CN105179942A - Compound hydrate inhibitor - Google Patents
Compound hydrate inhibitor Download PDFInfo
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- CN105179942A CN105179942A CN201510501019.9A CN201510501019A CN105179942A CN 105179942 A CN105179942 A CN 105179942A CN 201510501019 A CN201510501019 A CN 201510501019A CN 105179942 A CN105179942 A CN 105179942A
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Abstract
The invention discloses a compound hydrate inhibitor. The compound hydrate inhibitor is formed by mixing a copolymer, an emulgator and a dispersing agent. The copolymer is a mixture of one or more of polyvinylpyrrolidone, polyethylene caprolactam, polymethylacrylic acid and dimethylaminoethyl methacrylate. The emulgator is a polyhydric alcohol type non-ionic surface active agent. The dispersing agent is a quaternary ammonium salt compound. The copolymer with the dynamics inhibition performance is combined with the emulgator and the dispersing agent. Nucleation and growth of hydrate particles can be inhibited, and the purpose of dispersing the hydrate particles can also be achieved. The inhibitor can effectively inhibit the nucleation and the growth rate of a hydrate and can also achieve the purpose of preventing agglutination of the hydrate particles, and thus the flowing safety of an oil-gas-water three-phase delivery pipeline is effectively achieved. The compound hydrate inhibitor also has the advantages of being small in use amount, economical, environmentally friendly, efficient, excellent in performance and the like and has good application prospects.
Description
Technical field
The present invention relates to a kind of hydrate inhibitor, be specifically related to a kind of Compositional type hydrate inhibitor.
Background technique
Similar to ice crystal structure, gas hydrate is as CH by some low boiling point hydrocarbon gas molecule
4, C
2h
6, CO
2and H
2s etc., the non-stoichiometry crystal caged material formed under cryogenic high pressure condition with water molecule, the water molecule forming hydrate is called main body, and gas molecule is then called object.At oil-gas field development with the defeated process of collection, the high pressure special due to it and low temperature environment, very easily form crystal hydrate in parts such as valve, elbow, instrument, links, cause the underproduction, stop production even line fracture, causes oil gas to reveal befouling environment.Therefore, the research about gas hydrate risk prevention system technology is subject to the attention of oil and gas industry always, and gives the research of relevant hydrate Prevention Technique and support energetically.Hydrate prevention and controls mainly comprises conventional heat suppressing method and novel dynamic control method two class.
Traditional thermomechanics suppressing method is mainly through removing aqueous phase, heating pipeline, step-down and adding the methods such as hydrate thermodynamic inhibitor to change system hydrate thermomechanics formation condition, make hydrate generate pressure and generate temperature lower than pipeline delivery temperature higher than pipeline delivery pressure or hydrate, thus the formation of anhydrate in course of conveying.But above method exists larger shortcoming, such as, dehydration technique is difficult to aqueous phase in pipeline to eliminate completely, and may there be aqueous phase local, therefore still has larger blocking risk; Adopt the large usage quantity of thermodynamic inhibitor, be generally the 30vol%-50vol% of the system water yield, costly, and easily to environment etc.
Low dosage hydrate inhibitor is the new method of rising in recent years, and because the features such as its consumption is little, inhibition is obvious are subject to the attention of production of hydrocarbons and transportation department gradually, it mainly comprises kinetic inhibitor and hydrate polymerization inhibitor two class.Kinetic inhibitor does not change the thermodynamical equilibrium condition of gas hydrate synthesis, and hydrate growth of grain is slowly even stopped, and postpones the time of hydrate coring and increment, prevents hydrate grain growth.At the hydrate coring and increment initial stage, kinetic inhibitor is adsorbed in hydrate particle surface, the ring structure of Active agent is combined with hydrate crystal by hydrogen bond, thus prevents or delay hydrate crystal growth rate, and then ensures not block in course of conveying.From formed for the first time to hydrate crystal be called hydrate induction period during this period of time, it is stronger that longer explanation induction period inhibitor is suppressed to nuclear capability; Occur being called the hydrate growth phase during this period of time when being fully formed to hydrate from hydrate crystal, longer explanation in vegetative season inhibitor suppresses hydrate growth ability stronger.Hydrate polymerization inhibitor is some polymer and surface active agent, just can use under water-oil phase simultaneously existence condition.Hydrate polymerization inhibitor does not change the formation condition of hydrate equally, the formation of hydrate in permission system, but can control hydrate particle size, stops gathering and the deposition of hydrate particle, makes its finally conveying in stable slurry.Two kinds are had about what generally acknowledge in the current document of inhibition mechanism of hydrate polymerization inhibitor.The first inhibition mechanism is proposed by IFP, and they think that hydrate polymerization inhibitor is for some oil-water emulsion agent, not only can form even water-in-oil emulsion after interpolation, and can limit water droplet and be further converted to hydrate; The researcher of Shell Co. Ltd proposes the second inhibition mechanism, they have designed and synthesized a large amount of surface active agents with hydrophilic radical and lipophilic group, wherein, hydrophilic radical can effectively be adsorbed on hydrate crystal surface, upset the forming process of hydrate, and then slow down the growth of hydrate, and lipophilic group can change hydrate wettability of the surface, makes it easily be scattered in oil phase.
Single angle of Maximum subcoold temperature of mixing defeated system from hydrate inhibitor application system and oil-gas-water and can bear, hydrate polymerization inhibitor should be unique selection, but because hydrate polymerization inhibitor does not have a kinetic inhibition performance, during its individualism, at gas hydrate synthesis in earlier stage, because hydrate coring and increment speed is too fast, cause polymerization inhibitor molecule to have little time disperse water polymer beads, therefore in this stage, Hydrate Plugging situation very easily occurs.
