Systems and methods for determining the distillation characteristics of petroleum samples through partial distillation

CN117693389BActive Publication Date: 2026-09-01INSTR SCI DE LABORTOIRE ISL
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Patent Information

Application Number
CN202280049507.9
Authority / Receiving Office
CN · China
Patent Type
Patents(China)
Current Assignee / Owner
Priority Date
2021-07-13
Filing Date
2022-07-12
Publication Date
2026-09-01
Estimated Expiration
2042-07-12

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Abstract

An apparatus may include a memory storing instructions and a processor configured to execute instructions to determine an initial mass of a sample; distill the sample up to at least a thermal destruction temperature; record vapor temperature, liquid temperature, and vapor pressure values ​​associated with the sample at a set of time points during distillation; and determine the remaining mass of the sample. The processor is also configured to generate a pressure curve based on the vapor pressure values; calculate the summed integral area of ​​the generated pressure curve; and generate a distillation curve based on the calculated summed integral area, the initial mass of the sample, and the remaining mass of the sample, the distillation curve relating the vapor temperature and liquid temperature values ​​to the percentage of sample mass that has been evaporated.
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Description

Background Technology

[0001] Petroleum products are used as fuel sources for internal combustion engines. Different types of petroleum products have different compositions that exhibit different characteristics. Therefore, different compositions can affect the performance of petroleum products. Distillation processes can be performed on petroleum samples to determine various properties of the samples. Performing distillation processes and characterizing the results presents a variety of challenges. Attached Figure Description

[0002] Figure 1A A distillation apparatus according to an embodiment described herein is shown; Figure 1B A distillation apparatus according to another embodiment described herein is shown; Figure 2 Example components of a controller unit according to embodiments described herein are shown; Figure 3 Exemplary functional components of a controller unit according to embodiments described herein are shown; Figure 4 An example component of a distillation curve database according to embodiments described herein is shown; Figure 5 This is a flowchart of a process for performing distillation according to the embodiments described herein; Figure 6 This is a flowchart of a process for analyzing the results of distillation according to the embodiments described herein; Figure 7 Example graphs of distillation data according to embodiments described herein are shown; and Figure 8 An exemplary distillation curve according to an embodiment described herein is shown. Detailed Implementation

[0003] The following detailed description refers to the accompanying drawings. The same reference numerals in different drawings denote the same or similar elements.

[0004] Distillation apparatus can be used to automate the distillation of petroleum samples. Data obtained during the distillation of the petroleum sample can be used to generate distillation profiles, which correlate one or more properties of the petroleum sample with the temperature during distillation. The distillation profiles can then be used to select safe and reliable transport and storage methods and / or optimize refining processes for the products associated with the petroleum sample.

[0005] Petroleum samples can be placed in a distillation flask and heated to their initial boiling point. Sensors monitor the temperature and pressure of the vapor and the temperature of the liquid. Heating of the sample can continue until it boils dry or reaches another endpoint. One such endpoint is the thermal destruction of the sample. Therefore, the endpoint distillation temperature can be higher than the thermal destruction temperature of the sample. The thermal destruction temperature of a petroleum sample can correspond to the temperature at which hydrocarbons or other components of the petroleum sample begin to undergo chemical degradation through chemical reactions such as oxidation, depolymerization, chain cleavage, side group elimination, and / or other types of chemical reactions that alter the composition of the petroleum sample.

[0006] One method for analyzing the distillation characteristics of heavy petroleum samples with a final distillation temperature above their thermal destruction temperature is to mix the heavy petroleum sample with a solvent and distill the mixture. The distillation profile of the heavy petroleum sample can then be extracted from the data by comparing the obtained distillation profile with that of the pure solvent. However, performing such a procedure is both difficult and time-consuming for operators.

[0007] The embodiments described herein relate to the partial distillation of a petroleum sample at a final distillation temperature above its thermal destruction temperature. For example, the petroleum sample may include crude oil or other heavy petroleum products with a thermal destruction temperature of approximately 400°C. Furthermore, measurements collected during distillation can be used to generate a distillation profile that correlates temperature with the percentage of sample mass distilled to that temperature. To measure the percentage of sample mass, information related to the mass of the sample may need to be obtained and used to generate the distillation profile.

[0008] The embodiments described herein relate to a distillation apparatus that includes a mass sensor to determine the mass of a petroleum sample during distillation. In some embodiments, the mass sensor may be attached to an inner wall of the distillation apparatus. In other embodiments, the mass sensor may be located outside the housing of the distillation apparatus, for example, attached to an outer wall of the distillation apparatus.

[0009] The embodiments described herein further relate to a method for determining an initial and residual mass of a petroleum sample during distillation and using the initial and residual mass to determine a percentage of sample mass at specific time points during distillation. The method may include determining the initial mass of the sample; distilling the sample to at least a thermal destruction temperature; recording a set of vapor temperature values, a set of liquid temperature values, and a set of vapor pressure values ​​associated with the sample at a set of time points during distillation; and determining the residual mass of the sample. The temperature and pressure values ​​can be used to determine physical properties of the sample, such as the density of the liquid and / or the density of the vapor. The method may further include generating a pressure curve based on a set of vapor pressure values; calculating the summed integral area of ​​the generated pressure curve; and generating a distillation curve that correlates the set of vapor temperature values ​​and the set of liquid temperature values ​​with the percentage of sample mass based on the calculated summed integral area, the initial mass of the sample, and the residual mass of the sample.

