Distillation condenser based on two-phase closed thermosyphon

Abstract

To provide a two-phase closed thermosyphon type distillation condenser.SOLUTION: A distillation condenser may include: an inner condenser pipe including an inlet for receiving steam from a distillation container, and an outlet connected to a reception container for receiving a distilled liquid which is condensed from the steam; an outside pipe which surrounds the inner condenser pipe; and a heating element coupled to the exterior of the outside pipe. The distillation condenser may further include a controller that heats a working fluid in the outside pipe, and controls the heating element so that as a result of the heated working fluid, the distillation condenser functions as a two-phase closed thermosyphon (TPCT).SELECTED DRAWING: Figure 1

Description

[Background technology]

[0001] Petroleum products are used as fuel sources in combustion engines. Different types of petroleum products contain different components that exhibit different characteristics. Therefore, different components may affect the performance of the petroleum product. A distillation process may be performed on a petroleum sample to determine various properties of the sample. The distillation process may need to be performed under specific conditions to meet testing requirements. Maintaining precise distillation conditions may pose various challenges. [Brief explanation of the drawings]

[0002] [Figure 1] FIG. 1 illustrates a distillation system according to embodiments described herein. [Figure 2] FIG. 1 illustrates exemplary components and operation of a two-phase closed thermosyphon (TPCT) condenser according to embodiments described herein. [Figure 3] FIG. 1 illustrates an exemplary TPCT condenser according to embodiments described herein. [Figure 4] FIG. 2 illustrates exemplary components of a controller unit according to implementations described herein. [Figure 5] FIG. 2 illustrates exemplary functional components of a controller unit according to implementations described herein. [Figure 6] FIG. 1 illustrates exemplary components of a TPCT condenser settings database according to implementations described herein. [Figure 7] 1 is a flowchart of a process for performing distillation using a TPCT condenser according to embodiments described herein. [Figure 8] FIG. 2 illustrates a first exemplary plot of temperature data for a TPCT condenser according to embodiments described herein. [Figure 9] FIG. 10 illustrates a second exemplary plot of temperature data for a TPCT condenser according to embodiments described herein. DETAILED DESCRIPTION OF THE INVENTION

[0003] The following detailed description refers to the accompanying drawings, in which the same reference numbers in different drawings identify the same or similar elements.

[0004] The distillation apparatus can be used to perform automated distillation of a petroleum sample. Data obtained during the distillation of the petroleum sample can be used to generate a distillation curve, for example, that relates one or more properties of the petroleum sample to the temperature during distillation. The distillation curve can then be used to select a safe and reliable mode of transportation and storage and / or to optimize a refining process for a product associated with the petroleum sample.

[0005] During distillation, a condenser may be used to condense distillation vapors into a liquid distillate, which may be collected in a receiving vessel. The condenser may be cooled, for example, using a circulating cooling bath or using ice water without a circulating bath. To perform accurate distillation analysis and / or to meet test specifications for the distillation of petroleum samples, the condenser may need to meet certain requirements. For example, the temperature gradient along the length of the condenser tube immersed in the cooling bath may need to be below a gradient threshold (e.g., less than 1°C). As another example, the temperature of the condenser tube may need to remain at a specific temperature for a selected distillation sample. Furthermore, if different samples are to be distilled, each with different condenser temperature requirements, it may be necessary to quickly change the condenser temperature. An ice water bath or a circulating cooling bath may not be able to meet such a set of requirements.

[0006] The embodiments described herein relate to a distillation condenser based on a two-phase closed thermosyphon (TPCT). A thermosyphon is a heat exchange mechanism that uses convection due to a temperature gradient to circulate a fluid without the need for a mechanical pump. Closed thermosyphons are isochoric, meaning that the circulating fluid is confined within a fixed volume. Two-phase thermosyphons contain fluid in both the liquid and vapor phases.

[0007] The TPCT condenser may include an inner condenser tube including an inlet for receiving vapor from the distillation vessel and an outlet for connecting to a receiving vessel for receiving distilled liquid condensed from the vapor, an outer tube surrounding the inner condenser tube, and a connecting tube coupled to the outer tube and oriented perpendicular to the outer tube. In some embodiments, the connecting tube may open to a condensation area having a larger surface area. In other embodiments, the connecting tube may connect to a condensation block. The outer tube may contain a working fluid. The TPCT condenser may further include a heating element coupled to the exterior of the outer tube, a cooling element coupled to the connecting tube, and a controller for controlling the heating element and the cooling element.

[0008] The heating element can boil the working fluid and keep it at its boiling point, thus surrounding the inner condenser tube with a constant-temperature liquid bath. In other words, the boiling fluid remains at the same temperature throughout its volume, so the inner condenser tube containing the condensed distillate is maintained at a constant temperature along its entire length. The boiling working fluid vapor rises into the connecting tube, cools as a result of heat removal by the cooling element, condenses, and can fall back into the boiling working fluid as droplets. Thus, gravity-assisted circulation of the TPCT efficiently removes heat from the condenser and, therefore, from the condensed distillate inside the inner condenser tube.

[0009] The minimum volume of working fluid may be significantly smaller than the volume of the outer tube because the porosity of the gas-liquid mixture may increase in volume during boiling of the working fluid (e.g., the volume of the boiling fluid may double or even increase). A larger volume of boiling working fluid may ensure constant contact of the gas-liquid bubbles with the wall of the inner condenser tube, resulting in a lower temperature inertia for cooling the inner condenser tube and allowing for rapid changes in the operating temperature of the TPCT condenser. Continuous boiling of the working fluid may be achieved by controlling a heating element positioned relative to the bottom of the outer tube and a cooling element positioned relative to the top of the connecting tube.

[0010] The TPCT condenser may include multiple temperature sensors for monitoring the temperature inside the TPCT condenser. For example, the TPCT condenser may include a first temperature sensor coupled to the outer tube and positioned closer to the outlet than the inlet, a second temperature sensor coupled to the outer tube and positioned closer to the inlet than the outlet, and a third temperature sensor coupled to the connecting tube.

