CN103215098B - Preparation system and method of combustible ice - Google Patents
Preparation system and method of combustible ice Download PDFInfo
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- CN103215098B CN103215098B CN201310153913.2A CN201310153913A CN103215098B CN 103215098 B CN103215098 B CN 103215098B CN 201310153913 A CN201310153913 A CN 201310153913A CN 103215098 B CN103215098 B CN 103215098B
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Abstract
The invention relates to a preparation system and a preparation method of combustible ice. The preparation system comprises a synthesis subsystem, a water circulation subsystem and an extraction subsystem, wherein the prepared mixed liquid of distilled water and a surfactant is intruded into the synthesis subsystem by the water circulation subsystem; natural gas is introduced into the synthesis subsystem through a gas inlet pipe to generate combustible ice hydrate; and in the storage environment of the combustible ice, the extraction subsystem extracts combustible ice hydrate crystals after solid liquid separation through a vibrator. According to the reparation system and the preparation method of the combustible ice, the hydrate synthesis efficiency is high, the cost is low and extraction is convenient. Decomposition of natural gas hydrate during extraction is avoided, and important significance of performing physical and chemical form research on the combustible ice and realizing industrial production is achieved.
Description
Technical field
The present invention relates to a kind of preparation system and method for combustible ice, for automatically producing and extracting combustible ice.
Background technology
Sweet natural gas solid water compound is also called " combustible ice ", and being expected to becomes 21 century after the conventional oil and natural gas energy, first-selected clean energy.Gas hydrate have the features such as energy density is high, distribution is wide, scale is large, it is shallow to bury, one-tenth Tibetan physicochemical condition is superior, are the substitute energys of 21 century most DEVELOPMENT PROSPECT, in future source of energy structure, have important strategic position.1m
3the energy equivalence that combustible ice is contained is in 164m
3the calorific value of Sweet natural gas is huge super potential energy source.At present, the estimation that various countries expert is more consistent to the Sweet natural gas total amount in the whole world " combustible ice " is 2.0 × 10
16~ 2.1 × 10
16m
3, be equivalent to current 2 times of having verified the total carbon content of fossil oil, western scholar is called " the 21 century energy " or " future source of energy ".Scientist estimates, the distribution range of seabed " combustible ice " accounts for 10% of the ocean total area, is equivalent to 4,000 ten thousand km
2, be the Mineral resources of seabed most worthy up to now, enough mankind use 1000.
The exploitation of combustible ice is deep-sea shallow cut, and will drill at hundreds of rice deep-sea, technology and equipment must be very perfect, guarantee prospecting, extraction success and personal security.Concentrated and a large amount of exploitation combustible ice may destroy environments such as subsea and cause tsunami, or causes national fishing shelf upheaval even sea bed landslide.The main component of combustible ice is Sweet natural gas, it is a kind of gas of causing Greenhouse effect easier than carbonic acid gas, the usefulness of its Greenhouse effect is more than 20 times of the latter, once this leakage can not get controlling, Global Greenhouse Effect will increase rapidly, after atmosphere calefaction, seawater temperature also will increase, formation temperature rises, and will cause seabed combustible ice automatic classifying, cause vicious cycle.Therefore; the basic research such as natural gas hydrate phase balance emulation and microtexture is the most basic and most important advanced problems in natural gas hydrate exploration, exploitation and marine environmental protection research, has important reference role to the exploitation of gas hydrate new forms of energy.Because combustible ice exploitation difficulty is large, cost is high, still do not have sufficient natural combustible ice source to further investigate so far, and the generting machanism exploring artificial hydrate not only spends that fund is few, risk is low, and have theory value.
At present, relevant scholar has successfully explored the method for synthetic gas hydrate, and based on the generting machanism of gas hydrate, the physicochemical environment that simulation gas hydrate generate, obtains the combustible ice of synthetic.Combustible ice is formed under cryogenic high pressure condition, having departed from this environment will automatic classifying, prior art carries out the mixture separation of gas hydrate crystal and water under can only realizing normal temperature and pressure, and now gas hydrate major part has been decomposed, thus desirable gas hydrate crystal can not be obtained.Existing Natural Gas Hydrate Technology only can realize synthetic, and from instrument, effectively can not extract gas hydrate sample, constrains the work in everies such as combustible ice micro-structural test.Therefore, be necessary very much to invent a kind of level of automation high, easy to operate, safe and reliable, and the production of combustible ice can be realized and extract integration, the method keeping hydrate sample characteristics of for example completely and corollary apparatus.
