CN101074361A - Efficient composite hydrate inhibitor - Google Patents
Efficient composite hydrate inhibitor Download PDFInfo
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- CN101074361A CN101074361A CN 200710028224 CN200710028224A CN101074361A CN 101074361 A CN101074361 A CN 101074361A CN 200710028224 CN200710028224 CN 200710028224 CN 200710028224 A CN200710028224 A CN 200710028224A CN 101074361 A CN101074361 A CN 101074361A
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Abstract
An efficient composite hydrate inhibitor is stable and economical. Salt or alcohol is added into dynamic inhibitor. It has less hydrate and longer generating time, wide applied range and no environmental pollution.
Description
Technical field:
The present invention relates to the hydrate inhibitor technical field, particularly efficient composite hydrate inhibitor.
Background technology:
In Sweet natural gas and other petroleum fluids, when various lower boiling hydrocarbons such as methane, ethane, propane and carbonic acid gas, hydrogen sulfide etc. exist simultaneously with water, under certain temperature and pressure, be easy to generate similar ice shape crystalline hydrate, when serious, these hydrates can stop up pit shaft, pipeline, valve and equipment, thereby influence the normal operation of gas extraction, transportation and processing, therefore, the control of gas hydrate has become the emphasis to its research.Various lower boiling hydrocarbons such as methane, ethane, propane and carbonic acid gas, hydrogen sulfide etc. are present in Sweet natural gas and other petroleum fluids, under certain temperature and pressure, be easy to the oil and natural gas fluid in water generate have a cage structure seemingly ice shape crystalline hydrate.General gas hydrate could generate in temperature below freezing, but, generate above freezing also being easy to, for example under the pressure of about 1MPa along with the increase of pressure, ethane can form hydrate being lower than under 4 ℃ the temperature, and just can form hydrate below 14 ℃ under the pressure of 3MPa.Hydrate generates easily in following situation in oil and gas industry: 1, in the oil gas well mining process, because the variation of physical condition may form hydrate; 2, in the natural gas transportation and the course of processing, when especially containing saturated steam in the output gas; 3, run into arctic weather and be easy to generate the easy hydrate that forms in the gas hydrate sea-bottom oil-gas transport pipeline; 4, form gas hydrate in the drilling fluid easily; 5, in the very low temperature liquefaction sepn process of Sweet natural gas, also form hydrate easily.
In a single day hydrate forms, and its harm is catastrophic: line clogging, high pressure gas are blasted, and cause hydrocarbon seepage, even can cause the mineral reserve blast.Not only cause enormous economic loss, also can produce serious environmental and pollute, serious threat is to halobiontic life, and therefore, hydrate has become one of oil and gas industry to threaten greatly.Develop effective hydrate inhibitor and have crucial meaning.
Chemical inhibitor mainly can be divided three classes: thermodynamics inhibitor, kinetic inhibitor, anti polymerizer.Thermodynamics inhibition method is exactly by changing balancing each other of hydrate, makes it towards being unfavorable for that the direction that hydrate generates moves, and it mainly is by the water in the system of removing, rising system temperature, reduces means such as system pressure and realize.The consumption of thermodynamics inhibitor is generally 20～30% (with respect to the quality of water in the system), has shortcomings such as consumption is big, cost is high, strong toxicity, can not satisfy present demand.Kinetics inhibition method is exactly to suppress or postpone the growth time of hydrate by adding a certain amount of kinetic inhibitor, suppresses the purpose that hydrate generates thereby reach.The concentration that this class inhibitor adds is very low, and it does not influence the thermodynamic condition that hydrate generates, but can postpone the nucleation of hydrate and the time of crystal growth under the thermodynamic condition that hydrate forms, and the hydrate latch up phenomenon do not occur.Kinetic inhibitor action effect under the situation that pipeline (or oil well) seals or Δ T is bigger is not very desirable.Anti polymerizer is to prevent the coalescent of hydrate crystal grain by adding very low tensio-active agent of some concentration or polymkeric substance, to avoid stopping up the oil gas transport line.Though anti polymerizer can not stop the formation of gas hydrate in the pipeline, it can make the gas hydrate of generation be difficult to be agglomerated into piece.Anti polymerizer can be worked under the situation that pipeline (or oil well) seals or Δ T is bigger, but its action effect is not really desirable.
