CN105414159B - A method of petroleum desorption liquid is handled using graphite oxide aerogel - Google Patents
A method of petroleum desorption liquid is handled using graphite oxide aerogel Download PDFInfo
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- CN105414159B CN105414159B CN201510848247.3A CN201510848247A CN105414159B CN 105414159 B CN105414159 B CN 105414159B CN 201510848247 A CN201510848247 A CN 201510848247A CN 105414159 B CN105414159 B CN 105414159B
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- petroleum
- desorption liquid
- graphite oxide
- oxide aerogel
- aerogel
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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 present invention relates to oil-polluted soils to repair field, it is desirable to provide a method of petroleum desorption liquid is handled using graphite oxide aerogel.The method for handling petroleum desorption liquid using graphite oxide aerogel are as follows: first take oil-polluted soils, lauryl sodium sulfate, saponin, sodium metasilicate, ultrapure water, be mixed with petroleum desorption liquid；Then it takes graphite oxide aerogel to be immersed in petroleum desorption liquid obtained, after oscillation treatment, surfactant and petroleum hydrocarbon in desorption liquid can be efficiently separated.The graphite oxide aerogel is used to handle petroleum desorption liquid by the present invention, not only at low cost, high efficiency, but also easy to operate, pollution-free, can effectively realize the separation of surfactant and petroleum.
Description
Technical field
The present invention relates to oil-polluted soils to repair field, in particular to a kind of to be handled using graphite oxide aerogel
The method of petroleum desorption liquid.
Background technique
About 2/3 is produced by land oil field in our times petroleum total output.And in modern petroleum exploration, exploitation processing
Often soil is caused seriously to pollute in the process.Currently, surfactant enhanced remediation mode is mostly used to handle stone in the world
Soil contaminated by crude oil, it is applied widely, speed is fast, its desorption liquid although the method has many advantages, such as that low energy consumption, process is simple
In, a large amount of petroleum is mixed with surfactant, is not readily separated.If do not handled, the waste of resource is not only caused, but also
Secondary pollution easily is caused to soil, water body etc..
Currently, processing petroleum desorption liquid mostly uses extraction, resin adsorption method, evaporation concentration method etc., Dou Nengda in the world
To the effect of separation petroleum and surfactant.But nonetheless, these methods still have respective shortcoming.Such as extraction
Method is mainly handled using organic solvent, not only complicated for operation, but also is easily done harm to huamn body；At evaporation concentration method
Manage costly, and effect is not satisfactory.
Graphite oxide aerogel is a kind of adsorbent material with strong-hydrophobicity, lipophilicity and huge specific surface area,
With very strong adsorption capacity, therefore has in processing petroleum desorption liquid and have certain effect.But currently, about graphene oxide
The research of aeroge focuses primarily upon in processing this field of organic pollutants in water body, grinds to separation petroleum and surfactant
Study carefully very few, limits its effect in this field.
Summary of the invention
It is a primary object of the present invention to overcome deficiency in the prior art, a kind of at low cost, high efficiency, Er Qiecao are provided
Make simple, safe and efficient, effectively to realize surfactant and separated from petroleum method.In order to solve the above technical problems, this hair
Bright solution is:
A kind of method using graphite oxide aerogel processing petroleum desorption liquid is provided, remedying oil-polluted soil is used for
Earth, it is described using graphite oxide aerogel processing petroleum desorption liquid method specifically include the following steps:
(1) preparation of petroleum desorption liquid: taking oil-polluted soils, and desorbing agent is added, and makes oil-polluted soils and desorption
The mass ratio of agent is 1:12.5；Then oscillation treatment is carried out (at 70 DEG C), after oscillation, carries out centrifugal treating to get arriving
Petroleum desorption liquid；
The desorbing agent is configured by lauryl sodium sulfate, saponin, sodium metasilicate and ultrapure water, and dodecyl sulphur
The concentration of sour sodium, saponin and sodium metasilicate in desorbing agent is respectively 0.5g/L, 0.5g/L and 5g/L；
(2) repair process: under room temperature, taking graphite oxide aerogel to be immersed in petroleum desorption liquid made from step (1),
After oscillation treatment, surfactant and petroleum hydrocarbon in desorption liquid can be efficiently separated.
In the present invention, in the step (1), oscillation treatment is specifically referred to: being vibrated at 70 DEG C with 150r/min
50min。
In the present invention, in the step (1), centrifugal treating is specifically referred to: being centrifuged 15min with 3000r/min.
In the present invention, in the step (2), oscillation treatment is specifically referred to: vibrating 10min with 120r/min.
In the present invention, it to the graphite oxide aerogel after use in step (2), is sufficiently squeezed at normal temperature,
And placed at 100 DEG C, after the weight of graphene aerogel to be oxidized does not change, that is, it may be repeated repairing for step (3)
Multiple processing, is reused.
