CN108690065A - The more ethyoxyls of the mono- perfluoro decyl silicon-of dimethyl-- oleate multi-element compounds and the preparation method and application thereof - Google Patents

The more ethyoxyls of the mono- perfluoro decyl silicon-of dimethyl-- oleate multi-element compounds and the preparation method and application thereof Download PDF

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CN108690065A
CN108690065A CN201810447889.6A CN201810447889A CN108690065A CN 108690065 A CN108690065 A CN 108690065A CN 201810447889 A CN201810447889 A CN 201810447889A CN 108690065 A CN108690065 A CN 108690065A
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dimethyl
element compounds
perfluoro
mono
ethyoxyls
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沈健
王达炜
章峻
侯庆锋
周宁琳
杨仲斌
金锐
赵越
付磊
冯福玲
何磊
莫宏
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Nanjing University
Nanjing Normal University
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    • CCHEMISTRY; METALLURGY
    • C07ORGANIC CHEMISTRY
    • C07FACYCLIC, CARBOCYCLIC OR HETEROCYCLIC COMPOUNDS CONTAINING ELEMENTS OTHER THAN CARBON, HYDROGEN, HALOGEN, OXYGEN, NITROGEN, SULFUR, SELENIUM OR TELLURIUM
    • C07F7/00Compounds containing elements of Groups 4 or 14 of the Periodic System
    • C07F7/02Silicon compounds
    • C07F7/08Compounds having one or more C—Si linkages
    • C07F7/0803Compounds with Si-C or Si-Si linkages
    • C07F7/0825Preparations of compounds not comprising Si-Si or Si-cyano linkages
    • C07F7/0827Syntheses with formation of a Si-C bond
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08GMACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
    • C08G65/00Macromolecular compounds obtained by reactions forming an ether link in the main chain of the macromolecule
    • C08G65/02Macromolecular compounds obtained by reactions forming an ether link in the main chain of the macromolecule from cyclic ethers by opening of the heterocyclic ring
    • C08G65/26Macromolecular compounds obtained by reactions forming an ether link in the main chain of the macromolecule from cyclic ethers by opening of the heterocyclic ring from cyclic ethers and other compounds
    • C08G65/2639Macromolecular compounds obtained by reactions forming an ether link in the main chain of the macromolecule from cyclic ethers by opening of the heterocyclic ring from cyclic ethers and other compounds the other compounds containing elements other than oxygen, nitrogen or sulfur
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08GMACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
    • C08G65/00Macromolecular compounds obtained by reactions forming an ether link in the main chain of the macromolecule
    • C08G65/02Macromolecular compounds obtained by reactions forming an ether link in the main chain of the macromolecule from cyclic ethers by opening of the heterocyclic ring
    • C08G65/32Polymers modified by chemical after-treatment
    • C08G65/329Polymers modified by chemical after-treatment with organic compounds
    • C08G65/331Polymers modified by chemical after-treatment with organic compounds containing oxygen
    • C08G65/332Polymers modified by chemical after-treatment with organic compounds containing oxygen containing carboxyl groups, or halides, or esters thereof
    • C08G65/3322Polymers modified by chemical after-treatment with organic compounds containing oxygen containing carboxyl groups, or halides, or esters thereof acyclic
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    • C09K8/00Compositions for drilling of boreholes or wells; Compositions for treating boreholes or wells, e.g. for completion or for remedial operations
    • C09K8/58Compositions for enhanced recovery methods for obtaining hydrocarbons, i.e. for improving the mobility of the oil, e.g. displacing fluids
    • C09K8/584Compositions for enhanced recovery methods for obtaining hydrocarbons, i.e. for improving the mobility of the oil, e.g. displacing fluids characterised by the use of specific surfactants
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08GMACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
    • C08G2650/00Macromolecular compounds obtained by reactions forming an ether link in the main chain of the macromolecule
    • C08G2650/02Macromolecular compounds obtained by reactions forming an ether link in the main chain of the macromolecule characterized by the type of post-polymerisation functionalisation
    • C08G2650/04End-capping

Abstract

The invention discloses the more ethyoxyls of the mono- perfluoro decyl silicon-of a kind of dimethyl-- oleate multi-element compounds and the preparation method and application thereof, which is combined by perfluoro decane, dimethyl silicon fluoride, ethylene oxide and oleic acid;Preparation method includes mixing perfluoro decane with dimethyl silicon fluoride, acidification, is warming up to 150~170 DEG C of addition ethylene oxide, oleic acid is added after reaction, finally adjusts pH to 8~9.5;The multi-element compounds are applied to carry out foam flooding in oil field.The multi-element compounds of the present invention can not only efficiently blister, and foam stabilizing effect is good, and chromatographic isolation will not occur when stratum is migrated, especially better in hypotonic, in water-sensitive oil field foam flooding;The multi-element compounds preparation method is simple simultaneously, and operability is strong, at low cost.

