CN103908947A - Preparation method of magnetic porous carbon/ ferric oxide nano composite material for oil-water separation - Google Patents

Preparation method of magnetic porous carbon/ ferric oxide nano composite material for oil-water separation Download PDF

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CN103908947A
CN103908947A CN201410130580.6A CN201410130580A CN103908947A CN 103908947 A CN103908947 A CN 103908947A CN 201410130580 A CN201410130580 A CN 201410130580A CN 103908947 A CN103908947 A CN 103908947A
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porous carbon
mil
water
ferric oxide
oxide nano
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张娜
赵越
孙玉见
班元浩
杨雁茹
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Shanghai Institute of Technology
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Shanghai Institute of Technology
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Abstract

The invention discloses a preparation method of a magnetic porous carbon/ ferric oxide nano composite material for oil-water separation, wherein the magnetic porous carbon/ ferric oxide nano composite adsorption material for oil-water separation is porous carbon/Fe3O4 magnetic powder or porous carbon/gamma-Fe2O3 magnetic powder. The preparation method comprises the following steps: firstly, preparing a Fe-MIL-101 or Fe-MIL-100 metal-organic framework material of a porous structure by utilizing a hydrothermal method; then controlling the temperature to be 500-700 DEG C at the N2/H2 atmosphere or the vacuum state, and forging for 2-8 hours, thereby obtaining the magnetic porous carbon/ ferric oxide nano composite adsorption material for oil-water separation. The adsorption material can adsorb oil substances in water well; moreover, adsorption materials dispersed into a solution as well as the adsorbed oil materials can be recycled only by magnets; the preparation method is simple to operate, is low in production cost, is good safety performance, and is high in practicability.

Description

The preparation method of magnetic porous carbon/ferric oxide nano composite for a kind of water-oil separating
Technical field
The present invention relates to magnetic porous carbon/ferric oxide nano composite adsorbing material for a kind of water-oil separating, this material has larger specific area, good oleophilic drainage performance, mainly applies profit purifying technique.
Background technology
For solving alarming Leakage, porous carbon materials is because its unique character receives much concern.The pore structure of porous carbon materials is highly developed, has large specific area, consequent excellent absorption property.It is compared and has outstanding advantage with the adsorbent such as clay, perlite and natural zeolite, as: Carbon Materials is hydrophobic adsorbent, in the situation that having water or steam to exist, still can play a role; Material with carbon element is not only applicable to adsorb land leakage, also can be used for adsorbed water body leakage; And during for oil removing waterborne, after absorption, can not sink.Although porous carbon has plurality of advantages, in adsorption capacity, separate complexity, there is limitation in recuperability aspect.Therefore, more high-performance, more multi-selection, more intelligent, multifunctional porous carbon adsorbing material has to be developed.In this respect, Fe 3o 4graphite/carbon has shown to have absorbing dye ability; The oil suction character of the coated magnetic iron ore material with carbon element of hydrophobic silica is report to some extent also.But research is only confined to this.
In addition, the synthetic method of porous carbon materials has a variety of, traditional synthetic method has: (1) chemistry method alive, physical activation method and physical chemistry activation method (2) be carbonization organic aerogel (3) casting mold carbonizatin method under supercritical drying condition with slaine or Catalyzed by Organometallic Compounds activated carbon presoma, (4) hard inorganic template synthesis, these methods are prepared porous carbon materials and are being regulated the aperture of porous carbon, the perforate character of porous carbon, and preparation section more complicated, has affected the actual adsorption capacity of porous carbon.
Metal-organic framework materials in sorbing material (hereinafter to be referred as MOF material) is as a kind of novel porous material, there is the characteristics such as special periodic structure, high-specific surface area, high porosity, high adsorption due to it, shown application prospect widely in power such as absorption, electrochemistry, catalysis.But because the organic-metallic coordination skeleton of itself is easily subject to the impact of external environment, its ordered structure can be caved in, and has greatly limited the application of its water-oil separating in water-oil separating especially seawater.Therefore, metallic organic framework structural material is prepared into material with carbon element, keeps its original orderly porous state, it can be prepared into different porous carbon/oxide materials according to central metal ion difference, further advances its application in absorption, catalysis.