[0010] To generate an accurate pressure profile, it may be necessary to determine the initial boiling point. The embodiments described herein further relate to determining the initial boiling point during the distillation of a petroleum sample, determining the final boiling point of the petroleum sample, and generating a pressure profile from the initial boiling point to the final boiling point. In some embodiments, determining the initial boiling point may include identifying the time point during distillation at which the vapor pressure value increases to a typical vapor pressure value greater than the zero line, for example, by identifying the time point at which the vapor pressure value is at least a threshold amount greater than the highest value in a set of vapor pressure values ​​designated as the zero line.

[0011] In other embodiments, determining the initial boiling moment may include identifying the time point during distillation where the vapor pressure noise value increases to a typical vapor pressure value greater than the zero line, for example, by identifying the time point where the vapor pressure noise value is at least a threshold amount greater than the highest value in a set of vapor pressure values ​​designated as the zero line. In yet another embodiment, determining the initial boiling moment may include identifying a time point associated with a first positive extreme value of the first derivative of the vapor temperature with respect to time or a first positive extreme value of the second derivative of the vapor temperature with respect to time; or identifying a time point associated with a first negative extreme value of the second derivative of the liquid temperature with respect to time.

[0012] In some embodiments, determining the final boiling point may include detecting temperature fluctuations greater than a fluctuation threshold and determining that thermal destruction has been reached based on the detection of temperature fluctuations greater than the fluctuation threshold.

[0013] Generating a distillation profile may include, for each time point, calculating the ratio of the calculated sum of integral areas of the generated pressure profile to the sum of integral areas of the generated pressure profile up to that time point, multiplied by the ratio of the difference between the initial sample mass and the remaining sample mass to the initial sample mass. In some embodiments, extrapolation techniques may be used to extrapolate the distillation profile to generate a complete distillation profile.

[0014] Figure 1A A distillation apparatus 101 according to an embodiment described herein is shown. An embodiment of the distillation apparatus 101 is shown with a mass sensor 125 attached to the side wall of the distillation apparatus 101. Figure 1A As shown, the distillation apparatus 101 may include a distillation vessel 110, a support 120, a mass sensor 125, a heating element 130, a condenser 145, a steam temperature sensor 150, a liquid temperature sensor 160, a pressure sensor 170, a controller unit 180, and a fan 185.

[0015] Distillation vessel 110 may include a glass flask with a spherical shape to receive sample 112, such as a liquid petroleum sample. The distillation vessel may include a cylindrical neck having a lateral outlet tube 114, a capillary tube 115 located inside the outlet tube 114 and configured to be attached to a condenser 145, and a lid 116 configured to seal the distillation vessel 110. In some embodiments, distillation vessel 110 may be sized to receive 5 to 15 milliliters (ml) of sample 112 for analysis by distillation. In other embodiments, distillation vessel 110 may be sized to receive different volumes of sample.

[0016] Support 120 may include structural support for distillation vessel 110, mass sensor 125, and heating element 130. In some embodiments, mass sensor 125 may include a load cell, such as a strain gauge load cell, piezoelectric load cell, capacitive load cell, and / or other type of load cell that converts mechanical compression into an electrical signal. In other embodiments, mass sensor 125 may include different types of mass sensors, such as a microbalance. Heating element 130 may include a resistance heating element (or other types of heating elements, such as a gas source and a flame) for applying a controllable heat source to sample 112. In some embodiments, mass sensor 125 may be configured to measure the mass of distillation vessel 110 having sample 112 and lid 116, as well as the mass of heating element 130. In other embodiments, distillation vessel 110 may be supported separately from heating element 130 and attached to support 120 (e.g., the wall of distillation apparatus 101) via mass sensor 125. Therefore, the distillation vessel 110 can be heated by heating the enclosed space inside the distillation apparatus 101, and the mass sensor 125 can measure the mass of the distillation vessel 110 with the sample 112 without including the mass of the heating element 130 in the measurement.

[0017] Capillary 115 may include a tube (such as a stainless steel tube) located inside outlet tube 114 to receive vapor during distillation. During distillation, capillary 115 enables overpressure to be generated in distillation vessel 110 via gas flow 140. Condenser 145 may include tubes cooled during distillation by air cooling, liquid cooling, thermoelectric cooling (e.g., using a Peltier module), and / or other types of cooling processes to condense distilled vapor from sample 112 into a recovery vessel (not shown in Figure 1).

[0018] The vapor temperature sensor 150 may include a non-inertial temperature sensor, such as a thermocouple, a resistance temperature sensor, a thermistor temperature sensor, a semiconductor temperature sensor, and / or other types of temperature sensors. The vapor temperature sensor 150 is inserted through an opening in the lid 116 into the neck of the distillation vessel 110 to measure the vapor temperature of the sample 112 during distillation.

