Crude oil condensation point measuring device and method

Abstract

The invention discloses a crude oil condensation point measuring device and method.The crude oil condensation point measuring device comprises a heating-cooling circulation cavity, a sample test tube is arranged in the heating-cooling circulation cavity, and the sample test tube can rotate in the heating-cooling circulation cavity; a temperature sensor, an electromagnetic sensor and a magnetic ball are arranged in the sample test tube; the temperature sensor and the electromagnetic sensor are connected with the control display unit, so that the change of the potential in the movement of the magnetic ball can be monitored in real time, whether the magnetic ball still moves or not is judged, the sample test tube is rotated, and when the magnetic ball does not move any more and no potential change exists, the sample is proved to be solidified; the condensation point temperature of the sample can be obtained by obtaining the current temperature through the temperature sensor, the temperature obtaining accuracy is high, the device does not need a person to hold the sample test tube by hand for operation in the measurement process, the whole test process of the sample is carried out in the heating-cooling circulation cavity, the measurement result has no error, the accuracy is high, and the measurement efficiency is high.

Description

Technical Field

[0001] The invention belongs to the technical field of crude oil freezing point testing and relates to a crude oil freezing point determination device and method. Background Art

[0002] When conducting the solidification point determination method for petroleum products, the solidification point of crude oil is determined according to the standard GB / T510 petroleum product solidification point determination method. The measurement method is as follows: place the sample in a specified test tube and cool it to the expected temperature. Tilt the test tube to 45° from the horizontal and let it stand for 1 minute. Observe whether the liquid surface moves. The highest temperature when the liquid surface does not move is taken as the solidification point of the sample.

[0003] The following shortcomings exist in this experimental process: the experiment is manually operated and requires multiple repetitions to complete, with large human operation errors and low efficiency; during the sample loading process, the sample will stick to the wall, which will make it difficult to subsequently tilt the test tube to observe whether the sample has solidified; the freezing point test tube needs to be taken out to ambient temperature to observe whether the sample has solidified, resulting in large errors in the measurement results; when adding the sample to be tested, the amount poured cannot be accurately controlled; during sample testing, the experimenter can only observe one sample at a time, the test is time-consuming and inefficient; most crude oil is a black, opaque liquid, and there is a certain amount of interference in observing the liquid surface movement or solidification of the sample with the naked eye, resulting in inaccurate test results. Summary of the invention

[0004] The purpose of the present invention is to solve the problems in the prior art that there are large errors in manual operation, the pouring amount of the sample to be tested cannot be controlled, and the measurement results will have errors, and to provide a crude oil freezing point determination device and method.

[0005] In order to achieve the above object, the present invention adopts the following technical solutions:

[0006] A crude oil solidification point determination device comprises a heating-cooling circulation chamber, wherein a sample test tube is arranged in the heating-cooling circulation chamber, and the sample test tube can rotate in the heating-cooling circulation chamber;

[0007] A temperature sensor, an electromagnetic sensor and a magnetic ball are placed inside the sample test tube;

[0008] The temperature sensor and the electromagnetic sensor are connected to a control display unit.

[0009] A further improvement of the present invention is:

[0010] The heating-cooling circulation chamber includes a first heating-refrigeration liquid circulation device, wherein a fluid solution is stored in the first heating-refrigeration liquid circulation device;

[0011] The sample tube is disposed within the fluid solution.

[0012] A rotating bracket is arranged on the inner wall of the heating-cooling circulation chamber, and the sample test tube is fixed on the rotating bracket.

[0013] The sample test tube is connected to a sewage discharge device.

[0014] It also includes a preheating unit, which is used to heat the sample to be measured to a temperature required for measurement;

[0015] The outlet of the preheating unit is connected to the inlet of the sample test tube.

[0016] The preheating unit comprises a second heating-refrigerating liquid circulation device, in which a sample heating tube is placed, and an outlet of the sample heating tube is connected to an inlet of the sample test tube.

[0017] A stirrer is arranged in the sample heating tube.