In this patent, take the orderly metal-organic framework materials of the porous of iron content (Fe-MIL-101 or Fe-MIL-100) as raw material, through the synthetic new high-performance porous charcoal/iron oxide magnetic composite of pyrolysis, as high adsorption material recyclable, that realize water-oil separating.In the time there is oily leakage accident on sea, can sprinkle this kind of porous carbon/iron oxide magnetic material with helicopter, then with the electric ship that flat thin magnet is housed is mobile at sea, the sorbing material containing is reclaimed, and by the desorption in later stage organic solvent, sorbing material is separated with oily.Time material self there is certain catalytic capability; Chemical stability and the heat endurance of Carbon Materials are superior.
Summary of the invention
The object of the invention is the technical problem such as adsorption capacity and recuperability in order to solve above-mentioned porous carbon materials preparation section complexity and water-oil separating material and the preparation method of a kind of water-oil separating with magnetic porous carbon/ferric oxide nano composite adsorbing material is provided.
Know-why of the present invention
By the orderly metal-organic framework materials Fe-MIL-101 of the porous of thermal cracking iron content or the prepared compound sorbing material of magnetic porous carbon/ferric oxide nano for water-oil separating of Fe-MIL-100, be performance because it has larger specific area, porous character and stronger oleophilic drainage, the therefore good oily matter in adsorbed water; And because it has certain magnetic, only need the sorbing material compound magnetic porous carbon/ferric oxide nano that be scattered in solution and the oily material adsorbing can be reclaimed by magnet.
Technical scheme of the present invention
A kind of magnetic porous carbon/ferric oxide nano composite adsorbing material for water-oil separating, is porous carbon/Fe 3o 4magnaglo or porous carbon/γ-Fe 2o 3magnaglo.
The preparation method of magnetic porous carbon/ferric oxide nano composite adsorbing material for above-mentioned a kind of water-oil separating, specifically comprises the steps:
First, utilize hydro-thermal method to prepare to have Fe-MIL-101 or the Fe-MIL-100 metal-organic framework materials of loose structure;
Then, it is 2-5 ℃/min that the Fe-MIL-101 with loose structure of gained or Fe-MIL-100 metal-organic framework materials are preferably controlled to programming rate, at N 2/ H 2under atmosphere or vacuum state, be warming up to 500-700 ℃ of calcining 2-8h, obtain porous carbon/Fe 3o 4magnaglo or black porous carbon/γ-Fe 2o 3magnaglo, i.e. magnetic porous carbon/ferric oxide nano composite adsorbing material for water-oil separating.
Useful technique effect of the present invention
Magnetic porous carbon/ferric oxide nano composite adsorbing material for a kind of water-oil separating of the present invention, because it has larger specific area, porous character and stronger oleophilic drainage performance, the therefore good oily matter in adsorbed water.
Further, magnetic porous carbon/ferric oxide nano composite adsorbing material for a kind of water-oil separating of the present invention, because it contains Fe 3o 4or γ-Fe 2o 3, therefore thering is magnetic, therefore only need the sorbing material compound magnetic porous carbon/ferric oxide nano that be scattered in solution and the oily matter adsorbing can be reclaimed by magnet, there is stronger operability and development prospect.
Further, porous carbon/ferric oxide nano composite adsorbing material that a kind of water-oil separating of the present invention is used, because preparation method is simple, easy to operate, prepares cost of material used low, and therefore production cost is low, therefore, is suitable for suitability for industrialized production.
Accompanying drawing explanation
The XRD figure of the Fe-MIL-100 metal-organic framework materials of Fig. 1, embodiment 1 loose structure used;
Gained black porous carbon/γ-Fe in Fig. 2, embodiment 2 2o 3the XRD figure of Magnaglo.
The specific embodiment
Also by reference to the accompanying drawings the present invention is further set forth below by specific embodiment, but do not limit the present invention.