Description

The more ethyoxyls of the mono- perfluoro decyl silicon-of dimethyl-- oleate multi-element compounds and its system Preparation Method and application
Technical field
The invention belongs to foam flooding finish field more particularly to a kind of more ethyoxyl-oil of the mono- perfluoro decyl silicon-of dimethyl- Acid esters multi-element compounds and the preparation method and application thereof.
Background technology
The exploitation that aerated fluid is applied to oil field at home and abroad has more than 40 years history, aerated fluid the conventional displacement of reservoir oil, Transfer drive, steam bubble drive, steam bubble handle up, cyclic steam foam flooding, the water pumping gas production of aqueous gas well, sand-flushing, drilling well, All various aspects in the oil-gas field developments such as profile control, water blockoff, acidification, well cementing of cement and pressure break are applied, and are achieved willing Fixed effect.Largely practice have shown that, foam flooding is the important means for protecting oil reservoir, preventing oil layer pollution, improving oil and gas production. As the degree of recognition of foam technology is continuously improved in people, foam flooding means and foam flooding finish will become tertiary oil recovery One of leading technology.There are a large amount of hypotonic water-sensitive oil fields in oil field, the big multichannel of the oil field stratum is narrow, permeability pole Low, oil reservoir is migrated difficulty in the earth formation, and it is mostly the water-sensitive formations such as montmorillonite that stratum, which is constituted, and water-swellable will be originally narrow Channel block causes oil extraction operation that can not carry out.Therefore, conventional water drive or water base foam can not be taken to drive the oil reservoir Oil.
The oil-based foam displacement of reservoir oil is the effective means to solve the above problems.Using oily (usually using diesel oil or mineral oil) as continuously The foam flooding finish of phase is referred to as oil-based foam oil displacement agent.Compared with water base foam oil displacement agent, oil-based foam oil displacement agent it is main Feature is energy high temperature resistance, has very strong inhibition and salt resistance, resistant to pollution ability, lubricity is good, and can be effectively prevented from water drive Caused by the stratum such as montmorillonite expansion passage the problem of, mitigate the damage to oil-gas Layer.But oil phase compares the surface of water phase Can be extremely low, formation of foam is difficult, and is not easy to stablize, and conventional blister agent can not form oil-based foam, seriously affect oil-based foam The development of oil displacement agent.Currently, oil-based foam oil displacement agent is mainly made of oil, water, foaming agent, foam stabilizer, emulsifier etc..System with Water is dispersed phase, and using oil as continuous media, the materials such as addition emulsifier, foaming agent, foam stabilizer are formed by similar oils property Emulsion foam system, also known as inverse emulsification foam flooding finish, grease volume ratio is in (50~80):(50~20) left and right.So And with the necessary each component synergistic effect of conventional oil base foam flooding agent that emulsifier, foaming agent, foam stabilizer form, shape can be played The purpose of oil displacement efficiency is realized at oil-based foam.Due to its in chemical constitution, functional group and polarity there are larger difference, Serious chromatographic isolation can occur when migrating in stratum, the different location in stratum is respectively at so as to cause each component, it can not Synergy embodies, and in turn results in oil-based foam and cannot achieve oil displacement efficiency.O ' Neil et al. have studied a kind of oil-based foam stream Body, the oil-based foam fluid include mainly liquid control, Nephew class foaming agent, Pity vinegars, iron or lead crosslinking agent, gas etc.;Wherein liquid It can be diesel oil, the other aliphatic hydrocarbons of kerosene person that state, which is dazzled,;Foaming agent selects fluorinated surfactant.Specific steps include:By diesel oil, 1.0%HF-2 (fiuorinated acrylic copolymer resin), 0.15%HG-2 (phosphate fat) and 0.15%HX-2 (iron adhesive) are mixed It closes, using whisking at a high speed after device whisks 2min, gas release 47%, half-life period is more than 1h.Oil base bubble has been carried out in heart-to-heart talk et al. The foam stabilizer DRI- of 0.1% foaming agent DRI-YF-1 and 2% is added in foam drilling fluid technical research in 100ml diesel oil YW-1 is the chief component of oil-based foam drilling fluid, is evaluated foam volume, half-life period, rheological characteristic, as a result Show that foam volume reaches 500ml, half-life period 630s, half-life period and foam volume reach the more excellent level in the world.But It is that the composite request that above two oil base oil displacement agent can not meet foaming and foam stabilizing simultaneously (usually foams 300%, foam stabilizing More than 1h).Therefore, how to reach the relative equilibrium of the two, while meeting above-mentioned requirements, have become the most important thing of research. In addition, above-mentioned oil displacement agent is mostly mix reagent, migration in the earth formation can generate migration because of molecular results and polar difference The difference of speed leads to chromatographic isolation phenomenon, and each component synergistic effect is caused to weaken, even lose.