[0018] A method for determining the freezing point of crude oil comprises the following steps:

[0019] The sample to be tested is placed in the sample test tube, and the temperature of the heating-cooling circulation chamber is controlled to gradually decrease;

[0020] The temperature sensor monitors the temperature of the sample in the warm sample tube in real time;

[0021] Set the test threshold. When the temperature of the sample drops to the threshold, the sample tube is rotated every time the temperature of the heating-cooling circulation chamber drops by 2°C. The rotation of the sample tube will drive the magnetic beads to roll. When the magnetic beads roll, the electromagnetic sensor will collect electrical signals in real time.

[0022] When the electrical signal collected by the electromagnetic sensor in the rotating sample tube no longer changes, it means that the magnetic beads cannot roll and the sample has solidified. The current temperature collected by the temperature sensor is the solidification point temperature of the sample.

[0023] Furthermore, the threshold of the test is 8°C higher than the expected freezing point of the sample.

[0024] Furthermore, when the sample tube is rotated, the sample tube is vertically reversed, and during the flipping process, when the collected electrical signal changes, the sample tube is rotated to its original state;

[0025] The temperature of the heating-cooling circulation chamber is controlled to decrease by 2°C again, and the sample tube is vertically inverted again until the electrical signal no longer changes, and the test is terminated.

[0026] Compared with the prior art, the present invention has the following beneficial effects:

[0027] The invention discloses a crude oil freezing point determination device. The temperature of a sample test environment is adjusted through a heating-cooling circulation chamber. A temperature sensor, an electromagnetic sensor and a magnetic ball are placed in a sample test tube in which a sample to be tested is placed. The sample test tube can rotate inside the heating-cooling circulation chamber. When the sample test tube rotates, the magnetic ball is driven to move. During the movement of the magnetic ball, the electromagnetic sensor collects an electrical signal. The electrical signal is displayed through a control display unit. The change of electric potential during the movement of the magnetic ball can be monitored in real time, and then it can be determined whether the magnetic ball is still moving. The sample test tube is rotated. When the magnetic ball no longer moves, there is no change in electric potential, which proves that the sample has solidified. The freezing point temperature of the sample can be obtained by obtaining the current temperature through the temperature sensor. The temperature acquisition has high accuracy. During the measurement, the device does not need a person to hold the sample test tube for operation, and the whole process of the sample test is carried out in the heating-cooling circulation chamber. The measurement result has no error, high accuracy and high measurement efficiency.

[0028] Furthermore, in the present invention, the sample test tube is driven to rotate by rotating the bracket, so as to facilitate rotation during testing.

[0029] Furthermore, in the present invention, the sample test tube is connected to the sewage discharge device to facilitate the cleaning of the sample in the later stage of the experiment.

[0030] Furthermore, in the present invention, a preheating unit is also provided to ensure that the sample can reach the test temperature before measurement.

[0031] Furthermore, in the present invention, a stirrer is also provided to facilitate sufficient heating of the sample before measurement.

[0032] The invention also discloses a method for determining the freezing point of crude oil. When the temperature is gradually lowered to test the liquid, the magnetic beads are driven to roll by rotating the sample test tube. The electromagnetic sensor captures the electromagnetic signal generated during the rolling of the magnetic beads, and then determines whether the oil is still in a flowing state at this time. The electric signal is displayed by controlling the display unit, and the change of the electric potential in the movement of the magnetic ball can be monitored in real time, and then it can be determined whether the magnetic ball is still moving. The sample test tube is rotated, and when the magnetic ball no longer moves, there is no change in the electric potential, which proves that the sample has solidified. The freezing point temperature of the sample can be obtained by obtaining the current temperature through the temperature sensor. The temperature acquisition has high accuracy, and no manual operation is required during the detection, thereby reducing the error of manual operation. There is no need for human eyes to observe whether the liquid surface moves. The test time is short and the test result is accurate. The whole process of the sample test is carried out in the heating-cooling circulation cavity, thereby reducing the measurement error caused by the transfer process. BRIEF DESCRIPTION OF THE DRAWINGS

[0033] In order to more clearly illustrate the technical solutions of the embodiments of the present invention, the drawings required for use in the embodiments are briefly introduced below. It should be understood that the following drawings only show certain embodiments of the present invention and therefore should not be regarded as limiting the scope. For ordinary technicians in this field, other related drawings can be obtained based on these drawings without creative work.