[0011] The inner condenser tube, the outer tube, and the connecting tube may be fabricated from copper tubing. The copper tubing may enable efficient transfer of heat between the condensed distillate in the inner condenser tube and the working fluid inside the outer tube. Furthermore, in some embodiments, a copper mesh sleeve may extend over the outer surface of the inner condenser tube to enhance heat transfer. In some embodiments, the TPCT condenser may include a condensing block coupled to the connecting tube and configured to increase the surface area of ​​the connecting tube. The condensing block may increase the contact area between the working fluid vapor and the cooling element, enhancing the efficiency of heat removal from the TPCT condenser.

[0012] Additionally, in some embodiments, the TPCT condenser may include a porous ceramic layer disposed on the inner surface of the outer tube adjacent to the heating element. The porous ceramic layer may include, for example, silicon oxide obtained by foaming sodium silicate deposited on a metal surface. The porous ceramic layer may provide nucleation points for boiling of the working fluid and function as an additional boiling stabilizer that may prevent overheating and / or boiling crises from occurring.

[0013] In some embodiments, the working fluid may include an azeotropic mixture of methanol and pentane. In other embodiments, the working fluid may include different types of fluids, such as one or more of methanol, ethanol, pentane, and / or acetone. In still other embodiments, the working fluid may include a hydrofluoroolefin fluid. Hydrofluoroolefins may be used in situations requiring a high level of fire resistance due to their non-flammable nature. An exemplary hydrofluoroolefin that may be used includes cis-1,1,1,4,4,4-hexafluoro-2-butene.

[0014] The controller may be configured to determine a required condenser temperature for the sample, select a heating element setting for the heating element based on the determined required condenser temperature, select a cooling element setting for the cooling element based on the determined required condenser temperature, and apply the selected heating element setting and the selected cooling element setting to the distillation condenser to maintain the required condenser temperature during distillation of the sample. The TPCT condenser may be included in a distillation system including a distillation vessel and a set of sensors coupled to the distillation vessel, and the TPCT condenser may be coupled to the distillation vessel for receiving distillation vapors from the distillation vessel. The distillation system controller may generate a distillation curve for the sample based on values ​​obtained from the set of sensors during distillation of the sample. The distillation system controller may also control the TPCT controller. In other embodiments, the TPCT condenser may be controlled by a separate controller separate from the distillation system controller.

[0015] TPCT condensers may be capable of meeting the requirement of a low temperature gradient along the entire length of the inner condenser tube containing the condensed distillate and providing rapid removal of heat from the condensed distillate. For example, TPCT condensers may be capable of maintaining a constant temperature within ±0.5°C and a minimum temperature gradient along the length of the TPCT condenser of <0.5°C. Furthermore, TPCT condensers allow for rapid changes in the operating temperature of the working fluid bath. TPCT condensers do not require the use of a recirculation pump to circulate the working fluid. Elimination of the pump increases reliability and reduces the need for inspection. Furthermore, TPCT condensers exhibit a lower specific heat capacity compared to liquid recirculation baths or solid metal baths, allowing for spatial separation of the cooling source from the condenser's liquid bath. Separating the cooling element from the working fluid allows for efficient heat removal and easier maintenance and / or modification of the cooling element.

[0016] 1 illustrates a distillation system 100 according to an exemplary embodiment described herein. As shown in FIG. 1, distillation system 100 may include a distillation vessel 110, a TPCT condenser 120, a receiving vessel 122, a distillate level sensor 124, a drop sensor 126, a heating element 130, an enclosure 132, a vapor temperature sensor 150, a liquid temperature sensor 152, a fan 170, a controller unit 180, and a condenser controller 182. It should be understood that in other embodiments, distillation system 100 may include additional elements, such as additional sensors, controllers, heating elements, etc.

[0017] The distillation vessel 110 may include a glass flask having a spherical shape for receiving a sample 112, such as a liquid petroleum sample. The distillation vessel 110 may include a cylindrical neck with a side outlet tube 114 and a cap 116 configured to seal the distillation vessel 110. In some embodiments, the distillation vessel 110 may be sized to receive a specified amount of the sample 112 to be analyzed by distillation. The specified amount may range, for example, from 100 milliliters (ml) to 20 liters. In other embodiments, the distillation vessel 110 may be sized to receive different volumes of sample.

[0018] The TPCT condenser 120 may condense distillate vapor received from the distillation vessel 110 via the outlet tube 114 using a TPCT mechanism. The operation of the TPCT condenser 120 is described below with reference to FIG. 2. The receiving vessel 122 may receive the condensed distillate of the sample 112 via the outlet tube 114 of the TPCT condenser 120. The distillate level sensor 124 may measure the level of distillate collected in the receiving vessel 122 and / or may detect when a predetermined amount of distillate has collected in the receiving vessel 124. The drop sensor 126 may detect, measure, and / or count drops falling from the TPCT condenser 120 into the receiving vessel 122.

[0019] The heating element 130 may include a resistive heating element (or another type of heating element, such as, for example, a gas source and a flame) for applying a controllable heat source to the sample 112. The enclosure 132 may provide structural support for and / or partially or completely enclose the distillation vessel 110, the TPCT condenser 120, the heating element 130, and / or the fan 170. In some embodiments, the enclosure 132 may further provide structural support for and / or partially or completely enclose the controller unit 180 and / or the condenser controller 182.

[0020] The vapor temperature sensor 150 may include, for example, an inertia-free temperature sensor such as a thermocouple, a resistance temperature sensor, a thermistor temperature sensor, a semiconductor temperature sensor, and / or another type of temperature sensor. The vapor temperature sensor 150 may be inserted into the neck of the distillation vessel 110 through an opening in the cap 116 to measure the vapor temperature of the sample 112 during distillation.

[0021] The liquid temperature sensor 152 may include, for example, an inertia-free temperature sensor such as a thermocouple, a resistance temperature sensor, a thermistor temperature sensor, a semiconductor temperature sensor, and / or another type of temperature sensor. The liquid temperature sensor 152 may be inserted into the distillation vessel 110 through an opening in the cap 116 to the bottom of the bulb of the distillation vessel 110 and immersed in the sample 112 to measure the liquid temperature of the sample 112 during distillation. In some embodiments, multiple vapor temperature sensors may be used. A fan 170 may be positioned to cool the enclosure 132 and / or the distillation vessel 110 after distillation of the sample 112 is complete and may be operated at the end of the distillation.

