Window kettle rotating device and fluid stirring and mixing method

Abstract

The invention provides a window kettle rotating device and a fluid stirring and mixing method, and belongs to the field of scientific experimental instruments. The window kettle rotating device comprises a window kettle, a constant-temperature box and a rotating bracket arranged in the constant-temperature box, the window kettle can be mounted on the rotary bracket; a power mechanism is arranged outside the constant-temperature box; the power mechanism is connected with the rotating support. According to the invention, the window kettle can be rotated at a set temperature to fully stir and mix fluid in the kettle. And the visual volume ratio of the window kettle is greater than or equal to 90%, and the inner diameter of the kettle is less than or equal to 2.0 cm, so that the measurement precision of the volume of fluid in the kettle is improved.

Description

Technical Field

[0001] The invention belongs to the field of scientific experimental instruments, and in particular relates to a window kettle rotating device and a fluid stirring and mixing method. Background Art

[0002] The window kettle is an important instrument in scientific research, which is used to study the properties of solutes and fluids under high temperature and pressure, such as the phase change of oil and water, the solubility of surfactants, and the expansion effect of CO2 on the volume of crude oil.

[0003] Conventional window kettles can only be used in a static state. If you need to stir and mix the fluid in the window kettle under high temperature and high pressure, you can only use magnetic stirring. However, the stirring efficiency of the magnetic stirring is low, and the fluid in the kettle cannot be quickly mixed. Especially when the volume of the fluid in the kettle far exceeds the volume of the magnetic stirring, the efficiency of the magnetic stirring is further reduced. At this time, the final equilibrium can only be achieved by molecular diffusion, which not only greatly prolongs the experimental time, but also easily causes experimental errors due to "false equilibrium". In addition, the diameter of the magnetic stirring is large, and the inner diameter of the window kettle needs to be increased to accommodate the magnetic stirring, which reduces the measurement accuracy of the window kettle. However, in experiments such as oil-water phase state and liquid expansion, it is necessary to accurately measure the volume change of the liquid, and the accuracy is required to reach 0.1ml or more. At present, it is difficult for a window kettle with stirring to meet this accuracy requirement.

[0004] Therefore, it is necessary to design a new type of window kettle rotating device, which can fully stir and mix the fluid in the kettle while having a small enough inner diameter to accurately measure the volume change of the liquid in the kettle. In addition, the window kettle is required to be temperature and pressure resistant, and the visible and measurable volume accounts for more than 90% of the total volume. Summary of the invention

[0005] The purpose of the present invention is to overcome the problems of low stirring and mixing efficiency, insufficient measurement accuracy, and too small visual volume of the existing window kettle, and to provide a window kettle rotating device. The device can rotate the window kettle at a set temperature to fully stir and mix the fluid in the window kettle. Moreover, the visual volume of the window kettle accounts for ≥90%, and the inner diameter of the kettle is ≤2.0cm, thereby improving the measurement accuracy of the fluid volume in the kettle.

[0006] The present invention is achieved through the following technical solutions:

[0007] A first aspect of the present invention provides a window kettle rotating device, the device comprising: a window kettle, a constant temperature box, and a rotating bracket arranged in the constant temperature box;

[0008] The window kettle can be installed on a rotating bracket;

[0009] A power mechanism is arranged outside the thermostatic box;

[0010] The power mechanism is connected with the rotating bracket.

[0011] Preferably, the window kettle comprises: a transparent tube, a base, and a frame;

[0012] The transparent tube is a transparent tubular structure with openings at both ends, and scales are marked on the outer wall of the transparent tube;

[0013] A groove is provided in the middle of each base, and the two ends of the transparent tube can be inserted into the grooves of the two bases respectively;

[0014] The frame comprises at least two pull rods, each pull rod is parallel to the transparent tube, and two ends of each pull rod are respectively installed on two bases.

[0015] Preferably, the window kettle comprises: a transparent tube, a base, a pressure sleeve, and a nut;

[0016] The transparent tube is a transparent tubular structure with openings at both ends, and scales are marked on the outer wall of the transparent tube;

[0017] A groove is provided in the middle of each base, and the two ends of the transparent tube can be inserted into the grooves of the two bases respectively;

[0018] The pressure sleeve is a cylindrical structure with openings at both ends, and is provided with at least two long holes parallel to its central axis;

[0019] The two bases are respectively fixed to the two ends of the pressure sleeve through nuts.

[0020] Preferably, the transparent tube is made of quartz or sapphire;

[0021] The inner diameter of the transparent tube is 0.2-2.0 cm.

[0022] Optionally, a threaded hole is opened in the middle of one base, the threaded hole is connected to the groove and is coaxial;

[0023] One end of the sealing head can be screwed into the threaded hole;

[0024] The sealing head is a solid plug or a plug with a central through hole.

[0025] Preferably, an air inlet and an air outlet are provided on the thermostat;

[0026] The air inlet is connected to a gas flow controller;

[0027] A plurality of lighting lamps are arranged in the constant temperature box;

[0028] An observation window is provided on the wall of the thermostatic box.

[0029] Optionally, the other end of the sealing head is connected to one end of the coil, and the other end of the coil is connected to the carbon dioxide constant pressure system after extending out of the thermostat from the air outlet.

