CN112961717A - Method for quickly hydrating and separating gas hydrate based on phase-change micro-nano fluid - Google Patents
Method for quickly hydrating and separating gas hydrate based on phase-change micro-nano fluid Download PDFInfo
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- CN112961717A CN112961717A CN202110151545.2A CN202110151545A CN112961717A CN 112961717 A CN112961717 A CN 112961717A CN 202110151545 A CN202110151545 A CN 202110151545A CN 112961717 A CN112961717 A CN 112961717A
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- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10L—FUELS NOT OTHERWISE PROVIDED FOR; NATURAL GAS; SYNTHETIC NATURAL GAS OBTAINED BY PROCESSES NOT COVERED BY SUBCLASSES C10G, C10K; LIQUEFIED PETROLEUM GAS; ADDING MATERIALS TO FUELS OR FIRES TO REDUCE SMOKE OR UNDESIRABLE DEPOSITS OR TO FACILITATE SOOT REMOVAL; FIRELIGHTERS
- C10L3/00—Gaseous fuels; Natural gas; Synthetic natural gas obtained by processes not covered by subclass C10G, C10K; Liquefied petroleum gas
- C10L3/06—Natural gas; Synthetic natural gas obtained by processes not covered by C10G, C10K3/02 or C10K3/04
- C10L3/10—Working-up natural gas or synthetic natural gas
- C10L3/108—Production of gas hydrates
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Abstract
The invention relates to a method for quickly hydrating and separating gas hydrate based on phase-change micro-nano fluid, which comprises the following steps of: i, pouring a specified amount of target solution into a high-pressure reaction kettle; moving the clamper to change the distance between the magnetic steels to a specified distance; III, adjusting the temperature of the high-pressure reaction kettle to reach a preset temperature; IV, filling the gas into the high-pressure reaction kettle to reach a preset pressure; starting a control motor to enable a clamp holder to drive the magnetic steel to rotate around the high-pressure reaction kettle; the measured temperature and pressure data in the high-pressure reaction kettle are transmitted to a data collector through a temperature sensor and a pressure sensor, and then an industrial personal computer stores and processes the data; and VII, observing the reaction condition in the high-pressure reaction kettle through a visible transparent window, wherein the method has the advantages of enhancing the effect of gas hydration separation heat and mass transfer process and improving the generation effect of the hydrate by using the Ni-Mn-based phase-change micro-nano particles and combining the action of a rotating magnetic field.
Description
Technical Field
The invention relates to the technical field of gas separation and storage and transportation, in particular to a method for quickly hydrating and separating gas hydrate based on phase-change micro-nano fluid.
Background
At present, the development and utilization of coal mine gas are accelerated, and the method has important significance for ensuring the safe production of coal mines, increasing the supply of clean energy and reducing the emission of greenhouse gas. The gas hydration reaction separation process has the following two main processes:
1. constraints on heat transfer: since the formation of gas hydrates is an exothermic process, the heat generated during nucleation destroys the crystal nuclei, resulting in a slow growth of the crystal structure, in which heat transfer is a very important phenomenon. The hydrate has low heat conduction capability, and the heat generated by the hydrate cannot be effectively removed in time, so that the temperature of a gas hydration reaction system rises, and the gas hydration separation process is greatly weakened;
2. and (3) restriction of mass transfer: the gas and the water can not be fully contacted, and a plurality of multi-phase bodies form a plurality of phase interfaces, so that the mass transfer between gas phase and liquid phase in the system is seriously hindered, and the induction time is long and the hydrate generation rate is slow. The above problems result in long induction time, slow generation speed and large driving force of gas hydration reaction.