In hydrate inhibitor exploitation, China Patent No. CN103305200A " a kind of composite hydrate inhibitor " relate to a kind of composite hydrate inhibitor, be made up of Vinylcaprolactam homopolymer, alcohol or salt and water, but such inhibitor affects comparatively large by system Subcoold temperature, and easily occurs when hydrate body integration rate is larger to build up caking phenomenon.In China Patent No. CN102451640A " a kind of Non-ionic compound hydrate anti-agglomerant ", a kind of hydrate polymerization inhibitor is proposed, by polyoxyethylene dicarboxylic acids lipid Shuangzi non-ionic surfactant agent and polyol-based non-ionic surfactant composite after obtain, shortcoming is that such polymerization inhibitor adding quantity is larger, and the hydrate slurry comparatively thickness formed under compared with high-moisture percentage condition, it is large to manage defeated pressure drag.China Patent No. CN101892038A " a kind of high-efficiency and environmentally-friendly hydrate inhibitor " proposes to inject by the mixture of kinetic inhibitor and nitrate, acetate the hydrocarbon fluids produced or carry, the object suppressing Hydrate Plugging can be played, but such inhibitor only can movement starting mechanics inhibition, the Subcoold temperature that can bear is less, when forming hydrate in system, namely polymerization inhibition effect is lost, application area critical constraints.The gemini quaternary ammonium salt that a class has hydrate polymerization inhibition performance has been synthesized in China Patent No. CN104262184A " gemini quaternary ammonium salt class anti polymerizer and synthetic method and suppression hydrate accumulation method " thereof, but shortcoming for such anti polymerizer be organic synthesis product, biological degradability and the economic feature of environmental protection poor, and adding quantity is comparatively large, and apply limited in high-moisture percentage system.
Summary of the invention
The problem that adding quantity is many, rejection is poor is there is for current hydrate inhibitor, the advantage of binding kinetics inhibitor of the present invention and hydrate polymerization inhibitor, a kind of Compositional type hydrate inhibitor and the method suppressing hydrate to be built up are provided, be applicable to oil-gas-water multi-phase mixed delivering system, there is the features such as low, the economic environmental protection of consumption, rejection be excellent.
A kind of Compositional type hydrate inhibitor, be made up of copolymer, emulsifier and dispersant, the mass ratio of copolymer, emulsifier and dispersing agent is 0.01 ~ 2:0.01 ~ 5:0.01 ~ 5.
Described copolymer is by polyvinyl-pyrrolidone (as shown in molecular formula a), Polyvinylcaprolactame (as shown in molecular formula b), polymethacrylic acid (as shown in molecular formula c), and one or more mixtures made in dimethylamino ethyl ester; Described emulsifier is polyol-based non-ionic surfactant; Described dispersing agent is quaternary ammonium compound.
A polyvinyl-pyrrolidone (PVP)
B Polyvinylcaprolactame (PVCap)
C polymethacrylic acid dimethylaminoethyl (PDMA)
In formula, L, M and N=(10-100)
Preferably, the mass ratio of copolymer, emulsifier and dispersing agent is 0.5 ~ 1:1 ~ 2:1 ~ 3.
Preferably, described quaternary ammonium compound is the mixture of one or more of TBAB, four pentyl ammonium bromide, the quaternary ammonium salt containing 2-3 normal-butyl, the quaternary ammonium salt containing 2-3 n-pentyl or the quaternary ammonium salt containing 2-3 isopentyl.
Preferably, described polyol-based non-ionic surfactant is Span series polyol-based non-ionic surfactant.
Preferably, described Span series polyol-based non-ionic surfactant is by the mixture of one or more in Span20, Span40, Span60, Span65, Span80 and Span85 polyol-based non-ionic surfactant.
The present invention also provides the using method of above-mentioned a kind of Compositional type hydrate inhibitor.
The using method of above-mentioned a kind of Compositional type hydrate inhibitor, is characterized in that, adds above-mentioned Compositional type hydrate inhibitor to oil-gas-water and mixes in defeated system, and the quality of the Compositional type hydrate inhibitor of interpolation is 0.1% ~ 10% of water gross mass; The temperature that oil-gas-water mixes defeated system controls at 253K-323K; Stress control is at 0.1MPa-50.0MPa; The volume that oil-gas-water mixes water in defeated system is no more than 60% of oil and water total volume.
Preferably, the quality of the Compositional type hydrate inhibitor of interpolation is 1% ~ 3% of water gross mass.
A kind of Compositional type hydrate inhibitor of the present invention, copolymer is polymeric compound, and water soluble, ethanol, chloroform and most organic solvent, toxicity is less.
The Span series polyol-based non-ionic surfactant that mentioned emulsifier adopts, because of the hydrophilic radical in its structure and long alkyl chain lipophilic group, make it easily be adsorbed in oil-water interfaces, reduce interfacial tension, for good oil-water emulsion agent, WO emulsion can be formed.
Above-mentioned quaternary ammonium salt dispersing agent, soluble in water, ethanol etc., after forming hydrate particle in oil-gas-water system, in dispersing agent, hydrophilic radical is adsorbed on hydrate particle surface, in dispersing agent, alkyl lipophilic group stretches in oil phase, thus the accumulation between prevention hydrate particle, make it be dispersed in oil phase.
Present invention also offers the inhibiting mechanism of above-mentioned Compositional type hydrate inhibitor.Owing to not having the ability of disperse water polymer beads when kinetic inhibitor is used alone, therefore its application area critical constraints.In addition, because hydrate polymerization inhibitor does not have a kinetic inhibition performance, during its individualism, at gas hydrate synthesis in earlier stage, because hydrate coring and increment speed is too fast, cause polymerization inhibitor molecule to have little time disperse water polymer beads, in this stage, Hydrate Plugging situation very easily occurs.Therefore, the present invention is undertaken composite by having the copolymer of kinetic inhibition performance and emulsifier and dispersing agent, both can suppress the coring and increment of hydrate particle, also can play the object of disperse water polymer beads.Its concrete inhibiting mechanism is: before gas hydrate synthesis, and under oil-water emulsion agent effect, oil-gas-water system is that even water in oil emulsion exists, and the copolymer with kinetic inhibition effect is adsorbed in oil-water interfaces, can play the object suppressing hydrate nucleation; Along with the formation of hydrate shell, copolymer molecule is adsorbed on shell layer surface, cause growth of grain reduced rate, enough time is provided for quaternary ammonium salt dispersing agent plays its dispersibility, final under dispersing agent effect, hydrate is dispersed in oil phase with granule, in stablizing slurry conveying, blocking phenomenon of luming does not occur.
