CN109621906B - Method for preparing composite sponge capable of absorbing viscous crude oil - Google Patents
Method for preparing composite sponge capable of absorbing viscous crude oil Download PDFInfo
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- CN109621906B CN109621906B CN201811536600.4A CN201811536600A CN109621906B CN 109621906 B CN109621906 B CN 109621906B CN 201811536600 A CN201811536600 A CN 201811536600A CN 109621906 B CN109621906 B CN 109621906B
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- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/02—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
- B01J20/20—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising free carbon; comprising carbon obtained by carbonising processes
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/22—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising organic material
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/28—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties
- B01J20/28014—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties characterised by their form
- B01J20/28042—Shaped bodies; Monolithic structures
- B01J20/28045—Honeycomb or cellular structures; Solid foams or sponges
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/28—Treatment of water, waste water, or sewage by sorption
- C02F1/283—Treatment of water, waste water, or sewage by sorption using coal, charred products, or inorganic mixtures containing them
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/28—Treatment of water, waste water, or sewage by sorption
- C02F1/285—Treatment of water, waste water, or sewage by sorption using synthetic organic sorbents
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2101/00—Nature of the contaminant
- C02F2101/30—Organic compounds
- C02F2101/32—Hydrocarbons, e.g. oil
Abstract
The invention relates to a method for preparing a composite sponge capable of absorbing viscous crude oil, which is prepared by reducing graphene oxide and loading the graphene oxide on melamine sponge, and comprises the following steps: (1) preparing a graphene oxide dispersion liquid; (2) adding ammonia water and L-ascorbic acid with certain concentrations into the graphene oxide dispersion liquid; (3) putting sponge into the solution to perform hydrothermal reaction; (4) and taking out the reacted composite sponge and drying to obtain the graphene composite melamine sponge. The preparation method is simple and easy to implement, good in repeatability, free of secondary pollution, high in commercialization degree of the melamine sponge and low in price, and the obtained composite sponge can quickly adsorb viscous crude oil in water.
Description
Technical Field
The invention relates to an oil absorption functional material, in particular to a method for preparing a composite sponge capable of absorbing viscous crude oil.
Background
With the development of the petroleum industry, a large amount of petroleum flows into the ocean due to oil spilling in oil fields and transportation pipelines or accidents of cruise ships every year, and serious pollution is caused to water bodies and coastal environments. The rapid removal of the large-area viscous crude oil and the advanced treatment of secondary organic pollutants are very important and cannot be effectively solved.
In view of the characteristic that oil pollutants float on the water surface and in the nearby depth, the floating oil stain removing material is an ideal choice for realizing faster oil stain treatment and convenient recovery.
Since the discovery of graphene as a two-dimensional nanomaterial in 2004, the excellent physicochemical properties of graphene, such as a very large specific surface area, high thermal conductivity, high electrical conductivity, high strength, and high modulus, have become hot spots for research in various fields. The graphene is hydrophobic and oleophilic, so that the graphene is not easy to uniformly disperse in a water phase; the oxidized form of the graphene oxide is hydrophilic and oleophobic and is easy to disperse in a water phase. Therefore, the hydrophobic and oleophilic graphene is prepared by reducing the graphene oxide dispersion liquid at present. On the other hand, the viscosity of the crude oil is gradually reduced along with the temperature rise, the adsorption effect of the crude oil on an ice-cold sea surface is poor due to high viscosity, and the crude oil can be effectively absorbed only by heating the oil absorption material to reduce the viscosity of the crude oil. Ge et al utilize above-mentioned principle with the sponge that the parcel has the graphite alkene as floating type greasy dirt processing material, thereby reduced crude oil viscosity through the electrothermal effect of graphite alkene and improved crude oil adsorption rate greatly. However, the device needs a working material to be electrified and then heated to absorb oil, so that potential safety hazards exist or the device is easy to lose efficacy when applied to a water body. Meanwhile, the preparation method adopts hydroiodic acid to reduce the graphene oxide, and the hydroiodic acid has strong corrosivity and strong stimulation on a human body, and is not a safe and environment-friendly method.
