CN109628183A - A kind of method of storing natural gas hydrate - Google Patents
A kind of method of storing natural gas hydrate Download PDFInfo
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- CN109628183A CN109628183A CN201811552502.XA CN201811552502A CN109628183A CN 109628183 A CN109628183 A CN 109628183A CN 201811552502 A CN201811552502 A CN 201811552502A CN 109628183 A CN109628183 A CN 109628183A
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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 present invention relates to a kind of methods of storing natural gas hydrate.The method of the storing natural gas hydrate, the following steps are included: (1) is put into porous media and water identical with the pore volume of the porous media in micro-nano-scale restricted clearance, sealing and standing absorbs water by porous media, obtains aqueous porous media；(2) aqueous porous media is put into reaction vessel, the gas needed for injecting hydrate in reaction vessel and generating, synthetizing micro-nano scale restricted clearance gas hydrates；(3) micro-nano-scale restricted clearance gas hydrates are saved under normal pressure, that is, realizes the storage of gas hydrates.The present invention proposes the efficient gas hydrates conveying method of the energy-saving safety of completely new high-quality using the unique formation and decomposition kinetics characteristic of gas hydrates in the unique physico-chemical property and micro-nano-scale restricted clearance of water in micro-nano-scale restricted clearance.
Description
Technical field
The present invention relates to Natural Gas Hydrate Technology field, in particular to a kind of method of storing natural gas hydrate.
Background technique
Gas hydrates are the cage compound that natural gas and water are formed under cryogenic high pressure, 1 cubic metre of natural gas
Hydrate can discharge 164 cubic metres of natural gas at normal temperatures and pressures.It will by certain technique with huge gas storage capability
Natural gas synthesizes solid-state hydrate, and hydrate is then transported to gasholder station again, and hydrate gasification is finally decomposed to form day
This process of right gas, is gas hydrates method transportation of natural gas technology.Gas hydrates transportation of natural gas technology
It is divided into 3 steps, the i.e. rapid synthesis of hydrate, safety in transportation and storage, efficient-decomposition.
Quickly the gas hydrates sample of preparation high-quality is the key that gas hydrates method transportation of natural gas technology.
In macro-scale, the sample that laboratory is prepared by hydration method usually has that sample is lax, hole is big, need to be compacted fine and close ask
Topic, and sample carries out compacting densification, the pollution in transmission and treatment process or the possibility of decomposition of hydrate is brought, in macroscopical ruler
There is " climbing wall effect " in degree, lanthanum chloride hydrate, the generation of " climbing wall effect " is the hydrate due to generation on solid cold wall face
Accumulation, i.e., effect or the hydrate aggregation formation above gas-liquid interface gathered to reaction kettle inner wall surface." climbing wall effect "
Presence make the growth of hydrate uneven, the hydrate block surface after generation is very rough and uneven in surface.Common practice is to adopt
Densification in situ of pressurizeing is carried out to it with piston apparatus.But hydrate such as carbon dioxide hydrate excessive to hardness etc. can not carry out
Pressurization in situ is fine and close.In fact, many factors affect the formation and developmental process of hydrate crystal, such as reaction kettle inner wall table
Face situation, the chemical component of the solute in solution, electric field, the presence in magnetic field or even illuminance will affect hydrate crystal at
Core, growth.In macro-scale, research finds that reaction kettle material will affect the appearance position and gas hydrate synthesis of hydrate nucleation
Mass transfer characteristic in the process.
Using gas hydrates transportation of natural gas, compared with compressed natural gas, liquefied natural gas, gas-storing capacity is high, system
Although standby condition is more mild, the generating rate of hydrate is slower, and consistency is poor, needs to consider the problems such as recycling of water.
Summary of the invention
The object of the present invention is to provide a kind of method of storing natural gas hydrate, the present invention is limited using micro-nano-scale
The unique of gas hydrates forms and decomposes power in the unique physico-chemical property and micro-nano-scale restricted clearance of water in space
Characteristic is learned, proposes the efficient gas hydrates conveying method of the energy-saving safety of completely new high-quality.
The object of the present invention is to provide a kind of methods of storing natural gas hydrate, comprising the following steps:
(1) porous media and identical as the pore volume of the porous media is put into micro-nano-scale restricted clearance
Water, sealing and standing absorbs water by porous media, obtains aqueous porous media；
(2) the aqueous porous media that step (1) obtains is put into reaction vessel, it is raw in injecting hydrate in reaction vessel
At required gas, synthetizing micro-nano scale restricted clearance gas hydrates；
(3) the micro-nano-scale restricted clearance gas hydrates that step (2) obtains are saved under normal pressure, i.e. realization day
The storage of right gas hydrate.