The present invention compared with prior art, has following beneficial effect:
A kind of Compositional type hydrate inhibitor of the present invention is compared with currently available technology, can overcome that conventional heat inhibitor consumption is large preferably, environmental pollution is serious, to shortcomings such as tubing requirement are high, and the advantage of binding kinetics inhibitor and hydrate polymerization inhibitor, both the coring and increment speed delaying hydrate can effectively have been suppressed, the object that good prevention hydrate particle is built up can be played again, thus efficiently solve the flowing safety problem of oil-gas-water three-phase mixed transferring pipeline.In addition, Compositional type hydrate inhibitor provided by the invention also has the advantages such as low, the economic environmental protection of consumption, efficient, function admirable, has a good application prospect.
Accompanying drawing explanation
Fig. 1 is the structural representation of high-pressure sapphire reactor.
Fig. 2 is particle chord length distribution situation of change figure in gas hydrate generative process in embodiment 16.
Embodiment
Below in conjunction with Fig. 1 and Fig. 2, the present invention is described in detail.
The experiment porch adopted in following comparative example 1 and embodiment 1 to embodiment 7 is high-pressure sapphire reactor, and its structure as shown in Figure 1.This device mainly comprises high-pressure sapphire reaction kettle body 1, constant temperature air bath 2, temperature transducer 3 and pressure transducer 4, hand push pump 5, stirring system and computer data automated collection systems 6.The maximum functional volume of high-pressure sapphire reactor is 49cm
3, Maximum operating pressure is 50MPa, and operating temperature range is 183K-423K.With an Air-tight piston 7 in reactor, charging fluid and experimental system can be separated, reacting kettle inner pressure regulates by hand push pump 5.In addition, LGY150A type cold light source is configured with outside this sapphire reactor.
The concrete steps adopting above-mentioned high-pressure sapphire reactor to carry out applicating evaluating experiment are as follows:
(1) to after whole experimental system cleaning, configuration is containing the oil hydrosol of Compositional type hydrate inhibitor, and be placed in sapphire reaction kettle body 1, initialization system temperature is 274.2K, i.e. experimental temperature;
(2) when reactor temperature reaches predefined value and stable continue 4 hours after, system is vacuumized, and passes into experimental gas and replace 3 times, continue to pass into a certain amount of experimental gas and make it to reach dissolution equilibrium;
(3) passing into experimental gas to system pressure is 8.5MPa, i.e. experimental pressure; Close suction valve, open stirrer, whole experimentation mixing speed is invariable; Along with experiment is carried out, start to occur hydrate particle in system, the macroscopic form change of gas hydrate in observe system, system temperature, pressure and reaction time all adopt computer data automated collection systems 6 record;
(4) when system pressure is invariable and keep after 12h, restart after stopping stirring 12h, observe hydrate particle and whether can again be uniformly dispersed, with or without accumulation stopping state;
(5) get top tank air and carry out chromatographic analysis, calculate actual Subcoold temperature according to gas composition, Subcoold temperature is under identical experiment pressure, the temperature of equilibrium of gas hydrate and the difference of experimental temperature;
(6) regulating system temperature is 303K, after gas hydrate decomposes completely in reactor, restarts lower group of experiment.
Judge that the whether excellent standard of hydrate inhibitor rejection mainly comprises: (1) induction time.Time time by air inlet to first observed in system to hydrate particle, induction time is longer, and rejection is more excellent; (2) growth time.Time when reaching stable to system pressure by observing hydrate particle for the first time, growth time is longer, and rejection is better; (3) phenomenon is inhibited.Under experimental temperature and pressure condition, build up without the obvious hydrate of appearance at the end of experiment by there is hydrate particle in system, even particulate dispersion is in oil phase, system is slurry distribution, stirrer Absorbable organic halogens in reactor freely stirs up and down, after stopping stirring 12h to restart, hydrate particle can be uniformly dispersed again.
The experimental gas adopted in following all comparative examples and embodiment is simulation rock gas, and gas composition is as shown in table 1.
The composition of simulation rock gas used tested by table 1
Comparative example 1
This comparative example provides a kind of composite mixture, is mixed to get with mass ratio 1:2 by polyol-based non-ionic surfactant Span20 and TBAB (TBAB).
High-pressure sapphire reactor described in this comparative example adopts is evaluated, in reactor, profit system is made up of the-20# diesel oil of 3.0ml deionized water and 12ml, namely moisture content is the profit system of 20vol%, the adding quantity of the composite mixture of this comparative example is 3.0% of quality in profit system, and the experimental gas composition passed into is in table 1.
Find in the experimentation of this comparative example, induction time and the growth time of gas hydrate synthesis are respectively 18min and 34min, but gas hydrate synthesis in earlier stage, particle is formed in a large number and builds up fast, serious caking is all there is with liquid level place bottom jewel still, stirrer cannot unrestricted motion, thus illustrates that this compound has poor rejection.
Embodiment 1
Present embodiments provide a kind of Compositional type hydrate inhibitor, be mixed to get with the mass ratio of 1:1:1 by polyol-based non-ionic surfactant Span20, PVP (polyvinyl-pyrrolidone) and TBAB (TBAB).
