CN110187411B - Scale sample and method for saturation degree of hydrate - Google Patents

Scale sample and method for saturation degree of hydrate Download PDF

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CN110187411B
CN110187411B CN201910496563.7A CN201910496563A CN110187411B CN 110187411 B CN110187411 B CN 110187411B CN 201910496563 A CN201910496563 A CN 201910496563A CN 110187411 B CN110187411 B CN 110187411B
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hydrate
pressure
cavity
gas
water
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CN110187411A (en
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杜庆军
石丽娜
纪云开
赵二猛
周康
侯健
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China University of Petroleum East China
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China University of Petroleum East China
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    • G01MEASURING; TESTING
    • G01VGEOPHYSICS; GRAVITATIONAL MEASUREMENTS; DETECTING MASSES OR OBJECTS; TAGS
    • G01V13/00Manufacturing, calibrating, cleaning, or repairing instruments or devices covered by groups G01V1/00 – G01V11/00

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Abstract

The invention discloses a hydrate saturation scale sample which comprises a non-conductive cavity, a voltage-stabilizing piston, a voltage-stabilizing nut, a detection lead, a digital display pressure sensor, a detection probe, a signal converter, sand, water and gas. The non-conductive cavity is filled with sand, gas and water, the pressure stabilizing piston is arranged on one side of the inner part of the non-conductive cavity and is fixed with one end of the cavity through a pressure stabilizing piston threaded handle and a pressure stabilizing nut, and the water and the gas in the cavity keep stable pressure through rotating the pressure stabilizing nut. The middle part of the non-conductive cavity is provided with a hole, and the hole is connected with a digital display pressure sensor and used for monitoring the pressure of the cavity. The invention also discloses a method for scaling by utilizing the hydrate saturation scale sample, which is characterized in that when an instrument needing to be scaled is scaled, the sample needs to be placed in a low-temperature incubator, and when the hydrate is generated, the signal value of the instrument is recorded and compared with the saturation value corresponding to the sample. The method has strong practicability, and provides a tool for accurately measuring the saturation of the hydrate.