In conclusion existing, there is an urgent need for one kind simply and efficiently to blister, and foam stabilizing effect is good, more particularly in the earth formation The oil-based foam oil displacement agent that chromatographic isolation will not occur when migration, to improve hypotonic, water-sensitive oil reservoir oil recovery effect.
Invention content
Goal of the invention:The first object of the present invention be to provide it is a kind of blistering be easy, foam stability is strong, foam volume is big and The more ethyoxyls of the mono- perfluoro decyl silicon-of dimethyl-- oleate multi-element compounds without chromatographic isolation;The second object of the present invention is The preparation method of the multi-element compounds is provided;The third object of the present invention is to provide the application of the multi-element compounds.
Technical solution:The more ethyoxyls of the mono- perfluoro decyl silicon-of dimethyl-- oleate multi-element compounds of the present invention, structural formula For:
Wherein, n=6~24.
The present invention is by using the small perfluoro decane of difference in chemical constitution, functional group and polarity, dimethyl fluorine silicon Alkane, ethylene oxide and oleic acid are combined the multi-element compounds of above structure, and the multi-element compounds is enabled to transport in the earth formation Chromatographic isolation will not occur when shifting, improve oil recovery effect.Wherein, addition perfluoro decane effectively reduces the multi-element compounds Surface tension realizes barbotage;Addition ethylene oxide not only has the function of foam stabilizing, and has the function of helping emulsification, cooperates with Oleic acid is added, emulsifiability is improved, effectively forms oil based emulsions;Dimethyl silicon fluoride is added thus by perfluoro decane and ring Oxidative ethane (ethyoxyl) is linked in a molecule compound that comes from different backgrounds and possess different abilities, and it plays perfluoro decane with high-flexibility Steeping effect has certain facilitation.Preferably, n can be 10~18 in the multi-element compounds.
The method that the present invention prepares the more ethyoxyls of the mono- perfluoro decyl silicon-of dimethyl-- oleate multi-element compounds, including such as Lower step:Perfluoro decane is mixed with dimethyl silicon fluoride, is acidified, 150~170 DEG C of addition ethylene oxide are warming up to, after reaction Oleic acid is added, finally adjusts pH to 8~9.5.
Furtherly, in the preparation, the molar ratio of perfluoro decane and dimethyl silicon fluoride can be 1:0.5~3.Perfluoro decane Molar ratio with ethylene oxide can be 1:5~40.The molar ratio of perfluoro decane and oleic acid can be 1:0.5~2.4.
Furtherly, in the preparation, the perfluoro decane of addition and dimethyl silicon fluoride are anti-under the conditions of 50~70 DEG C Answer 1~2h.Add 1~2h of reacting ethylene oxide.Add 1.5~2h of elaidin reaction.
The more ethyoxyls of the mono- perfluoro decyl silicon-of dimethyl-- oleate multi-element compounds answering in the oil removing of oil field of the present invention With.
Advantageous effect:Compared with prior art, remarkable advantage of the invention is:The multi-element compounds can not only it is simple, It efficiently blisters, and foam stabilizing effect is good, chromatographic isolation will not occur when can migrate in the earth formation, be more suitable for hypotonic, water-sensitive Foam flooding finish in oil field, oil recovery effect is good, particularly with low oil content (oil content 50-70%), high wax foam system Using effect protrudes;Preparation method is simple simultaneously, and operability is strong, at low cost.