Summary of the invention
Technical problem to be solved by this invention is to provide a kind of preparation system and method for combustible ice, and it can realize the production of combustible ice and extract integration, thus ensure that the sample characteristics of for example of finished product hydrate.
According to the preparation system of combustible ice of the present invention, comprise synthon system, water cycle subsystem and extract subsystem, it is characterized in that, utilize water cycle subsystem in synthon system, pass into the mixed solution of distilled water and the tensio-active agent prepared, and utilize admission passage in synthon system, to pass into Sweet natural gas to generate combustible ice hydrate, extract subsystem and extract the combustible ice hydrate crystal after solid-liquid separation by vibrator.
Preferably, synthon system mainly comprises high pressure visual reaction kettle, constant temperature circulator, vacuum unit, temperature and pressure transmitter and data collecting system, wherein constant temperature circulator is for controlling the temperature in reactor, constant temperature circulator, vacuum unit are all connected with reactor with temperature and pressure transmitter, and data collecting system can gather the pressure and temperature in reactor by temperature and pressure transmitter.
Preferably, water cycle subsystem mainly comprises reinforced beaker and recycle pump, wherein in reactor, injects mixed solution by reinforced beaker, is withdrawn in reinforced beaker by unnecessary mixed solution after end of synthesis by recycle pump.
Preferably, extract the main involving vibrations device of subsystem and holder, vibrator, for being peeled off from still wall by the hydrate crystal generated in still, imports holder under gravity; Further, when extracting subsystem work, temperature and pressure when utilizing constant temperature circulator, admission passage and temperature and pressure transmitter to monitor and control extraction, and controlled at combustible ice can in storage environment, to meet the requirement of combustible ice to storage environment.
According to a further aspect in the invention, relate to and utilize above-mentioned preparation system to prepare the method for combustible ice, comprise the following steps:
Step one: utilize vacuum pump to vacuumize the reactor and pipeline that clean up also precooling, open liquid phase valve, utilize vacuum to suck in still by the deionized-distilled water prepared and tensio-active agent mixed solution from reinforced beaker, close liquid phase valve;
Step 2: discharge in still by gas cylinder from reactor top by the Sweet natural gas controlled by pressure regulator valve after surge tank buffering, controls natural gas density in still by under meter and pressure transmitter and controls the pressure in reactor;
Step 3: open constant temperature circulator and regulate temperature in the kettle to design temperature scope and make still internal pressure be stabilized in setting pressure scope, allow gas hydrate nucleus generate completely;
Step 4: open still bottom outlet valve, by filter screen, surplus liquid in still is filtered out;
Step 5: rotate filter screen to open passage at the bottom of still, open vibrator, make the hydrate crystal that generates in still under gravity in reactor and filter screen peel off, enter holder by the outlet of reactor;
Step 6: after the whole discharging of hydrate of reaction generation enters holder, closes holder valve and extracts;
Step 7: extract surplus liquid out by recycle pump and be back in beaker.
In accordance with a further aspect of the present invention, relate to and utilize above-mentioned preparation system to prepare the method for combustible ice, comprise the following steps:
Step one: with deionized-distilled water by reactor cleaning several, then open temp Controlling System, adopts constant temperature circulator to control within the scope of design temperature by the temperature in reactor, circulating cooling reactor 90s ~ 180s;
Step 2: utilize vacuum pump to vacuumize 3 ~ 5 minutes to reactor and pipeline thereof, sucks in still by the mixed solution of the deionized-distilled water prepared and tensio-active agent from reinforced beaker;
Step 3: close down vacuum pump, to outward winding surge tank outlet valve, Sweet natural gas is released from gas cylinder, after surge tank precooling, enter pressure regulator valve reduce pressure further, the precooling Sweet natural gas passing into 275 ~ 277K from the top of reactor in reactor reacts, and still internal pressure is maintained setting pressure scope;
Step 4: start the vibrator be arranged on bottom reactor, regulate supporting time controller to make it drive reactor horizontal vibration per half an hour once, each 5 minutes, so repeatedly, the abundant mixing in realization response still, accelerates the generation of hydrate;
Gas hydrate and liquid separation are come by filter screen by step 5: after gas hydrate nucleus generates completely in question response still;
Step 6: filter screen is rotated clockwise 90 ° to open passage at the bottom of still, opens vibrator, is fully stripped down by the hydrate crystal in reactor and on filter screen, imports hydrate hold-up vessel;
Step 7: hold-up vessel is controlled under design temperature scope and setting pressure scope environment, after the whole discharging of hydrate of reaction generation enters holder, close holder valve, open vent valve, when still internal pressure recovers barometric point, close outlet valve, and surplus liquid is drawn back reinforced beaker by ON cycle pump.
