CN109621906A - A method of preparing the composite sponge for caning absorb sticky state crude oil - Google Patents
A method of preparing the composite sponge for caning absorb sticky state crude oil Download PDFInfo
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- CN109621906A CN109621906A CN201811536600.4A CN201811536600A CN109621906A CN 109621906 A CN109621906 A CN 109621906A CN 201811536600 A CN201811536600 A CN 201811536600A CN 109621906 A CN109621906 A CN 109621906A
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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
- B01J20/02—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
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- Life Sciences & Earth Sciences (AREA)
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- Engineering & Computer Science (AREA)
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Abstract
The present invention relates to a kind of method for preparing and caning absorb the composite sponge of sticky state crude oil, restored by graphene oxide and be loaded on melamine sponge be made, using following steps: (1) prepare graphene oxide dispersion；(2) certain density ammonium hydroxide, L-AA are added in graphene oxide dispersion；(3) sponge is put into above-mentioned solution, carries out hydro-thermal reaction；(4) composite sponge after reaction is taken out into drying to get the compound melamine sponge of graphene has been arrived.Preparation method is simple by the present invention, reproducible, does not generate secondary pollution, and melamine sponge commercialized degree is high, cheap, and obtained composite sponge being capable of sticky state crude oil in quick adsorption water.
Description
Technical field
The present invention relates to a kind of oil absorptive function material, the compounding sea of sticky state crude oil is can absorb more particularly, to a kind of prepare
Continuous method.
Background technique
With the development of petroleum industry, every year because oil field, conveying pipe oil spilling or pleasure boat accident have a large amount of petroleum streams
Enter ocean, serious pollution is caused to water body and coastal environment.For this large area viscous crude oil it is quick removal and it is secondary
The advanced treating of organic pollutant is extremely important but could not effectively be solved always a problem.
The characteristics of swimming in the water surface and neighbouring depth in view of oil pollutant, realized with float type oily waste degradation material compared with
Fast oily waste treatment and easily recycling are more satisfactory selections.
Graphene is as a kind of two-dimension nano materials, since 2004 are found, just with its great specific surface area, height
The superior physical and chemical performance such as thermal conductivity, high conductivity, high intensity, high-modulus becomes the hot spot of each area research.Graphene
Hydrophobic oleophilic oil, therefore be not easy to be dispersed in water phase；Its oxide morphology --- graphene oxide is then hydrophilic and oleophobic, is easy to divide
It is dispersed in water phase.Therefore the graphite of hydrophobic oleophilic oil is prepared often by way of restoring to graphene oxide dispersion at present
Alkene.On the other hand, the viscosity with temperature of crude oil is increased and is gradually decreased, and the crude oil on ice-cold sea causes because viscosity is higher
Its adsorption effect is very poor, only allows oil absorption material fever that viscosity of crude is caused to reduce, is just able to achieve to the effective of sticky state crude oil
It absorbs.Ge et al., using the sponge for being enclosed with graphene as float type oily waste treatment material, passes through graphene using above-mentioned principle
Electrocaloric effect reduce viscosity of crude to substantially increasing the crude oil rate of adsorption.But in view of this device needs work materials logical
Electric heating up oil suction later, applying in water body will be present security risk or is easy to fail.Preparation method selects hydrogen iodine simultaneously
Acid restores graphene oxide, and hydroiodic acid corrosivity is extremely strong, has strong impulse effect to human body, not a kind of safety collar
The method of guarantor.
Summary of the invention
It is an object of the present invention to overcome the above-mentioned drawbacks of the prior art and provide a kind of safe green can
The preparation method for absorbing the composite sponge of sticky state crude oil, can make prepared composite sponge oleophilic drainage, high porosity and
With preferable photo-thermal effect.
The purpose of the present invention can be achieved through the following technical solutions:
A method of the composite sponge for caning absorb sticky state crude oil is prepared, using following steps:
(1) graphene oxide powder is added in pure water, prepares graphene oxide dispersion；
(2) concentrated ammonia liquor, L-AA are added in graphene oxide dispersion, by the way that L-AA is added, no
It is only capable of playing the role of graphene oxide being reduced to redox graphene, graphene and sponge can also be made to form water-setting
Glue is supported on sponge securely；
(3) melamine sponge is put into above-mentioned solution, carries out hydro-thermal reaction；
(4) sponge after reaction is taken out dry to get to the composite sponge for caning absorb sticky state crude oil.
The concentration of graphene oxide dispersion described in step (1) is 0.5mg/ml-3mg/ml.If graphene oxide point
The concentration of dispersion liquid is too low, not obvious enough to the modification of sponge；If excessive concentration, the porosity of sponge is reduced, cost is excessively high.