Description of the drawings
Fig. 1 is the infrared spectrum of multi-element compounds of the present invention;
Fig. 2 is oil-based foam microscopic appearance figure when multi-element compounds using the present invention carry out the displacement of reservoir oil;
Fig. 3 is foaming effect figure of the multi-element compounds using the present invention to different moisture content miscella;
Fig. 4 is 72h foam stabilizing effect of the multi-element compounds using the present invention to different moisture content miscella.
Specific implementation mode
Technical scheme of the present invention is described in further detail below in conjunction with the accompanying drawings.
The more ethyoxyls of the mono- perfluoro decyl silicon-of dimethyl-- oleate multi-element compounds of the present invention, structural formula are:
Wherein, n=6~24.
The multi-element compounds prepared by the present invention carry out structural characterization, and the results are shown in Figure 1 for acquisition.In 2870cm-1 There are the stretching vibrations of this C-H for left and right, in 1395cm-1And 1365cm-1There are the bending vibration of methyl, and 1365cm-1The intensity at peak It is larger, thus prove that dimethyl silicon fluoride has been modified on perfluoro decane.3400 or so there are stronger-OH absorption peaks, In the absorption peak of 1700 or so presence-CH=O carbonyls, thus prove that oleic acid is modified up.It can thus be appreciated that dimethyl-is mono- The more ethyoxyls of perfluoro decyl silicon-- oleate multi-element compounds are successfully synthesized.
Embodiment 1
The more ethyoxyls of the mono- perfluoro decyl silicon-of dimethyl-- oleate multi-element compounds of the present invention, structural formula are:
Wherein, n=10~18.
Preparation method includes the following steps:First, the dimethyl silicon fluoride of 50g perfluoro decanes and 12g are placed in reactor In, lead to nitrogen protection, 1.5h is stirred to react at 60 DEG C;Secondly, the concentrated sulfuric acid is added in system, is warming up to 150 DEG C, is slowly added to 60g ethylene oxide, the reaction was continued 1.5h;Again, 100 DEG C or so are cooled to, 28g elaidin reactions 1.5h is added;Finally, hydrogen is added Sodium oxide molybdena adjusts pH value to 9, you can the multi-element compounds of the present invention are made.
When multi-element compounds prepared by the embodiment are applied to the displacement of reservoir oil, surface observation, blistering are carried out to its oil-based foam And foam stability energy is characterized, the result of acquisition is as shown in Figures 2 to 4.As shown in Figure 2, multi-element compounds shape of the invention At foam size much smaller far beyond the foam size that existing foaming agent is formed (present invention is substantially micron-sized bubble Foam, and existing foam it is most subject to grade, that is, be much larger than 100 microns or more).Therefore, it is formed compared to existing foaming agent Foam, multi-element compounds foam system of the invention can realize good migration in the low-permeability oilfield of gap very little, more applicable In low-permeability oilfield, and existing foaming agent is then difficult to;And the compound formed foam under the extruding of coverslip still Original foam pattern can be kept, illustrates its with good stability and foamy body, is conducive to the oil field displacement of reservoir oil.
By Fig. 3 and Fig. 4 it is found that the oil-based foam commonly used in the oil field displacement of reservoir oil wishes to blister multiplying power 300% or more, surely Steep half-life period be more than 1h (foam stabilizing 50%), and the present invention can realize can reach in water content 25% or so blister multiplying power it is big In 300%, and realize that 72h foam stabilizings are more than 80% (i.e. the foam stabilizing time is much larger than 72h).
Embodiment 2
The more ethyoxyls of the mono- perfluoro decyl silicon-of dimethyl-- oleate multi-element compounds of the present invention, structural formula are:
Wherein, n=6~14.
Preparation method includes the following steps:First, the dimethyl silicon fluoride of 50g perfluoro decanes and 9.4g are placed in reactor In, lead to nitrogen protection, 1.5h is stirred to react at 60 DEG C;Secondly, the concentrated sulfuric acid is added in system, is warming up to 150 DEG C, is slowly added to 40g ethylene oxide, the reaction was continued 1.5h;Again, 100 DEG C or so are cooled to, 25g elaidin reactions 1.5h is added;Finally, hydrogen is added Sodium oxide molybdena adjusts pH value to 8.5, you can the multi-element compounds of the present invention are made.
Embodiment 3
The more ethyoxyls of the mono- perfluoro decyl silicon-of dimethyl-- oleate multi-element compounds of the present invention, structural formula are:
Wherein, n=12~16.
