CN107541200A - A kind of preparation method of displacement of reservoir oil furfural extract oil sulfonate - Google Patents
A kind of preparation method of displacement of reservoir oil furfural extract oil sulfonate Download PDFInfo
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- CN107541200A CN107541200A CN201610470507.2A CN201610470507A CN107541200A CN 107541200 A CN107541200 A CN 107541200A CN 201610470507 A CN201610470507 A CN 201610470507A CN 107541200 A CN107541200 A CN 107541200A
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Abstract
A kind of preparation method the present invention relates to displacement of reservoir oil with furfural extract oil sulfonate, it is divided to following two steps：(1) furfural extract oil is added in four-hole bottle, is warming up to 20 60 DEG C, be passed through the SO that concentration is 3 10%3Sulfonating reaction is carried out, is reacted 0.5 3 hours, stopping is passed through SO3, reaction temperature is kept, continues reaction 13 hours, obtains intermediate product sulfonic acid；(2) control temperature that the NaOH solution that concentration is 5 30% is added dropwise into intermediate product, reacts 0.5 1 hours, produces product at 30 55 DEG C.The displacement of reservoir oil prepared by present invention furfural extract oil sulfonate, it is 1 with cocoanut fatty acid diethanolamide (6501) composition mass ratio:1 1.5 oil displacement system, lab simulation improve oil recovery factor up to 18.2%, reach good application effect.
Description
Technical field
It is more particularly to a kind of to be applied to high-temperature oil reservoir displacement of reservoir oil furfural extract oil the present invention relates to technical field of tertiary oil recovery
Sulfonate surfactant and preparation method thereof.
Background technology
In oil field development, even in optimal reservoir, traditional primary oil recovery（Utilize the natural energy of reservoir）With two
Secondary oil recovery（Water filling or gas injection etc.）The 40%-60% of prime stratum crude oil reserve can only be produced；If formation condition is undesirable, once and
Even also 80% original oil in place remains in underground after secondary oil recovery.
The tertiary oil recovery technology that has used now, i.e., with either physically or chemically being exploited.It is used to adopt three times both at home and abroad
The kinds of surfactants of oil is a lot, and the petroleum sulfonate using fraction oil of petroleum as Material synthesis is widely used in adopting three times
Oil.For high temperature, high salinity reservoir, present people mainly use the preferable anionic group of temperature tolerance and salt tolerance is preferably non-
Ionic group is connected in same molecular structure, can reach heat-resistant salt-resistant effect simultaneously.But due to such surfactant
Complex manufacturing, be not suitable for large-scale production.
At present, domestic common oil reservoir, the more universal surfactant oil displacement of application is sulfonate surfactant, its
Petrochina sulfonate and alkyl benzene sulfonate surfactant portion are maximum.But for high temperature, high salinity reservoir, above-mentioned two
The compatibility on class surfactant and stratum is poor, is unable to reach ultralow interfacial tension, and then can not increase substantially recovery ratio.
Simultaneously as petroleum sulfonate raw material derives from decompression residuum or leftover bits and pieces mostly, can sulfonate component (aromatic hydrocarbons) content it is few, and then
Cause that active principle content in product is less, and oil displacement efficiency is general in high temperature, high salinity reservoir.Therefore, for high temperature, high salt oil
Hide, develop it is a kind of it is cheap, temperature resistance is good, be adapted to this kind of reservoir condition surface active agent for tertiary oil recovery have it is important
Meaning.
The content of the invention
The technical problems to be solved by the invention are to provide one kind and are applied to high-temperature oil reservoir displacement of reservoir oil furfural extract oil sulfonic acid
Type surfactant and preparation method thereof；Described furfural extract oil sulfonate temperature resistance is good, cost is cheap, can shape with crude oil
Into 10-3MN/m ultralow interfacial tensions, it is obvious to improve high temperature and high salt oil deposit oil recovery factor.
The preparation method of the displacement of reservoir oil of the present invention furfural extract oil sulfonate, it is characterised in that comprise the following steps：
(1) furfural extract oil is added in reactor, is warming up to 20-60 DEG C, be passed through SO3Sulfonating reaction is carried out, reaction 0.5-3 is small
When, stopping is passed through SO3, reaction temperature is kept, continues to react 1-3 hours, obtains intermediate product sulfonic acid；(2) control temperature exists
30-55 DEG C, NaOH solution is added dropwise into intermediate product, reacts 0.5-1 hours, produces product.
Usually, raw material furfural extract oil arene content >=35%.
The SO3Concentration is 3-10%, preferably SO3Concentration is 5%.
The NaOH concentration is 5-30%, and preferably NaOH concentration is 15%.
Reaction temperature in the step (1) is 40 DEG C, and the reaction temperature in (2) is 35 DEG C.
