表4的数据可以看出,待测完井液的pH值小于2,反应前后完井液的密度变化为0.2SG以下,反应后的完井液过400目的滤网后沉淀的量为100g/1000mL以上,存在明显沉淀,且重复实验的结果一致(即1天、3天、7天、15天、30天的实验结果一致),反应前后完井液的锌离子含量的变化在一部分重复实验中为0.05kg/L以上,因此初步判断所述完井液不适用于含硫化氢原油;(a)-6 Preliminary judgment on whether the completion fluid is suitable for crude oil containing hydrogen sulfide: From the data in Tables 3 and 4, it can be seen that the pH value of the completion fluid to be tested is less than 2, the density change of the completion fluid before and after the reaction is less than 0.2SG, the amount of precipitation of the completion fluid after the reaction after passing through a 400-mesh filter is more than 100g/1000mL, there is obvious precipitation, and the results of repeated experiments are consistent (i.e., the experimental results of 1 day, 3 days, 7 days, 15 days, and 30 days are consistent), and the change of the zinc ion content of the completion fluid before and after the reaction is more than 0.05kg/L in some repeated experiments. Therefore, it is preliminarily judged that the completion fluid is not suitable for crude oil containing hydrogen sulfide;
但是,仍然将所述完井液进行下述的步骤(2)~(8),以最终判断该完井液是否适用于含硫化氢原油;However, the completion fluid is still subjected to the following steps (2) to (8) to ultimately determine whether the completion fluid is suitable for crude oil containing hydrogen sulfide;
(2)按照以下公式(1)计算硫化氢的逸度,并将计算得到的硫化氢的逸度作为实验的设定压力,
(2) Calculate the fugacity of hydrogen sulfide according to the following formula (1), and use the calculated fugacity of hydrogen sulfide as the set pressure of the experiment.
公式(1)中,为硫化氢的逸度,单位为MPa;为硫化氢的分压,单位为MPa;为逸度系数;In formula (1), is the fugacity of hydrogen sulfide, in MPa; is the partial pressure of hydrogen sulfide, in MPa; is the fugacity coefficient;
其中,硫化氢的分压为在含硫化氢原油中硫化氢的分压,其具体计算方法为本领域常规的,一般而言是用系统总压力(也就是含硫化氢原油的地层压力)乘硫化氢在气相中的摩尔分数得到;逸度系数按照《SRK方程的改进及其在相平衡计算中的应用》(罗明检,天津大学硕士学位论文,2005年12月)中在第6~8页公开的对SRK方程结合1参数van der Waals混合规则得到的混合物中组分的逸度系数计算公式进行计算,即,式(2-34);计算得到硫化氢的逸度为5.8MPa;The partial pressure of hydrogen sulfide is the partial pressure of hydrogen sulfide in the hydrogen sulfide-containing crude oil. The specific calculation method is conventional in the art. Generally speaking, it is obtained by multiplying the total system pressure (that is, the formation pressure of the hydrogen sulfide-containing crude oil) by the molar fraction of hydrogen sulfide in the gas phase. The fugacity coefficient According to the calculation formula for the fugacity coefficient of the components in the mixture obtained by combining the SRK equation with the one-parameter van der Waals mixing rule disclosed on pages 6 to 8 in "Improvement of the SRK equation and its application in phase equilibrium calculation" (Luo Mingjian, master's degree thesis of Tianjin University, December 2005), that is, formula (2-34), the fugacity of hydrogen sulfide is calculated to be 5.8 MPa;
(3)将1000mL原油泵入高温高压反应釜,然后向高温高压反应釜中通入硫化氢气体2小时直至原油饱和硫化氢;(3) 1000 mL of crude oil was pumped into a high temperature and high pressure reactor, and then hydrogen sulfide gas was introduced into the high temperature and high pressure reactor for 2 hours until the crude oil was saturated with hydrogen sulfide;
(4)采用活性炭对待测完井液进行除氧,然后向高温高压反应釜中通入除过氧的待测完井液1000mL;(4) deoxygenating the completion fluid to be tested using activated carbon, and then introducing 1000 mL of the deoxygenated completion fluid to be tested into a high-temperature and high-pressure reactor;
