CN101279936A - Alkyl phenol sulfonic polyoxyethylene ether sulfate and preparation thereof - Google Patents

Alkyl phenol sulfonic polyoxyethylene ether sulfate and preparation thereof Download PDF

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CN101279936A
CN101279936A CNA200710039052XA CN200710039052A CN101279936A CN 101279936 A CN101279936 A CN 101279936A CN A200710039052X A CNA200710039052X A CN A200710039052XA CN 200710039052 A CN200710039052 A CN 200710039052A CN 101279936 A CN101279936 A CN 101279936A
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polyoxyethylene ether
phenol sulfonic
alkyl phenol
ether sulfate
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陈荣福
沙鸥
张卫东
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China Petroleum and Chemical Corp
Sinopec Shanghai Research Institute of Petrochemical Technology
China Petrochemical Corp
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Sinopec Shanghai Research Institute of Petrochemical Technology
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Abstract

The invention relates to alkylphenol sulfonic polyoxyethylene aether sodium sulfovinate and the preparation method thereof, mainly aiming at solving the problems that current oil displacement agent containing surfactant is poor in oil displacement efficiency under high temperature with the existence of high salt and that the oil displacement agent contains alkali and causes damages to the stratum and the oil field and erodes the equipment and the pipes, which results in high production cost. The invention adopts alkylphenol sulfonic polyoxyethylene aether sodium sulfovinate with general molecular formula (I)to solve the problem; wherein M is alkali metal, ammonium group or amidocyanogen; R is alkyl from C1-C22; n is any integer from 1 to 30. The alkylphenol sulfonic polyoxyethylene aether sodium sulfovinate can be applied to the production of tertiary oil recovery in oil fields.

Description

Alkyl phenol sulfonic polyoxyethylene ether sulfate and preparation method thereof
Technical field
The present invention relates to a kind of alkyl phenol sulfonic polyoxyethylene ether sulfate and preparation method thereof.
Background technology
China's main oilfield is through once with behind the secondary recovery having entered high water-cut stage, crude production rate descends year by year, for improving oil recovery factor, develop remaining reserves to greatest extent, tertiary oil recovery technology is guaranteeing to have brought into play important effect aspect the oilfield stable production high yield.Ternary composite driving (alkali-polymkeric substance-tensio-active agent) technology of wherein using tensio-active agent be owing to still can increase substantially oil displacement efficiency under the situation of low surfactant consumption, so it has become the new technology at economic and technical all very successful raising oil recovery factor.Its dominant mechanism is: after the oil field enters high water-cut stage, surplus oil with discontinuous oil film by trap in the hole of reservoir rocks, two main power that act on the oil droplet are viscaps, if select suitable surfactant system for use, reduce the interfacial tension between profit, make interfacial tension between the oil bearing reservoir profit from the lower or ultralow value (10 of 20~30 milli ox/Mi Jiangzhi -3~10 -4Milli ox/rice), just can reduce the resistance that the oil droplet distortion was brought when surplus oil was moved, thereby significantly improve oil displacement efficiency.Tensio-active agent improves oil recovery factor and depends mainly on sweep efficiency and the oil displacement efficiency of tensio-active agent in oil reservoir.Promptly
Er=Eυ·Ed
In the formula: Er represents recovery ratio, %; E υ represents sweep efficiency, %; Ed represents oil displacement efficiency, %.Therefore, improving Er must start with from improving Ev and Ed.Promoting agent (comprising tensio-active agent and alkali) has effects such as the oil water interfacial tension of reduction, can improve Ed (oil displacement efficiency).This effect can be described by combined effect parameter hollow billet number (N):
Ed∝N
N=motivating force/viscous force ∝ μ υ/Y Ow
In the formula: μ represents to inject phase viscosity; υ represents to inject the phase flow stream velocity; Y OwInterfacial tension between the expression profit.Practice proves: reduce residual oil saturation effectively, the hollow billet number must be improved 3~4 orders of magnitude.Because oil reservoir injection rate and pressure are limited, it is not enough therefore depending merely on raising μ and υ, but can be with oil water interfacial tension Y OwReduce by 3 or the higher order of magnitude, thereby improve the hollow billet number greatly and Ed (oil displacement efficiency) is significantly improved, this also is the main oil-displacement mechanism of promoting agent.And to improve sweep efficiency, and main way is the mobility that reduces displacing fluid, this point can realize by adding polymkeric substance increase displacing fluid viscosity.Adopt in the operation three, utilization ASP ternary composite driving (tensio-active agent/alkali/polymkeric substance) flooding system, can make the ultra low interfacial tension between profit that the displacement of reservoir oil (Ed) rate of imitating is increased by adding tensio-active agent, inject fluid viscosity raising sweep efficiency (Ev) by injection of polymer to increase, inject alkali to reduce the absorption of tensio-active agent.Make full use of the useful synergistic combination effect of ASP, improve oil recovery factor (Er).