The method provided according to the present invention carries out ultrasound to dispersion liquid using ultrasonic cell disruption instrument, and ultrasonic time is
5min-20min, instrument power 100W-300W.
The method provided according to the present invention, the concentration of concentrated ammonia liquor described in step (2) are 10mmol/L-100mmol/L,
The concentration of L-AA is 0.05mmol/L-2mmol/L.The effect of concentrated ammonia liquor is to make graphene oxide by electrostatic repulsion
More easily disperse, but excessive concentration is then unfavorable for the stability of liquid.The effect of L-AA is to restore graphene oxide
At the graphene of reduction-state, and graphene and sponge is made to form hydrogel, keeps Load Balanced secured, but excessive concentration, then can lead
The polycondensation of graphene composite sponge is caused, its performance is affected.
The method provided according to the present invention, hydrothermal temperature described in step (3) are 80 DEG C -100 DEG C, heating time
It is 40min-120min.Hydro-thermal reaction can provide the environment of high temperature and pressure, restore graphene oxide, if temperature is excessively high, the time
It is too long, sponge structure on the one hand can be destroyed, is on the other hand also runed counter to reduction energy consumption.
The method provided according to the present invention, drying temperature described in step (4) are 50 DEG C -80 DEG C, and drying time is
12h-24h。
The present invention is dispersed in water phase using graphene oxide as presoma, by graphene oxide, can be real by hydro-thermal reaction
Show the reduction of graphene oxide and be loaded to melamine sponge, only needs to adjust adding for L-AA in the process
Amount, i.e., the reducing degree of controllable graphene oxide and the load capacity for the graphene for being loaded to sponge.
Compared with prior art, the invention has the following advantages that
(1) obtained by the present invention composite sponge is loose porous, large specific surface area, density are low, can be used as oils adsorption material
Material, has widened its application prospect；
(2) the present invention can control the reducing degree of graphene oxide and born by the dosage of adjusting L-AA
It is loaded onto the load capacity of the graphene of sponge, preparation process is simple, safe, easily operated, does not generate secondary pollution, manufacturing cycle
It is short；
(3) the supporting substrate object selected by the present invention --- melamine sponge commercialized degree is high, low in cost, to ring
Border does not generate secondary pollution, application easy to spread.
Detailed description of the invention
Fig. 1 is the scanning electron microscope (SEM) photograph of the composite sponge for caning absorb sticky state crude oil of preparation；
The digital photograph of the composite sponge for caning absorb sticky state crude oil prepared in Fig. 2 present invention, A and B are respectively sponge
Comparative diagram before oil suction and after oil suction；
Fig. 3 is Infrared Thermogram of the sponge under simulated solar irradiation irradiation in the present invention, and A and B are respectively blank melamine
The Infrared Thermogram of the composite sponge for caning absorb sticky state crude oil of amine sponge and preparation.
Specific embodiment
The present invention is described in detail combined with specific embodiments below.Following embodiment will be helpful to the technology of this field
Personnel further understand the present invention, but the invention is not limited in any way.It should be pointed out that the ordinary skill of this field
For personnel, without departing from the inventive concept of the premise, various modifications and improvements can be made.These belong to the present invention
Protection scope.
A method of the composite sponge for caning absorb sticky state crude oil is prepared, using following steps:
(1) graphene oxide powder is added in pure water, it is 0.5mg/ml-3mg/ml graphite oxide that concentration, which is prepared,
Alkene dispersion liquid, while ultrasonic treatment 5min-20min can also be carried out to dispersion liquid using ultrasonic cell disruption instrument, it is ultrasonic
Power control is 100W-300W；
(2) concentrated ammonia liquor, L-AA are added in graphene oxide dispersion, concentrated ammonia liquor disperses in graphene oxide
Concentration in liquid is 10mmol/L-100mmol/L, and concentration of the L-AA in graphene oxide dispersion is
0.05mmol/L-2mmol/L is added L-AA, can not only play graphene oxide being reduced to redox graphene
Effect, graphene and sponge can also be made to form hydrogel, be supported on sponge securely, the dosage meeting of L-AA
Influence the amount of the graphene finally loaded on sponge.To a certain extent, L-AA dosage is more, loads on sponge
Graphene is also more；
(3) melamine sponge to be put into above-mentioned solution, carries out hydro-thermal reaction, reaction temperature is 80 DEG C -100 DEG C,
Heating time is 40min-120min；
(4) sponge after reaction is taken out, dry 12h-24h is under conditions of 50 DEG C -80 DEG C to get sticky to caning absorb
The composite sponge of state crude oil.
More detailed case study on implementation below, by following case study on implementation further illustrate technical solution of the present invention with
And the technical effect that can be obtained.