[0030] Preferably, the rotating bracket comprises a supporting frame and a partition;

[0031] The support frame includes a long board and a short board, and the two long boards and the two short boards form a rectangular frame;

[0032] A plurality of U-shaped grooves with openings facing outward are formed on each long board, and the U-shaped grooves on the two long boards correspond to each other one by one;

[0033] A plurality of partitions parallel to the short boards are arranged between the two short boards, and the two ends of the partitions are respectively connected to the long boards on both sides; the connection between the partitions and the long boards is located between two adjacent U-shaped grooves;

[0034] A connecting hole is opened at the center of each short plate, a rotating shaft is connected to the connecting hole, and the rotating shaft can be connected to the power mechanism;

[0035] The rotating bracket also includes two limit baffles, which are arranged parallel to the long plate, and two ends of the limit baffles are fixed to the outer surface of the long plate by bolts.

[0036] Preferably, 1-5 rotating brackets are installed in the constant temperature box, and the multiple rotating brackets are arranged in sequence from top to bottom.

[0037] The second aspect of the present invention provides a fluid stirring and mixing method, which is implemented using the above-mentioned window kettle rotating device, and the method comprises:

[0038] Put the fluid to be tested into the sight glass kettle, and then fix the sight glass kettle on the rotating bracket;

[0039] The thermostat is started to heat or maintain a constant temperature, and the rotating bracket is driven to rotate by the power mechanism to stir and mix the fluid to be tested in the window kettle; at the same time, the inert gas enters the thermostat from the air inlet and is discharged from the exhaust port;

[0040] Stop the rotation, observe and measure the properties of the fluid to be tested in the window kettle.

[0041] Compared with the prior art, the invention has the following beneficial effects: the invention can rotate the window kettle at a set temperature to fully stir and mix the fluid in the kettle. Moreover, the visible volume of the window kettle accounts for ≥90%, and the inner diameter of the kettle is ≤2.0 cm, which improves the measurement accuracy of the fluid volume in the kettle. BRIEF DESCRIPTION OF THE DRAWINGS

[0042] Figure 1 A structural schematic diagram of a window kettle rotating device;

[0043] Figure 2-1 A schematic diagram of the cross-sectional structure of a window kettle;

[0044] Figure 2-2A schematic diagram of the three-dimensional structure of a window kettle;

[0045] Figure 3-1 A schematic diagram of the cross-sectional structure of another window kettle;

[0046] Figure 3-2 Another schematic diagram of the three-dimensional structure of a window kettle;

[0047] Figure 4 A schematic diagram of the structure of another window kettle rotating device;

[0048] Figure 5-1 A schematic diagram of the three-dimensional structure of the rotating bracket in the window kettle rotating device;

[0049] Figure 5-2 A schematic diagram of the main structure of the rotating bracket in the window kettle rotating device;

[0050] Figure 5-3 A schematic diagram of the side view structure of the rotating bracket in the window kettle rotating device;

[0051] Figure 6 Surfactant water solubility test results;

[0052] Figure 7 A schematic diagram of the structure of another window kettle rotating device;

[0053] Figure 8 The expansion coefficient of crude oil varies with pressure. DETAILED DESCRIPTION

[0054] The present invention is further described in detail below in conjunction with the accompanying drawings:

[0055] The endpoints and any values ​​of the ranges disclosed in this article are not limited to the precise ranges or values, and these ranges or values ​​should be understood to include values ​​close to these ranges or values. For numerical ranges, the endpoint values ​​of each range, the endpoint values ​​of each range and the individual point values, and the individual point values ​​can be combined with each other to obtain one or more new numerical ranges, which should be considered as specifically disclosed in this article.

[0056] like Figure 1 , Figure 4 As shown, the present invention provides a window kettle rotating device, comprising a window kettle 4, a thermostat 1, and a rotating bracket 5 arranged in the thermostat 1; the window kettle 4 can be installed on the rotating bracket 5; a power mechanism 3 is arranged outside the thermostat 1, and the power mechanism 3 is connected to the rotating bracket 5. An air inlet 6 and an air outlet 8 are arranged on the thermostat 1; the air inlet 6 is connected to a gas flow meter 7.

[0057] Furthermore, a plurality of lighting lamps 2 are arranged in the thermostat 1 .

[0058] Preferably, an observation window is provided on the wall of the thermostat 1, and in combination with the built-in lighting lamp 2, the changes of the fluid in the window kettle 4 in the thermostat 1 under high temperature can be observed from the outside of the thermostat 1, and photos can be taken as evidence. The window kettle 4 is marked with a scale, and the volume of the internal liquid can be accurately read. Therefore, the device of the present invention can stir the mixed fluid under high temperature and high pressure, and observe, measure and record the corresponding phenomena.

[0059] A window kettle 4 Figure 2-1 and Figure 2-2 As shown, it includes: a transparent tube 401, a base 403, and a frame. The two ends of the transparent tube 401 are respectively mounted on the two bases 403, and the bases 403 on both sides are connected by the frame. Specifically, the transparent tube 401 is a transparent tubular structure with both ends open, which is made of transparent material, and scales are marked on the outer wall of the transparent tube 401. A groove is opened in the middle of each base 403, and a base sealing ring 404 is arranged on the wall of the groove. The two ends of the transparent tube 401 can be respectively inserted into the grooves of the two bases 403, and the sealing of the two ends of the transparent tube 401 is achieved by the sealing ring. The frame includes at least two pull rods 402, each of which is parallel to the transparent tube 401, and the two ends of each pull rod 402 are respectively mounted on the two bases 403. Specifically, threads are provided at both ends of each tie rod 402, and a tie rod mounting hole is opened on the edge of each base 403. The two ends of each tie rod 402 pass through the tie rod mounting holes on the bases 403 on both sides and are connected with nuts. In this way, the two bases 403 are supported by multiple tie rods 402, and the transparent tube 401 is supported by the two bases 403 at the same time. On the one hand, the strength of the frame is guaranteed, and on the other hand, it does not affect the observation of the substances in the window kettle 4. Figure 2-2 The window kettle 4 shown in the figure uses four tie rods 402, which are evenly distributed on the circumference and surround the transparent tube 401. The size of the tie rods 402 and the grooves on the base 403 can ensure the visible volume ratio of the transparent tube 401. Preferably, in order to facilitate installation on the rotating bracket 5, a protrusion is provided on the outer end of the base 403, and a thread is provided on the outer wall of the protrusion.

