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Journal of Industrial and Engineering Chemistry xxx (2017) xxx–xxx

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Journal of Industrial and Engineering Chemistry


journal homepage: www.elsevier.com/locate/jiec

Fabrication of hydrophobic and oleophilic polyurethane foam sponge


modified with hydrophobic Al2O3 for oil/water separation
Liying Konga , Yang Lia , Fengxian Qiua,* , Tao Zhanga , Qing Guoa , Xiaoying Zhanga ,
Dongya Yanga , Jicheng Xua,b , Mengwei Xuec
a
School of Chemistry and Chemical Engineering, Jiangsu University, Zhenjiang, 212013, China
b
Institute of Chemical and Materials Engineering, Zhenjiang College, Zhenjiang 212003, China
c
School of Environmental Science, Nanjing Xiaozhuang University, Nanjing 211171, China

A R T I C L E I N F O A B S T R A C T

Article history:
Received 27 August 2016 In current work, hydrophobic and oleophilic polyurethane (Al2O3/PUF) foam sponge was prepared by
Received in revised form 23 July 2017 foaming technology. The material was characterized by XRD, TEM, BET, SEM and water contact angles
Accepted 28 September 2017 (CA). The Al2O3/PUF was applied to removal of oil or organic solvent from oil/water system. Water contact
Available online xxx angle of Al2O3/PUF could exceed 140 . The absorption capacity of Al2O3/PUF could be obtained 37 g/g and
found to be reusable up to 10 cycles while maintaining its high absorption capacity. The result indicated
Keywords: that prepared foam sponge has good potential application in oil–water separation.
Polyurethane © 2017 Published by Elsevier B.V. on behalf of The Korean Society of Industrial and Engineering
Hydrophobic Al2O3
Chemistry.
Foam sponge
Oil absorption

Introduction oxide–silica, nanostructured porous silicon and so on) [17].


Polyurethane (PU) in the form of foam possessed a large specific
Crude oil spills, the petrochemical and metallurgical indus- area and enough space for absorption. Davis et al. demonstrated a
tries, pharmaceutical factories and toxic organic solvents have method to reduce the surface roughness of a spray-casted
caused serious environmental pollution on a global scale [1]. It polyurethane/silica/fluoroacrylic superhydrophobic nanocompo-
is extremely urgent and important to develop effective and site coating. By changing the main slurry carrier fluid, fluoropol-
inexpensive materials that can remove oils or organic solvents ymer medium, surface pretreatment, and spray parameters, the
from water [2,3]. Some cleanup techniques for oil spills and arithmetic surface roughness values of 8.7, 2.7, and 1.6 mm on three
organic solvents including in situ burning, chemical dispersion, test surfaces were achieved. All the superhydrophobic surfaces
oil skimming and physical absorption can be found in the showed lower ice adhesion than that of the polished aluminum
previous works [4,5]. Due to the simplicity and efficacy of surface [18]. Steele et al. investigated substrate adhesion for
physical absorption, it becomes a widely appreciated method to superhydrophobic coatings fabricated from Moisture-cured poly-
remove oil spills and organic solvents. Oil and solvents urethanes (MCPUs) modified with waterborne perfluoroalkyl
absorption requires cheap, reliable, environmentally friendly methacrylic copolymer (PMC) and a fatty amine/amino-silane
absorbents with high oil absorption capacity, oil/water surface modified montmorillonite clay nanofiller (organoclay)
selectivity and reusability [6,7]. [19]. Polyurethane foam (PUF) is an efficient absorbent for oil or
Recently, several efforts have been made to develop synthetic organic molecule, which exhibits a range of valuable application
organic sorbents with low cost, high oil absorption capacity and properties such as low apparent density, good mechanical
good oil–water selectiveness, such as organic polymer [8], properties, high weather ability and low thermal conductivity
inorganic nanowire membranes [9], macroporous nanocomposites [20]. Li et al. reported that PU cubes were modified by grafting
[10], carbon nanotubes [11], Iranian activated bentonite [12], polymerization with oleophilic monomer lauryl methacrilate
inorganic metal oxide [13–15], biological structure carbon [16] and (LMA) in solvent and coating with LMA microspheres [21].
silica particles (such as nanosilica, microsphere silica, graphene Calcagnile et al. presented a novel composite material based on
commercially available polyurethane foams (PUF) functionalized
with colloidal superparamagnetic iron oxide nanoparticles and
submicrometer polytetrafluoroethylene (PTFE) particles, which
* Corresponding author.
E-mail address: fxqiuchem@163.com (F. Qiu).
can efficiently separate oil from water. Untreated foam surfaces are

https://doi.org/10.1016/j.jiec.2017.09.050
1226-086X/© 2017 Published by Elsevier B.V. on behalf of The Korean Society of Industrial and Engineering Chemistry.