At present, in tertiary oil recovery, the tensio-active agent that generally uses contains the tensio-active agent of phenyl ring as sulfonated petro-leum, alkylbenzene sulfonate or other.Document CN1458219A discloses the pure binary ultra low interfacial tension of the surfactant polymer combination flooding prescription that a kind of tertiary oil recovery is used, use therein tensio-active agent is sulfonated petro-leum or is the complexed surfactant that host adds thinner and other surfactant compound with the sulfonated petro-leum, the weight percent of its component is a sulfonated petro-leum 50~100%, alkylsulfonate 0~50%, carboxylate salt 0~50%, alkylaryl sulphonate 0~35%, low-carbon alcohol 0~20%.These tensio-active agents have the source extensively, and no matter quantity advantage big, that price is low for common oil reservoir, is combination flooding or single surfactant flooding, all has the mass-producing product, are also obtaining ideal effect aspect the raising recovery ratio.But deep day by day along with the oilfield exploitation degree, the oil recovery stratum is more and more darker, and the use temperature of tensio-active agent is more and more higher, the water-mineralizing degree is also more and more higher.The surfactant system of the above successful Application in common oil reservoir (one, two class oil reservoirs), under the high salt of high temperature (formation temperature is greater than 80 ℃) (more than salinity 20000 mg/litre) condition (three class oil reservoirs), because chemical structure malleable, compound system poor stability produce serious chromatographic separation in oil displacement process, cause the oil displacement efficiency variation.In order to reduce oil/water termination tension force to a greater extent, often add the alkali of high density, as sodium hydroxide, yellow soda ash etc.Alkali can generate new tensio-active agent on the spot with the reaction of acidic substance in the crude oil, and adds tensio-active agent and plays synergistic effect.Document CN1439689A discloses a kind of ternary composite oil-displacing system and application thereof of alkali, mixed surfactant and polymer, and the alkali of wherein selecting for use is Na 2CO 3But in use, alkali not only brings huge injury to stratum and oil well etc., and equipment and corrosive pipeline are serious, spends substantial contribution in maintenance, maintenance; And, have to improve greatly the working concentration of polymkeric substance for reaching required viscosity because alkali can seriously reduce the viscosity and the visco-elasticity of polymkeric substance, the oil recovery comprehensive cost is improved.
Summary of the invention
One of technical problem to be solved by this invention is that the oil-displacing agent that contains tensio-active agent in the prior art exists under the high temperature and high salt condition oil displacement efficiency poor, simultaneously owing to contain alkali, injury is brought on stratum and oil well, etching apparatus and pipeline, the problem that production cost is high provides a kind of new alkyl phenol sulfonic polyoxyethylene ether sulfate.The surfactant composition that contains alkyl phenol sulfonic polyoxyethylene ether sulfate still can form 10 with crude oil under alkali-free, high temperature and high salt condition -3~10 -4Milli ox/rice ultra low interfacial tension improves the high temperature and high salt oil deposit recovery ratio.Two of technical problem to be solved by this invention provides the preparation method of alkyl phenol sulfonic polyoxyethylene ether sulfate.This method has the advantages that technology is simple, equipment requirements is low, be easy to produce.
For one of solving the problems of the technologies described above, the technical solution used in the present invention is as follows: a kind of alkyl phenol sulfonic polyoxyethylene ether sulfate, and its general molecular formula is:
Figure A20071003905200061
Wherein M is basic metal, ammonium or amido; R is C 1~C 22Alkyl; N is any one integer in 1~30.
