CN106244129A - A kind of surfactant oil displacement and preparation method thereof - Google Patents
A kind of surfactant oil displacement and preparation method thereof Download PDFInfo
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Abstract
The invention provides a kind of surfactant oil displacement, and described surfactant is cloudy non-surface-active agent, and its general formula of molecular structure is:Wherein R is C5~C20One in alkyl;The span of x is the arbitrary integer of 1~10;M is monovalent cation, for Li+、Na+、K+、NH4 +In one.Relative to prior art, cloudy non-surface-active agent described in the invention as tertiary oil recovery combination chemical flooding oil displacement agent, can have the advantage that the oil water interfacial tension value of its single dose solution of cloudy non-surface-active agent prepared by the present invention and poly-/table binary system is all 10‑3The mN/m order of magnitude, meets the interfacial tension standard-required of the tertiary oil recovery combination chemical flooding surfactant to being used, and solves the chromatographic isolation problem that in existing chemical flooding technology of reservoir sweep, high temperature and high salt oil deposit compound surfactant exists.
Description
Technical field
The invention belongs to the tertiary oil recovery chemical displacement of reservoir oil and improves recovery ratio field, especially relates to a kind of displacement of reservoir oil and uses
There is surfactant of anion and nonionic characteristic and preparation method thereof simultaneously.
Background technology
The chemical combined flooding oil tech using surfactant can increase substantially oil recovery factor.The work of surfactant
With being to reduce the interfacial tension between oil reservoirs profit, reduce oil droplet when making remaining oil move and deform the resistance brought, thus greatly
Width improves oil displacement efficiency.In the tertiary oil recovery at home and abroad of anion surfactant and nonionic surfactant most widely used
General, anion surfactant interfacial activity is high, and adsorbance is little in the earth formation, but its salt tolerance and anti-hydraulic properties are poor;Non-
Although ionic surface active agent has preferable salt tolerant, resistance to hard water ability, but temperature sensitive, it is impossible to meet high temperature, high salt oil
Hide requirement, and environment is had certain pollution.In actual applications, by nonionic surfactant and anionic surface are lived
Property agent carry out compounding anion surfactant salt tolerance difference and the problem of nonionic surfactant temperature tolerance difference of solving, be
The method that oil field is the most commonly used at present.
Along with the compound surfactant extensive application in tertiary oil recovery technology, expose problems with: owing to driving
Oil systems is compounding compound, usually contains multiple (two or more) anion surfactant and nonionic surfactant,
In injection process, oil displacement system is adsorbed step by step by stratum, problem chromatographic isolation easily occur, thus reduces oil displacement system
Working substance content and oil displacement efficiency.
One of anionic and nonionic surfactant focus being always tertiary oil recovery field research in recent years, owing to its molecule is tied
Two kinds of anionic groups of different nature and non-ionic group are designed in same surfactant molecule by structure so that it is hold concurrently
Tool anion and the advantage of nonionic surfactant, have complementary advantages, and interface performance is excellent, can be in the widest concentration range
Oil water interfacial tension is made to keep ultralow value.Particularly with poly-/table binary displacement system, owing to there is no not only avoiding of alkali
The problems such as the blocking of oil reservoir, fouling and corrosion, and ultralow interfacial tension can be formed with crude oil.
Summary of the invention
In view of this, the invention aims to high temperature, high salinity reservoir, the surface activity that alkali-free is applied under the conditions of using
Agent oil displacement system, proposes a kind of displacement of reservoir oil with having anion and the cloudy non-surface-active agent of nonionic characteristic and preparation side thereof simultaneously
Method, to solve the chromatographic isolation problem that in existing chemical displacement of reservoir oil technology, high temperature and high salt oil deposit compound surfactant exists.
For reaching above-mentioned purpose, the technical scheme of the invention is achieved in that
A kind of surfactant oil displacement, described surfactant is cloudy non-surface-active agent, and its general formula of molecular structure is:
Wherein R is C5~C20One in alkyl;The span of x is the arbitrary integer of 1~10;M is monovalent cation,
For Li+、Na+、K+、NH4 +In one.
Further, R is C10~C16One in alkyl;X is the arbitrary integer between 3~8.
