CN105037223A - Continuous extraction separation method of unsulfonated oil in petroleum sulfonate - Google Patents
Continuous extraction separation method of unsulfonated oil in petroleum sulfonate Download PDFInfo
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- CN105037223A CN105037223A CN201510392233.5A CN201510392233A CN105037223A CN 105037223 A CN105037223 A CN 105037223A CN 201510392233 A CN201510392233 A CN 201510392233A CN 105037223 A CN105037223 A CN 105037223A
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- petroleum sulfonate
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Abstract
The invention relates to a separation method of unsulfonated oil in petroleum sulfonate, and concretely relates to a continuous extraction separation method of unsulfonated oil in petroleum sulfonate. The continuous extraction separation method of unsulfonated oil in petroleum sulfonate, used for realizing unchanged interface tension of the petroleum sulfonate obtained after extraction separation, is provided to overcome the defect of interface tension rising of the petroleum sulfonate obtained after extraction separation. The method comprises the following steps: pumping petroleum sulfonate and water into a first-stage mixing and clarifying extractor according to a mass ratio of 1:0.5-1:2, clarifying, separating primary unsulfonated oil and an aqueous soltuion of primary petroleum sulfonate, pumping the aqueous soltuion of primary petroleum sulfonate into a second-stage mixing and clarifying extractor, separating secondary unsulfonated oil and an aqueous soltuion of secondary petroleum sulfonate, and dehydrating the aqueous soltuion of secondary petroleum sulfonate to form a final product. The method has the advantages of simplicity, low cost, and effective separation of highly-equivalent oil-soluble petroleum sulfonate, the interface tension of the finally obtained petroleum sulfonate is unchanged, the oil displacement effect of the petroleum sulfonate does not decrease, and the separated unsulfonated oil can be reused.
Description
Technical field
The present invention relates to unsulfonated oil isolation technique in sulfonated petro-leum, belong to technical field of oilfield chemistry.
Background technology
The sulfonated petro-leum of the displacement of reservoir oil is utilize specific fraction oil of petroleum to be that main raw material neutralizes the product obtained through oversulfonate in the industrial production.A large amount of unsulfonated oils is all contained, if unsulfonated oil content in grand celebration sulfonated petro-leum is more than 40% in the assessment of petroleum sulfonate for oil displacement product of current each explained hereafter.The existence of a large amount of unsulfonated oil not only affects the performance of mahogany acid product salt, also can cause the waste of resource, can not meet the needs of the stable displacement of reservoir oil and the use standard in oil field.
At present for unsulfonated oil separating in sulfonated petro-leum, also have research both at home and abroad, the main extraction process that adopts is separated unsulfonated oil, but does not all form continuous print technique, and in the selection of extraction agent, do not consider that point oily rate is on the impact of Oil Displacing Capacity.Patent US4144266 in and before adopt single extracting and separating unsulfonated oil, need to leave standstill through long-time (several weeks), then separated from mahogany acid product salt by some residual oil, this method divides oily rate low, needs the time longer.Patent US4269789 adopts combination extraction agent Skellysolve A, isopropyl alcohol and water, Skellysolve A: Virahol: water ratio is 4:4:1 ~ 0.5:1:1, water 0.25 ~ 2ml/g charging.Point oily rate of the method extracting and separating unsulfonated oil is high, extraction agent can reclaim and recycle, but the experimental data that after not relating to extraction, whether the performance of sulfonated petro-leum remains unchanged, and found through experiments the sulfonated petro-leum after adopting the method extracting and separating, its interfacial tension raises.Draw by analysis, the oil-soluble sulfonic acid salt of some high equivalent weights is there is in sulfonate due to separation, itself and unsulfonated oil character are close, when being separated unsulfonated oil, this part sulfonate can remove along with unsulfonated oil simultaneously, effective table being content of sulfonated petro-leum is caused to reduce, interfacial tension raises, and when being applied to the displacement of reservoir oil, oil displacement efficiency is declined.Method is not also had to consider the separation of high equivalent weight oil-soluble sulfonic acid salt specially when extracting and separating at present.