Description

Scale sample and method for saturation degree of hydrate
Technical Field
The invention relates to a hydrate saturation scale sample and a scale method, and belongs to the technical field of unconventional oil and gas development.
Background
Natural gas hydrates are a new type of energy source found in the ocean and in the permafrost for the last two decades. Natural gas hydrate is a solid crystalline substance synthesized from natural gas and water molecules under high pressure and low temperature conditions, is white or light grey like ice and snow in appearance, can be ignited like alcohol blocks, and is popularly called as 'combustible ice'. China has successfully implemented natural gas hydrate trial production in the south China sea Hopkins area, and becomes the fourth country with hydrate trial production capability after Canada, America and Japan.
At present, a great deal of experimental research has been carried out on the development of the natural gas hydrate, particularly on the generation, decomposition, flowing rule and the like of the natural gas hydrate under different conditions. In the research process, the saturation of the hydrate and the change of the hydrate in the development process are the most important indexes for analyzing the exploitation mechanism of the hydrate reservoir. At present, resistivity test probes and acoustic probes are mainly developed by utilizing the electrical property and the acoustic property of natural gas hydrate reservoirs. However, in the practical application process, the detection signal is influenced by various factors, and the detection result is difficult to establish an accurate relation with the true hydrate saturation. Therefore, there is also a lack in the art of calibration standards that can be used to calibrate resistivity test probes and sonic probes.
Disclosure of Invention
The invention provides a hydrate saturation scale sample and a scale method.
The technical scheme of the invention is as follows:
a hydrate saturation scale sample and a scale method are characterized in that the hydrate saturation scale sample comprises a non-conductive cavity, a voltage stabilizing piston, a voltage stabilizing nut, a detection lead, a digital display pressure sensor, a detection probe, a signal converter, sand, water and gas; the sand grains are filled in the non-conductive cavity, and water and gas are filled in pores among the sand grains; the pressure stabilizing piston is arranged at one side of the inner part of the non-conductive cavity and is fixed with one end of the cavity through a pressure stabilizing piston threaded handle and a pressure stabilizing nut, and water and gas in the cavity keep stable pressure through rotating the pressure stabilizing nut; the middle part of the non-conductive cavity is provided with a hole and is connected with a digital display pressure sensor; round holes are formed in the end faces of the two sides of the non-conductive cavity, and the pressure stabilizing piston threaded handle extends out of the round hole in the center of the end face of one side of the non-conductive cavity; the pressure stabilizing piston threaded handle is of a hollow structure, one end of a detection lead is connected with a detection probe placed in sand filled in the cavity through the hollow structure of the threaded handle and a round hole in the end face on the other side of the cavity, the other end of the detection lead on two sides is connected with a signal adapter, and the signal adapter is used for connecting an instrument needing to be calibrated.
A method for carrying out calibration by using the hydrate saturation calibration sample comprises the following steps:
(1) calculating a temperature and pressure relation curve of the generated hydrate according to the gas type in the hydrate saturation scale sample cavity;
(2) designing the pressure during calibration, and determining the temperature of the generated hydrate corresponding to the pressure according to the temperature and pressure relation curve of the hydrate;
(3) the pressure in the cavity is adjusted by rotating the pressure stabilizing nut, so that the digital display pressure gauge reaches the designed pressure;
(4) setting the temperature of the constant temperature box to be lower than the temperature of generating the hydrate but higher than the freezing point temperature of water, placing the hydrate saturation standard sample in the low temperature constant temperature box for a long enough time to enable the hydrate to be completely generated, and adjusting by rotating a pressure stabilizing nut if the pressure of the digital display pressure gauge is inconsistent with the set pressure during the period;
(5) connecting an instrument needing calibration through a detection lead, recording the signal value of the instrument, and calculating the saturation of the hydrate;
(6) and (5) selecting other hydrate saturation scale samples, repeating the steps (3) to (5), inverting the hydrate saturation by using the test result, comparing the hydrate saturation with the saturation value corresponding to the standard sample, and correcting instrument parameters.
The hydrate saturation scale sample is characterized in that: the non-conductive cavity is made of a non-conductive and heat-conductive rigid material, the cavity is of a cylindrical structure, the inner side of the cavity is subjected to roughening treatment, and the withstand pressure is not less than 15 MPa.
The hydrate saturation scale sample is characterized in that: the sand grains are uniform in size and stable in acoustic wave property; the water is saline water; the gas is methane, natural gas, carbon dioxide or other gases capable of generating hydrate.
The hydrate saturation scale sample is characterized in that: one side of the pressure stabilizing piston thread handle is made of a non-conductive but heat-conducting rigid material, and the other side of the pressure stabilizing piston thread handle is made of a rubber material, so that sand grains can be extruded, and the pressure of water and gas in the non-conductive cavity can be changed.
The hydrate saturation scale sample is characterized in that: the hydrate saturation in the non-conductive cavity is determined by calculation according to the volume ratio of water to gas, and a series of standard samples with different hydrate saturations can be manufactured by designing different volume ratios of water to gas.
Drawings
FIG. 1 is a schematic perspective view of a hydrate saturation scale;
FIG. 2 is a side sectional view of a hydrate saturation scale;
FIG. 3 is a graph of temperature versus pressure for methane hydrate formation
Reference numerals: the device comprises a non-conductive cavity 1, sand 2, a gas and water mixture 3, a pressure stabilizing piston 4, a pressure stabilizing piston rubber layer 5, a pressure stabilizing nut 6, a pressure stabilizing piston threaded handle 7, a detection lead 8, a detection probe 9, an opening 9, a pressure sensor 10, a pressure sensor digital display meter 11 and a signal conversion joint 12.
Detailed Description
The invention is further described below with reference to the accompanying drawings and examples.
The hydrate saturation scale sample provided by the invention is of an integral structure. As shown in fig. 1, the hydrate saturation scale sample comprises a non-conductive cavity 1, a voltage-stabilizing piston 3, a voltage-stabilizing nut 5, a detection lead 7, a pressure sensor 10, a detection probe 8, a signal converter 11, sand, water and gas mixture 2; the sand, water and gas mixture 2 is filled in the non-conductive cavity 1, the pressure stabilizing piston 3 is installed at one side of the inner part of the non-conductive cavity and is fixed with one end of the cavity through the pressure stabilizing piston threaded handle 6 and the pressure stabilizing nut 5, and the water and the gas in the cavity keep stable pressure by rotating the pressure stabilizing nut 5. The middle part of the non-conductive cavity is provided with an opening 9 which is connected with a digital display pressure sensor 10. Round holes are formed in the end faces of two sides of the non-conductive cavity 1, and the voltage-stabilizing piston threaded shank 6 extends out of the central round hole in the end face of one side of the non-conductive cavity. The pressure stabilizing piston thread handle 6 is of a hollow structure, one end of the detection lead 7 is connected with a detection probe 8 placed in sand filled in the cavity through the hollow structure of the pressure stabilizing piston thread handle 6 and a round hole on the end face on the other side of the cavity, the other end of the detection lead 7 on two sides is connected with a signal conversion joint 11, and the signal conversion joint 11 is used for connecting an instrument needing to be calibrated.
The specific steps of using a calibration standard with a hydrate saturation of 30% to calibrate an instrument needing calibration are described as follows:
firstly, determining a temperature and pressure relation curve of the generation of the hydrate according to the type of gas in the standard sample. The temperature and pressure relationship curve for methane hydrate is shown in FIG. 3.
Secondly, the pressure when the scales are designed is 4.0MPa, and the temperature of the generated hydrate corresponding to the pressure is determined to be 4.2 ℃ according to the temperature and pressure relation curve of the hydrate in the figure 3;
thirdly, adjusting the pressure in the cavity by rotating the pressure stabilizing nut to enable the display pressure of the digital display pressure gauge to be 4.0 MPa;
fourthly, setting the temperature of the incubator to be lower than the temperature of generating the hydrate and higher than the freezing point, setting the temperature to be 3 ℃, placing the hydrate saturation standard sample in the cryostat for 48 hours to enable the hydrate to be completely generated, and adjusting the temperature by rotating a pressure stabilizing nut if the pressure of the digital display pressure gauge is inconsistent with the set pressure during the period;
fifthly, connecting a resistivity testing instrument needing to be calibrated through a detection lead, and recording the signal value of the instrument;
and sixthly, selecting other hydrate saturation scale samples, repeating the steps (3) to (5), inverting the hydrate saturation by using the test result, comparing the hydrate saturation with the saturation value corresponding to the standard sample, and correcting instrument parameters.