Please cite this article in press as: L. Kong, et al., Fabrication of hydrophobic and oleophilic polyurethane foam sponge modified with
hydrophobic Al2O3 for oil/water separation, J. Ind. Eng. Chem. (2017), https://doi.org/10.1016/j.jiec.2017.09.050
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2 L. Kong et al. / Journal of Industrial and Engineering Chemistry xxx (2017) xxx–xxx

inherently hydrophobic and oleophobic, but they can be rendered whereas when they get modified, they become hydrophobic and
water-repellent and oil-absorbing by a solvent-free, electrostatic oleophilic, exhibiting water-repellent and oil-absorbing behavior
polytetrafluoroethylene particle deposition technique. It was [30]. The products were characterized with X-ray powder
found that combined functionalization of the PTFE-treated foam diffraction (XRD), transmission electron microscopy (TEM),
surfaces with colloidal iron oxide nanoparticles significantly Brunauer–Emmett–Teller (BET), scanning electron microscopy
increases the speed of oil absorption [22]. Moreover, the PUF is (SEM), water contact angles (WCA) and fourier transform infrared
a porous and a hydrophilic polymer with the characteristics of low spectroscopy (FT-IR). Furthermore, the process of oil absorption
cost, high absorption ability, good elasticity and easy large scale was investigated by numerous kinds of oils and organic solvents.
fabrication [23]. Therefore, polyurethane foam composites have To our knowledge, this study is the first report about the
been intensively explored as a promising oil–water separation preparation of Al2O3/PUF foam sponge and its application on the
absorbent with a remarkable absorption capability resulting from oils and organic solvents absorption.
their pores structure, excellent elasticity and mechanical stabili-
ties, and diverse chemical modification of surface [24–26]. Experimental
Hollow micro and nanospheres with well-defined structure and
shape, low density, high specific surface area, large void fraction, Materials
low thermal expansion and refractive index, make them useful as
adsorption, catalysis, electrochemistry and sensors due to high Polyether polyol (NJ-330, M = 3000 g/mol) was obtained from
specific surface area, high porosity and excellent physical– Ningwu Chemical Co., in Jurong, Jiangsu, China. Isophorone
chemical properties, moreover aluminum oxides itself are low diisocyanate (IPDI, purity  99.5% and -NCO content  37.5%) was
toxicity and cost [27–29]. Due to this well dispersion of the hollow supplied by Rongrong Chemical Co., in Shanghai, China. Dibutyltin
Al2O3 in the polymer matrix and the interfacial interaction dilaurate (DBLT), silicone oil ([-Si(CH3)2O-]n), and sodium bicar-
between the inorganic and organic phases, the Al2O3 composites bonate (NaHCO3), aluminium potassium sulfate (KAl(SO4)22H2O),
has been significantly improved in the thermal stability and urea (CO(NH2)2), g-methacryloxypropyl trimethoxysilane
mechanical properties. In this work, hollow Al2O3 spheres were (KH570), aluminium sulfate (Al2(SO4)318H2O), and Sudan III were
prepared by one-pot hydrothermal synthetic routes and thermal purchased from Sinopharm Chemical Reagent Co., Ltd., in
treatment. Then the hydrophobic Al2O3 was obtained using hollow Shanghai, China. Diesel oil was brought from Sinopec, in Zhenjiang,
Al2O3 spheres modified with g-methacryloxypropyltrimethoxysi- Jiangsu, China. Bean oil was produced by Nanjing Baoyang Trade
lane (KH-570). A hydrophobic and oleophilic polyurethane (Al2O3/ CO., in Nanjing, Jiangsu, China.
PUF) foam sponge was prepared with polyether polyol (NJ-330),
hydrophobic Al2O3, sodium bicarbonate, silicone oil, dibutyltin Preparation of hydrophobic and oleophilic foam polyurethane sponge
dilaurate (as catalyst, DBLT) and isophorone diisocyanate (IPDI) as (Al2O3/PUF)
raw materials by foam technology. This Al2O3/PUF foam sponge
could cover all the reticulated network of the foams. The The hydrophobic and oleophilic polyurethane foam sponge was
unmodified foams exhibit inherent hydro- and oleophobicity, prepared by three steps.