Embodiment 1
(1) 90mg graphene oxide powder is added in 30ml pure water, uses ultrasonic cell disruption instrument 300W ultrasound
The graphene oxide stock solution of 3mg/ml is prepared in 10min；
(2) 4.667ml graphene oxide stock solution is taken, it is anti-that 9.305ml pure water, 28 μ L ammonium hydroxide and 12.3mg L- is added
Bad hematic acid；
(3) melamine sponge is put into 20ml hydrothermal reaction kettle together with above-mentioned solution, carries out hydro-thermal reaction, hydro-thermal
Reaction temperature is 95 DEG C, time 60min；
(4) sponge after reaction is taken out into drying, drying temperature is 60 DEG C, and the time is 18h to get to caning absorb sticky state
The composite sponge of crude oil.
Embodiment 2
(1) 90mg graphene oxide powder is added in 30ml pure water, uses ultrasonic cell disruption instrument 100W ultrasound
The graphene oxide stock solution of 3mg/ml is prepared in 30min；
(2) 4.667ml graphene oxide stock solution is taken, it is anti-that 9.305ml pure water, 28 μ L ammonium hydroxide and 12.3mg L- is added
Bad hematic acid；
(3) melamine sponge is put into 20ml hydrothermal reaction kettle together with above-mentioned solution, carries out hydro-thermal reaction, hydro-thermal
Reaction temperature is 95 DEG C, time 60min；
(4) sponge after reaction is taken out into drying, drying temperature is 60 DEG C, and the time is 18h to get to caning absorb sticky state
The composite sponge of crude oil.
Embodiment 3
(1) 90mg graphene oxide powder is added in 30ml pure water, uses ultrasonic cell disruption instrument 300W ultrasound
The graphene oxide stock solution of 3mg/ml is prepared in 10min；
(2) 9.333ml graphene oxide stock solution is taken, it is anti-that 4.639ml pure water, 28 μ L ammonium hydroxide and 12.3mg L- is added
Bad hematic acid；
(3) melamine sponge is put into 20ml hydrothermal reaction kettle together with above-mentioned solution, carries out hydro-thermal reaction, hydro-thermal
Reaction temperature is 95 DEG C, time 60min；
(4) sponge after reaction is taken out into drying, drying temperature is 60 DEG C, and the time is 18h to get to caning absorb sticky state
The composite sponge of crude oil.
Embodiment 4
(1) 90mg graphene oxide powder is added in 30ml pure water, uses ultrasonic cell disruption instrument 300W ultrasound
The graphene oxide stock solution of 3mg/ml is prepared in 10min；
(2) 4.667ml graphene oxide stock solution is taken, it is anti-that 9.277ml pure water, 56 μ L ammonium hydroxide and 12.3mg L- is added
Bad hematic acid；
(3) melamine sponge is put into 20ml hydrothermal reaction kettle together with above-mentioned solution, carries out hydro-thermal reaction, hydro-thermal
Reaction temperature is 95 DEG C, time 60min；
(4) sponge after reaction is taken out into drying, drying temperature is 60 DEG C, and the time is 18h to get to caning absorb sticky state
The composite sponge of crude oil.
Embodiment 5
(1) 90mg graphene oxide powder is added in 30ml pure water, uses ultrasonic cell disruption instrument 300W ultrasound
The graphene oxide stock solution of 3mg/ml is prepared in 10min；
(2) 4.667ml graphene oxide stock solution is taken, it is anti-that 9.305ml pure water, 28 μ L ammonium hydroxide and 24.7mg L- is added
Bad hematic acid；
(3) melamine sponge is put into 20ml hydrothermal reaction kettle together with above-mentioned solution, carries out hydro-thermal reaction, hydro-thermal
Reaction temperature is 95 DEG C, time 60min；
(4) sponge after reaction is taken out into drying, drying temperature is 60 DEG C, and the time is 18h to get to caning absorb sticky state
The composite sponge of crude oil.
Embodiment 6
(1) 90mg graphene oxide powder is added in 30ml pure water, uses ultrasonic cell disruption instrument 300W ultrasound
The graphene oxide stock solution of 3mg/ml is prepared in 10min；
(2) 4.667ml graphene oxide stock solution is taken, it is anti-that 9.305ml pure water, 28 μ L ammonium hydroxide and 12.3mg L- is added
Bad hematic acid；
(3) melamine sponge is put into 20ml hydrothermal reaction kettle together with above-mentioned solution, carries out hydro-thermal reaction, hydro-thermal
Reaction temperature is 100 DEG C, time 50min；
(4) sponge after reaction is taken out into drying, drying temperature is 60 DEG C, and the time is 18h to get to caning absorb sticky state
The composite sponge of crude oil.