Disclosure of Invention
The invention aims to overcome the defects in the prior art and provide a safe and green preparation method of the composite sponge capable of absorbing viscous crude oil, so that the prepared composite sponge is oleophilic and hydrophobic, has high porosity and has better photothermal effect.
The purpose of the invention can be realized by the following technical scheme:
a method for preparing a composite sponge capable of absorbing viscous crude oil comprises the following steps:
(1) adding graphene oxide powder into pure water to prepare a graphene oxide dispersion liquid;
(2) adding concentrated ammonia water and L-ascorbic acid into the graphene oxide dispersion liquid, wherein the L-ascorbic acid is added, so that not only can the effect of reducing graphene oxide into reduced graphene oxide be achieved, but also the graphene and the sponge can form hydrogel and be firmly loaded on the sponge;
(3) putting melamine sponge into the solution to perform hydrothermal reaction;
(4) and taking out the reacted sponge and drying to obtain the composite sponge capable of absorbing viscous crude oil.
The concentration of the graphene oxide dispersion liquid in the step (1) is 0.5-3 mg/ml. If the concentration of the graphene oxide dispersion liquid is too low, the sponge is not obviously modified; if the concentration is too high, the porosity of the sponge is reduced, and the cost is too high.
According to the method provided by the invention, an ultrasonic cell disruptor is adopted to carry out ultrasonic treatment on the dispersion liquid, the ultrasonic treatment time is 5min-20min, and the power of the ultrasonic treatment instrument is 100W-300W.
According to the method provided by the invention, the concentration of the concentrated ammonia water in the step (2) is 10mmol/L-100mmol/L, and the concentration of the L-ascorbic acid is 0.05mmol/L-2 mmol/L. The strong ammonia water has the effect of making the graphene oxide more easily dispersed through electrostatic repulsion, but the stability of the liquid is not facilitated if the concentration is too high. The L-ascorbic acid has the effects of reducing graphene oxide into reduced graphene, enabling the graphene and the sponge to form hydrogel, enabling the load to be uniform and firm, and causing condensation polymerization of the graphene composite sponge due to too high concentration, so that the performance of the graphene composite sponge is affected.
According to the method provided by the invention, the hydrothermal reaction temperature in the step (3) is 80-100 ℃, and the heating time is 40-120 min. The hydrothermal reaction can provide a high-temperature and high-pressure environment to reduce the graphene oxide, and if the temperature is too high and the time is too long, the sponge structure is damaged, and the energy consumption is reduced.
According to the method provided by the invention, the drying temperature in the step (4) is 50-80 ℃, and the drying time is 12-24 h.
According to the method, graphene oxide is used as a precursor, the graphene oxide is dispersed in a water phase, the graphene oxide can be reduced and loaded to the melamine sponge through a hydrothermal reaction, and the reduction degree of the graphene oxide and the loading amount of the graphene loaded to the sponge can be controlled only by adjusting the adding amount of the L-ascorbic acid in the process.
Compared with the prior art, the invention has the following advantages:
(1) the composite sponge prepared by the invention is loose and porous, has large specific surface area and low density, can be used as an oil adsorbing material, and widens the application prospect;
(2) according to the invention, the reduction degree of the graphene oxide and the loading capacity of the graphene loaded to the sponge can be controlled by adjusting the adding amount of the L-ascorbic acid, the preparation process is simple, safe and easy to operate, no secondary pollution is generated, and the preparation period is short;
(3) the melamine sponge serving as the load substrate selected by the invention has high commercialization degree and low cost, does not generate secondary pollution to the environment, and is easy to popularize and apply.