[0019] The liquid temperature sensor 160 may include an inertial-free temperature sensor, such as a thermocouple, a resistance temperature sensor, a thermistor temperature sensor, a semiconductor temperature sensor, and / or other types of temperature sensors. The liquid temperature sensor 160 may be inserted downward into the distillation vessel 110 through the opening in the lid 116 to reach the lower portion of the spherical portion of the distillation vessel 110 and immersed in the sample 112 to measure the liquid temperature of the sample 112 during distillation.

[0020] Pressure sensor 170 may include a pressure sensor to measure the vapor pressure inside distillation vessel 110 during distillation. During distillation, pressure sensor 170 may measure the overpressure in distillation vessel 110 caused by vapor passing through outlet pipe 114, rather than the vapor equilibrium pressure in distillation vessel 110. In some embodiments, pressure sensor 170 may include a differential pressure sensor, such as a diaphragm having a piezoresistive, piezoelectric, and / or capacitive strain gauge. In other embodiments, pressure sensor 170 may include another type of pressure sensor, such as an absolute pressure sensor. During distillation, a gas flow 140 is applied to the neck of distillation vessel 110 to protect pressure sensor 170 from the hot vapor. Gas flow 140 may be provided by a miniature compressor (not shown in FIG. 1) controlled by controller unit 180 and may include ambient air, inert gas, and / or other types of gas. For example, using an inert gas can increase the highest possible measurement temperature before thermal damage occurs due to reduced oxidation of the vapor in distillation vessel 110. Gas flow 140 provides a constant pressure during distillation, which needs to be taken into account to determine the actual pressure of the vapor. Because steam passes through the constricted orifice of capillary 115, the pressure inside distillation vessel 110 corresponds to an overpressure relative to ambient pressure. Therefore, the measured steam pressure may depend not only on the equilibrium steam pressure of the sample 112 evaporated at a specific temperature, but also on the heating intensity and the confined flow through capillary 115. Thus, the actual steam pressure is determined by subtracting the zero-line pressure value from the measured pressure.

[0021] The controller unit 180 may include a processor, microcontroller, and / or computer device, which controls the operation of the distillation vessel 110, collects measurements during distillation, and generates a distillation profile based on the collected measurements. Reference will be made below. Figure 2 and Figure 3 Example components of controller unit 180 are described. Fan 185 can operate at the end of distillation to cool distillation vessel 110 after distillation of sample 112 is complete.

[0022] Figure 1B A distillation apparatus 102 according to another embodiment described herein is shown. The distillation apparatus 102 is shown in an embodiment where a mass sensor 125 is located outside the housing 122 of the distillation apparatus 102. For example, the mass sensor 125 may be attached to the outer wall of the housing 122.

[0023] like Figure 1BAs shown, the distillation apparatus 102 may include a distillation vessel 110, a housing 122, a mass sensor 125, a heating element 130, a condenser 145, a steam temperature sensor 150, a liquid temperature sensor 160, a pressure sensor 170, a controller unit 180, and a fan 185. The housing 122 may enclose the heating element 130 and support and / or partially enclose the distillation vessel 110. The heating element 130, condenser 145, steam temperature sensor 150, liquid temperature sensor 160, pressure sensor 170, controller unit 180, and / or fan 185 may be as described above. Figure 1A The operation is described.

[0024] The mass sensor 125 may include a container support 126 and a distillation container 110 for supporting the mass of the sample 112 during measurement. The mass of the sample 112 can be measured by placing the distillation container 110 containing the sample 112 on the container support 126 before distillation to measure the initial mass; placing it on the heating element 130 to perform distillation; and then placing it back on the container support 126 after distillation to measure the remaining mass of the sample 112 after distillation.

[0025] Although Figure 1A The distillation apparatus 101 in the middle enables the measurement of the mass of the sample 112 when the distillation vessel 110 is in the appropriate position for distillation and may not require moving the distillation vessel 110 to measure the initial mass and remaining mass of the sample 112, but the distillation apparatus 101 may require a more complex construction. Figure 1B The distillation apparatus 102 may require moving the distillation vessel 110 before and / or after distillation to measure the mass of the sample 112, but this allows for a simpler construction of the distillation apparatus 102. Although Figure 1A and 1B Exemplary components of distillation apparatus 101 and 102 are shown, but in other embodiments, distillation apparatus 101 and / or 102 may include components that are more... Figure 1A and 1B The aforementioned fewer components, different components, different configuration components, or additional components. Furthermore or alternatively, one or more components in distillation apparatus 101 and / or 102 may perform functions described as being performed by one or more other components of distillation apparatus 101 and / or 102.

[0026] Figure 2 An illustration shows an example component of the controller unit 180 according to an embodiment described herein. Figure 2 As shown, the controller unit 180 may include a bus 210, a processor 220, a memory 230, an input device 240, an output device 250, and a communication interface 260.