(5)将高温高压反应釜加热至设定温度,所述设定温度为100℃,并调整其压力至步骤(2)得到的设定压力,即5.8MPa,然后使之保持稳定;每3天测量一次高温高压反应釜的温度和压力,如果温度和/或压力与设定温度和/或设定压力不同,则调整高温高压反应釜的温度和/或压力,使它们与设定温度和设定压力相同; (5) heating the high-temperature and high-pressure reactor to a set temperature of 100° C., and adjusting its pressure to the set pressure obtained in step (2), i.e., 5.8 MPa, and then keeping it stable; measuring the temperature and pressure of the high-temperature and high-pressure reactor every 3 days, and if the temperature and/or pressure are different from the set temperature and/or set pressure, adjusting the temperature and/or pressure of the high-temperature and high-pressure reactor to make them the same as the set temperature and set pressure;
其中,高温高压反应釜的温度是通过加热的强度进行调整的,高温高压反应釜的压力是通过通入硫化氢气体进行调整的,当测量的高温高压反应釜的压力低于所述设定压力0.5MPa以上时,则向高温高压反应釜中通过通入硫化氢气体,补充压力至设定压力,在进行压力调整时,硫化氢气体的流速为10mm/min以下,流量为200mL/min;The temperature of the high-temperature and high-pressure reactor is adjusted by the intensity of heating, and the pressure of the high-temperature and high-pressure reactor is adjusted by introducing hydrogen sulfide gas. When the measured pressure of the high-temperature and high-pressure reactor is lower than the set pressure by more than 0.5 MPa, hydrogen sulfide gas is introduced into the high-temperature and high-pressure reactor to supplement the pressure to the set pressure. When the pressure is adjusted, the flow rate of the hydrogen sulfide gas is less than 10 mm/min, and the flow rate is 200 mL/min.
(6)达到设定的反应时间后,卸掉压力,停止加热并使高温高压反应釜冷却至室温,排出其中的流体;其中,设定的反应时间为7天;(6) After the set reaction time is reached, the pressure is released, the heating is stopped, the high temperature and high pressure reactor is cooled to room temperature, and the fluid therein is discharged; wherein the set reaction time is 7 days;
(7)在常温常压下检测反应后的完井液的基本性能和主离子含量,所述反应后的完井液的基本性能检测至少包括密度检测、pH值检测,结果如表2、表3和表4所示;(7) Testing the basic properties and main ion content of the completion fluid after the reaction at normal temperature and pressure, wherein the basic properties testing of the completion fluid after the reaction at least includes density testing and pH value testing, and the results are shown in Table 2, Table 3 and Table 4;
表2反应前后完井液的基本性能和主离子含量在常温常压下的检测结果
Table 2 Test results of basic properties and main ion content of completion fluid before and after reaction at normal temperature and pressure
表3反应前后CaBr2/ZnCl2完井液的基本性能在常温常压下的检测结果
Table 3 Test results of basic properties of CaBr 2 /ZnCl 2 completion fluid before and after reaction at normal temperature and pressure
表4反应前后CaBr2/ZnCl2完井液的主离子含量在常温常压下的检测结果
Table 4 Detection results of main ion content of CaBr 2 /ZnCl 2 completion fluid before and after reaction at normal temperature and pressure
(8)结果为:待测完井液的pH值小于2,反应前后完井液的密度变化为0.2SG以下,但是反应后的完井液过400目的滤网后沉淀的量为100g/1000mL以上,存在明显沉淀,因此所述完井液不适用于含硫化氢原油。 (8) The results are as follows: the pH value of the completion fluid to be tested is less than 2, and the density change of the completion fluid before and after the reaction is less than 0.2SG. However, the amount of precipitation of the completion fluid after the reaction after passing through a 400-mesh filter is more than 100 g/1000 mL, and there is obvious precipitation. Therefore, the completion fluid is not suitable for crude oil containing hydrogen sulfide.