Scheme 1. The synthetic route of hydrophobic and oleophilic polyurethane (Al2O3/PUF) foam sponge.

Please cite this article in press as: L. Kong, et al., Fabrication of hydrophobic and oleophilic polyurethane foam sponge modified with
hydrophobic Al2O3 for oil/water separation, J. Ind. Eng. Chem. (2017), https://doi.org/10.1016/j.jiec.2017.09.050
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L. Kong et al. / Journal of Industrial and Engineering Chemistry xxx (2017) xxx–xxx 3

(1) Hollow spheres of Al2O3 were prepared by one-pot hydrother- capacity of the Al2O3/PUF, 0.2 g (m0) of Al2O3/PUF foam sponge was
mal method. Briefly, KAl(SO4)22H2O (0.0015 mol), immersed in 30 mL oils or organic solvents, and let it stand for 12 h
Al2(SO4)318H2O (0.0005 mol) and CO(NH2)2 (0.004 mol) pow- to reach saturation of absorption at room temperature. Then, the
ders were dissolved in 40 mL distilled water and stirred for Al2O3/PUF foam sponge was weighed immediately (m1). The
0.5 h at room temperature. Then the mixed solution was added absorption capacity (g/g) was evaluated by the following equation:
into a 100 mL Teflon-lined stainless autoclave and maintained m1  m0
at 180  C for 3 h. After reaching room temperature, the white Q¼ ð1Þ
m0
precipitate was collected and washed with distilled water and
anhydrous alcohol several times. And then the product was where Q was the absorption capacity of absorbed oil or organic
dried in an oven at 80  C for 12 h. Finally, the sample was solvent by Al2O3/PUF foam sponge (g/g); m0 was the initial weight
calcined at 600  C for 2 h and hollow Al2O3 spheres were of the Al2O3/PUF foam sponge (g/g), and m1 was the weight of
obtained and yield was 88%. Al2O3/PUF foam sponge (g/g) at equilibrium.
(2) Hydrophobic Al2O3 was obtained using hollow Al2O3 spheres
modified with g-methacryloxypropyltrimethoxysilane (KH- Regeneration
570). The process is as follows: KH-570 and deionized water
were added into round bottom flask and stirred for 30 min to In order to examine the regeneration capacity of the oil
insure obtaining homogeneous solution. Fixed the mKH570: absorbent, the saturated Al2O3/PUF foam sponge was immersed in
mAl2O3 = 1:5, the as-prepared Al2O3 was put into to the solution anhydrous ethanol for desorption. For the reusability tests, 0.15–
and reacted by microwave irradiation (700 W, 85  C and 0.25 g sample was immersed in 25 mL of oil for saturated
70 min). The hydrophobic Al2O3 was washed by deionized absorption. Later, the saturated Al2O3/PUF foam sponge was
water for 3 times and dried at 60  C for 12 h. The hydrophobic immersed in 50 mL anhydrous ethanol to release the absorbed oil.
Al2O3 was obtained and yield was 87%. Then, the Al2O3/PUF foam sponge was dried in an oven for 12 h at
(3) The hydrophobic and oleophilic polyurethane (Al2O3/PUF) 80  C. This absorption–desorption procedure was repeated 10
foam sponge was prepared by foam technique. A certain times to conform the reusability of Al2O3/PUF foam sponge. After