[0027] Bus 210 may include paths that allow communication between components of device 200. Processor 220 may include any type of single-core processor, multi-core processor, microprocessor, latch-based processor, and / or processing logic (or various types of processors, microprocessors, and / or processing logic) that interprets and executes instructions. In other embodiments, processor 220 may include application-specific integrated circuits (ASICs), field-programmable gate arrays (FPGAs), and / or other types of integrated circuits or processing logic.

[0028] Memory 230 may include any type of dynamic storage device capable of storing information and / or instructions for execution by processor 220 and / or any type of non-volatile storage device capable of storing information for use by processor 220. For example, memory 230 may include random access memory (RAM) or other types of dynamic storage devices, read-only memory (ROM) devices or other types of static storage devices, content-addressable memory (CAM), magnetic and / or optical recording memory devices and their corresponding drives (such as hard disk drives, optical drives, etc.), and / or removable forms of memory (such as flash memory).

[0029] Input device 240 allows an operator to input information into device 200. Input device 240 may include, for example, a keyboard, mouse, pen, microphone, remote control, audio capture device, image and / or video capture device, touchscreen display, and / or other types of input devices. In some embodiments, device 200 may be remotely managed and may not include input device 240. In other words, device 200 may be "headless" and may, for example, not include a keyboard.

[0030] Output device 250 can output information to the operator of device 200. Output device 250 may include a display, printer, speaker, and / or other types of output devices. For example, device 200 may include a display, which may include a liquid crystal display (LCD), a light-emitting diode (LED) display, etc., for displaying content to the operator. In some embodiments, device 200 can be remotely managed and may not include output device 250. In other words, device 200 may be "headless" and may, for example, not include a display.

[0031] Communication interface 260 may include a transceiver enabling device 200 to communicate with other devices and / or systems via wireless communication (e.g., radio frequency, infrared, and / or visual optics), wired communication (e.g., wires, twisted pairs, coaxial cables, transmission lines, fiber optic cables, and / or waveguides), or a combination of wireless and wired communication. Communication interface 260 may include a transmitter that converts baseband signals to radio frequency (RF) signals and / or a receiver that converts RF signals to baseband signals. Communication interface 260 may be coupled to an antenna for transmitting and receiving RF signals.

[0032] Communication interface 260 may include logic components, including input and / or output ports, input and / or output systems, and / or other input and output components that facilitate the transfer of data to other devices. For example, communication interface 260 may include a network interface card (such as an Ethernet card) for wired communication and / or a wireless network interface card (such as a WiFi card) for wireless communication. Communication interface 260 may also include a Universal Serial Bus (USB) port for communication over wired cables, a Bluetooth™ wireless interface, a Radio Frequency Identification (RFID) interface, a Near Field Communication (NFC) wireless interface, and / or any other type of interface that converts data from one form to another.

[0033] As will be described in detail below, apparatus 200 can perform certain operations related to performing a distillation process and generating a distillation curve based on the results of the distillation process. Apparatus 200 can perform these operations in response to processor 220 executing software instructions contained in a computer-readable medium (such as memory 230). A computer-readable medium can be defined as a non-transitory storage device. The memory device can be implemented in a single physical memory device or distributed across multiple physical memory devices. Software instructions can be read into memory 230 from another computer-readable medium or another device. The software instructions contained in memory 230 can cause processor 220 to perform the processes described herein. Alternatively, hard-wired circuitry can be used in place of or in combination with software instructions to perform the processes described herein. Therefore, the embodiments described herein are not limited to any particular combination of hardware circuitry and software.

[0034] Although Figure 2 Example components of the controller unit 180 are shown, but in other embodiments, the controller unit 180 may include more than Figure 2 The fewer components, different components, additional components, or different configuration components described herein. Additionally or alternatively, one or more components of the controller unit 180 may perform one or more tasks described as being performed by one or more other components of the controller unit 180.

[0035] Figure 3 Example functional components of the controller unit 180 are shown. For example, the functional components of the controller unit 180 may be implemented via a processor 220 that executes instructions from the memory 230. Figure 3 As shown, the controller unit 180 may include a distillation manager 310, a heating element controller 320, a data collector 330, a distillation curve generator 340, a distillation curve database (DB) 350, and a user interface 360.

[0036] Distillation manager 310 can manage the distillation process of distillation apparatus 101 or 102. For example, distillation manager 310 can initiate distillation via heating element controller 320 based on a request received from a user through user interface 360. Heating element controller 320 can control heating element 130. Distillation manager 310 can acquire distillation data using data collector 330, generate distillation curves using distillation curve generator 340, and provide the generated distillation curves to the user through user interface 360.

[0037] Data collector 330 manages data collection during distillation. Data collector 330 may include a mass sensor controller 332, a steam temperature sensor controller 334, a liquid temperature sensor controller 336, and a pressure sensor controller 338. Mass sensor controller 332 controls mass sensor 125. Steam temperature sensor controller 334 controls steam temperature sensor 150. Liquid temperature sensor controller 336 controls liquid temperature sensor 160. Pressure sensor controller 338 controls pressure sensor 170.