In the technique scheme, the basic metal preferred version is sodium or potassium, and more preferably scheme is for being selected from sodium; The R preferred version is for being selected from C 4~C 15Alkyl, more preferably scheme is for being selected from C 8~C 12Alkyl; The n preferred version is any one integer in 4~20, and more preferably scheme is any one integer in 5~10.
For solve the problems of the technologies described above two, the technical solution used in the present invention is as follows: a kind of preparation method of alkyl phenol sulfonic polyoxyethylene ether sulfate may further comprise the steps:
A) alkylphenol and oxyethane are 85~160 ℃ in temperature of reaction, and pressure is under 0~0.40MPa gauge pressure condition, under catalyst action, react alkylphenol polyoxyethylene; The alkyl of wherein said alkylphenol is the alkyl that contains 1~22 carbon atom; The mol ratio of oxyethane and alkylphenol is 1~30: 1; Described catalyzer is the basic cpd of calcium, and consumption is 0.3~3% of an alkylphenol weight;
B) the step a) synthetic alkylphenol polyoxyethylene and the vitriol oil are under 40~60 ℃ of conditions in temperature of reaction, react to get alkyl phenol sulfonic polyoxyethylene ether in 0.5~10 hour; Wherein the mol ratio of the vitriol oil and alkylphenol polyoxyethylene is 2~5: 1;
C) step b) synthetic alkyl phenol sulfonic polyoxyethylene ether and chlorsulfonic acid are under 20~60 ℃ of conditions in temperature of reaction, reacted 0.5~5 hour, the basic cpd that adds alkali metal containing, ammonium or amido at last, be neutralized to neutrality, get alkyl phenol sulfonic polyoxyethylene ether sulfate, wherein the mol ratio of alkyl phenol sulfonic polyoxyethylene ether and chlorsulfonic acid is 2~0.5: 1.
In the technique scheme, a) the temperature of reaction preferable range is 140~160 ℃ in the step, and the pressure preferable range is 0.20~0.40MPa gauge pressure; B) the temperature of reaction preferable range is 40~45 ℃ in the step, and the reaction times preferable range is 2.0~5 hours; C) the temperature of reaction preferable range is 20~50 ℃ in the step, and the reaction times preferable range is 2.0~5 hours; The alkyl preferred version of described alkylphenol be contain 4~15 carbon atoms alkyl more preferably scheme be the alkyl that contains 8~12 carbon atoms.The basic cpd preferred version of amino-contained is for being selected from monoethanolamine, diethanolamine or trolamine, and more preferably scheme is for being selected from trolamine.
Alkyl phenol sulfonic polyoxyethylene ether sulfate of the present invention can pass through the infrared analysis spectral characterization, and sweep limit is 4000~400cm -1In wave number is 3100~3000cm -1, 1609cm -1, 1512cm -1, 830cm -1The place is the absorption characteristic peak of phenyl ring, is 1120cm in wave number -1The place is the characteristic peak of C-O-C key, is 1350cm in wave number -1The place is the characteristic peak of polyethylene oxide, at wave number 2840~3000cm -1The place is the characteristic peak of chain alkyl, is 1251cm in wave number -1, 680cm -1The place is for sulfonic characteristic peak on the phenyl ring, at wave number 1251cm -1The place is-OSO 3The characteristic peak that the stretching vibration of S=O group produces among the M.
Alkyl phenol sulfonic polyoxyethylene ether sulfate of the present invention can be used in the surfactant composition of tertiary oil recovery.This surfactant composition comprises following component by weight percentage:
1) 0.01~5.0% alkyl phenol sulfonic polyoxyethylene ether sulfate;
2) 0.01~3.0% polymkeric substance;
3) water of surplus;
Wherein said polymkeric substance is at least a in polyacrylamide, modified polyacrylamide or the xanthan gum.
In the technique scheme, the water preferred version is that clear water or sewage are injected in the oil field; By weight percentage, the consumption preferable range of alkyl phenol sulfonic polyoxyethylene ether sulfate is 0.1~1.0%, and more preferably scope is 0.1~0.3%; The consumption preferable range of polymkeric substance is 0.05~0.5%; More preferably scope is 0.1~0.2%.
