CN102604670A - Method for preparing raw material of oil sulfonate for displacing oil in oilfield - Google Patents
Method for preparing raw material of oil sulfonate for displacing oil in oilfield Download PDFInfo
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- CN102604670A CN102604670A CN2012100342279A CN201210034227A CN102604670A CN 102604670 A CN102604670 A CN 102604670A CN 2012100342279 A CN2012100342279 A CN 2012100342279A CN 201210034227 A CN201210034227 A CN 201210034227A CN 102604670 A CN102604670 A CN 102604670A
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- furfural
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- sulfonate
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Abstract
The invention relates to a method for preparing the raw material of oil sulfonate, in particular to a method for preparing the raw material of oil sulfonate for displacing oil in the oilfield, which can ensure that the sulfonation reaction process is easy to control, the conversion rate is high, the generation amount of the acid residue is low, and the quality stability of the oil sulfonate product is improved. The distillate of oil is used as a raw material to extract furfural, wherein the distillate is the distillate of 260-520 DEGC of the crude oil or the distillate at a certain section of the crude oil; the raw oil and the furfural are fed into a primary extraction tower together, the remaining of an extract is fed into a secondary extraction tower directly from the top thereof, and the furfural is fed into the secondary extraction tower from the bottom thereof; and the extract which is obtained on the lower part of the secondary extraction tower is evaporated to remove the furfural so as to obtain the extract oil which is the raw material for producing the oil sulfonate. According to the technology of the invention, the raw oil retains the main components used for producing the oil sulfonate in the raw material, the oil sulfonate has higher interface performance and can be produced by adopting the gas-phase film type sulfonation method, the conversion rate of the raw material is improved, the by-products of reaction reduction are few, and the stability of the product is strong.
Description
Technical field
The present invention relates to a kind of preparation method of sulfonated petro-leum raw material, the displacement of reservoir oil of especially a kind of oil field is with the preparation method of sulfonated petro-leum raw material.
Background technology
Along with carrying out in a deep going way of tertiary oil production in oil field, the research of oil-displacing agent is more and more received people's attention.Because the sulfonated petro-leum raw material is wide, price is low, and good with the crude oil compatibleness, interfacial activity is strong, sulfonated petro-leum has become a kind of important oil field oil-displacing agent product.The method that with the fraction oil of petroleum is the feedstock production sulfonated petro-leum has had more report.The method of CN102190605A 150～550 ℃ of fraction oil of petroleum of sulfonation under-10～-20 ℃ of conditions; CN101955451A is through adding solvent carries out membrane-type sulfonation to 350～500 ℃ of fraction oil of petroleum method in raw oil; CN1472199A 2～8 sulfonation reaction jars of connecting; Utilize 150～580 ℃ of raw oils to prepare the sulfonated petro-leum method continuously, 200～550 ℃ of fraction oil of petroleum methods of CN101318112A sulfonation, but these methods all are directly to use crude oil fractions oil to be raw material; Sulfonation process coking occurs easily, oversulfonate manifests, and low, the poor stability of sulfonated product actives.CN102190604A adopt paraffinic base, intermediate base, naphthenic base or aromatic base second line of distillation, subtract three-way, subtract four line petroleum fractionss, after hydrotreatment, obtain sulfonated product.But, raw oil is carried out hydrotreatment, equipment drops into height, process control procedure is complicated.The CN101811999A column chromatography carries out the petroleum fractions oil treatment, prepares the method for different fractions oil family component, adopts column chromatography to handle fraction oil of petroleum, not only need a large amount of eluting solvents, and treatment capacity is little, is difficult to accomplish scale production.
