A supercritical carbon dioxide system viscosity tester and its testing method

Abstract

The present invention discloses a supercritical carbon dioxide system viscosity tester and a measuring method thereof, including a feeding system, a test kettle, a bracket, an electric crank system, and a thermostat. The feeding system is composed of a carbon dioxide storage tank, a material tank, a compressor, a high-pressure metering pump, a high-pressure hose I, a high-pressure hose II, a one-way valve I and a one-way valve II. The test kettle is composed of a head, a kettle body, an O-ring, a kettle cavity, a falling ball, an upper needle valve, a lower needle valve, a jet mixer, a force-sensitive sensor I, a force-sensitive sensor II, a vent valve, a pressure gauge, a thermometer, and a connecting bolt. The jet mixer is composed of a nozzle, an inhalation pipe, a tapered section, and a diffusion section. The present invention can adjust the test angle and can fully mix the fluid. The present invention has the advantages of a wide measurement range, can measure high pressures up to 100MPa and high temperatures of 200°C, and can also cope with fluids of various viscosities; at the same time, the present invention also has the advantages of high measurement accuracy.

Description

Technical Field

[0001] The invention relates to a viscosity tester and a testing method thereof, in particular to a falling ball type supercritical carbon dioxide system viscosity tester and a testing method thereof. Background Art

[0002] A fluid whose temperature and pressure are above the critical point is called a supercritical fluid. It has the properties of a gas and can be easily compressed or expanded, and like a liquid, it has a large density. Its viscosity is smaller than that of a liquid, and it has better fluidity and thermal conductivity. In many applications of supercritical fluids such as oxidation, spraying, and nano-micron preparation, fluid viscosity is an essential parameter. Therefore, the invention of a supercritical carbon dioxide system viscosity meter is of great significance. CN207439863 U discloses a high-temperature and high-pressure viscometer, which can measure the viscosity of complex system fluids under high-temperature and high-pressure conditions and the viscosity of fluids that change from substances to flowable fluids as temperature and pressure change; CN205670108 U discloses a viscosity tester, which provides a high-precision, high-efficiency, and easy-to-operate high-temperature and high-pressure gravity-sensing falling ball liquid viscosity tester; CN 212083162 U discloses a high-temperature and high-pressure falling ball viscosity metering device, which synchronously simulates the influence of different displacement fluid viscosities on the displacement effect under the same temperature and pressure reservoir conditions. The above-mentioned testers have limited ranges and also have measurement precision problems caused by insufficient mixing of the material system. Summary of the invention

[0003] In order to solve the above technical problems, the present invention provides a supercritical carbon dioxide system viscosity meter and a testing method thereof, which realizes efficient and accurate viscosity measurement of supercritical carbon dioxide.

[0004] The invention provides a supercritical carbon dioxide system viscosity tester, comprising a feeding system and a testing system, wherein the feeding system comprises a material tank, a high-pressure metering pump, a one-way valve I, a carbon dioxide storage tank, a compressor, a one-way valve II, a high-pressure hose I and a high-pressure hose II, wherein the material tank, the high-pressure metering pump and the one-way valve I are sequentially connected and communicated with the testing system through the high-pressure hose I, and the carbon dioxide storage tank, the compressor and the one-way valve II are sequentially connected and communicated with the testing system through the high-pressure hose II; the testing system comprises a testing kettle, a bracket, an electric crank system and a constant temperature box, wherein the testing kettle is supported by the bracket and can rotate around a fulcrum, one end of the electric crank system is connected to the upper end or the lower end of the testing kettle, the electric crank system is used to control the tilt angle of the testing kettle, and the testing kettle, the bracket and the electric crank system are placed in the constant temperature box.

[0005] Furthermore, the test kettle has a kettle body and a kettle cavity, including a head, an O-ring, a falling ball, an upper needle valve, a jet mixer, a vent valve, a lower needle valve, a force sensitive sensor I, a temperature gauge, a pressure gauge, a force sensitive sensor II, and connecting bolts, wherein the head and the kettle body are sealed and connected by connecting bolts and O-rings, the jet mixer is installed on the outer wall of the test kettle through a flange and is connected to the kettle cavity, the force sensitive sensor I and the force sensitive sensor II are respectively arranged at the upper and lower ends of the kettle cavity, the falling ball is placed in the kettle cavity, the upper needle valve and the lower needle valve are respectively arranged at the upper and lower parts of the kettle cavity, and the upper needle valve and the lower needle valve are used to block or release the falling ball.

[0006] Furthermore, the jet mixer includes a nozzle, a tapered section, and a diffuser section which are connected in sequence, and the suction pipe is arranged on the side wall of the nozzle and is connected to the tapered section.

[0007] Furthermore, the one-way valve I is connected to the suction pipe through a high-pressure hose I, and the one-way valve II is connected to the nozzle through a high-pressure hose II.

[0008] Furthermore, the kettle body test kettle is also provided with a vent valve for releasing the pressure in the kettle cavity, and a temperature gauge and a pressure gauge for testing the physical indicators in the kettle cavity.