High-pressure sapphire reactor described in the present embodiment adopts is evaluated, in reactor, profit system is made up of the-20# diesel oil of 3.0ml deionized water and 12ml, namely moisture content is the profit system of 20vol%, the adding quantity of the Compositional type hydrate inhibitor of the present embodiment is 2.0% of quality in system, and the experimental gas composition passed into is in table 1.
Find in the experimentation of the present embodiment, the induction time of gas hydrate synthesis and growth time can reach 40min and 150min respectively, in whole experimentation, hydrate particle is dispersed in oil phase, continuous operation 12h does not occur that hydrate builds up the phenomenon of caking blocking, and reactor stirrer can freely move up and down; After stopping stirring, find that gas hydrate particle is deposited on bottom reactor gradually, upper strata is oil phase, can restart smoothly after stopping stirring 12h, hydrate particle disperses again, builds up caking phenomenon without occurring, thus illustrates that the inhibitor that the present embodiment provides has good rejection.
Embodiment 2
Present embodiments provide a kind of Compositional type hydrate inhibitor, be mixed to get with the mass ratio of 2:1:1 by polyol-based non-ionic surfactant Span20, PVP (polyvinyl-pyrrolidone) and TBAB (TBAB).
High-pressure sapphire reactor described in the present embodiment adopts is evaluated, in reactor, profit system is made up of the-20# diesel oil of 3.0ml deionized water and 12ml, namely moisture content is the profit system of 20vol%, the adding quantity of the Compositional type hydrate inhibitor of the present embodiment is 2.0% of quality in system, and the experimental gas composition passed into is in table 1.
Find in the experimentation of the present embodiment, the induction time of gas hydrate synthesis and growth time can reach 72min and 300min respectively, in whole experimentation, hydrate particle is dispersed in oil phase, continuous operation 12h does not occur that hydrate builds up the phenomenon of caking blocking, and reactor stirrer can freely move up and down; After stopping stirring, find that gas hydrate particle is deposited on bottom reactor gradually, upper strata is oil phase, can restart smoothly after stopping stirring 12h, hydrate particle disperses again, builds up caking phenomenon without occurring, thus illustrates that the inhibitor that the present embodiment provides has good rejection.
Embodiment 3
Present embodiments provide a kind of Compositional type hydrate inhibitor, be mixed to get with the mass ratio of 1:1:1 by polyol-based non-ionic surfactant Span40, PVP (polyvinyl-pyrrolidone) and TBAB (TBAB).
High-pressure sapphire reactor described in the present embodiment adopts is evaluated, in reactor, profit system is made up of the-20# diesel oil of 3.0ml deionized water and 12ml, namely moisture content is the profit system of 20vol%, the adding quantity of the Compositional type hydrate inhibitor of the present embodiment is 2.0% of quality in system, and the experimental gas composition passed into is in table 1.
Find in the experimentation of the present embodiment, the induction time of gas hydrate synthesis and growth time can reach 39min and 194min respectively, in whole experimentation, hydrate particle is dispersed in oil phase, continuous operation 12h does not occur that hydrate builds up the phenomenon of caking blocking, and reactor stirrer can freely move up and down; After stopping stirring, find that gas hydrate particle is deposited on bottom reactor gradually, upper strata is oil phase, can restart smoothly after stopping stirring 12h, hydrate particle disperses again, builds up caking phenomenon without occurring, thus illustrates that the inhibitor that the present embodiment provides has good rejection.
Embodiment 4
Present embodiments provide a kind of Compositional type hydrate inhibitor, be mixed to get with the mass ratio of 1:1:1 by polyol-based non-ionic surfactant Span60, PVP (polyvinyl-pyrrolidone) and TBAB (TBAB).
High-pressure sapphire reactor described in the present embodiment adopts is evaluated, in reactor, profit system is made up of the-20# diesel oil of 3.0ml deionized water and 12ml, namely moisture content is the profit system of 20vol%, the adding quantity of the Compositional type hydrate inhibitor of the present embodiment is 2.0% of quality in system, and the experimental gas composition passed into is in table 1.
Find in the experimentation of the present embodiment, the induction time of gas hydrate synthesis and growth time can reach 38min and 151min respectively, in whole experimentation, hydrate particle is dispersed in oil phase, continuous operation 12h does not occur that hydrate builds up the phenomenon of caking blocking, and reactor stirrer can freely move up and down; After stopping stirring, find that gas hydrate particle is deposited on bottom reactor gradually, upper strata is oil phase, can restart smoothly after stopping stirring 12h, hydrate particle disperses again, builds up caking phenomenon without occurring, thus illustrates that the inhibitor that the present embodiment provides has good rejection.
Embodiment 5
Present embodiments provide a kind of Compositional type hydrate inhibitor, be mixed to get with the mass ratio of 1:1:1 by polyol-based non-ionic surfactant Span80, PVP (polyvinyl-pyrrolidone) and TBAB (TBAB).
High-pressure sapphire reactor described in the present embodiment adopts is evaluated, in reactor, profit system is made up of the-20# diesel oil of 3.0ml deionized water and 12ml, namely moisture content is the profit system of 20vol%, the adding quantity of the Compositional type hydrate inhibitor of the present embodiment is 2.0% of quality in system, and the experimental gas composition passed into is in table 1.
Find in the experimentation of the present embodiment, the induction time of gas hydrate synthesis and growth time can reach 52min and 215min respectively, in whole experimentation, hydrate particle is dispersed in oil phase, continuous operation 12h does not occur that hydrate builds up the phenomenon of caking blocking, and reactor stirrer can freely move up and down; After stopping stirring, find that gas hydrate particle is deposited on bottom reactor gradually, upper strata is oil phase, can restart smoothly after stopping stirring 12h, hydrate particle disperses again, builds up caking phenomenon without occurring, thus illustrates that the inhibitor that the present embodiment provides has good rejection.