[0060] During installation, first connect one end of each tie rod 402 to a base 403 through a nut, then insert one end of the transparent tube 401 into the base 403, then fill the fluid into the transparent tube 401, and then insert the other end of the transparent tube 401 into another base 403, and then pass the other end of each tie rod 402 through the base 403 and connect it with the nut, so that the transparent tube 401 is sealed and fixed to the frame by the base 403 and the O-ring.

[0061] Another structure of window kettle 4 is as follows Figure 3-1 and Figure 3-2As shown, the window kettle 4 includes a transparent tube 401, a base 403, a pressure sleeve 407, and a nut 408; the two ends of the transparent tube 401 are respectively mounted on two bases 403, and the two bases 403 are respectively fixed to the two ends of the pressure sleeve 407 through nuts 408. The pressure sleeve 407 plays a fixed supporting role, and the pressure sleeve 407 is more evenly stressed, which can effectively reduce the damage of the transparent tube 401 caused by uneven stress.

[0062] Specifically, the transparent tube 401 is a tubular structure with both ends open and made of transparent material, and scales are marked on the outer wall of the transparent tube 401. A groove is opened in the middle of each base 403, and a base sealing ring 404 is arranged on the wall of the groove. The two ends of the transparent tube 401 can be inserted into the grooves of the two bases 403 respectively, and the sealing of the two ends of the transparent tube 401 is achieved by the sealing ring. The pressure sleeve 407 is a tubular structure with both ends open, and at least two long holes parallel to its central axis are opened on it, which is convenient for observing the substances in the window kettle 4. The visual volume ratio of the transparent tube 401 can be ensured by the size of the long holes on the pressure sleeve 407 and the grooves on the base 403.

[0063] Annular steps are provided on the outer walls of the two bases 403, which are respectively mounted on the two ends of the pressure sleeve 407; threads are provided on the outer walls of the two ends of the pressure sleeve 407. Central through holes are provided on the two nuts 408, which are connected to the pressure sleeve 407 through threads, and the outer ends of the bases 403 pass through the central through holes of the nuts 408. Preferably, in order to facilitate installation on the rotating bracket 5, a protrusion is provided on the outer end of the base 403, and threads are provided on the outer wall of the protrusion.

[0064] During installation, first insert one end of the transparent tube 401 into a base 403, then fix the base 403 to one end of the pressure sleeve 407 by a nut 408, fill the fluid into the transparent tube 401, and then insert the other end of the transparent tube 401 into another base 403, and fix the base to the other end of the pressure sleeve 407 by a nut 408. In this way, the transparent tube 401 is sealed and fixed in the pressure sleeve 407 by the base 403 and the O-ring.

[0065] In the structures of the above two window kettles 4, optionally, a threaded hole is opened in the middle of a base 403, the threaded hole is connected to the groove and is coaxial, and one end of the sealing head 406 can be screwed into the threaded hole. In order to facilitate installation on the rotating bracket 5, a protrusion is provided at the outer end of the sealing head 406, and a thread is provided on the outer wall of the protrusion. The sealing head 406 and the base 403 are sealed by a sealing head sealing ring 405. The sealing head 406 can be a solid plug for sealing one end of the transparent tube 401; it can also be a plug with a central through hole, and the inner cavity of the transparent tube 401 can be connected to other components (such as a valve, a pressure gauge and a thermocouple) through the central through hole of the plug. In this way, the transparent tube 401 can be filled with liquid or poured out of the liquid without disassembling the base 403, and the sealing head 406 can be directly unscrewed, which is very convenient for loading and unloading the liquid.

[0066] The transparent tube 401 is made of quartz or sapphire, and is used to contain the test fluid, and has an operating temperature of 0-350° C., preferably 30-300° C. The inner diameter of the transparent tube 401 is 0.2-2.0 cm, preferably 0.3-1.0 cm.

[0067] The base 403, frame, pressure sleeve 407, and sealing head 406 can be made of stainless steel, Hastelloy, titanium alloy or copper, preferably stainless steel and Hastelloy, and are used to fix the transparent tube 401. The base 403 blocks less than 10% of the total volume of the transparent tube 401.

[0068] The sealing head sealing ring 405 and the base sealing ring 404 in the window kettle 4 are O-rings for sealing the transparent tube 401. The material of the O-ring can be fluororubber, perfluororubber, graphite, polytetrafluoroethylene, nitrile rubber or EPDM, preferably fluororubber, perfluororubber, graphite and polytetrafluoroethylene, more preferably fluororubber and perfluororubber.

[0069] Compared with the existing window kettle, the window kettle 4 of the present invention can withstand temperature (0-350°C) and pressure (0-30MPa) by selecting sealing rings, sealing heads 406 and bases 403 of suitable materials and sizes, and uses a rotary plug-in sealing head 406, so it is convenient to disassemble, install and load liquid. Moreover, the protrusions on the base 403 and the sealing head 406 can be stuck into the rotating bracket 5, and the protrusions have external threads, which can be fixed on the rotating bracket 5 using nuts, so that the window kettle 4 can be conveniently hung on the rotating bracket 5.