[0009] Furthermore, the bracket includes a rotating bearing, a support rod, and a base, and the rotating bearing is connected to the test kettle.

[0010] Furthermore, the electric crank system includes a connecting bearing I, a fixed-length crank, a connecting bearing II, an adjustable crank, a connecting bearing III and a motor. The fixed-length crank is connected to the test kettle through the connecting bearing I, and the adjustable crank is a retractable structure; the shorter the adjustable crank is, the greater the inclination angle of the test kettle is. α The larger the adjustable crank is, the more suitable it is for testing fluids with low viscosity; conversely, the longer the adjustable crank is and the smaller the inclination angle α of the test kettle is, the more suitable it is for testing fluids with high viscosity. The fixed-length crank and the adjustable crank are connected by a connecting bearing II. The motor is used to control the rotation of the adjustable crank. By controlling the length and rotation angle of the adjustable crank, the test kettle can be made to circulate or be in different inclination states, thereby achieving sufficient mixing of the supercritical carbon dioxide system and viscosity measurement.

[0011] Furthermore, the maximum pressure that the feeding system and the test kettle can withstand is 100 MPa, and the maximum temperature is 200°C.

[0012] The present invention provides a method for using a supercritical carbon dioxide system viscosity tester, characterized in that during measurement, a fluid is introduced into a test kettle, a needle valve is opened to lower a falling ball after adjusting the angle, and the falling ball is measured by a force sensitive sensor. The following viscosity calculation formula is substituted to calculate the fluid viscosity:

[0013] η =[d 2 ( ρ 0- ρ ) t sin αf w ] / (18 l )

[0014] in, η is the fluid viscosity;

[0015] d is the diameter of the falling ball;

[0016] ρ 0 is the falling ball density;

[0017] ρ is the fluid density;

[0018] g is the acceleration due to gravity;

[0019] l is a certain distance that the steel ball falls at a constant speed;

[0020] t is the falling time of the steel ball within the distance l;

[0021] f w It is the correction factor for the influence of the pipe wall, which can be obtained by measuring the viscosity of water under standard conditions;

[0022] α is the tilt angle.

[0023] The advantages of the present invention are:

[0024] The supercritical carbon dioxide system viscosity tester has the advantages of compact and simple overall structure, convenient use, wide measuring range and high measuring accuracy, and has broad application prospects. BRIEF DESCRIPTION OF THE DRAWINGS

[0025] Figure 1 This is the system composition diagram of the supercritical carbon dioxide system viscosity tester;

[0026] Figure 2 It is the side view of the test system;

[0027] Figure 3 It is a cross-sectional front view of the test kettle;

[0028] Figure 4 It is a cross-sectional side view of the test kettle;

[0029] Figure 5 It is a side view of the rotating bracket;

[0030] Figure 6 It is the front view of the electric crank system;

[0031] Figure 7 It is a side view of the electric crank system;

[0032] Figure 8 It is a cross-sectional view of a jet mixer;

[0033] Fig. 9 is the minimum tilt angle;

[0034] Fig.10 is the maximum tilt angle;

[0035] Fig.11 The variable crank is in the longest state;

[0036] Fig.12 This is the shortest state of the variable crank.

[0037] The numbers in the figure are: 1, material tank 2, high-pressure metering pump 3, one-way valve I 4, carbon dioxide storage tank 5, compressor 6, one-way valve II 7, high-pressure hose I 8, high-pressure hose II 9, test kettle 10, rotating bracket 11, electric crank system 12, constant temperature box 9-1, head 9-2, O-ring 9-3, falling ball 9-4, upper needle valve 9-5, jet mixer 9-6, kettle cavity 9-7, vent valve 9-8, lower needle valve 9-9, kettle body 9-10, force sensitive sensor I 9-11, temperature gauge 9-12, pressure gauge 9-13, force sensitive sensor II 9-14, connecting bolt 10-1, rotating shaft 10-2, support rod 10-3, base 11-1, connecting bearing I 11-2, fixed-length crank 11-3, connecting shaft II 11-4, adjustable crank 11-5, connecting shaft III 11-6, motor. DETAILED DESCRIPTION

[0038] The present invention will be further described in detail below with reference to the accompanying drawings and by way of examples. The following examples are intended to explain the present invention but the present invention is not limited to the following examples.

[0039] Implementation Case 1

[0040] like Figure 1 As shown, the material tank (1), the high-pressure metering pump (2), the one-way valve I (3), the carbon dioxide storage tank (4), the compressor (5), the one-way valve II (6), the high-pressure hose (7), the high-pressure hose II (8), and the test kettle (9) are connected in sequence, and the test kettle (9), the bracket (10), the electric crank system (11), and the constant temperature box (12) are installed.

