CN105414159A - Method for treating petroleum desorption solution through graphene oxide aerogel - Google Patents
Method for treating petroleum desorption solution through graphene oxide aerogel Download PDFInfo
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- CN105414159A CN105414159A CN201510848247.3A CN201510848247A CN105414159A CN 105414159 A CN105414159 A CN 105414159A CN 201510848247 A CN201510848247 A CN 201510848247A CN 105414159 A CN105414159 A CN 105414159A
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- graphite oxide
- oxide aerogel
- desorption liquid
- oil
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B09—DISPOSAL OF SOLID WASTE; RECLAMATION OF CONTAMINATED SOIL
- B09C—RECLAMATION OF CONTAMINATED SOIL
- B09C1/00—Reclamation of contaminated soil
Abstract
The invention relates to the field of petroleum-contaminated soil remediation and aims at providing a method for treating a petroleum desorption solution through graphene oxide aerogel. The method for treating the petroleum desorption solution through the graphene oxide aerogel includes the steps that firstly, petroleum-contaminated soil, sodium dodecyl sulfate, saponin, sodium silicate and ultrapure water are selected firstly and mixed, and the petroleum desorption solution is prepared; and secondly, the graphene oxide aerogel is soaked into the petroleum desorption solution and vibrated, and a surfactant and petroleum hydrocarbon in the desorption solution can be separated effectively. According to the method, the graphene oxide aerogel is used for treating the petroleum desorption solution, cost is low, benefits are high, operation is easy, pollution is avoided, and the surfactant and petroleum can be separated effectively.
Description
Technical field
The invention relates to oil-polluted soils and repair field, particularly a kind of method utilizing graphite oxide aerogel process oil desorption liquid.
Background technology
In our times oil total output, about 2/3 by land field produces.And often severe contamination can be caused to soil in modern petroleum exploration, exploitation process.At present, many employing surfactant enhanced remediation mode process oil-polluted soils in the world, although the method has, energy consumption is low, flow process is simple, the advantages such as applied widely, speed is fast, but in its desorption liquid, a large amount of oil and surfactant mix, not easily separated.If do not processed, not only cause the waste of resource, and easily secondary pollution is caused to soil, water body etc.
At present, process oil desorption liquid many employings extraction, resin adsorption method, evaporation concentration method etc. in the world, the effect being separated oil and surfactant can be reached.But nonetheless, these methods still have respective weak point.As extraction, mainly utilize organic solvent to process, not only complicated operation, and easily human body is worked the mischief; Evaporation concentration method disposal cost is high, and effect is not satisfactory.
Graphite oxide aerogel is a kind of sorbing material with strong-hydrophobicity, lipophile and huge specific area, has very strong adsorption capacity, and therefore in process oil desorption liquid, tool has certain effect.But at present, the research about graphite oxide aerogel mainly concentrates in process this field of organic pollutants in water body, very few to the research being separated oil and surfactant, limit its effect in this field.
Summary of the invention
Main purpose of the present invention is to overcome deficiency of the prior art, provides that a kind of cost is low, high efficiency, and simple to operate, safe and efficient, effectively can realize the method for surfactant and separated from petroleum.For solving the problems of the technologies described above, solution of the present invention is:
There is provided a kind of method utilizing graphite oxide aerogel process oil desorption liquid, for remedying oil-polluted soils, the described method of graphite oxide aerogel process oil desorption liquid that utilizes specifically comprises the steps:
(1) preparation of oil desorption liquid: get oil-polluted soils, add desorbing agent, and make the mass ratio of oil-polluted soils and desorbing agent be 1:12.5; Then (at 70 DEG C) carry out oscillation treatment, after vibration terminates, carry out centrifugal treating, namely obtain oil desorption liquid;
Described desorbing agent is configured by lauryl sodium sulfate, saponin, sodium metasilicate and ultra-pure water and forms, and lauryl sodium sulfate, saponin and the sodium metasilicate concentration in desorbing agent is respectively 0.5g/L, 0.5g/L and 5g/L;
(2) repair process: under normal temperature, gets graphite oxide aerogel and is immersed in the obtained oil desorption liquid of step (1), after oscillation treatment, effectively can be separated surfactant and petroleum hydrocarbon in desorption liquid.