Claims (20)

  1. 一种水基完井液在含硫化氢原油中适应性的测试方法,其包括以下步骤:A method for testing the adaptability of a water-based completion fluid in crude oil containing hydrogen sulfide comprises the following steps:
    (1)对待测完井液进行检测,所述检测至少包括对所述待测完井液的基本性能的检测,所述待测完井液的基本性能检测至少包括密度检测;(1) testing the completion fluid to be tested, wherein the testing at least includes testing the basic properties of the completion fluid to be tested, and the basic properties testing of the completion fluid to be tested at least includes density testing;
    (2)将原油泵入高温高压反应釜,然后向高温高压反应釜中通入硫化氢气体一段时间直至原油饱和硫化氢;(2) pumping crude oil into a high-temperature and high-pressure reactor, and then introducing hydrogen sulfide gas into the high-temperature and high-pressure reactor for a period of time until the crude oil is saturated with hydrogen sulfide;
    (3)对待测完井液进行除氧,然后向高温高压反应釜中通入除过氧的待测完井液;(3) deoxygenating the completion fluid to be tested, and then introducing the deoxygenated completion fluid to be tested into a high-temperature and high-pressure reactor;
    (4)将高温高压反应釜加热至设定温度,并调整其压力至设定压力,所述设定压力为硫化氢的逸度,然后使之保持稳定;每隔一段时间测量一次高温高压反应釜的温度和压力,如果温度和/或压力与设定温度和/或设定压力不同,则调整高温高压反应釜的温度和/或压力,使它们与设定温度和设定压力相同;(4) heating the high-temperature and high-pressure reactor to a set temperature, adjusting its pressure to a set pressure, wherein the set pressure is the fugacity of hydrogen sulfide, and then keeping it stable; measuring the temperature and pressure of the high-temperature and high-pressure reactor at regular intervals, and if the temperature and/or pressure are different from the set temperature and/or set pressure, adjusting the temperature and/or pressure of the high-temperature and high-pressure reactor to make them the same as the set temperature and set pressure;
    (5)达到设定的反应时间后,卸掉压力,停止加热并使高温高压反应釜冷却至室温,排出其中的流体;(5) After the set reaction time is reached, the pressure is released, the heating is stopped, the high temperature and high pressure reactor is cooled to room temperature, and the fluid therein is discharged;
    (6)对反应后的完井液进行检测,所述检测至少包括对所述反应后的完井液的基本性能的检测,所述反应后的完井液的基本性能检测至少包括密度检测;(6) testing the completion fluid after the reaction, wherein the testing at least includes testing the basic properties of the completion fluid after the reaction, and the basic properties of the completion fluid after the reaction at least includes density testing;
    (7)至少基于步骤(1)得到的待测完井液的检测结果以及步骤(6)得到的反应后完井液的检测结果,判断所述完井液是否适用于含硫化氢原油。(7) Based at least on the test result of the completion fluid to be tested obtained in step (1) and the test result of the completion fluid after reaction obtained in step (6), determine whether the completion fluid is suitable for use in crude oil containing hydrogen sulfide.
  2. 根据权利要求1所述的水基完井液在含硫化氢原油中适应性的测试方法,其中,所述测试方法在步骤(1)之后还包括初步筛选,所述初步筛选包括:The method for testing the adaptability of a water-based completion fluid in hydrogen sulfide-containing crude oil according to claim 1, wherein the testing method further comprises a preliminary screening after step (1), wherein the preliminary screening comprises:
    (a)-1将原油泵入高温高压反应釜,然后向高温高压反应釜中通入硫化氢气体一段时间直至原油饱和硫化氢;(a)-1 Pump crude oil into a high temperature and high pressure reactor, and then introduce hydrogen sulfide gas into the high temperature and high pressure reactor for a period of time until the crude oil is saturated with hydrogen sulfide;
    (a)-2对待测完井液进行除氧,然后向高温高压反应釜中通入除过氧的待测完井液;(a)-2 Deoxygenate the completion fluid to be tested, and then introduce the deoxygenated completion fluid to be tested into a high-temperature and high-pressure reactor;