Summary of the invention
The object of the invention is the deficiency existed for prior art, provide one effectively can retain high equivalent weight oil-soluble sulfonic acid salt, unsulfonated oil continuous extraction separation method in the sulfonated petro-leum making sulfonated petro-leum interfacial tension after score oil constant.
The invention provides unsulfonated oil continuous extraction separation method in a kind of sulfonated petro-leum, sulfonated petro-leum and water are pumped into first step mixer-settler extractor by the mass ratio of 1:0.5 ~ 1:2, carry out clarified separation, isolate a unsulfonated oil and a mahogany acid salt brine solution, a mahogany acid salt brine solution is pumped into second stage mixer-settler extractor again, isolate secondary unsulfonated oil and secondary mahogany acid salt brine solution, after described secondary sulfonated petro-leum aqueous solution dehydration, obtain the mahogany acid salt brine solution needing concentration.
Described sulfonated petro-leum component is: volatile matter (water): 10 ~ 35w%, unsulfonated oil: 20 ~ 45w%, sulfonated petro-leum: 35 ~ 45w%.
Described first step mixer-settler extractor temperature is 70 ~ 80 DEG C, and agitator speed is 1000 ~ 3000r/min, settling time 1.5h.
The temperature of described second stage mixer-settler extractor is 90 ~ 95 DEG C, and agitator speed is 1000 ~ 3000r/min, settling time 1.67h.
The present invention has following beneficial effect:
This continuous extraction separation method is simple, and adopt water consumption substitution alcohol, cost significantly declines; Effectively can retain high equivalent weight oil-soluble sulfonic acid salt, make not containing high equivalent weight oil-soluble sulfonic acid salt in unsulfonated oil, the sulfonated petro-leum interfacial tension after separation is constant, and when being applied to the displacement of reservoir oil, oil displacement efficiency can not reduce simultaneously; Isolated unsulfonated oil can collect recycling.
Accompanying drawing explanation
Fig. 1 is continuous separation method schematic flow sheet of the present invention,
In figure, 1 is water, and 2 is sulfonated petro-leum, and 3 is a unsulfonated oil, and 4 is secondary unsulfonated oil, and 5 is mahogany acid salt brine solution, and E1, E2 are mixer-settler extractor;
Fig. 2 is the interfacial tension figure that existing single divides sulfonated petro-leum before and after oil;
Fig. 3 is the interfacial tension figure adopting the inventive method to divide sulfonated petro-leum before and after oil.
Embodiment
Below by the specific embodiment provided, the present invention will be further described, but not as a limitation of the invention.
As shown in Figure 1, for the schematic flow sheet of separation method of the present invention, sulfonated petro-leum 2 and water 1 add mixer-settler extractor E1 in proportion, a unsulfonated oil 3 and a mahogany acid salt brine solution is obtained after flash liberation, one time mahogany acid salt brine solution pumps in mixer-settler extractor E2 again, obtains secondary unsulfonated oil 4 and mahogany acid salt brine solution 5.
Embodiment 1:
Adopt Virahol to be the unsulfonated oil that extraction agent is separated in sulfonated products, Virahol: sulfonated petro-leum continuously feeding mass ratio is 1:1, sulfonated petro-leum forms: volatile matter, 31.45w%; Unsulfonated oil, 23.62w%; Sulfonated petro-leum, 37.11w%; Inorganic salt, 7.82w%.At 50 DEG C, carry out single-stage continuous extraction separation, a point oily rate is 62.38%.Adopt this unsulfonated oil of Infrared spectroscopy, at wave number 1175 and 1045cm
-1near have the absorption peak of obvious sulfonated petro-leum S=O, illustrate that the unsulfonated oil that this method is separated carries more effective surface promoting agent when a point oily rate is 62.38%, thus cause sulfonated petro-leum product performance to be deteriorated.