[0022] Controller unit 180 may include a processor, microcontroller, and / or computing device that controls the operation of distillation system 100, collects measurements during distillation, and generates a distillation curve based on the collected measurements. Condenser controller 182 may control the operation of TPCT condenser 120. In some embodiments, the functions of condenser controller 182 may be performed by controller unit 182. Exemplary components of controller unit 180 and / or condenser controller 182 are described below with reference to FIGS. 4, 5, and 6.

[0023] 1 illustrates exemplary components of distillation system 100, in other embodiments, distillation system 100 may include fewer components, different components, components in a different arrangement, or additional components than those illustrated in FIGURE 1. Additionally or alternatively, one or more components of distillation system 100 may perform functions described as being performed by one or more other components of distillation system 100.

[0024] 2 illustrates example components and operation of the TPCT condenser 120. As shown in FIG. 2, the TPCT condenser 120 may include an inner condenser tube 210, an outer tube 220, a connecting tube 230, a heating element 240, a porous ceramic layer 244, a cooling element 250, temperature sensors 262, 264, and 266, and a working fluid 270.

[0025] The inner condenser tube 210 may include an inlet configured to connect to the outlet tube 114 of the distillation vessel 110 to receive vapors of the distilled sample 112. The vapors may condense inside the inner condenser tube 210 to become a distilled liquid. The inner condenser tube 210 may further include an outlet that connects to a receiving vessel 122 (not shown in FIG. 2 ) for receiving the distilled liquid. The inner condenser tube 210 may be oriented such that the inlet is higher than the outlet and the distilled liquid flows downward and out the outlet.

[0026] The outer pipe 220 may surround the inner condenser pipe 210 and form a sealed container around the inner condenser pipe 210. In some embodiments, the outer pipe 220 may be coaxially aligned with the inner condenser pipe 210, with the longitudinal axis of the inner condenser pipe 210 being the same as the longitudinal axis of the outer pipe 220. In other embodiments, the outer pipe 220 may be non-coaxially aligned with the inner condenser pipe 210. For example, the longitudinal axis of the inner condenser pipe 210 may be below the longitudinal axis of the outer pipe 220, which may create more volume above the inner condenser pipe 210 and facilitate upward movement of boiling bubbles and / or vapor into the connecting pipe 230.

[0027] The connecting pipe 230 may be connected to the outer pipe 220 and oriented perpendicular to the longitudinal axis of the outer pipe 220. The connecting pipe 230 may include an area extending from the connecting pipe 230's attachment point to the outer pipe 220, creating a larger surface area coupled to the cooling element 250. The larger surface area may increase the efficiency of heat removal through the wall of the connecting pipe 230 by the cooling element 250. The outer pipe 220 and the connecting pipe 230 may enclose a volume containing the working fluid 270. The dimensions of the lower section of the connecting pipe 230 may be selected so that the vapor velocity in the connecting pipe 230 is significantly lower than the speed of sound in the vapor of the working fluid (e.g., less than Mach 0.2) at maximum heat flow during operation. A vapor velocity limit lower than the speed of sound may ensure minimal entrainment of condensate flowing downward under gravity.

[0028] In some embodiments, the inner condenser tube 210, the outer tube 220, and the connecting tube 230 may be formed using a metallic material. For example, the inner condenser tube 210, the outer tube 220, and the connecting tube 230 may each comprise copper tubing. A metal such as copper may be selected to provide high thermal conductivity. In other embodiments, a different type of material may be used for the inner condenser tube 210, the outer tube 220, and the connecting tube 230, such as glass tubing.

[0029] The heating element 240 may be coupled to the outer tube 220 at a location that promotes boiling of the working fluid 270. For example, the heating element 240 may be coupled to and / or attached to the outer tube 220 at or within a specific distance of the lowest point of the outer tube 220 when the TPCT condenser 120 is attached to the distillation vessel 110 (e.g., within a distance corresponding to plus or minus X% of the length of the outer tube 220 from the lowest point). The heating element 240 may provide heat input 242 to the working fluid 270 during operation of the TPCT condenser 120. The heating element 240 may include, for example, a resistive heating element (or another type of electronically controllable heating element, such as, for example, a dielectric heating element, an induction heating element, etc.) for applying a controllable heat source to the working fluid 270. The heat input 242 from the heating element 240 may be controlled by the condenser controller 182 and / or the controller unit 180. The heat transfer surface from the heating element 240 to the outer wall of the outer tube 220 may be minimized for maximum heat flux density to ensure monotonic boiling of the working fluid 270 at minimum heating power without the occurrence of boiling crisis and / or liquid superheating phenomena.

[0030] The heating element 240 may be disposed adjacent to a porous ceramic layer 244. The porous ceramic layer 244 may be applied to the inner surface of the outer tube 220 at the location where the heating element 240 is to be coupled to the outer tube 220. The porous ceramic layer 244 may function as an additional boiling stabilizer, providing nucleation points for boiling and preventing overheating and / or boiling crises. The porous ceramic layer 244 may include a ceramic foam. For example, the porous ceramic layer 244 may include silicon dioxide obtained by foaming sodium silicate deposited on a metal surface. In other embodiments, additional or alternative boiling stabilizers may be used, such as glass beads on the interior of the outer tube 220, a ceramic coating on the interior of the outer tube 220 (e.g., a potassium silicate coating), threads or other types of protrusions on the interior surface of the outer tube 220, and / or other types of boiling stabilizer structures.

[0031] The cooling element 250 may be coupled to the connecting tube 230 at a location that facilitates condensation of the vapor of the working fluid 270. For example, the cooling element 250 may be coupled to and / or attached to the connecting tube 230 at or within a specific distance of the highest point of the connecting tube 230 when the TPCT condenser 120 is attached to the distillation vessel 110 (e.g., a distance corresponding to plus or minus X% of the length of the connecting tube 230 from the highest point, within at least X% of the height of the connecting tube 230 from the attachment point of the connecting tube 230 to the outer tube 220, etc.). The cooling element 250 may provide heat rejection 252 from the working fluid 270 during operation of the TPCT condenser 120. The cooling element 250 may include, for example, a thermoelectric Peltier effect device (or another type of electronically controllable cooling device, such as, for example, a vapor compression refrigeration device, an adsorption refrigeration device, an absorption refrigeration device, etc.) for applying a controllable cooling source to the working fluid 270. The heat rejection 252 from the cooling element 250 may be controlled by the condenser controller 182 and / or the controller unit 180 .