[0034] Figure 1 It is a structural schematic diagram of the present invention;

[0035] Figure 2 It is a structural schematic diagram of multiple batches of testing of the present invention.

[0036] Among them: 1-computer terminal control platform; 2-drainage device; 3-rotating bracket; 4-first heating-refrigeration liquid circulation device; 5-temperature sensor; 6-electromagnetic sensor; 7-magnetic ball; 8-three-way valve; 9-agitator; 10-sample to be tested; 11-second heating-refrigeration liquid circulation device; 12-electric pump; 13-sample test tube; 14-sample heating tube. DETAILED DESCRIPTION

[0037] In order to make the purpose, technical solutions and advantages of the embodiments of the present invention clearer, the technical solutions in the embodiments of the present invention will be clearly and completely described below in conjunction with the drawings in the embodiments of the present invention. Obviously, the described embodiments are part of the embodiments of the present invention, not all of the embodiments. Generally, the components of the embodiments of the present invention described and shown in the drawings here can be arranged and designed in various different configurations.

[0038] Therefore, the following detailed description of the embodiments of the present invention provided in the accompanying drawings is not intended to limit the scope of the invention claimed for protection, but merely represents selected embodiments of the present invention. Based on the embodiments of the present invention, all other embodiments obtained by ordinary technicians in this field without creative work are within the scope of protection of the present invention.

[0039] It should be noted that similar reference numerals and letters denote similar items in the following drawings, and therefore, once an item is defined in one drawing, further definition and explanation thereof is not required in subsequent drawings.

[0040] In the description of the embodiments of the present invention, it should be noted that if the terms "upper", "lower", "horizontal", "inner", etc. appear, the orientation or position relationship indicated is based on the orientation or position relationship shown in the accompanying drawings, or is the orientation or position relationship in which the product of the invention is usually placed when used. It is only for the convenience of describing the present invention and simplifying the description, and does not indicate or imply that the device or element referred to must have a specific orientation, be constructed and operated in a specific orientation, and therefore cannot be understood as a limitation on the present invention.

[0041] Furthermore, the terms “first”, “second”, etc. are merely used for distinguishing descriptions and should not be understood as indicating or implying relative importance.

[0042] In addition, if the term "horizontal" appears, it does not mean that the component must be absolutely horizontal, but can be slightly tilted. For example, "horizontal" only means that its direction is more horizontal than "vertical", which does not mean that the structure must be completely horizontal, but can be slightly tilted.

[0043] In the description of the embodiments of the present invention, it is also necessary to explain that, unless otherwise clearly stipulated and limited, the terms "set", "installed", "connected" and "connected" should be understood in a broad sense. For example, it can be a fixed connection, a detachable connection, or an integral connection; it can be a mechanical connection or an electrical connection; it can be a direct connection or an indirect connection through an intermediate medium, and it can be the internal connection of two elements.

[0044] For those skilled in the art, the specific meanings of the above terms in the present invention can be understood according to specific circumstances.

[0045] The present invention is further described in detail below in conjunction with the accompanying drawings:

[0046] See also Figure 1 The embodiment of the present invention discloses a crude oil freezing point determination device, which aims to provide a high-precision, high-efficiency, batch, automated, and intelligent crude oil freezing point determination device, which can not only reduce the workload of experimenters and determine multiple samples at the same time, but also reduce the influence of human subjective factors during freezing point measurement, and more accurately determine the freezing point of crude oil. At the same time, batch operation can avoid the cold bath device from heating and cooling back and forth, and can effectively reduce energy consumption.

[0047] include:

[0048] Computer terminal control platform 1; sewage discharge device 2; rotating bracket 3; first heating-refrigerating liquid circulation device 4; temperature sensor 5; electromagnetic sensor 6; magnetic ball 7; three-way valve 8; stirrer 9; sample to be tested 10; second heating-refrigerating liquid circulation device 11; electric pump 12; sample test tube 13 and sample heating tube 14.