Preferably, tensio-active agent is sodium lauryl sulphate; Above-mentioned design temperature scope is-1 DEG C ~ 4 DEG C, and setting pressure scope is 30 ± 5MPa.
Preferably, reactor is the dihedral reactor be processed into by the mode that titanium alloy monobloc forging part inside hollows out, and reactor bottom is provided with fastening point, for assembling vibrator.
Apparatus and method prepared by combustible ice automatization according to the present invention, its lanthanum chloride hydrate efficiency is high, cost is low, extraction is convenient.The method not only avoid the decomposition of gas hydrate when extracting, and overcomes the defect that prior art effectively can not extract combustible ice sample, and to the physical chemistry morphological research of combustible ice and realize industrial production and be significant.
Accompanying drawing explanation
Fig. 1 is the structural principle schematic diagram of combustible ice preparation system of the present invention.
Fig. 2 is the schematic diagram of the reactor structure in preparation system of the present invention.
Fig. 3 is the schematic diagram of kettle of the present invention and holder connection mechanism.
Reference numeral:
1. gas cylinder; 2. surge tank; 3. pressure regulator valve; 4. vacuum meter; 5. vacuum pump; 6. precision pressure gauge; 7. under meter; 8. recycle pump; 9. temperature sensor; 10. pressure transmitter; 11. data collecting instruments; 12. reactors; 13. vibrators; 14. holders; 15 ~ 23. valves; 24. discharge outlets; 25. air collectors; 26. constant temperature circulators; 27. beakers; 28. liquid phase valves; 29. outlet valves; 30. filter screens; 31. screw seats; 32. bolts; 33. metal sheets; 34. fastening point.
Embodiment
For making the object, technical solutions and advantages of the present invention clearly understand, hereinafter will be described in detail to embodiments of the invention by reference to the accompanying drawings.It should be noted that, when not conflicting, the embodiment in the application and the feature in embodiment can arbitrary combination mutually.
Preparation system structural principle of the present invention is see Fig. 1.By the system that combustible ice automatization according to the present invention is prepared and extracted, synthon system, water cycle subsystem and the large subsystem of extraction subsystem three are organically combined into an entirety, thus realization production-extract integrated object.
According to the method for combustible ice automatic production of the present invention and extraction, the distilled water prepared is passed into synthon system with tensio-active agent mixed solution by water cycle subsystem together with Sweet natural gas react, the combustible ice hydrate crystal generated imports and extracts subsystem after solid-liquid separation under vibrator effect, the temperature and pressure of regulation system, control the storage condition of combustible ice, complete the extraction of combustible ice.
Preferably, synthon system according to the present invention mainly comprises high pressure visual reaction kettle 12, constant temperature circulator 26, Sweet natural gas admission passage, vacuum unit, temperature and pressure transmitter and data collecting system, and constant temperature circulator 26 is wherein for controlling the temperature in reactor 12.Water cycle subsystem mainly comprises reinforced beaker 27, recycle pump 8, and wherein in reactor 12, inject mixed solution by reinforced beaker 27, surplus liquid is drawn back reinforced beaker 27 by end of synthesis Posterior circle pump 8, so repeatedly.Extract the main involving vibrations device 13 of subsystem and holder 14, vibrator 13, for being peeled off from still wall by the hydrate crystal generated in still, imports holder 14 under gravity.Leaching process directly carries out after combustible ice generates, and does not depart from its solid environment, effectively ensure that finished product solid form stable in leaching process.