Summary of the invention:
The objective of the invention is provides efficient composite hydrate inhibitor at the deficiencies in the prior art.
For achieving the above object, the present invention adopts following technical scheme:
It is mixed by kinetic inhibitor and salt or alcohols, and during use, with respect to the mass percent of water in the system, the consumption of kinetic inhibitor is 0.3～1%, and the consumption of salt or alcohol is 1～8%.
Wherein, kinetic inhibitor, can adopt following a few class:
(1) acylamide polymer is as PAM (polyacrylamide), PEAM (poly-N-ethyl acrylamide), PDEAM (poly-N, N-diethyl acrylamide), PDMAM (poly-N,N-DMAA) and PAPYD (polypropylene acyl group tetramethyleneimine).
(2) ketone polymkeric substance is as Polyvinylpyrolidone (PVP) (PVP).
(3) imines base polymer is as polyvinyl-suitable divinyl imide, poly-N-acyl group imines.
(4) organic salt is as alkyl aryl sulphonic acid and an alkali metal salt thereof, ammonium salt.
(5) copolymer analog, as VC-73 (dimethylamino ethyl methacrylate, vinyl pyrrolidone, caprolactam terpolymer), VC/VP (vinyl pyrrolidone is pressed the multipolymer that caprolactam forms at 1: 1), (1-butylene, 1-hexene, 1-decene, vinylchlorid, ethene) guanidine-acetic acid salt (or ester), ethyl propenoate, 2-ethylhexyl acrylate (or ester), styrol copolymer.
Salt can adopt sodium-chlor, calcium chloride, sodium sulfate, one or more in calcium sulfate, the ammonium chloride.
Alcohols can adopt one or more in methyl alcohol, ethylene glycol, Virahol, the glycol ether.
The present invention compares with pure kinetic inhibitor has following characteristics:
(1) action effect is good: pure kinetic inhibitor can only prolong the rise time of hydrate, can not reduce the growing amount of hydrate, and concentration also has promoter action less than 5% salt and pure generation to hydrate, and the rise time (than pure kinetic inhibitor longer) of composite inhibitor hydrate except prolonging hydrate, can also reduce the growing amount of hydrate, its action effect has obtained reinforcement from two aspects, makes the more difficult obstruction pipeline of hydrate of generation.In addition, the amount increase along with salt and alcohol suppresses the effect enhancing, and when the amount of salt or alcohol surpassed 8%, the amplification of inhibition effect reduced, and considered from the angle of economy, and the addition of salt or alcohol is generally 1～8% in the medium power inhibitor of the present invention.
(2) application is more extensive: the problem that pure kinetic inhibitor faces in application is to suppress active on the low side, it is bigger to be affected by the external environment, versatility is poor, application has very big limitation, because the effect of compound inhibitor improves greatly, and can also reduce the generation of hydrate, therefore more stable, versatility is stronger.
(3) cost is lower, more economical: salt and alcohol that the selected additive of the present invention is some cheapnesss, be easy to get, and addition is also little, and the consumption of composite back kinetic inhibitor can be lower, so just greatly reduces gas industries and is used to suppress the cost that hydrate generates.
The present invention adds certain salt or alcohols in existing kinetic inhibitor, it is longer when not only the rise time of hydrate (reaction induction time and deadline) is than independent the use, and can also reduce the growing amount of hydrate, improved the inhibition effect of kinetic inhibitor widely, make kinetic inhibitor better effects if, more stable, range of application is more extensive.
Embodiment:
Below the present invention is further described in detail, but embodiments of the present invention are not limited to this.