The surfactant composition that alkyl phenol sulfonic polyoxyethylene ether sulfate of the present invention is used for tertiary oil recovery has the following advantages:
(1) can alkali-free in the composition.The surfactant composition that contains alkyl phenol sulfonic polyoxyethylene ether sulfate still can form 10 with underground crude oil under the alkali-free condition -3~10 -4The ultra low interfacial tension of milli ox/rice has not only overcome when using at the scene high concentration alkali to the huge injury of stratum and oil well, and has met environmental protection requirement, and equipment is not had injury, can reach the oil displacement efficiency of the best;
(2) heatproof, salt tolerant.The surfactant composition that contains alkyl phenol sulfonic polyoxyethylene ether sulfate in formation temperature greater than 80 ℃, salinity greater than 20000 mg/litre, Ca 2+, Mg 2+Concentration is still can form 10 with underground crude oil under the condition of 0~1000 mg/litre -3~10 -4The ultra low interfacial tension of milli ox/rice improves oil recovery factor 17.3%, has obtained better technical effect.
The present invention is further elaborated below by embodiment.
Figure of description
Fig. 1 is the infrared analysis spectrum of alkyl phenol sulfonic polyoxyethylene ether sulfate.
Wherein, wave number 3100~3000cm -1, 1609cm -1, 1512cm -1, 830cm -1The place is the absorption characteristic peak of phenyl ring, wave number 1120cm -1The place is the characteristic peak of C-O-C key, wave number 1350cm -1The place is the characteristic peak of polyethylene oxide, wave number 2840~3000cm -1The place is the characteristic peak of chain alkyl, wave number 1251cm -1, 680cm -1The place is sulfonic characteristic peak on the phenyl ring, wave number 1251cm -1The place is-OSO 3The characteristic peak that the stretching vibration of S=O group produces among the M.
Embodiment
[embodiment 1]
Synthesizing of nonyl phenol sulfonic polyethenoxy (5) ether sodium sulfovinate
(1) in the reactor that condensing works, whipping appts and gas distributor are housed, adds 110 gram nonyl phenols and 1.5 calcium oxide catalysts that restrain, when logical nitrogen limit, limit is heated to 135 ℃, add the water of nonyl phenol weight 10%, stirring reaction 1 hour.First then normal pressure steams water, the back decompression is under 20 mmhg vacuum, vacuumize steaming in 20 minutes in 140 ℃ and remove moisture, this solution is cooled to 80 ℃, slowly drips the vitriol oil of catalyst neutralisation theoretical acid amount 20 (weight) %, system temperature is heated to 85~90 ℃, open vacuum system, dehydration is 1 hour under high vacuum,, then the system temperature of reaction is transferred to 150 ℃ and slowly feeds 112 and restrain oxyethane and carry out alkoxylation with the air in the system of removing with nitrogen purging 3~4 times; After reaction finishes, use the nitrogen purging system, removes unreacted oxyethane, cool off post neutralization, decolouring, filtration, dewater Nonyl pheno (5) ether.
(2) step (1) institute's synthetic nonyl phenol phenol polyethenoxy (5) ether 220 grams are placed the reactor that reflux condensate device, thermometer, agitator are housed, be warming up to 45 ℃, stir the vitriol oil that slowly drips 100 grams 98% down, 1.5 add in hour, insulation reaction finished reaction in 2 hours again, got brown viscous liquid through aftertreatment and was nonyl phenol sulfonic polyethenoxy (5) ether.
(3) with step (2) institute's synthetic nonyl phenol sulfonic polyethenoxy (5) ether 270 grams (0.5 mole), place reactor, dropwise add 65 gram chlorsulfonic acids under micro-vacuum (0.02MPa), violent stirring, the dropping time was controlled at 1.5~2 hours, 20~30 ℃ of control reaction temperature; Be warming up to 40~50 ℃ after chlorsulfonic acid adds and continue to react 2~3 hours, add aqueous sodium hydroxide solution after reaction finishes and be neutralized to neutrality, get nonyl phenol sulfonic polyethenoxy (5) ether sodium sulfovinate.