[0032] Temperature sensors 262, 264, and 266 may monitor the temperature of the working fluid 270 during operation of the TPCT condenser 120. Temperature sensors 262, 264, and 266 may each include a thermocouple, a resistance temperature sensor, a thermistor temperature sensor, a semiconductor temperature sensor, and / or another type of temperature sensor. Temperature sensor 262 may be attached to the outer surface of the outer pipe 220 at a location closer to the outlet of the outer pipe 220 than to the inlet of the outer pipe 220 (e.g., on the lower half of the outer pipe when the TPCT condenser 120 is attached to the condensing vessel 110, within a specific distance of the outlet of the outer pipe 220, etc.). Temperature sensor 264 may be attached to the outer surface of the outer pipe 220 at a location closer to the inlet of the outer pipe 220 than to the outlet of the outer pipe 220 (e.g., on the upper half of the outer pipe when the TPCT condenser 120 is attached to the condensing vessel 110, within a specific distance of the inlet of the outer pipe 220, etc.). The temperature sensor 266 may be attached to an outer surface of the connecting tube 230. The condenser controller 182 and / or the controller unit 180 may monitor the temperature of the working fluid 270 during operation of the TPCT condenser 120 using the temperature sensors 262, 264, and / or 266 and may adjust the setting of the heating element 240 and / or the setting of the cooling element during operation of the TPCT condenser 120 based on temperature readings obtained from the temperature sensors 262, 264, and / or 266.

[0033] The working fluid 270 may include a fluid surrounded by the wall of the outer tube 220 and the wall of the inner condenser tube 210. The volume of the working fluid 270 may be selected so that the entire outer surface of the inner condenser tube 210 is always and / or normally wetted by the working fluid 270. The working fluid 270 may include a low-toxicity and low-flammability substance having a melting point significantly higher than the minimum operating temperature of the TPCT condenser 120 (e.g., higher than the lowest required operating temperature of the TPCT condenser 120 based on the distillation standard of the substance to be distilled), a sufficient vapor pressure within the operating range of the TPCT condenser 120, and a critical temperature significantly below the maximum operating temperature of the TPCT condenser 120. In some embodiments, the working fluid 270 may include an individual substance, such as, for example, methanol, ethanol, acetone, pentane, and / or another substance. In other embodiments, the working fluid 270 may preferably include an azeotrope of multiple substances, such as, for example, an azeotrope of methanol and pentane. Azeotropes can maintain the same concentration ratio in the liquid and vapor phases. An azeotrope of methanol and pentane can enable an operating range of 0 to 70°C for the TPCT condenser 120. In other embodiments, working fluid 270 can include different fluids, such as, for example, methanol, ethanol, pentane, and / or acetone. In yet other embodiments, working fluid 270 can include a hydrofluoroolefin, such as, for example, cis-1,1,1,4,4,4-hexafluoro-2-butene.

[0034] The working fluid 270 may fill the outer tube 220 up to the point where the connecting tube 230 connects to the outer tube 220. During operation, heat inflow 242 from the heating element 240 may cause the working fluid 270 to boil and evaporate into the connecting tube 230. Thus, the outer tube 220 may form an evaporation zone 278. Vapor 274 of the working fluid 270 may rise in the connecting tube 230 and condense into condensate droplets 276 when it encounters the heat exhaust 252 caused by the cooling element 250. Thus, the connecting tube 230 may form a condensation zone 280. The condensate droplets 276 may fall back into the boiling region of the working fluid 270, causing circulation of the working fluid 270, which transfers heat from the inner condenser tube 210 to the cooling element 250 while maintaining the inner condenser tube 210 at a constant temperature. Constant boiling of the working fluid 270 under isochoric conditions in all operating modes of the TPCT condenser 120 (e.g., while maintaining a setpoint temperature, while changing from one setpoint temperature to another, etc.) can ensure a constant temperature throughout the volume of the working fluid 270 and rapid and efficient heat removal by the TPCT condenser 120.

[0035] Figure 3 shows an exemplary assembly 300 including the TPCT condenser 120. As shown in Figure 3, the TPCT condenser 120 may include an inner condenser tube 210, an outer tube 220, and a connecting tube 230 formed from copper tubing that is curved from the distillation vessel 110 to a location in the enclosure 132 (not shown in Figure 3) for connection to the receiving vessel 122. Temperature sensors 262 and 264 may each include a thermocouple in a jacket soldered to the outer tube 220. Temperature sensor 266 may include a thermocouple in a jacket soldered to the connecting tube 230.

[0036] The connecting pipe 230 may include a condensing block 310 and a fill valve 320. The condensing block 310 may include a hollow rectangular prism made from copper plate containing channels through which the vapor 274 travels inside the condensing block 310. The condensing block 310 may include multiple cavities connected to the outer pipe 220 via the connecting pipe 230, in which condensation of the working fluid 270 occurs. The cooling element 250 may be attached to the condensing block 310, which may increase the surface area for condensation and the time the vapor 274 spends in contact with the wall cooled by the cooling element 250. The fill valve 320 may be used to fill the TPCT condenser 120 with the working fluid 270. Although not shown in FIG. 3 for illustrative purposes, the outer pipe 220 of the TPCT condenser 120 may be wrapped in insulation (e.g., foam insulation, fiberglass insulation, etc.) during operation to improve the thermal stability of the working fluid 270.

[0037] 2 and 3 illustrate example components of the TPCT condenser 120, in other implementations, the TPCT condenser 120 may include fewer, different, additional, or differently arranged components than those shown in Figure 2 or 3. Additionally or alternatively, one or more components of the TPCT condenser 120 may perform one or more tasks described as being performed by one or more other components of the TPCT condenser 120.

[0038] 4 is a diagram illustrating example components of controller unit 180 and / or condenser controller 182 according to implementations described herein. As shown in FIG. 4, controller unit 180 and / or condenser controller 182 may each include a bus 410, a processor 420, a memory 430, an input device 440, an output device 450, and a communication interface 460.