Drawings
FIG. 1 is a scanning electron microscope image of a prepared composite sponge capable of absorbing crude oil in a viscous state;
FIG. 2 is a digital photograph of a composite sponge capable of absorbing crude oil in a viscous state prepared in the present invention, wherein A and B are respectively a comparison chart of the sponge before and after oil absorption;
FIG. 3 is an infrared thermograph of the sponge under simulated sunlight irradiation, and A and B are respectively an infrared thermograph of a blank melamine sponge and a prepared composite sponge capable of absorbing viscous crude oil.
Detailed Description
The present invention will be described in detail with reference to specific examples. The following examples will assist those skilled in the art in further understanding the invention, but are not intended to limit the invention in any way. It should be noted that variations and modifications can be made by persons skilled in the art without departing from the spirit of the invention. All falling within the scope of the present invention.
A method for preparing a composite sponge capable of absorbing viscous crude oil comprises the following steps:
(1) adding graphene oxide powder into pure water to prepare graphene oxide dispersion liquid with the concentration of 0.5-3 mg/ml, and simultaneously carrying out ultrasonic treatment on the dispersion liquid for 5-20 min by adopting an ultrasonic cell disruption instrument, wherein the ultrasonic power is controlled to be 100-300W;
(2) adding concentrated ammonia water and L-ascorbic acid into the graphene oxide dispersion liquid, wherein the concentration of the concentrated ammonia water in the graphene oxide dispersion liquid is 10-100 mmol/L, the concentration of the L-ascorbic acid in the graphene oxide dispersion liquid is 0.05-2 mmol/L, and adding the L-ascorbic acid can reduce the graphene oxide into reduced graphene oxide, can also enable the graphene and sponge to form hydrogel and be firmly loaded on the sponge, and the adding amount of the L-ascorbic acid can influence the final loaded graphene amount on the sponge. In a certain degree, the more the L-ascorbic acid is added, the more the graphene is loaded on the sponge;
(3) putting melamine sponge into the solution, and carrying out hydrothermal reaction at the temperature of 80-100 ℃ for 40-120 min;
(4) and taking out the reacted sponge, and drying for 12-24 h at the temperature of 50-80 ℃ to obtain the composite sponge capable of absorbing viscous crude oil.
The following are more detailed embodiments, and the technical solutions and the technical effects obtained by the present invention will be further described by the following embodiments.
Example 1
(1) Adding 90mg of graphene oxide powder into 30ml of pure water, and performing ultrasonic treatment for 10min by using an ultrasonic cell disruptor under 300W to prepare a 3mg/ml graphene oxide stock solution;
(2) taking 4.667ml of graphene oxide stock solution, adding 9.305ml of pure water, 28 mu L of ammonia water and 12.3mg of L-ascorbic acid;
(3) putting the melamine sponge and the solution into a 20ml hydrothermal reaction kettle together, and carrying out hydrothermal reaction at the temperature of 95 ℃ for 60 min;
(4) and taking out the reacted sponge, and drying at 60 ℃ for 18h to obtain the composite sponge capable of absorbing viscous crude oil.
Example 2
(1) Adding 90mg of graphene oxide powder into 30ml of pure water, and carrying out ultrasonic treatment for 30min by using an ultrasonic cell disruptor with 100W to prepare a 3mg/ml graphene oxide stock solution;
(2) taking 4.667ml of graphene oxide stock solution, adding 9.305ml of pure water, 28 mu L of ammonia water and 12.3mg of L-ascorbic acid;
(3) putting the melamine sponge and the solution into a 20ml hydrothermal reaction kettle together, and carrying out hydrothermal reaction at the temperature of 95 ℃ for 60 min;
(4) and taking out the reacted sponge, and drying at 60 ℃ for 18h to obtain the composite sponge capable of absorbing viscous crude oil.