Kinetic inhibitor is some water-soluble or aqueous dispersion polymers, and they only suppress the formation of hydrate at aqueous phase, the concentration of adding very low (at aqueous phase usually less than 1%), and it does not influence the thermodynamic condition that hydrate generates.At the initial stage of crystal of hydrate nucleation and growth, they are adsorbed in the surface of hydrate particle, the ring texture of inhibitor is by the crystal combination of hydrogen bond and hydrate, delay the hydrate crystal nucleation time or stop crystalline further to be grown up, fluid is lower than hydrate-formation temperature (promptly at certain condensate depression Δ t) current downflow in its temperature in the pipeline thereby make, and the hydrate latch up phenomenon do not occur.The problem that kinetic inhibitor faces in application is to suppress active on the low side, and it is bigger to be affected by the external environment.
The present invention adopts cryogenic high pressure band visor suspension stirring test device as experimental installation, this equipment mainly partly is made up of the autoclave of being with visor, magnetic stirring apparatus, supercharging device, gas cold-trap/cold cycle groove, camera system etc., provide low temperature environment by the cold cycle groove, hydrate carries out in autoclave, reactor has visor, response situation in the still can be observed by supporting camera, experimental data and image can be gathered in real time by computer.The operating pressure of this system is 0～20MPa, and temperature range is-10～120 ℃.The formation of hydrate can be judged by the temperature in visual form direct viewing and when reaction or the variation of pressure.The action effect of kinetic inhibitor can judge that the time is long more according to the induction time and the reaction deadline of hydrate, and the effect of inhibitor is good more.In addition, the amount that hydrate generates is few more, is not easy to block pipeline more, and effect is good more.
The condition of reaction beginning is 0 ℃, the pressure of 5.8Mpa, and the equilibrium pressure that the methane hydrate of reaction generates in the time of 0 ℃ is 2.6Mpa.Before the reaction beginning, use the clean reactor of deionized water and washed with methanol successively, after the vacuum-drying, 40ml deionized water or the mixed solution that is added with inhibitor are added reactor, in order to get rid of the air in the still, feed reactant gases earlier: the methane of purity 99.99%, when the pressure in the still is raised to 1Mpa, discharge gas, three times repeatedly, finish aforesaid operations after, temperature in the still is cooled to 0 ℃, feed methane (cooling off in advance before entering autoclave), make the pressure in the still reach 5.8Mpa, begin stirring and make it to keep 300rmp, because methane is water-soluble, so at this moment the pressure in the still slightly descends, pressure reaches 4.2Mpa, after reaction reaches balance, react the amount of the methane that is consumed by pressure drop.It is that induction time is 33min that pure water hydrate under these conditions begins to generate the required time, and the reaction deadline is 145min, and the pressure in the reaction is reduced to 0.9Mpa.
Below be several embodiment of the present invention:
Embodiment one
The compound kinetic inhibitor of selecting for use consists of: kinetic inhibitor is Polyvinylpyrolidone (PVP) (PVP), the quality percentage composition (refers to account for aqueous mass percent in the system by 0.5%, below all with), sodium-chlor is by 3% (refer to account for aqueous mass percent in the system, below all with); Experimental procedure as above, the result shows, the induction time that contains the system hydrate of 0.5%PVP is 84min, reaction deadline 276min, the pressure of methane gas is reduced to 0.8Mpa, and the induction time that contains this compound type inhibitor system is 100min, reaction deadline 355min, the pressure of methane gas is reduced to 0.5Mpa, and the rejection of PVP obviously improves behind the sodium-chlor of adding 5%.
Embodiment two
The compound kinetic inhibitor of selecting for use consists of: kinetic inhibitor is Polyvinylpyrolidone (PVP) (PVP), and the quality percentage composition is 0.5%, and sodium-chlor is 5%; Experimental procedure as above, the result shows, the induction time that contains the system hydrate of 0.5%PVP is 84min, reaction deadline 276min, the pressure of methane gas is reduced to 0.8Mpa, and the induction time that contains this compound type inhibitor system is 140min, reaction deadline 377min, the pressure of methane gas is reduced to 0.4Mpa, and it suppresses effect and obviously improves.