    (a)-3将高温高压反应釜加热至设定温度,并调整其压力至常压作为设定压力,然后使之保持稳定;每隔一段时间测量一次高温高压反应釜的温度,如果温度与设定温度不同,则调整高温高压反应釜的温度,使其与设定温度相同;(a)-3 Heat the high-temperature and high-pressure reactor to a set temperature, adjust its pressure to normal pressure as the set pressure, and then keep it stable; measure the temperature of the high-temperature and high-pressure reactor at regular intervals, and if the temperature is different from the set temperature, adjust the temperature of the high-temperature and high-pressure reactor to make it the same as the set temperature;
    (a)-4达到设定的反应时间后,停止加热,并使高温高压反应釜冷却至室温,排出其中的流体;(a)-4 After reaching the set reaction time, stop heating, cool the high temperature and high pressure reactor to room temperature, and discharge the fluid therein;
    (a)-5对反应后的完井液进行检测,所述检测至少包括对所述反应后的完井液的基本性能的检测,所述反应后的完井液的基本性能检测至少包括密度检测;(a)-5 testing the completion fluid after the reaction, wherein the testing at least includes testing the basic properties of the completion fluid after the reaction, and the basic properties of the completion fluid after the reaction at least includes density testing;
    (a)-6至少基于待测完井液的检测结果以及反应后完井液的检测结果,初步判断 所述完井液是否适用于含硫化氢原油,将初步判断结果为适用于含硫化氢原油的完井液进行步骤(2)~(7),以最终判断所述完井液是否适用于含硫化氢原油。(a)-6 Based at least on the test results of the completion fluid to be tested and the test results of the completion fluid after reaction, a preliminary judgment is made. Whether the completion fluid is suitable for crude oil containing hydrogen sulfide is determined by performing steps (2) to (7) on the completion fluid that is initially determined to be suitable for crude oil containing hydrogen sulfide, so as to finally determine whether the completion fluid is suitable for crude oil containing hydrogen sulfide.
  3. 根据权利要求2所述的水基完井液在含硫化氢原油中适应性的测试方法,其中,步骤(a)-6还包括:对于初步判断结果为不适用于含硫化氢原油的完井液也进行步骤(2)~(7),以最终判断所述完井液是否适用于含硫化氢原油。According to the method for testing the adaptability of water-based completion fluid in hydrogen sulfide-containing crude oil as described in claim 2, step (a)-6 also includes: for the completion fluid that is initially judged to be unsuitable for hydrogen sulfide-containing crude oil, steps (2) to (7) are also performed to finally judge whether the completion fluid is suitable for hydrogen sulfide-containing crude oil.
  4. 根据权利要求1所述的水基完井液在含硫化氢原油中适应性的测试方法,其中,在步骤(1)中,所述待测完井液的基本性能检测还包括pH值检测、粘度检测、结晶温度检测以及浊度检测中的一种或几种的组合。According to the test method for the adaptability of water-based completion fluid in hydrogen sulfide-containing crude oil according to claim 1, wherein, in step (1), the basic performance test of the completion fluid to be tested also includes one or a combination of pH value detection, viscosity detection, crystallization temperature detection and turbidity detection.
  5. 根据权利要求1所述的水基完井液在含硫化氢原油中适应性的测试方法,其中,在步骤(1)中,对待测完井液进行的检测还包括检测所述待测完井液的离子含量。According to the method for testing the adaptability of water-based completion fluid in hydrogen sulfide-containing crude oil as claimed in claim 1, wherein in step (1), the testing of the completion fluid to be tested also includes testing the ion content of the completion fluid to be tested.
  6. 根据权利要求1或2所述的水基完井液在含硫化氢原油中适应性的测试方法,其中,在步骤(2)和步骤(a)-1中,泵入高温高压反应釜的原油的量为1000~3000mL;The method for testing the adaptability of a water-based completion fluid in hydrogen sulfide-containing crude oil according to claim 1 or 2, wherein in step (2) and step (a)-1, the amount of crude oil pumped into the high-temperature and high-pressure reactor is 1000 to 3000 mL;
    在步骤(2)和步骤(a)-1中,通入硫化氢气体的时间为1.5~2.5小时。In step (2) and step (a)-1, the time for introducing hydrogen sulfide gas is 1.5 to 2.5 hours.
  7. 根据权利要求1或2所述的水基完井液在含硫化氢原油中适应性的测试方法,其中,步骤(2)和步骤(a)-1还包括:向高温高压反应釜中通入二氧化碳气体一段时间直至原油饱和硫化氢和二氧化碳。The method for testing the adaptability of water-based completion fluid in hydrogen sulfide-containing crude oil according to claim 1 or 2, wherein step (2) and step (a)-1 further comprise: introducing carbon dioxide gas into the high-temperature and high-pressure reactor for a period of time until the crude oil is saturated with hydrogen sulfide and carbon dioxide.
