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Title
Abstract
Background
sulfate and lauroyl sulfate have also been used efficiently for this chemical
transformation. (P.A.G. Cormack et al., 2012)
Motivation
Problem
statement
The conventional sulfonation agent, sulfuric acid can create many limitations on
Objective
To synthesize the strong cation exchange resin using different the milder
Scopes
reaction time.
Synthesis of sulfonated hypercrosslinked polymer using lauroyl sulfate at
and
pore
size
sulfonated
Literature
Review
Citation
Authors
Sulfonic
acid
(-SO3H)-
functionalized
Methodolog
y
Materials
Acetic anyhydride (98%), anhydrous dichloromethane (99.8%), concentrated
sulfuric acid (98%), lauric acid (98%), cyclohexane (99.5%), chlorosulfonic acid
(99%), 1,2-dichloroethane (99.8%), acetone (99%) will be supplied by SigmaAldrich.
Preparation of sulfonation agent
1. Acetyl sulfate
0.405 g of acetic anhydride and 2.5 mL of anhydrous dichloromethane will be
mixed in a round-bottomed flask under nitrogen atmosphere. The flask will be placed
in an ice bath to cool the reaction mixture and 0.163 mL concentrated sulfuric acid
will be added. The flask will be removed from the ice bath and will be allowed to
equilibrate to room temperature. (P.A.G. Cormack et al, 2012).
2. Lauroyl sulfate
0.665 g of lauric acid will be dissolved in cyclohexane (30 mL) under a
nitrogen atmosphere. Chlorosulfonic acid (0.022 mL, 0.038 g, 0.323 mmol) will be
added and the mixture will be stirred at room temperature for one hour under
nitrogen atmosphere. (P.A.G. Cormack et al, 2012).
Synthesis of sulfonated hypercrosslinked polymer
1. Using acetyl sulfate
2.5 g of dried hypercrosslinked beads will be swollen in 60 mL of 1,2dichloroethane for 6 h at 30 C will be followed by dropwise addition 15 mL of
acetyl sulfate. After that, the mixture will be stirred for 1 h for complete dispersion.
The mixture will be subsequently heated to 40 C and will be maintained at this
temperature for , 1, 2, and 4 hours. The resulting beads will be separated by
filtration, washed with water and acetone and will be dried at 60 C in an oven for at
least 24 h.
2. Using lauroyl sulfate
2.5 g of dried hypercrosslinked beads will be swollen in 60 mL of 1,2dichloroethane for 6 h at 30 C will be followed by dropwise addition 15 mL of
lauroyl sulfate. After that, the mixture will be stirred for 1 h for complete dispersion.
The mixture will be subsequently heated to 50 C and will be maintained at this
temperature for 6, 12, 18, and 24 hours. The resulting beads will be separated by
filtration, washed with water and acetone and will be dried at 60 C in an oven for at
least 24 h.
Instrumentation and Characterization of sulfonated hypercrosslinked polymer
The resin samples will be determined the ion exchange capacities contents by
using acid-base titration method. In a typical procedure, 0.1 g of resin sample will be
added to 10 mL of 1.0 M NaOH solution and will have shaken for one hour at room
temperature. The mixture will be filtered and 2.0 mL of the filtrate will be titrated
with 0.1 M HCl solution using phenolphthalein as a color indicator. (Ozer O. et al.,
2013). Fourier Transform Infrared (FTIR) and F-Ray Fluorescence (XRF) will be
used for elemental analysis of the final product are supplied by Universiti Malaysia
Pahang. Thermal Gravimetric Analysis (TGA) using TGA Q-500 system and
Differential scanning calorimetry (DSC) will be used to thermal analysis of final
product. Brunauer, Emmett, and Teller (BET) using Thermo-Scientific and Liquid
Nitrogen, N2 used as adsorbate temp 77 Kelvin will be used to calculate the specific
surface area and pore size of the final product. Scanning electron microscopy (SEM)
by using unit JOEL-JSM-7800F model. This model will be conducted at conditions
2KX, 5KX, 100X and 500X to determine the structural analysis of final product.