Embodiment three
The compound kinetic inhibitor of selecting for use consists of: kinetic inhibitor is Polyvinylpyrolidone (PVP) (PVP), and the quality percentage composition is 0.5%, and sodium-chlor is 8%; Experimental procedure as above, the result shows, the induction time that contains the system hydrate of 0.5%PVP is 84min, reaction deadline 276min, the pressure of methane gas is reduced to 0.85Mpa, and the induction time that contains this compound type inhibitor system is 155min, reaction deadline 360min, the pressure of methane gas is reduced to 0.35Mpa, and it suppresses effect and obviously improves.
Embodiment four
The compound kinetic inhibitor of selecting for use consists of: kinetic inhibitor is Polyvinylpyrolidone (PVP) (PVP), and the quality percentage composition is 1%, and sodium-chlor is 5%; Experimental procedure as above, the result shows, the induction time that contains the system hydrate of i%PVP is 126min, reaction deadline 336min, the pressure of methane gas is reduced to 0.80Mpa, and the system induction time that contains this compound type inhibitor system is 198min, reaction deadline 403min, the pressure of methane gas is reduced to 0.41Mpa, and it suppresses effect and obviously improves.
Embodiment five
The compound kinetic inhibitor of selecting for use consists of: kinetic inhibitor is Polyvinylpyrolidone (PVP) (PVP), and the quality percentage composition is 1%, and methyl alcohol is 5%; Experimental procedure as above, the result shows, the induction time that contains the system hydrate of 1%PVP is 126min, reaction deadline 336min, the pressure of methane gas is reduced to 0.80Mpa, and the induction time that contains this compound type inhibitor system is 189min, reaction deadline 398min, the pressure of methane gas is reduced to 0.39Mpa, and it suppresses effect and obviously improves.
Embodiment six
The compound kinetic inhibitor of selecting for use consists of: kinetic inhibitor is poly-N-ethyl acrylamide (PEAM), and the quality percentage composition is 1%, and sodium-chlor is 5%; Experimental procedure as above, the result shows, the induction time that contains the system hydrate of 1%PEAM is 100min, reaction deadline 258min, the pressure of methane gas is reduced to 0.82Mpa, and the induction time that contains this compound type inhibitor system is 161min, reaction deadline 397min, the pressure of methane gas is reduced to 0.41Mpa, and it suppresses effect and obviously improves.
Embodiment seven
The compound kinetic inhibitor of selecting for use consists of: kinetic inhibitor is poly-N-ethyl acrylamide (PEAM), and the quality percentage composition is 1%, and methyl alcohol is 5%; Experimental procedure as above, the result shows, the induction time that contains the system hydrate of 1%PEAM is 100min, reaction deadline 258min, the pressure of methane gas is reduced to 0.82Mpa, and the induction time that contains this compound type inhibitor system is 162min, reaction deadline 369min, the pressure of methane gas is reduced to 0.38Mpa, and it suppresses effect and obviously improves.
Embodiment eight
The compound kinetic inhibitor of selecting for use consists of: kinetic inhibitor is the hexadecyl Phenylsulfonic acid, and the quality percentage composition is 1%, and sodium-chlor is 5%; Experimental procedure as above, the result shows, the induction time that contains the system hydrate of 1% hexadecyl Phenylsulfonic acid is 82min, reaction deadline 186min, the pressure of methane gas is reduced to 0.8Mpa, and contains the induction time 138min of compound type inhibitor system, reaction deadline 287min, the pressure of methane gas is reduced to 0.42Mpa, and it suppresses effect and obviously improves.
Embodiment nine
The compound kinetic inhibitor of selecting for use consists of: kinetic inhibitor is the hexadecyl Phenylsulfonic acid, and the quality percentage composition is 1%, and methyl alcohol is 5%; Experimental procedure as above, the result shows, the induction time that contains the system hydrate of 1% hexadecyl Phenylsulfonic acid is 82min, reaction deadline 186min, the pressure of methane gas is reduced to 0.8Mpa, and the induction time that contains compound type inhibitor system is 151min, reaction deadline 302min, the pressure of methane gas is reduced to 0.38Mpa, and it suppresses effect and obviously improves.