Embodiment 7
(1) 90mg graphene oxide powder is added in 30ml pure water, uses ultrasonic cell disruption instrument 300W ultrasound
The graphene oxide stock solution of 3mg/ml is prepared in 10min；
(2) 4.667ml graphene oxide stock solution is taken, it is anti-that 9.305ml pure water, 28 μ L ammonium hydroxide and 12.3mg L- is added
Bad hematic acid；
(3) melamine sponge is put into 20ml hydrothermal reaction kettle together with above-mentioned solution, carries out hydro-thermal reaction, hydro-thermal
Reaction temperature is 95 DEG C, time 60min；
(4) sponge after reaction is taken out into drying, drying temperature is 50 DEG C, and the time is for 24 hours to get to caning absorb sticky state
The composite sponge of crude oil.
Fig. 1 is the scanning electron microscope (SEM) photograph of the composite sponge for caning absorb sticky state crude oil of preparation, and figure middle frame structure is three
Poly cyanamid sponge skeleton, the film loaded on skeleton are the graphene of reduction, it can be seen that redox graphene is more close
Ground is loaded on melamine sponge skeleton.Fig. 2 is the number of the composite sponge for caning absorb sticky state crude oil prepared in the present invention
Code photo, A and B are respectively comparative diagram of the composite sponge before oil suction and after oil suction, and originally loose porous composite sponge is being inhaled
It receives and is filled up by crude oil in hole after sticky state crude oil, composite sponge can reach this effect in 5min under light illumination.Fig. 3 is this
Infrared Thermogram of the sponge under simulated solar irradiation irradiation in invention, A and B be respectively blank melamine sponge and preparation can
The Infrared Thermogram of the composite sponge of sticky state crude oil is absorbed, picture right rectangular column represents temperature range, different colours pair
Answer different temperatures, it can be seen that there is no apparent temperature to distinguish with ambient enviroment under light illumination for A figure blank sponge, and B figure is multiple
It closes sponge to be rapidly heated under light illumination to 80 DEG C or so, is distinguished obviously with ambient temperature, embody its good photo-thermal effect.
The above description of the embodiments is intended to facilitate ordinary skill in the art to understand and use the invention.
Person skilled in the art obviously easily can make various modifications to these embodiments, and described herein general
Principle is applied in other embodiments without having to go through creative labor.Therefore, the present invention is not limited to the above embodiments, ability
Field technique personnel announcement according to the present invention, improvement and modification made without departing from the scope of the present invention all should be of the invention
Within protection scope.
Claims (8)
1. a kind of prepare the method for caning absorb the composite sponge of sticky state crude oil, which is characterized in that this method uses following steps:
(1) graphene oxide powder is added in pure water, prepares graphene oxide dispersion；
(2) concentrated ammonia liquor, L-AA are added in graphene oxide dispersion；
(3) sponge is put into above-mentioned solution, carries out hydro-thermal reaction；
(4) sponge after reaction is taken out dry to get to the composite sponge for caning absorb sticky state crude oil.
2. a kind of the method for caning absorb the composite sponge of sticky state crude oil is prepared according to claim 1, which is characterized in that
The concentration of graphene oxide dispersion described in step (1) is 0.5mg/ml-3mg/ml.
3. a kind of the method for caning absorb the composite sponge of sticky state crude oil is prepared according to claim 2, which is characterized in that
Also dispersion liquid is ultrasonically treated using ultrasonic cell disruption instrument, ultrasonic time 5min-20min, power 100W-
300W。
4. a kind of the method for caning absorb the composite sponge of sticky state crude oil is prepared according to claim 1, which is characterized in that
Concentration of the concentrated ammonia liquor in graphene oxide dispersion described in step (2) is 10mmol/L-100mmol/L.
5. a kind of the method for caning absorb the composite sponge of sticky state crude oil is prepared according to claim 1, which is characterized in that
Concentration of the L-AA in graphene oxide dispersion described in step (2) is 0.05mmol/L-2mmol/L.
6. a kind of the method for caning absorb the composite sponge of sticky state crude oil is prepared according to claim 1, which is characterized in that
Hydrothermal temperature described in step (3) is 80 DEG C -100 DEG C, and heating time is 40min-120min.
7. a kind of the method for caning absorb the composite sponge of sticky state crude oil is prepared according to claim 1, which is characterized in that
Dry temperature described in step (4) is 50 DEG C -80 DEG C, time 12h-24h.
8. a kind of the method for caning absorb the composite sponge of sticky state crude oil is prepared according to claim 1, which is characterized in that
The sponge is melamine sponge.
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| CN110591144A (en) * | 2019-08-19 | 2019-12-20 | 江苏大学 | Preparation and application of solar-driven self-heating multistage sulfide in-situ growth black sponge |
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| 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 |
| CN110591144A (en) * | 2019-08-19 | 2019-12-20 | 江苏大学 | Preparation and application of solar-driven self-heating multistage sulfide in-situ growth black sponge |
| 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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