The process of combustible ice is prepared below in conjunction with accompanying drawing 1-3 detailed description method according to the present invention.As shown in Figure 1, vacuum pump 5 is utilized to vacuumize the reactor 12 and pipeline that clean up also precooling, open liquid phase valve 28, utilize vacuum to suck in still by the deionized-distilled water prepared and tensio-active agent mixed solution from reinforced beaker 27, close liquid phase valve 28.The Sweet natural gas controlled by pressure regulator valve 3 after cushioning through surge tank 2 is discharged in still by gas cylinder 1 from reactor 12 top, controls by under meter 7 and pressure transmitter 10 pressure that natural gas density in still controls in reactor.Opening constant temperature circulator 26 regulates still environment temperature to design temperature scope, such as, within the scope of-1 DEG C ~ 4 DEG C, and makes still internal pressure be stabilized in setting pressure scope, such as 30 ± 5MPa.After gas hydrate nucleus generates completely, close under meter valve 20, open still bottom outlet valve 29, by the filter screen 30 in such as 0.075mm aperture, surplus liquid in still is filtered out, will be extracted out by recycle pump 8 and turn back in beaker 27 after surplus liquid.Filter screen 30 being rotated clockwise 90 ° makes passage at the bottom of itself and still parallel longitudinal to open passage, opens vibrator 13, makes hydrate crystal and filter screen 30 stripping interior from reactor 12 under gravity generated in still, enters holder 14 by the outlet of reactor.After the whole discharging of hydrate of reaction generation enters holder, close holder valve and extract.After extraction completes, close holder valve 23, open drain tap 21, close down constant temperature circulator 26, when still internal pressure recovers barometric point, close outlet valve 29, unload holder 14.
Selectively, following steps can be adopted to prepare combustible ice:
Step one: with deionized-distilled water by reactor cleaning several, then open temp Controlling System, adopts constant temperature circulator the temperature of reactor to be set as within the scope of-1 DEG C ~ 4 DEG C, circulating cooling reactor 90s ~ 180s.
Step 2: utilize vacuum pump to vacuumize 3 ~ 5 minutes to reactor and pipeline thereof, sucks the mixed solution of the deionized-distilled water prepared and tensio-active agent in still from reinforced beaker.Tensio-active agent wherein preferably can adopt sodium lauryl sulphate (SDS).
Step 3: close down vacuum pump, to outward winding surge tank outlet valve, Sweet natural gas is released from gas cylinder, after surge tank precooling, enter pressure regulator valve reduce pressure further, the precooling Sweet natural gas gas passing into 275 ~ 277K from the top of reactor in reactor reacts, and still internal pressure is maintained setting pressure scope.
Step 4: start the vibrator be arranged on bottom reactor, regulate supporting time controller to make it drive reactor horizontal vibration per half an hour once, each 5 minutes, so repeatedly, the abundant mixing in realization response still, accelerates the generation of hydrate.
Gas hydrate and liquid separation are come by filter screen by step 5: after gas hydrate nucleus generates completely in question response still.
Step 6: filter screen is rotated clockwise 90 ° to open passage at the bottom of still, opens vibrator, is fully stripped down by the hydrate crystal in reactor and on filter screen, imports hydrate hold-up vessel.
Step 7: hold-up vessel is controlled under design temperature scope and setting pressure scope environment, such as control under-1 DEG C ~ 4 DEG C and 30 ± 5MPa environment, after the whole discharging of hydrate of reaction generation enters holder, close holder valve, open vent valve, when still internal pressure recovers barometric point, close outlet valve, unload holder, and surplus liquid is drawn back reinforced beaker by ON cycle pump.
In order to understand the present invention better, be described in further detail each system works device of the present invention and principle:
In Sweet natural gas admission passage of the present invention, Sweet natural gas is discharged by gas cylinder 1, after surge tank 2 cushions, controlled by pressure regulator valve 3 and system stability can be made at the pressure of setting, under meter 7 records Sweet natural gas and enters in still the instantaneous and integrated flow participating in reacting from reactor top.Setting pressure table 6 on admission passage, measures the pressure change in reactor.The top hole pressure controlled due to gas cylinder 1 is unstable, guarantees to enter stablizing and preventing gas backstreaming from working the mischief of air-flow in reactor 12, then controlled by pressure regulator valve 3 by buffering gas tank 2.