Embodiment ten
The compound kinetic inhibitor of selecting for use consists of: kinetic inhibitor is VC-73 (dimethylamino ethyl methacrylate, vinyl pyrrolidone, a caprolactam terpolymer), and the quality percentage composition is 1%, and sodium-chlor is 5%; Experimental procedure as above, the result shows, the induction time that contains the system hydrate of 1%VC-73 is 142min, reaction deadline 340min, the pressure of methane gas is reduced to 0.81Mpa, is 183min and contain compound type inhibitor system induction time, reaction deadline 412min, the pressure of methane gas is reduced to 0.4Mpa, and it suppresses effect and obviously improves.
Embodiment 11
The compound kinetic inhibitor of selecting for use consists of: kinetic inhibitor is VC-73 (dimethylamino ethyl methacrylate, vinyl pyrrolidone, a caprolactam terpolymer), and the quality percentage composition is 1%, and methyl alcohol is 5%; Experimental procedure as above, the result shows, the induction time that contains the system hydrate of 1%VC-73 is 142min, reaction deadline 340min, the pressure of methane gas is reduced to 0.81Mpa, is 180min and contain compound type inhibitor system induction time, reaction deadline 394min, the pressure of methane gas is reduced to 0.38Mpa, and it suppresses effect and obviously improves.
Embodiment 12
The compound kinetic inhibitor of selecting for use consists of: kinetic inhibitor is VC-73 (dimethylamino ethyl methacrylate, vinyl pyrrolidone, a caprolactam terpolymer), and the quality percentage composition is 1%, and ammonium chloride is 5%; Experimental procedure as above, the result shows, the induction time that contains the system hydrate of 1%VC-73 is 142min, reaction deadline 340min, the pressure of methane gas is reduced to 0.81Mpa, is 171min and contain this compound type inhibitor system induction time, reaction deadline 402min, the pressure of methane gas is reduced to 0.43Mpa, and it suppresses effect and obviously improves.
Claims (8)
1, efficient composite hydrate inhibitor is characterized in that: it is mixed by kinetic inhibitor and salt or alcohols, and during use, with respect to the mass percent of water in the system, the consumption of kinetic inhibitor is 0.3～1%, and the consumption of salt or alcohol is 1～8%.
2, efficient composite hydrate inhibitor according to claim 1; it is characterized in that: kinetic inhibitor is an acylamide polymer; as polyacrylamide, poly-N-ethyl acrylamide, poly-N, N-diethyl acrylamide, poly-N,N-DMAA and polypropylene acyl group tetramethyleneimine.
3, efficient composite hydrate inhibitor according to claim 1 is characterized in that: kinetic inhibitor is the ketone polymkeric substance, as Polyvinylpyrolidone (PVP).
4, efficient composite hydrate inhibitor according to claim 1 is characterized in that: kinetic inhibitor is the imines base polymer, as polyvinyl-suitable divinyl imide, poly-N-acyl group imines.
5, efficient composite hydrate inhibitor according to claim 1 is characterized in that: kinetic inhibitor is an organic salt, as alkyl aryl sulphonic acid and an alkali metal salt thereof, ammonium salt.
6, efficient composite hydrate inhibitor according to claim 1, it is characterized in that: kinetic inhibitor is a copolymer analog, press the multipolymer that caprolactam forms at 1: 1, acetate or ester, ethyl propenoate, 2-ethylhexyl acrylate or ester, styrol copolymer as dimethylamino ethyl methacrylate, vinyl pyrrolidone, caprolactam terpolymer, vinyl pyrrolidone.
7, efficient composite hydrate inhibitor according to claim 1 is characterized in that: salt can be sodium-chlor, Repone K, calcium chloride, sodium sulfate, one or more in calcium sulfate, the ammonium chloride.
8, efficient composite hydrate inhibitor according to claim 1 is characterized in that: alcohol is one or more in methyl alcohol, ethylene glycol, Virahol, the glycol ether.