  8. 根据权利要求1或2所述的水基完井液在含硫化氢原油中适应性的测试方法,其中,在步骤(3)和步骤(a)-2中,向高温高压反应釜中通入的除过氧的待测完井液的量为1000~3000mL。The method for testing the adaptability of a water-based completion fluid in hydrogen sulfide-containing crude oil according to claim 1 or 2, wherein in step (3) and step (a)-2, the amount of the deoxygenated completion fluid to be tested introduced into the high-temperature and high-pressure reactor is 1000 to 3000 mL.
  9. 根据权利要求1或2所述的水基完井液在含硫化氢原油中适应性的测试方法,其中,在步骤(4)和步骤(a)-3中,所述设定温度为待测完井液工作地层的原油温度。The method for testing the adaptability of water-based completion fluid in hydrogen sulfide-containing crude oil according to claim 1 or 2, wherein in step (4) and step (a)-3, the set temperature is the crude oil temperature of the working formation of the completion fluid to be tested.
  10. 根据权利要求1所述的水基完井液在含硫化氢原油中适应性的测试方法,其中,在步骤(4)中,每60~80小时测量一次高温高压反应釜的温度和压力。The method for testing the adaptability of water-based completion fluid in hydrogen sulfide-containing crude oil according to claim 1, wherein, in step (4), the temperature and pressure of the high-temperature and high-pressure reactor are measured every 60 to 80 hours.
  11. 根据权利要求2所述的水基完井液在含硫化氢原油中适应性的测试方法,其中,在步骤(a)-3中,每24~80小时测量一次高温高压反应釜的温度。The method for testing the adaptability of water-based completion fluid in hydrogen sulfide-containing crude oil according to claim 2, wherein in step (a)-3, the temperature of the high-temperature and high-pressure reactor is measured once every 24 to 80 hours.
  12. 根据权利要求1所述的水基完井液在含硫化氢原油中适应性的测试方法,其中,在步骤(4)中,高温高压反应釜的温度是通过加热的强度进行调整的,高温高压反应釜的压力是通过通入硫化氢气体进行调整的;当测量的高温高压反应釜的压力低于所述设定压力0.5MPa以上时,则向高温高压反应釜中通过通入硫化氢气体,补充压力至设定压力;在进行压力调整时,硫化氢气体的流速为10mm/min以下,流量为150~250mL/min。 According to claim 1, the test method for the adaptability of water-based completion fluid in hydrogen sulfide-containing crude oil, wherein, in step (4), the temperature of the high-temperature and high-pressure reactor is adjusted by the intensity of heating, and the pressure of the high-temperature and high-pressure reactor is adjusted by introducing hydrogen sulfide gas; when the measured pressure of the high-temperature and high-pressure reactor is lower than the set pressure by more than 0.5 MPa, hydrogen sulfide gas is introduced into the high-temperature and high-pressure reactor to supplement the pressure to the set pressure; when the pressure is adjusted, the flow rate of the hydrogen sulfide gas is less than 10 mm/min, and the flow rate is 150 to 250 mL/min.
  13. 根据权利要求1或2所述的水基完井液在含硫化氢原油中适应性的测试方法,其中,在步骤(5)中,所述设定的反应时间为6-8天;The method for testing the adaptability of water-based completion fluid in hydrogen sulfide-containing crude oil according to claim 1 or 2, wherein in step (5), the set reaction time is 6-8 days;
    在步骤(a)-4中,所述设定的反应时间为1天-2个月。In step (a)-4, the set reaction time is 1 day to 2 months.
  14. 根据权利要求1或2所述的水基完井液在含硫化氢原油中适应性的测试方法,其中,在步骤(6)和步骤(a)-5中,所述反应后的完井液的基本性能检测还包括pH值检测、粘度检测、结晶温度检测以及浊度检测中的一种或几种的组合。According to the test method for the adaptability of water-based completion fluid in hydrogen sulfide-containing crude oil according to claim 1 or 2, wherein, in step (6) and step (a)-5, the basic performance test of the completion fluid after the reaction also includes one or a combination of pH value detection, viscosity detection, crystallization temperature detection and turbidity detection.