amounts of hydrophobic Al2O3, NJ-330 (10 g), NaHCO3 (0.3 g), each cycle, the Al2O3/PUF foam sponge was weighed before and
silicone oil (0.2 g) and DBLT (0.2 g) were mixed in a plastic cup, after oil absorption.
and stirred to perform the uniform solution. Then IPDI (2.3 g)
was added into the mixture and rapidly stirred. While the Results and discussion
mixture turned to white with some bubbles, the mixture was
transferred into blast oven and kept the temperature about Characterization of hollow Al2O3 spheres
100  C for 3 h [30]. After that, the hydrophobic and oleophilic
foam polyurethane sponge reinforced (Al2O3/PUF) was XRD patterns of hollow Al2O3 spheres at 600  C for 2 h (a) and
obtained. A series of Al2O3/PUF materials were prepared with 180  C for 3 h (b) are shown in Fig. 1. As can be seen from Fig. 1(a),
different mass content of hydrophobic Al2O3 of 0, 1%, 2%, 3%, 4% all the diffraction peaks of 66.9 , 45.9 , 39.5 , 37.3 and 32.7 are in
and 5%, and named as PUF, Al2O3/PUF-1, Al2O3/PUF-2, Al2O3/ good accordance with those of the (440), (400), (222), (311) and
PUF-3, Al2O3/PUF-4 and Al2O3/PUF-5, respectively. The syn- (220) planes of the Al2O3 crystal orthorhombic (JCPDS card no. 80-
thetic route of hydrophobic and oleophilic polyurethane 1098) [31–33]. In Fig. 1(b), the well-defined diffraction peaks at
(Al2O3/PUF) foam sponge is shown in Scheme 1. 14.3 , 28.1, 38.3 , 45.6 , 49.1, 51.4 , 54.9 , 60.5 , 63.8 , 64.8 and
67.8 can be indexed as (020), (120), (031), (131), (200), (151),
(080), (231), (002) and (171) planes, respectively, in the cubic phase
Characterization of Al-OOH (JCPDS card no. 80-1098). No other diffraction peaks are
detected, which suggests a high purity aluminium oxide. Based on
X-ray powder diffraction (XRD) analysis was conducted on a the result, calcinations conditions were chosen at 600  C for 2 h in
Shimadzu LabX-6000 X-ray (Japan) diffractometer with Cu Ka preparation process of hollow Al2O3 spheres. TEM images of
radiation at 40 kV and 30 mA over the 2u range of 10–80 at a hollow Al2O3 spheres at different magnification are presented in
scanning speed of 7 /min. Fourier transform infrared (FT-IR)
spectra were collected on a FT-IR spectrophotometer (AVATAR 360,
Nicolet, USA). The samples were prepared as KBr pellets and
scanned 24 times in the 4000–400 cm1 ranges of wavenumbers.
Scanning electron microscopy (SEM) was performed at accelerat-
ing voltage of 20 kV (SEM, S-4800, Hitachi, Tokyo) and the SEM
specimens were prepared by sputter coating a thin gold layer
approximately 3 nm thick. Transmission electron microscopy
(TEM) was performed on a PHI-Tecnai 12 electron microscope
with an accelerating voltage of 120 kV. The samples for TEM
measurements were ultrasonically dispersed in ethanol. The water
contact angles (CA) were measured at room temperature and
ambient relative humidity with the drop-shape analysis software
(Krüss DSA 100, Germany). The Brunauer–Emmet–Teller (BET)
surface area was determined by nitrogen adsorption in a Micro-
meritics ASAP 2030 nitrogen adsorption apparatus (USA).