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| CN101544817B (en) * | 2009-04-28 | 2011-04-13 | 中国石油大学(北京) | Composition for enhancing hydrate inhibition effect and method for inhibiting formation of hydrate |
| CN102190750A (en) * | 2011-04-21 | 2011-09-21 | 华南理工大学 | Copolymer of styrene and N-vinyl pyrrolidone, and preparation method and application thereof |
| CN101691905B (en) * | 2009-10-13 | 2013-02-13 | 华南理工大学 | Hydrate inhibitor applicable to high moisture content system |
| CN103242484A (en) * | 2013-05-16 | 2013-08-14 | 西南石油大学 | Propenol/N-vinyl pyrrolidone copolymer and preparation method thereof |
| CN103305200A (en) * | 2013-05-09 | 2013-09-18 | 常州大学 | Compound type hydrate inhibitor |
| CN104293326A (en) * | 2014-10-09 | 2015-01-21 | 中国石油大学(华东) | Composite natural gas hydrate inhibitor for drilling fluid |
| CN104864266A (en) * | 2015-05-07 | 2015-08-26 | 中国海洋石油总公司 | Unimolecular hydrate inhibitor |
| CN105542731A (en) * | 2016-01-25 | 2016-05-04 | 中国科学院广州能源研究所 | Drilling fluid with aquo-complex inhabitation performance |
| CN105859963A (en) * | 2016-04-15 | 2016-08-17 | 西南石油大学 | Polycyclic polymerized natural gas hydrate dynamic inhibitor and preparation method |
| CN106190060A (en) * | 2015-05-25 | 2016-12-07 | 西北大学 | A kind of Compositional type hydrate inhibitor for natural gas |
| CN106468395A (en) * | 2016-09-09 | 2017-03-01 | 常州大学 | A kind of gas hydrate inhibitor and preparation method thereof |
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| CN101544817B (en) * | 2009-04-28 | 2011-04-13 | 中国石油大学(北京) | Composition for enhancing hydrate inhibition effect and method for inhibiting formation of hydrate |
| CN101691905B (en) * | 2009-10-13 | 2013-02-13 | 华南理工大学 | Hydrate inhibitor applicable to high moisture content system |
| CN102190750A (en) * | 2011-04-21 | 2011-09-21 | 华南理工大学 | Copolymer of styrene and N-vinyl pyrrolidone, and preparation method and application thereof |
| CN102190750B (en) * | 2011-04-21 | 2012-12-05 | 华南理工大学 | Copolymer of styrene and N-vinyl pyrrolidone, and preparation method and application thereof |
| CN103305200A (en) * | 2013-05-09 | 2013-09-18 | 常州大学 | Compound type hydrate inhibitor |
| CN103242484A (en) * | 2013-05-16 | 2013-08-14 | 西南石油大学 | Propenol/N-vinyl pyrrolidone copolymer and preparation method thereof |
| CN104293326A (en) * | 2014-10-09 | 2015-01-21 | 中国石油大学(华东) | Composite natural gas hydrate inhibitor for drilling fluid |
| CN104864266A (en) * | 2015-05-07 | 2015-08-26 | 中国海洋石油总公司 | Unimolecular hydrate inhibitor |
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| CN111499785A (en) * | 2020-04-30 | 2020-08-07 | 中海石油(中国)有限公司 | Natural gas hydrate inhibitor with hyperbranched structure and preparation method and application thereof |
| CN112877047A (en) * | 2021-01-27 | 2021-06-01 | 四川柏诗特能源科技有限公司 | Efficient prevention and control agent and process for solving low-temperature freezing and blocking of natural gas production pipeline |
| CN112877047B (en) * | 2021-01-27 | 2022-08-23 | 四川柏诗特能源科技有限公司 | Efficient prevention and control agent and process for solving low-temperature freezing and blocking of natural gas production pipeline |
| CN113388379A (en) * | 2021-07-21 | 2021-09-14 | 中国石油大学(北京) | Hydrate kinetic inhibitor and preparation method and application thereof |
| CN113388379B (en) * | 2021-07-21 | 2022-04-05 | 中国石油大学(北京) | Hydrate kinetic inhibitor and preparation method and application thereof |
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