[0039] Bus 410 may include paths that allow communication between components of controller unit 180 and / or condenser controller 182. Processor 420 may include any type of single-core processor, multi-core processor, microprocessor, latch-based processor, central processing unit (CPU), and / or processing logic (or family of processors, microprocessors, and / or processing logic) that interprets and executes instructions. In other embodiments, processor 420 may include an application-specific integrated circuit (ASIC), a field-programmable gate array (FPGA), and / or another type of integrated circuit or processing logic.

[0040] Memory 430 may include any type of dynamic storage device capable of storing information and / or instructions for execution by processor 420, and / or any type of non-volatile storage device capable of storing information for use by processor 420. For example, memory 430 may include random access memory (RAM) or another type of dynamic storage device, read-only memory (ROM) device or another type of static storage device, content addressable memory (CAM), magnetic and / or optical recording memory devices and their corresponding drives (e.g., hard disk drives, optical drives, etc.), and / or removable forms of memory such as flash memory.

[0041] Input device(s) 440 may allow an operator to input information into controller unit 180 and / or condenser controller 182. Input device(s) 440 may include, for example, a keyboard, a mouse, a pen, a microphone, a remote control, an audio capture device, an image and / or video capture device, a touchscreen display, and / or another type of input device. In some embodiments, controller unit 180 and / or condenser controller 182 may be remotely managed and may not include input device(s) 440. In other words, controller unit 180 and / or condenser controller 182 may be “headless,” for example, and may not include a keyboard.

[0042] Output device(s) 450 may output information to an operator of controller unit 180 and / or condenser controller 182. Output device(s) 450 may include a display, a printer, a speaker, and / or another type of output device. For example, controller unit 180 and / or condenser controller 182 may include a display, which may include a liquid crystal display (LCD), a light emitting diode (LED) display, etc., for displaying content to an operator. In some embodiments, controller unit 180 and / or condenser controller 182 may be remotely managed and may not include output device(s) 450. In other words, controller unit 180 and / or condenser controller 182 may be “headless,” e.g., may not include a display.

[0043] The communication interface 460 may include a transceiver that enables the controller unit 180 and / or the condenser controller 182 to communicate with other devices and / or systems via wireless communication (e.g., radio frequency, infrared, and / or visual optics, etc.), wired communication (e.g., conductor wire, twisted pair cable, coaxial cable, transmission line, fiber optic cable, and / or waveguide, etc.), or a combination of wireless and wired communication. The communication interface 460 may include a transmitter that converts baseband signals to radio frequency (RF) signals and / or a receiver that converts RF signals to baseband signals. The communication interface 460 may be coupled to an antenna for transmitting and receiving RF signals.

[0044] Communications interface 460 may include logical components including input and / or output ports, input and / or output systems, and / or other input and output components that facilitate the transmission of data to other devices. For example, communications interface 460 may include a network interface card (e.g., an Ethernet card) for wired communications and / or a wireless network interface (e.g., WIFI) card for wireless communications. Communications interface 460 may also include a universal serial bus (USB) port for communications over a cable, 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.

[0045] As described in more detail below, the controller unit 180 and / or the condenser controller 182 may perform certain operations related to running the distillation process and controlling the TPCT condenser 120 during distillation. The controller unit 180 and / or the condenser controller 182 may perform these operations in response to the processor 420 executing software instructions contained in a computer-readable medium, such as the memory 430. A computer-readable medium may be defined as a non-transitory memory device. The memory device may be implemented within a single physical memory device or distributed across multiple physical memory devices. The software instructions may be loaded into the memory 430 from another computer-readable medium or another device. The software instructions contained in the memory 430 may cause the processor 420 to perform the processes described herein. Alternatively, hardware circuitry may be used in place of or in combination with software instructions to implement the processes described herein. Therefore, the implementations described herein are not limited to any specific combination of hardware circuitry and software.

[0046] 4 illustrates exemplary components of controller unit 180 and / or condenser controller 182, in other implementations, controller unit 180 and / or condenser controller 182 may include fewer, different, additional, or differently arranged components than those shown in FIG. 4. Additionally or alternatively, one or more components of controller unit 180 and / or condenser controller 182 may perform one or more tasks described as being performed by one or more other components of controller unit 180 and / or condenser controller 182.

[0047] 5 illustrates exemplary functional components of controller unit 180 and / or condenser controller 182. The functional components of controller unit 180 and / or condenser controller 182 may be implemented, for example, via processor 420 executing instructions from memory 430. For example, the components of controller unit 180 and / or condenser controller 182 may correspond to the structure of processor 420, along with the instructions in memory 430 for implementing the functionality of that component. Alternatively or additionally, some or all of the components of controller unit 180 and / or condenser controller 182 may be implemented via hardwired circuitry. For example, the components of controller unit 180 and / or condenser controller 182 may correspond to the structure of some or all of an ASIC, FPGA, and / or another type of integrated circuit.

[0048] As shown in FIG. 5 , the controller unit 180 and / or the condenser controller 182 may include a distillation manager 510, a heating element controller 520, a data collector 530, a distillation curve generator 540, a distillation curve database (DB) 550, a user interface 560, a TPCT condenser controller 570, a TPCT condenser setting DB 572, a heating element controller 574, and a cooling element controller 576.

[0049] Distillation manager 510 may manage the distillation process of distillation system 100. For example, distillation manager 510 may initiate distillation based on a request from a user received via user interface 560 using heating element controller 520. Heating element controller 520 may control heating elements 130. Distillation manager 510 may acquire distillation data using data collector 530, generate a distillation curve using distillation curve generator 540, store the distillation curve data in distillation curve DB 550, and provide information related to the generated distillation curve to a user via user interface 560. Data collector 530 may manage the collection of data during distillation. Distillation curve generator 540 may generate a distillation curve based on the data acquired from data collector 530 and stored in distillation curve DB 550.

[0050] User interface 560 may include a user interface that allows a user to control distillation system 100 and / or receive information generated by controller unit 180, such as generated distillation curves, messages regarding completed or ongoing distillation processes, and / or other types of messages. Additionally, user interface 560 may include a user interface that allows a user to control TPCT condenser 120. For example, user interface 560 may allow a user to configure TPCT condenser 120 for a particular type of sample. User interface 560 may be configured to interact with input device(s) 440 and / or output device(s) 450.