Embodiment 6
Present embodiments provide a kind of Compositional type hydrate inhibitor, be mixed to get with the mass ratio of 1:1:1 by polyol-based non-ionic surfactant Span20, PVCap (Polyvinylcaprolactame) and TBAB (TBAB).
High-pressure sapphire reactor described in the present embodiment adopts is evaluated, in reactor, profit system is made up of the-20# diesel oil of 3.0ml deionized water and 12ml, namely moisture content is the profit system of 20vol%, the adding quantity of the Compositional type hydrate inhibitor of the present embodiment is 2.0% of quality in system, and the experimental gas composition passed into is in table 1.
Find in the experimentation of the present embodiment, the induction time of gas hydrate synthesis and growth time can reach 78min and 261min respectively, in whole experimentation, hydrate particle is dispersed in oil phase, continuous operation 12h does not occur that hydrate builds up the phenomenon of caking blocking, and reactor stirrer can freely move up and down; After stopping stirring, find that gas hydrate particle is deposited on bottom reactor gradually, upper strata is oil phase, can restart smoothly after stopping stirring 12h, hydrate particle disperses again, builds up caking phenomenon without occurring, thus illustrates that the inhibitor that the present embodiment provides has good rejection.
Embodiment 7
Present embodiments provide a kind of Compositional type hydrate inhibitor, be mixed to get with the mass ratio of 1:1:1 by polyol-based non-ionic surfactant Span20, PVP (polyvinyl-pyrrolidone) and TPAB (four pentyl ammonium bromide).
High-pressure sapphire reactor described in the present embodiment adopts is evaluated, in reactor, profit system is made up of the-20# diesel oil of 3.0ml deionized water and 12ml, namely moisture content is the profit system of 20vol%, the adding quantity of the Compositional type hydrate inhibitor of the present embodiment is 2.0% of quality in system, and the experimental gas composition passed into is in table 1.
Find in the experimentation of the present embodiment, the induction time of gas hydrate synthesis and growth time can reach 32min and 141min respectively, in whole experimentation, hydrate particle is dispersed in oil phase, continuous operation 12h does not occur that hydrate builds up the phenomenon of caking blocking, and reactor stirrer can freely move up and down; After stopping stirring, find that gas hydrate particle is deposited on bottom reactor gradually, upper strata is oil phase, can restart smoothly after stopping stirring 12h, hydrate particle disperses again, builds up caking phenomenon without occurring, thus illustrates that the inhibitor that the present embodiment provides has good rejection.
Embodiment 8
Present embodiments provide a kind of Compositional type hydrate inhibitor, be mixed to get with the mass ratio of 2:5:5 by polyol-based non-ionic surfactant Span20, PVP (polyvinyl-pyrrolidone) and TPAB (four pentyl ammonium bromide).
High-pressure sapphire reactor described in the present embodiment adopts is evaluated, in reactor, profit system is made up of the-20# diesel oil of 3.0ml deionized water and 12ml, namely moisture content is the profit system of 20vol%, the adding quantity of the Compositional type hydrate inhibitor of the present embodiment is 2.0% of quality in system, and the experimental gas composition passed into is in table 1.
Find in the experimentation of the present embodiment, the induction time of gas hydrate synthesis and growth time can reach 40min and 123min respectively, in whole experimentation, hydrate particle is dispersed in oil phase, continuous operation 12h does not occur that hydrate builds up the phenomenon of caking blocking, and reactor stirrer can freely move up and down; After stopping stirring, find that gas hydrate particle is deposited on bottom reactor gradually, upper strata is oil phase, can restart smoothly after stopping stirring 12h, hydrate particle disperses again, builds up caking phenomenon without occurring, thus illustrates that the inhibitor that the present embodiment provides has good rejection.
Embodiment 9
Present embodiments provide a kind of Compositional type hydrate inhibitor, be mixed to get with the mass ratio of 1:2:2 by polyol-based non-ionic surfactant Span20, PVP (polyvinyl-pyrrolidone) and TPAB (four pentyl ammonium bromide).
High-pressure sapphire reactor described in the present embodiment adopts is evaluated, in reactor, profit system is made up of the-20# diesel oil of 3.0ml deionized water and 12ml, namely moisture content is the profit system of 20vol%, the adding quantity of the Compositional type hydrate inhibitor of the present embodiment is 2.0% of quality in system, and the experimental gas composition passed into is in table 1.
Find in the experimentation of the present embodiment, the induction time of gas hydrate synthesis and growth time can reach 36min and 127min respectively, in whole experimentation, hydrate particle is dispersed in oil phase, continuous operation 12h does not occur that hydrate builds up the phenomenon of caking blocking, and reactor stirrer can freely move up and down; After stopping stirring, find that gas hydrate particle is deposited on bottom reactor gradually, upper strata is oil phase, can restart smoothly after stopping stirring 12h, hydrate particle disperses again, builds up caking phenomenon without occurring, thus illustrates that the inhibitor that the present embodiment provides has good rejection.
Embodiment 10
Present embodiments provide a kind of Compositional type hydrate inhibitor, be mixed to get with the mass ratio of 1:2:3 by polyol-based non-ionic surfactant Span20, PVP (polyvinyl-pyrrolidone) and TPAB (four pentyl ammonium bromide).
High-pressure sapphire reactor described in the present embodiment adopts is evaluated, in reactor, profit system is made up of the-20# diesel oil of 3.0ml deionized water and 12ml, namely moisture content is the profit system of 20vol%, the adding quantity of the Compositional type hydrate inhibitor of the present embodiment is 2.0% of quality in system, and the experimental gas composition passed into is in table 1.
