CN107311147A - CNT as hydrate accelerant application - Google Patents
CNT as hydrate accelerant application Download PDFInfo
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- CN107311147A CN107311147A CN201710548075.7A CN201710548075A CN107311147A CN 107311147 A CN107311147 A CN 107311147A CN 201710548075 A CN201710548075 A CN 201710548075A CN 107311147 A CN107311147 A CN 107311147A
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J3/00—Processes of utilising sub-atmospheric or super-atmospheric pressure to effect chemical or physical change of matter; Apparatus therefor
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J19/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
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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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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B2202/00—Structure or properties of carbon nanotubes
- C01B2202/06—Multi-walled nanotubes
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/10—Particle morphology extending in one dimension, e.g. needle-like
- C01P2004/13—Nanotubes
- C01P2004/133—Multiwall nanotubes
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Abstract
The invention discloses application of the CNT as hydrate accelerant, the accelerator that CNT is generated as hydrate is added in the forward direction water of hydrate reaction of formation, the induction time of heat transfer, reduction hydrate generation can be strengthened by the use of CNT as good Heat Conduction Material, promote the generation of hydrate；Thermodynamics accelerator TBAB is added into system simultaneously, raise the generation temperature of hydrate, pressure is reduced, promote the generation of hydrate in terms of dynamics and thermodynamics two, solve current Hydrate Formation Conditions harshness, induction time length, the problem of generating rate is slow.Industrial applications for Hydrate Technology provide wide prospect.
Description
Technical field：
The present invention relates to gas hydrate generation and applied technical field, and in particular to CNT promotes as hydrate
The application of agent.
Background technology：
Gas hydrate is by small gas molecule (CH4、CO2、N2、C2H4Deng) with hydrone in certain condition (low temperature, height
Pressure) under the non-stoichiometric class ice-like crystalline compounds that are formed.Wherein host molecule (hydrone) is formed by hydrogen bond action
The polyhedron hole of caged, guest molecule (gas molecule) is filled in hydrone by van der Waals interaction to be made up of hydrone
Polyhedron hole in.Methane content 80%~99.9%, Air-pollution From Combustion be than coal, oil, natural gas all in gas hydrates
Much smaller, and rich reserves, global reserves reach 1015‐1018m2, enough mankind use 1000.Therefore as following important
Fungible energy source.In addition, gas hydrates can be used in gas storage and transportation, seawater due to its special cagelike structure
Desalinate, the technical field such as gas separation, Oil-gas Separation, solution enrichment.But, the formation condition of current hydrate is still more severe
Carve, the formation condition for being mainly manifested in hydrate is low temperature, high pressure, the induction time of hydrate generation is long, and hydrate generation is slow
In terms of, these bottlenecks significantly limit the extensive use of Hydrate Technology.Therefore, domestic and international researcher proposes a variety of promote
The method of hydrate generation.Conventional method includes addition accelerator or promotes to be hydrated by physical methods such as stirring, bubblings
The generation of thing.The thermodynamics accelerator having now been found that can be divided into two major classes.One class is common thermodynamics accelerator, this kind of promotion
Agent does not change hydrate structure, only influence hydrate phase balance condition, such as tetrahydrofuran (THF), pentamethylene (CP) dodecyl
Sodium sulfonate (SDS) etc.；Another kind of is half cage modle thermodynamics accelerator, and this kind of promotion agent molecule and hydrone participate in hydrate together
The structure of cage, generates half Study of Clathrate Hydrates, so also referred to as half cage modle accelerator, such as TBAB (TBAB), the tetrabutyl
Ammonium chloride (TBAC), tetrabutyl ammonium nitrate (TBANO3), tetrabutyl phosphonium bromide phosphorus (TBPB) etc..These methods really can be in certain journey
The temperature of change hydrate generation, pressure (raising the generation temperature of hydrate, pressure reduction), the life for accelerating hydrate on degree
Into speed.But still can not meet hydrate requirement on industrial application.
The content of the invention：
It is an object of the invention to provide application of the CNT as hydrate accelerant, by the use of CNT as good
Heat Conduction Material can strengthen heat transfer, reduction hydrate generation induction time, promote hydrate generation；Add simultaneously into system
Mechanics accelerator TBAB is heated, raises the generation temperature of hydrate, pressure is reduced, and solves current Hydrate Formation Conditions severe
Quarter, induction time length, the problem of generating rate is slow.