High pressure visable hydrate reaction still of the present invention can see Fig. 1 and Fig. 2, and wherein figure below of Fig. 2 is the upward view of upper figure.High pressure visual reaction kettle 12 is the dihedral reactors be processed into by the mode that titanium alloy monobloc forging part inside hollows out, and kettle bottom is circle export structure, and maximum working pressure (MWP) can reach 40MPa, and operating temperature range is-20 DEG C ~ 120 DEG C.The upper end cover of reactor 12 is provided with two sensor insertion hole, two constant temperature circulator circuit holes, Sweet natural gas air inlet port, a Sweet natural gas venting hole and a liquid filling orifice.Wherein, in two sensor insertion hole, be respectively arranged with temperature sensor 9 and pressure transmitter 10, respectively the temperature and pressure parameter of energy accurate-metering gas hydrate synthetic system; Two constant temperature circulator circuit holes connect constant temperature circulator 26, for controlling the temperature of reactor to set(ting)value.Reactor 12 bottom is provided with 4 fastening point 34, along from outlet edge suitably apart from symmetrical, for assembling vibrator 13.
The formation basic theory of the gas hydrate that the present invention utilizes is: water molecules and the natural gas molecule be dissolved in water constantly gather, until the size of the group of gathering and concentration reach critical nucleation condition, gas hydrate just start to generate.Because liquid-gas interface reaches nucleation concentration conditions at first, hydrate is the first nucleation and growth process at interface usually.The growth of hydrate will experience dissolution phase at first, after reaching hypersaturated state, oversaturated gas molecule and water molecules interact and form complex state structure, grow to critical size, by the autocatalytic effect of crystal after hydrate nucleus is formed, namely hydrate starts raised growth.
The present invention also comprises the Measurement and Control System and data collecting system that control reactor temperature and pressure:
Refrigeration temperature control system adopts constant temperature circulator, controls temperature of reaction, can provide the high and low isoperibol in-40 DEG C ~ 105 DEG C temperature ranges, be specially adapted to the equipment such as chemical reaction kettle by the mode of automatic temperature-controlled.Have air-cooled type efficient hermetically sealed compressor, cooling rate is fast; Microcomputer-based intelligent controls, and temperature is accurate; Digital display resolving power 0.1 DEG C or 0.01 DEG C, have measured temperature drift correction function; Temperature overtemperature prote, automatic cut-off power is also reported to the police; The advantages such as refrigeration system is overheated, overcurrent is protected automatically.Temperature of reaction adopts RTD to measure by temperature sensor, and precision is ± 0.1K, and during measurement, probe extend into about 20mm in reactant, measures the change of temperature in hydration generative process.
Pressure in reactor is controlled by high-pressure natural gas density of the induced air, under constant volume constant temperature condition, still internal pressure is regulated by air input, and measured by pressure transmitter 10, be presented on precision pressure gauge 6, after pressure equilibrium is broken, inlet system is automatically started working and is reached next balance, is therefore very beneficial for the constant of gaseous tension in reactor.
Data collecting system 11 major function comprises temperature in the kettle display, the display of still internal pressure, charge flow rate Signal aspects etc.Meanwhile, Interferogram Analysis when the temperature and pressure digital display data in reactor gather by computer is unified and puts into effect.
Water cycle subsystem of the present invention comprises reinforced beaker 27, liquid phase valve 28, separator valve 22, recycle pump 8 and circulation fluid turnover pipeline, and Main Function is conveying, absorption, separation, circulation mixed solution.By vacuum pump 5, the deionized-distilled water prepared and tensio-active agent mixed solution are transported in still before carrying out compound experiment, after treating lanthanum chloride hydrate, ON cycle pump 8 absorbs mixed solution, solid-liquid separation is come, mixed solution gets back to reinforced beaker 27 through circulation line, so repeatedly.