In in micro-nano-scale restricted clearance, hydrone raman frequency is reduced, and the attraction enhancing between hydrone makes
It obtains OH key to increase, weakens the effect of OH chemical bond.Design feature makes the water in micro-nano-scale restricted clearance very in this way
Still exist in liquid form at a temperature of low.Under room temperature, in micro-nano-scale restricted clearance, hydrone DDAA (double
Donor-double acceptor), two kinds of structure Gaussian peaks of DA (single donor-single acceptor) account for 90% with
On, compared with being good for Gaussian peak with the OH of the Free water hydrone under normality, the DDAA structure of water is high in micro-nano-scale restricted clearance
This peak is remarkably reinforced, and the Gaussian peak of its DA obviously weakens, relative to the Free water under macro-scale normality, micro-nano-scale by
Limiting water part DA thaumatropy in space is DDAA structure, so that the ratio of DDAA structure is higher than the ratio of DA structure.To
Hydrone is by trap in the tetrahedron hydrogen bond network structure that hydrone is constituted in micro-nano-scale restricted clearance.It is this micro-nano
The structure of water is advantageous to the formation of gas hydrates in scale restricted clearance.It is micro-nano under the conditions of certain degree of supercooling
The synthetic reaction of water and natural gas in scale restricted clearance is almost the gas hydrates sample ten moment completed, and synthesized
Divide densification.The present invention is not easy to form ice using this of the water in micro-nano-scale restricted clearance, easily the hydration of formation natural gas
Object, and the very fine and close architectural characteristic of gas hydrates sample synthesized, the sample of rapid synthesis gas hydrates.
Micro-nano-scale restricted clearance gas hydrates are decomposed at normal temperature, obtain natural gas, and be in micro-nano meter ruler
Spend the water of restricted clearance.The water of micro-nano-scale restricted clearance can be re-used for synthetizing micro-nano scale restricted clearance gas water
Close object.
Preferably, porous media described in step (1) is column chromatographic silica gel or three-dimensional porous graphene oxide.
Preferably, gas described in step (2) is methane.
Preferably, step (2) comprises the concrete steps that: being put into the aqueous porous media that step (1) obtains in reaction vessel, reacts
The high pressure gas needed for hydrate generates is passed through in container several times to be vacuumized, is generated in injecting hydrate in reaction vessel
Pressure is 12~16MPa in required gas to reaction vessel, closes reaction vessel, and synthetizing micro-nano scale restricted clearance is natural
Gas hydrate.
Preferably, step (3) comprises the concrete steps that: the micro-nano-scale restricted clearance natural gas that step (2) is obtained is hydrated
Object adjusts the pressure of gas hydrates in reaction vessel to required pressure, so that natural gas by discharging portion gas
Hydrate is in metastable state region or stationary zones, after temperature, pressure in reaction vessel is stablized, by the temperature in reaction vessel
Degree is cooled to 227~237K, and after temperature is stablized, the pressure for discharging gas in reaction vessel is normal pressure, saves under normal pressure, i.e., in fact
The storage of existing gas hydrates.
Gas hydrates 227K at 1atm is decomposed in micro-nano-scale restricted clearance, undergoes hydrate-subcooled water-height
The evolution process of the amorphous ice of density decomposes subcooled water after occurring and forms the very amorphous ice of high density at once, and very highly dense
Spending amorphous ice, there are the long periods.Very without fixed shape crystal structure is not present, it is more like one in the amorphous ice of high density
It is kind extremely viscous, solid liquid is presented so that guest molecule can not be overflowed in the short time, the unusual amorphous ice of high density
Package is in the gas hydrates of crystalline state, hinders the heat absorption of decomposable process, enables gas hydrates when longer
Between stable presence.The present invention forms very high density without fixed using gas hydrate dissociation in micro-nano-scale restricted clearance
Shape ice, package be in crystalline state gas hydrates, hinder the heat absorption of decomposable process, enable gas hydrates compared with
The existing characteristic of long-time stable 227K at 1atm saves gas hydrates, and carrying cost is effectively reduced.
At normal temperatures and pressures, gas hydrate dissociation in micro-nano-scale restricted clearance forms natural gas and water, slowly
Natural gas is released, safety is increased.The heat absorption of decomposition derives from air, without additional heating.And the water being decomposed to form according to
It so rests in micro-nano-scale restricted clearance, the synthesis of gas hydrates sample can be repeatedly used for, avoid the recycling of water
Problem.