Preparation method includes the following steps:First, the dimethyl silicon fluoride of 50g perfluoro decanes and 9.4g are placed in reactor In, lead to nitrogen protection, 1.5h is stirred to react at 60 DEG C;Secondly, the concentrated sulfuric acid is added in system, is warming up to 150 DEG C, is slowly added to 55g ethylene oxide, the reaction was continued 1.5h;Again, 100 DEG C or so are cooled to, 26g elaidin reactions 1.5h is added;Finally, hydrogen is added Sodium oxide molybdena adjusts pH value to 8, you can the multi-element compounds of the present invention are made.
Embodiment 4
The more ethyoxyls of the mono- perfluoro decyl silicon-of dimethyl-- oleate multi-element compounds of the present invention, structural formula are:
Wherein, n=18~24.
Preparation method includes the following steps:First, the dimethyl silicon fluoride of 50g perfluoro decanes and 14g are placed in reactor In, lead to nitrogen protection, 1.5h is stirred to react at 60 DEG C;Secondly, the concentrated sulfuric acid is added in system, is warming up to 150 DEG C, is slowly added to 80g ethylene oxide, the reaction was continued 1.5h;Again, 100 DEG C or so are cooled to, 39g elaidin reactions 1.5h is added;Finally, hydrogen is added Sodium oxide molybdena adjusts pH value to 9.5, you can the multi-element compounds of the present invention are made.
Embodiment 5
The more ethyoxyls of the mono- perfluoro decyl silicon-of dimethyl-- oleate multi-element compounds of the present invention, structural formula are:
Wherein, n=12~18.
Preparation method includes the following steps:First, the dimethyl silicon fluoride of 50g perfluoro decanes and 11g are placed in reactor In, lead to nitrogen protection, 1.5h is stirred to react at 60 DEG C;Secondly, the concentrated sulfuric acid is added in system, is warming up to 150 DEG C, is slowly added to 62g ethylene oxide, the reaction was continued 1.5h;Again, 100 DEG C or so are cooled to, 28g elaidin reactions 1.5h is added;Finally, hydrogen is added Sodium oxide molybdena adjusts pH value to 8.5, you can the multi-element compounds of the present invention are made.
Embodiment 6
The more ethyoxyls of the mono- perfluoro decyl silicon-of dimethyl-- oleate multi-element compounds of the present invention, structural formula are:
Wherein, n=13~17.
Preparation method includes the following steps:First, the dimethyl silicon fluoride of 50g perfluoro decanes and 12g are placed in reactor In, lead to nitrogen protection, 1.5h is stirred to react at 60 DEG C;Secondly, the concentrated sulfuric acid is added in system, is warming up to 150 DEG C, is slowly added to 70g ethylene oxide, the reaction was continued 1.5h;Again, 100 DEG C or so are cooled to, 26g elaidin reactions 1.5h is added;Finally, hydrogen is added Sodium oxide molybdena adjusts pH value to 9, you can the multi-element compounds of the present invention are made.
Embodiment 7
Basic step is same as Example 1, the difference is that the molar ratio of perfluoro decane and dimethyl silicon fluoride, specifically It is 1:0.3,1:0.5,1:1,1:2,1:3,1:3.5.Multi-element compounds prepared by the embodiment are carried out characterization of structure and properties can Know, uses molar ratio for 1:The multi-element compounds that 0.5~3 perfluoro decane is prepared with dimethyl silicon fluoride can not only it is simple, It efficiently blisters, and foam stabilizing effect is good, chromatographic isolation will not occur when can migrate in the earth formation.When perfluoro decane and dimethyl The molar ratio of silicon fluoride is 1:When 0.3, then one side perfluoro decane price, cost increase is larger, and when molar ratio is 1:3.5 When, then dimethyl silicon fluoride can cause reaction product impurity to increase because there is autohemagglutination, and product yield reduces, under using effect Drop.