[0049] In the embodiment of the present invention, the first heating-refrigerating liquid circulation device 4 is connected to the computer terminal control platform 1. The first heating-refrigerating liquid circulation device 4 is provided with a fluid containing cavity, i.e., a sample tube 13. The sample tube 13 is connected to a rotating bracket 3. The rotating bracket 3 can be electrically connected to the computer terminal control platform 1 and can adjust the sample tube 13 to stand upright, tilted, or reversed. A magnetic ball 7, a temperature sensor 5, and an electromagnetic sensor 6 are placed in the sample tube 13. The temperature sensor 5 and the electromagnetic sensor 6 are both connected to corresponding signal conversion and processing devices. The signal conversion and processing devices are respectively connected to corresponding data acquisition cards. The data acquisition cards are all connected to the computer terminal control platform 1. The bottom of the sample tube 13 is respectively connected to a sewage discharge device 2 and a sample heating tube 14, both of which are connected to the computer terminal control platform 1.

[0050] Example 1

[0051] The embodiment of the present invention discloses a crude oil freezing point determination device, comprising a heating-cooling circulation chamber, wherein a sample tube 13 is arranged in the heating-cooling circulation chamber, and the sample tube 13 can rotate inside the heating-cooling circulation chamber; a temperature sensor 5, an electromagnetic sensor 6 and a magnetic ball 7 are placed inside the sample tube 13; the temperature sensor 5 and the electromagnetic sensor 6 are connected to a control display unit.

[0052] Example 2

[0053] The embodiment of the present invention discloses a crude oil freezing point determination device, comprising a heating-cooling circulation cavity, wherein a sample tube 13 is arranged in the heating-cooling circulation cavity, and the sample tube 13 can rotate inside the heating-cooling circulation cavity; a temperature sensor 5, an electromagnetic sensor 6 and a magnetic ball 7 are placed inside the sample tube 13; the temperature sensor 5 and the electromagnetic sensor 6 are connected to a control display unit, the heating-cooling circulation cavity comprises a first heating-refrigeration liquid circulation device 4, and a fluid solution is stored inside the first heating-refrigeration liquid circulation device 4; the sample tube 13 is arranged inside the fluid solution.

[0054] In this embodiment, the first heating-cooling liquid circulation device 4 is an existing box, which can heat or cool itself by adjusting the switch.

[0055] Example 3

[0056] The embodiment of the present invention discloses a crude oil freezing point determination device, comprising a heating-cooling circulation chamber, wherein a sample tube 13 is arranged in the heating-cooling circulation chamber, and the sample tube 13 can rotate inside the heating-cooling circulation chamber; a temperature sensor 5, an electromagnetic sensor 6 and a magnetic ball 7 are placed inside the sample tube 13; the temperature sensor 5 and the electromagnetic sensor 6 are connected to a control display unit; a rotating bracket 3 is arranged on the inner wall of the heating-cooling circulation chamber, and the sample tube 13 is fixed on the rotating bracket 3.

[0057] In this embodiment, the rotating bracket 3 may be connected to a motor, and the rotating bracket 3 is driven and adjusted by the motor to rotate. A cavity is provided on the rotating bracket 3, and the sample test tube 13 is fixed in the cavity.

[0058] Example 4

[0059] The embodiment of the present invention discloses a crude oil freezing point determination device, comprising a heating-cooling circulation chamber, wherein a sample tube 13 is arranged in the heating-cooling circulation chamber, and the sample tube 13 can rotate inside the heating-cooling circulation chamber; a temperature sensor 5, an electromagnetic sensor 6 and a magnetic ball 7 are placed inside the sample tube 13; the temperature sensor 5 and the electromagnetic sensor 6 are connected to a control display unit; and the sample tube 13 is connected to a sewage discharge device 2.

[0060] In the embodiment of the present invention, the sewage discharge device 2 is connected to the bottom of the sample test tube 13 through a pipeline, and the sewage discharge device 2 can be used to recover the sample after the experiment.