[0070] like Figure 5-1 to Figure 5-3 As shown, the rotating bracket 5 includes a support frame and a partition 503. The support frame includes two parallel long plates 501 and two parallel short plates 502. The two long plates 501 and the two short plates 502 form a rectangular frame. A plurality of partitions 503 parallel to the short plates 502 are arranged between the two short plates 502 (in Figure 1 , Figure 4 and Figure 7 The partition 503 is not shown in the figure, and the two ends of the partition 503 are respectively connected to the long boards 501 on both sides. The partition 503 prevents the support frame from being deformed, and also separates the window kettles, so as to prevent the window kettles from hitting the adjacent window kettles when being disassembled. A plurality of U-shaped grooves 504 with openings facing outward are formed on each long board 501, and the number of the U-shaped grooves 504 is 1-30, preferably 1-20, and the width of the U-shaped groove 504 matches the diameter of the protrusions on the base 403 of the window kettle 4 and the protrusions on the sealing head 406, and the protrusions can be embedded in the U-shaped grooves 504.

[0071] Preferably, the connection between the partition 503 and the long board 501 is located between two adjacent U-shaped grooves 504. The U-shaped grooves 504 on the two long boards 501 correspond to each other. After the protrusions at both ends of a window kettle 4 are respectively inserted into the corresponding U-shaped grooves 504 on the two long boards 501, the central axis of the window kettle 4 is parallel to the short board 502. In this way, after multiple window kettles 4 are installed on the rotating bracket 5, they are all parallel to the short board 502.

[0072] Furthermore, the rotating bracket 5 includes two limit baffles 505, which are arranged parallel to the long board 501, and the two ends of the limit baffles 505 are fixed to the outer surface of the long board 501 by bolts. When in use, the protrusions at the two ends of each window kettle 4 are firstly embedded into the corresponding U-shaped grooves 504 on the two long boards 501, and then the two limit baffles 505 are used to block the protrusions at the two ends of each window kettle 4, and then the limit baffles 505 are fixed to the long board 501 by bolts, and the window kettle 4 can also be better fixed by installing nuts on the protrusions. In this way, the two limit baffles 505 limit the protrusions at the two ends of the window kettle 4 in the U-shaped grooves 504.

[0073] A connecting hole is opened at the center of each short plate 502, and a rotating shaft is fixedly connected to the connecting hole to support the rotating bracket 5 and connect to the power mechanism 3, so that the power mechanism 3 can drive the rotating bracket 5 to rotate through the rotating shaft, and the rotating bracket 5 drives the window kettle 4 to rotate, thereby stirring and mixing the fluid in the window kettle 4.

[0074] The material of the rotating bracket 5 is aluminum alloy, stainless steel, Hastelloy, titanium alloy or copper, preferably aluminum alloy, stainless steel and copper. Each rotating bracket 5 can fix 1-30 window kettles 4, preferably 1-20 window kettles 4.

[0075] Bearing seats and bearings are provided on both side walls of the thermostatic box 1, and the central axes of the bearings on both sides are located on the same straight line. The rotating shafts at both ends of the rotating bracket 5 are respectively connected to the bearings on both sides, and one end of a rotating shaft passes through the side wall of the thermostatic box 1 and is connected to the power mechanism 3 located outside the thermostatic box 1. In this way, the rotating shaft can be driven to rotate by the power mechanism 3, and the rotating shaft drives the rotating bracket 5 to rotate, thereby rotating the window kettle 4, so as to achieve the purpose of stirring and mixing the fluid in the window kettle 4.

[0076] The number of bearing seats, bearings and power mechanisms 3 provided on the thermostatic box 1 is determined according to the number of rotating brackets 5 to be installed. Figure 1 In the embodiment shown, since two upper and lower rotating brackets 5 need to be installed, two groups of bearing seats, bearings, and power mechanisms 3 are installed on the wall of the thermostatic box 1. The central axes of the two bearings in each group are located on the same straight line, and the central axes of the bearings in the two groups are arranged in parallel. In this way, the upper and lower rotating brackets 5 can be installed in the thermostatic box 1, and the rotation is achieved through the respective power mechanisms 3.

[0077] The power mechanism 3 can be a manual rotating device or an automatic rotating device. The manual rotating device uses an existing rotating wheel, which drives the rotating bracket 5 and the window kettle 4 installed on the rotating bracket 5 to rotate. The automatic rotating device uses an existing motor, which drives the rotating bracket 5 and the window kettle 4 installed on the rotating bracket 5 to rotate. The speed of the automatic rotation is 0-100rpm, preferably 1-50rpm.

[0078] The thermostat 1 is used to heat the window kettle 4 and stably maintain the temperature at 0-350°C, preferably 30-300°C, and more preferably 40-250°C (a temperature display is provided on the thermostat 1). The fluid in the window kettle 4 can be observed, measured, and photographed through the observation window on the thermostat 1. 1-5 rotating brackets 5, preferably 1-3 rotating brackets 5, can be installed in each thermostat 1. The multiple rotating brackets 5 are arranged in sequence from top to bottom to facilitate observation of the window kettle 4 in the thermostat 1.

[0079] The air inlet 6 is arranged at the bottom and / or side of the thermostat 1, and the air outlet 8 is arranged at the top of the thermostat 1, for respectively introducing inert gas and exhausting waste gas to prevent the accumulation of combustible gas in the thermostat 1. The number of the air inlet 6 is 1-10, preferably 1-5. The number of the air outlet 8 is 1-5, preferably 1-3.