To synthetic nonyl phenol sulfonic polyethenoxy (5) ether sodium sulfovinate, use U.S. Nicolet-5700 infrared spectrometer, adopt liquid-film method to carry out Infrared spectroscopy (sweep limit 4000~400cm -1), have characteristic peak shown in Figure 1.
[embodiment 2]
Synthesizing of 4-dodecylphenol sulfonic polyethenoxy (10) ether sodium sulfovinate
(1) in the reactor that condensing works, whipping appts and gas distributor are housed, adds 131 gram 4-dodecylphenols and 1.8 calcium oxide catalysts that restrain, when logical nitrogen limit, limit is heated to 135 ℃, add the water of 4-dodecylphenol weight 10%, stirring reaction 1 hour.First then normal pressure steams water, the back decompression is under 20 mmhg vacuum, vacuumize steaming in 20 minutes in 140 ℃ and remove moisture, this solution is cooled to 80 ℃, slowly drips the vitriol oil of catalyst neutralisation theoretical acid amount 20 (weight) %, system temperature is heated to 85~90 ℃, open vacuum system, dehydration is 1 hour under high vacuum,, then the system temperature of reaction is transferred to 150 ℃ and slowly feeds 222 and restrain oxyethane and carry out alkoxylation with the air in the system of removing with nitrogen purging 3~4 times; After reaction finishes, use the nitrogen purging system, removes unreacted oxyethane, cool off post neutralization, decolouring, filtration, dewater dodecyl phenol polyethenoxy (10) ether.
(2) step (1) institute's synthetic dodecyl phenol polyethenoxy (10) ether 350 grams are placed the reactor that reflux condensate device, thermometer, agitator are housed, be warming up to 45 ℃, stir the vitriol oil that slowly drips 150 grams 98% down, 1.5 add in hour, insulation reaction finished reaction in 2 hours again, got brown viscous liquid through aftertreatment and was 4-dodecylphenol sulfonic polyethenoxy (10) ether.
(3) with 0.5 mole in step (2) institute's synthetic 4-dodecylphenol sulfonic polyethenoxy (10) ether, place reactor, dropwise add 65 gram chlorsulfonic acids under micro-vacuum (0.02MPa), violent stirring, the dropping time was controlled at 1.5~2 hours, 20~30 ℃ of control reaction temperature; Be warming up to 40~50 ℃ after chlorsulfonic acid adds and continue to react 2~3 hours, add aqueous sodium hydroxide solution after reaction finishes and be neutralized to neutrality, get 4-dodecylphenol sulfonic polyethenoxy (10) ether sodium sulfovinate.
To synthetic 4-dodecylphenol sulfonic polyethenoxy (10) ether sodium sulfovinate, use U.S. Nicolet-5700 infrared spectrometer, adopt liquid-film method to carry out Infrared spectroscopy (sweep limit 4000~400cm -1), have characteristic peak shown in Figure 1.
[embodiment 3]
Synthesizing of octyl phenol sulfonic polyethenoxy (10) ether sulfuric acid triethanolamine salt
(1) in the reactor that condensing works, whipping appts and gas distributor are housed, adds 98 gram octyl phenols and 1.2 calcium oxide catalysts that restrain, when logical nitrogen limit, limit is heated to 135 ℃, add the water of octyl phenol weight 10%, stirring reaction 1 hour.First then normal pressure steams water, the back decompression is under 20 mmhg vacuum, vacuumize steaming in 20 minutes in 140 ℃ and remove moisture, this solution is cooled to 80 ℃, slowly drips the vitriol oil of catalyst neutralisation theoretical acid amount 20 (weight) %, system temperature is heated to 85~90 ℃, open vacuum system, dehydration is 1 hour under high vacuum,, then the system temperature of reaction is transferred to 150 ℃ and slowly feeds 223 and restrain oxyethane and carry out alkoxylation with the air in the system of removing with nitrogen purging 3~4 times; After reaction finishes, use the nitrogen purging system, removes unreacted oxyethane, cool off post neutralization, decolouring, filtration, dewater octyl phenol polyoxy ethene (10) ether.