[0041] Open the end cap (9-1), place the falling ball (9-3) into the kettle chamber (9-6) near the upper end of the end cap, close the upper end needle valve (9-4) to hold the falling ball (9-3), keep the lower end needle valve (9-8) in an open state, insert an O-ring (9-2) for sealing, and connect the end cap (9-1) to the kettle body (9-9) through the connecting bolt (9-14); open the carbon dioxide storage tank (1), the one-way valve I (3) and the vent valve (9-7), close the vent valve (9-7) after the device is completely filled with carbon dioxide, open the high-pressure metering pump (2), the compressor (5) and the one-way valve II (6), and introduce water into the test kettle (9).

[0042] like Fig. 9 , define the angle between the test kettle connection surface and the vertical plane as the inclination angle α. Adjust the length of the adjustable crank (11-4) to make the inclination angle of the test kettle 30°, open the upper needle valve (9-4), and measure the time t when the falling ball reaches the force sensitive sensor I (9-10).

[0043] Close the lower needle valve (9-8), start the motor (11-6) of the electric crank system, drive the connecting shaft II (11-5) to rotate, rotate the adjustable crank (11-4), and drive the test kettle (9) to rotate through the connecting shaft II (11-3). Turn the test kettle upside down so that the inclination angle of the test kettle is 150°, measure the time t when the falling ball reaches the force sensitive sensor II (9-13), and repeat this process to obtain multiple sets of data.

[0044] According to formula (1), the correction coefficient of the tube wall effect of the instrument is calculated: f w .

[0045] Implementation Case 2

[0046] like Figure 1 As shown, the material tank (1), the high-pressure metering pump (2), the one-way valve I (3), the carbon dioxide storage tank (4), the compressor (5), the one-way valve II (6), the high-pressure hose (7), the high-pressure hose II (8), and the test kettle (9) are connected in sequence, and the test kettle (9), the bracket (10), the electric crank system (11), and the constant temperature box (12) are installed.

[0047] Open the end cap (9-1), place the ball (9-3) into the kettle chamber (9-6) near the upper end of the end cap, close the upper end needle valve (9-4) to hold the ball (9-3), keep the lower end needle valve (9-8) in an open state, insert an O-ring (9-2) for sealing, and connect the end cap (9-1) to the kettle body (9-9) through the connecting bolt (9-14); open the carbon dioxide storage tank (1), the one-way valve I (3) and the vent valve (9-7), and close the vent valve after the device is completely filled with carbon dioxide. 9-7), open the high-pressure metering pump (2), the compressor (5) and the one-way valve II (6), so that the paint and the carbon dioxide enter the jet mixer (9-5) for primary mixing, and at the same time start the motor (11-6) of the electric crank to drive the connecting shaft III (11-5) to rotate, so that the adjustable crank (11-4) rotates, and the fixed-length crank (11-2) drives the test kettle (8) to shake up and down through the connecting shaft II (11-3), so that the paint and the carbon dioxide are mixed for a second time in the test kettle (9).

[0048] like Fig. 9 , define the angle between the connection surface of the test kettle and the vertical plane as the inclination angle α. After the pressure reaches 10MPa, turn off the air compressor, and then indirectly turn on the air compressor to keep the pressure at 10MPa. Turn on the power of the thermostat to make the temperature in the test kettle (8) reach 50°C. After the temperature and pressure are stable, adjust the length of the adjustable crank (11-4) to make the inclination angle of the test kettle 30°, open the upper needle valve (9-4), and measure the time it takes for the falling ball to reach the force sensitive sensor I (9-10). t .

[0049] Close the lower needle valve (9-8), start the motor (11-6) of the electric crank system, drive the connecting shaft II (11-5) to rotate, rotate the adjustable crank (11-4), and drive the test kettle (9) to rotate through the connecting shaft II (11-3). Turn the test kettle upside down so that the inclination angle of the test kettle is 150°, and measure the time it takes for the falling ball to reach the force sensitive sensor II (9-13). t , repeat this process to obtain multiple sets of data.

[0050] After the reaction is finished, stop heating and open the vent valve (9-7) to release the pressure. After the test kettle cools down, open the test kettle for cleaning. Calculate the fluid viscosity according to formula (1).

[0051] Implementation Case 3

[0052] like Figure 1As shown, the material tank (1), the high-pressure metering pump (2), the one-way valve I (3), the carbon dioxide storage tank (4), the compressor (5), the one-way valve II (6), the high-pressure hose (7), the high-pressure hose II (8), and the test kettle (9) are connected in sequence, and the test kettle (9), the bracket (10), the electric crank system (11), and the constant temperature box (12) are installed.

[0053] Open the end cap (9-1), place the ball (9-3) into the kettle chamber (9-6) near the upper end of the end cap, close the upper end needle valve (9-4) to hold the ball (9-3), keep the lower end needle valve (9-8) in an open state, insert an O-ring (9-2) for sealing, and connect the end cap (9-1) to the kettle body (9-9) through the connecting bolt (9-14); open the carbon dioxide storage tank (1), the one-way valve I (3) and the vent valve (9-7), and close the vent valve after the device is completely filled with carbon dioxide. 9-7), open the high-pressure metering pump (2), the compressor (5) and the one-way valve II (6), so that the paint and the carbon dioxide enter the jet mixer (9-5) for primary mixing, and at the same time start the motor (11-6) of the electric crank to drive the connecting shaft III (11-5) to rotate, so that the adjustable crank (11-4) rotates, and the fixed-length crank (11-2) drives the test kettle (8) to shake up and down through the connecting shaft II (11-3), so that the paint and the carbon dioxide are mixed for a second time in the test kettle (9).