[0038] Distillation curve generator 340 can generate distillation curves based on data acquired from data collector 330 and stored in distillation curve DB 350. (See below for reference.) Figure 4 Example information that can be stored in the distillation curve DB 350 is described. The distillation curve generator 340 can determine the initial boiling time and the final boiling time from the distillation data and can generate a pressure curve from the initial boiling time to the final boiling time using a set of pressure values ​​included in the distillation data. The distillation curve generator 340 can then calculate the total summative area of ​​the generated pressure curve and, for each time point, calculate the ratio of the summative area up to that time point to the total summative area, multiplied by the ratio of the difference between the initial mass and the remaining mass of the sample to the initial mass of the sample, to generate the mass percentage of the sample distilled up to that time point. The distillation curve generator 340 can then generate a distillation curve that correlates temperature with the mass percentage. In some embodiments, the distillation curve generator 340 can use extrapolation techniques to extrapolate the distillation curve to generate a complete distillation curve.

[0039] User interface 360 ​​may include a user interface that enables a user to control distillation apparatus 101 or 102 and / or receive information generated by controller unit 180 (such as generated distillation curves, information about completed or ongoing distillation processes, and / or other types of information). User interface 360 ​​may be configured to interact with input device 240 and / or output device 250.

[0040] Although Figure 3Example components of the controller unit 180 are shown, but in other embodiments, the controller unit 180 may include more than Figure 3 The fewer components, different components, additional components, or different configuration components described herein. Additionally or alternatively, one or more components of the controller unit 180 may perform one or more tasks described as being performed by one or more other components of the controller unit 180.

[0041] Figure 4 An example component of the DB 350 distillation profile is shown. (Example:) Figure 4 As shown, the distillation curve DB 350 may include one or more distillation records 400. Each distillation record 400 may store information related to a specific distillation performed using distillation apparatus 101 or 102. The distillation record 400 may include a sample identification (ID) field 410, an initial mass field 420, a remaining mass field 430, and a distillation data table 440.

[0042] The Sample ID field 410 can store an ID associated with distillation. The Initial Mass field 420 can store the initial mass associated with the distilled sample (e.g., Sample 112). The Remaining Mass field 430 can store the remaining mass associated with the distilled sample. The Distillation Data Table 440 can store distillation data associated with the distillation of the sample. The Distillation Data Table 440 may include a set of time point entries 440. Each time point entry 440 can store information related to a specific time point during distillation.

[0043] For example, time point entry 440 may include a time field 442, a steam temperature field 444, a liquid temperature field 446, a measured pressure field 448, an actual pressure field 450, a density field 452, a total area field 454, and a mass percentage field 456. Time field 442 may store information identifying a specific time point. Steam temperature field 444 may store a steam temperature value associated with a specific time point. Liquid temperature field 446 may store a liquid temperature value associated with a specific time point. Measured pressure field 448 may store a measured steam pressure value associated with a specific time point. The measured steam pressure value may correspond to the overpressure generated in distillation vessel 110 during distillation due to steam passing through outlet pipe 114. Actual pressure field 450 may store an actual steam pressure field, associated with a specific time point, and calculated using the difference between the measured pressure field associated with the specific time point and the ambient pressure in distillation vessel 110 with gas flow 140.

[0044] The density field 452 may include the calculated steam density value related to a specific point in time. The total area field 454 may store the total integrated area value calculated for a specific point in time. The mass percentage field 456 may store the mass percentage value calculated for a specific point in time.

[0045] Although Figure 4 An example component of the distillation profile DB 350 is shown, but in other embodiments, the distillation profile DB 350 may include a larger... Figure 4 The fewer components, different components, additional components, or different configuration components described herein.

[0046] Figure 5 This is a flowchart of a distillation process 500 performed according to embodiments described herein. In some embodiments, Figure 5 The process can be performed by and / or using distillation apparatus 101 or 102. In other embodiments, Figure 5 Part or all of the process may be performed by or using another device or a group of devices independent of distillation apparatus 101 and / or 102.

[0047] like Figure 5 As shown, process 500 may include determining the initial mass of the sample (block 510). For example, after sample 112 is placed in distillation vessel 110, controller unit 180 may use mass sensor 125 to record the initial mass of sample 112. Process 500 may further include initiating distillation of the sample (block 520); recording vapor temperature, liquid temperature, and vapor pressure values ​​at each of a set of time points during distillation (block 530); and distilling the sample to at least the thermal destruction temperature (block 540). For example, controller unit 180 may initiate gas flow 140 and then initiate heating of distillation vessel 110 using heating element 130. Controller unit 180 may acquire vapor temperature, liquid temperature, and vapor pressure values ​​using vapor temperature sensor 150, liquid temperature sensor 160, and pressure sensor 170, respectively.