  15. 根据权利要求1或2所述的水基完井液在含硫化氢原油中适应性的测试方法,其中,在步骤(6)和步骤(a)-5中,对反应后的完井液进行的检测还包括检测所述反应后的完井液的离子含量。According to the test method for the adaptability of water-based completion fluid in hydrogen sulfide-containing crude oil according to claim 1 or 2, wherein, in step (6) and step (a)-5, the detection of the completion fluid after the reaction also includes detecting the ion content of the completion fluid after the reaction.
  16. 根据权利要求1所述的水基完井液在含硫化氢原油中适应性的测试方法,其中,在步骤(7)中,判断所述完井液是否适用于含硫化氢原油包括以下方式:如果反应前后完井液的密度变化大于0.2SG或反应后的完井液存在明显沉淀,则所述完井液不适用于含硫化氢原油;所述明显沉淀为过300~400目的滤网后沉淀的量为100g/1000mL以上;According to the test method for the adaptability of water-based completion fluid in hydrogen sulfide-containing crude oil according to claim 1, wherein, in step (7), judging whether the completion fluid is suitable for hydrogen sulfide-containing crude oil includes the following manner: if the density change of the completion fluid before and after the reaction is greater than 0.2SG or there is obvious precipitation in the completion fluid after the reaction, then the completion fluid is not suitable for hydrogen sulfide-containing crude oil; the obvious precipitation is that the amount of precipitation after passing through a 300-400 mesh filter is 100g/1000mL or more;
    优选地,在步骤(7)中,判断所述完井液是否适用于含硫化氢原油进一步包括以下方式:如果待测完井液的pH值为2以上,或者如果反应前后完井液的粘度变化为10mPa.s以上,或者如果反应前后完井液的结晶温度变化为5℃以上,或者如果反应前后完井液的浊度变化为10NTU以上,则所述完井液不适用于含硫化氢原油;Preferably, in step (7), judging whether the completion fluid is suitable for crude oil containing hydrogen sulfide further comprises the following manner: if the pH value of the completion fluid to be tested is greater than 2, or if the viscosity of the completion fluid before and after the reaction changes by more than 10 mPa.s, or if the crystallization temperature of the completion fluid before and after the reaction changes by more than 5°C, or if the turbidity of the completion fluid before and after the reaction changes by more than 10 NTU, then the completion fluid is not suitable for crude oil containing hydrogen sulfide;
    优选地,在步骤(7)中,判断所述完井液是否适用于含硫化氢原油进一步包括以下方式:如果反应前后完井液的主要离子含量的变化为0.05kg/L以上,则所述完井液不适用于含硫化氢原油。Preferably, in step (7), judging whether the completion fluid is suitable for crude oil containing hydrogen sulfide further comprises the following method: if the change in the main ion content of the completion fluid before and after the reaction is greater than 0.05 kg/L, the completion fluid is not suitable for crude oil containing hydrogen sulfide.
  17. 根据权利要求2所述的水基完井液在含硫化氢原油中适应性的测试方法,其中,在步骤(a)-6中,初步判断所述完井液是否适用于含硫化氢原油包括以下方式:如果反应前后完井液的密度变化大于0.2SG或反应后的完井液存在明显沉淀,则所述完井液不适用于含硫化氢原油;如果反应前后完井液的密度变化为0.2SG以下且反应后的完井液不存在明显沉淀,则初步判断所述完井液适用于含硫化氢原油;所述明显沉淀为过300~400目的滤网后沉淀的量为100g/1000mL以上;The test method for the adaptability of a water-based completion fluid in a crude oil containing hydrogen sulfide according to claim 2, wherein in step (a)-6, the preliminary judgment of whether the completion fluid is suitable for the crude oil containing hydrogen sulfide includes the following manners: if the density change of the completion fluid before and after the reaction is greater than 0.2SG or there is obvious precipitation in the completion fluid after the reaction, the completion fluid is not suitable for the crude oil containing hydrogen sulfide; if the density change of the completion fluid before and after the reaction is less than 0.2SG and there is no obvious precipitation in the completion fluid after the reaction, it is preliminarily judged that the completion fluid is suitable for the crude oil containing hydrogen sulfide; the obvious precipitation is the amount of precipitation after passing through a 300-400 mesh filter screen of more than 100g/1000mL;