Utilize hydro-thermal method preparation to have the Fe-MIL-101 metal-organic framework materials of loose structure, concrete steps are as follows:
According to FeCl 36H 2o: terephthalic acid (TPA): the ratio that the mol ratio of DMF is 1:2.6:200, by FeCl 36H 2o and terephthalic acid (TPA) ultrasonic dissolution are at N, in dinethylformamide, then transfer in reactor and seal, controlling temperature is 150 ℃ of reaction 15h, the pure N of the crystal obtaining, after dinethylformamide cyclic washing 3 times, vacuum drying at 80 ℃, obtains Fe-MIL-101 metal-organic framework materials;
The Fe-MIL-100 metal-organic framework materials that utilizes hydro-thermal method to prepare to have loose structure, concrete steps are as follows:
According to iron powder: trimesic acid: hydrofluoric acid: nitric acid: the ratio that the mol ratio of water is 1:0.66:2:0.56:300 weighs, first iron powder is dissolved in to hydrofluoric acid, stirring reaction, dropwise add again nitric acid, then add water, ultrasonic oscillation to iron powder is dissolved in water completely, finally add trimesic acid to obtain suspension, then transfer in reactor and seal, controlling temperature is 160 ℃ of reaction 14h, the crystal obtaining is with after ethanol cyclic washing 3 times, and vacuum drying at 100 ℃, obtains Fe-MIL-100 metal-organic framework materials.
Embodiment 1
A kind of magnetic porous carbon/ferric oxide nano composite adsorbing material for water-oil separating, is porous carbon/Fe 3o 4powder.
The preparation method of magnetic porous carbon/ferric oxide nano composite adsorbing material for above-mentioned a kind of water-oil separating, specifically comprises the steps:
First, utilize hydro-thermal method to prepare to have the Fe-MIL-101 metal-organic framework materials of loose structure;
Then be, 5 ℃/min by the Fe-MIL-101 metal-organic framework materials control programming rate with loose structure of gained, at H 2: N 2flow is under 4%:96% condition, is warming up to 600 ℃, and calcining 6h, obtains porous carbon/Fe 3o 4magnaglo, i.e. magnetic porous carbon/ferric oxide nano composite adsorbing material for water-oil separating.
Above-mentioned presoma Fe-MIL-101 used scans through Rigaku Rigaku D/max 2000/PC type X-ray diffractometer, the XRD of gained schemes as shown in Figure 1, as can be seen from Figure 1 0-10 ° of low-angle has stronger diffraction maximum, especially go out peak at 2.5 ° of low-angles, illustrate and synthesized the metal-organic framework structural material Fe-MIL-101 with porous ordered structure.
Porous carbon/the Fe of above-mentioned gained 3o 4magnaglo, through Kang Ta company of the U.S., Autosorb-1 carries out BET detection, and its specific area is 231m 2/ g.
Porous carbon/the Fe of above-mentioned gained 3o 4magnaglo, through Kang Ta company of the U.S., Autosorb-1 detects, and carries out pore-size distribution detection, contains the mesopore that is about 1.8nm.
Porous carbon/the Fe of above-mentioned gained 3o 4magnaglo, detects through the promise SL200KB of section of U.S. contact angle analyzer, with the contact angle of water be 135 °, illustrate that it has stronger oleophylic, hydrophobic performance.
Embodiment 2
A kind of magnetic porous carbon/ferric oxide nano composite adsorbing material for water-oil separating, is porous carbon/γ-Fe 2o 3powder.
The preparation method of magnetic porous carbon/ferric oxide nano composite adsorbing material for above-mentioned a kind of water-oil separating, specifically comprises the steps:
First, utilize hydro-thermal method to prepare to have the Fe-MIL-100 metal-organic framework materials of loose structure;
Then, be 2.5 ℃/min by the Fe-MIL-100 metal-organic framework materials control programming rate with loose structure of gained, under vacuum state, through 500 ℃ of calcining 8h, obtain black porous carbon/γ-Fe 2o 3powder, i.e. magnetic porous carbon/ferric oxide nano composite adsorbing material for water-oil separating.
Above-mentioned gained black porous carbon/γ-Fe 2o 3magnaglo is that the magnetic porous carbon/ferric oxide nano composite adsorbing material of water-oil separating scans through Rigaku Rigaku D/max 2000/PC type X-ray diffractometer, the XRD of gained schemes as shown in Figure 2, as can be seen from Figure 2 Fe-MIL-100 metallic organic framework structure disappears, there is diffraction maximum in high angle, belong to γ-Fe 2o 3with the diffraction maximum of C, illustrate and prepared porous carbon/γ-Fe 2o 3magnaglo, i.e. magnetic porous carbon/ferric oxide nano composite adsorbing material for water-oil separating.
Porous carbon/γ-the Fe of above-mentioned gained 2o 3magnaglo, through Kang Ta company of the U.S., Autosorb-1 carries out BET detection, and its specific area is 401m 2/ g.