The present invention adopts sodium lauryl sulphate (SDS) as the principles of chemistry of tensio-active agent to be: in static systems, synthesis of natural gas hydrate needs the time in a few week usually, and in static systems, adding the sodium lauryl sulphate of certain mass mark, hydrate generating rate will reach 700 times of pure aquatic system.The existence of tensio-active agent effectively can reduce surface tension, reduce gas, liquid interfacial resistance, raising interfacial layer gaseous mass concentration, gas molecule is stressed in the liquid phase, the effect of mass concentration difference, and rapid solution also reaches hypersaturated state initiation air-water bunch generation initiation nucleation.Add the speed of growth that generates hydrate in the aqueous solution of tensio-active agent and final gassiness volume ratio is all significantly improved.In addition, tensio-active agent can also change the microtexture of liquid and have anti-coalescence effect, prevents coalescent due to hydrate and situation that is that cause free water cannot continue to enter into solid hydrate occurs.SDS system reduces due to surface tension, and gas molecule easily dissolves in liquid phase and participates in reaction, and the decline of reaction later stage speed is not obvious, and thus final product gassiness volume ratio is higher.
The connection of reactor 12 of the present invention and holder 14, see Fig. 3, adopts the fastening reactor 12 of bolt 32 and holder 14, and wherein in Fig. 3, left side represents with the figure on right side the state be connected with when not being connected respectively.Holder 14 is symmetrical arranged 4 screw seats 31, and outside connection tube wall, correspondence position is fixed one piece and is symmetrically distributed with 4 annular metal sheets 33 slightly larger than the large small through hole of screw diameter, for inserting bolt 32 fixed storage.Screw seat 31 of the present invention is cast in the female part of band supporting with bolt 32 size on holder 14.During assembling, by bolt 32 through annular metal sheet 33 precession screw seat 31, during dismounting holder 14, valve-off 29 and 23, bolt 32 of outwarding winding.
The present invention extracts subsystem and comprises holder 14, vibrator 13 and temperature, pressure regulating mechanism.The double-deck pressure resistant reservoir tank that holder 14 adopts aluminium and steel to do, is evacuated between two-layer, makes inner bag reach heat insulation with the external world, keep the balance of temperature.Supporting time controller installed by vibrator 13, and regulating time controller makes its per vibration half an hour once, each 5 minutes.When assembling with reactor 12, fixed by 4 fastening point of kettle bottom 34, see Fig. 2, hollow out into cylindric in the middle of vibrator 13, diameter, slightly larger than exit diameter, is convenient to reactor 12 and is connected the mouth of pipe with holder 14 and passes.When vibrator 13 works, vibrational frequency is 3600 ~ 7200r/min, also can experimentally need to select different vibrational frequencies and time of vibration.Temperature, pressure regulating mechanism utilizes constant temperature circulator 26 and Sweet natural gas inlet system, is opened into working order, reaches-1 DEG C ~ 4 DEG C and 30 ± 5MPa storage under ambient conditions combustible ice solid.
Although the embodiment disclosed by the present invention is as above, the embodiment that described content just adopts for the ease of understanding the present invention, and be not used to limit the present invention.Technician in any the technical field of the invention; under the prerequisite not departing from the spirit and scope disclosed by the present invention; any amendment and change can be done what implement in form and in details; but scope of patent protection of the present invention, the scope that still must define with appending claims is as the criterion.