In the present invention, in described step (1), oscillation treatment specifically refers to: with 150r/min vibration 50min at 70 DEG C.
In the present invention, in described step (1), centrifugal treating specifically refers to: with the centrifugal 15min of 3000r/min.
In the present invention, in described step (2), oscillation treatment specifically refers to: with 120r/min vibration 10min.
In the present invention, to the graphite oxide aerogel after use in step (2), fully extrude at normal temperatures, and place at 100 DEG C, after the weight of graphene aerogel to be oxidized does not change, the repair process of step (3) can be repeated, reuse.
In the present invention, in described step (2), after graphite oxide aerogel process oil desorption liquid, utilize ultraviolet spectrophotometry can measure the concentration of oil desorption liquid PetroChina Company Limited..
There is provided a kind of preparation method of graphite oxide aerogel, concrete grammar is: get graphene oxide and dimethyl formamide is mixed with graphene oxide solution, and makes graphene oxide concentration in the solution be 2g/L; In graphene oxide solution, add ascorbic acid again, make ascorbic acid concentration in the solution be 4g/L; Ultrasonic extraction 2h is carried out to solution, then solution is transferred in vial, be placed at 75 DEG C and become hydrogel (preferred 16h standing time); Finally, by hydrogel freeze drying 12h, namely graphite oxide aerogel is obtained.
In the present invention, after solution becomes hydrogel, first transfer water gel, in beaker, after soaking one week (to remove the small-molecule substance such as ascorbic acid and its oxide), then carries out follow-up freeze drying process by deionized water.
Compared with prior art, the invention has the beneficial effects as follows:
Graphite oxide aerogel prepared by the present invention has prepares the features such as simple, safe and efficient, and the present invention by this graphite oxide aerogel for the treatment of oil desorption liquid, not only cost is low, high efficiency, and simple to operate, pollution-free, effectively can realize being separated of surfactant and oil; Therefore graphite oxide aerogel is in process this field of oil desorption liquid, is with a wide range of applications.
Accompanying drawing explanation
Fig. 1 is graphite oxide aerogel adsorption deionizing water schematic diagram.
Fig. 2 is graphite oxide aerogel absorption oil schematic diagram.
Fig. 3 is the Electronic Speculum figure of graphite oxide aerogel.
Fig. 4 is the Electronic Speculum figure after graphite oxide aerogel absorption oil.
Fig. 5 is graphite oxide aerogel recycling design sketch.
Detailed description of the invention
Below in conjunction with accompanying drawing and detailed description of the invention, the present invention is described in further detail:
The following examples can make professional and technical personnel's comprehend the present invention of this specialty, but do not limit the present invention in any way.Wherein, all reagent all uses the pure standard of top grade, utilizes ultra-pure water to carry out solution preparation.
Embodiment 1
(1) preparation of oil desorption liquid: get oil-polluted soils, desorbing agent is added according to the mass ratio of 1:12.5, desorbing agent is configured by lauryl sodium sulfate, saponin, sodium metasilicate and ultra-pure water and forms, and lauryl sodium sulfate, saponin and the sodium metasilicate concentration in desorbing agent is respectively 0.5g/L, 0.5g/L and 5g/L, with 150r/min vibration 50min at 70 DEG C, after vibration terminates, centrifugal 15min under 3000r/min, obtains oil desorption liquid.
(2) preparation of graphite oxide aerogel: (concentration of graphene oxide in dimethyl formamide is 2g/L) adds ascorbic acid (ascorbic acid concentration is in the solution 4g/L), ultrasonic extraction 2h in the graphene oxide solution of dimethyl formamide preparation; Then shift solution in vial, place 16h at 75 DEG C, until become hydrogel; After end, freeze drying 12h, obtains graphite oxide aerogel.