The present invention is achieved by the following technical programs：
CNT as hydrate accelerant application.
Its preferred reaction conditions is：CNT is added in the forward direction water of hydrate reaction of formation to generate as hydrate
Accelerator, can reduce hydrate generation induction time, quickly generate hydrate.
The CNT is multi-walled carbon nanotube.
Experiment shows, mass fraction is 0.1%, the song that balances each other that 0.5%, 1.0% CNT is generated to hydrate
Line has not significant impact.But the induction time of hydrate generation is reduced with the increase of carbon nanotube concentration.Its preferred quality
Fraction is 1.0%.
The CNT as hydrate accelerant application, it is preferable that in the forward direction water of hydrate reaction of formation
The accelerator that CNT is generated as hydrate is added, is led between 1.0~20.0 DEG C and under 1.0~6.0MPa application conditions
Enter reacting gas, hydrate is quickly generated after being sufficiently mixed；Thermodynamics accelerator TBAB is added into reaction system simultaneously, makes water
The rise of generation temperature, the pressure reduction of compound；The hydrate reaction gas is CH4、CO2One or more of.
The hydrate reaction gas is CH4、CO2In one kind or CO2With CH4The mixed gas of composition, exists using temperature
Between 1.0~20.0 DEG C, applying pressure in 1.0~6.0MPa, induction time can be dropped to from 350 minutes or so 150 minutes with
Under, while hydrate void fraction also has very big lifting, it is greatly promoted the generation of hydrate.
Beneficial effects of the present invention are as follows：
1) CNT has good thermal conductivity, and its thermal conductivity is up to 343Wm at room temperature-1K-1, can be in hydrate
In generating process, the heat discharged in rapid transfer hydrate formation, the induction time of reduction hydrate generation, quickly
Hydrate is generated, driven terms of mechanics promotes the generation of hydrate.
2) hydrate accelerant recycling can also, CNT is water insoluble, be used as.
3) while adding the thermodynamics accelerator that TBAB is generated as hydrate into water, hydrate generation can be significantly improved
Temperature, reduce hydrate generation pressure.
In a word, the present invention can strengthen heat transfer, reduction hydrate as good Heat Conduction Material by the use of CNT and generate
Induction time, promotes the generation of hydrate；Thermodynamics accelerator TBAB is added into system simultaneously, makes the generation temperature of hydrate
Rise, pressure reduction, promote the generation of hydrate in terms of dynamics and thermodynamics two, solve current hydrate generation bar
Part harshness, induction time length, the problem of generating rate is slow.For Hydrate Technology industrial applications provide it is wide before
Scape.
Brief description of the drawings：
Fig. 1 is embodiment 1-3 and comparative example 1 system phase equilibrium line；
Fig. 2 is embodiment 4-6 and comparative example 2 pressure versus time curve.
Embodiment：
Further illustrated the following is to the present invention, rather than limitation of the present invention.
Embodiment 1：
Experiment determines balancing each other a little for a certain system using " constant volume pressure search method ".Reactor is clear with deionized water
Wash three times, and autoclave and experiment pipe-line system are purged with nitrogen, it is ensured that the unobstructed drying of system.It is by 30mL concentration
0.1%wt CNTs, concentration is added to reactor for 38.5%wtTBAB liquid, accounts for 1/3rd of kettle inner volume.
Reactor is vacuumized.It is passed through CO2(40.0mol%)+CH4(60.0mol%) mixed gas 1.5-5.5MPa.Treat temperature, pressure
After stable, it is 500rmp to open stirring, sets bath temperature parameter system temperature is down to 1 DEG C or so, promotes hydrate to generate.