Claims (5)
1. the preparation system of a combustible ice, comprise synthon system, water cycle subsystem and extract subsystem, it is characterized in that, utilize described water cycle subsystem in described synthon system, pass into the mixed solution of distilled water and the tensio-active agent prepared, and utilizing admission passage to pass into Sweet natural gas to generate combustible ice hydrate in described synthon system, described extraction subsystem extracts the combustible ice hydrate crystal after solid-liquid separation by vibrator;
The preparation method of described combustible ice preparation system comprises the following steps:
Step one: with deionized-distilled water by reactor cleaning several, then open temp Controlling System, adopts constant temperature circulator to control within the scope of design temperature by the temperature in reactor, circulating cooling reactor 90s ~ 180s;
Step 2: utilize vacuum pump to vacuumize 3 ~ 5 minutes to reactor and pipeline thereof, sucks in still by the mixed solution of the deionized-distilled water prepared and tensio-active agent from reinforced beaker;
Step 3: close down vacuum pump, to outward winding surge tank outlet valve, Sweet natural gas is released from gas cylinder, after surge tank precooling, enter pressure regulator valve reduce pressure further, the precooling Sweet natural gas passing into 275 ~ 277K from the top of reactor in reactor reacts, and still internal pressure is maintained setting pressure scope;
Step 4: start the vibrator be arranged on bottom reactor, regulate supporting time controller to make it drive reactor horizontal vibration per half an hour once, each 5 minutes, so repeatedly, the abundant mixing in realization response still, accelerates the generation of hydrate;
Gas hydrate and liquid separation are come by filter screen by step 5: after gas hydrate nucleus generates completely in question response still;
Step 6: filter screen is rotated clockwise 90 ° to open passage at the bottom of still, opens vibrator, is fully stripped down by the hydrate crystal in reactor and on filter screen, imports hydrate hold-up vessel;
Step 7: hold-up vessel is controlled under design temperature scope and setting pressure scope environment, after the whole discharging of hydrate of reaction generation enters holder, close holder valve, open vent valve, when still internal pressure recovers barometric point, close outlet valve, and surplus liquid is drawn back reinforced beaker by ON cycle pump;
Described combustible ice preparation system and method are by synthon system, water cycle subsystem and the large subsystem of extraction subsystem three organically combine into an entirety, tight association, indispensable, there are energy-conserving and environment-protective, level of automation is high, advantages of simple structure and simple, produce-extract its synthesis storage condition of integrated strict guarantee by combustible ice, the combustible ice fundamentally overcoming synthetic can contact the defect that severely degrade appears in normal temperature and pressure environment in existing extractive technique, the sample characteristics of for example of efficient guarantee finished product hydrate, really green integration technology and super potential energy source perfect adaptation are got up.
2. preparation system according to claim 1, it is characterized in that, wherein said synthon system mainly comprises high pressure visual reaction kettle, constant temperature circulator, vacuum unit, temperature and pressure transmitter and data collecting system, wherein said constant temperature circulator is for controlling the temperature in described reactor, described constant temperature circulator, described vacuum unit are all connected with described reactor with described temperature and pressure transmitter, and described data collecting system can gather the pressure and temperature in described reactor by described temperature and pressure transmitter.
3. preparation system according to claim 1 and 2, it is characterized in that, wherein said water cycle subsystem mainly comprises reinforced beaker and recycle pump, wherein in described reactor, inject mixed solution by described reinforced beaker, unnecessary mixed solution is withdrawn in described reinforced beaker by described recycle pump after extracting and terminating by synthesis.
4. preparation system according to claim 1, it is characterized in that, the main involving vibrations device of wherein said extraction subsystem and holder, described vibrator for being peeled off from still wall by the hydrate crystal generated in still, imports described holder under gravity in extraction subsystem operation process; And, during described extraction subsystem work, utilize described constant temperature circulator, described admission passage and described temperature and pressure transmitter to monitor and control temperature and pressure when extracting, and controlled at combustible ice can in storage environment, to meet the requirement of combustible ice to storage environment.
5. preparation system according to claim 1, the design temperature scope of wherein said reactor and holder is-1 DEG C ~ 4 DEG C, and the setting pressure scope of described reactor and holder is 30 ± 5MPa.
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| CN103861529B (en) * | 2014-04-09 | 2016-04-06 | 中能天地（北京）节能科技股份有限公司 | A kind of combustible ice self-organizing process units |
| CN106226139B (en) * | 2016-08-29 | 2018-11-23 | 中国地质大学（北京） | The synthesis and monitoring method of hydrate in a kind of permafrost region consolidated rock sample |
| CN106895256B (en) * | 2017-01-19 | 2021-06-08 | 华南理工大学 | Pigment hydrate accelerant and application thereof in preparation of gas hydrate with high gas storage density |
| CN109731530A (en) * | 2018-12-17 | 2019-05-10 | 中国科学院广州能源研究所 | Electrostatic atomization acts on lower hydrate continuous generation device |
| CN111781011B (en) * | 2020-08-04 | 2023-03-28 | 中国船舶科学研究中心 | Pressure-maintaining and fidelity-keeping sampling device for combustible ice storage test cabin |
| CN113533676B (en) * | 2021-07-23 | 2023-07-07 | 中国石油大学(华东) | Laboratory simulation method for determining generation efficiency of deep-sea submarine natural gas hydrate |
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