Embodiment 2:
Employing combination extraction agent Skellysolve A, Virahol are separated the unsulfonated oil in sulfonated products with water, Skellysolve A: Virahol: water: sulfonated petro-leum charge-mass ratio 1:1.4:0.6:2, and sulfonated petro-leum forms: volatile matter, 11.73w%; Unsulfonated oil, 43.30w%; Sulfonated petro-leum, 40.30w%; Inorganic salt, 4.67w%.Carry out single-stage continuous extraction separation under room temperature, a point oily rate is 82.07%.The interface performance of sulfonated petro-leum before and after point oil is evaluated, as shown in Figure 2, the interfacial tension of sulfonated petro-leum obviously raises, and illustrate that being separated unsulfonated oil with this understanding makes the effective table being content being separated rear sulfonated petro-leum reduce, its oil displacement efficiency is deteriorated.Determination of Trace Sulfur content analysis is carried out to being separated the unsulfonated oil obtained, sulphur content in unsulfonated oil when dividing oily rate to be 82.07% is the sulfur content in crude oil of 0.179%(synthesis is 0.1126%), and adopt Infrared spectroscopy unsulfonated oil, at wave number 1175 and 1045cm
-1near have the absorption peak of obvious sulfonated petro-leum S=O, illustrate that the unsulfonated oil that this method is separated carries more effective surface promoting agent, thus cause the sulfonated petro-leum oil displacement efficiency after point oil to be deteriorated.
Embodiment 3:
Get sulfonated petro-leum (volatile matter: 11.73w%, unsulfonated oil: 43.30w%, sulfonated petro-leum: 40.30w%; Inorganic salt, 4.67w%) pump into first step mixer-settler extractor with water with mass ratio 1:2 simultaneously, combined feed total feed flow is 5L/h, and agitator speed is 1000r/min, and settling time is 1.5h.In tempering tank, entering clarifying tank through stirring, at 70 DEG C, clarifying layering.Upper is oil phase mutually, a unsulfonated oil is flowed out by overflow weir, lower is a mahogany acid salt brine solution mutually, one time mahogany acid salt brine solution continues to enter second stage mixer-settler extractor by pump again, under 95 DEG C of conditions, first clarification after stirring, agitator speed is 1000r/min, settling time is 1.67h, isolates secondary unsulfonated oil and secondary mahogany acid salt brine solution.The first fraction oil rate that draws by experiment is the 64%, second fraction oil rate is 12%, and total score oil rate reaches 76%.
Can be obtained by Determination of Trace Sulfur content analysis, sulphur content in unsulfonated oil when total score oil rate is 76% is the sulfur content in crude oil of 0.0964%(synthesis is 0.1126%), and adopt Infrared spectroscopy unsulfonated oil, without the absorption peak of obvious sulfonated petro-leum S=O, illustrate that the mixing oil of secondary unsulfonated oil and a unsulfonated oil is not substantially containing sulfonated petro-leum, thus ensure that the separating effect of unsulfonated oil and sulfonated petro-leum.
Evaluate the interface performance of sulfonated petro-leum before and after extraction point oil, as shown in Figure 3, in two-stage total score oil rate 76% time, the sulfonated petro-leum interfacial tension before and after being separated is constant, illustrates that sulfonated petro-leum performance is not affected before separation afterwards.
Embodiment 4:
Get sulfonated petro-leum (volatile matter: 10w%, unsulfonated oil: 44w%, sulfonated petro-leum: 41w%; Inorganic salt, 5w%), the mass ratio changing sulfonated petro-leum and water is 1:2, first step mixer-settler extractor temperature 70 C, agitator speed is 1000r/min, settling time 1.5h, the temperature of second stage mixer-settler extractor is 90 DEG C, and agitator speed is 1000r/min, settling time 1.67h.
Embodiment 5:
Get sulfonated petro-leum (volatile matter: 30w%, unsulfonated oil: 20w%, sulfonated petro-leum: 36w%; Inorganic salt, 14w%), the mass ratio changing sulfonated petro-leum and water is 1:0.5, first step mixer-settler extractor temperature 80 DEG C, agitator speed is 3000r/min, settling time 1.5h, and the temperature of second stage mixer-settler extractor is 95 DEG C, agitator speed is 3000r/min, settling time 1.67h.