[0048] Distillation can continue until the thermal destruction temperature is reached. In some embodiments, thermal destruction can be determined by visual inspection by the operator. For example, the operator can observe changes in the color of the vapor being distilled in distillation vessel 110, changes observed in sample 112, etc. In other embodiments, thermal destruction can be automatically detected by controller unit 180 based on temperature fluctuations. For example, when the thermal destruction temperature is reached, the vapor temperature and / or liquid temperature may stop rising and begin to fluctuate. Controller unit 180 may be configured to detect vapor temperature and / or liquid temperature fluctuations greater than a fluctuation threshold and stop distillation by stopping heating of distillation vessel 110. Controller unit 180 may activate fan 185 to cool distillation vessel 110 at the end of distillation.

[0049] Process 500 may further include measuring the remaining mass of the sample (box 550). For example, controller unit 180 may record the remaining mass of sample 112 using mass sensor 125 after distillation has stopped. Furthermore, process 500 may also include generating a distillation curve based on the initial mass, remaining mass, and a set of recorded vapor temperature, liquid temperature, and vapor pressure values ​​(box 560). Reference will be made below. Figure 6 Describe an example process for generating distillation curves.

[0050] Figure 6 This is a flowchart illustrating the process of analyzing the results of distillation according to the embodiments described herein. In some embodiments, Figure 6 The process can be performed by and / or using distillation apparatus 101 or 102. In other embodiments, Figure 6 Part or all of the process may be performed by or using another device or a set of devices independent of distillation apparatus 101 or 102.

[0051] like Figure 6 As shown, process 600 may include determining an initial boiling point (box 610), determining a final boiling point (box 620), and generating a pressure profile from the initial boiling point to the final boiling point (box 630). In some embodiments, determining the initial boiling point may include identifying the time point during distillation where the vapor pressure value increases to a typical vapor pressure value greater than the zero line, for example, by identifying the time point where the vapor pressure value is higher than the highest value in a set of vapor pressure values ​​designated as the zero line value by at least a threshold amount. For example, the zero line in the data may be established by identifying data points associated with a slope within a specific range of zero slope lines and / or using another technique.

[0052] In other embodiments, determining the initial boiling point may include identifying the time point during distillation where the steam pressure noise value increases to a typical steam pressure value greater than the zero line; for example, identifying the time point where the steam pressure noise value is greater than the highest value in a set of steam pressure values ​​designated as the zero line by at least a threshold amount. In yet another embodiment, determining the initial boiling point may include identifying a time point associated with a sharp rise in steam temperature. This sharp rise in steam temperature may be based on identifying a steam temperature... T vap The first derivative with respect to time t: The first positive value, based on identifying steam temperature T vap Second derivative with respect to time: The first positive value, and / or based on identifying a slowdown in the rate of temperature rise in the liquid, characterized by a decrease in the liquid temperature. T liq Relative to time Tvap Second derivative with respect to time: The first negative extreme value.

[0053] In some embodiments, determining the final boiling point may include detecting temperature fluctuations greater than a fluctuation threshold and determining that thermal destruction has been reached based on the detected temperature fluctuations greater than the fluctuation threshold.

[0054] Process 600 may further include calculating the total sum-of-the-parts area of ​​the generated pressure curve (box 640) and, for each time point, calculating the ratio of the total sum-of-the-parts area of ​​the generated pressure curve to the sum-of-the-parts area up to that time point, and then multiplying it by the ratio of the difference between the initial mass and the remaining mass to the initial mass (box 650). For example, controller unit 180 may calculate the total sum-of-the-parts area under the pressure curve. SS m Defined as: in P vap Corresponding to steam pressure, t Corresponding to time, ρ vap This corresponds to vapor density. For example, the ideal gas law can be used to determine vapor density.

[0055] Once the total area of ​​integration is determined, at time point i The mass percentage of the sample evaporated at the location can be calculated as follows: in m init Corresponding to the initial mass and m res The corresponding remaining mass.

[0056] Process 600 may further include generating a distillation profile that correlates temperature with the mass percentage of the evaporated sample based on a calculated ratio (box 660). For example, controller unit 180 can generate a distillation profile for each time point. i The calculated time points i The percentage of mass at that point in time i The distillation curve is generated by correlating the steam temperature and the liquid temperature.

[0057] Figure 7 An example plot 700 of distillation data according to an embodiment described herein is shown. Figure 7 As shown, plot 700 includes vapor temperature values ​​obtained for crude oil samples with a final distillation temperature above the thermal destruction temperature. T vap )Drawing, liquid temperature values ​​( T liq )Drawing and steam pressure values ​​(P vap ) Plot. Plot 700 shows the initial boiling moment 710 where the steam pressure value begins to rise above the zero line at least the threshold. In addition, plot 700 shows the final boiling moment 720 where the steam temperature value and liquid temperature value begin to decrease after thermal destruction begins.