Porous carbon/γ-the Fe of above-mentioned gained 2o 3magnaglo, through Kang Ta company of the U.S., Autosorb-1 detects, and carries out pore-size distribution detection, contains the aperture that is about 0.8nm.
Porous carbon/γ-the Fe of above-mentioned gained 2o 3magnaglo, detects through the promise SL200KB of section of U.S. contact angle analyzer, with the contact angle of water be 143 °, illustrate that it has stronger oleophylic, hydrophobic performance.
Embodiment 3
A kind of magnetic porous carbon/ferric oxide nano composite adsorbing material for water-oil separating, is porous carbon/Fe 3o 4powder.
The preparation method of magnetic porous carbon/ferric oxide nano composite adsorbing material for above-mentioned a kind of water-oil separating, specifically comprises the steps:
First, utilize hydro-thermal method to prepare to have the Fe-MIL-100 metal-organic framework materials of loose structure;
Then be, 2 ℃/min by the Fe-MIL-100 metal-organic framework materials control programming rate with loose structure of gained, at H 2: N 2flow is under 4%:96% condition, is warming up to 500 ℃, and calcining 4h, obtains porous carbon/Fe 3o 4magnaglo, i.e. magnetic porous carbon/ferric oxide nano composite adsorbing material for water-oil separating.
Porous carbon/the Fe of above-mentioned gained 3o 4magnaglo, through Kang Ta company of the U.S., Autosorb-1 carries out BET detection, and its specific area is 422m 2/ g.
Porous carbon/the Fe of above-mentioned gained 3o 4magnaglo, through Kang Ta company of the U.S., Autosorb-1 detects, and carries out pore-size distribution detection, contains the aperture that is about 0.8nm.
Porous carbon/the Fe of above-mentioned gained 3o 4magnaglo, detects through the promise SL200KB of section of U.S. contact angle analyzer, with the contact angle of water be 142 °, illustrate that it has stronger oleophylic, hydrophobic performance.
Embodiment 4
A kind of magnetic porous carbon/ferric oxide nano composite adsorbing material for water-oil separating, is porous carbon/γ-Fe 2o 3powder.
The preparation method of magnetic porous carbon/ferric oxide nano composite adsorbing material for above-mentioned a kind of water-oil separating, specifically comprises the steps:
First, utilize hydro-thermal method to prepare to have the Fe-MIL-101 metal-organic framework materials of loose structure;
Then, be 2.5 ℃/min by the Fe-MIL-101 metal-organic framework materials control programming rate with loose structure of gained, under vacuum state, through 700 ℃ of calcining 2h, obtain black porous carbon/γ-Fe 2o 3powder, i.e. magnetic porous carbon/ferric oxide nano composite adsorbing material for water-oil separating.
Porous carbon/γ-the Fe of above-mentioned gained 2o 3magnaglo, through Kang Ta company of the U.S., Autosorb-1 carries out BET detection, and its specific area is 202m 2/ g.
Porous carbon/γ-the Fe of above-mentioned gained 2o 3magnaglo, through Kang Ta company of the U.S., Autosorb-1 detects, and carries out pore-size distribution detection, contains the mesopore that diameter is about 2.1nm.
Porous carbon/γ-the Fe of above-mentioned gained 2o 3magnaglo, detects through the promise SL200KB of section of U.S. contact angle analyzer, with the contact angle of water be 127 °, illustrate that it has stronger oleophylic, hydrophobic performance.
Can find out magnetic porous carbon/ferric oxide nano composite adsorbing material for a kind of water-oil separating of the present invention, i.e. porous carbon/γ-Fe by the above embodiments 1-4 2o 3magnaglo or porous carbon/Fe 3o 4magnaglo, has large specific area, wherein porous carbon/γ-Fe 2o 3the specific area of Magnaglo can reach 202-422m 2/ g, porous carbon/Fe 3o 4the specific area of Magnaglo can reach 231-401m 2/ g;
Further can find out magnetic porous carbon/ferric oxide nano composite adsorbing material for a kind of water-oil separating of the present invention, i.e. porous carbon/γ-Fe 2o 3magnaglo or porous carbon/Fe 3o 4magnaglo has loose structure, wherein porous carbon/γ-Fe 2o 3the aperture of Magnaglo is 0.8-2.1nm, porous carbon/Fe 3o 4the aperture of Magnaglo is 0.8-1.8nm;
Further can find out magnetic porous carbon/ferric oxide nano composite adsorbing material for a kind of water-oil separating of the present invention, i.e. porous carbon/γ-Fe 2o 3magnaglo or porous carbon/Fe 3o 4magnaglo, with the contact angle of water, wherein porous carbon/γ-Fe 2o 3magnetic powder is 127-143 °, porous carbon/Fe 3o 4magnaglo is 135-142 °, therefore has stronger oleophylic, hydrophobic performance.