Further preferably, the pressure of gas hydrates in reaction vessel is adjusted in step (3) to 2.75MPa, so that day
Right gas hydrate is in metastable state region or stationary zones.
Method of the invention overcomes the deficiency of prior art sample treatment, and compared with prior art, the present invention has
Following excellent results:
1, the present invention utilizes the unique physico-chemical property and micro-nano-scale restricted clearance of water in micro-nano-scale restricted clearance
Unique formation of interior gas hydrates and decomposition kinetics characteristic, propose that the energy-saving safety of completely new high-quality is efficiently natural
Gas hydrate conveying method.
2, the present invention proposes to use micro-nano-scale restricted clearance water synthesis of natural gas hydrate sample, and in 227K normal pressure
Storing natural gas hydrate decomposes the gas hydrates storage and transportation side that gas hydrates obtain natural gas at normal temperatures and pressures
Method.Micro-nano-scale restricted clearance water synthesis of natural gas hydrate is very rapid, after 227K decompression, gas hydrates surface layer
The unusual amorphous ice of high density is formed, gas hydrates are wrapped in, enabling gas hydrates, 227K is protected under normal pressure
It deposits, gas hydrates slowly decompose at normal temperatures and pressures, obtain natural gas.This method have hydrate generating rate compared with
Fastly, sample consistency preferably, be effectively reduced carrying cost, decompose slowly, increase safety, without skills such as recycling in view of water
Art advantage.
Detailed description of the invention
Attached drawing 1 is the experiment flow structural schematic diagram of the method for storing natural gas hydrate of the embodiment of the present invention.
Specific implementation method
The present invention is further described by following specific embodiments, but does not limit the present invention.Storage day in the present invention
The method of right gas hydrate is suitable for most of gas that natural gas can be covered, and comes by taking methane as an example in the embodiment of the present invention
Explanation.
As shown in Figure 1, a kind of method of storing natural gas hydrate, specifically includes the following steps:
1, synthetizing micro-nano scale restricted clearance water, micro-nano-scale restricted clearance porous media are column chromatographic silica gel,
Or three-dimensional porous graphene oxide, it will be identical with column chromatographic silica gel or three-dimensional porous graphene oxide pore volume
Water and column chromatographic silica gel or three-dimensional porous graphene oxide are sufficiently mixed.Sealing and standing 5 days, to guarantee that water is more
Hole Absorption of Medium.Water in the present invention is distilled water.
2, aqueous column chromatographic silica gel or aqueous three-dimensional porous graphene oxide are put into reaction kettle.Reaction kettle is not
Become rusty steel reaction kettle.
3, the high pressure gas being repeatedly passed through in reaction kettle needed for hydrate generates, such as methane gas blow away reaction kettle and pipe
Air in road, or take by way of vacuumizing the air in reaction kettle and pipeline away.
4, reaction kettle is cooled to hydrate phase balance point hereinafter, and having certain degree of supercooling, gas in simultaneous buffering tank
Pre-cooling.
5, required high pressure gas is generated in injection hydrate in reaction kettle later, and reaches certain pressure, close reaction
Kettle.
6, injection hydrate generates required high pressure gas to certain pressure, micro-nano-scale restricted clearance day in reaction kettle
Right gas hydrate synthesizes within a few hours to be finished.
7, after synthesis of natural gas hydrate sample, by discharging portion gas, the pressure of gas hydrates in adjusting kettle,
Pressure finally makes gas hydrates sample be in metastable state region or stationary zones to required pressure value.
8, after 5h, after temperature, pressure is stablized, it is cooled to 227K, after temperature is stablized, release reaction gas reactor to normal pressure,
Valve is closed, gas hydrates surface layer forms the amorphous ice of very high density.
8, gas hydrates save under 227K normal pressure, transport.
9, air bath is closed, reaction kettle is to slowly warm up to room temperature, and gas hydrate dissociation forms natural gas and water, naturally
By overflowing in micro-nano-scale restricted clearance, water rests in micro-nano-scale restricted clearance gas gas, can be repeatedly used for synthesizing
Gas hydrates in micro-nano-scale restricted clearance.
Embodiment 1
With aperture about 20nm, column chromatographic silica gel, distilled water and the methane gas of partial size about 0.1~0.3mm is experiment material
Material carries out the synthesis of methane hydrate sample using above-mentioned steps, the gas hydrates for saving and decompositing methane gas store up
Transport test experiments.