It is of the invention to be by the displacement of reservoir oil prepared by above-mentioned preparation method furfural extract oil sulfonate, its structural formula：
Wherein, R is alkyl group；- SO3Na position is ortho position, meta or contraposition, it is preferable that R is C7-C13 alkyl
Group ,-SO3Na position is meta.
The displacement of reservoir oil furfural extract oil sulfonate prepared using the present invention, with cocoanut fatty acid diethanolamide (6501)
It is 1 to form mass ratio:1-1.5 oil displacement system, it is 85 DEG C, salinity 15000-50000ppm in formation temperature, calcium ions and magnesium ions
During 400-800ppm, the interfacial tension value of the double IV time block crude oil in river of Henan Oil Field can be reduced to 10-3The mN/m orders of magnitude.It is indoor
Simulation improves oil recovery factor up to 18.2%, reaches good application effect.
Brief description of the drawings
Fig. 1 is the infrared spectrogram of displacement of reservoir oil furfural extract oil sulfonate of the embodiment of the present invention.
Embodiment
Embodiment and the experimental example further explanation present invention are prepared below by specific.
The displacement of reservoir oil prepared in following examples can be characterized by the following method with furfural extract oil sulfonate：Using U.S.
State Nicolet iS5-J Fourier infrared spectrographs, determine product chemistry structure.
As shown in Figure 1：2925、2855 cm-1Left and right is the characteristic absorption peak of alkyl chain；1636 cm-1Left and right is phenyl ring bone
Frame vibration absorption peak；1457 cm-1It is the absworption peak of methyl flexural vibrations；1181cm-1Left and right is S=O asymmetric stretching vibration
Characteristic absorption peak；1049cm-1Left and right is the characteristic absorption peak of S=O symmetrical stretching vibrations., can be true by the analysis to Fig. 1
Fixed output quota thing is furfural extract oil sulfonate.
Embodiment 1
(1), the preparation of intermediate furfural extract oil sulfonic acid
Furfural extract oil is added in four-hole bottle, stirring is opened, is warming up to 40 DEG C, is passed through the SO that concentration is 5%3Mixed gas
Sulfonating reaction is carried out, is reacted 1 hour, stopping is passed through SO3, reaction temperature is kept, aging 1.5 hours, that is, obtains intermediate product sulphur
Acid.
(2), the preparation of furfural extract oil sulfonate
Control four-hole bottle temperature to open stirring at 35 DEG C, the NaOH solution that concentration is 15% is slowly added dropwise into intermediate product, adjusts
PH value is saved to 8-9, continues stirring 1 hour, after water removal is dried, produces product furfural extract oil sulfonate.
(3), the test of interfacial tension
Oil displacement system：The mass ratio of furfural extract oil sulfonate and cocoanut fatty acid diethanolamide (6501) is 1:1 composition
System
Experimental temperature：85℃
Test rotating speed：4500rpm
Crude oil：The double block crude oil of river IV time of Henan Oil Field
Simulation water：Salinity about 20000ppm, calcium ions and magnesium ions 500ppm
Tester：TX-500C rotating interfacial tensimeters
Test result is as shown in table 1 below：
| Oil displacement system mass concentration (%) | Oil water interfacial tension (10-3mN/m) |
| 0.10 | 2.72 |
| 0.15 | 1.29 |
| 0.20 | 4.31 |
| 0.25 | 3.84 |
| 0.30 | 5.12 |
Oil displacement system mass concentration is 0.15%, and laboratory simulation flooding effect improves oil recovery factor up to 18.2% compared with water drive.
Embodiment 2
(1), the preparation of intermediate furfural extract oil sulfonic acid
Furfural extract oil is added in four-hole bottle, stirring is opened, is warming up to 45 DEG C, is passed through the SO that concentration is 8%3Mixed gas
Sulfonating reaction is carried out, is reacted 1 hour, stopping is passed through SO3, reaction temperature is kept, aging 1.5 hours, that is, obtains intermediate product sulphur
Acid.
(2), the preparation of furfural extract oil sulfonate
Control four-hole bottle temperature to open stirring at 30 DEG C, the NaOH solution that concentration is 15% is slowly added dropwise into intermediate product, adjusts
PH value is saved to 8-9, continues stirring 1 hour, after water removal is dried, produces product furfural extract oil sulfonate.
(3), the test of interfacial tension
Oil displacement system：The mass ratio of furfural extract oil sulfonate and cocoanut fatty acid diethanolamide (6501) is 1:1.2 group
Into system
Experimental temperature：85℃
Test rotating speed：4500rpm
Crude oil：The double block crude oil of river IV time of Henan Oil Field
Simulation water：Salinity about 15000ppm, calcium ions and magnesium ions 400ppm
Tester：TX-500C rotating interfacial tensimeters
Test result is as shown in table 2 below：
| Oil displacement system mass concentration (%) | Oil water interfacial tension (10-3mN/m) |
| 0.10 | 4.27 |
| 0.15 | 3.91 |
| 0.20 | 3.58 |
| 0.25 | 2.40 |
| 0.30 | 4.18 |
Oil displacement system mass concentration is 0.25%, and laboratory simulation flooding effect improves oil recovery factor up to 16.4% compared with water drive.