Oil or organic solvent absorption experiment

The experiments of oil or organic solvent absorption were Fig. 1. XRD patterns of hollow Al2O3 spheres at 600  C for 2 h (a) and 180  C for 3 h
carried out as follows. To investigate the maximal absorption (b).

Please cite this article in press as: L. Kong, et al., Fabrication of hydrophobic and oleophilic polyurethane foam sponge modified with
hydrophobic Al2O3 for oil/water separation, J. Ind. Eng. Chem. (2017), https://doi.org/10.1016/j.jiec.2017.09.050
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4 L. Kong et al. / Journal of Industrial and Engineering Chemistry xxx (2017) xxx–xxx

Fig. 2. TEM images of hollow Al2O3 spheres at different magnification.

Fig. 2. From Fig. 2(a), the diameters of hollow Al2O3 spheres are which the mesopores arise from the stacking of the laminar units
about 4 mm, which are comprised of the nano-dot. As can be seen (Fig. 3(a)) [35]. The specific surface area of the hollow Al2O3
from Fig. 2(b), the morphology of the as-prepared hollow Al2O3 spheres is 214.79 m2/g. The pore size distribution curve of hollow
spheres is presented as nanosheets with a thickness of less than Al2O3 spheres by the BJH method is shown in Fig. 3(b), and the
100 nm, which is similar to previous reports [31,32]. The pore result shows the peak at pore diameter ranged from 15 to 40 nm.
structure and the BET surface area of hollow Al2O3 spheres were The hollow Al2O3 spheres have a large specific surface and pore
analyzed on the basis of nitrogen adsorption isotherms; and the structure, which are beneficial to enhance its absorption capacity.
typical nitrogen sorption isotherms (a) and BJH (Barret–Joyner–
Halenda) desorption pore size distribution curve (b) are shown in SEM and water contact angle analysis
Fig. 3. As can be seen from Fig. 3, the nitrogen adsorption isotherm
of hollow Al2O3 spheres is type IV with a type H3 hysteresis loop SEM images of pure PUF (a), hollow Al2O3 spheres (b) and Al2O3/
[34], which corresponds to characteristic mesoporous materials of PUF-3 foam sponge (c) are shown in Fig. 4. Fig. 4(a) presents

Fig. 3. Typical nitrogen sorption isotherms (a) and BJH (Barret–Joyner–Halenda) desorption pore size distribution curve (b) of hollow Al2O3 spheres (p: pressure of adsorbate;
p0: saturated vapor pressure of liquid adsorbate at adsorption temperature).

Fig. 4. SEM images of pure PUF (a), hollow Al2O3 spheres (b) and Al2O3/PUF-3 foam sponge (c).

Please cite this article in press as: L. Kong, et al., Fabrication of hydrophobic and oleophilic polyurethane foam sponge modified with
hydrophobic Al2O3 for oil/water separation, J. Ind. Eng. Chem. (2017), https://doi.org/10.1016/j.jiec.2017.09.050
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L. Kong et al. / Journal of Industrial and Engineering Chemistry xxx (2017) xxx–xxx 5

Fig. 5. Water contact angles of hollow Al2O3 spheres (a), hydrophobic Al2O3 (b), PUF (c) and Al2O3/PUF-3 (d) foam sponge.

roughly open-cell structures with a non-uniform cell size PUF foam sponge has better surface hydrophobic properties than
distribution. As can be observed from Fig. 4(b), the amorphous pure PUF foam not containing hollow alumina. All facts indicated
Al2O3 spheres possess hollow core/shell structures. The complex the as-prepared Al2O3/PUF foam sponge possesses stable hydro-
shells are formed by self-assembly of nanoflakes, which resulting phobicity.
in the partial ordering of loosely connected flakes. As can be seen
from Fig. 4(c), Al2O3 are scattered in the PUF matrix, indicating that Absorption properties of the Al2O3/PUF foam sponge
the Al2O3/PUF foam sponge was successfully synthesized.
Water contact angles measurement of hollow Al2O3 spheres (a), The absorption properties on the Al2O3/PUF foam sponge were
hydrophobic Al2O3 (b), PUF (c) and Al2O3/PUF-3 (d) foam sponges investigated; and the process of the oil absorption experiment is
are shown in Fig. 5. As can be seen from Fig. 5, water contact angles shown in Fig. 6. The oils from water are collected through a simple
of hollow Al2O3 spheres, hydrophobic Al2O3, PUF and Al2O3/PUF-3 mechanical squeezing process. Once a piece of as-prepared Al2O3/
foam sponges are 0 , 136 , 127 and 144 , respectively. The results PUF-3 foam sponge is placed in oil–water mixtures, the oils can be
could illustrate that the hollow Al2O3 spheres modified with KH- are quickly absorbed by the composite in a few seconds.
570 is hydrophobic, and Al2O3/PUF foam sponge can be improved The absorption capacities of the Al2O3/PUF-3 foam sponge for
after modified by hydrophobic Al2O3; in other words, the Al2O3/ different oil and organic solvents are shown in Fig. 7(a). As can be

Fig. 6. A series of photos for the process of absorption and collection of lubricating oil (dyed with oil red) from the water. (For interpretation of the references to color in this
figure legend, the reader is referred to the web version of this article.)

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hydrophobic Al2O3 for oil/water separation, J. Ind. Eng. Chem. (2017), https://doi.org/10.1016/j.jiec.2017.09.050
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Fig. 7. The absorption capacities of the Al2O3/PUF-3 foam sponge for oil and organic solvents (a); the effect of hydrophobic Al2O3 content on the absorption capacities of the
Al2O3/PUF foam sponge (b).

spheres evenly can be dispersed in polyurethane polymer, which


has a certain supporting function for foam holes and improved the
surface of PUF foam sponge. Hence, the absorption property of
Al2O3/PUF foam sponge is better than that of pure PUF foam
sponge.