Aqueous column chromatographic silica gel is synthesized, it will water identical with column chromatographic silica gel pore volume and column chromatography silicon
Glue is sufficiently mixed, stirring.Sealing and standing 5 days, to guarantee that distilled water is absorbed by column chromatographic silica gel hole.It is put in reaction kettle
Enter aqueous column chromatographic silica gel.Take the air in reaction kettle and pipeline away by way of vacuumizing.Reaction kettle is cooled to hydration
Phase balance point hereinafter, and the degree of supercooling with 5K or more, gas pre-cooling in simultaneous buffering tank, so that methane gas and aqueous
Column chromatographic silica gel is in about 273K.Later in injecting precooled methane gas in reaction kettle, and reach 12MPa, closes
Reaction kettle.Methane hydrate synthesizes within a few hours in column chromatographic silica gel hole finishes.
Air bath temperature is adjusted, so that hydrate sample temperature, close to quaternary phase equilibria point temperature 269.18K, temperature, pressure is steady
After fixed, portion gas is discharged, pressure is down to 2.75MPa, so that hydrate sample is in metastable state region.Adjust air bath temperature
Degree, so that temperature in the kettle about 227K is released stress after temperature is stablized to normal pressure.Close reaction kettle.In column chromatographic silica gel hole
Methane hydrate saves under 227K normal pressure, transport.
Air bath is closed, reaction kettle is to slowly warm up to room temperature, and methane hydrate is decomposed to form in column chromatographic silica gel hole
Methane gas and water, by overflowing in column chromatographic silica gel hole, water rests in column chromatographic silica gel hole methane gas, can be repeatedly
For the gas hydrates in synthetizing micro-nano scale restricted clearance.
Discovery is tested repeatedly, is 12~16MPa when injecting methane gas to reacting kettle inner pressure in reaction kettle, is closed anti-
Answer kettle, synthetizing micro-nano scale restricted clearance gas hydrates.It, will be in reaction kettle after reactor temperature pressure is stablized
Storage and transport under gas hydrates normal pressure can be realized to 227~237K in greenhouse cooling.
Embodiment 2
With 0.55~1.2nm of thickness, 0.5~3 μm of diameter, 200~480m of specific surface area2.g–1, pore volume 1.3cm3.g–1
Three-dimensional porous graphene oxide, distilled water and methane gas be experimental material, utilize institute's inventive method step carry out methane water
The synthesis for closing object sample, the gas hydrates storage and transportation test experiments for saving and decompositing methane gas.
Contain a large amount of oxygen-containing functional groups such as hydroxyl, carboxyl and epoxy group in three-dimensional porous graphene oxide structure, so that
Graphene oxide easily absorbs water, and it is loose porous that dry three-dimensional porous graphene oxide is presented powder, in spongy, after adding water
It dissolves rapid and complete, almost recovers immediately original colloidal sol character.
Synthesize aqueous three-dimensional porous graphene oxide.Will water identical with three-dimensional porous graphene oxide pore volume with
Three-dimensional porous graphene oxide is sufficiently mixed, stirring.Sealing and standing 5 days, to guarantee distilled water by three-dimensional porous graphite oxide
Alkene hole absorbs.It is put into aqueous three-dimensional porous graphene oxide in reaction kettle, takes reaction kettle and pipe away by way of vacuumizing
Air in road.Hydrate phase balance point is cooled in reaction kettle hereinafter, and with 5K or more degree of supercooling, simultaneous buffering tank
Interior gas pre-cooling, so that methane gas and oxidizing aqueous Graphene are in about 273K.It is precooled in being injected in reaction kettle later
Methane gas, and reach 12MPa, close reaction kettle.Methane hydrate is in a few hours in three-dimensional porous graphene oxide hole
Interior synthesis finishes.
Air bath temperature is adjusted, so that hydrate sample temperature, close to quaternary phase equilibria point temperature 269.18K, temperature, pressure is steady
After fixed, portion gas is discharged, pressure is down to 2.75MPa, so that hydrate sample is in metastable state region.Adjust air bath temperature
Degree, so that temperature in the kettle about 227K is released stress after temperature is stablized to normal pressure.Close reaction kettle.Three-dimensional porous graphene oxide
Methane hydrate saves under 227K normal pressure in hole, transport.