[0080] The illuminating lamp 2 is used to provide a light source in the thermostat 1, so as to facilitate observation, measurement and photography of the fluid in the window kettle 4. The number and position of the illuminating lamps 2 are distributed according to the size of the thermostat 1 to ensure that the light source is evenly distributed without dead angles. The working temperature of the illuminating lamp 2 is 0-350°C, preferably 30-300°C, and more preferably 40-250°C; the number of the illuminating lamps is 1-30, preferably 2-20. Each illuminating lamp 2 has an independent control switch.

[0081] The gas flow meter 7 is used to control the flow rate of the injected inert gas, and can continuously inject inert gases such as nitrogen, argon or carbon dioxide at a specified flow rate. The control flow rate is 0.1-50L / h, preferably 1-20L / h. The gas flow meter 7 is connected to the gas source outlet in the laboratory. The gas source can be from a steel cylinder or a public facility in an industrial park.

[0082] When in use, the fluid to be measured is loaded into the window kettle 4, and then the window kettle 4 is fixed on the rotating bracket 5. The thermostat 1 is started to heat or maintain a constant temperature, and the rotating bracket 5 is driven to rotate by the power mechanism 3, so that the window kettle 4 rotates at a certain speed during heating or maintaining a constant temperature, and the fluid in the window kettle 4 is stirred and mixed. After stopping the rotation, the internal lighting 2 is used to observe and measure the properties of the fluid in the window kettle 4. For example, through the scale on the transparent tube 401, the change of the fluid volume with temperature, the volume of crude oil dissolved in the water phase, the volume expansion of crude oil caused by CO2, the miscibility of CO2 and oil phase, etc. can be quantitatively measured, so as to calculate the fluid density, oil solubility coefficient, volume expansion coefficient, miscibility pressure and other fluid properties. During the heating or constant temperature process, the inert gas is injected into the thermostat 1 through the gas flowmeter 7 and the air inlet 6, and discharged from the exhaust port, so as to prevent the flammable gas from accumulating in the thermostat 1 and prevent the flammable gas and liquid from catching fire at high temperature due to the leakage of the material in the window kettle 4.

[0083] Embodiments of the present invention are as follows:

[0084] Example 1

[0085] The oil-water phase state of crude oil and surfactant solution at 200°C was observed, and the oil solubility coefficient was measured.

[0086] This embodiment uses a quartz tube full window kettle, that is, the transparent tube 401 is made of quartz. The window kettle 4 includes a temperature-resistant and pressure-resistant quartz tube (inner diameter 0.5 cm, volume 5 ml, minimum scale 0.02 ml), a stainless steel base 403, a frame and a sealing head 406 (using a solid plug), and a fluororubber O-ring, such as Figure 2-1As shown. The two ends of the quartz tube are inserted into the bases 403 at both ends and sealed with base sealing rings 404. The shielding volume of a single base 403 is ≤0.2ml, so the visible volume of the window kettle 4 is ≥4.6ml, accounting for ≥92% of the total volume. The base 403 at one end is opened and sealed with a solid plug and a sealing head tight ring 405. When adding liquid, remove the sealing head 406, add 2.0ml of crude oil and surfactant aqueous solution into the transparent tube 401, and then seal the sealing head 406.

[0087] The window kettle 4 filled with liquid is installed on the window kettle rotating device. Figure 1 shown.

[0088] The window kettle rotating device in this embodiment includes two layers of aluminum alloy rotating brackets 5. One end of the rotating bracket 5 is connected to the power mechanism 3, and the other end is connected to the rotating bearing. Each layer of rotating brackets 5 can fix up to 20 window kettles 4. The thermostat 1 used in this embodiment can stably maintain the temperature at 30-250°C, and the temperature is stable at 200°C in this embodiment. A glass observation window is installed on the door of the thermostat 1, and the fluid in the kettle can be observed and photographed through the observation window. The thermostat 1 is arranged with upper, middle and lower layers of lighting lamps 2, each layer of lighting lamps 2 has six, and each lighting lamp 2 has an independent switch. This embodiment uses an automatic rotating device, and the rotation speed can be adjusted within the range of 0-100rpm. In this embodiment, the rotation speed of the window kettle 4 is 10rpm. In this embodiment, carbon dioxide is used as an inert protective gas, and a rotor flowmeter is used to control the flow of carbon dioxide. The rotor flowmeter control range is 1-50L / h, and the injection flow rate in this embodiment is 20L / h. Carbon dioxide inert gas is injected from three air inlets 6 at the bottom of the thermostat 1, and waste gas is exhausted from an air outlet 8 at the top.

[0089] When in use, the window kettle 4 rotates at a speed of 10 rpm at 200°C, so that the oil and water phases in the kettle are fully mixed. After the mixture is evenly mixed, stop rotating, observe the oil-water phase state, record the amount of crude oil or aqueous solution dissolved in the emulsion, and calculate the oil solubility coefficient. It is common knowledge in the art to obtain the amount of crude oil or aqueous solution dissolved in the emulsion and calculate the oil solubility coefficient by observing the oil-water phase state in the window kettle 4. Here is a brief introduction as follows: stop rotating, observe the stability of the oil-water interface, and read the interface position of the emulsion phase and the water phase or crude oil phase. If an oil-water lower phase emulsion is produced, read the interface position of the emulsion phase and the crude oil phase, and calculate the crude oil reduction (V0) according to the change in the interface position as the amount of crude oil dissolved in the emulsion. The oil solubility coefficient is then equal to V0 / V s , where V s is the volume of surfactant in the system. If an oil-water upper phase emulsion is produced, read the interface position of the water phase and the emulsion phase, and calculate the reduction in the water phase (V w), as the amount of water dissolved in the emulsion, the water solubility coefficient is equal to V w / V s If an oil-water mid-phase emulsion is produced, read the water phase and the emulsion phase, as well as the interface between the oil phase and the emulsion phase, respectively, and calculate the reduction of the water phase and the oil phase, and calculate the oil and water solubility coefficients.