Find in the experimentation of the present embodiment, the induction time of gas hydrate synthesis and growth time can reach 37min and 150min respectively, in whole experimentation, hydrate particle is dispersed in oil phase, continuous operation 12h does not occur that hydrate builds up the phenomenon of caking blocking, and reactor stirrer can freely move up and down; After stopping stirring, find that gas hydrate particle is deposited on bottom reactor gradually, upper strata is oil phase, can restart smoothly after stopping stirring 12h, hydrate particle disperses again, builds up caking phenomenon without occurring, thus illustrates that the inhibitor that the present embodiment provides has good rejection.
Embodiment 11
Present embodiments provide a kind of Compositional type hydrate inhibitor, be mixed to get with the mass ratio of 1:2:3 by polyol-based non-ionic surfactant Span20, PVP (polyvinyl-pyrrolidone) and TPAB (four pentyl ammonium bromide).
High-pressure sapphire reactor described in the present embodiment adopts is evaluated, in reactor, profit system is made up of the-20# diesel oil of 3.0ml deionized water and 12ml, namely moisture content is the profit system of 20vol%, the adding quantity of the Compositional type hydrate inhibitor of the present embodiment is 0.1% of quality in system, and the experimental gas composition passed into is in table 1.
Find in the experimentation of the present embodiment, the induction time of gas hydrate synthesis and growth time can reach 20min and 90min respectively, in whole experimentation, hydrate particle is dispersed in oil phase, continuous operation 12h does not occur that hydrate builds up the phenomenon of caking blocking, and reactor stirrer can freely move up and down; After stopping stirring, find that gas hydrate particle is deposited on bottom reactor gradually, upper strata is oil phase, can restart smoothly after stopping stirring 12h, hydrate particle disperses again, builds up caking phenomenon without occurring, thus illustrates that the inhibitor that the present embodiment provides has good rejection.
Embodiment 12
Present embodiments provide a kind of Compositional type hydrate inhibitor, be mixed to get with the mass ratio of 1:2:3 by polyol-based non-ionic surfactant Span20, PVP (polyvinyl-pyrrolidone) and TPAB (four pentyl ammonium bromide).
High-pressure sapphire reactor described in the present embodiment adopts is evaluated, in reactor, profit system is made up of the-20# diesel oil of 3.0ml deionized water and 12ml, namely moisture content is the profit system of 20vol%, the adding quantity of the Compositional type hydrate inhibitor of the present embodiment is 10% of quality in system, and the experimental gas composition passed into is in table 1.
Find in the experimentation of the present embodiment, the induction time of gas hydrate synthesis and growth time can reach 53min and 172min respectively, in whole experimentation, hydrate particle is dispersed in oil phase, continuous operation 12h does not occur that hydrate builds up the phenomenon of caking blocking, and reactor stirrer can freely move up and down; After stopping stirring, find that gas hydrate particle is deposited on bottom reactor gradually, upper strata is oil phase, can restart smoothly after stopping stirring 12h, hydrate particle disperses again, builds up caking phenomenon without occurring, thus illustrates that the inhibitor that the present embodiment provides has good rejection.
Embodiment 13
Present embodiments provide a kind of Compositional type hydrate inhibitor, be mixed to get with the mass ratio of 1:2:3 by polyol-based non-ionic surfactant Span20 and TPAB (four pentyl ammonium bromide).
High-pressure sapphire reactor described in the present embodiment adopts is evaluated, in reactor, profit system is made up of the-20# diesel oil of 3.0ml deionized water and 12ml, namely moisture content is the profit system of 20vol%, the adding quantity of the Compositional type hydrate inhibitor of the present embodiment is 1% of quality in system, and the experimental gas composition passed into is in table 1.
Find in the experimentation of the present embodiment, the induction time of gas hydrate synthesis and growth time can reach 31min and 121min respectively, in whole experimentation, hydrate particle is dispersed in oil phase, continuous operation 12h does not occur that hydrate builds up the phenomenon of caking blocking, and reactor stirrer can freely move up and down; After stopping stirring, find that gas hydrate particle is deposited on bottom reactor gradually, upper strata is oil phase, can restart smoothly after stopping stirring 12h, hydrate particle disperses again, builds up caking phenomenon without occurring, thus illustrates that the inhibitor that the present embodiment provides has good rejection.
Embodiment 14
Present embodiments provide a kind of Compositional type hydrate inhibitor, be mixed to get with the mass ratio of 1:2:3 by PVP (polyvinyl-pyrrolidone), polyol-based non-ionic surfactant Span20 and TPAB (four pentyl ammonium bromide).
High-pressure sapphire reactor described in the present embodiment adopts is evaluated, in reactor, profit system is made up of the-20# diesel oil of 3.0ml deionized water and 12ml, namely moisture content is the profit system of 20vol%, the adding quantity of the Compositional type hydrate inhibitor of the present embodiment is 3% of quality in system, and the experimental gas composition passed into is in table 1.
Find in the experimentation of the present embodiment, the induction time of gas hydrate synthesis and growth time can reach 41min and 162min respectively, in whole experimentation, hydrate particle is dispersed in oil phase, continuous operation 12h does not occur that hydrate builds up the phenomenon of caking blocking, and reactor stirrer can freely move up and down; After stopping stirring, find that gas hydrate particle is deposited on bottom reactor gradually, upper strata is oil phase, can restart smoothly after stopping stirring 12h, hydrate particle disperses again, builds up caking phenomenon without occurring, thus illustrates that the inhibitor that the present embodiment provides has good rejection.
Embodiment 15
Present embodiments provide a kind of Compositional type hydrate inhibitor, be mixed to get with the mass ratio of 1:2:3 by PVP (polyvinyl-pyrrolidone), polyol-based non-ionic surfactant Span20 and TPAB (four pentyl ammonium bromide).
High-pressure sapphire reactor described in the present embodiment adopts is evaluated, in reactor, profit system is made up of the-20# diesel oil of 3.0ml deionized water and 12ml, namely moisture content is the profit system of 60vol%, the adding quantity of the Compositional type hydrate inhibitor of the present embodiment is 2.0% of quality in system, and the experimental gas composition passed into is in table 1.
