CN102784604A - Promoter for generation of gas hydrate, and preparation method and application thereof - Google Patents
Promoter for generation of gas hydrate, and preparation method and application thereof Download PDFInfo
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Abstract
The invention discloses a promoter for generation of gas hydrates, and a preparation method and application thereof. The promoter for generation of gas hydrates is a dry powdery solution formed after high speed shearing and dispersion of a surfactant solution and strong hydrophobic solid particles in a high intensity stirrer, wherein the surfactant solution is an aqueous solution of one or more anionic surfactants, cationic surfactants or nonionic surfactants, and the strong hydrophobic solid particles are one or more selected from the hydrophobically modified particles consisting of silica, titanium dioxide, titanium sesquioxide, alumina, zinc oxide, calcium carbonate, montmorillonite, diatomite, fly ash, zeolite, talcum and mica particles, etc. The promoter provided by the invention is highly dispersed solution microdroplets and has a great gas-liquid contact area, the dispersed microdroplets contain surfactants, which enables gas-liquid contact during growth process of hydrates to be further reinforced, and therefore, a generation rate of gas hydrates and gas storage amount in a static system are substantially improved; meanwhile, the promoter has the advantages of low cost, no pollution and convenient preparation and usage.
Description
Technical field
The present invention relates to the gas hydrate generation technique, be specifically related to gas hydrate and generate promoter and preparation and application.
Background technology
Gas hydrate is a kind of non-stoichiometric envelope shape cage compound that under the cryogenic high pressure condition, is generated by gas and water, and gas molecule is wrapped in the cage modle lattice of hydrone formation.Hydrate Technology can be applicable to research fields such as energy gas (natural gas, hydrogen etc.) accumulating, small field exploitation, carbon dioxide capture, desalinization, sewage disposal and mixed gas separation.Along with gas hydrates a large amount of discoveries in the world, hydrate gas storage technology has become a big research focus of energy field and resources domain, has caused numerous scholars' great interest.
Gas hydrate has that gas-storing capacity is big, the characteristics of clean and safe, convenient transportation, but at present its synthetic technology that is that all right is ripe, mainly be that actual gas storage rate of hydrate and gas-storing capacity are all not high.The generation of gas hydrate is complicated gas-liquid-solid heterogeneous heat and mass transfer process, how efficiently fast gas hydrate become the Hydrate Technology key in application.
At present, the technology that promotes gas hydrate to generate fast mainly contains following several kinds: the static contact method of ice powder, interpolation surfactant method, porous media completion method, bubble method of perturbation and mechanical mixing method.(1) ice powder static contact method be earlier with water or the aqueous solution that contains additive through ice powder freezing, that grind, process after the screening certain grain size; Then under undisturbed situation; Gas is contacted with the ice powder; Can increase the contact area of gas and solid water greatly, shorten the hydration induction time, make the quick nucleation of hydrate, growth.(2) adding surfactant method is in water, to add certain surfactant, impels hydrate in growth course, to form porous branch shape hydrate film, increases the solution-air contact, shortens the hydration induction time, thereby accelerates the generating rate of hydrate.(3) the porous media completion method is that a kind of porous media that adopts quickens the technology that gas hydrate generates, and gas is fed in the mixed system of porous media and pure water, increases the solution-air contact area, shortens the hydration induction time, generates gas hydrate fast.(4) the bubble method of perturbation is that the orifice plate that gas is passed through in the reactor produces bubble, gas duck in drink constantly rise, fragmentation, increase the solubility of gas in water, shorten the hydration induction time, thereby accelerate hydrate nucleation, growth.(5) mechanical mixing method is that an agitator is set in reactor, can quicken the dissolving of gas in water through stirring, and impels gas fully to contact with water, shortens the hydration induction time, increases hydration rate.Also having the method that bubble method of perturbation and mechanical mixing method are combined, is that orifice plate and agitator are set in reactor simultaneously, can further increase the contact area of gas and water, the generation of acceleration gas hydrate.
Said method all is through increasing the air-water contact area or increase the mode that gas gets into liquid phase speed, shorten the hydration induction time, improving gas hydrate generating rate and gas-storing capacity when promoting that gas hydrate generates.But also there is shortcoming in several method: 1. the air-water contact area is limited, and local contact is inhomogeneous, has influenced the generating rate and the gas-storing capacity of gas hydrate to a certain extent; 2. bubble method of perturbation and mechanical mixing method have increased extra experimental facilities, and operation inconvenience also causes the increase of gas storage cost; 3. the fuel factor that produces during mechanical agitation also can influence hydrating condition inevitably.