[0090] The results of the oil-water phase test are shown in Table 1. Photos were taken as evidence.

[0091]

[0092]

[0093] Table 1

[0094] Example 2

[0095] The solubility of surfactants in aqueous solutions was observed at 100-350°C.

[0096] This embodiment uses a sapphire full-window kettle, that is, the transparent tube 401 is made of sapphire. Figure 3-1 and Figure 3-2 As shown, the base 403 is fixed to the pressure sleeve 407 using a nut 408 to play a sealing role. The pressure sleeve 407 is more evenly stressed, which can effectively reduce the damage of the transparent tube 401 caused by uneven stress. Therefore, the expensive sapphire tube can be protected and its service life can be extended. However, the shielding area of ​​the pressure sleeve 407 is larger than the pull rod 402, which may affect the observation of the fluid at both ends of the transparent tube 401. The window kettle 4 is composed of a temperature-resistant and pressure-resistant sapphire tube with an inner diameter of 1.0 cm, a volume of 20 ml, and a minimum scale of 0.1 ml, a Hastelloy base 403 and a stainless steel pressure sleeve 407, as well as a graphite O-ring. The two ends of the sapphire tube are inserted into the bases 403 at both ends and sealed with O-rings. The shielding volume of a single base 403 is ≤0.8 ml, so the visible volume of the window kettle 4 is ≥18.4 ml, accounting for ≥92% of the total volume. When adding liquid, remove the base 403 at one end, add 15.0 ml of surfactant aqueous solution, and then seal the base 403.

[0097] The window kettle 4 filled with liquid is installed on the window kettle rotating device. Figure 4As shown. The window kettle rotating device in this embodiment includes a stainless steel rotating bracket 5. One end of the rotating bracket 5 is connected to the power mechanism 3, and the other end is connected to the rotating bearing. Each rotating bracket 5 can fix up to 5 window kettles 4 for testing different systems at the same time. The thermostat 1 used in this embodiment can stably maintain the temperature at 50-350°C. The initial test temperature in this embodiment is 100°C, which is gradually increased to 350°C. An observation window is provided on the door of the thermostat 1, through which the fluid in the window kettle 4 can be observed and photographed. The thermostat 1 is arranged with upper and lower layers of lighting lamps 2, each layer of lighting lamps 2 has three lamps, and each lighting lamp 2 has an independent switch. This embodiment uses an automatic rotating device, and the rotation speed can be adjusted within the range of 0-100rpm. In this embodiment, the rotation speed of the window kettle 4 is 50rpm. In this embodiment, nitrogen is used as an inert protective gas, and a mass flowmeter is used to control the nitrogen flow rate. The flowmeter control range is 0.1-5L / h, and the injection flow rate in this embodiment is 3L / h. Nitrogen inert gas is injected from three air inlets 6 at the bottom and side of the thermostat 1, and waste gas is discharged from an air outlet 8 at the top.

[0098] When in use, the window kettle 4 rotates at 50 rpm at a set temperature, so that the surfactant solution in the window kettle 4 remains disturbed. After the temperature stabilizes, the rotation is stopped, and the clarity of the aqueous solution is observed to determine the dissolution of the surfactant, and a photo is taken as evidence. The test results of the surfactant water solubility are as follows: Figure 6 As shown, Figure 6 In the figure, the hollow circles represent clear and transparent solutions, and the solid circles represent turbid solutions or phase separation.

[0099] Example 3

[0100] Observe the volume expansion effect of carbon dioxide on crude oil at 100°C.

[0101] The structure of the window kettle 4 used in this embodiment is the same as that of embodiment 2. Figure 3-1 and Figure 3-2 As shown. The difference is that the transparent tube 401 uses a temperature-resistant and pressure-resistant sapphire tube with an inner diameter of 0.5 cm, a volume of 5.0 ml, and a minimum scale of 0.02 ml; a perfluoro rubber O-ring is used; the sealing head 406 uses a plug with a central through hole, and its diameter is 3.0 mm. The outer end of the sealing head 406 has a ferrule joint, which can be connected to a stainless steel pipeline. When adding liquid, remove the sealing head 406, add 2.0 ml of crude oil, and then seal the sealing head 406.

[0102] The window kettle 4 filled with liquid is installed on the window kettle rotating device. Figure 7 shown.

[0103] The window kettle rotating device in this embodiment includes a rotating bracket 5. One end of the rotating bracket 5 passes through the bearing and is connected to the power mechanism 3, and the other end is connected to the bearing. Each rotating bracket 5 can fix up to 4 window kettles 4. The constant temperature box 1 used in this embodiment can stably maintain the temperature at 30-250°C, and the temperature in this embodiment is 100°C. A glass observation window is installed on the door of the constant temperature box 1, and the fluid in the kettle can be observed and photographed through the observation window. Two layers of lighting lamps 2 are arranged in the constant temperature box 1, and each layer of lighting lamps 2 has three lamps, and each lighting lamp 2 has an independent switch. This embodiment uses a manual rotating device. In this embodiment, the window kettle 4 rotates 180° and then rotates back to its original position, and repeats this process to maintain the rotation speed at 10-30rpm.