(3), under normal temperature, get graphite oxide aerogel and immerse in oil desorption liquid, vibrate under 120r/min 10min.After end, utilize the concentration of determined by ultraviolet spectrophotometry oil desorption liquid PetroChina Company Limited..
(4) under normal temperature, fully extrude graphite oxide aerogel, and place a few hours at 100 DEG C, after weight does not change, repeat the process of (3).
The hydrophobicity of embodiment 2 graphite oxide aerogel and lipophile
For detecting the hydrophobicity of graphite oxide aerogel, this test arranges four times (5min, 10min, 15min, 20min), detects its size to deionized water adsorbance.As shown in Figure 1,5min to 15min, graphite oxide aerogel is comparatively obvious to the adsorbance increase of deionized water, and keep stable subsequently, adsorbance during 20min is 0.35g/g, demonstrates the hydrophobicity that it is good.For proving its good lipophile, this test also arranges four times (5min, 10min, 15min, 20min).As can be seen from Figure 2, oxidation stone is when 20min, and graphite oxide aerogel is 20.08g/g to the maximal absorptive capacity of oil, demonstrates the oil absorption that it is powerful.ESEM is utilized to detect graphite oxide aerogel.As can be seen from Fig. 3, Fig. 4, graphite oxide aerogel is loose porous, and there is a lot of fold on surface, therefore can adsorb a large amount of oil.
Embodiment 3 graphite oxide aerogel recycle effect
Oil in oil desorption liquid has important value, therefore needs to recycle it.This test is recycled graphite oxide aerogel by pressing method, and not only method is simple, and is easy to operation.As seen from Figure 5, along with the increase of reuse number of times, though the adsorbance of graphite oxide aerogel to oil declines to some extent, maintain about 70% always.Result shows, graphite oxide aerogel not only has good adsorption capacity to oil, and recycles effective, is therefore with a wide range of applications in process oil desorption liquid field.
Finally, it should be noted that above what enumerate is only specific embodiments of the invention.Obviously, the invention is not restricted to above embodiment, a lot of distortion can also be had.All distortion that those of ordinary skill in the art can directly derive or associate from content disclosed by the invention, all should think protection scope of the present invention.
Claims (8)
1. utilize a method for graphite oxide aerogel process oil desorption liquid, for remedying oil-polluted soils, it is characterized in that, the described method of graphite oxide aerogel process oil desorption liquid that utilizes specifically comprises the steps:
(1) preparation of oil desorption liquid: get oil-polluted soils, add desorbing agent, and make the mass ratio of oil-polluted soils and desorbing agent be 1:12.5; Then carry out oscillation treatment, after vibration terminates, carry out centrifugal treating, namely obtain oil desorption liquid;
Described desorbing agent is configured by lauryl sodium sulfate, saponin, sodium metasilicate and ultra-pure water and forms, and lauryl sodium sulfate, saponin and the sodium metasilicate concentration in desorbing agent is respectively 0.5g/L, 0.5g/L and 5g/L;
(2) repair process: under normal temperature, gets graphite oxide aerogel and is immersed in the obtained oil desorption liquid of step (1), after oscillation treatment, effectively can be separated surfactant and petroleum hydrocarbon in desorption liquid.
2. a kind of method utilizing graphite oxide aerogel process oil desorption liquid according to claim 1, it is characterized in that, in described step (1), oscillation treatment specifically refers to: with 150r/min vibration 50min at 70 DEG C.
3. a kind of method utilizing graphite oxide aerogel process oil desorption liquid according to claim 1, it is characterized in that, in described step (1), centrifugal treating specifically refers to: with the centrifugal 15min of 3000r/min.
4. a kind of method utilizing graphite oxide aerogel process oil desorption liquid according to claim 1, it is characterized in that, in described step (2), oscillation treatment specifically refers to: with 120r/min vibration 10min.