    优选地,在步骤(a)-6中,初步判断所述完井液是否适用于含硫化氢原油进一步包括以下方式:如果待测完井液的pH值为2以上,或者如果反应前后完井液的粘度变化为10mPa.s以上,或者如果反应前后完井液的结晶温度变化为5℃以上,或者如果反应前后完井液的浊度变化为10以上,则所述完井液不适用于含硫化氢原油;Preferably, in step (a)-6, the preliminary determination of whether the completion fluid is suitable for crude oil containing hydrogen sulfide further comprises the following manner: if the pH value of the completion fluid to be tested is greater than 2, or if the viscosity of the completion fluid before and after the reaction changes by more than 10 mPa.s, or if the crystallization temperature of the completion fluid before and after the reaction changes by more than 5°C, or if the turbidity of the completion fluid before and after the reaction changes by more than 10, then the completion fluid is not suitable for crude oil containing hydrogen sulfide;
    优选地,在步骤(a)-6中,初步判断所述完井液是否适用于含硫化氢原油进一步 包括以下方式:如果反应前后完井液的主要离子含量的变化为0.05kg/L以上,则所述完井液不适用于含硫化氢原油。Preferably, in step (a)-6, it is preliminarily determined whether the completion fluid is suitable for further use in crude oil containing hydrogen sulfide. The method includes the following: if the change in the main ion content of the completion fluid before and after the reaction is greater than 0.05 kg/L, the completion fluid is not suitable for crude oil containing hydrogen sulfide.
  18. 一种水基完井液在含硫化氢原油中适应性的测试设备,所述设备用于实现权利要求1-17中任一项所述的水基完井液在含硫化氢原油中适应性的测试方法,所述设备至少包括:高温高压反应釜、硫化氢罐、完井液通入管线、气体排出管线、测压装置以及温度控制装置;所述温度控制装置包括加热单元、测温单元和调节单元;A testing device for the adaptability of a water-based completion fluid in a hydrogen sulfide-containing crude oil, the device being used to implement the testing method for the adaptability of a water-based completion fluid in a hydrogen sulfide-containing crude oil as described in any one of claims 1 to 17, the device comprising at least: a high-temperature and high-pressure reactor, a hydrogen sulfide tank, a completion fluid inlet pipeline, a gas outlet pipeline, a pressure measuring device, and a temperature control device; the temperature control device comprising a heating unit, a temperature measuring unit, and a regulating unit;
    其中,所述硫化氢罐通过管线连接于所述高温高压反应釜;所述完井液通入管线连接于所述高温高压反应釜;所述气体排出管线连接于所述高温高压反应釜;所述测压装置通过三通设置于所述气体排出管线上;所述加热单元设置于所述高温高压反应釜的内部;所述测温单元连接于所述高温高压反应釜;所述调节单元收集所述测温单元测定的温度后,控制所述加热单元的加热强度以实现对所述高温高压反应釜的温度的调整。Wherein, the hydrogen sulfide tank is connected to the high-temperature and high-pressure reactor through a pipeline; the completion fluid inlet pipeline is connected to the high-temperature and high-pressure reactor; the gas exhaust pipeline is connected to the high-temperature and high-pressure reactor; the pressure measuring device is arranged on the gas exhaust pipeline through a tee; the heating unit is arranged inside the high-temperature and high-pressure reactor; the temperature measuring unit is connected to the high-temperature and high-pressure reactor; after the regulating unit collects the temperature measured by the temperature measuring unit, it controls the heating intensity of the heating unit to adjust the temperature of the high-temperature and high-pressure reactor.
  19. 根据权利要求18所述的水基完井液在含硫化氢原油中适应性的测试设备,其中,所述硫化氢罐的罐口设置有减压调节器;The testing equipment for the adaptability of water-based completion fluid in crude oil containing hydrogen sulfide according to claim 18, wherein the tank mouth of the hydrogen sulfide tank is provided with a pressure reducing regulator;
    所述硫化氢罐的罐口设置有补压阀,所述补压阀控制针阀和单向阀。The tank mouth of the hydrogen sulfide tank is provided with a pressure-compensating valve, and the pressure-compensating valve controls a needle valve and a one-way valve.