[0104] Furthermore, the sealing head 406 of the window kettle 4 is connected to one end of a stainless steel coil 9 with an outer diameter of 3 mm, and the other end of the coil 9 extends out of the thermostat 1 from the air outlet 8 and is connected to the carbon dioxide constant pressure system 10. When the window kettle 4 rotates, the coil 9 acts as a buffer spring and repeatedly expands and contracts. The carbon dioxide constant pressure system 10 includes a carbon dioxide pump and a carbon dioxide back pressure valve. High-pressure carbon dioxide is injected into the window kettle 4 through the carbon dioxide pump, and the carbon dioxide back pressure valve is used to keep the system pressure constant, so that the high pressure in the window kettle 4 is ensured by carbon dioxide.

[0105] In this embodiment, argon is used as an inert protective gas, and a rotor flowmeter is used to control the argon flow rate. The rotor flowmeter has a control range of 1-50 L / h, and the injection flow rate in this embodiment is 10 L / h. Argon is injected into the thermostat 1 from three air inlets 6 at the bottom of the thermostat 1 and two air inlets 6 on the side, and the exhaust gas is discharged from three air outlets 8 at the top.

[0106] When in use, inject 3-20MPa carbon dioxide into the window kettle 4 at a temperature of 100°C, and rotate back and forth at 10-30rpm at each test pressure to fully mix the oil and carbon dioxide in the kettle. After mixing evenly, stop rotating, observe and record the volume of crude oil, and calculate the expansion coefficient of crude oil. The expansion coefficient calculation method is as follows: After equilibrium, read the crude oil volume V according to the scale of the window kettle 4 f , then the expansion coefficient is equal to V f / V I , where V I is the initial volume of crude oil, such as Figure 8 And take photos as evidence.

[0107] Example 4

[0108] This embodiment is the same as the embodiment 1, but does not have the power mechanism 3, that is, the rotating bracket 5 cannot rotate. The oil and water can only be mixed by diffusion. Although the state of the oil and water at high temperature can still be observed, within the same test time as in the embodiment 1, the oil and water do not emulsify, and the oil solubility coefficient is basically 0.

[0109] Example 5

[0110] This embodiment is the same as the embodiment 2, but does not have the power mechanism 3, and the volume of the window kettle 4 is too large, and the visible volume is ≤80%. The turbidity of the surfactant B at 200°C can still be observed. However, at 250°C, due to the lack of rotation and stirring, the precipitate gathers at the bottom of the kettle and is blocked by the pressure sleeve 407. Only a clear and transparent solution can be observed through the visible part, so it is mistakenly believed that the surfactant B becomes soluble again at a temperature ≥250°C.

[0111] Example 6

[0112] This embodiment is the same as embodiment 3, but the power mechanism 3 is not provided. Since it cannot rotate, CO2 can only diffuse into the oil phase through molecular thermal motion. Although crude oil expansion can still be observed, the equilibrium time is 10-100 times that in embodiment 3, which greatly prolongs the experimental time.

[0113] Comparative Example 1

[0114] Use a conventional pressure-volume-temperature (PVT) window kettle to test the oil-water phase. The volume of a conventional window kettle is 100ml, and a magnetic stirrer is used, and the minimum measurement accuracy is 1.0ml. It is necessary to add 30ml of aqueous solution and crude oil to the conventional window kettle, and then stir at a specified temperature until equilibrium. However, this method has the following problems:

[0115] First, the amount of crude oil used increases significantly, resulting in a waste of precious samples.

[0116] Secondly, it is difficult to fully mix the oil and water phases using magnetic stirring, especially when the crude oil viscosity is ≥100mPa·s, it is even more difficult to achieve full mixing, which often leads to an underestimation of the oil solubility coefficient.

[0117] Finally, the measurement accuracy of conventional PVT window kettles is too low to accurately and quantitatively calculate the oil solubility coefficient.

[0118] Comparative Example 2

[0119] The high-temperature water solubility of the surfactant was tested using a conventional pressure-volume-temperature (PVT) window kettle. Conventional window kettles use magnetic stirring, which can only stir up precipitates with a density greater than that of water. However, the surfactant A in Example 2 was hydrolyzed at 300°C, and a water-insoluble surfactant phase with a lower density than the water phase appeared. When using magnetic stirring, the separated surfactant cannot be mixed into the water phase, so the water phase is clear and transparent, which may cause the experimenter to mistakenly believe that the surfactant A is still clear and transparent at 300°C.

[0120] When the device of the present invention is used for mixing, the surfactant phase floating on the water surface can be mixed into the water phase to produce a turbid solution that is easy to observe.

[0121] Comparative Example 3

[0122] The effect of carbon dioxide on the volume expansion of crude oil was tested using a conventional pressure-volume-temperature (PVT) window kettle. Conventional window kettles use magnetic stirring, and can only rely on stirring the crude oil to form a vortex, thereby pulling carbon dioxide into the oil phase. However, for crude oil with a viscosity ≥ 100 mPa·s, it is impossible to fully stir the crude oil using magnetic stirring, resulting in carbon dioxide being unable to fully contact the crude oil and having to rely on diffusion to reach equilibrium. Its equilibrium time is 10-100 times that of the device of the present invention, and causes the experimenter to misjudge the equilibrium point. In addition, the measurement accuracy of conventional window kettles is low, and it is impossible to accurately and quantitatively calculate the expansion coefficient of crude oil.