Summary of the invention
The object of the invention just provides and a kind ofly makes that the sulfonation reaction process is easy to control, transformation efficiency is high, the acid sludge growing amount is few, has improved the preparation method of the oil field displacement of reservoir oil of sulfonated petro-leum product quality stability with the sulfonated petro-leum raw material.Technical scheme is to be that to carry out furfural extracting distillate be 260～520 ℃ of distillates of crude oil or wherein a certain section distillate to raw material with the fraction oil of petroleum.At first raw oil and furfural get into the single extraction tower, and the single extraction condition is: the mass ratio of furfural and distillate is 1: 1～1: 3; 50～80 ℃ of tower top temperatures, 30～50 ℃ of column bottom temperatures.The raffinate that tower top is obtained directly gets into the secondary extraction tower after collecting, and raffinate gets into from cat head, and furfural gets at the bottom of tower, and the extracting condition is: the mass ratio of raffinate and furfural is 1: 1.8～1: 4.8; 90～120 ℃ of tower top temperatures, 50～80 ℃ of column bottom temperatures.The Extract that secondary extraction tower bottom obtains, evaporation is removed after the furfural, and the extraction oil that obtains is the sulfonated petro-leum raw materials for production.Adopt the raw oil of the present invention's technology to keep the main ingredient that is beneficial to sulfonated petro-leum production in the raw material; Handle the sulfonated petro-leum interface performance raising that the back produces; Can adopt gas phase membrane-type sulfonation mode, also can adopt still formula liquid phase sulfonation mode to produce sulfonated petro-leum, feed stock conversion improves, side reaction product reduces, the product stabilizing power is strong.
Embodiment
Embodiment 1
Be that to carry out furfural extracting distillate be 260～520 ℃ of distillates of crude oil or wherein a certain section distillate to raw material with the fraction oil of petroleum.At first raw oil and furfural get into the single extraction tower, and the single extraction condition is: the mass ratio of furfural and distillate is 1: 1～1: 3; 50～80 ℃ of tower top temperatures, 30～50 ℃ of column bottom temperatures.The raffinate that tower top is obtained directly gets into the secondary extraction tower after collecting, and raffinate gets into from cat head, and furfural gets at the bottom of tower, and the extracting condition is: the mass ratio of raffinate and furfural is 1: 1.8～1: 4.8; 90～120 ℃ of tower top temperatures, 50～80 ℃ of column bottom temperatures.The Extract that secondary extraction tower bottom obtains, evaporation is removed after the furfural, and the extraction oil that obtains is the sulfonated petro-leum raw materials for production.
Embodiment 2
320～530 ℃ of distillates of refinery, aromaticity content 42.6%, gum asphaltic content 12.4%, carrying out the single extraction condition is 45 ℃ of column bottom temperatures, 70 ℃ of tower top temperatures, furfural and distillate mass ratio 1: 2.Raffinate gets into the secondary extraction tower, 60 ℃ of column bottom temperatures, and 110 ℃ of tower top temperatures, raffinate and furfural mass ratio 1: 2.8 after obtaining Extract and steaming furfural, obtain secondary and extract out oilyly, analyze wherein aromaticity content 68.9%, gum asphaltic content 3.3%.Get the 300g distillate and add in the sulfonation reaction still, add 200 ethylene dichloride again, stir; Temperature drips sulfan 95g after below 20 ℃, keeps reactor temperature to be lower than 20 ℃ in the dropping process; Dropwise continued and stir 30min, be neutralized to pH value 7～9 with 25% ammoniacal liquor at 50～70 ℃ then, 30min is left standstill in 70 ℃ of insulations; Deviate from lower layer of water, the sulfonated petro-leum that obtains is deviate from solvent under 80 ℃ of conditions, obtain the mahogany acid product salt.Under similarity condition, the raw oil after handling is carried out sulfonation, make the mahogany acid product salt.