In sum, magnetic porous carbon/ferric oxide nano composite adsorbing material for a kind of water-oil separating of the present invention, i.e. porous carbon/γ-Fe 2o 3magnaglo or porous carbon/Fe 3o 4magnaglo is because its larger specific area, porous character and stronger oleophilic drainage are performance, therefore the good oily matter in adsorbed water.
Further, magnetic porous carbon/ferric oxide nano composite adsorbing material for a kind of water-oil separating of the present invention, i.e. porous carbon/γ-Fe 2o 3magnaglo or porous carbon/Fe 3o 4magnaglo, due to γ-Fe 2o 3, Fe 3o 4existence, make porous carbon/γ-Fe 2o 3magnaglo or porous carbon/Fe 3o 4magnaglo has higher magnetic, can this kind of water-oil separating material recovery be recycled by magnetic, realizes the reusing of material, sustainable development.
Above said content is only the basic explanation of the present invention under conceiving, and according to any equivalent transformation that technical scheme of the present invention is done, all should belong to protection scope of the present invention.

Claims (3)

1. magnetic porous carbon/ferric oxide nano composite adsorbing material for water-oil separating, is characterized in that the described magnetic porous carbon/ferric oxide nano composite adsorbing material of water-oil separating is porous carbon/Fe 3o 4magnaglo or porous carbon/γ-Fe 2o 3magnaglo, its method preparation as follows:
First, utilize hydro-thermal method to prepare to have Fe-MIL-101 or the Fe-MIL-100 metal-organic framework materials of loose structure;
Then, by the Fe-MIL-101 with loose structure of gained or Fe-MIL-100 metal-organic framework materials at N 2/ H 2under atmosphere or vacuum state, controlling temperature is 500-700 ℃ of calcining 2-8h, obtains porous carbon/Fe 3o 4magnaglo or porous carbon/γ-Fe 2o 3magnaglo, i.e. magnetic porous carbon/ferric oxide nano composite adsorbing material for magnetic water-oil separating.
2. magnetic porous carbon/ferric oxide nano composite adsorbing material for a kind of water-oil separating as claimed in claim 1, it is characterized in that by the Fe-MIL-101 with loose structure of gained or Fe-MIL-100 metal-organic framework materials control programming rate be 2-5 ℃/min, at N 2/ H 2under atmosphere or vacuum state, be warming up to 500-700 ℃.
3. magnetic porous carbon/ferric oxide nano composite adsorbing material for a kind of water-oil separating as claimed in claim 1 or 2, is characterized in that the described Fe-MIL-101 metal-organic framework materials that utilizes hydro-thermal method to prepare to have loose structure, and concrete steps are as follows:
According to FeCl 36H 2o: terephthalic acid (TPA): the ratio that the mol ratio of DMF is 1:2.6:200, by FeCl 36H 2o and terephthalic acid (TPA) ultrasonic dissolution are at N, in dinethylformamide, then transfer in reactor and seal, controlling temperature is 150 ℃ of reaction 15h, the pure N of the crystal obtaining, after dinethylformamide cyclic washing 3 times, vacuum drying at 80 ℃, obtains Fe-MIL-101 metal-organic framework materials;
The described Fe-MIL-100 metal-organic framework materials that utilizes hydro-thermal method to prepare to have loose structure, concrete steps are as follows:
According to iron powder: trimesic acid: hydrofluoric acid: nitric acid: the ratio that the mol ratio of water is 1:0.66:2:0.56:300 weighs, first iron powder is dissolved in to hydrofluoric acid, stirring reaction, dropwise add again nitric acid, then add water, ultrasonic oscillation to iron powder is dissolved in water completely, finally add trimesic acid to obtain suspension, then transfer in reactor and seal, controlling temperature is 160 ℃ of reaction 14h, the crystal obtaining is with after ethanol cyclic washing 3 times, and vacuum drying at 100 ℃, obtains Fe-MIL-100 metal-organic framework materials.
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