CN-121972041-A - Liquid carbon dioxide ultrasonic emulsification equipment, emulsification method thereof and quantitative characterization method of demulsification process of liquid carbon dioxide ultrasonic emulsification equipment

CN121972041ACN 121972041 ACN121972041 ACN 121972041ACN-121972041-A

Abstract

The application relates to the technical field of emulsification, in particular to liquid carbon dioxide ultrasonic emulsification equipment, an emulsification method thereof and a quantitative characterization method of a demulsification process thereof, which comprises a reaction kettle device, a high-pressure sealing flange ring, an ultrasonic device and a control system; the reaction kettle device comprises a reaction kettle, a temperature module, a pressure module and a window module, wherein the reaction kettle contains a mixed solution of a surfactant and liquid carbon dioxide, the temperature module regulates the temperature, the pressure module regulates the pressure, the window module shows the morphology of the mixed solution, the ultrasonic device enables the mixed solution to be emulsified into carbon dioxide/water emulsion, the control system comprises an image module, a control module and a processing module, the image module acquires emulsion morphology images through the window module, the processing module analyzes the emulsification effect according to the images, the control module controls emulsification parameters according to the emulsification effect, and the emulsification parameters comprise the temperature and the pressure of the reaction kettle and the power and the frequency of the ultrasonic device. The device can realize intelligent feedback regulation and control of the emulsification process.

Inventors

YIN ZHENYUAN
SUN JIAYU
LIU XUEJIAN

Assignees

清华大学深圳国际研究生院

Dates

Publication Date: 20260505
Application Date: 20260324

Claims (10)