[0054] like Fig. 9 , define the angle between the connection surface of the test kettle and the vertical plane as the inclination angle α. After the pressure reaches 100MPa, turn off the air compressor, and then turn on the air compressor indirectly to keep the pressure at 100MPa. Turn on the power of the thermostat to make the temperature in the test kettle (8) reach 50°C. After the temperature and pressure are stable, adjust the length of the adjustable crank (11-4) to make the inclination angle of the test kettle 60°, open the upper needle valve (9-4), and measure the time t when the falling ball reaches the force sensitive sensor I (9-10).

[0055] Close the lower needle valve (9-8), start the motor (11-6) of the electric crank system, drive the connecting shaft II (11-5) to rotate, rotate the adjustable crank (11-4), and drive the test kettle (9) to rotate through the connecting shaft II (11-3). Turn the test kettle upside down so that the inclination angle of the test kettle is 120°, and measure the time it takes for the falling ball to reach the force sensitive sensor II (9-13). t , repeat this process to obtain multiple sets of data.

[0056] After the reaction is completed, stop pressurizing and heating, open the vent valve (9-7) to release the pressure, and after the test kettle cools down, open the test kettle for cleaning. Calculate the fluid viscosity according to formula (1).

[0057] Implementation Case 4

[0058] like Figure 1 As shown, the material tank (1), the high-pressure metering pump (2), the one-way valve I (3), the carbon dioxide storage tank (4), the compressor (5), the one-way valve II (6), the high-pressure hose (7), the high-pressure hose II (8), and the test kettle (9) are connected in sequence, and the test kettle (9), the bracket (10), the electric crank system (11), and the constant temperature box (12) are installed.

[0059] Open the end cap (9-1), place the ball (9-3) into the kettle chamber (9-6) near the upper end of the end cap, close the upper end needle valve (9-4) to hold the ball (9-3), keep the lower end needle valve (9-8) in an open state, insert an O-ring (9-2) for sealing, and connect the end cap (9-1) to the kettle body (9-9) through the connecting bolt (9-14); open the carbon dioxide storage tank (1), the one-way valve I (3) and the vent valve (9-7), and close the vent valve after the device is completely filled with carbon dioxide. 9-7), open the high-pressure metering pump (2), the compressor (5) and the one-way valve II (6), so that the paint and the carbon dioxide enter the jet mixer (9-5) for primary mixing, and at the same time start the motor (11-6) of the electric crank to drive the connecting shaft III (11-5) to rotate, so that the adjustable crank (11-4) rotates, and the fixed-length crank (11-2) drives the test kettle (8) to shake up and down through the connecting shaft II (11-3), so that the paint and the carbon dioxide are mixed for a second time in the test kettle (9).

[0060] like Fig. 9 , define the angle between the connection surface of the test kettle and the vertical plane as the inclination angle α. After the pressure reaches 100MPa, turn off the air compressor, and then indirectly turn on the air compressor to keep the pressure at 10MPa. Turn on the power of the thermostat to make the temperature in the test kettle (8) reach 120℃. After the temperature and pressure are stable, adjust the length of the adjustable crank (11-4) to make the inclination angle of the test kettle 45°, open the upper needle valve (9-4), and measure the time it takes for the falling ball to reach the force sensitive sensor I (9-10). t .

[0061] Close the lower needle valve (9-8), start the motor (11-6) of the electric crank system, drive the connecting shaft II (11-5) to rotate, rotate the adjustable crank (11-4), and drive the test kettle (9) to rotate through the connecting shaft II (11-3). Turn the test kettle upside down so that the inclination angle of the test kettle is 135°, and measure the time it takes for the falling ball to reach the force sensitive sensor II (9-13). t , repeat this process to obtain multiple sets of data.

[0062] After the reaction is finished, stop heating and open the vent valve (9-7) to release the pressure. After the test kettle cools down, open the test kettle for cleaning. Calculate the fluid viscosity according to formula (1).

[0063] Implementation Case 5

[0064] like Figure 1 As shown, the material tank (1), the high-pressure metering pump (2), the one-way valve I (3), the carbon dioxide storage tank (4), the compressor (5), the one-way valve II (6), the high-pressure hose (7), the high-pressure hose II (8), and the test kettle (9) are connected in sequence, and the test kettle (9), the bracket (10), the electric crank system (11), and the constant temperature box (12) are installed.