Air bath is closed, reaction kettle is to slowly warm up to room temperature, methane hydrate point in three-dimensional porous graphene oxide hole
Solution forms methane gas and water, and for methane gas by overflowing in three-dimensional porous graphene oxide hole, water rests on three-dimensional porous oxidation
In graphene hole, the gas hydrates that can be repeatedly used in synthetizing micro-nano scale restricted clearance.
Above-listed detailed description is illustrating for possible embodiments of the present invention, and the embodiment is not to limit this hair
Bright the scope of the patents, all equivalence enforcements or change without departing from carried out by the present invention, is intended to be limited solely by the scope of patent protection of this case
In.
Claims (6)
1. a kind of method of storing natural gas hydrate, which comprises the following steps:
(1) porous media and identical with the pore volume of the porous media is put into micro-nano-scale restricted clearance
Water, sealing and standing absorb water by porous media, obtain aqueous porous media；
(2) the aqueous porous media that step (1) obtains is put into reaction vessel, generates institute in injecting hydrate in reaction vessel
The gas needed, synthetizing micro-nano scale restricted clearance gas hydrates；
(3) the micro-nano-scale restricted clearance gas hydrates that step (2) obtains are saved under normal pressure, i.e. realization natural gas
The storage of hydrate.
2. the method for storing natural gas hydrate according to claim 1, which is characterized in that more described in step (1)
Hole medium is column chromatographic silica gel or three-dimensional porous graphene oxide.
3. the method for storing natural gas hydrate according to claim 1, which is characterized in that gas described in step (2)
Body is methane.
4. the method for storing natural gas hydrate according to claim 1, which is characterized in that step (2) comprises the concrete steps that:
It is put into the aqueous porous media that step (1) obtains in reaction vessel, is passed through several times in reaction vessel needed for hydrate generates
High pressure gas is vacuumized, in reaction vessel inject hydrate generate needed for gas to reaction vessel in pressure be 12~
16MPa closes reaction vessel, synthetizing micro-nano scale restricted clearance gas hydrates.
5. the method for storing natural gas hydrate according to claim 1, which is characterized in that step (3) comprises the concrete steps that:
The micro-nano-scale restricted clearance gas hydrates that step (2) is obtained adjust reaction vessel by discharging portion of natural gas
The pressure of interior gas hydrates is to required pressure, so that gas hydrates are in metastable state region or steady-state zone
The greenhouse cooling in reaction vessel to 227~237K is released after temperature is stablized after temperature, pressure in reaction vessel is stablized in domain
The pressure for putting natural gas in reaction vessel is normal pressure, is saved under normal pressure, that is, realizes the storage of gas hydrates.
6. the method for storing natural gas hydrate according to claim 5, which is characterized in that adjust reaction in step (3)
The pressure of gas hydrates is to 2.75MPa in container, so that gas hydrates are in metastable state region or steady-state zone
Domain.
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| CN201811552502.XA CN109628183B (en) | 2018-12-18 | 2018-12-18 | Method for storing natural gas hydrate |
| PCT/CN2018/124246 WO2020124660A1 (en) | 2018-12-18 | 2018-12-27 | Method for storing natural gas hydrate |
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| CN201811552502.XA CN109628183B (en) | 2018-12-18 | 2018-12-18 | Method for storing natural gas hydrate |
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| CN114015487A (en) * | 2021-11-10 | 2022-02-08 | 燕山大学 | Preparation method of nano ice hydrate |
| CN114718518A (en) * | 2020-12-22 | 2022-07-08 | 中国科学院广州能源研究所 | Quantitative method for distinguishing distribution and form of natural gas hydrate with microporosities |
| WO2024032830A1 (en) * | 2023-10-13 | 2024-02-15 | 中国科学院广州能源研究所 | Method for improving gas storage amount of natural gas hydrate based on crystal regulation and control principle |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN111120869A (en) * | 2020-01-10 | 2020-05-08 | 兰州理工大学 | Biological natural gas storage and use system and storage and use method |
| CN114718518A (en) * | 2020-12-22 | 2022-07-08 | 中国科学院广州能源研究所 | Quantitative method for distinguishing distribution and form of natural gas hydrate with microporosities |
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| WO2024032830A1 (en) * | 2023-10-13 | 2024-02-15 | 中国科学院广州能源研究所 | Method for improving gas storage amount of natural gas hydrate based on crystal regulation and control principle |
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| Publication number | Publication date |
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| WO2020124660A1 (en) | 2020-06-25 |
| CN109628183B (en) | 2020-10-30 |
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