According to the temperature, pressure data mapping collected, when pressure is drastically reduced, and temperature when raising suddenly, then hydrate is raw
Into.After hydrate generation is enough, control system is heated up with 1-2K/h speed, and keeping temperature pressure reaches after heating every time
2h after balance.When pressure occur significantly raise when illustrate hydrate start decomposition, control system with 0.1K/h speed progressively
Heating, makes hydrate slowly decompose, and keeping temperature pressure reaches 4h after balance after heating every time.By the pressure in experimentation and
Temperature is plotted on out-of-phase diagram, and the flex point of decomposition curve is exactly balancing each other a little for hydrate.As shown in figure 1, when pressure is respectively
When 1.54MPa, 2.42MPa, 3.39MPa, 4.31MPa, 5.32MPa, corresponding Phase Equilibrium Temperature be respectively 287.97K,
289.56K、290.92K、291.63K、292.54K。
Embodiment 2
According to the experimental method of embodiment 1, completion CNT is 0.5%wt, and TBAB concentration is 38.5%wt, and gas is
CO2(40.0mol%)+CH4The phase equilibrium line of (60.0mol%) mixed gas.As shown in figure 1, when pressure is respectively
When 1.54MPa, 2.47MPa, 3.46MPa, 4.35MPa, 5.33MPa, corresponding Phase Equilibrium Temperature be respectively 288.03K,
289.78K、290.83K、291.85K、292.37K。
Embodiment 3
According to the experimental method of embodiment 1, completion CNT is 1.0%wt, and TBAB concentration is 38.5%wt, and gas is
CO2(40.0mol%)+CH4The phase equilibrium line of (60.0mol%) mixed gas.As shown in figure 1, when pressure is respectively
When 1.41MPa, 2.37MPa, 3.40MPa, 4.37MPa, 5.37MPa, corresponding Phase Equilibrium Temperature be respectively 287.78K,
289.35K、290.85K、291.86K、292.41K。
Comparative example 1
According to the experimental method of embodiment 1, it is 38.5%wt to complete TBAB concentration, and gas is CO2(40.0mol%)+CH4
The phase equilibrium line of (60.0mol%) mixed gas.When pressure be respectively 1.54MPa, 2.42MPa, 3.38MPa, 4.47MPa,
During 5.39MPa, corresponding Phase Equilibrium Temperature is respectively 287.97K, 289.54K, 290.83K, 291.99K, 292.61K.
As shown in figure 1, from the comparison of embodiment 1, example 2, example 3 and comparative example 1, when carbon nanotube concentration is 0.1%
When wt, 0.5%wt, 1.0%wt, there is no notable difference with being not added with the phase equilibrium line of system of CNT, illustrate carbon nanometer
Pipe is to CO2(40.0mol%)+CH4(60.0mol%) system profile of equilibrium does not influence
Embodiment 4
It is 0.1%wt CNTs by 30mL concentration, concentration is that 38.5%wtTBAB liquid is added to reactor.Vacuumize
After be passed through CO2(40.0mol%)+CH4(60.0mol%) mixed gas.The pressure for making gas is 3.5MPa under the conditions of 25 DEG C,
After temperature stabilization 1h, design temperature is 9 DEG C, and unlatching speed of agitator is 500rmp.The degree of supercooling of system is 8 DEG C.Treat hydrate
Terminate experiment after generation, temperature, pressure complete stability.The induction time of hydrate generation is 91.3min.
Embodiment 5
It is 0.5%wt CNTs by 30mL concentration, concentration is that 38.5%wtTBAB liquid is added to reactor.Vacuumize
After be passed through CO2(40.0mol%)+CH4(60.0mol%) mixed gas.The pressure for making gas is 3.5MPa under the conditions of 25 DEG C,
After temperature stabilization 1h, design temperature is respectively 9 DEG C, and it is 500rmp to open stirring.The degree of supercooling of system is 8 DEG C.Treat hydrate
Terminate experiment after generation, temperature, pressure complete stability.The induction time of hydrate generation is 83.3min.
Embodiment 6
It is 1.0%wt CNTs by 30mL concentration, concentration is that 38.5%wtTBAB liquid is added to reactor.Vacuumize
After be passed through CO2(40.0mol%)+CH4(60.0mol%) mixed gas.The pressure for making gas is 3.5MPa under the conditions of 25 DEG C,
After temperature stabilization 1h, design temperature is respectively 9 DEG C, and it is 500rmp to open stirring.The degree of supercooling of system is 8 DEG C.Treat hydrate
Terminate experiment after generation, temperature, pressure complete stability.The induction time of hydrate generation is 72.3min.