Reusability

Chloroform, soybean oil and methylbenzene were chosen to


evaluate the reusability of the Al2O3/PUF-3 foam sponge; and
the result is shown in Fig. 8(a, b and c). The absorption capacity
for chloroform, soybean oil and methylbenzene are 37.0, 6.8,
and 15.8 g/g, respectively. As can be seen from Fig. 8, the
increase in the absorption cycles has no obvious effect on the
oil absorbency, which will offer important opportunities in
industry and everyday life, such as oil spill cleanup, separation
of living waste oil. The slight decrease in the absorption
capacity is due to the residual oil inside the foams, which
Fig. 8. The effect of recycle times on the absorption capacity of the Al2O3/PUF-3
cannot be fully removed just by a simple manual squeezing
foam sponge.
process. The regeneration experiments are shown that the
Al2O3/PUF foam sponge with decent reusability and stability is
seen from Fig. 7(a), obviously, the absorption capacity of different the ideal material for oil absorption.
oil and organic solvents such as tetrachloromethane (CCl4), Comparison of maximum absorption capacity of Al2O3/PUF
chloroform (CCl3), methylbenzene, bean oil, diesel oil and hexane foam sponge for oil and organic solvent with other previously
on Al2O3/PUF foam sponge are bigger than that of the pure PUF. The prepared absorbents is presented in Table 1. Compared with
consequence is exposited that the absorption capacity of Al2O3/ previous sorbents, hydrophobic and oleophilic Al2O3/PUF foam
PUF foam sponge can be improved visibly. sponge has a higher absorption capacity [13,29,36–39]. It could be
To investigate the effect of hydrophobic Al2O3 content on the concluded that the synthesized Al2O3/PUF foam sponge can be a
absorption capacities, the Al2O3/PUF foam sponge was prepared good solution for decreasing the current environmental crisis of
with different contents of hydrophobic Al2O3. The content of the serious water contamination arising from oil spills.
hydrophobic Al2O3 was fitted 1.0%–5.0% based on the sum mass of
polyether polyol and isophorone diisocyanate. The effect of Conclusion
hydrophobic Al2O3 content on the absorption capacities of the
Al2O3/PUF foam sponge is shown in Fig. 7(b). As can be seen in In current work, the hollow Al2O3 spheres were prepared by
Fig. 7(b), the absorption capacity increases distinctly with the one-pot hydrothermal method. Then the hydrophobic Al2O3 was
increasing content of hydrophobic Al2O3 and while the hydropho- obtained using hollow Al2O3 spheres modified with g-methacry-
bic Al2O3 content is 3.0%, the biggest absorption capacity of the loxypropyltrimethoxysilane (KH-570). An inexpensive method to
Al2O3/PUF-3 foam sponge can be achieved 37 times of its own fabricate hydrophobic and oleophilic polyurethane (Al2O3/PUF)
weight. Hydrophobic modification by KH-570 of hollow Al2O3 foam sponge was prepared with hydrophobic Al2O3 and

Table 1
Comparison of maximum absorption capacity of Al2O3/PUF foam sponge with other reported absorbents.

Absorbent Absorption capacity (g/g) Reference


Mn2O3/resin composites 34.0 36
Superwetting nanowire membranes 20.0 37
PUF modified with nanoclay 18.0–22.0 38
Porous Al2O3/acrylic resin composites 30 29
MnO2/p(BA-co-BMA-co-MMA) hybrid resin 34.56 13
Magnetic cellulose aerogel 28.0 39
Al2O3/PUF foam sponge 37.0 This work

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hydrophobic Al2O3 for oil/water separation, J. Ind. Eng. Chem. (2017), https://doi.org/10.1016/j.jiec.2017.09.050
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L. Kong et al. / Journal of Industrial and Engineering Chemistry xxx (2017) xxx–xxx 7

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Please cite this article in press as: L. Kong, et al., Fabrication of hydrophobic and oleophilic polyurethane foam sponge modified with
hydrophobic Al2O3 for oil/water separation, J. Ind. Eng. Chem. (2017), https://doi.org/10.1016/j.jiec.2017.09.050

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