Claims (5)

1. The hydrate saturation scale sample is characterized by comprising a non-conductive cavity, a voltage stabilizing piston, a voltage stabilizing nut, a detection lead, a digital display pressure sensor, a detection probe, a signal converter, sand, water and gas; sand grains are filled in the non-conductive cavity, and water and gas are filled in pores among the sand grains; the pressure stabilizing piston is arranged at one side of the inner part of the non-conductive cavity and is fixed with one end of the cavity through a pressure stabilizing piston threaded handle and a pressure stabilizing nut, and water and gas in the cavity keep stable pressure through rotating the pressure stabilizing nut; the middle part of the non-conductive cavity is provided with a hole and is connected with a digital display pressure sensor; round holes are formed in the end faces of the two sides of the non-conductive cavity, and the pressure stabilizing piston threaded handle extends out of the round hole in the center of the end face of one side of the non-conductive cavity; the pressure stabilizing piston threaded handle is of a hollow structure, one end of a detection lead is connected with a detection probe placed in sand filled in the cavity through the hollow structure of the threaded handle and a round hole in the end face on the other side of the cavity, the other ends of the detection leads on the two sides are respectively connected with a signal conversion joint, and the signal conversion joint is used for connecting an instrument needing to be calibrated; the method for scaling by using the hydrate saturation scale sample comprises the following steps:
(1) calculating a temperature and pressure relation curve of the generated hydrate according to the gas type in the hydrate saturation scale sample cavity;
(2) designing the pressure during calibration, and determining the temperature of the generated hydrate corresponding to the pressure according to the temperature and pressure relation curve of the hydrate;
(3) the pressure in the cavity is adjusted by rotating the pressure stabilizing nut, so that the digital display pressure gauge reaches the designed pressure;
(4) setting the temperature of the constant temperature box to be lower than the temperature of generating the hydrate but higher than the freezing point temperature of water, placing the hydrate saturation standard sample in the low temperature constant temperature box for a long enough time to enable the hydrate to be completely generated, and adjusting by rotating a pressure stabilizing nut if the pressure of the digital display pressure gauge is inconsistent with the set pressure during the period;
(5) connecting an instrument needing calibration through a detection lead, recording the signal value of the instrument, and calculating the saturation of the hydrate;
(6) and (5) selecting other hydrate saturation scale samples, repeating the steps (3) to (5), inverting the hydrate saturation by using the test result, comparing the hydrate saturation with the saturation value corresponding to the standard sample, and correcting instrument parameters.
2. The hydrate saturation scale of claim 1, wherein: the non-conductive cavity is made of a non-conductive and heat-conductive rigid material, the cavity is of a cylindrical structure, the inner side of the cavity is subjected to roughening treatment, and the withstand pressure is not less than 15 MPa.
3. The hydrate saturation scale of claim 1, wherein: the sand grains are uniform in size and stable in acoustic wave property; the water is saline water; the gas is methane, natural gas, carbon dioxide or other gases capable of generating hydrate.
4. The hydrate saturation scale of claim 1, wherein: one side of the pressure stabilizing piston thread handle is made of a non-conductive but heat-conducting rigid material, and the other side of the pressure stabilizing piston thread handle is made of a rubber material, so that sand grains can be extruded, and the pressure of water and gas in the non-conductive cavity can be changed.
5. The hydrate saturation scale of claim 1, wherein: the hydrate saturation in the non-conductive cavity is determined by calculation according to the volume ratio of water to gas, and a series of standard samples with different hydrate saturations can be manufactured by designing different volume ratios of water to gas.
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CN103267807A (en) * 2013-05-03 2013-08-28 上海和伍新材料科技有限公司 Method and device for calibrating probe in ultrasonic detection equipment
CN105572761A (en) * 2015-12-14 2016-05-11 中国石油天然气集团公司 Correction and calibration system of sensing and imaging logging technology
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CN103267807A (en) * 2013-05-03 2013-08-28 上海和伍新材料科技有限公司 Method and device for calibrating probe in ultrasonic detection equipment
CN105572761A (en) * 2015-12-14 2016-05-11 中国石油天然气集团公司 Correction and calibration system of sensing and imaging logging technology
CN109374489A (en) * 2018-08-21 2019-02-22 中国地质大学(武汉) The hydrate sediment NMR relaxation signals amount caliberating device and method of joint X-CT technology
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