At present, the most mechanical strengthening method is to strengthen the generation of hydrate in a reaction kettle by stirring, the stirring mainly strengthens mass transfer and heat transfer, the liquid rotates along with blades, the gas-liquid contact area is increased, the gas dissolution efficiency is accelerated, and the heat generated by the generation of hydrate can be transferred in time. Further shortening the induction time of the hydrate, improving the generation rate, increasing the gas storage capacity and the like. The increase of stirring can increase the gas-liquid contact area, improve the gas hydration rate and ensure the fluid dispersibility. But the hydration reaction still stays at the gas-liquid interface, the induction time is not obviously shortened, and slight settlement and layering phenomena can be slightly generated in the kettle along with the increase of the experimental time, and the homogeneity is reduced although the particle suspension property can be met. In addition, the energy consumption of the system is increased by adding the blades for stirring, the system is not suitable for industrial production, and the danger of high-pressure gas leakage is increased by adding the stirring rotating shaft.
Therefore, in order to overcome the defects, a method for quickly hydrating and separating the gas hydrate based on the phase-change micro-nano fluid is needed.
Disclosure of Invention
Technical problem to be solved
The invention aims to solve the technical problem that the existing equipment has low gas hydration reaction efficiency.
(II) technical scheme
In order to solve the technical problems, the invention provides a method for quickly hydrating and separating gas hydrate based on phase-change micro-nano fluid, which comprises the following steps,
i, pouring a specified amount of target solution into a high-pressure reaction kettle, and connecting various systems and pipelines;
rotating the hand wheel to move the clamp holder, so that the distance between the magnetic steels is changed to a specified distance;
opening a constant temperature box to adjust the temperature of the high-pressure reaction kettle to reach a preset temperature;
IV, opening an air compressor, a gas booster pump and a valve, and filling gas in a gas cylinder and a gas storage tank into the high-pressure reaction kettle to reach a preset pressure;
closing the valve, starting a control motor to enable an electric rotating platform to drive a linear sliding table to rotate, driving the magnetic steel to rotate around the high-pressure reaction kettle by the clamp holder, and stirring a target solution containing magnetic particles through magnetic force;
the measured temperature and pressure data in the high-pressure reaction kettle are transmitted to a data collector through a temperature sensor and a pressure sensor, and then an industrial personal computer stores and processes the data;
and VII, observing the reaction condition in the high-pressure reaction kettle through a visible transparent window, and monitoring the hydration reaction process by combining temperature and pressure data.
As a further explanation of the present invention, it is preferable that the target solution contains Ni — Mn based phase-change micro-nano particles.
As a further explanation of the invention, the high-pressure reaction kettle is preferably made of titanium alloy material, the pressure variation range in the high-pressure reaction kettle is 0-10 MPa, and the temperature variation range in the high-pressure reaction kettle is-20-50 ℃.
As a further explanation of the invention, preferably, the variation range of the magnetic steel spacing is 0-230 mm, and the intensity range of the magnetic field generated by the magnetic steel is 0-0.33T.
As a further description of the present invention, preferably, the air compressor is started after being connected to a 380V power supply, air drawn in from the air cylinder passes through a filter in the air compressor, is converted into compressed air through reciprocating motion of a piston in the air compressor, and finally enters the air storage tank for storage, and when the high-pressure reaction kettle needs to be pressurized, a valve between the high-pressure reaction kettle and the air storage tank is opened.
As a further explanation of the present invention, it is preferable that the gas booster pump is not required to be turned on when the output pressure of the air compressor reaches the desired pressure value.
(III) advantageous effects
The technical scheme of the invention has the following advantages: (connection relationship)
The phase-change micro-nano fluid replaces a single liquid phase, and the characteristics of high thermal conductivity and phase change heat absorption of the phase-change micro-nano fluid are fully utilized, so that the multi-gas hydration reaction process is remarkably improved, and the gas hydration separation process is strengthened. The phase-change micro-nano fluid has the characteristics of high specific surface area, active Brownian motion, small size, controllable concentration and the like, and can provide more active sites for the nucleation process of the hydrate. Therefore, the phase-change micro-nano fluid can well promote the heat transfer and mass transfer processes of gas hydration separation and strengthen the gas hydration separation process.
Drawings
FIG. 1 is a system diagram of a reaction apparatus of the present invention;
FIG. 2 is a sectional view of a reaction vessel according to the present invention.