  20. 根据权利要求18所述的水基完井液在含硫化氢原油中适应性的测试设备,其中,所述测试设备还包括二氧化碳罐,所述二氧化碳罐通过三通连接于所述硫化氢罐与所述高温高压反应釜相连接的管线。 The testing equipment for the adaptability of water-based completion fluid in hydrogen sulfide-containing crude oil according to claim 18, wherein the testing equipment also includes a carbon dioxide tank, and the carbon dioxide tank is connected to the pipeline connecting the hydrogen sulfide tank and the high-temperature and high-pressure reactor through a tee.
PCT/CN2023/104395 2022-09-30 2023-06-30 Test method and device for the adaptability of water-based completion fluid in crude oil containing hydrogen sulfide WO2024066592A1 (en)

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Citations (9)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US20080126383A1 (en) * 2006-09-11 2008-05-29 Tetra Technologies, Inc. System and method for predicting compatibility of fluids with metals
US20100144559A1 (en) * 2006-08-03 2010-06-10 Baker Hughes Incorporated Kinetic Gas Hydrate Inhibitors in Completion Fluids
CN103645285A (en) * 2013-12-17 2014-03-19 中国海洋石油总公司 Visualized natural gas hydrate simulation test device and method
CN104155232A (en) * 2014-07-31 2014-11-19 中国石油大学(北京) Device for evaluating sulfur resistance of gel used in well completion process of unbalanced drill
CN104213905A (en) * 2013-06-05 2014-12-17 中国石油天然气股份有限公司 Automatic well killing process method and device for downhole operation
CN107159058A (en) * 2017-06-29 2017-09-15 新疆科力新技术发展股份有限公司 The method for automating high-temperature high-voltage reaction device and gasification and non-vaporized synthesis
CN207396273U (en) * 2017-10-18 2018-05-22 西南石油大学 A kind of experimental provision for measuring sulphur deposition influence factor in polymorphic type pit shaft
CN111089940A (en) * 2018-10-24 2020-05-01 中国石油化工股份有限公司 Evaluation device and evaluation method for desulfurization effect of desulfurizing agent
CN114214052A (en) * 2021-12-13 2022-03-22 中海石油(中国)有限公司 Compound corrosion inhibitor for high-density completion fluid in micro-sulfur-containing environment and preparation method and application thereof

Patent Citations (9)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US20100144559A1 (en) * 2006-08-03 2010-06-10 Baker Hughes Incorporated Kinetic Gas Hydrate Inhibitors in Completion Fluids
US20080126383A1 (en) * 2006-09-11 2008-05-29 Tetra Technologies, Inc. System and method for predicting compatibility of fluids with metals
CN104213905A (en) * 2013-06-05 2014-12-17 中国石油天然气股份有限公司 Automatic well killing process method and device for downhole operation
CN103645285A (en) * 2013-12-17 2014-03-19 中国海洋石油总公司 Visualized natural gas hydrate simulation test device and method
CN104155232A (en) * 2014-07-31 2014-11-19 中国石油大学(北京) Device for evaluating sulfur resistance of gel used in well completion process of unbalanced drill
CN107159058A (en) * 2017-06-29 2017-09-15 新疆科力新技术发展股份有限公司 The method for automating high-temperature high-voltage reaction device and gasification and non-vaporized synthesis
CN207396273U (en) * 2017-10-18 2018-05-22 西南石油大学 A kind of experimental provision for measuring sulphur deposition influence factor in polymorphic type pit shaft
CN111089940A (en) * 2018-10-24 2020-05-01 中国石油化工股份有限公司 Evaluation device and evaluation method for desulfurization effect of desulfurizing agent
CN114214052A (en) * 2021-12-13 2022-03-22 中海石油(中国)有限公司 Compound corrosion inhibitor for high-density completion fluid in micro-sulfur-containing environment and preparation method and application thereof

Non-Patent Citations (1)

* Cited by examiner, † Cited by third party
Title
XIONG, XINDONG, LONG GANG, XIONG XIAO-DONG, QING BING AND XUE LI-NA: "Completion Technologies for HTHP Gas Wells with H2S", NATURAL GAS TECHNOLOGY AND ECONOMY, vol. 05, no. 02, 30 April 2011 (2011-04-30), pages 57 - 80, XP009553764, ISSN: 2095-1132 *

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