Embodiment 6:
Get sulfonated petro-leum (volatile matter: 20w%, unsulfonated oil: 30w%, sulfonated petro-leum: 40w%; Inorganic salt, 10w%), the mass ratio changing sulfonated petro-leum and water is 1:1.5, first step mixer-settler extractor temperature 75 DEG C, agitator speed is 2000r/min, settling time 1.5h, and the temperature of second stage mixer-settler extractor is 93 DEG C, agitator speed is 2000r/min, settling time 1.67h.
Infrared spectroscopy is adopted to be separated the unsulfonated oil obtained to the product of embodiment 4 ~ 6 respectively, the absorption peak without obvious sulfonated petro-leum S=O in unsulfonated oil can be found, illustrate that the mixing oil of secondary unsulfonated oil and a unsulfonated oil is not substantially containing sulfonated petro-leum, thus ensure that the separating effect of unsulfonated oil and sulfonated petro-leum.
Evaluate the interface performance of sulfonated petro-leum before and after extraction point oil, can obtain result similar to Figure 3, the sulfonated petro-leum interfacial tension before and after being separated is constant.
Above content is the further description done the present invention in conjunction with concrete embodiment, can not assert that specific embodiment of the invention is confined to these explanations.For general technical staff of the technical field of the invention, without departing from the inventive concept of the premise, some simple deduction or replace can also be made, all should be considered as belonging to protection scope of the present invention.
Claims (4)
1. unsulfonated oil continuous extraction separation method in a sulfonated petro-leum, it is characterized in that: sulfonated petro-leum and water are pumped into first step mixer-settler extractor by the mass ratio of 1:0.5 ~ 1:2, carry out clarified separation, isolate a unsulfonated oil and a mahogany acid salt brine solution, a mahogany acid salt brine solution is pumped into second stage mixer-settler extractor again, isolate secondary unsulfonated oil and secondary mahogany acid salt brine solution, after described secondary sulfonated petro-leum aqueous solution dehydration, obtain the mahogany acid salt brine solution needing concentration.
2. unsulfonated oil continuous extraction separation method in sulfonated petro-leum as claimed in claim 1, it is characterized in that: described sulfonated petro-leum component is: volatile matter (water): 10 ~ 35w%, unsulfonated oil: 20 ~ 45w%, sulfonated petro-leum: 35 ~ 45w%, surplus is inorganic salt.
3. unsulfonated oil continuous extraction separation method in sulfonated petro-leum as claimed in claim 1, is characterized in that: described first step mixer-settler extractor temperature is 70 ~ 80 DEG C, and agitator speed is 1000 ~ 3000r/min, settling time 1.5h.
4. unsulfonated oil continuous extraction separation method in sulfonated petro-leum as claimed in claim 3, is characterized in that: the temperature of described second stage mixer-settler extractor is 90 ~ 95 DEG C, and agitator speed is 1000 ~ 3000r/min, settling time 1.67h.
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Cited By (2)
Publication number | Priority date | Publication date | Assignee | Title |
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CN112567002A (en) * | 2018-07-09 | 2021-03-26 | 罗地亚经营管理公司 | Formulations based on sulfonated lactones for assisted oil recovery |
CN112877095A (en) * | 2019-11-29 | 2021-06-01 | 中石油克拉玛依石化有限责任公司 | Sodium removing method for sulfonated raffinate oil |
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2015
- 2015-07-07 CN CN201510392233.5A patent/CN105037223A/en active Pending
Cited By (4)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN112567002A (en) * | 2018-07-09 | 2021-03-26 | 罗地亚经营管理公司 | Formulations based on sulfonated lactones for assisted oil recovery |
CN112567002B (en) * | 2018-07-09 | 2023-09-08 | 罗地亚经营管理公司 | Sulfonated endo-ketone based formulation for assisting oil recovery |
CN112877095A (en) * | 2019-11-29 | 2021-06-01 | 中石油克拉玛依石化有限责任公司 | Sodium removing method for sulfonated raffinate oil |
CN112877095B (en) * | 2019-11-29 | 2022-07-05 | 中石油克拉玛依石化有限责任公司 | Sodium removing method for sulfonated raffinate oil |
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