In the figure: 1. an electric rotating table; 2. a linear sliding table; 21. a hand wheel; 3. a holder; 4. magnetic steel; 5. a high-pressure reaction kettle; 51. a temperature sensor; 52. a pressure sensor; 53. a visible transparent window; 6. a thermostat; 7. an air compressor; 71. a gas cylinder; 72. a gas storage tank; 73. a gas booster pump; 74. a valve; 8. an industrial personal computer; 81. a data acquisition unit; 82. and controlling the motor.
Detailed Description
In order to make the objects, technical solutions and advantages of the embodiments of the present invention clearer, the technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are some, but not all, embodiments of the present invention. All other embodiments, which can be obtained by a person skilled in the art without any inventive step based on the embodiments of the present invention, are within the scope of the present invention.
A method for quickly hydrating and separating gas hydrate based on phase-change micro-nano fluid is shown in figure 1 and comprises the following steps,
i, pouring 0-100ml of target solution into a high-pressure reaction kettle 5, wherein 40ml of target solution can be selected generally, and the target solution contains Ni-Mn-based phase-change micro-nano particles and a dispersing agent and is connected with various systems and pipelines. Each system includes reaction system, pneumatic system and test system, reaction system includes electric rotating table 1, a word slip table 2, holder 3, magnet steel 4, high-pressure batch autoclave 5 and thermostated container 6, electric rotating table 1 erects in thermostated container 6, a word slip table 2 rotates to be connected on electric rotating table 1, 3 sliding connection of two holders are on 2 upper portions of a word slip table, two holder 3 distribute on the same diameter line, magnet steel 4 links firmly in holder 3, high-pressure batch autoclave 5 places in thermostated container 6, high-pressure batch autoclave 5 is located between two holders 3 and the rotation axis coincidence of 5 axes of high-pressure batch autoclave and a word slip table 2. Referring to fig. 2, the high-pressure reaction kettle 5 is made of titanium alloy material, the pressure variation range in the high-pressure reaction kettle 5 is 0-10 MPa, the rated temperature range of the high-pressure reaction kettle 5 is-20-50 ℃, and a visible transparent window 53 is fixedly connected in the high-pressure reaction kettle 5, so that an experimenter can observe the reaction condition in the high-pressure reaction kettle 5.
The pneumatic system comprises an air compressor 7, an air bottle 71, an air storage tank 72 and a gas booster pump 73, the pneumatic system is erected outside the constant temperature box 6, the air bottle 71 is connected with the air inlet end of the air compressor 7 through a pipeline, the air outlet end of the air compressor 7 is connected with the air inlet end of the air storage tank 72 through a pipeline, the air outlet end of the air storage tank 72 is connected with the air inlet end of the gas booster pump 73, and the air outlet end of the gas booster pump 73 is connected with the high-pressure reaction kettle 5 through a pipeline. Valves 74 are respectively arranged on a pipeline between the air bottle 71 and the air compressor 7, a pipeline between the air compressor 7 and the air storage tank 72, and a pipeline between the gas booster pump 73 and the high-pressure reaction kettle 5, and the valves 74 are electromagnetic valves.
The test system comprises a temperature sensor 51, a pressure sensor 52, an industrial personal computer 8, a data collector 81 and a control motor 82, the temperature sensor 51 and the pressure sensor 52 are all placed in the high-pressure reaction kettle 5, the industrial personal computer 8, the data collector 81 and the control motor 82 are all placed outside a constant temperature box 6, wherein the temperature sensor 51 and the pressure sensor 52 are all electrically connected with the data collector 81 through electric leads, the data collector 81 is electrically connected with the industrial personal computer 8 through electric leads, the industrial personal computer 8 is electrically connected with the control motor 82 through electric leads, and the control motor 82 is electrically connected with the electric rotary table 1 through electric leads.
II, the clamp holder 3 is moved by rotating the hand wheel 21 on the linear sliding table 2, so that the distance between the magnetic steels 4 is changed to a specified distance, generally, the change range of the distance between the magnetic steels 4 is 0-230 mm, the strength range of the magnetic field generated by the magnetic steels 4 is 0-0.33T, and the size of the magnetic field strength can be controlled by adjusting the change of the distance between the magnetic steels 4.