5. a kind of method utilizing graphite oxide aerogel process oil desorption liquid according to claim 1, it is characterized in that, to the graphite oxide aerogel after use in step (2), fully extrude at normal temperatures, and place at 100 DEG C, after the weight of graphene aerogel to be oxidized does not change, the repair process of step (3) can be repeated, reuse.
6. a kind of method utilizing graphite oxide aerogel process oil desorption liquid according to claim 1, it is characterized in that, in described step (2), after graphite oxide aerogel process oil desorption liquid, utilize ultraviolet spectrophotometry can measure the concentration of oil desorption liquid PetroChina Company Limited..
7. a preparation method for graphite oxide aerogel, is characterized in that, concrete grammar is: get graphene oxide and dimethyl formamide is mixed with graphene oxide solution, and makes graphene oxide concentration in the solution be 2g/L; In graphene oxide solution, add ascorbic acid again, make ascorbic acid concentration in the solution be 4g/L; Ultrasonic extraction 2h is carried out to solution, then solution is transferred in vial, be placed at 75 DEG C and become hydrogel; Finally, by hydrogel freeze drying 12h, namely graphite oxide aerogel is obtained.
8. the preparation method of a kind of graphite oxide aerogel according to claim 7, is characterized in that, after solution becomes hydrogel, first transfer water gel, in beaker, after soaking one week, then carries out follow-up freeze drying process by deionized water.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110152599A (en) * | 2018-03-01 | 2019-08-23 | 济南开发区星火科学技术研究院 | It is a kind of can efficient process petroleum desorption liquid graphite oxide aerogel preparation method |
| CN110153162A (en) * | 2018-02-05 | 2019-08-23 | 山东佳星环保科技有限公司 | It is a kind of can efficient process petroleum desorption liquid graphite oxide aerogel preparation method |
| CN111821910A (en) * | 2019-04-19 | 2020-10-27 | 宁波锋成先进能源材料研究院 | Amphiphilic surfactant, eluting agent and application thereof |
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| US20120034442A1 (en) * | 2010-08-06 | 2012-02-09 | Lawrence Livermore National Security, Llc | Graphene aerogels |
| CN103599924A (en) * | 2013-11-29 | 2014-02-26 | 浙江大学 | Novel desorbent for processing diesel polluted soil and preparation method thereof |
| CN104128364A (en) * | 2014-06-25 | 2014-11-05 | 浙江大学 | Novel petroleum desorption agent reinforced by sodium carbonate |
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Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20120034442A1 (en) * | 2010-08-06 | 2012-02-09 | Lawrence Livermore National Security, Llc | Graphene aerogels |
| CN103599924A (en) * | 2013-11-29 | 2014-02-26 | 浙江大学 | Novel desorbent for processing diesel polluted soil and preparation method thereof |
| CN104128364A (en) * | 2014-06-25 | 2014-11-05 | 浙江大学 | Novel petroleum desorption agent reinforced by sodium carbonate |
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| XUETONG ZHANG ETAL: "Mechanically Strong and Highly Conductive Graphene Aerogels and Its Use as Electrodes for Electrochemical Power Sources", 《JOURNAL OF MATERIALS CHEMISTRY》 * |
| 王昭群: "高度有序3D石墨烯基高分子复合材料的制备及导电性", 《全国石墨烯材料技术，发展与应用交流研讨会》 * |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110153162A (en) * | 2018-02-05 | 2019-08-23 | 山东佳星环保科技有限公司 | It is a kind of can efficient process petroleum desorption liquid graphite oxide aerogel preparation method |
| CN110152599A (en) * | 2018-03-01 | 2019-08-23 | 济南开发区星火科学技术研究院 | It is a kind of can efficient process petroleum desorption liquid graphite oxide aerogel preparation method |
| CN111821910A (en) * | 2019-04-19 | 2020-10-27 | 宁波锋成先进能源材料研究院 | Amphiphilic surfactant, eluting agent and application thereof |
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