Summary of the invention
The object of the invention is to overcome the shortcoming that the prior art operation is inconvenient, gas storage rate is slow, the gas storage cost is high, proposes a kind of technology---dried solution gas storage of surfactant of quick gas hydrate.This dried solution is that the surfactant solution of certain mass proportioning and strong-hydrophobicity solids are sheared a kind of dried, pulverous, the flowable mixture of disperseing the back to form in the high-intensity stirrer high speed.The not only droplet of dried solution after the dispersion own has very high specific area; Increase the solution-air contact; And surfactant impels hydrate in growth course, to form porous branch shape film, further strengthens contacting of gas and solution, shortens the hydration induction time; Improve gas hydrate generating rate and gas-storing capacity in the static systems greatly, cost is low, pollution-free simultaneously, preparation is easy to use.
Know-why of the present invention:
Gas hydrate generates promoter---and the dried solution of surfactant (dry solution) is that the surfactant solution of certain mass proportioning and strong-hydrophobicity solids are sheared a kind of dried, pulverous, the flowable mixture of disperseing the back to form in the high-intensity stirrer high speed; Its essence is that the strong-hydrophobicity particle is wrapped in the surfactant solution droplet surface uniformly, thereby reach the purpose that solution is dispersed into droplet.Looked by the solution droplet of hydrophobic particles parcel to look like pressed powder, and can flow, so be called dried solution.
Hydrophobic particles is similar to the ice powder to the dispersion effect of surfactant solution, all is liquid height is disperseed and increases its specific area, and enhance liquid contacts with gas, raising hydrate generating rate.But dried solution is different from the ice powder again, and what be wrapped in the dried solution is liquid droplet, and droplet size is between 1 ~ 20 μ m, and specific area is at 0.3 ~ 6 m
2G
-1Between, increase solution-air contact greatly, and surfactant impels hydrate in growth course, to form porous branch shape film, further strengthen solution-air again and contact.The dried solution of surfactant can be preserved more than 6 months by normal temperature.The ice powder then is the solid water particle, and particle size is tens to the hundreds of micron, and its specific area is than a little one magnitude of dried solution, and the preparation process of ice powder is complicated, guarantees that again it does not melt simultaneously.The high-specific surface area of dried solution has been realized the abundant contact of air-water, shortens the hydration induction time, can improve the nucleation and growth speed of gas hydrate in the static systems greatly.
The object of the invention realizes through following technical scheme.
Gas hydrate generates promoter, consists of surfactant, water and hydrophobic particles; Hydrophobic particles is wrapped in the surfactant solution surface, forms droplet.
Said surfactant is anion surfactant, cationic surfactant or non-ionic surface active agent.
Said hydrophobic particles is the particle behind the hydrophobically modified; Said particle is more than one in silica, titanium dioxide, titanium sesquioxide, aluminium oxide, zinc oxide, calcium carbonate, imvite, diatomite, flyash, zeolite, talcum, the mica.Preferred hydrophobicity gas phase nano silica HB630.
The mass fraction of surfactant is 0.01% ~ 0.50% in the said promoter; The mass fraction of hydrophobic particles is 3% ~ 20% in the promoter, and all the other are water.
The size of said droplet is between 1 ~ 20 μ m, and specific area is at 0.3 ~ 6 m
2G
-1
Described gas hydrate generates the preparation method of promoter, is surfactant solution and hydrophobic particles high-speed stirred are disperseed to obtain gas hydrate generation promoter; The rotating speed of said high-speed stirred is controlled at 1500 ~ 20000 rpm, and mixing time is 0.5 ~ 2 min.
Said surfactant is anion surfactant, cationic surfactant or non-ionic surface active agent.
Said hydrophobic particles is the particle behind the hydrophobically modified; Said particle is more than one in silica, titanium dioxide, titanium sesquioxide, aluminium oxide, zinc oxide, calcium carbonate, imvite, diatomite, flyash, zeolite, talcum, the mica.Preferred hydrophobicity gas phase nano silica HB630.
The mass fraction of surfactant is 0.01% ~ 0.50% in the said promoter; The mass fraction of hydrophobic particles is 3% ~ 20% in the promoter, and all the other are water.
Surfactant mass fraction in the dried solution is 0.01% ~ 0.50%, preferred 0.03% ~ 0.10%; Hydrophobicity gas phase nano silica quality mark is 3% ~ 20%, preferred 5% ~ 10%; All the other are water.
Gas hydrate according to the invention generates the preparation method of promoter; Be with after the strong-hydrophobicity solids mix with surfactant solution; Shear dispersion in the agitator high speed and process dried solution, agitator speed is controlled at 1500 ~ 20000 rpm, and mixing time is 0.5 ~ 2 min.