And III, opening a constant temperature box 6 to adjust the temperature of the high-pressure reaction kettle 5 to reach a preset temperature, wherein different preset temperatures are required to be set for different experimental systems.
And IV, the air compressor 7 is started to operate after being connected with a 380V power supply, air sucked from the air bottle 71 firstly passes through a filter in the air compressor 7, then is converted into compressed air through the reciprocating motion of a piston in the air compressor 7, and finally enters the air storage tank 72 for storage. When the high-pressure reaction kettle 5 needs to be pressurized, the valve 2 between the high-pressure reaction kettle 5 and the gas storage tank 72 is opened, so that the gas can be filled into the high-pressure reaction kettle 5 to reach the preset pressure; when the output pressure of the air compressor 7 can reach the required air pressure value, the gas booster pump 73 does not need to be started subsequently.
And V, closing the valve 74, starting the control motor 11 to enable the electric rotating platform 1 to drive the linear sliding table 2 to rotate, wherein the rotating speed range needs to be 0-200 r/min, at the moment, the clamp holder 3 drives the magnetic steel 4 to rotate around the high-pressure reaction kettle 5, and the target solution containing the magnetic particles is stirred through magnetic force.
And VI, transmitting the measured temperature and pressure data in the high-pressure reaction kettle 5 into a data acquisition unit 81 through a temperature sensor 51 and a pressure sensor 52, and then storing and processing the data by an industrial personal computer 8.
And VII, observing the reaction condition in the high-pressure reaction kettle 5 through a visible transparent window 53, and monitoring the hydration reaction process by combining temperature and pressure data. Wherein the hydrate can be judged to start reacting when the temperature starts to rise significantly.
By adopting the method, the characteristics of high thermal conductivity and phase change heat absorption of the phase change type micro-nano fluid are fully utilized, and the Ni-Mn based phase change type micro-nano particles with martensite phase change are adopted, so that external heat can be absorbed when phase change occurs, the environmental temperature is reduced, heat generated in the hydrate generation process is taken away in time, and heat transfer in the gas hydration separation process is enhanced. And based on the magnetic characteristic of Ni-Mn based phase-change micro-nano fluid, the external rotating magnetic field additionally realizes the suspension stirring of the target, because the micro-nano fluid has the characteristics of high specific surface area (the heat exchange area between particles and the fluid is increased, the heat transfer is accelerated, more reaction interfaces are provided, the nucleation rate is improved), Brownian motion activity (the particles collide with each other in a gas-liquid boundary layer due to Brownian motion, the thickness of a mass transfer boundary layer is reduced, the mechanical property of surrounding liquid phase fluid can be changed), small size (the size of the suspended particles is smaller than the thickness of the gas-liquid mass transfer boundary layer, the particles can pass through the gas-liquid boundary layer to the gas-liquid interface to adsorb gas-liquid molecules and then return to a liquid-phase main body under the action of osmosis to achieve the purpose of gas transportation), controllable concentration and the like, the mass transfer process of gas, the induction time is greatly shortened.
In addition, the effect object of peripheral hardware rotating magnetic field is micro-nano granule itself, and not drives the magnetic stirrer through magnetic field and stir, and can adjust rotating magnetic field's rotational speed size through control motor 82, also can control the distance of magnetic field to high pressure batch autoclave 5 through a word slip table 2, thereby change the intensity size in the magnetic field that receives in high pressure batch autoclave 5, and then can realize prolonging hydrate granule suspension time, shorten induction time, effectively improve the effect of the synthetic efficiency of hydrate. The problems associated with conventional mixers are likewise avoided.
Finally, it should be noted that: the above examples are only intended to illustrate the technical solution of the present invention, but not to limit it; although the present invention has been described in detail with reference to the foregoing embodiments, it will be understood by those of ordinary skill in the art that: the technical solutions described in the foregoing embodiments may still be modified, or some technical features may be equivalently replaced; and such modifications or substitutions do not depart from the spirit and scope of the corresponding technical solutions of the embodiments of the present invention.