Example 3
(1) Adding 90mg of graphene oxide powder into 30ml of pure water, and performing ultrasonic treatment for 10min by using an ultrasonic cell disruptor under 300W to prepare a 3mg/ml graphene oxide stock solution;
(2) 9.333ml of graphene oxide stock solution is taken, 4.639ml of pure water, 28 mu L of ammonia water and 12.3mg of L-ascorbic acid are added;
(3) putting the melamine sponge and the solution into a 20ml hydrothermal reaction kettle together, and carrying out hydrothermal reaction at the temperature of 95 ℃ for 60 min;
(4) and taking out the reacted sponge, and drying at 60 ℃ for 18h to obtain the composite sponge capable of absorbing viscous crude oil.
Example 4
(1) Adding 90mg of graphene oxide powder into 30ml of pure water, and performing ultrasonic treatment for 10min by using an ultrasonic cell disruptor under 300W to prepare a 3mg/ml graphene oxide stock solution;
(2) taking 4.667ml of graphene oxide stock solution, adding 9.277ml of pure water, 56 mu L of ammonia water and 12.3mg of L-ascorbic acid;
(3) putting the melamine sponge and the solution into a 20ml hydrothermal reaction kettle together, and carrying out hydrothermal reaction at the temperature of 95 ℃ for 60 min;
(4) and taking out the reacted sponge, and drying at 60 ℃ for 18h to obtain the composite sponge capable of absorbing viscous crude oil.
Example 5
(1) Adding 90mg of graphene oxide powder into 30ml of pure water, and performing ultrasonic treatment for 10min by using an ultrasonic cell disruptor under 300W to prepare a 3mg/ml graphene oxide stock solution;
(2) taking 4.667ml of graphene oxide stock solution, adding 9.305ml of pure water, 28 mu L of ammonia water and 24.7mg of L-ascorbic acid;
(3) putting the melamine sponge and the solution into a 20ml hydrothermal reaction kettle together, and carrying out hydrothermal reaction at the temperature of 95 ℃ for 60 min;
(4) and taking out the reacted sponge, and drying at 60 ℃ for 18h to obtain the composite sponge capable of absorbing viscous crude oil.
Example 6
(1) Adding 90mg of graphene oxide powder into 30ml of pure water, and performing ultrasonic treatment for 10min by using an ultrasonic cell disruptor under 300W to prepare a 3mg/ml graphene oxide stock solution;
(2) taking 4.667ml of graphene oxide stock solution, adding 9.305ml of pure water, 28 mu L of ammonia water and 12.3mg of L-ascorbic acid;
(3) putting the melamine sponge and the solution into a 20ml hydrothermal reaction kettle together for hydrothermal reaction at 100 ℃ for 50 min;
(4) and taking out the reacted sponge, and drying at 60 ℃ for 18h to obtain the composite sponge capable of absorbing viscous crude oil.
Example 7
(1) Adding 90mg of graphene oxide powder into 30ml of pure water, and performing ultrasonic treatment for 10min by using an ultrasonic cell disruptor under 300W to prepare a 3mg/ml graphene oxide stock solution;
(2) taking 4.667ml of graphene oxide stock solution, adding 9.305ml of pure water, 28 mu L of ammonia water and 12.3mg of L-ascorbic acid;
(3) putting the melamine sponge and the solution into a 20ml hydrothermal reaction kettle together, and carrying out hydrothermal reaction at the temperature of 95 ℃ for 60 min;
(4) and taking out the reacted sponge and drying at 50 ℃ for 24 hours to obtain the composite sponge capable of absorbing viscous crude oil.