[0058] Figure 8 An exemplary distillation curve 800 according to an embodiment described herein is shown. Figure 8 As shown, the distillation curve represents the mass percentage of the sample that has been evaporated at a specific temperature. Distillation curve 800 shows the percentage based on the vapor temperature value (T). vap ) plotting and based on liquid temperature values ​​(T) liq (Drawing). For example... Figure 8 As shown, when the thermal destruction temperature is reached, approximately 60% of the sample has been boiled dry or evaporated, resulting in a partial distillation profile. In some embodiments, the partial distillation profile can be extrapolated to a full distillation profile using extrapolation techniques, for example, using a Riaz distribution model with a determined initial boiling time and parameters determined from the distillation profile using linear regression. Another extrapolation method that can be used is the Dimudu, Zharkova, and Abayev model of petroleum product fractionation, which uses the initial boiling time, the final boiling time, and a set of coefficients characterizing the component distribution in the sample. Partial and / or full distillation profiles can be used to optimize refining processes and / or select safe transportation and / or storage methods, etc.

[0059] Various preferred embodiments have been described in the foregoing description with reference to the accompanying drawings. However, it will be apparent that various modifications and changes can be made thereto, and many additional embodiments can be implemented without departing from the broader scope of the invention as set forth in the following claims. Therefore, the description and drawings should be considered illustrative rather than restrictive.

[0060] For example, although about Figure 5 and Figure 6 A series of block diagrams are described, but in other embodiments, the order of the blocks can be modified. Furthermore, independent blocks and / or signals can be executed in parallel.

[0061] Clearly, in the embodiments shown in the figures, the above-described systems and / or methods can be implemented using a variety of different forms of software, firmware, and hardware. The actual software code or dedicated control hardware used to implement these systems and methods is not limited to this embodiment. Therefore, the operation and behavior of the systems and methods are not described with reference to specific software code—and it should not be understood that software and control hardware can be designed based on the description herein to implement the systems and methods.

[0062] Furthermore, some of the above-described components may be implemented as parts that perform one or more functions. Components used herein may include hardware (such as a processor, ASIC, or FPGA) or a combination of hardware and software (such as a processor that executes software).

[0063] It should be emphasized that the term "comprising" or "including" when used means the presence of the stated feature, integer, step, or component, but does not exclude the presence of one or more additional features, integers, steps, components, or groups thereof.

[0064] As used herein, the term "logic" can refer to a combination of one or more processors configured to execute instructions stored in one or more memory locations, can refer to hardwired circuitry, and / or can refer to combinations thereof. Furthermore, logic can be contained in a single device or can be distributed across multiple, possibly remote, devices.

[0065] For the purposes of describing and defining the present invention, it is necessary to note that the term "substantially" is used herein to indicate the degree of inherent uncertainty attributable to any quantitative comparison, numerical value, measurement, or other representation. The term "substantially" is also used herein to represent the extent to which a quantitative representation may differ from the stated reference value without altering the essential function of the relevant subject matter.

[0066] Unless explicitly stated otherwise, no element, action, or instruction used in this application should be construed as essential or indispensable to this embodiment. Furthermore, the article "a" as used herein means including one or more items. Additionally, unless explicitly stated otherwise, the phrase "based on" means "at least in part based on".

Claims

1. A method for determining distillation characteristics, comprising: The initial mass of a sample is determined using a mass sensor, wherein the sample comprises crude oil; The sample is distilled down to at least the thermal destruction temperature, wherein distilling the sample down to at least the thermal destruction temperature includes heating the sample up to at least 400 degrees Celsius; At multiple time points during distillation, multiple steam temperature values ​​are determined for the sample using a steam temperature sensor, multiple liquid temperature values ​​are determined for the sample using a liquid temperature sensor, and multiple steam pressure values ​​are determined for the sample using a pressure sensor. The remaining mass of the sample is determined using the mass sensor. A pressure curve is generated based on the multiple steam pressure values; Calculate the summation area of ​​the generated pressure curve; and A distillation curve is generated based on the calculated summative integral area, the initial mass of the sample, and the remaining mass of the sample, the distillation curve relating the plurality of vapor temperature values ​​and the plurality of liquid temperature values ​​to the percentage of the mass of the sample that has been evaporated.

2. The method according to claim 1, wherein, The generated pressure curve includes: Determine the initial boiling point of the sample; Determine the final boiling point of the sample; and Generate the pressure curve from the initial boiling point to the final boiling point.

3. The method according to claim 2, wherein, Determining the initial boiling time of the sample includes: Identify the time points among the plurality of time points associated with a steam pressure value that is at least a threshold amount greater than the highest value in a set of steam pressure values ​​designated as zero line value.

4. The method according to claim 2, wherein, The determination of the initial boiling time of the sample includes: Identify the time points among the plurality of time points associated with a steam pressure noise value that is at least a threshold amount greater than the highest value in a set of steam pressure values ​​designated as zero.

5. The method according to claim 2, wherein, Determining the initial boiling moment of the sample includes at least one of the following: Identify the time point associated with the steam temperature value among the plurality of time points that is associated with the first positive extreme value of the first derivative of the steam temperature with respect to time or the first positive extreme value of the second derivative of the steam temperature with respect to time; or Identify the time point associated with the liquid temperature value among the plurality of time points that is associated with the first negative extreme value of the second derivative of the liquid temperature with respect to time.