Embodiment 8
Basic step is same as Example 1, the difference is that the molar ratio of perfluoro decane and ethylene oxide, specially 1: 4.5,1:5,1:10,1:20,1:30,1:40,1:45.Multi-element compounds prepared by the embodiment are carried out characterization of structure and properties can Know, uses molar ratio for 1:The multi-element compounds that 5~40 perfluoro decane is prepared with ethylene oxide can not only be simply and efficiently Blistering, and foam stabilizing effect is good, and chromatographic isolation will not occur when can migrate in the earth formation.When rubbing for perfluoro decane and ethylene oxide You are than being 1:When 4.5, then more ethyoxyl negligible amounts, cause more ethyoxyl foam stabilizing effects to decline, and foam system stability declines, And when molar ratio is 1:When 45, then ethyoxyl quantity is more, causes system molecular chain length long, and foam performance is impacted, foaming Bad stability.This is because when ethylene oxide addition is too low, then the reactive number of ethylene oxide tails off, more oxyethyl chains Increase limited;And addition it is excessively high when, then ethylene oxide number is excessive, and more oxyethyl chains, which are grown beyond, needs number.
Embodiment 9
Basic step is same as Example 1, the difference is that the molar ratio of perfluoro decane and oleic acid, specially 1: 0.45,1:0.5,1:1,1:1.5,1:2,1:2.4,1:3.Multi-element compounds prepared by the embodiment carry out characterization of structure and properties It is found that using molar ratio for 1:The multi-element compounds that 0.5~2.4 perfluoro decane is prepared with oleic acid can not only be simple, efficient Ground blisters, and foam stabilizing effect is good, and chromatographic isolation will not occur when can migrate in the earth formation.When mole of perfluoro decane and oleic acid Than being 1:When 0.45, then whole production can not can not be made further with elaidin reaction in oleic acid number deficiency, partial reaction intermediate Product, and when molar ratio is 1:When 3, then the surface energy of reaction system changes, and reaction carries out slowly, or even stops.
Embodiment 10
Basic step is same as Example 1, the difference is that reaction when perfluoro decane is reacted with dimethyl silicon fluoride Temperature, specially 40 DEG C, 50 DEG C, 60 DEG C, 70 DEG C, 80 DEG C.Multi-element compounds prepared by the embodiment carry out structural behaviour table Sign is it is found that the multi-element compounds that perfluoro decane is prepared with dimethyl silicon fluoride under the conditions of 50~70 DEG C can not only be simple, high The blistering of effect ground, and foam stabilizing effect is good, and chromatographic isolation will not occur when can migrate in the earth formation.When perfluoro decane and dimethyl fluorine When reaction temperature when silane reaction is less than 50 DEG C, then reaction can not carry out, and when temperature is higher than 70 DEG C, then due to this reaction For exothermic reaction, reaction speed can be caused too fast, reaction system stability declines, and causes dangerous.
Embodiment 11
Basic step is same as Example 1, the difference is that perfluoro decane and dimethyl silicon fluoride reaction time, specifically For 0.5h, 1h, 1.5h, 2h, 2.5h.Multi-element compounds prepared by the embodiment carry out characterization of structure and properties it is found that the perfluor last of the ten Heavenly stems The multi-element compounds that alkane reacts 1~2h preparations with dimethyl silicon fluoride can not only simply and efficiently blister, and foam stabilizing effect It is good, chromatographic isolation will not occur when can migrate in the earth formation.When reaction when perfluoro decane is reacted with dimethyl silicon fluoride Between be less than 1h when, then reaction cannot fully carry out, yield reduce.And when reacted between be higher than 2h when, then react and be basically completed, To extend reality in vain, production efficiency is reduced, is wasted time and the energy (heating).
Embodiment 12
Basic step is same as Example 1, the difference is that the reaction temperature after acidification, specially 140 DEG C, 150 ℃,160℃,170℃,180℃.Multi-element compounds prepared by the embodiment are subjected to characterization of structure and properties it is found that being risen after acidification The multi-element compounds that temperature is prepared to 150~170 DEG C can not only simply and efficiently blister, and foam stabilizing effect is good, can be on stratum Chromatographic isolation will not occur when middle migration.When reaction temperature after acidification is less than 150 DEG C, then reacts progress slowly or even stop Only, it is unable to get required reaction product, and when the reaction temperature after acidification is higher than 170 DEG C, then reaction speed is too fast, reaction Heat can not be transmitted in time, and reaction controlling is difficult, even will appear danger.
Embodiment 13
Basic step is same as Example 1, the difference is that the time of reacting ethylene oxide is added, specially 0.5h, 1h,1.5h,2h,2.5h.Multi-element compounds prepared by the embodiment carry out characterization of structure and properties it is found that addition ethylene oxide is anti- Answering multi-element compounds prepared by 1~2h can not only simply and efficiently blister, and foam stabilizing effect is good, can migrate in the earth formation Chromatographic isolation occurs for Shi Buhui.When the time that reacting ethylene oxide is added being less than 1h, then reaction cannot be carried out fully, yield drop It is low.And when reacted between when being higher than 2h, then react and be basically completed, extend practical to be invalid, reduce production efficiency, when waste Between and the energy (heating).