Embodiment 7
It is that 1.0%wt carbon nano tube liquids are added to reactor by 30mL concentration.CO is passed through after vacuumizing2
(40.0mol%)+CH4(60.0mol%) mixed gas.The pressure for making gas is 5MPa under the conditions of 25 DEG C, works as temperature stabilization
After 1h, design temperature is respectively 3 DEG C, and it is 500rmp to open stirring.The degree of supercooling of system is 8 DEG C.Treat that hydrate is generated, temperature pressure
Terminate experiment after power complete stability.The induction time of hydrate generation is 117.0min.
Embodiment 8
It is 1.0%wt CNTs by 30mL concentration, concentration is that 20%wtTBAB liquid is added to reactor.After vacuumizing
It is passed through CO2(40.0mol%)+CH4(60.0mol%) mixed gas.The pressure for making gas is 5MPa under the conditions of 25 DEG C, works as temperature
After the stable 1h of degree, design temperature is respectively 11 DEG C, and it is 500rmp to open stirring.The degree of supercooling of system is 8 DEG C.Treat that hydrate is given birth to
Into end experiment after temperature, pressure complete stability.The induction time of hydrate generation is 99.5min.
Comparative example 2
It is that 38.5%wtTBAB liquid is added to reactor by 30mL concentration.CO is passed through after vacuumizing2(40.0mol%)+
CH4(60.0mol%) mixed gas.The pressure for making gas is 3.5MPa under the conditions of 25 DEG C, after temperature stabilization 1h, setting temperature
Degree is respectively 9 DEG C, and it is 500rmp to open stirring.The degree of supercooling of system is 8 DEG C.After after hydrate generation, temperature, pressure is completely steady
Terminate experiment after fixed.The induction time of hydrate generation is 323.4min.
Embodiment 4, embodiment 5, embodiment 6 are compared with comparative example 2 as can be seen that as shown in Fig. 2 adding CNT
Induction time required for system generation hydrate is much smaller than the system without CNT.Add CNT, induction time
Dropped to from 350 minutes or so less than 150 minutes, while hydrate void fraction also has very big lifting, be greatly promoted hydrate
Generation.And embodiment 4, embodiment 5, embodiment 6 compare understand with the increase of carbon nanotube concentration, induction time gradually becomes
It is short.And can be judged from Fig. 2 by pressure drop, the system gas-storing capacity increase of CNT is added, and carbon nanotube concentration is
1.0wt% gas-storing capacities are maximum.
Embodiment 9
It is 1.0%wt CNTs by 30mL concentration, concentration is added to reactor for 38.5%wt TBAB liquid.Take out true
CH is passed through after sky4Gas.The pressure for making gas is 1.5MPa under the conditions of 25 DEG C, after temperature, pressure stable 1h, design temperature
Respectively 8 DEG C, 10 DEG C, 11 DEG C, it is 500rmp to open stirring.The degree of supercooling of system is respectively 5 DEG C, 4 DEG C, 3 DEG C.Treat that hydrate is given birth to
Into end experiment after temperature, pressure complete stability.When degree of supercooling is respectively 5 DEG C, 4 DEG C, 3 DEG C, during the induction of hydrate generation
Between be respectively 95.0min, 257.0min, 1147.0min.
Embodiment 10
It is 1%wt CNTs by 30mL concentration, concentration is added to reactor for 38.5%wt TBAB liquid.Vacuumize
After be passed through CH4Gas.The pressure for making gas is 3.5MPa under the conditions of 25 DEG C, after temperature, pressure stable 1h, design temperature point
Wei not be 8 DEG C, 10 DEG C, 11 DEG C, it is 500rmp to open stirring.The degree of supercooling of system is respectively 8 DEG C, 7 DEG C, 6 DEG C.Treat that hydrate is given birth to
Into end experiment after temperature, pressure complete stability.When degree of supercooling is respectively 8 DEG C, 7 DEG C, 6 DEG C, during the induction of hydrate generation
Between be respectively 106.0min, 111.7min, 154.5min.