1. The liquid carbon dioxide ultrasonic emulsification equipment is characterized by comprising a reaction kettle device, a high-pressure sealing flange ring, an ultrasonic device and a control system; the reaction kettle device comprises a reaction kettle, a temperature module, a pressure module and a window module, wherein the reaction kettle is configured to contain a mixed solution containing a surfactant solution and liquid carbon dioxide, the temperature module is configured to adjust the temperature of the reaction kettle, the pressure module is configured to adjust the pressure of the reaction kettle, and the window module is configured to be installed on the wall surface of the reaction kettle, so that the window module shows the shape of the mixed solution; The ultrasonic device is at least partially arranged in the reaction kettle and is configured to be contacted with the mixed solution, and the ultrasonic device is configured to output mechanical vibration to emulsify the mixed solution into carbon dioxide/water emulsion; The control system comprises an image module, a control module and a processing module, wherein the image module is configured to acquire an image of the appearance of the carbon dioxide/water emulsion obtained by emulsifying the mixed solution through the window module, the processing module is configured to analyze the emulsifying effect of the carbon dioxide/water emulsion according to the image, the control module is configured to control emulsifying parameters according to the emulsifying effect, and the emulsifying parameters at least comprise the temperature and the pressure of the reaction kettle and the power and the frequency of the ultrasonic device.
2. The liquid carbon dioxide phacoemulsification machine of claim 1, wherein the ultrasonic device comprises a housing and an ultrasonic transducer and an ultrasonic horn at least partially housed within the housing, the ultrasonic horn being provided with an ultrasonic tool head; The ultrasonic transducer is configured to output mechanical vibration, at least part of the ultrasonic amplitude transformer is arranged in the reaction kettle and is in contact with the mixed solution, the ultrasonic amplitude transformer is configured to amplify the amplitude of the mechanical vibration, and the ultrasonic tool head is configured to receive the mechanical vibration and transmit the mechanical vibration to the mixed solution.
3. The liquid carbon dioxide phacoemulsification machine of claim 2, wherein the ultrasonic device includes at least one of the following features: (1) The frequency of the ultrasonic transducer is 20 kHz-60 kHz, the power is 500W-3000W, and the power adjusting range is 1% -99%; (2) The ultrasonic amplitude transformer is of a stepped variable diameter structure, and is designed by lambda/2 resonance; (3) The length of the ultrasonic amplitude transformer in the reaction kettle is 63 mm or 190 mm.
4. The liquid carbon dioxide phacoemulsification machine of claim 1, wherein the reaction vessel means includes at least one of the following features: (1) The material of the reaction kettle comprises stainless steel; (2) The roughness Ra of the inner wall surface of the reaction kettle is less than or equal to 0.4 mu m; (3) The outer wall of the reaction kettle comprises a carbon steel heat-insulating layer; (4) The temperature module comprises an embedded heating wire.
5. The liquid carbon dioxide phacoemulsification machine of claim 1, wherein the window module includes a sapphire window, a titanium alloy sealing flange, and a metal wrap gasket; the sapphire window is installed on the wall surface of the reaction kettle through the titanium alloy sealing flange, the metal winding gasket is installed between the sapphire window and the reaction kettle, and the metal winding gasket is configured to seal a gap between the sapphire window and the reaction kettle.
6. The liquid carbon dioxide phacoemulsification machine of claim 5, wherein the sapphire window has a thickness of 10 mm-15 mm.
7. The liquid carbon dioxide phacoemulsification device of claim 1, wherein the surfactant comprises at least one of a nonionic surfactant, an anionic surfactant, or a cationic surfactant.
8. The liquid carbon dioxide ultrasonic emulsification device according to claim 1, wherein the reaction kettle is further provided with a temperature sensor, a pressure sensor and an illumination system, and the control module is electrically connected with the temperature sensor, the pressure sensor and the illumination system; The temperature sensor is configured to detect the temperature of the reaction kettle, the pressure sensor is configured to detect the pressure of the reaction kettle, the control module is configured to control the temperature and the pressure of the reaction kettle and the power and the frequency of the ultrasonic device according to the temperature result of the temperature sensor and the pressure result of the pressure sensor, so that the ultrasonic device is configured to output mechanical vibration under preset conditions, the lighting system is configured to provide a light source in the reaction kettle, wherein the preset conditions comprise that the demulsification interval of the carbon dioxide/water emulsion is more than 7 h or the volume ratio of the carbon dioxide/water emulsion is less than 80 percent based on the volume of the reaction kettle.
9. An emulsification method based on liquid carbon dioxide ultrasonic emulsification equipment is characterized by comprising the following steps: injecting surfactant solution and liquid carbon dioxide into a reaction kettle, and installing an ultrasonic device on the reaction kettle to enable the ultrasonic device to be in contact with the mixed solution; Setting the temperature and the pressure of a reaction kettle and the power and the frequency of an ultrasonic device, starting the ultrasonic device, emulsifying the mixed solution, and recording the temperature and the pressure of the reaction kettle and the frequency and the power of the ultrasonic device in the emulsifying process; Collecting an image of the appearance of the carbon dioxide/water emulsion in the emulsification process, analyzing the emulsification effect of the carbon dioxide/water emulsion according to the image, adjusting the power of the ultrasonic device, observing the change of the emulsification effect, and analyzing the optimal power range according to the change of the emulsification effect; Changing the temperature of the reaction kettle based on the optimal power range, re-collecting an image of the appearance of the carbon dioxide/water emulsion after the temperature change, and analyzing the influence of the temperature on the emulsification effect of the carbon dioxide/water emulsion according to the image before and after the temperature change; Establishing a mapping relation between the morphology of the carbon dioxide/water emulsion and the temperature and pressure of the reaction kettle and the frequency and power of the ultrasonic device by combining images of the morphology of the carbon dioxide/water emulsion under different powers and temperatures through recorded temperature and pressure of the reaction kettle and frequency and power of the ultrasonic device; Based on the mapping relation, analyzing the temperature and pressure of the reaction kettle and the emulsification effect generated by the combination of the frequency and the power of the ultrasonic device, and determining the optimal temperature and pressure of the reaction kettle and the optimal combination of the frequency and the power of the ultrasonic device.
10. The quantitative characterization method of the demulsification process based on the liquid carbon dioxide ultrasonic emulsification equipment is characterized by comprising the following steps of: Starting an ultrasonic device, emulsifying a carbon dioxide/water emulsion, entering a demulsification process, obtaining data capable of reflecting the phase change of the emulsion system, and determining a group of demulsification dynamics characteristic time parameters t d based on the data, wherein t ds is demulsification starting time, which indicates that a stable phase boundary is formed between a disperse phase and a continuous phase in the emulsion system for the first time, namely, the time corresponding to the start of the demulsification process is indicated, t d10 、t d50 and t d90 are respectively the time corresponding to the time when the demulsification volume of the emulsion reaches 10%, 50% and 90% of the total volume of the initial emulsion, and t dc is demulsification completion time, which indicates that the demulsification process of the emulsion is ended, the system state tends to be stable along with the time, and the time corresponding to the time when the demulsification volume of the emulsion no longer changes significantly; And quantitatively analyzing the demulsification process of the carbon dioxide/water emulsion based on the demulsification dynamic characteristic time parameter t d so as to characterize the stability and demulsification dynamic characteristics of the carbon dioxide/water emulsion system.