Claims (6)
1. The method for quickly hydrating and separating the gas hydrate based on the phase-change micro-nano fluid is characterized by comprising the following steps of: comprises the following steps of (a) carrying out,
i, pouring a specified amount of target solution into a high-pressure reaction kettle (5), and connecting various systems and pipelines;
II, moving the clamp holder (3) by rotating the hand wheel (21), and further changing the distance between the magnetic steels (4) to a specified distance;
opening a constant temperature box (6) to adjust the temperature of the high-pressure reaction kettle (5) to reach a preset temperature;
IV, starting an air compressor (7), a gas booster pump (73) and a valve (74), and filling gas in a gas cylinder (71) and a gas storage tank (72) into the high-pressure reaction kettle (5) to reach a preset pressure;
v, closing the valve (74), starting the control motor (82) to enable the electric rotating platform (1) to drive the linear sliding table (2) to rotate, driving the magnetic steel (4) to rotate around the high-pressure reaction kettle (5) by the clamp holder (3), and stirring a target solution containing magnetic particles through magnetic force;
the measured temperature and pressure data in the high-pressure reaction kettle (5) are transmitted to a data collector (81) through a temperature sensor (51) and a pressure sensor (52), and then an industrial personal computer (13) stores and processes the data;
and VII, observing the reaction condition in the high-pressure reaction kettle (5) through a visible transparent window (53), and monitoring the hydration reaction process by combining temperature and pressure data.
2. The method for rapidly hydrating and separating the gas hydrate based on the phase-change micro-nano fluid according to claim 1, wherein the method comprises the following steps: the target solution contains Ni-Mn-based phase-change micro-nano particles.
3. The method for rapidly hydrating and separating the gas hydrate based on the phase-change micro-nano fluid according to claim 1, wherein the method comprises the following steps: the high-pressure reaction kettle (5) is made of titanium alloy materials which do not influence a magnetic field, the pressure change range in the high-pressure reaction kettle (5) is 0-10 MPa, and the temperature change range in the high-pressure reaction kettle (5) is-20-50 ℃.
4. The method for rapidly hydrating and separating the gas hydrate based on the phase-change micro-nano fluid according to claim 1, wherein the method comprises the following steps: the change range of the distance between the magnetic steels (4) is 0-230 mm, and the strength range of the magnetic field generated by the magnetic steels (4) is 0-0.33T.
5. The method for rapidly hydrating and separating the gas hydrate based on the phase-change micro-nano fluid according to claim 1, wherein the method comprises the following steps: the air compressor (7) is started to operate after being connected with a 380V power supply, air sucked from the air bottle (71) firstly passes through a filter in the air compressor (7), then is converted into compressed air through reciprocating motion of a piston in the air compressor (7), finally enters the air storage tank (72) for storage, and when the high-pressure reaction kettle (5) needs to be pressurized, a valve (74) between the high-pressure reaction kettle (5) and the air storage tank (72) is opened.
6. The method for rapidly hydrating and separating the gas hydrate based on the phase-change micro-nano fluid according to claim 5, wherein the method comprises the following steps: when the output pressure of the air compressor (7) reaches the required air pressure value, the air booster pump (73) does not need to be started.
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2021
- 2021-02-03 CN CN202110151545.2A patent/CN112961717A/en active Pending
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| CN101055777A (en) * | 2007-03-08 | 2007-10-17 | 中国科学院物理研究所 | Magnetic material with the magnetic field driving martensite phase change effect and its making method |
| EP2339595A1 (en) * | 2009-12-14 | 2011-06-29 | Eto Magnetic Gmbh | Magnetic shape memory alloy material |
| US20140287110A1 (en) * | 2013-03-14 | 2014-09-25 | Persedo LLC | Hybrid Technique for the Conversion/Removal of Contaminants in Alcohol-Water or Like Medium |
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