Comparative example 3
It is that 38.5%wtTBAB solution is added to reactor by 30mL concentration.CH is passed through after vacuumizing4Gas.Make gas
Pressure is 1.5MPa under the conditions of 25 DEG C, and after temperature, pressure stable 1h, design temperature is respectively 8 DEG C, 10 DEG C, 11 DEG C, is opened
Stir as 500rmp.The degree of supercooling of system is respectively 5 DEG C, 4 DEG C, 3 DEG C.Treat that hydrate is generated, tied after temperature, pressure complete stability
Beam is tested.When degree of supercooling is respectively 5 DEG C, the induction time of hydrate generation is respectively 432min.When degree of supercooling is 4 DEG C and 3 DEG C
When, there is no hydrate generation more than 2100min and 2600min respectively.
Comparative example 4
It is that 38.5%wtTBAB solution is added to reactor by 30mL concentration.CH is passed through after vacuumizing4Gas.Make gas
Pressure is 3.5MPa under the conditions of 25 DEG C, and after temperature, pressure stable 1h, design temperature is respectively 8 DEG C, 10 DEG C, 11 DEG C, is opened
Stir as 500rmp.The degree of supercooling of system is respectively 9 DEG C, 8 DEG C, 7 DEG C after after hydrate generation, after temperature, pressure complete stability
Terminate experiment.When degree of supercooling is respectively 9 DEG C, 8 DEG C, 7 DEG C, hydrate generation induction time be respectively 127.3min,
177.7min、249.4min。
From embodiment 9 and comparative example 3；Embodiment 10 is compareed with comparative example 4 and learnt：In same pressure, same degree of supercooling
Under the conditions of, induction time obvious shortening of the system than the system hydrate generation without CNT of CNT is added, and
Quickly generating for hydrate can be promoted.With one it can be seen from embodiment 9 or embodiment 10 or comparative example 3 or comparative example 4
Under the conditions of system, uniform pressure, degree of supercooling is bigger, and induction time is shorter.
Claims (5)
1. CNT is used as the application of hydrate accelerant.
2. CNT according to claim 1 is used as the application of hydrate accelerant, it is characterised in that in hydrate life
The accelerator that CNT is generated as hydrate is added into the forward direction water of reaction.
3. CNT according to claim 1 or 2 is used as the application of hydrate accelerant, it is characterised in that the carbon
Nanotube is multi-walled carbon nanotube.
4. CNT according to claim 2 is used as the application of hydrate accelerant, it is characterised in that the carbon nanometer
Pipe mass fraction is 1.0%.
5. CNT according to claim 1 is used as the application of hydrate accelerant, it is characterised in that in hydrate life
The accelerator that is generated as hydrate of CNT is added into the forward direction water of reaction, between 1.0~20.0 DEG C and 1.0~
Reacting gas is passed through under 6.0MPa application conditions, hydrate is quickly generated after being sufficiently mixed；Heat is added into reaction system simultaneously
Mechanics accelerator TBAB；The hydrate reaction gas is CH4、CO2One or more of.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN110090544A (en) * | 2019-04-03 | 2019-08-06 | 华南理工大学 | It is a kind of to strengthen hydration separation CH using porous particle4/CO2Method |
| CN112361483A (en) * | 2020-11-10 | 2021-02-12 | 河南理工大学 | Building roof heat insulation method utilizing hydrate cold accumulation |
| CN115650230A (en) * | 2022-11-03 | 2023-01-31 | 清华大学深圳国际研究生院 | CO (carbon monoxide) 2 Method for promoting hydrate formation and CO 2 Method for calculating sealing quantity |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN110090544A (en) * | 2019-04-03 | 2019-08-06 | 华南理工大学 | It is a kind of to strengthen hydration separation CH using porous particle4/CO2Method |
| CN110090544B (en) * | 2019-04-03 | 2021-11-09 | 华南理工大学 | Method for strengthening hydration and separation of CH by using porous particles4/CO2Method (2) |
| CN112361483A (en) * | 2020-11-10 | 2021-02-12 | 河南理工大学 | Building roof heat insulation method utilizing hydrate cold accumulation |
| CN115650230A (en) * | 2022-11-03 | 2023-01-31 | 清华大学深圳国际研究生院 | CO (carbon monoxide) 2 Method for promoting hydrate formation and CO 2 Method for calculating sealing quantity |
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Application publication date: 20171103 |