The present invention also provides for the preparation method of a kind of described surfactant oil displacement, comprises the steps:
(1) amidation process of alkyl acid methyl ester: by alkyl acid methyl ester and ethanolamine according to required proportioning with a certain amount of
Sodium hydroxide solution mixes, and under nitrogen protection environment, Stress control is in below 0.3MPa, reaction temperature 65~80 DEG C, reaction
Time 3~4h, and discharge methanol, reaction obtains alkyl alcohol amide;
(2) sulfonating reaction of alkyl alcohol amide: alkyl alcohol amide step (1) obtained and sulfur trioxide are by required
Proportioning is reacted at a temperature of 45~55 DEG C, and nitrogen is protected, and Stress control, at below 0.3MPa, in the response time 4~6h, is passed through nitrogen
Get rid of unreacted SO3Gas, obtains alkylamide ethyoxyl sulfonic acid;
(3) the neutralization reaction of alkylamide ethyoxyl sulfonic acid: alkylamide ethyoxyl sulfonic acid step (2) obtained is slow
Joining in alkali liquor, 50 DEG C of abundant reactions of constant temperature, regulation pH value, to neutral, obtains alkylamide ethyoxyl sulfonate;
(4) addition reaction of alkylamide ethyoxyl sulfonate: the alkylamide ethyoxyl sulfonate that step (3) is obtained
Mix with a certain amount of catalyst sodium hydroxide by required proportioning with oxirane, reaction temperature 130 DEG C, Stress control 5~
8MPa, reacts 6~8h, obtains containing polyoxyethylene ether and the alkylamide of two kinds of groups of ethyoxyl sulfonate simultaneously.
Further, in described step (1), alkyl acid methyl ester and ethanolamine mol ratio are 1:(1~1.5), sodium hydroxide is used
Amount is the 0.2~3% of alkyl acid methyl ester quality.
Further, alkyl alcohol amide and mol ratio 1:(1.2~2 of sulfur trioxide in described step (2)).
Further, the quality adding sodium hydroxide in described step (4) is alkylamide ethyoxyl sulfonate quality
0.5~3%.
Present invention additionally comprises the discrimination method of described surfactant oil displacement, described discrimination method is lived about surface
The ionic discriminating of property agent comprises the steps:
(1) indicator solution preparation: by containing 0.1g/L bromo Midi drone and the ethanol of 0.05g/L curing indigo plant VN150
Sulfuric acid solution mixes as mixed indicator solution;
(2) test method: take a small amount of surfactant samples to be measured and be dissolved in a small amount of water, be divided into two parts, a solution
PH value be transferred to 1, another part is transferred to 11, quiet after respectively adding 10mL mixed indicator solution and 10mL chloroform, fully shake
Put layering, observe the color of chloroform layer, if the chloroform layer that result of the test is two parts of solution all shows pink, show to live in this surface
Property agent display anionic property.
Further, in described discrimination method, discriminating about SURFACTANTS Nonionic comprises the steps:
(1) indicator solution preparation: 174g ammonium thiocyanate and 28g cobalt nitrate are dissolved in 1L distilled water, prepare to obtain sulfur
Cyanic acid cobalt reagent;
(2) test method: take the aqueous surfactant solution 5mL to be measured of 1%, adds in 5mL Cobaltous rhodanide reagent, shake
Make to be sufficiently mixed, after placing 2h, observe solution colour change, if result of the test display solution colour is blue, show there is polyoxy second
Ene-type surfactant exists, this surfactant display nonionic.
Relative to prior art, the cloudy non-surface-active agent described in the invention can be as tertiary oil recovery combination chemical flooding
With oil displacement agent, have the advantage that
(1) cloudy non-surface-active agent and the Dagang Oilfield Gang Xi tri-district polymer flooding that prepared by the preparation method of the present invention are on-the-spot
The polymer (polyacrylamide) used has good oil reservoir matching, with polyacrylamide as poly-/table binary displacement of reservoir oil
System has preferable interfacial activity;
(2) oil-water interfaces of its single dose solution of cloudy non-surface-active agent prepared by the present invention and poly-/table binary system are opened
Force value is all 10-3The mN/m order of magnitude, meets the interfacial tension mark of the tertiary oil recovery combination chemical flooding surfactant to being used
Alignment request, solves the chromatographic isolation that in existing chemical flooding technology of reservoir sweep, high temperature and high salt oil deposit compound surfactant exists and asks
Topic.