[0065] Open the end cap (9-1), place the ball (9-3) into the kettle chamber (9-6) near the upper end of the end cap, close the upper end needle valve (9-4) to hold the ball (9-3), keep the lower end needle valve (9-8) in an open state, insert an O-ring (9-2) for sealing, and connect the end cap (9-1) to the kettle body (9-9) through the connecting bolt (9-14); open the carbon dioxide storage tank (1), the one-way valve I (3) and the vent valve (9-7), and close the vent valve after the device is completely filled with carbon dioxide. 9-7), open the high-pressure metering pump (2), the compressor (5) and the one-way valve II (6), so that the paint and the carbon dioxide enter the jet mixer (9-5) for primary mixing, and at the same time start the motor (11-6) of the electric crank to drive the connecting shaft III (11-5) to rotate, so that the adjustable crank (11-4) rotates, and the fixed-length crank (11-2) drives the test kettle (8) to shake up and down through the connecting shaft II (11-3), so that the paint and the carbon dioxide are mixed for a second time in the test kettle (9).

[0066] like Fig. 9 , define the angle between the connection surface of the test kettle and the vertical plane as the inclination angle α. After the pressure reaches 50MPa, turn off the air compressor, and then indirectly turn on the air compressor to keep the pressure at 50MPa. Turn on the power of the thermostat to make the temperature in the test kettle (8) reach 120℃. After the temperature and pressure are stable, adjust the length of the adjustable crank (11-4) to make the inclination angle of the test kettle 60°, open the upper needle valve (9-4), and measure the time it takes for the falling ball to reach the force sensitive sensor I (9-10). t .

[0067] Close the lower needle valve (9-8), start the motor (11-6) of the electric crank system, drive the connecting shaft II (11-5) to rotate, rotate the adjustable crank (11-4), and drive the test kettle (9) to rotate through the connecting shaft II (11-3). Turn the test kettle upside down so that the inclination angle of the test kettle is 120°, and measure the time it takes for the falling ball to reach the force sensitive sensor II (9-13). t, repeat this process to obtain multiple sets of data.

[0068] After the reaction is finished, stop heating and open the vent valve (9-7) to release the pressure. After the test kettle cools down, open the test kettle for cleaning. According to (1), calculate the fluid viscosity.

[0069] Implementation Case 6

[0070] like Figure 1 As shown, the material tank (1), the high-pressure metering pump (2), the one-way valve I (3), the carbon dioxide storage tank (4), the compressor (5), the one-way valve II (6), the high-pressure hose (7), the high-pressure hose II (8), and the test kettle (9) are connected in sequence, and the test kettle (9), the bracket (10), the electric crank system (11), and the constant temperature box (12) are installed.

[0071] Open the end cap (9-1), place the ball (9-3) into the kettle chamber (9-6) near the upper end of the end cap, close the upper end needle valve (9-4) to hold the ball (9-3), keep the lower end needle valve (9-8) in an open state, insert an O-ring (9-2) for sealing, and connect the end cap (9-1) to the kettle body (9-9) through the connecting bolt (9-14); open the carbon dioxide storage tank (1), the one-way valve I (3) and the vent valve (9-7), and close the vent valve after the device is completely filled with carbon dioxide. 9-7), open the high-pressure metering pump (2), the compressor (5) and the one-way valve II (6), so that the paint and the carbon dioxide enter the jet mixer (9-5) for primary mixing, and at the same time start the motor (11-6) of the electric crank to drive the connecting shaft III (11-5) to rotate, so that the adjustable crank (11-4) rotates, and the fixed-length crank (11-2) drives the test kettle (8) to shake up and down through the connecting shaft II (11-3), so that the paint and the carbon dioxide are mixed for a second time in the test kettle (9).

[0072] like Fig. 9 , define the angle between the connection surface of the test kettle and the vertical plane as the inclination angle α. After the pressure reaches 100MPa, turn off the air compressor, and then indirectly turn on the air compressor to keep the pressure at 100MPa. Turn on the power of the thermostat to make the temperature in the test kettle (8) reach 120℃. After the temperature and pressure are stable, adjust the length of the adjustable crank (11-4) to make the inclination angle of the test kettle 30°, open the upper needle valve (9-4), and measure the time it takes for the falling ball to reach the force sensitive sensor I (9-10). t .

[0073] Close the lower needle valve (9-8), start the motor (11-6) of the electric crank system, drive the connecting shaft II (11-5) to rotate, rotate the adjustable crank (11-4), and drive the test kettle (9) to rotate through the connecting shaft II (11-3). Turn the test kettle upside down so that the inclination angle of the test kettle is 150°, and measure the time it takes for the falling ball to reach the force sensitive sensor II (9-13). t , repeat this process to obtain multiple sets of data.

[0074] After the reaction is finished, stop heating and open the vent valve (9-7) to release the pressure. After the test kettle cools down, open the test kettle for cleaning. Calculate the fluid viscosity according to formula (1).

[0075] Implementation Case 7

[0076] like Figure 1 As shown, the material tank (1), the high-pressure metering pump (2), the one-way valve I (3), the carbon dioxide storage tank (4), the compressor (5), the one-way valve II (6), the high-pressure hose (7), the high-pressure hose II (8), and the test kettle (9) are connected in sequence, and the test kettle (9), the bracket (10), the electric crank system (11), and the constant temperature box (12) are installed.