[0051] The TPCT condenser controller 570 may control the TPCT condenser 120. For example, the TPCT condenser controller 570 may select heating element settings and / or cooling element settings for the TPCT condenser 120 for the sample being distilled. The TPCT condenser controller 570 may select a setting set for the sample based on information stored in the TPCT condenser setting DB 572. Exemplary information that may be stored in the TPCT condenser setting DB 572 is described below with reference to FIG. 6. The heating element controller 574 may control the heating element 240. The cooling element controller 576 may control the cooling element 250.

[0052] 5 illustrates exemplary components of controller unit 180 and / or condenser controller 182, in other implementations, controller unit 180 and / or condenser controller 182 may include fewer, different, additional, or differently arranged components than those illustrated in FIG. 5. Additionally or alternatively, one or more components of controller unit 180 and / or condenser controller 182 may perform one or more tasks described as being performed by one or more other components of controller unit 180 and / or condenser controller 182.

[0053] 6 illustrates exemplary components of the TPCT condenser setting DB 572. As shown in FIG. 6, the TPCT condenser setting DB 572 may include one or more TPCT condenser setting records 600. Each TPCT condenser setting record 600 may store information related to a particular setting for the TPCT condenser 120. The TPCT condenser setting record 600 may include a sample material field 610, a target condenser temperature field 620, a heating element setting 630, and a cooling element setting 640.

[0054] The sample material field 610 may store information identifying a particular sample material. The target condenser temperature field 620 may store information identifying a target temperature for the TPCT condenser 120 for a particular sample material. The heating element settings 630 may store information identifying a heating element setting for the heating element 240 to maintain the TPCT condenser 120 at the target temperature. The cooling element settings 640 may store information identifying a cooling element setting for the cooling element 250 to maintain the TPCT condenser 120 at the target temperature. The heating element settings and cooling element settings may include, for example, a percentage of maximum power applied to the heating element 240 and / or a percentage of maximum power applied to the cooling element 250.

[0055] Although FIG. 6 illustrates exemplary components of a TPCT condenser settings DB 572, in other implementations, the TPCT condenser settings DB 572 may include fewer components, different components, additional components, or components in a different arrangement than those illustrated in FIG. 6.

[0056] Figure 7 is a flow chart of a process 700 for performing distillation using a TPCT condenser according to embodiments described herein. In some embodiments, the process of Figure 7 may be performed by and / or using distillation system 100. In other embodiments, some or all of the process of Figure 7 may be performed by or using another device or group of devices separate from distillation system 100.

[0057] 7, process 700 may include selecting a sample to distill (block 710) and determining condenser requirements associated with the selected sample (block 720). For example, a user may select a sample material to distill and may select the sample material using user interface 560. In response, distillation system 100 may determine a target temperature for TPCT condenser 120 and select heating element settings for heating element 240 and cooling element settings for cooling element 250 for the target temperature based on information stored in TPCT condenser settings DB 572.

[0058] Process 700 may further include obtaining a temperature value from a condenser temperature sensor (block 730), selecting a heating element setting and a cooling element setting for the TPCT condenser based on the determined condenser requirements (block 740), applying the selected heating element setting to the heating element of the TPCT condenser (block 750), and applying the selected cooling element setting to the cooling element of the TPCT condenser (block 760). For example, condenser controller 182 and / or controller unit 180 may obtain temperature readings from temperature sensor 262, temperature sensor 264, and / or temperature sensor 266, compare the obtained temperature readings to a target temperature, and adjust the heating element setting and the cooling element setting to reach the target temperature of working fluid 270. Condenser controller 182 and / or controller unit 180 may then apply the selected heating element setting to heating element 240 and the selected cooling element setting to cooling element 250. The heating element setting may correspond to the amount of power applied to the heating element 240 as a percentage of the maximum power that can be applied to the heating element 240. The cooling element setting may correspond to the amount of power applied to the cooling element 250 as a percentage of the maximum power that can be applied to the cooling element 250. In other embodiments, the heater element setting and / or cooling element setting may correspond to a temperature setting, a duration setting, and / or other type of setting for controlling the heating element 240 and / or the cooling element 250.

[0059] Process 700 may further include continuing distillation of the sample using the TPCT condenser for a selected duration (block 770). For example, controller unit 180 may control heating element 130 to initiate distillation of sample 112 while TPCT condenser 120 is maintained at the target temperature, or may continue distillation of sample 112 if distillation has already begun in distillation vessel 110. Controller unit 180 may collect distillation data during distillation using vapor temperature sensor 150 and / or liquid temperature sensor 152 and store the collected distillation data in distillation curve DB 550.

[0060] The selected duration may correspond to the duration before the heating element settings and cooling element settings are recalculated based on temperature readings from temperature sensor 262, temperature sensor 264, and / or temperature sensor 266. For example, the heating element settings and cooling element settings may be recalculated every 0.5 seconds, every second, or using another selected duration from the start of distillation until the specified end of distillation, because the amount of heat energy removed from inner condenser tube 210 may vary significantly over time during distillation. Thus, after the selected duration has passed, a determination may be made as to whether the distillation is complete (block 780). The distillation may be determined to be complete after a predetermined period of time has elapsed, when all of the sample 112 has evaporated, when the distillate level sensor 124 detects that the distillate in receiving vessel 122 has reached a predetermined volume, and / or based on another criterion. If it is determined that the distillation is not complete (block 780, No), processing may return to block 730 and obtain a new temperature value from the condenser temperature sensor. If it is determined that the distillation is complete (block 780, yes), the distillation of the sample using the TPCT condenser may be completed (block 790).

[0061] FIG. 8 shows a first exemplary plot 800 of temperature data for the TPCT condenser 120. As shown in FIG. 8, the plot 800 illustrates the temperature of the TPCT condenser 120 in response to specific heating and cooling element settings and switching between different temperature set points. The horizontal axis represents time in seconds, and the vertical axis represents the measured temperature on the left side of the plot 800 and the percentage of heating power applied to the heating element 240 and the percentage of cooling power applied to the cooling element 250 on the right side of the plot 800. The plotted lines correspond to the measured temperature by temperature sensor 262 (T1), the measured temperature by temperature sensor 264 (T2), the measured temperature by temperature sensor 266 (T3), the percentage of heating power applied to the heating element 240, and the percentage of cooling power applied to the cooling element 250. The plot 800 illustrates five different operating settings.