Fig. 1 is a scanning electron microscope image of the prepared composite sponge capable of absorbing viscous crude oil, wherein a frame structure is a melamine sponge framework, a film loaded on the framework is reduced graphene, and it can be seen that the reduced graphene oxide is more closely loaded on the melamine sponge framework. Fig. 2 is a digital photograph of the composite sponge capable of absorbing viscous crude oil prepared in the invention, wherein a and B are respectively a comparison graph of the composite sponge before oil absorption and after oil absorption, the original loose and porous composite sponge is filled with crude oil in pores after absorbing viscous crude oil, and the composite sponge can achieve the effect within 5min under illumination. Fig. 3 is an infrared thermograph of the sponge under simulated sunlight irradiation, a and B are respectively an infrared thermograph of a blank melamine sponge and a prepared composite sponge capable of absorbing viscous crude oil, a right rectangular column of the image represents a temperature range, different colors correspond to different temperatures, it can be seen that the blank sponge of the image a has no obvious temperature difference with the surrounding environment under the illumination, and the composite sponge of the image B is rapidly heated to about 80 ℃ under the illumination, is obviously distinguished from the surrounding environment temperature, and embodies good photothermal effect thereof.
The embodiments described above are described to facilitate an understanding and use of the invention by those skilled in the art. It will be readily apparent to those skilled in the art that various modifications to these embodiments may be made, and the generic principles described herein may be applied to other embodiments without the use of the inventive faculty. Therefore, the present invention is not limited to the above embodiments, and those skilled in the art should make improvements and modifications within the scope of the present invention based on the disclosure of the present invention.
Claims (6)
1. The application of the composite sponge capable of absorbing the viscous crude oil is characterized in that the composite sponge is applied to effectively absorb the viscous crude oil on ice-cold sea;
the preparation method of the composite sponge comprises the following steps:
(1) adding graphene oxide powder into pure water to prepare a graphene oxide dispersion liquid;
(2) adding concentrated ammonia water and L-ascorbic acid into the graphene oxide dispersion liquid;
the concentration of the L-ascorbic acid in the graphene oxide dispersion liquid is 0.05mmol/L-2 mmol/L;
(3) putting sponge into the solution to perform hydrothermal reaction; the sponge is melamine sponge;
(4) and taking out the reacted sponge and drying to obtain the composite sponge capable of absorbing viscous crude oil, wherein the melamine sponge framework of the composite sponge is loaded with film-like reduced graphene.
2. The use of the composite sponge capable of absorbing viscous crude oil according to claim 1, wherein the concentration of the graphene oxide dispersion in the step (1) is 0.5mg/mL to 3 mg/mL.
3. The application of the composite sponge capable of absorbing viscous crude oil according to claim 2, wherein the dispersion liquid is subjected to ultrasonic treatment by an ultrasonic cell disruption instrument, wherein the ultrasonic treatment time is 5min to 20min, and the power is 100W to 300W.
4. The application of the composite sponge capable of absorbing viscous crude oil according to claim 1, wherein the concentration of the concentrated ammonia water in the graphene oxide dispersion liquid in the step (2) is 10mmol/L-100 mmol/L.
5. The application of the composite sponge capable of absorbing viscous crude oil according to claim 1, wherein the hydrothermal reaction temperature in the step (3) is 80-100 ℃, and the heating time is 40-120 min.
6. The use of the composite sponge capable of absorbing crude oil in viscous state according to claim 1, wherein the drying temperature in the step (4) is 50-80 ℃ and the drying time is 12-24 h.
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| CN110128696A (en) * | 2019-06-27 | 2019-08-16 | 中素新科技有限公司 | Hydrophobicity graphene oil suction sponge and its preparation method and application |
| CN110183723A (en) * | 2019-06-27 | 2019-08-30 | 中素新科技有限公司 | Graphene-based oil suction sponge and its preparation method and application |
| CN110591144B (en) * | 2019-08-19 | 2022-02-15 | 江苏大学 | Preparation and application of solar-driven self-heating multistage sulfide in-situ growth black sponge |
| CN111138859A (en) * | 2020-01-09 | 2020-05-12 | 合肥工业大学 | Three-dimensional structure nano composite intelligent sponge, preparation method and application |
| CN111229168A (en) * | 2020-02-14 | 2020-06-05 | 上海第二工业大学 | Method for recovering high-viscosity leaked crude oil by using graphene-based material |
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