[0061] Example 5

[0062] The embodiment of the present invention discloses a crude oil freezing point determination device, comprising a heating-cooling circulation chamber, wherein a sample test tube 13 is arranged in the heating-cooling circulation chamber, and the sample test tube 13 can rotate inside the heating-cooling circulation chamber; a temperature sensor 5, an electromagnetic sensor 6 and a magnetic ball 7 are placed inside the sample test tube 13; the temperature sensor 5 and the electromagnetic sensor 6 are connected to a control display unit; and a preheating unit is also included, wherein the preheating unit is used to heat the sample to be tested to a temperature required for measurement; the outlet of the preheating unit is connected to the inlet of the sample test tube 13.

[0063] Example 6

[0064] This embodiment discloses a crude oil freezing point determination device based on Embodiment 5, including a heating-cooling circulation cavity, in which a sample tube 13 is arranged, and the sample tube 13 can rotate inside the heating-cooling circulation cavity; a temperature sensor 5, an electromagnetic sensor 6 and a magnetic ball 7 are placed inside the sample tube 13; the temperature sensor 5 and the electromagnetic sensor 6 are connected to a control display unit; the preheating unit includes a second heating-cooling liquid circulation device 11, in which a sample heating tube 14 is placed, and the outlet of the sample heating tube 14 is connected to the inlet of the sample tube 13.

[0065] Furthermore, liquid is also stored in the second heating-cooling liquid circulation device 11, and the internal sample heating tube 14 is heated or cooled by the liquid. A stirrer 9 is arranged on the top of the second heating-cooling liquid circulation device 11. The stirrer 9 passes through the top of the sample heating tube 14 from top to bottom, and the lower end of the stirrer 9 extends into the interior of the sample heating tube 14 to stir the internal sample 10 to be tested so as to quickly and fully heat it to the temperature required for measurement.

[0066] Furthermore, in the embodiment of the present invention, an electric pump 12 is also included, and a pipe is connected to the sample heating tube 14, one end of the pipe is connected to the sample heating tube 14, and the other end is connected to the inlet of the sample test tube 13, and a three-way valve 8 is installed on the pipe. The electric pump 12 drives the sample to be tested 10 in the sample heating tube 14 to enter the sample test tube 13.

[0067] The embodiment of the present invention also discloses a method for determining the pour point of crude oil, comprising the following steps:

[0068] Step 1:

[0069] Inject liquid into the sample heating tube 14 until the liquid level reaches the safety mark, and stop injecting liquid into the sample heating tube 14;

[0070] The second heating-refrigerating liquid circulation device 11 is started, and the second heating-refrigerating liquid circulation device 11 is controlled by the computer terminal control platform 1 to heat the liquid in the sample heating tube 14 to the sample loading temperature;

[0071] Step 2:

[0072] The oil sample to be measured after preheating and stirring is passed through a pipeline from the sample heating tube 14 into the sample test tube 13 to the limit of the sample loading amount.

[0073] Step 3:

[0074] The temperature of the heating-cooling liquid circulator 11 is adjusted to achieve a cooling rate of the oil sample of 0.5-1°C / min. When the oil sample drops to 8°C above the expected freezing point, the rotating bracket 3 is rotated every 2°C to reverse the sample tube 13. During the reversal process, the magnetic beads 7 roll with the sample, and the electromagnetic sensor 6 collects an electrical signal.

[0075] During this process, the image of the electromagnetic sensor 6 is monitored in real time, and the electrical signal is mainly observed. If a change in the induced potential is found, the sample tube 13 is quickly turned back to its original position, and the temperature is continued to drop by 2°C. This operation is repeated until the induced potential does not change during the reversal of the experimental sample, indicating that the experimental sample has been gelled. This temperature is the gelling point temperature, and finally the gelling point temperature is recorded.

[0076] Step 4:

[0077] Then the cavity is turned back to 0°, i.e., a vertical position, and the sample in the sample tube 13 is discharged through the sewage discharge device 2. Subsequently, a cleaning agent can be injected into the cavity. After cleaning, the waste liquid is discharged and the power supply is cut off.