Detailed description of the invention
Unless otherwise indicated, term used herein is respectively provided with the implication that those skilled in the art's routine understands, in order to
Readily appreciate the present invention, terms more used herein have been carried out following definitions.
Using in the specification and in the claims, odd number type " " and " this " include plural reference, unless on
The most separately have and clearly state.Such as, term " (one) cell " includes the cell of plural number, including its mixture.
All of Digital ID, such as pH, temperature, time, concentration, including scope, be all approximation.It is to be understood that, although
Term " about " is all added before all of Digital ID of the clearest and the most definite narration.Simultaneously it will also be understood that, although the clearest and the most definite
Narration, reagent described herein is only example, and its equivalent is known in the art.
In order to be best understood from technique scheme, it is described in detail below in conjunction with embodiment.
Embodiment 1:
Prepare polyoxyethylene ether (x=3)-ethyoxyl sodium sulfonate-decane amide, specifically comprise the following steps that
(1) amidation process of decane acid methyl ester: to airtight equipped with four mouthfuls of condensing unit, agitating device and temperature regulating device
Being sequentially added into 0.5g sodium hydroxide, 200g decane acid methyl ester, 61g ethanolamine and 50g distilled water in reactor, stirring is warming up to 70
DEG C, nitrogen is protected, and Stress control is after below 0.3MPa, reaction 3~4h, and methanol is reclaimed in evacuation condensation, and products therefrom is
Decane glycollic amide;
(2) sulfonating reaction of decane glycollic amide: the decane glycollic amide that step (1) obtains all is proceeded to temperature control injection
In reactor, nitrogen protect, below Stress control 0.3MPa, 1.2mol sulfan gasification after with 3~5mL/s speed
Spurting into reactor, circulating water, temperature maintains 45~55 DEG C, is filled with nitrogen and gets rid of unnecessary SO after reaction 5h3Gas, institute
Obtain product and be decane amide ethyoxyl sulfonic acid;
(3) the neutralization reaction of decane amide ethyoxyl sulfonic acid: sodium hydroxide solution is slowly added into what step (2) obtained
In product, constant temperature 50 DEG C stirring, regulate pH value after reaction 6h the most neutral, obtain decane amide ethyoxyl sodium sulfonate;
(4) addition reaction of decane amide ethyoxyl sodium sulfonate: the decane amide ethyoxyl sodium sulfonate that step (3) is obtained
Proceeding to high temperature high pressure enclosed reactor, add 5g sodium hydroxide and 50g distilled water, start agitating device, nitrogen is protected, and is passed through
3mol oxirane, is warming up to 130 DEG C, and Stress control, at 5MPa, reacts 5h, obtains polyoxyethylene ether (x=3)-ethyoxyl sulphur
Acid sodium-decane amide.
Polyoxyethylene ether (the x=3)-ethyoxyl sodium sulfonate-decane amide of preparation is carried out (non-) ionic test, result
Confirm this surfactant and both shown anionic property, show yet nonionic.
Embodiment 2:
Prepare polyoxyethylene ether (x=6)-ethyoxyl sodium sulfonate-dodecane amide, specifically comprise the following steps that
(1) amidation process of methyl laurate: to close equipped with four mouthfuls of condensing unit, agitating device and temperature regulating device
Closing and be sequentially added into 2.28g sodium hydroxide, 228g methyl laurate, 73g ethanolamine and 50g distilled water in reactor, stirring rises
Temperature is to 70 DEG C, and nitrogen is protected, and Stress control is after below 0.3MPa, reaction 3~4h, and methanol is reclaimed in evacuation condensation.Product is i.e.