(2) step (1) institute's synthetic octyl phenol phenol polyethenoxy (10) ether 320 grams are placed the reactor that reflux condensate device, thermometer, agitator are housed, be warming up to 45 ℃, stir the vitriol oil that slowly drips 150 grams 98% down, 1.5 add in hour, insulation reaction finished reaction in 2 hours again, got brown viscous liquid through aftertreatment and was octyl phenol sulfonic polyethenoxy (10) ether.
(3) with step (2) institute's synthetic octyl phenol sulfonic polyethenoxy (10) ether 370 grams (0.5 mole), place reactor, dropwise add 65 gram chlorsulfonic acids under micro-vacuum (0.02MPa), violent stirring, the dropping time was controlled at 1.5~2 hours, 20~30 ℃ of control reaction temperature; Be warming up to 40~50 ℃ of continuation after chlorsulfonic acid adds and reacted 2~3 hours, the trolamine aqueous solution that reaction finishes back adding 30% is neutralized to neutrality, gets octyl phenol sulfonic polyethenoxy (10) ether sulfuric acid triethanolamine salt.
To synthetic octyl phenol sulfonic polyethenoxy (10) ether sulfuric acid triethanolamine salt, use U.S. Nicolet-5700 infrared spectrometer, adopt liquid-film method to carry out Infrared spectroscopy (sweep limit 4000~400cm -1), have characteristic peak shown in Figure 1.
[embodiment 4]
Get [embodiment 1] synthetic nonyl phenol sulfonic polyethenoxy (5) ether sodium sulfovinate X (weight) %, polyacrylamide 0.15 (weight) %, Shengli Oil Field win the Tuo Er district and win seven wells injection water, stir 30 minutes, obtain a kind of surfactant composition.Shengli Oil Field wins Tuo Er district victory seven well injection water quality analytical resultss and sees Table 1.In the time of 90.2 ℃, this surfactant composition and Shengli Oil Field win the ultra low interfacial tension that forms between the Tuo Er district 0-141 well dewatered oil and see Table 2.Interfacial tension is dripped the interfacial tensimeter measurement with the 500 types rotation that Texas ,Usa university produces.
Table 1
Project Cl - SO 4 2- HCO 3 - Na ++K + Ca 2+ Mg 2= Water-mineralizing degree TDS The water type
Mg/litre 10150 0 516 6231 322 93 27312 CaCl 2
Table 2
X (weight) % 0.05 0.1 0.2 0.3
Interfacial tension (milli ox/rice) 0.0091 0.0072 0.0056 0.0043
[embodiment 5]
Get [embodiment 2] synthetic 4-dodecylphenol sulfonic polyethenoxies (10) ether sodium sulfovinate X (weight) %, polyacrylamide 0.15 (weight) %, Shengli Oil Field win Tuo Er district sewage, stir 30 minutes, obtain a kind of surfactant composition.Shengli Oil Field wins Tuo Er district 0-141 well output water Analysis Results of Water Quality and sees Table 3.In the time of 90.2 ℃, this surfactant composition and Shengli Oil Field win the ultra low interfacial tension that forms between the Tuo Er district 0-141 well dewatered oil and see Table 4.Interfacial tension is dripped the interfacial tensimeter measurement with the 500 types rotation that Texas ,Usa university produces.
Table 3
Project Cl - SO 4 2- HCO 3 - Na ++K + Ca 2+ Mg 2= Water-mineralizing degree TDS The water type
Mg/litre 13535 0 761 8252 499 126 23175 CaCl 2
Table 4
X (weight) % 0.05 0.1 0.2 0.3
Interfacial tension (milli ox/rice) 0.0085 0.0078 0.0075 0.0068
[embodiment 6]
Get [embodiment 3] synthetic octyl phenol sulfonic polyethenoxies (10) ether sulfuric acid triethanolamine salt X (weight) %, polyacrylamide 0.15 (weight) %, total mineralization is 30000 mg/litre, Ca 2+, Mg 2+Concentration is the preparation water of 1000 mg/litre, stirs 30 minutes, obtains a kind of surfactant composition.In the time of 90.2 ℃, this surfactant composition and Shengli Oil Field win the ultra low interfacial tension that forms between the Tuo Er district 0-141 well dewatered oil and see Table 5.Interfacial tension is dripped the interfacial tensimeter measurement with the 500 types rotation that Texas ,Usa university produces.