[0062] In setting 1, from 0 to 840 seconds, the target set point for the TPCT condenser 120 is 20°C, which is achieved by a 50% heating rate for the heating element 240 and a 50% cooling rate for the cooling element 250. As shown in Figure 8, all three temperature sensors T1, T2, and T3 measure a temperature of 20°C.

[0063] The next target set point for the TPCT condenser 120 is 60°C. When the temperature of the TPCT condenser 120 needs to be increased quickly, the heating element setting can be set to 100% power and the cooling element setting can be set to 0% power (i.e., turned off) to reduce the condensation of the vapor 274 to a minimum, thereby reducing the energy flow to a minimum, resulting in faster heating of the evaporation zone 278. Alternatively, the cooling element 250 can be switched to reverse mode to also heat the condensation zone 280. The Peltier element can be operated in reverse mode to heat the surface rather than cooling it. Heating the connecting tube 230 and the condensation zone 280 can shorten the switchover time from the previous temperature to a new temperature (e.g., from 20°C to 60°C) by stopping the condensation process of the vapor 274, allowing the energy of the heat input 242 to be spent only on rapidly heating the working fluid 270. Thus, in setting 2, from 840 seconds to about 1100 seconds, a 100% power setting is applied to the heating element 240 and a -50% power setting is applied to the cooling element 250 (ie, the cooling element 250 is operated in reverse mode).

[0064] In setting 3, at 1200 seconds, the target set point for the TPCT condenser 120 is changed to 60°C, which can be achieved with a 50% heating rate for the heating element 240 and a -10% cooling rate for the cooling element 250. The TPCT condenser 120 quickly stabilizes at a temperature of 60°C, as measured by all three temperature sensors T1, T2, and T3. The target set point of 60°C is maintained from 1200 seconds to 1700 seconds.

[0065] The next target set point for the TPCT condenser 120 is 0°C. If the temperature of the TPCT condenser 120 is to be reduced, the heating of the working fluid 270 can be increased while maximizing the power to the cooling element 250. Increasing the heat can increase the circulatory movement of the vapor 274 to the cooling element 250. Thus, at setting 4, from 1700 seconds to about 2000 seconds, a 100% power setting is applied to the heating element 240 and 100% power is applied to the cooling element 250 to increase the cooling of the working fluid 270.

[0066] At setting 5, at approximately 2100 seconds, the target set point for the TPCT condenser 120 is changed to 0°C, which is achieved with a 50% heating rate for the heating element 240 and an 80% cooling rate for the cooling element 250. The TPCT condenser 120 quickly stabilizes at a temperature of 0°C, as measured by all three temperature sensors T1, T2, and T3. The 0°C target set point is maintained from 2000 seconds to 2400 seconds.

[0067] FIG. 9 shows a second example plot 900 of temperature data for the TPCT condenser 120 generated using the same sample data used in generating plot 800. As shown in FIG. 9, plot 900 shows the temperature of the TPCT condenser 120 in response to the heating and cooling element settings shown in FIG. 8. The horizontal axis shows time in seconds, and the vertical axis shows the measured temperature on the left side of plot 900 and the temperature difference between the temperature sensors on the right side of plot 900. The plotted lines correspond to the temperature measured by temperature sensor 262 (T1), the measured temperature of temperature sensor 264 (T2), the measured temperature of temperature sensor 266 (T3), the temperature difference between T1 and T2, and the temperature difference between T1 and T3.

[0068] The difference between T1 and T2 indicates the stability of the thermostatic mode that maintains the TPCT condenser 120 at the setpoint temperature. As shown in Figure 9, the value of T1-T2 tends toward zero, indicating a constant temperature state where the temperature gradient between different points in the working fluid 270 is minimal. The difference between T1 and T3 indicates the efficiency of heat transfer between the evaporation zone 278 and the condensation zone 280. As shown in Figure 9, the value of T1-T3 does not exceed 0.5°C while at the setpoint temperature or when transitioning to a new setpoint temperature. The minimal temperature gradient and its monotonic dependence on the heat transferred from the evaporation zone 278 to the condensation zone 280 indicate that undesirable flooding is not occurring. Continuous monitoring of the temperature of the TPCT condenser 120 at different points via temperature sensors 262, 264, and 266 allows for monitoring the performance of the TPCT condenser 120 during operation.

[0069] In the foregoing specification, various preferred embodiments have been described with reference to the accompanying drawings. However, it will be apparent that various modifications and changes can be made and additional embodiments can be implemented without departing from the broader scope of the invention as set forth in the following claims. Accordingly, the specification and drawings should be regarded in an illustrative rather than a restrictive sense.

[0070] For example, although embodiments are described herein for a TPCT condenser that is maintained at a set temperature during distillation, in other embodiments, the TPCT condenser may be used in other applications requiring a constant temperature and the ability to rapidly change from a first set temperature to a second temperature. As an example, a TPCT condenser may be used as a thermostatic bath for a chemical reaction vessel that needs to maintain a solution at a specific temperature for a chemical reaction and / or needs to rapidly change between different temperature set points.

[0071] Additionally, although a series of blocks are described with respect to Figure 7, the order of the blocks may be changed in other implementations. Additionally, non-dependent blocks and / or signals may be executed in parallel.

[0072] It will be apparent that the systems and / or methods as described above may be implemented in many different forms of software, firmware, and hardware in the embodiments illustrated in the figures. The actual software code or specialized control hardware used to implement these systems and methods is not limiting of the embodiments. Thus, the operation and behavior of the systems and methods are described without reference to specific software code, and it will be understood that software and control hardware can be designed to implement the systems and methods based on the description herein.

[0073] Furthermore, certain portions described above may be implemented as components that perform one or more functions. A component as used herein may include hardware, such as a processor, ASIC, or FPGA, or a combination of hardware and software (e.g., a processor running software).

[0074] It should be emphasized that as used in this specification, the term "comprises" / "comprising" is to be interpreted as specifying the presence of stated features, integers, steps or components, but does not exclude the presence or addition of one or more other features, integers, steps, components or groups thereof.