[0077] Open the end cap (9-1), place the ball (9-3) into the kettle chamber (9-6) near the upper end of the end cap, close the upper end needle valve (9-4) to hold the ball (9-3), keep the lower end needle valve (9-8) in an open state, insert an O-ring (9-2) for sealing, and connect the end cap (9-1) to the kettle body (9-9) through the connecting bolt (9-14); open the carbon dioxide storage tank (1), the one-way valve I (3) and the vent valve (9-7), and close the vent valve after the device is completely filled with carbon dioxide. 9-7), open the high-pressure metering pump (2), the compressor (5) and the one-way valve II (6), so that the paint and the carbon dioxide enter the jet mixer (9-5) for primary mixing, and at the same time start the motor (11-6) of the electric crank to drive the connecting shaft III (11-5) to rotate, so that the adjustable crank (11-4) rotates, and the fixed-length crank (11-2) drives the test kettle (8) to shake up and down through the connecting shaft II (11-3), so that the paint and the carbon dioxide are mixed for a second time in the test kettle (9).

[0078] like Fig. 9, define the angle between the connection surface of the test kettle and the vertical plane as the inclination angle α. After the pressure reaches 10MPa, turn off the air compressor, and then indirectly turn on the air compressor to keep the pressure at 10MPa. Turn on the power of the thermostat to make the temperature in the test kettle (8) reach 200℃. After the temperature and pressure are stable, adjust the length of the adjustable crank (11-4) to make the inclination angle of the test kettle 60°, open the upper needle valve (9-4), and measure the time it takes for the falling ball to reach the force sensitive sensor I (9-10). t .

[0079] Close the lower needle valve (9-8), start the motor (11-6) of the electric crank system, drive the connecting shaft II (11-5) to rotate, rotate the adjustable crank (11-4), and drive the test kettle (9) to rotate through the connecting shaft II (11-3). Turn the test kettle upside down so that the inclination angle of the test kettle is 120°, and measure the time it takes for the falling ball to reach the force sensitive sensor II (9-13). t , repeat this process to obtain multiple sets of data.

[0080] After the reaction is finished, stop heating and open the vent valve (9-7) to release the pressure. After the test kettle cools down, open the test kettle for cleaning. Calculate the fluid viscosity according to formula (1).

[0081] Implementation Case 8

[0082] like Figure 1 As shown, the material tank (1), the high-pressure metering pump (2), the one-way valve I (3), the carbon dioxide storage tank (4), the compressor (5), the one-way valve II (6), the high-pressure hose (7), the high-pressure hose II (8), and the test kettle (9) are connected in sequence, and the test kettle (9), the bracket (10), the electric crank system (11), and the constant temperature box (12) are installed.

[0083] Open the end cap (9-1), place the ball (9-3) into the kettle chamber (9-6) near the upper end of the end cap, close the upper end needle valve (9-4) to hold the ball (9-3), keep the lower end needle valve (9-8) in an open state, insert an O-ring (9-2) for sealing, and connect the end cap (9-1) to the kettle body (9-9) through the connecting bolt (9-14); open the carbon dioxide storage tank (1), the one-way valve I (3) and the vent valve (9-7), and close the vent valve after the device is completely filled with carbon dioxide. 9-7), open the high-pressure metering pump (2), the compressor (5) and the one-way valve II (6), so that the paint and the carbon dioxide enter the jet mixer (9-5) for primary mixing, and at the same time start the motor (11-6) of the electric crank to drive the connecting shaft III (11-5) to rotate, so that the adjustable crank (11-4) rotates, and the fixed-length crank (11-2) drives the test kettle (8) to shake up and down through the connecting shaft II (11-3), so that the paint and the carbon dioxide are mixed for a second time in the test kettle (9).

[0084] like Fig. 9 , define the angle between the connection surface of the test kettle and the vertical plane as the inclination angle α. After the pressure reaches 100MPa, turn off the air compressor, and then turn on the air compressor indirectly to keep the pressure at 100MPa. Turn on the power of the thermostat to make the temperature in the test kettle (8) reach 200℃. After the temperature and pressure are stable, adjust the length of the adjustable crank (11-4) to make the inclination angle of the test kettle 30°, open the upper needle valve (9-4), and measure the time it takes for the falling ball to reach the force sensitive sensor I (9-10). t .

[0085] Close the lower needle valve (9-8), start the motor (11-6) of the electric crank system, drive the connecting shaft II (11-5) to rotate, rotate the adjustable crank (11-4), and drive the test kettle (9) to rotate through the connecting shaft II (11-3). Turn the test kettle upside down so that the inclination angle of the test kettle is 150°, and measure the time it takes for the falling ball to reach the force sensitive sensor II (9-13). t , repeat this process to obtain multiple sets of data.

[0086] After the reaction is finished, stop heating and open the vent valve (9-7) to release the pressure. After the test kettle cools down, open the test kettle for cleaning. Calculate the fluid viscosity according to formula (1).