6. The method according to claim 1, further comprising: Detect temperature fluctuations exceeding the fluctuation threshold; as well as The thermal damage temperature has been determined to have been reached based on the detected temperature fluctuation exceeding the fluctuation threshold.

7. The method according to claim 1, wherein, Generating the distillation curve includes: The ratio of the calculated total integral area of ​​the pressure curve at the first time point among the plurality of time points to the total integral area of ​​the generated pressure curve up to the first time point is multiplied by the ratio of the difference between the initial mass of the sample and the remaining mass of the sample to the initial mass of the sample.

8. The method according to claim 1, further comprising: Extrapolation techniques are used on the generated distillation curves to generate complete distillation curves.

9. An apparatus for determining distillation characteristics, comprising: Memory, which stores instructions; as well as A processor configured to execute the instructions to: The initial mass of a sample is determined using a mass sensor, wherein the sample comprises crude oil; The sample is distilled down to at least the thermal destruction temperature, wherein distilling the sample down to at least the thermal destruction temperature includes heating the sample up to at least 400 degrees Celsius; At multiple time points during distillation, multiple steam temperature values ​​are determined for the sample using a steam temperature sensor, multiple liquid temperature values ​​are determined for the sample using a liquid temperature sensor, and multiple steam pressure values ​​are determined for the sample using a pressure sensor. The remaining mass of the sample is determined using the mass sensor. A pressure curve is generated based on the multiple steam pressure values; Calculate the summation area of ​​the generated pressure curve; and A distillation curve is generated based on the calculated summative integral area, the initial mass of the sample, and the remaining mass of the sample, the distillation curve relating the plurality of vapor temperature values ​​and the plurality of liquid temperature values ​​to the percentage of the mass of the sample that has been evaporated.

10. The apparatus according to claim 9, wherein, When the pressure curve is generated, the processor is further configured as follows: Determine the initial boiling point of the sample; Determine the final boiling point of the sample; and Generate a pressure curve from the initial boiling point to the final boiling point.

11. The apparatus according to claim 10, wherein, When determining the initial boiling moment of the sample, the processor is further configured to: Identify the time points among the plurality of time points associated with a steam pressure value that is at least a threshold amount greater than the highest value in a set of steam pressure values ​​designated as zero line value.

12. The apparatus according to claim 10, wherein, When determining the initial boiling moment of the sample, the processor is further configured to: Identify the time points among the plurality of time points associated with a steam pressure noise value that is at least a threshold amount greater than the highest value in a set of steam pressure values ​​designated as zero.

13. The apparatus according to claim 10, wherein, When determining the initial boiling moment of the sample, the processor is further configured to perform at least one of the following: Identify the time point associated with the steam temperature value among the plurality of time points that is associated with the first positive extreme value of the first derivative of the steam temperature with respect to time or the first positive extreme value of the second derivative of the steam temperature with respect to time; or Identify the time point associated with the liquid temperature value among the plurality of time points that is associated with the first negative extreme value of the second derivative of the liquid temperature with respect to time.

14. The apparatus according to claim 9, wherein, In generating the distillation curve, the processor is further configured as follows: The ratio of the calculated total integral area of ​​the pressure curve at the first time point among the plurality of time points to the total integral area of ​​the generated pressure curve up to the first time point is multiplied by the ratio of the difference between the initial mass of the sample and the remaining mass of the sample to the initial mass of the sample.

15. The apparatus according to claim 9, wherein, The processor is further configured as follows: Extrapolate the generated distillation curve to generate a complete distillation curve.

16. The apparatus of claim 9, further comprising: A distillation flask, comprising a mass sensor to determine the initial mass and the remaining mass of the sample.

17. The apparatus according to claim 16, wherein, The distillation flask further includes: A steam temperature sensor is used to acquire the plurality of steam temperature values; Liquid temperature sensors acquire the plurality of liquid temperature values; and Pressure sensors are used to obtain the multiple steam pressure values.

18. A system for determining distillation characteristics, comprising: The controller is constructed as follows: Determine the initial mass of the sample; The sample is distilled down to at least the thermal destruction temperature, wherein distilling the sample down to at least the thermal destruction temperature includes heating the sample up to at least 400 degrees Celsius; Multiple vapor temperature values, multiple liquid temperature values, and multiple vapor pressure values ​​associated with the sample were determined at multiple time points during distillation. Determine the remaining mass of the sample; A pressure curve is generated based on the multiple steam pressure values; Calculate the summation area of ​​the generated pressure curve; and A distillation curve is generated based on the calculated summed integral area, the initial mass of the sample, and the remaining mass of the sample, the distillation curve relating the plurality of vapor temperature values ​​and the plurality of liquid temperature values ​​to the percentage of the sample mass that has been evaporated; and Distillation apparatus, including A mass sensor is used to determine the initial mass and the remaining mass of the sample; A steam temperature sensor is used to acquire the plurality of steam temperature values; Liquid temperature sensors acquire the plurality of liquid temperature values; and Pressure sensors are used to obtain the multiple steam pressure values.

Citation Information

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