Description

Liquid carbon dioxide ultrasonic emulsification equipment, emulsification method thereof and quantitative characterization method of demulsification process of liquid carbon dioxide ultrasonic emulsification equipment Technical Field The application relates to the technical field of emulsification, in particular to liquid carbon dioxide ultrasonic emulsification equipment, an emulsification method thereof and a quantitative characterization method of a demulsification process thereof. Background The hydrate method CO 2 sealing technology is one of key means for coping with challenges such as greenhouse effect exacerbation and extreme climate frequency, utilizes the characteristic of forming solid CO 2 hydrate in a deep sea environment, has the advantages of high gas storage density, strong stability, low leakage risk and the like, and becomes one of the most promising ocean CO 2 sealing schemes. However, the existing hydrate method is still faced with two major core challenges when being practically applied, namely, the injection efficiency is low, the prior art is mainly dependent on mechanical injection, the injection mode is limited by the pore structure, wettability and interfacial tension of the submarine sediment, the permeability is poor, sediment space is difficult to fully utilize, if a chemical accelerator is adopted to improve the injection efficiency, environmental risks can be caused, the hydrate conversion rate is low, the generation of hydrate can be inhibited in a submarine high-salt environment (salinity is about 3.5 wt%), and the uncertainty of the nucleation and growth process of the hydrate can be further aggravated by multi-factor coupling of temperature, pressure and fluid composition, and the hydrate conversion rate is reduced. Disclosure of Invention In view of the above, the present application provides a liquid carbon dioxide ultrasonic emulsification device, an emulsification method thereof, and a quantitative characterization method of a demulsification process thereof, which can solve at least one of the above-mentioned technical problems. The application provides liquid carbon dioxide ultrasonic emulsification equipment, which comprises a reaction kettle device, a high-pressure sealing flange ring, an ultrasonic device and a control system, wherein the reaction kettle device comprises a reaction kettle, a temperature module, a pressure module and a window module, the reaction kettle is configured to contain a mixed solution containing surfactant solution and liquid carbon dioxide, the temperature module is configured to regulate the temperature of the reaction kettle, the pressure module is configured to regulate the pressure of the reaction kettle, the window module is configured to be installed on the wall surface of the reaction kettle, the window module is enabled to show the appearance of the mixed solution, the ultrasonic device is at least partially arranged in the reaction kettle and is configured to be in contact with the mixed solution, the ultrasonic device is configured to output mechanical vibration, the mixed solution is emulsified into carbon dioxide/water emulsion, the high-pressure sealing flange ring seals a gap between the reaction kettle device and the ultrasonic device, the control system comprises an image module, the control module and a processing module, the image module is configured to be installed on the wall surface of the reaction kettle, the window module is enabled to show the appearance of the mixed solution, the ultrasonic device is configured to obtain the emulsifying effect of the carbon dioxide emulsion by at least one of the image and the water emulsion by the image processing device is configured to obtain the emulsifying effect according to at least one of the image and the image emulsifying effect. The ultrasonic device is integrated on the reaction kettle through the high-pressure sealing flange ring, so that the ultrasonic device can stably operate under the high-pressure condition of the reaction kettle, and in the emulsification process of the mixed solution, the ultrasonic device can efficiently disperse the mixed solution into micron-sized carbon dioxide/water emulsion, and the emulsification effect of the mixed solution is improved. the reaction kettle is provided with a window module, the window module provides an image acquisition window of the appearance of the carbon dioxide/water emulsion for the image module, and the window module is matched with the image analysis and processing module of the control module to adjust the emulsification parameters, so that a highly dispersed micro-droplet structure is formed in a water phase by liquid CO 2 in the system, the contact area of CO 2 and water is obviously increased, the optimal dynamic condition is provided for converting the carbon dioxide/water emulsion into CO 2 hydrate, the conversion efficiency of the CO 2 hydrate is improved, the membrane barrier of the CO 2 hydrate in t