| Raw material | The product active matter content, % | Single sulfonic acid content, % | Win two regional boundary surface tensions |
| Raw oil is untreated | 41.2 | 72 | 4.2×10 -3mN/m |
| Raw materials treated oil | 67.5 | 93 | 1.5×10 -3mN/m |
Embodiment 3
260～450 ℃ of distillates of refinery, aromaticity content 43.1%, gum asphaltic content 11.3%, carrying out the single extraction condition is 35 ℃ of column bottom temperatures, 60 ℃ of tower top temperatures, furfural and distillate mass ratio 1: 2.Raffinate gets into the secondary extraction tower, 60 ℃ of column bottom temperatures, and 100 ℃ of tower top temperatures, raffinate and furfural mass ratio 1: 3 after obtaining Extract and steaming furfural, obtain secondary and extract out oilyly, analyze wherein aromaticity content 72.3%, gum asphaltic content 2.7%.Get the 300g distillate and add in the sulfonation reaction still, add 200 ethylene dichloride again, stir; Temperature drips sulfan 95g after below 20 ℃, keeps reactor temperature to be lower than 20 ℃ in the dropping process; Dropwise continued and stir 30min, be neutralized to pH value 7～9 with 25% ammoniacal liquor at 50～70 ℃ then, 30min is left standstill in 70 ℃ of insulations; Deviate from lower layer of water, the sulfonated petro-leum that obtains is deviate from solvent under 80 ℃ of conditions, obtain the mahogany acid product salt.Under similarity condition, the raw oil after handling is carried out sulfonation, make the mahogany acid product salt.
| Raw material | The product active matter content, % | Single sulfonic acid content, % | Win two regional boundary surface tensions |
| Raw oil is untreated | 43.2 | 73 | 3.7×10 -2mN/m |
| Raw materials treated oil | 74.5 | 97 | 2.6×10 -3mN/m |
Embodiment 4
Refinery subtracts 410～500 ℃ of distillates of four lines, aromaticity content 31.2%, and gum asphaltic content 8.3%, carrying out the single extraction condition is 40 ℃ of column bottom temperatures, 70 ℃ of tower top temperatures, furfural and distillate mass ratio 1: 3.Raffinate gets into the secondary extraction tower, 70 ℃ of column bottom temperatures, and 110 ℃ of tower top temperatures, raffinate and furfural mass ratio 1: 2.8 after obtaining Extract and steaming furfural, obtain secondary and extract out oilyly, analyze wherein aromaticity content 67.1%, gum asphaltic content 1.6%.Get the 300g distillate and add in the sulfonation reaction still, add 200 ethylene dichloride again, stir; Temperature drips sulfan 95g after below 20 ℃, keeps reactor temperature to be lower than 20 ℃ in the dropping process; Dropwise continued and stir 30min, be neutralized to pH value 7～9 with 25% ammoniacal liquor at 50～70 ℃ then, 30min is left standstill in 70 ℃ of insulations; Deviate from lower layer of water, the sulfonated petro-leum that obtains is deviate from solvent under 80 ℃ of conditions, obtain the mahogany acid product salt.Under similarity condition, the raw oil after handling is carried out sulfonation, make the mahogany acid product salt.
| Raw material | The product active matter content, % | Single sulfonic acid content, % | Win two regional boundary surface tensions |
| Raw oil is untreated | 38.3 | 68 | 5.3×10 -2mN/m |
| Raw materials treated oil | 70.1 | 95 | 4.7×10 -2mN/m |
Embodiment 5
Refinery subtracts three-way 330～450 ℃ of distillates, aromaticity content 45.3%, and gum asphaltic content 10.6%, carrying out the single extraction condition is 40 ℃ of column bottom temperatures, 70 ℃ of tower top temperatures, furfural and distillate mass ratio 1: 2.Raffinate gets into the secondary extraction tower, 70 ℃ of column bottom temperatures, and 110 ℃ of tower top temperatures, raffinate and furfural mass ratio 1: 2.6 after obtaining Extract and steaming furfural, obtain secondary and extract out oilyly, analyze wherein aromaticity content 70.7%, gum asphaltic content 2.8%.Get the 300g distillate and add in the sulfonation reaction still, add 200 ethylene dichloride again, stir; Temperature drips sulfan 95g after below 20 ℃, keeps reactor temperature to be lower than 20 ℃ in the dropping process; Dropwise continued and stir 30min, be neutralized to pH value 7～9 with 25% ammoniacal liquor at 50～70 ℃ then, 30min is left standstill in 70 ℃ of insulations; Deviate from lower layer of water, the sulfonated petro-leum that obtains is deviate from solvent under 80 ℃ of conditions, obtain the mahogany acid product salt.Under similarity condition, the raw oil after handling is carried out sulfonation, make the mahogany acid product salt.