Find in the experimentation of the present embodiment, the induction time of gas hydrate synthesis and growth time can reach 30min and 121min respectively, in whole experimentation, hydrate particle is dispersed in oil phase, continuous operation 12h does not occur that hydrate builds up the phenomenon of caking blocking, and reactor stirrer can freely move up and down; After stopping stirring, find that gas hydrate particle is deposited on bottom reactor gradually, upper strata is oil phase, can restart smoothly after stopping stirring 12h, hydrate particle disperses again, builds up caking phenomenon without occurring, thus illustrates that the inhibitor that the present embodiment provides has good rejection.
Following embodiment 16 and embodiment 17 are on the basis of existing experiment porch, are provided with in the autoclave of online particle laser visual fractional analysis instrument PVM measure probe and online Focused Beam Reflectance detector FBRM measure probe and test.This device mainly comprises: band water-bath and churned mechanically autoclave, PVM measure probe and FBRM measure probe and relevant connection device and data acquistion system.Autoclave material is stainless steel, can bear pressure maximum 32MPa, and the effective volume of autoclave is 534.72mL; Water bath with thermostatic control operating temperature range is 253K-323K; Mechanical agitation is made up of parts such as impellers in motor and still, and the reaction system in autoclave is mixed.
Wherein PVM measure probe is made up of six bundle laser, illuminates probe front region by laser beam, and then microscopic pattern change in shooting viewing area.FBRM measure probe is measured by Emission Lasers equally, it launches near-infrared wavelength by Optical Fiber Transmission to probe end, probe end has an optical lens rotated that light can be made to deflect, in experimentation, the laser scanning of launching will be reflected to during particle surperficial, and chord length is determined by the sweep rate of the time and laser that measure reflection.In measuring phase, the experimental demand of laser scanning speed can regulate between 2m/s-16m/s.The drop measured in a certain time interval by the sapphire form before probe or the quantity of particle chord length obtain chord length distribution by statistics.
The concrete steps adopting above-mentioned autoclave to carry out testing are as follows:
(1), before experiment starts, autoclave and all connected elements all rinse with cleaning solution, dry up with nitrogen.Clean PVM measure probe and FBRM measure probe, make it reach and measure the rear installation of requirement;
(2) inhibitor of the profit system configured in advance by 220mL and the present embodiment injects autoclave, is dissolved in air in solution by vacuumizing venting;
(3) open FBRM measure probe, PVM measure probe, temperature data collecting system and pressure data acquisition system, water-bath is adjusted to experimental temperature 274.2K, starts cooling, and open and stir, rotating speed is 1000r/min, turn-on data acquisition system;
(4) after the temperature in autoclave reaches experimental temperature and keeps 4h, stop stirring, passing into experimental gas to experimental pressure is 7.5MPa, and observes gas hydrate forming process change of form and particle size distribution Changing Pattern;
(5) regulate bath temperature to 303K, after treating decomposition of hydrate, exhaust discharge opeing restarts lower group of experiment.
In embodiment 16 and embodiment 17, in autoclave, profit system is made up of the-20# diesel oil of 22ml deionized water and 198ml, namely moisture content is the mixed defeated system of 10vol%, the adding quantity of the present embodiment inhibitor is 2.0% of quality in system, gas phase used is simulation rock gas, and gas composition is as shown in table 1.
Embodiment 16
Present embodiments provide a kind of Compositional type hydrate inhibitor, be mixed to get with the mass ratio of 1:1:1 by PVP (polyvinyl-pyrrolidone), polyol-based non-ionic surfactant Span20 and TBAB (TBAB).
Above-mentioned Compositional type hydrate inhibitor being applied to moisture content is in the profit system of 10vol%, and the form of mensurated gas composition hydrate in forming process and particle size distribution rule.
In the present embodiment experimentation, the picture taken by PVM when generating gas hydrate completely, can find out the uniform hydrate slurry of final formation.The hydrate slurry particle chord length distribution situation of change measured by FBRM, as shown in Figure 2, along with the formation of hydrate, in system, gas hydrate particle size offsets to large particle size, but along with experiment is carried out, gas hydrate particle size tends towards stability, do not occur blocking caking phenomenon, namely all without the sticky wall occurring gas hydrate on popping one's head at two, thus illustrate that the Compositional type inhibitor of the present embodiment has good rejection.
Embodiment 17
Present embodiments provide a kind of Compositional type hydrate inhibitor, be mixed to get with the mass ratio of 1:1:1 by PVP (polyvinyl-pyrrolidone), polyol-based non-ionic surfactant Span20 and TBAB (TBAB).
In the present embodiment, in reactor, profit system is made up of the-20# diesel oil of 44ml deionized water and 176ml, and namely moisture content is the profit system of 20vol%, and the adding quantity of the inhibitor of the present embodiment is 2.0% of quality in system.
In the whole experimentation of the present embodiment, along with the formation of gas hydrate in system, by gas hydrate particle size offseting to large particle size in discovery system in FBRM, but along with experiment is carried out, gas hydrate particle size tends towards stability, without occurring block wall sticking phenomenon all without the sticky wall occurring gas hydrate on namely popping one's head at two, thus illustrate that the Compositional type inhibitor of the present embodiment has good rejection.
A kind of Compositional type hydrate inhibitor of the present invention, when temperature controls at 253K-323K; Stress control, when 0.1MPa-50.0MPa, also can realize the object suppressing hydrate growth.
A kind of Compositional type hydrate inhibitor of the present invention, copolymer is polymeric compound, and water soluble, ethanol, chloroform and most organic solvent, toxicity is less.
The Span series polyol-based non-ionic surfactant that mentioned emulsifier adopts, because of the hydrophilic radical in its structure and long alkyl chain lipophilic group, make it easily be adsorbed in oil-water interfaces, reduce interfacial tension, for good oil-water emulsion agent, WO emulsion can be formed.