References
Abrams I. M., Millar J. R.. (1997). A History of the Origin and Development of
Macroporous ion-exchange resins. Reactive & Functional Polymers, 35, pp 7
pp 22.
Ahmed M., Malik M. A., Pervez S., Raffiq M.. (2004). Effect of porosity on
sulfonation of macroporous styrene-divinylbenzene beads. European Polymer
Journal, 40, pp 1609 pp 1613.
Allan J. T. S., Prest L. E., Easton E. B.. (2015). The sulfonation of polyvinyl chloride:
Synthesis and characterization for proton conducting membrane applications.
Journal of Membrane Science, 489, pp 175 pp 182.
Cormack P. A. G., Davies A., Fontanals N.. (2012). Synthesis and characterization of
microporous polymer microspheres with strong cation-exchange character.
Reactive & Functional Polymers, 72, pp 939-946.
Dale J. A., Irving J.. (1992). Comparison of strong base resin types. In: Slater MJ
(ed.) Ion Exchange Advances - Proceeding of IEX92. Pp 33 pp 40.
Elabda Y. A., Napadensky E.. (2004). Sulfonation and characterization of
poly(styrene-isobutylene-styrene) triblock copolymers at high ion-exchange
poly(EGDMA-co-HEMA)
networks:
Morphological
oil
with
different
alcohols
by
cation
ion-exchange
and
nano-confinement
effect.
Applied
Catalysis
B:
Meng Q. B., Yang G. S., Lee Y. S.. (2013). Preparation of highly porous
hypercrosslinked polystyrene adsorbents: Effect of hydrophilicity on the
adsorption and microwave-assisted desorption behaviour toward benzene.
Microporous and mesoporous materials, 181, pp 222 pp 227.
Meyer M., Schrickel J.. (2013, February). Sulfonated polymers: Simple chemistry for
high-tech materials & applications. Specialty Chemicals Magazine, pp 1 - pp
6.
Millar G. J., Couperthwaite S. J., Papworth S.. (2016). Ion exchange of sodium
chloride and sodium bicarbonate solutions using strong acid cation resins in
relation to coal seam water treatment. Journal of Water Process Engineering,
11, pp 60 pp 67.
Millar G. J., Schot A., Couperthwaite S. J., Shilling A., Nuttall K., Bruyn M. D..
(2015). Equilibrium and column studies of iron exchange with strong acid
cation resin. Journal of Environmental Chemical Engineering, 3, pp 373 pp
385.
Millar G. J., Schot A., Couperthwaite S. J., Shilling A., Nuttall K., Bruyn M. D..
(2015). Equilibrium and column studies of iron exchange with strong acid
cation resin. Journal of Environmental Chemical Engineering 3 pp 373 pp
385.
Miller W. S., Castagna C.J., Pieper A. W.. (2009). Understanding Ion-Exchange
Resins for Water Treatment Systems, Journal of GE water and Process
Technologies, pp1 pp 7.
Ozer O., Ince A., Karagoz B., Bicak N.. (2013). Crosslinked PS-DVB microspheres
with sulfonated polystyrene with sulfonated polystyrene brushes as new
generation of ion exchange resins. Desalination, 309, pp 141 pp 147.
Rajesh A. M., Bhatt S. A., Brahmbhatt H., Anand P. S., Popat K. M.. (2015). Taste
masking of ciprofloxacin by ion-exchange resin and sustain release at gastricintestinal through interpenetrating polymer network. Asian journal of
pharmaceutical sciences, 10, pp 331 pp 340.
Shi Q., Li A., Zhou Q., Shuang C., Li Y., Ma Y.. (2014). Utilization of waste cation
exchange resin to prepare carbon/iron composites for the adsorption of
contaminants in water. Journal of Industrial and Engineering Chemistry, 20,
pp 4256 pp 4260.
Shin K. S., Choi E. M., Hwang T. S.. (2010). Preparation and characterization of ion-