For dodecane glycollic amide;
(2) sulfonating reaction of dodecane glycollic amide: the dodecane glycollic amide that step (1) obtains all is proceeded to temperature control
In injection reactor, nitrogen is protected, with 3~5mL/s after the gasification of below Stress control 0.3MPa, 1.5mol sulfan
Speed spurts into reactor, circulating water, and temperature maintains 45~55 DEG C, is filled with nitrogen and gets rid of unnecessary SO after reaction 5h3Gas
Body.Product is dodecane amide ethyoxyl sulfonic acid;
(3) the neutralization reaction of dodecane amide ethyoxyl sulfonic acid: sodium hydroxide solution is slowly added into step (2) and obtains
Product in, constant temperature 50 DEG C stirring, regulate pH value after reaction 6h to neutral, obtain dodecane amide ethyoxyl sodium sulfonate;
(4) addition reaction of dodecane amide ethyoxyl sodium sulfonate: the dodecane amide ethyoxyl sulphur that step (3) is obtained
Acid sodium proceeds to high temperature high pressure enclosed reactor, adds 4g sodium hydroxide and 50g distilled water, starts agitating device, and nitrogen is protected, logical
Entering 6mol oxirane, be warming up to 130 DEG C, Stress control, at about 6MPa, reacts 5h, obtains polyoxyethylene ether (x=6)-second
Epoxide sodium sulfonate-dodecane amide.
Polyoxyethylene ether (the x=6)-ethyoxyl sodium sulfonate-dodecane amide of preparation is carried out (non-) ionic test, knot
Fruit is confirmed this surfactant and had both shown anionic property, show yet nonionic.
Embodiment 3:
Prepare polyoxyethylene ether (x=8)-ethyoxyl sodium sulfonate-palmitic amide, specifically comprise the following steps that
(1) amidation process of methyl palmitate: to close equipped with four mouthfuls of condensing unit, agitating device and temperature regulating device
Closing and be sequentially added into 8.5g sodium hydroxide, 284g methyl palmitate, 91.5g ethanolamine and 70g distilled water in reactor, stirring rises
Temperature is to 70 DEG C, and nitrogen is protected, and Stress control is after below 0.3MPa, reaction 3~4h, and methanol is reclaimed in evacuation condensation.Product is i.e.
For cetane ethanol amide;
(2) sulfonating reaction of cetane ethanol amide: the cetane ethanol amide that step (1) obtains all is proceeded to temperature control
In injection reactor, nitrogen protect, below Stress control 0.3MPa, 2mol sulfan gasification after with 3~5mL/s speed
Degree spurts into reactor, circulating water, and temperature maintains 45~55 DEG C, is filled with nitrogen and gets rid of unnecessary SO after reaction 5h3Gas.
Product is palmitic amide ethyoxyl sulfonic acid;
(3) the neutralization reaction of palmitic amide ethyoxyl sulfonic acid: sodium hydroxide solution is slowly added into step (2) and obtains
Product in, constant temperature 50 DEG C stirring, regulate pH value after reaction 6h to neutral, obtain palmitamide ethyoxyl sodium sulfonate;
(4) addition reaction of palmitic amide ethyoxyl sodium sulfonate: the palmitic amide ethyoxyl sulphur that step (3) is obtained
Acid sodium proceeds to high temperature high pressure enclosed reactor, adds 12.4g sodium hydroxide and 80g distilled water, starts agitating device, and nitrogen is protected
Protecting, be passed through 8mol oxirane, be warming up to 130 DEG C, Stress control, at 8MPa, reacts 5h, obtains polyoxyethylene ether (x=8)-second
Epoxide sodium sulfonate-palmitic amide.
Polyoxyethylene ether (the x=8)-ethyoxyl sodium sulfonate-palmitic amide of preparation is carried out (non-) ionic test, knot
Fruit is confirmed this surfactant and had both shown anionic property, show yet nonionic.
Prepared cloudy non-surface-active agent is carried out the discrimination method of ionic and nonionic by above-described embodiment
Concretely comprise the following steps: (1) preparation mixed indicator solution: containing 0.1g/L bromo Midi drone and 0.05g/L curing indigo plant VN150
Ethanol sulfuric acid solution;
(2) test method: take a small amount of surfactant samples to be measured and be dissolved in a small amount of water, be divided into two parts, a solution
PH value be transferred to 1;Another part is transferred to 11, quiet after respectively adding 10mL mixed indicator solution and 10mL chloroform, fully shake
Putting layering, observe the color of chloroform layer, result of the test is that the chloroform layer of two parts of solution all shows pink, shows this surface activity
Agent display anionic property;
(3) preparation Cobaltous rhodanide reagent: 174g ammonium thiocyanate and 28g cobalt nitrate are dissolved in 1L distilled water;
(4) test method: take the aqueous surfactant solution 5mL to be measured of 1%, adds in 5mL Cobaltous rhodanide reagent, shake
Make to be sufficiently mixed, after placing 2h, observe solution colour change, if result of the test display solution colour is blue, show there is polyoxy second
Ene-type surfactant exists, this surfactant display nonionic.