[0087] Implementation Case 9

[0088] like Figure 1As shown, the material tank (1), the high-pressure metering pump (2), the one-way valve I (3), the carbon dioxide storage tank (4), the compressor (5), the one-way valve II (6), the high-pressure hose (7), the high-pressure hose II (8), and the test kettle (9) are connected in sequence, and the test kettle (9), the bracket (10), the electric crank system (11), and the constant temperature box (12) are installed.

[0089] Open the end cap (9-1), place the ball (9-3) into the kettle chamber (9-6) near the upper end of the end cap, close the upper end needle valve (9-4) to hold the ball (9-3), keep the lower end needle valve (9-8) in an open state, insert an O-ring (9-2) for sealing, and connect the end cap (9-1) to the kettle body (9-9) through the connecting bolt (9-14); open the carbon dioxide storage tank (1), the one-way valve I (3) and the vent valve (9-7), and close the vent valve after the device is completely filled with carbon dioxide. 9-7), open the high-pressure metering pump (2), the compressor (5) and the one-way valve II (6), so that the paint and the carbon dioxide enter the jet mixer (9-5) for primary mixing, and at the same time start the motor (11-6) of the electric crank to drive the connecting shaft III (11-5) to rotate, so that the adjustable crank (11-4) rotates, and the fixed-length crank (11-2) drives the test kettle (8) to shake up and down through the connecting shaft II (11-3), so that the paint and the carbon dioxide are mixed for a second time in the test kettle (9).

[0090] like Fig. 9 , define the angle between the connection surface of the test kettle and the vertical plane as the inclination angle α. After the pressure reaches 100MPa, turn off the air compressor, and then turn on the air compressor indirectly to keep the pressure at 100MPa. Turn on the power of the thermostat to make the temperature in the test kettle (8) reach 200℃. After the temperature and pressure are stable, adjust the length of the adjustable crank (11-4) to make the inclination angle of the test kettle 45°, open the upper needle valve (9-4), and measure the time it takes for the falling ball to reach the force sensitive sensor I (9-10). t .

[0091] Close the lower needle valve (9-8), start the motor (11-6) of the electric crank system, drive the connecting shaft II (11-5) to rotate, rotate the adjustable crank (11-4), and drive the test kettle (9) to rotate through the connecting shaft II (11-3). Turn the test kettle upside down so that the inclination angle of the test kettle is 135°, and measure the time it takes for the falling ball to reach the force sensitive sensor II (9-13). t , repeat this process to obtain multiple sets of data.

[0092] After the reaction is finished, stop heating and open the vent valve (9-7) to release the pressure. After the test kettle cools down, open the test kettle for cleaning. Calculate the fluid viscosity according to formula (1).

[0093] Implementation Case 10

[0094] like Figure 1 As shown, the material tank (1), the high-pressure metering pump (2), the one-way valve I (3), the carbon dioxide storage tank (4), the compressor (5), the one-way valve II (6), the high-pressure hose (7), the high-pressure hose II (8), and the test kettle (9) are connected in sequence, and the test kettle (9), the bracket (10), the electric crank system (11), and the constant temperature box (12) are installed.

[0095] Open the end cap (9-1), place the ball (9-3) into the kettle chamber (9-6) near the upper end of the end cap, close the upper end needle valve (9-4) to hold the ball (9-3), keep the lower end needle valve (9-8) in an open state, insert an O-ring (9-2) for sealing, and connect the end cap (9-1) to the kettle body (9-9) through the connecting bolt (9-14); open the carbon dioxide storage tank (1), the one-way valve I (3) and the vent valve (9-7), and close the vent valve after the device is completely filled with carbon dioxide. 9-7), open the high-pressure metering pump (2), the compressor (5) and the one-way valve II (6), so that the paint and the carbon dioxide enter the jet mixer (9-5) for primary mixing, and at the same time start the motor (11-6) of the electric crank to drive the connecting shaft III (11-5) to rotate, so that the adjustable crank (11-4) rotates, and the fixed-length crank (11-2) drives the test kettle (8) to shake up and down through the connecting shaft II (11-3), so that the paint and the carbon dioxide are mixed for a second time in the test kettle (9).

[0096] like Fig. 9 , define the angle between the connection surface of the test kettle and the vertical plane as the inclination angle α. After the pressure reaches 50MPa, turn off the air compressor, and then indirectly turn on the air compressor to keep the pressure at 50MPa. Turn on the power of the thermostat to make the temperature in the test kettle (8) reach 200℃. After the temperature and pressure are stable, adjust the length of the adjustable crank (11-4) to make the inclination angle of the test kettle 45°, open the upper needle valve (9-4), and measure the time it takes for the falling ball to reach the force sensitive sensor I (9-10). t .

[0097] Close the lower needle valve (9-8), start the motor (11-6) of the electric crank system, drive the connecting shaft II (11-5) to rotate, rotate the adjustable crank (11-4), and drive the test kettle (9) to rotate through the connecting shaft II (11-3). Turn the test kettle upside down so that the inclination angle of the test kettle is 135°, and measure the time it takes for the falling ball to reach the force sensitive sensor II (9-13). t , repeat this process to obtain multiple sets of data.