| Raw material | The product active matter content, % | Single sulfonic acid content, % | Win two regional boundary surface tensions |
| Raw oil is untreated | 47.4 | 77 | 8.6×10 -3mN/m |
| Raw materials treated oil | 78.2 | 98 | 5.9×10 -3mN/m |
Claims (1)
1. the oil field displacement of reservoir oil is with the preparation method of sulfonated petro-leum raw material; It is characterized in that: be that raw material carries out the furfural extracting with the fraction oil of petroleum; Distillate is 260～520 ℃ of distillates of crude oil or wherein a certain section distillate; At first raw oil and furfural get into the single extraction tower, and the single extraction condition is: the mass ratio of furfural and distillate is 1: 1～1: 3; 50～80 ℃ of tower top temperatures, 30～50 ℃ of column bottom temperatures; The raffinate that tower top is obtained directly gets into the secondary extraction tower after collecting, and raffinate gets into from cat head, and furfural gets at the bottom of tower, and the extracting condition is: the mass ratio of raffinate and furfural is 1: 1.8～1: 4.8; 90～120 ℃ of tower top temperatures, 50～80 ℃ of column bottom temperatures; The Extract that secondary extraction tower bottom obtains, evaporation is removed after the furfural, and the extraction oil that obtains is the sulfonated petro-leum raw materials for production.
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| CN2012100342279A CN102604670A (en) | 2012-02-10 | 2012-02-10 | Method for preparing raw material of oil sulfonate for displacing oil in oilfield |
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| CN2012100342279A CN102604670A (en) | 2012-02-10 | 2012-02-10 | Method for preparing raw material of oil sulfonate for displacing oil in oilfield |
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Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS5513271B2 (en) * | 1975-03-18 | 1980-04-08 | ||
| CN1084099A (en) * | 1993-07-12 | 1994-03-23 | 安徽新源石油化工技术开发有限公司 | Short-side-chain condensed-ring aromatic hydrocarbon mixed sulfonate surfactant taking heavy aromatic hydrocarbon of solvent extract of catalytic cracking cycle oil as raw material |
| CN1468849A (en) * | 2002-07-15 | 2004-01-21 | �����ι�˾ | Prepn of faintly alkaline alkylbenzene sulfonate |
| CN101597513A (en) * | 2009-07-14 | 2009-12-09 | 中国海洋石油总公司 | A kind of environment-friendly rubber oil and preparation method thereof |
| 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 |
-
2012
- 2012-02-10 CN CN2012100342279A patent/CN102604670A/en active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS5513271B2 (en) * | 1975-03-18 | 1980-04-08 | ||
| CN1084099A (en) * | 1993-07-12 | 1994-03-23 | 安徽新源石油化工技术开发有限公司 | Short-side-chain condensed-ring aromatic hydrocarbon mixed sulfonate surfactant taking heavy aromatic hydrocarbon of solvent extract of catalytic cracking cycle oil as raw material |
| CN1468849A (en) * | 2002-07-15 | 2004-01-21 | �����ι�˾ | Prepn of faintly alkaline alkylbenzene sulfonate |
| CN101597513A (en) * | 2009-07-14 | 2009-12-09 | 中国海洋石油总公司 | A kind of environment-friendly rubber oil and preparation method thereof |
| 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 |
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Application publication date: 20120725 |