Experimental example 1:
Dagang Oilfield Gang Xi tri-district is used to inject polyoxyethylene ether-ethyoxyl sulfonic acid that embodiment 1~3 is prepared by water respectively
Sodium-alkylamide is configured to containing 0.05,0.1,0.2,0.3,0.5wt% (by percentage to the quality) surfactant
0.15wt% polyacrylamide (degree of hydrolysis 40%, relative molecular weight is 25,000,000) aqueous solution, observes surfactant in polymerization
Dissolving situation in thing aqueous solution.Result of the test is: 5 kinds of preparation liquid are the dispersed solution without layering.
Experimental example 2:
Polyoxyethylene ether-ethyoxyl sodium sulfonate-alkylamide prepared by embodiment 1~3 is made into the table of 0.3wt% concentration
Face aqueous surfactant solutions, with port, shallow 10-7 well dehydration degassed crude is as oil phase, test Dagang Oilfield Guantao 60 DEG C of reservoir temperatures of group
Under crude oil time dependent oil water interfacial tension value, result of the test is shown in Table 1.
Experimental example 3:
Polyoxyethylene ether-ethyoxyl sodium sulfonate-alkylamide and polyacrylamide prepared by embodiment 1~3 as poly-/
Table binary displacement system, investigates its oil water interfacial tension value.Test method is: first, utilizes the scene water preparation of Gang Xi tri-district
0.15wt% polyacrylamide (degree of hydrolysis 40%, relative molecular weight is 25,000,000) aqueous solution;Secondly, add 0.3wt% this
The surfactant of bright preparation, stirs, and is configured to surfactant prepared by the concentration present invention containing 0.3wt%
0.15wt% polyacrylamide solution;Finally, with port, shallow 10-7 well dehydration degassed crude is as oil phase, tests Dagang Oilfield Guantao
Organizing the crude oil time dependent oil water interfacial tension value under 60 DEG C of reservoir temperatures, result of the test is shown in Table 1.
Comparative example 1:
With embodiment 4, with 0.3wt% petroleum sulfonate, (Zhong Sheng petroleum sulfonate factory provides difference triumphantly, has
Effect content 40%) alternate embodiment 1~3 preparation polyoxyethylene ether-ethyoxyl sodium sulfonate-alkylamide, test its profit circle
Surface tension changes.Result of the test is shown in Table 1.
Comparative example 2:
With embodiment 4, difference with containing 0.3wt% petroleum sulfonate (triumph Zhong Sheng petroleum sulfonate factory provides,
Effective content 40%) 0.15wt% polyacrylamide solution, test its oil water interfacial tension change.Result of the test is shown in Table 1.
The different oil displacement system of table 1 is to Gang Xi tri-district oil reservoir interfacial tension value
Being found out by the result of the test in table 1, comparing petroleum sulfonate anionic surfactant, the moon prepared by the present invention is non-
The oil water interfacial tension value of its single dose solution of surfactant and poly-/table binary system is all 10-3The mN/m order of magnitude, meets three
The interfacial tension standard-required of the secondary oil recovery combination chemical flooding surfactant to being used.
The foregoing is only the preferred embodiment of the invention, not in order to limit the invention, all at this
Within the spirit of innovation and creation and principle, any modification, equivalent substitution and improvement etc. made, should be included in the invention
Protection domain within.
Claims (8)
1. a surfactant oil displacement, it is characterised in that: described surfactant is cloudy non-surface-active agent, and its molecule is tied
Structure formula is:
Wherein R is C5~C20One in alkyl;The span of x is the arbitrary integer of 1~10;M is monovalent cation, for Li+、Na+、K+、NH4 +In one.
Surfactant oil displacement the most according to claim 1, it is characterised in that: R is C10~C16One in alkyl;x
It it is the arbitrary integer between 3~8.