[0098] After the reaction is finished, stop heating and open the vent valve (9-7) to release the pressure. After the test kettle cools down, open the test kettle for cleaning. Calculate the fluid viscosity according to formula (1).

Claims

1. A supercritical carbon dioxide system viscosity tester, characterized in that: The invention comprises a feeding system and a testing system, wherein the feeding system comprises a material tank (1), a high-pressure metering pump (2), a one-way valve I (3), a carbon dioxide storage tank (4), a compressor (5), a one-way valve II (6), a high-pressure hose I (7) and a high-pressure hose II (8), wherein the material tank (1), the high-pressure metering pump (2) and the one-way valve I (3) are sequentially connected and communicated with the testing system through the high-pressure hose I (7), and the carbon dioxide storage tank (4), the compressor (5) and the one-way valve II (6) are sequentially connected and communicated with the testing system through the high-pressure hose II (8); the testing system comprises a testing kettle (9), a bracket (10), an electric crank system (11) and a constant temperature box (12), wherein the testing kettle (9) is supported by the bracket (10) and can rotate around a fulcrum, wherein one end of the electric crank system (11) is connected to the upper end or the lower end of the testing kettle (9), and the electric crank system (11) is used to control the tilt angle of the testing kettle (9), and the testing kettle (9), the bracket (10) and the electric crank system (11) are placed in the constant temperature box (12); The test kettle comprises a kettle body (9-9) and a kettle cavity (9-6), and also comprises a head (9-1), an O-ring (9-2), a drop ball (9-3), an upper needle valve (9-4), a jet mixer (9-5), a vent valve (9-7), a lower needle valve (9-8), a force sensitive sensor I (9-10), a temperature gauge (9-11), a pressure gauge (9-12), a force sensitive sensor II (9-13), and connecting bolts (9-14), wherein the head (9-1) and the kettle body (9-9) are connected by connecting bolts (9-14) and The O-ring (9-2) is sealed and connected, the jet mixer (9-5) is installed on the outer wall of the test kettle through a flange and is connected to the kettle chamber (9-6), the force sensitive sensor I (9-10) and the force sensitive sensor II (9-13) are respectively arranged at the upper and lower ends of the kettle chamber (9-6), the falling ball (9-3) is placed in the kettle chamber (9-6), the upper needle valve (9-4) and the lower needle valve (9-8) are respectively arranged at the upper part and the lower part of the kettle chamber (9-6), and the upper needle valve (9-4) and the lower needle valve (9-8) are used to block or release the falling ball (9-3); The electric crank system comprises a connecting bearing I (11-1), a fixed-length crank (11-2), a connecting bearing II (11-3), an adjustable crank (11-4), a connecting bearing III (11-5) and a motor (11-6); the fixed-length crank (11-2) is connected to the test kettle (9) via the connecting bearing I (11-1); the adjustable crank (11-4) is a telescopic structure; the shorter the adjustable crank (11-4), the greater the inclination angle α of the test kettle The larger the adjustable crank (11-4), the more suitable it is for testing fluids with low viscosity; conversely, the longer the adjustable crank (11-4), the smaller the inclination angle α of the test kettle, and the more suitable it is for testing fluids with high viscosity. The fixed-length crank (11-2) and the adjustable crank (11-4) are connected via a connecting bearing II (11-3). The motor (11-6) is used to control the rotation of the adjustable crank (11-4). By controlling the length and rotation angle of the adjustable crank (11-4), the test kettle (9) is made to circulate or the test kettle (9) is made to be in different inclination states, thereby achieving full mixing of the supercritical carbon dioxide system and viscosity measurement.

2. The supercritical carbon dioxide system viscosity tester according to claim 1, characterized in that: The jet mixer comprises a nozzle (9-5-2), a tapered section (9-5-3), and a diffuser section (9-5-4) which are connected in sequence; a suction pipe (9-5-1) is provided on the side wall of the nozzle (9-5-2); and the suction pipe (9-5-1) is connected to the tapered section (9-5-3).

3. The supercritical carbon dioxide system viscosity tester according to claim 2, characterized in that: The one-way valve I (3) is connected to the suction pipe via a high-pressure hose I (7), and the one-way valve II (6) is connected to the nozzle via a high-pressure hose II (8).

4. The supercritical carbon dioxide system viscosity tester according to claim 1, characterized in that: The kettle body (9-9) test kettle is also provided with a vent valve (9-7) for releasing the pressure in the kettle cavity (9-6), a temperature gauge (9-11) and a pressure gauge (9-12) for testing physical indicators in the kettle cavity (9-6).

5. The supercritical carbon dioxide system viscosity tester according to claim 1, characterized in that: The support comprises a rotating bearing (10-1), a supporting rod (10-2), and a base (10-3); the rotating bearing (10-1) is connected to the test kettle (9).

6. The supercritical carbon dioxide system viscosity tester according to claim 1, characterized in that: The maximum pressure that the feeding system and the test kettle can withstand is 100 MPa, and the maximum temperature is 200°C.

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