In the present invention, in the step (2), after graphite oxide aerogel handles petroleum desorption liquid, ultraviolet point is utilized
Light photometry can measure the concentration of petroleum in petroleum desorption liquid.
A kind of preparation method of graphite oxide aerogel is provided, method particularly includes: take graphene oxide and dimethyl methyl
Amide is configured to graphene oxide solution, and makes the concentration 2g/L of graphene oxide in the solution；It is molten to graphene oxide again
Ascorbic acid is added in liquid, makes the concentration 4g/L of ascorbic acid in the solution；Ultrasonic extraction 2h is carried out to solution, it then will be molten
Liquid is transferred in vial, is placed at 75 DEG C to becoming hydrogel (standing time preferred 16h)；Finally, hydrogel is freezed
Dry 12h, i.e. acquisition graphite oxide aerogel.
In the present invention, after solution becomes hydrogel, hydrogel is first shifted into beaker, is impregnated after a week with deionized water
(remove the small-molecule substances such as ascorbic acid and its oxide), then carry out subsequent freeze-drying process.
Compared with prior art, the beneficial effects of the present invention are:
Graphite oxide aerogel prepared by the present invention has the characteristics that prepare simple, safe and efficient, and the present invention should
Graphite oxide aerogel is for handling petroleum desorption liquid, not only at low cost, high efficiency, but also easy to operate, pollution-free, can have
Effect realizes the separation of surfactant and petroleum；Therefore graphite oxide aerogel processing this field of petroleum desorption liquid in,
It is with a wide range of applications.
Detailed description of the invention
Fig. 1 is graphite oxide aerogel adsorption deionizing water schematic diagram.
Fig. 2 is that graphite oxide aerogel adsorbs petroleum schematic diagram.
Fig. 3 is the electron microscope of graphite oxide aerogel.
Fig. 4 is that graphite oxide aerogel adsorbs the electron microscope after petroleum.
Fig. 5 is that graphite oxide aerogel reuses effect picture.
Specific embodiment
Present invention is further described in detail with specific embodiment with reference to the accompanying drawing:
The following examples can make the professional technician of this profession that the present invention be more fully understood, but not with any side
The formula limitation present invention.Wherein, all reagents use excellent pure grade standard, carry out solution preparation using ultrapure water.
Embodiment 1
(1) preparation of petroleum desorption liquid: taking oil-polluted soils, and desorbing agent, desorption is added according to the mass ratio of 1:12.5
Agent is configured by lauryl sodium sulfate, saponin, sodium metasilicate and ultrapure water, and lauryl sodium sulfate, saponin and silicon
Concentration of the sour sodium in desorbing agent is respectively 0.5g/L, 0.5g/L and 5g/L, vibrates 50min, oscillation at 70 DEG C with 150r/min
After, it is centrifuged 15min under 3000r/min, obtains petroleum desorption liquid.
(2) preparation of graphite oxide aerogel: (the oxidation stone in the graphene oxide solution that dimethylformamide is prepared
Concentration of the black alkene in dimethylformamide is 2g/L) ascorbic acid (concentration of ascorbic acid in the solution is 4g/L) is added,
Ultrasonic extraction 2h；Then transfer solution places 16h at 75 DEG C in vial, until becoming hydrogel；After, freezing is dry
Dry 12h obtains graphite oxide aerogel.
(3) it under room temperature, takes graphite oxide aerogel to immerse in petroleum desorption liquid, vibrates 10min under 120r/min.Terminate
Afterwards, the concentration of petroleum in determined by ultraviolet spectrophotometry petroleum desorption liquid is utilized.
(4) under room temperature, graphite oxide aerogel is sufficiently squeezed, and place a few hours at 100 DEG C, do not occurred to weight
After variation, the process of (3) is repeated.
The hydrophobicity and lipophilicity of 2 graphite oxide aerogel of embodiment
For the hydrophobicity for detecting graphite oxide aerogel, this test four times of setting (5min, 10min, 15min,
20min), its size to deionized water adsorbance is detected.As shown in Figure 1,5min to 15min, graphite oxide aerogel pair
The adsorbance increase of deionized water is more obvious, then keeps stablizing, adsorbance when 20min is 0.35g/g, it was demonstrated that it is good
Good hydrophobicity.To prove its good lipophilicity, this test is also provided with four times (5min, 10min, 15min, 20min).
Figure it is seen that oxidation stone, in 20min, graphite oxide aerogel is 20.08g/g, card to the maximal absorptive capacity of petroleum
Its powerful oil absorption capacity is illustrated.Graphite oxide aerogel is detected using scanning electron microscope.It can be seen by Fig. 3, Fig. 4
Out, graphite oxide aerogel is loose porous, and there are many folds on surface, therefore can adsorb a large amount of petroleum.