Gas hydrate of the present invention generates the application of promoter in gas hydrate becomes.
Application in gas hydrate may further comprise the steps:
(1) promoter for preparing is joined in the autoclave;
(2) kettle and pipeline are evacuated to below 0.01 MPa, regulating temperature is-10 ~ 20 ℃, feeds gas and makes reacting kettle inner pressure be controlled at 0.5 ~ 12 MPa, observes the variation of temperature and pressure in the hydro-combination process.
The present invention is with respect to advantage and beneficial effect that prior art had.
Gas hydrate of the present invention generates promoter; Realized high degree of dispersion to surfactant solution; Specific area increases than the specific area of state of aggregation solution greatly, and surfactant impels hydrate in growth course, to form porous branch shape film, so dried solution increases the solution-air contact area in the hydrate generative process; Shorten the hydration induction time, generation and the raising gas-storing capacity that quickens gas hydrate had remarkable result.Dried solution quickens the generation of gas hydrate; Show mainly after hydration temperature, the pressure stability that after a few minutes, gas hydrate just begins to generate, and begins generation phase at hydrate; Pressure sharply descends; Hydration reaction end in tens of minutes again afterwards, system temperature, pressure tend towards stability once more, and gas-storing capacity is near desirable gas-storing capacity.With in the past the static contact method of ice powder, add surfactant method, porous media completion method, bubble method of perturbation, mechanical mixing method etc. and strengthen the hydration compared with techniques; Hydration induction time and reaction time are obviously shortened in the dried solution gas storage of surfactant, improve gas-storing capacity.
The dried solution of surfactant of the present invention is that the surfactant solution of certain mass proportioning and strong-hydrophobicity solids are sheared a kind of dried, pulverous, the flowable mixture of disperseing the back to form in the high-intensity stirrer high speed, have that cost is low, preparation is easy to use characteristics.Utilize trunk solution storing carbon dioxide, hydrogen sulfide, hydrogen, nitrogen, oxygen, alkanes gas, rare gas and their gaseous mixture etc.; Hydration rate and gas-storing capacity have been improved greatly; And avoided the required energy consumption of mechanical agitation; Method is simply suitable, for the accumulating of global energy gas and carbon dioxide discharge-reduction work provide new technical support.
The specific embodiment
Through embodiment the present invention is further set forth below.
Surfactant in the embodiment of the invention can be one or more of anion surfactant, cationic surfactant and non-ionic surface active agent; Lauryl sodium sulfate (SDS) solution with mass fraction 0.03%, 0.05%, 0.10% is example, but is not limited to this.The strong-hydrophobicity solids are one or more in the particles such as the silica, titanium dioxide, titanium sesquioxide, aluminium oxide, zinc oxide, calcium carbonate, imvite, diatomite, flyash, zeolite, talcum, mica behind the hydrophobically modified; With mass fraction is that 5%, 7.5%, 10% hydrophobicity gas phase nano silica HB630 is an example, but is not limited to this.Agitator speed is controlled to be 18000 rpm, and mixing time is 1 min.Gas can be carbon dioxide, hydrogen sulfide, hydrogen, nitrogen, oxygen, alkanes gas, rare gas and their gases such as gaseous mixture, is example with methane and carbon dioxide, but is not limited to this.
Embodiment 1
The dried solution of preparation lauryl sodium sulfate (SDS), wherein the SDS mass fraction is 0.03%, hydrophobicity gas phase nano silica HB630 mass fraction is 5%.Taking by weighing the dried solution of 15.00 g, to put into dischargeable capacity be 300 cm
3In the autoclave, agitated reactor and connecting line thereof are vacuumized, vacuum is reached below 0.01 MPa.Feed methane gas then, 1 ℃ of conditioned reaction still temperature, pressure 6 MPa carry out the constant volume reaction.Behind constant 15 min of temperature and pressure, temperature in the kettle begins to rise, and pressure obviously reduces, and methane hydrate begins to generate, experience 35 min again after, temperature in the kettle, pressure level-off, methane hydrate generate and finish.Begin to be generated to hydration reaction from methane hydrate and finish, the whole process time spent is less than 1 h, obviously shorten than the time with pure water synthesizing methane hydrate under the same experimental conditions, and the approaching desirable gas-storing capacity of gas-storing capacity.