[0078] See also Figure 2 The present invention can also increase the volume of the first heating-refrigerating liquid circulation device 4, place multiple sample tubes 13, and test the samples in the multiple sample tubes 13 at the same time, so as to realize batch experiments and improve the efficiency of the experiments.

[0079] The embodiment of the present invention can complete 40 to 60 samples of crude oil and oil product freezing point tests in one working day. The energy consumption of the same workload is reduced by 80% compared with the conventional manual method, and the number of laboratory personnel is reduced by 75%. The measurement time of batch samples is reduced, the work efficiency is improved, and the laboratory operating cost is reduced. At the same time, the experimental test results are more accurate, and the equipment can be used.

[0080] The above are only preferred embodiments of the present invention and are not intended to limit the present invention. For those skilled in the art, the present invention may have various modifications and variations. Any modification, equivalent replacement, improvement, etc. made within the spirit and principle of the present invention shall be included in the protection scope of the present invention.

Claims

1. A crude oil pour point measuring device, characterized in that: It comprises a heating-cooling circulation chamber, in which a sample test tube (13) is arranged, and the sample test tube (13) can rotate inside the heating-cooling circulation chamber; A temperature sensor (5), an electromagnetic sensor (6) and a magnetic ball (7) are placed inside the sample test tube (13); The temperature sensor (5) and the electromagnetic sensor (6) are connected to a control display unit.

2. A crude oil pour point measuring device according to claim 1, characterized in that: The heating-cooling circulation chamber comprises a first heating-refrigerating liquid circulation device (4), wherein a fluid solution is stored inside the first heating-refrigerating liquid circulation device (4); The sample tube (13) is arranged inside the fluid solution.

3. A crude oil pour point measuring device according to claim 1, characterized in that: A rotating bracket (3) is arranged on the inner wall of the heating-cooling circulation chamber, and the sample test tube (13) is fixed on the rotating bracket (3).

4. A crude oil pour point measuring device according to claim 1, characterized in that: The sample test tube (13) is connected to the sewage discharge device (2).

5. The crude oil pour point measuring device according to claim 1, characterized in that: It also includes a preheating unit, which is used to heat the sample to be measured to a temperature required for measurement; The outlet of the preheating unit is connected to the inlet of the sample test tube (13).

6. A crude oil pour point measuring device according to claim 5, characterized in that: The preheating unit comprises a second heating-refrigerating liquid circulation device (11), a sample heating tube (14) is placed in the second heating-refrigerating liquid circulation device (11), and the outlet of the sample heating tube (14) is connected to the inlet of the sample test tube (13).

7. A crude oil pour point measuring device according to claim 6, characterized in that: A stirrer (9) is arranged inside the sample heating tube (14).

8. A method for determining the pour point of crude oil, characterized in that: The following steps are involved: Placing the sample to be tested in the sample test tube (13), and controlling the temperature of the heating-cooling circulation chamber to gradually decrease; The temperature sensor (5) monitors the temperature of the sample in the warm sample test tube (13) in real time; A test threshold is set. When the temperature of the sample drops to the threshold, the sample test tube (13) is rotated once every time the temperature of the heating-cooling circulation chamber drops by 2°C. The rotation of the sample test tube (13) drives the magnetic beads (7) to roll. When the magnetic beads (7) roll, the electromagnetic sensor (6) collects electrical signals in real time. When the electrical signal collected by the electromagnetic sensor (6) in the rotating sample tube (13) no longer changes, it means that the magnetic beads (7) cannot roll and the sample has solidified. The current temperature collected by the temperature sensor (5) is the solidification point temperature of the sample.

9. A method for determining the pour point of crude oil according to claim 8, characterized in that: The threshold of the test is 8°C above the expected freezing point of the sample.

10. A method for determining the freezing point of crude oil according to claim 9, characterized in that: When rotating the sample test tube (13), the sample test tube (13) is vertically reversed, and during the flipping process, when the collected electrical signal changes, the sample test tube (13) is rotated back to its original state; The temperature of the heating-cooling circulation chamber is controlled to decrease by 2°C again, and the sample tube (13) is vertically inverted again until the electrical signal no longer changes, and the test is terminated.

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