3 graphite oxide aerogel of embodiment recycles effect
Petroleum in petroleum desorption liquid has important utility value, it is therefore desirable to be recycled to it.This test
Graphite oxide aerogel is recycled by pressing method, not only method is simple, but also easily operated.It can by Fig. 5
To find out, as the increase of reuse number maintains always though graphite oxide aerogel declines the adsorbance of petroleum
70% or so.The result shows that graphite oxide aerogel not only has preferable adsorption capacity to petroleum, but also recycle
Effect is good, therefore is with a wide range of applications in processing petroleum desorption liquid field.
Finally it should be noted that the above enumerated are only specific embodiments of the present invention.It is clear that the invention is not restricted to
Above embodiments can also have many variations.Those skilled in the art can directly lead from present disclosure
Out or all deformations for associating, it is considered as protection scope of the present invention.
Claims (8)
1. a kind of method using graphite oxide aerogel processing petroleum desorption liquid, is used for remedying oil-polluted soils, special
Sign is, the method using graphite oxide aerogel processing petroleum desorption liquid specifically include the following steps:
(1) preparation of petroleum desorption liquid: taking oil-polluted soils, and desorbing agent is added, and makes oil-polluted soils and desorbing agent
Mass ratio is 1:12.5；Then oscillation treatment is carried out, after oscillation, carries out centrifugal treating to get petroleum desorption liquid is arrived；
The desorbing agent is configured by lauryl sodium sulfate, saponin, sodium metasilicate and ultrapure water, and dodecyl sulphate
The concentration of sodium, saponin and sodium metasilicate in desorbing agent is respectively 0.5g/L, 0.5g/L and 5g/L；
(2) repair process: under room temperature, taking graphite oxide aerogel to be immersed in petroleum desorption liquid made from step (1), oscillation
After processing, surfactant and petroleum hydrocarbon in desorption liquid can be efficiently separated.
2. a kind of method using graphite oxide aerogel processing petroleum desorption liquid according to claim 1, feature
It is, in the step (1), oscillation treatment is specifically referred to: 50min is vibrated with 150r/min at 70 DEG C.
3. a kind of method using graphite oxide aerogel processing petroleum desorption liquid according to claim 1, feature
It is, in the step (1), centrifugal treating is specifically referred to: 15min is centrifuged with 3000r/min.
4. a kind of method using graphite oxide aerogel processing petroleum desorption liquid according to claim 1, feature
It is, in the step (2), oscillation treatment is specifically referred to: 10min is vibrated with 120r/min.
5. a kind of method using graphite oxide aerogel processing petroleum desorption liquid according to claim 1, feature
It is, to the graphite oxide aerogel after use in step (2), is sufficiently squeezed at normal temperature, and is transferred in 100 DEG C
It sets, after the weight of graphene aerogel to be oxidized does not change, that is, may be repeated the repair process of step (2), carry out weight
It is multiple to utilize.
6. a kind of method using graphite oxide aerogel processing petroleum desorption liquid according to claim 1, feature
It is, in the step (2), after graphite oxide aerogel handles petroleum desorption liquid, can be measured using ultraviolet spectrophotometry
The concentration of petroleum in petroleum desorption liquid.
7. a kind of method using graphite oxide aerogel processing petroleum desorption liquid according to claim 1, feature
It is, the preparation method of the graphite oxide aerogel specifically: graphene oxide and dimethylformamide is taken to be configured to oxygen
Graphite alkene solution, and make the concentration 2g/L of graphene oxide in the solution；It is added again into graphene oxide solution anti-bad
Hematic acid makes the concentration 4g/L of ascorbic acid in the solution；Ultrasonic extraction 2h is carried out to solution, then transfers the solution into glass
In bottle, placed at 75 DEG C to becoming hydrogel；Finally, hydrogel is freeze-dried 12h, i.e. acquisition graphene oxide airsetting
Glue.
8. a kind of method using graphite oxide aerogel processing petroleum desorption liquid according to claim 7, feature
It is, in the preparation method of the graphite oxide aerogel, after solution becomes hydrogel, first shifts hydrogel into beaker,
It is impregnated after a week with deionized water, then carries out subsequent freeze-drying process.
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| 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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| 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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| US8993113B2 (en) * | 2010-08-06 | 2015-03-31 | Lawrence Livermore National Security, Llc | Graphene aerogels |
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Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
Non-Patent Citations (2)
| Title |
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| Mechanically Strong and Highly Conductive Graphene Aerogels and Its Use as Electrodes for Electrochemical Power Sources;Xuetong Zhang etal;《Journal of Materials Chemistry》;20111231;第1-2页 |
| 高度有序3D石墨烯基高分子复合材料的制备及导电性;王昭群;《全国石墨烯材料技术，发展与应用交流研讨会》;20150117;第28页 |
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