Embodiment 14
Basic step is same as Example 1, the difference is that the time of elaidin reaction is added, specially 1h, 1.5h, 2h,2.5h.Multi-element compounds prepared by the embodiment carry out characterization of structure and properties it is found that hydroxy benzene sulfonic acid reaction 1.5 is added Multi-element compounds prepared by~2h can not only simply and efficiently blister, and foam stabilizing effect is good, when can migrate in the earth formation not Chromatographic isolation can occur.When the time that elaidin reaction is added being less than 1.5h, then reaction cannot be carried out fully, and yield reduces.And It when being higher than 2h between when reacted, then reacts and has been basically completed, extend practical to be invalid, reduce production efficiency, waste time and energy Source (heating).
By above-described embodiment it is found that the more ethyoxyls of the mono- perfluoro decyl silicon-of dimethyl-- oleate diversification of the present invention Closing object can not only simply and efficiently blister, and foam stabilizing effect is good, and chromatographic isolation will not occur when can migrate in the earth formation; Preparation method is simple simultaneously, and at low cost, operability is strong.

Claims (10)

1. a kind of more ethyoxyls of mono- perfluoro decyl silicon-of dimethyl-- oleate multi-element compounds, it is characterised in that:The polynary chemical combination The structural formula of object is:
Wherein, n=6~24.
2. the more ethyoxyls of the mono- perfluoro decyl silicon-of dimethyl-according to claim 1-oleate multi-element compounds, feature It is:N=10~18.
3. a kind of more ethyoxyls of the mono- perfluoro decyl silicon-of dimethyl-described in claim 1-oleate multi-element compounds of preparing Method, it is characterised in that include the following steps:Perfluoro decane is mixed with dimethyl silicon fluoride, is acidified, is warming up to 150~170 DEG C be added ethylene oxide, oleic acid is added after reaction, finally adjust pH to 8~9.5.
4. the more ethyoxyls of the mono- perfluoro decyl silicon-of the dimethyl-- oleate multi-element compounds according to claim 3 of preparing Method, it is characterised in that:The molar ratio of the perfluoro decane and dimethyl silicon fluoride is 1:0.5~3.
5. the more ethyoxyls of the mono- perfluoro decyl silicon-of the dimethyl-- oleate multi-element compounds according to claim 3 of preparing Method, it is characterised in that:The molar ratio of the perfluoro decane and ethylene oxide is 1:5~40.
6. the more ethyoxyls of the mono- perfluoro decyl silicon-of the dimethyl-- oleate multi-element compounds according to claim 3 of preparing Method, it is characterised in that:The molar ratio of the perfluoro decane and oleic acid is 1:0.5~2.4.
7. the more ethyoxyls of the mono- perfluoro decyl silicon-of the dimethyl-- oleate multi-element compounds according to claim 3 of preparing Method, it is characterised in that:The perfluoro decane reacts 1~2h with dimethyl silicon fluoride under the conditions of 50~70 DEG C.
8. the more ethyoxyls of the mono- perfluoro decyl silicon-of the dimethyl-- oleate multi-element compounds according to claim 3 of preparing Method, it is characterised in that:1~2h of the addition reacting ethylene oxide.
9. the more ethyoxyls of the mono- perfluoro decyl silicon-of the dimethyl-- oleate multi-element compounds according to claim 3 of preparing Method, it is characterised in that:1.5~2h of the addition elaidin reaction.
10. a kind of existed using the more ethyoxyls of the mono- perfluoro decyl silicon-of dimethyl-- oleate multi-element compounds described in claim 1 Application in the oil removing of oil field.
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CN111642515A (en) * 2020-06-01 2020-09-11 南京师范大学 Cyhalothrin nano slow-release pesticide preparation and preparation method thereof

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CN111587890A (en) * 2020-06-01 2020-08-28 南京师范大学 Methylamino abamectin benzoate nano slow-release pesticide preparation and preparation method thereof
CN111642515A (en) * 2020-06-01 2020-09-11 南京师范大学 Cyhalothrin nano slow-release pesticide preparation and preparation method thereof

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