Above-mentioned quaternary ammonium salt dispersing agent, soluble in water, ethanol etc., after forming hydrate particle in oil-gas-water system, in dispersing agent, hydrophilic radical is adsorbed on hydrate particle surface, in dispersing agent, alkyl lipophilic group stretches in oil phase, thus the accumulation between prevention hydrate particle, make it be dispersed in oil phase.
Present invention also offers above-mentioned Compositional type hydrate inhibitor and mix inhibiting mechanism in defeated system in oil gas water three phase.Owing to not having the ability of disperse water polymer beads when kinetic inhibitor is used alone, therefore its application area critical constraints.In addition, because hydrate polymerization inhibitor does not have a kinetic inhibition performance, during its individualism, at gas hydrate synthesis in earlier stage, because hydrate coring and increment speed is too fast, cause polymerization inhibitor molecule to have little time disperse water polymer beads, in this stage, Hydrate Plugging situation very easily occurs.Therefore, the present invention is undertaken composite by having the copolymer of kinetic inhibition performance and emulsifier and dispersing agent, both can suppress the coring and increment of hydrate particle, also can play the object of disperse water polymer beads.Its concrete inhibiting mechanism is: before gas hydrate synthesis, under oil-water emulsion agent effect, oil-gas-water system is that even water in oil emulsion exists, and has the copolymer of kinetic inhibition effect and dispersing agent is all adsorbed in oil-water interfaces, can play the object suppressing hydrate nucleation; Along with the formation of hydrate shell, copolymer molecule is adsorbed on shell layer surface, cause growth of grain reduced rate, enough time is provided for quaternary ammonium salt dispersing agent plays its dispersibility, final under dispersing agent effect, hydrate is dispersed in oil phase with granule, in stablizing slurry conveying, blocking phenomenon of luming does not occur.
A kind of Compositional type hydrate inhibitor of the present invention is compared with currently available technology, can overcome that conventional heat inhibitor consumption is large preferably, environmental pollution is serious, to shortcomings such as tubing requirement are high, and the advantage of binding kinetics inhibitor and hydrate polymerization inhibitor, both the coring and increment speed delaying hydrate can effectively have been suppressed, the object that good prevention hydrate particle is built up can be played again, thus efficiently solve the flowing safety problem of oil-gas-water three-phase mixed transferring pipeline.In addition, Compositional type polymerization inhibitor provided by the invention also has the advantages such as low, the economic environmental protection of consumption, efficient, function admirable, has a good application prospect.
Certainly, above-mentioned explanation is not limitation of the present invention, and the present invention is also not limited in above-mentioned citing, and the change that those skilled in the art make in essential scope of the present invention, remodeling, interpolation or replacement also should belong to protection scope of the present invention.
Claims (7)
1. a Compositional type hydrate inhibitor, is characterized in that, is made up of copolymer, emulsifier and dispersant, and the mass ratio of copolymer, emulsifier and dispersing agent is 0.01 ~ 2:0.01 ~ 5:0.01 ~ 5;
Described copolymer is polyvinyl-pyrrolidone, one or more mixtures made in Polyvinylcaprolactame and polymethacrylic acid dimethylamino ethyl ester; Described emulsifier is polyol-based non-ionic surfactant; Described dispersing agent is quaternary ammonium compound.
2. a kind of Compositional type hydrate inhibitor as claimed in claim 1, it is characterized in that, the mass ratio of copolymer, emulsifier and dispersing agent is 0.5 ~ 1:1 ~ 2:1 ~ 3.
3. a kind of Compositional type hydrate inhibitor as claimed in claim 1, it is characterized in that, described quaternary ammonium compound is TBAB, four pentyl ammonium bromide, the quaternary ammonium salt containing 2-3 normal-butyl, the quaternary ammonium salt containing 2-3 n-pentyl or one or more mixtures made of quaternary ammonium salt containing 2-3 isopentyl.
4. a kind of Compositional type hydrate inhibitor as claimed in claim 1, is characterized in that, described polyol-based non-ionic surfactant is Span series polyol-based non-ionic surfactant.
5. a kind of Compositional type hydrate inhibitor as claimed in claim 4, it is characterized in that, described Span series polyol-based non-ionic surfactant is by the mixture of one or more in Span20, Span40, Span60, Span65, Span80 and Span85 polyol-based non-ionic surfactant.
6. a kind of using method of Compositional type hydrate inhibitor as described in claim 1 to 5 any one, it is characterized in that, adding above-mentioned Compositional type hydrate inhibitor to oil-gas-water mixes in defeated system, and the quality of the Compositional type hydrate inhibitor of interpolation is 0.1% ~ 10% of water gross mass; The temperature that oil-gas-water mixes defeated system controls at 253K-323K; Stress control is at 0.1MPa-50.0MPa; The volume that oil-gas-water mixes water in defeated system is no more than 60% of oil and water total volume.
7. the using method of a kind of Compositional type hydrate inhibitor as claimed in claim 6, is characterized in that, the quality of the Compositional type hydrate inhibitor of interpolation is 1% ~ 3% of water gross mass.
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| CN105505358A (en) * | 2015-12-29 | 2016-04-20 | 中国科学院广州能源研究所 | Hydrate inhibitor for deep-water oilfield development |
| CN105860405A (en) * | 2016-04-21 | 2016-08-17 | 中国石油化工股份有限公司 | Novel hydrate dynamics inhibitor and application thereof |
| CN107314245A (en) * | 2016-06-12 | 2017-11-03 | 中国石油化工股份有限公司 | Compositional type hydrate polymerization inhibitor composition containing lecithin and application thereof |
| CN113817519A (en) * | 2020-06-18 | 2021-12-21 | 中国石油化工股份有限公司 | Composition for promoting high-efficiency solid hydrate, preparation method thereof and method for enhancing hydrate generation |
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