[0075] As used herein, the term "logic" may refer to a combination of one or more processors configured to execute instructions stored in one or more memory devices, may refer to hardwired circuitry, and / or may refer to a combination thereof. Furthermore, logic may be contained in a single device or distributed across multiple, possibly remote, devices.

[0076] It is further noted that for purposes of describing and defining the present invention, the term "substantially" is utilized herein to represent the inherent degree of uncertainty that may result from any quantitative comparison, value, measurement, or other representation. The term "substantially" is also utilized herein to represent the extent to which a quantitative representation may vary from the stated standard without resulting in a change in the basic functionality of the subject matter at issue.

[0077] No element, act, or instruction used in the present application should be construed as critical or essential to an embodiment unless explicitly described as such. Also, as used herein, the article "a" is intended to include one or more items. Furthermore, the phrase "based on" is intended to mean "based at least in part on," unless otherwise specified.

Claims

1. 1. A distillation condenser comprising: an inner condenser tube including an inlet for receiving vapor from the distillation vessel and an outlet connecting to a receiving vessel for receiving distilled liquid condensed from said vapor; an outer tube surrounding the inner condenser tube; a heating element coupled to the exterior of the outer tube; a controller configured to control the heating element to heat a working fluid in the outer tube and, as a result of the heated working fluid, cause the distillation condenser to function as a two-phase closed-circuit thermosiphon (TPCT); A distillation condenser comprising:

2. a connecting pipe coupled to the outer pipe and oriented perpendicular to the outer pipe, the working fluid vapor rising through the connecting pipe; 10. The distillation condenser of claim 1 further comprising:

3. a condensing block coupled to the connecting tube configured to increase a surface area of ​​the connecting tube, wherein vapor of the working fluid condenses in the condensing block; 3. The distillation condenser of claim 2, further comprising:

4. a cooling element coupled to the condensing block, the controller further configured to control the cooling element to condense the working fluid vapor in the condensing block.

4. The distillation condenser of claim 3 further comprising:

5. a first temperature sensor coupled to the outer tube and positioned closer to the outlet than to the inlet; a second temperature sensor coupled to the outer tube and positioned closer to the inlet than to the outlet; a third temperature sensor coupled to the condensing block; 5. The distillation condenser of claim 4, further comprising:

6. 10. The distillation condenser of claim 1, wherein the inner condenser tube and the outer tube each comprise copper tubing.

7. a porous ceramic layer disposed on the interior surface of the outer tube at a location adjacent the heating element; 10. The distillation condenser of claim 1 further comprising:

8. 10. The distillation condenser of claim 1 further comprising the working fluid, wherein the working fluid comprises an azeotropic mixture of methanol and pentane.

9. 10. The distillation condenser of claim 1, further comprising the working fluid, wherein the working fluid comprises at least one of methanol, ethanol, pentane, acetone, or a hydrofluoroolefin.

10. Cooling element and wherein the controller: Determining the condenser temperature required for the sample; selecting a heating element setting for the heating element based on the determined required condenser temperature; selecting a cooling element setting for the cooling element based on the determined required condenser temperature; applying the selected heating element setting and the selected cooling element setting to the distillation condenser to maintain the required condenser temperature during distillation of the sample; 10. The distillation condenser of claim 1 configured to:

11. Distillation vessel, a plurality of sensors coupled to the distillation vessel; and a condenser coupled to the distillation vessel and configured to function as a two-phase closed thermosyphon (TPCT); a distillation apparatus comprising: generating a distillation curve for the sample based on a plurality of values ​​obtained from the plurality of sensors during distillation of the sample; and controlling operation of the TPCT to maintain the condenser at a specified temperature during the distillation of the sample. a controller configured to A distillation system comprising:

12. 12. The distillation system of claim 11, wherein circulation through the TPCT is gravity assisted.

13. 12. The distillation system of claim 11, wherein the condenser includes an inner condenser tube and the TPCT surrounds the inner condenser tube in a constant temperature liquid bath.

14. The condenser is an inner condenser tube including an inlet for receiving vapor from the distillation vessel and an outlet for connecting to a receiving vessel for receiving distilled liquid condensed from the vapor; an outer tube surrounding the inner condenser tube; a heating element coupled to the exterior of the outer tube; Including, 12. The distillation system of claim 11, wherein the controller is configured to control the heating element to heat a working fluid in the outer tube and cause the condenser to function as the TPCT as a result of the heated working fluid.

15. The condenser is a connecting pipe coupled to the outer pipe and oriented perpendicular to the outer pipe, wherein vapor of the working fluid rises in the connecting pipe; a condensing block coupled to the connecting tube and configured to increase a surface area of ​​the connecting tube, wherein vapor of the working fluid condenses in the condensing block; a cooling element coupled to the condensing block, the controller being further configured to control the cooling element to condense the working fluid vapor in the condensing block; and The distillation system of claim 14 further comprising:

16. The controller: determining the specific temperature for the condenser; selecting a heating element setting for the heating element based on the determined particular temperature; selecting a cooling element setting for the cooling element based on the determined particular temperature; applying the selected heating element setting and the selected cooling element setting to the condenser to maintain the condenser at the specified temperature during the distillation of the sample; 16. The distillation system of claim 15, further configured to:

17. 15. The distillation system of claim 14, wherein the condenser further comprises a porous ceramic layer disposed on an interior surface of the outer tube at a location adjacent the heating element.

18. 12. The distillation system of claim 11, wherein the condenser comprises a working fluid comprising an azeotropic mixture of methanol and pentane.

19. 12. The distillation system of claim 11, wherein the condenser comprises a working fluid comprising at least one of methanol, ethanol, pentane, acetone, or a hydrofluoroolefin.

20. Determining the condenser temperature required for the sample; selecting a heating element setting for a condenser heating element based on the determined required condenser temperature; selecting a cooling element setting for the condenser cooling element based on the determined required condenser temperature; applying the heating element setting to the heating element and the cooling element setting to the cooling element during distillation of the sample, wherein the condenser functions as a two-phase closed thermosiphon (TPCT) that maintains the condenser at the required condenser temperature during the distillation of the sample; A method comprising:

Images