[0123] From the above analysis, it can be seen that the rotary stirring using the device of the present invention can affect all crude oil and water phases, and even for high-viscosity crude oil, it can be fully contacted with carbon dioxide, thereby improving the stirring and mixing efficiency. However, when using conventional magnetic stirring, it is difficult to form a vortex for high-viscosity crude oil, which further reduces its stirring efficiency. In addition, the device of the present invention has a constant temperature function, which can reduce the viscosity of crude oil by heating, which is more conducive to the mixing of oil and water phases.

[0124] In the description of the present invention, it should be noted that, unless otherwise clearly specified and limited, the terms "connected" and "connection" should be understood in a broad sense, for example, it can be a fixed connection, a detachable connection, or an integral connection; it can be a mechanical connection or an electrical connection; it can be a direct connection or an indirect connection through an intermediate medium. For ordinary technicians in this field, the specific meanings of the above terms in the present invention can be understood according to specific circumstances.

[0125] In the description of the present invention, unless otherwise specified, the terms "upper", "lower", "left", "right", "inside", "outside", etc. indicate directions or positional relationships based on the directions or positional relationships shown in the accompanying drawings. They are only for the convenience of describing the present invention and simplifying the description, and do not indicate or imply that the device or element referred to must have a specific direction, be constructed and operated in a specific direction. Therefore, they cannot be understood as limitations on the present invention.

[0126] The above technical solution is only one implementation mode of the present invention. For those skilled in the art, it is easy to make various types of improvements or modifications based on the principles disclosed in the present invention, and it is not limited to the technical solution described in the above specific embodiments of the present invention. Therefore, the above description is only preferred and does not have a restrictive meaning.

Claims

1. A window kettle rotating device, characterized in that: The device comprises: a window kettle, a constant temperature box, and a rotating bracket arranged in the constant temperature box; The window kettle can be installed on a rotating bracket; A power mechanism is arranged outside the thermostatic box; The power mechanism is connected with the rotating bracket.

2. The window kettle rotating device according to claim 1, characterized in that: The window kettle comprises: a transparent tube, a base and a frame; The transparent tube is a transparent tubular structure with openings at both ends, and scales are marked on the outer wall of the transparent tube; A groove is provided in the middle of each base, and the two ends of the transparent tube can be inserted into the grooves of the two bases respectively; The frame comprises at least two pull rods, each pull rod is parallel to the transparent tube, and two ends of each pull rod are respectively installed on two bases.

3. The window kettle rotating device according to claim 1, characterized in that: The window kettle comprises: a transparent tube, a base, a pressure sleeve and a nut; The transparent tube is a transparent tubular structure with openings at both ends, and scales are marked on the outer wall of the transparent tube; A groove is provided in the middle of each base, and the two ends of the transparent tube can be inserted into the grooves of the two bases respectively; The pressure sleeve is a cylindrical structure with openings at both ends, and is provided with at least two long holes parallel to its central axis; The two bases are respectively fixed to the two ends of the pressure sleeve through nuts.

4. The window kettle rotating device according to claim 1, characterized in that: The transparent tube is made of quartz or sapphire; The inner diameter of the transparent tube is 0.2-2.0 cm.

5. The window kettle rotating device according to claim 2 or 3, characterized in that: A threaded hole is formed in the middle of a base, the threaded hole is connected to the groove and is coaxial with the groove; One end of the sealing head can be screwed into the threaded hole; The sealing head is a solid plug or a plug with a central through hole.

6. The window kettle rotating device according to claim 1, characterized in that: An air inlet and an air outlet are arranged on the thermostat; The air inlet is connected to a gas flow controller; A plurality of lighting lamps are arranged in the constant temperature box; An observation window is provided on the wall of the thermostatic box.

7. The window kettle rotating device according to claim 5, characterized in that: The other end of the sealing head is connected to one end of the coil, and the other end of the coil is connected to the carbon dioxide constant pressure system after extending out of the constant temperature box from the gas outlet.

8. The window kettle rotating device according to claim 1, characterized in that: The rotating bracket includes a supporting frame and a partition; The support frame includes a long board and a short board, and the two long boards and the two short boards form a rectangular frame; A plurality of U-shaped grooves with openings facing outward are formed on each long board, and the U-shaped grooves on the two long boards correspond to each other one by one; A plurality of partitions parallel to the short boards are arranged between the two short boards, and the two ends of the partitions are respectively connected to the long boards on both sides; the connection between the partitions and the long boards is located between two adjacent U-shaped grooves; A connecting hole is opened at the center of each short plate, a rotating shaft is connected to the connecting hole, and the rotating shaft can be connected to the power mechanism; The rotating bracket also includes two limit baffles, which are arranged parallel to the long plate, and two ends of the limit baffles are fixed to the outer surface of the long plate by bolts.

9. The window kettle rotating device according to claim 1, characterized in that: One to five rotating brackets are installed in the constant temperature box, and the multiple rotating brackets are arranged in sequence from top to bottom.

10. A fluid stirring and mixing method, characterized in that: The method is implemented using the window kettle rotating device according to any one of claims 1 to 9, and the method comprises: Put the fluid to be tested into the sight glass kettle, and then fix the sight glass kettle on the rotating bracket; The thermostat is started to heat or maintain a constant temperature, and the rotating bracket is driven to rotate by the power mechanism to stir and mix the fluid to be tested in the window kettle; at the same time, the inert gas enters the thermostat from the air inlet and is discharged from the exhaust port; Stop the rotation, observe and measure the properties of the fluid to be tested in the window kettle.

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