Embodiment 2
The dried solution of preparation lauryl sodium sulfate (SDS), wherein the SDS mass fraction is 0.05%, hydrophobicity gas phase nano silica HB630 mass fraction is 7.5%.Taking by weighing the dried solution of 15.00 g, to put into dischargeable capacity be 300 cm
3In the autoclave, agitated reactor and connecting line thereof are vacuumized, vacuum is reached below 0.01 MPa.Feed methane gas then, 1 ℃ of conditioned reaction still temperature, pressure 6 MPa carry out the constant volume reaction.Behind constant 8 min of temperature and pressure, temperature in the kettle begins to rise, and pressure obviously reduces, and methane hydrate begins to generate, experience 25 min again after, temperature in the kettle, pressure level-off, methane hydrate generate and finish.Begin to be generated to hydration reaction from methane hydrate and finish, about whole process time spent 0.5 h, obviously shorten than the time with pure water synthesizing methane hydrate under the same experimental conditions, and the approaching desirable gas-storing capacity of gas-storing capacity.
Embodiment 3
The dried solution of preparation lauryl sodium sulfate (SDS), wherein the SDS mass fraction is 0.10%, hydrophobicity gas phase nano silica HB630 mass fraction is 10%.Taking by weighing the dried solution of 15.00 g, to put into dischargeable capacity be 300 cm
3In the autoclave, agitated reactor and connecting line thereof are vacuumized, vacuum is reached below 0.01 MPa.Feed methane gas then, 1 ℃ of conditioned reaction still temperature, pressure 6 MPa carry out the constant volume reaction.Behind constant 18 min of temperature and pressure, temperature in the kettle begins to rise, and pressure obviously reduces, and methane hydrate begins to generate, experience 33 min again after, temperature in the kettle, pressure level-off, methane hydrate generate and finish.Begin to be generated to hydration reaction from methane hydrate and finish, the whole process time spent is less than 1 h, obviously shorten than the time with pure water synthesizing methane hydrate under the same experimental conditions, and the approaching desirable gas-storing capacity of gas-storing capacity.
Embodiment 4
The dried solution of preparation lauryl sodium sulfate (SDS), wherein the SDS mass fraction is 0.03%, hydrophobicity gas phase nano silica HB630 mass fraction is 5%.Taking by weighing the dried solution of 15.00 g, to put into dischargeable capacity be 300 cm
3In the autoclave, agitated reactor and connecting line thereof are vacuumized, vacuum is reached below 0.01 MPa.Feed carbon dioxide then, 1 ℃ of conditioned reaction still temperature, pressure 3 MPa carry out the constant volume reaction.Behind constant 12 min of temperature and pressure, temperature in the kettle begins to rise, and pressure obviously reduces, and methane hydrate begins to generate, experience 28 min again after, temperature in the kettle, pressure level-off, titanium dioxide pool hydrate generate and finish.Begin to be generated to hydration reaction from carbon dioxide hydrate and finish, the whole process time spent is less than 1 h, obviously shorten than the time with the synthetic carbon dioxide hydrate of pure water under the same experimental conditions, and gas-storing capacity is near desirable gas-storing capacity.
Embodiment 5
The dried solution of preparation lauryl sodium sulfate (SDS), wherein the SDS mass fraction is 0.05%, hydrophobicity gas phase nano silica HB630 mass fraction is 7.5%.Taking by weighing the dried solution of 15.00 g, to put into dischargeable capacity be 300 cm
3In the autoclave, agitated reactor and connecting line thereof are vacuumized, vacuum is reached below 0.01 MPa.Feed carbon dioxide then, 1 ℃ of conditioned reaction still temperature, pressure 3 MPa carry out the constant volume reaction.Behind constant 6 min of temperature and pressure, temperature in the kettle begins to rise, and pressure obviously reduces, and methane hydrate begins to generate, experience 23 min again after, temperature in the kettle, pressure level-off, titanium dioxide pool hydrate generate and finish.Begin to be generated to hydration reaction from carbon dioxide hydrate and finish, the whole process time spent is less than 0.5 h, obviously shorten than the time with the synthetic carbon dioxide hydrate of pure water under the same experimental conditions, and gas-storing capacity is near desirable gas-storing capacity.
Embodiment 6
The dried solution of preparation lauryl sodium sulfate (SDS), wherein the SDS mass fraction is 0.10%, hydrophobicity gas phase nano silica HB630 mass fraction is 10%.Taking by weighing the dried solution of 15.00 g, to put into dischargeable capacity be 300 cm
3In the autoclave, agitated reactor and connecting line thereof are vacuumized, vacuum is reached below 0.01 MPa.Feed carbon dioxide then, 1 ℃ of conditioned reaction still temperature, pressure 3 MPa carry out the constant volume reaction.Behind constant 10 min of temperature and pressure, temperature in the kettle begins to rise, and pressure obviously reduces, and methane hydrate begins to generate, experience 25 min again after, temperature in the kettle, pressure level-off, titanium dioxide pool hydrate generate and finish.Begin to be generated to hydration reaction from carbon dioxide hydrate and finish, about whole process time spent 0.5 h, obviously shorten than the time with the synthetic carbon dioxide hydrate of pure water under the same experimental conditions, and gas-storing capacity is near desirable gas-storing capacity.