3. the preparation method of the surfactant oil displacement described in claim 1, it is characterised in that comprise the steps:
(1) amidation process of alkyl acid methyl ester: by alkyl acid methyl ester and ethanolamine according to required proportioning and a certain amount of hydrogen-oxygen
Changing sodium solution mixing, under nitrogen protection environment, Stress control is in below 0.3MPa, reaction temperature 65~80 DEG C, response time 3
~4h, and discharge methanol, reaction obtains alkyl alcohol amide;
(2) sulfonating reaction of alkyl alcohol amide: alkyl alcohol amide step (1) obtained and sulfur trioxide are by required proportioning
Reacting at a temperature of 45~55 DEG C, nitrogen is protected, and Stress control, in below 0.3MPa, response time 4~6h, is passed through nitrogen and gets rid of
Unreacted SO3Gas, obtains alkylamide ethyoxyl sulfonic acid;
(3) the neutralization reaction of alkylamide ethyoxyl sulfonic acid: alkylamide ethyoxyl sulfonic acid step (2) obtained is slowly added to
In alkali liquor, 50 DEG C of abundant reactions of constant temperature, regulation pH value, to neutral, obtains alkylamide ethyoxyl sulfonate;
(4) addition reaction of alkylamide ethyoxyl sulfonate: the alkylamide ethyoxyl sulfonate that step (3) is obtained with
Oxirane is mixed with a certain amount of catalyst sodium hydroxide by required proportioning, reaction temperature 130 DEG C, Stress control 5~
8MPa, reacts 6~8h, obtains containing polyoxyethylene ether and the alkylamide of two kinds of groups of ethyoxyl sulfonate simultaneously.
The preparation method of surfactant oil displacement the most according to claim 3, it is characterised in that: in described step (1)
Alkyl acid methyl ester and ethanolamine mol ratio are 1:(1~1.5), sodium hydroxide concentration is the 0.2~3% of alkyl acid methyl ester quality.
The preparation method of surfactant oil displacement the most according to claim 3, it is characterised in that: in described step (2)
Alkyl alcohol amide and mol ratio 1:(1.2~2 of sulfur trioxide).
The preparation method of surfactant oil displacement the most according to claim 3, it is characterised in that: in described step (4)
Add quality is alkylamide ethyoxyl sulfonate quality the 0.5~3% of sodium hydroxide.
The discrimination method of surfactant oil displacement the most according to claim 1 and 2, it is characterised in that described discriminating side
In method, the discriminating about surface active agent ion comprises the steps:
(1) indicator solution preparation: by containing 0.1g/L bromo Midi drone and the ethanol sulfuric acid of 0.05g/L curing indigo plant VN150
Solution mixes as mixed indicator solution;
(2) test method: take a small amount of surfactant samples to be measured and be dissolved in a small amount of water, be divided into two parts, the pH of a solution
Value is transferred to 1, and another part is transferred to 11, stands and divide after respectively adding 10mL mixed indicator solution and 10mL chloroform, fully shake
Layer, observes the color of chloroform layer, if the chloroform layer that result of the test is two parts of solution all shows pink, shows this surfactant
Display anionic property.
8. according to the discrimination method of the surfactant oil displacement described in claim 1 or 2 or 7, it is characterised in that described discriminating
In method, the discriminating about SURFACTANTS Nonionic comprises the steps:
(1) indicator solution preparation: 174g ammonium thiocyanate and 28g cobalt nitrate are dissolved in 1L distilled water, prepare to obtain Hydrogen thiocyanate
Cobalt reagent;
(2) test method: take the aqueous surfactant solution 5mL to be measured of 1%, adds in 5mL Cobaltous rhodanide reagent, and shake makes to fill
Divide mixing, after placing 2h, observe solution colour change, if result of the test shows that solution colour is blue, show there is polyoxyethylene-type
Surfactant exists, this surfactant display nonionic.
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CN109280021A (en) * | 2017-12-13 | 2019-01-29 | 中国石油天然气股份有限公司 | Surfactant oil displacement and oil displacement agent |
CN109280021B (en) * | 2017-12-13 | 2021-08-03 | 中国石油天然气股份有限公司 | Surfactant for oil displacement and oil displacement agent |
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