Embodiment 3
(1), the preparation of intermediate furfural extract oil sulfonic acid
Furfural extract oil is added in four-hole bottle, stirring is opened, is warming up to 40 DEG C, is passed through the SO that concentration is 10%3Mixed gas
Sulfonating reaction is carried out, is reacted 2 hours, stopping is passed through SO3, reaction temperature is kept, aging 1 hour, that is, obtains intermediate product sulfonic acid.
(2), the preparation of furfural extract oil sulfonate
Control four-hole bottle temperature to open stirring at 35 DEG C, the NaOH solution that concentration is 15% is slowly added dropwise into intermediate product, adjusts
PH value is saved to 8-9, continues stirring 0.5 hour, after water removal is dried, produces product furfural extract oil sulfonate.
(3), the test of interfacial tension
Oil displacement system：The mass ratio of furfural extract oil sulfonate and cocoanut fatty acid diethanolamide (6501) is 1:1.5 group
Into system
Experimental temperature：85℃
Test rotating speed：4500rpm
Crude oil：The double block crude oil of river IV time of Henan Oil Field
Simulation water：Salinity about 30000ppm, calcium ions and magnesium ions 800ppm
Tester：TX-500C rotating interfacial tensimeters
Test result is as shown in table 3 below：
| Oil displacement system mass concentration (%) | Oil water interfacial tension (10-3mN/m) |
| 0.10 | 3.06 |
| 0.15 | 3.85 |
| 0.20 | 2.78 |
| 0.25 | 5.19 |
| 0.30 | 5.82 |
Oil displacement system mass concentration is 0.20%, and laboratory simulation flooding effect improves oil recovery factor up to 12.9% compared with water drive.
Claims (9)
1. a kind of displacement of reservoir oil preparation method of furfural extract oil sulfonate, it is characterised in that comprise the following steps：(1) by furfural
Tapped oil is added in reactor, is warming up to 20-60 DEG C, is passed through SO3Sulfonating reaction is carried out, 0.5-3 hours is reacted, stops being passed through
SO3, reaction temperature is kept, continues to react 1-3 hours, obtains intermediate product sulfonic acid；
(2) control temperature that NaOH solution is added dropwise into intermediate product at 30-55 DEG C, react 0.5-1 hours, produce product.
2. preparation method according to claim 1, it is characterised in that raw material furfural extract oil arene content >=35%.
3. preparation method according to claim 1, it is characterised in that SO3Concentration is 3-10%.
4. preparation method according to claim 3, it is characterised in that SO3Concentration is 5%.
5. preparation method according to claim 1, it is characterised in that NaOH concentration 5-30%.
6. preparation method according to claim 5, it is characterised in that NaOH concentration 15%.
7. preparation method according to claim 1, it is characterised in that the reaction temperature in step (1) is 40 DEG C, in (2)
Reaction temperature be 35 DEG C.
8. a kind of displacement of reservoir oil furfural extract oil sulfonate prepared by any described preparation methods of claim 1-7, its feature
It is：Structural formula is：
Wherein, R is alkyl group；- SO3Na position is ortho position, meta or contraposition.
9. the displacement of reservoir oil according to claim 8 furfural extract oil sulfonate, it is characterised in that R is C7-C13 alkyl collection
Group ,-SO3Na position is meta.
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101659861A (en) * | 2008-08-29 | 2010-03-03 | 中国石油天然气股份有限公司 | Preparation method of petroleum sulfonate oil displacement agent |
| CN101955450A (en) * | 2009-07-20 | 2011-01-26 | 中国石油天然气股份有限公司 | Petroleum sulfonate composition and preparation method and application thereof |
| US20160168447A1 (en) * | 2014-12-11 | 2016-06-16 | Instituto Mexicano Del Petróleo | Hydroxypropyl betaine based zwitterionic geminal liquids, obtaining process and use as wettability modifiers with inhibitory/dispersants properties of asphaltenes |
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- 2016-06-24 CN CN201610470507.2A patent/CN107541200A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101659861A (en) * | 2008-08-29 | 2010-03-03 | 中国石油天然气股份有限公司 | Preparation method of petroleum sulfonate oil displacement agent |
| CN101955450A (en) * | 2009-07-20 | 2011-01-26 | 中国石油天然气股份有限公司 | Petroleum sulfonate composition and preparation method and application thereof |
| US20160168447A1 (en) * | 2014-12-11 | 2016-06-16 | Instituto Mexicano Del Petróleo | Hydroxypropyl betaine based zwitterionic geminal liquids, obtaining process and use as wettability modifiers with inhibitory/dispersants properties of asphaltenes |
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