Table 5
X (weight) % 0.05 0.1 0.2 0.3
Interfacial tension (milli ox/rice) 0.0095 0.0058 0.0045 0.00092
[embodiment 7~9]
In length is 30 centimetres, and diameter is 2.5 centimetres, and rate of permeation is 1.5 microns 2Rock core on carry out oil displacement test.Earlier win Tuo Er district local water with Shengli Oil Field and be driven to moisturely 92%, behind the surfactant composition of metaideophone 0.3pv (rock pore volume) [embodiment 4~6], water drive is extremely moisture 100%, can improve oil recovery factor 17.3%.

Claims (9)

1. alkyl phenol sulfonic polyoxyethylene ether sulfate, its general molecular formula is:
Figure A2007100390520002C1
Wherein M is basic metal, ammonium or amido; R is C 1~C 22Alkyl; N is any one integer in 1~30.
2. according to the described alkyl phenol sulfonic polyoxyethylene ether sulfate of claim 1, it is characterized in that described basic metal is sodium or potassium; R is C 4~C 15Alkyl; N is any one integer in 4~20.
3. according to the described alkyl phenol sulfonic polyoxyethylene ether sulfate of claim 2, it is characterized in that described basic metal is sodium; R is C 8~C 12Alkyl; N is any one integer in 5~10.
4. the preparation method of the described alkyl phenol sulfonic polyoxyethylene ether sulfate of claim 1 may further comprise the steps:
A) alkylphenol and oxyethane are 85~160 ℃ in temperature of reaction, and pressure is under 0~0.40MPa gauge pressure condition, under catalyst action, react alkylphenol polyoxyethylene; The alkyl of wherein said alkylphenol is the alkyl that contains 1~22 carbon atom; The mol ratio of oxyethane and alkylphenol is 1~30: 1; Described catalyzer is the basic cpd of calcium, and consumption is 0.3~3% of an alkylphenol weight;
B) the step a) synthetic alkylphenol polyoxyethylene and the vitriol oil are under 40~60 ℃ of conditions in temperature of reaction, react to get alkyl phenol sulfonic polyoxyethylene ether in 0.5~10 hour; Wherein the mol ratio of the vitriol oil and alkylphenol polyoxyethylene is 2~5: 1;
C) step b) synthetic alkyl phenol sulfonic polyoxyethylene ether and chlorsulfonic acid are under 20~60 ℃ of conditions in temperature of reaction, reacted 0.5~5 hour, the basic cpd that adds alkali metal containing, ammonium or amido at last, be neutralized to neutrality, get alkyl phenol sulfonic polyoxyethylene ether sulfate, wherein the mol ratio of alkyl phenol sulfonic polyoxyethylene ether and chlorsulfonic acid is 2~0.5: 1.
5. the preparation method of alkyl phenol sulfonic polyoxyethylene ether sulfate according to claim 4 is characterized in that a) temperature of reaction is 140~160 ℃ in the step, and pressure is 0.20~0.40MPa gauge pressure.
6. the preparation method of alkyl phenol sulfonic polyoxyethylene ether sulfate according to claim 4 is characterized in that b) temperature of reaction is 40~45 ℃ in the step, the reaction times is 2.0~5 hours.
7. the preparation method of alkyl phenol sulfonic polyoxyethylene ether sulfate according to claim 4 is characterized in that c) temperature of reaction is 20~50 ℃ in the step, the reaction times is 2.0~5 hours.
8. the preparation method of alkyl phenol sulfonic polyoxyethylene ether sulfate according to claim 4, the alkyl that it is characterized in that described alkylphenol is the alkyl that contains 4~15 carbon atoms.
9. the preparation method of alkyl phenol sulfonic polyoxyethylene ether sulfate according to claim 8, the alkyl that it is characterized in that described alkylphenol is the alkyl that contains 8~12 carbon atoms.
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