Claims (10)
1. gas hydrate generates promoter, it is characterized in that, consists of surfactant, water and hydrophobic particles; Hydrophobic particles is wrapped in the surfactant solution surface, forms droplet.
2. gas hydrate according to claim 1 generates promoter, it is characterized in that said surfactant is anion surfactant, cationic surfactant or non-ionic surface active agent.
3. gas hydrate according to claim 1 generates promoter, it is characterized in that said hydrophobic particles is the particle behind the hydrophobically modified; Said particle is more than one in silica, titanium dioxide, titanium sesquioxide, aluminium oxide, zinc oxide, calcium carbonate, imvite, diatomite, flyash, zeolite, talcum, the mica.
4. preparation method according to claim 1 is characterized in that, the mass fraction of surfactant is 0.01% ~ 0.50% in the said promoter; The mass fraction of hydrophobic particles is 3% ~ 20% in the promoter, and all the other are water.
5. gas hydrate according to claim 1 generates promoter, it is characterized in that the size of said droplet is between 1 ~ 20 μ m, and specific area is at 0.3 ~ 6 m
2G
-1
6. the described gas hydrate of one of claim 1-5 generates the preparation method of promoter, it is characterized in that, surfactant solution and hydrophobic particles high-speed stirred are disperseed to obtain gas hydrate generation promoter; The rotating speed of said high-speed stirred is controlled at 1500 ~ 20000 rpm, and mixing time is 0.5 ~ 2 min.
7. preparation method according to claim 6 is characterized in that, said surfactant is anion surfactant, cationic surfactant or non-ionic surface active agent.
8. preparation method according to claim 6 is characterized in that, said hydrophobic particles is the particle behind the hydrophobically modified; Said particle is more than one in silica, titanium dioxide, titanium sesquioxide, aluminium oxide, zinc oxide, calcium carbonate, imvite, diatomite, flyash, zeolite, talcum, the mica.
9. preparation method according to claim 6 is characterized in that, the mass fraction of surfactant is 0.01% ~ 0.50% in the said promoter; The mass fraction of hydrophobic particles is 3% ~ 20% in the promoter, and all the other are water.
10. the described gas hydrate of one of claim 1-5 generates the application of promoter in hydrate generates.
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| CN110564472A (en) * | 2019-08-22 | 2019-12-13 | 湘南学院 | Method for inhibiting hydrate decomposition and hydrate storage and transportation method |
| CN110564472B (en) * | 2019-08-22 | 2020-10-16 | 湘南学院 | Method for inhibiting hydrate decomposition and hydrate storage and transportation method |
| CN113817443A (en) * | 2020-06-18 | 2021-12-21 | 中国石油化工股份有限公司 | Hydrate decomposition inhibiting composition, coupling enhanced solid hydrate and method for enhancing storage and transportation stability of solid hydrate |
| CN113817441A (en) * | 2020-06-18 | 2021-12-21 | 中国石油化工股份有限公司 | Hydrate accelerant composition containing nano particles, application thereof and preparation method of hydrate |
| CN113817440A (en) * | 2020-06-18 | 2021-12-21 | 中国石油化工股份有限公司 | Compound hydrate accelerant, application and gas storage and transportation method |
| CN113817443B (en) * | 2020-06-18 | 2022-08-30 | 中国石油化工股份有限公司 | Hydrate decomposition inhibiting composition, coupling enhanced solid hydrate and method for enhancing storage and transportation stability of solid hydrate |
| CN113817441B (en) * | 2020-06-18 | 2022-11-08 | 中国石油化工股份有限公司 | Hydrate accelerant composition containing nano particles, application thereof and preparation method of hydrate |
| CN114591770A (en) * | 2022-01-26 | 2022-06-07 | 中冶南方工程技术有限公司 | Coal-based natural gas hydrate slurry and preparation method thereof |
| CN115490203A (en) * | 2022-09-21 | 2022-12-20 | 中国科学院广州能源研究所 | Method for promoting hydrate hydrogen storage by using solid nanoparticles |
| CN115490203B (en) * | 2022-09-21 | 2024-04-30 | 中国科学院广州能源研究所 | Method for promoting hydrate hydrogen storage by using solid nano particles |
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