Synthesis And Characterization Of Low Molecular Mass Amphiphilic Block Copolymers And Potential Use In Surfactant Assisted Particle Micro Mixing PDF Download

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Synthesis and Characterization of Low Molecular Mass Amphiphilic Block Copolymers and Potential Use in Surfactant Assisted Particle Micro-mixing

Synthesis and Characterization of Low Molecular Mass Amphiphilic Block Copolymers and Potential Use in Surfactant Assisted Particle Micro-mixing
Author: Ekaterini Karakatsanis
Publisher:
Total Pages:
Release: 2013
Genre:
ISBN:
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In industry the effective mixing and de-agglomeration of two solid particles is vital in applications that require the intimate contact of homogeneously mixed reagents. One such application is in the preparation of pyrotechnic delay elements with reproducible burn speeds. The concept of surfactant assisted particle micro-mixing is proposed. This theory is based in the use of two amphiphilic polymeric surfactants to form two separate stable dispersions of the two solid particles to be mixed, but with the subsequent requirement that the dispersants are able to interact with each other. The formation of the individual dispersions allows for the deagglomeration of the particles and thus their preparation for homogeneous mixing, which is facilitated by the interacting surfactants. Low molecular mass block copolymers of styrene and acrylic acid and poly(ethylene oxide)-poly(propylene oxide) (PEO-PPO) surfactants are the proposed dispersants which will allow for the surfactant interaction by means of hydrogen bonding between the poly(acrylic acid) block and the PEO. The poly(styrene-co-acrylic acid) block copolymer will be synthesised via Atom Transfer Radical Polymerisation (ATRP) and subsequently used in the dispersion experiments. The synthesis of the polystyrene macroinitiators to initiate the block copolymerisation of the t-butyl acrylate was carried out satisfactorily, with good molecular masses and molecular mass distributions. In addition, lH-NMR analysis carried out on the polystyrene macroinitiators confirmed their synthesis. The use of the polystyrene macroinitiators was successful in synthesising poly(styrene-co-t-butyl acrylate) block copolymers with slightly higher polydispersities in comparison to the macroinitiatiators themselves, but acceptable. Hydrolysis of the poly(styrene-co-t-butyl acrylate) block copolymer to poly(styrene-co-acrylic acid) was successful in the presence of trifluoroacetic acid as catalyst. Attempts to hydrolyse in basic conditions (NaOH) and alternatively in acidic conditions (HCI) were not successful. Use of the poly(styrene-co-acrylic acid) amphiphilic block copolymer to emulsion polymerise styrene requires the ionised form of the polymer and was therefore not favourable to observe surfactant-surfactant hydrogen bonding. In addition, attempts to synthesise a wax emulsion stabilised by a PEO containing surfactant proved to be unsuccessful. Subsequently, the micro-mixing experiments were carried out by using a poly(acrylic acid) stabilised melamine dispersion and a commercially available PEO containing surfactant stabilised wax emulsion. The interaction between the melamine and the poly(acrylic acid) allows for the formation of a stable melamine dispersion at above 7% poly(acrylic acid) : melamine ratio (mass basis). Analysis by SEM shows that without the poly(acrylic acid) dispersant no wax particles are found to occur on the melamine particle surface. However, in an attempt to determine whether the amount of wax interaction increases with poly(acrylic acid) content, it was found that in the absence of poly(acrylic acid) dispersant, the most amount of wax precipitated out with the melamine. This is possibly attributable to the preferential occlusion of the wax particles between the melamine particles rather than surface attachment. Introduction of the poly(acrylic acid), however, shows via SEM analysis that the hydrogen bond interaction between the acrylic acid group and the ethylene oxide group does occur, since the attachment of the wax particles on the melamine particle surface is observed. Although results show that the surfactant-surfactant interaction allows for the micro mixing of particles, some refinement is required with respect to the systems that this phenomenon can be applied to. In addition, factors such as particle type, particle size and surfactant type will influence the micro-mixing interaction. It is therefore recommended that these factors be investigated in order to completely identify the micro-mixing phenomenon.

Amphiphilic Block Copolymers

Amphiphilic Block Copolymers
Author: P. Alexandridis
Publisher: Elsevier
Total Pages: 449
Release: 2000-10-18
Genre: Science
ISBN: 0080527108
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It is the belief of the editors of this book that the recognition of block copolymers as being amphiphilic molecules and sharing common features with other well-studied amphiphiles will prove beneficial to both the surfactant and the polymer communities. An aim of this book is to bridge the two communities and cross-fertilise the different fields. To this end, leading researchers in the field of amphiphilic block copolymer self-assembly, some having a background in surfactant chemistry, and others with polymer physics roots, have agreed to join forces and contribute to this book.The book consists of four entities. The first part discusses theoretical considerations behind the block copolymer self-assembly in solution and in the melt. The second part provides case studies of self-assembly in different classes of block copolymers (e.g., polyethers, polyelectrolytes) and in different environments (e.g., in water, in non-aqueous solvents, or in the absence of solvents). The third part presents experimental tools, ranging from static (e.g., small angle neutron scattering) to dynamic (e.g., rheology), which can prove valuable in the characterization of block copolymer self-assemblies. The fourth part offers a sampling of current applications of block copolymers in, e.g., formulations, pharmaceutics, and separations, applications which are based on the unique self-assembly properties of block copolymers.

Block Copolymers

Block Copolymers
Author: Francisco Balta Calleja
Publisher: CRC Press
Total Pages: 604
Release: 2000-06-09
Genre: Technology & Engineering
ISBN: 9780824703820
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A summary of block copolymer chemical structures and synthesis. It discusses physical methods of characterization such as computer simulation, microhardness, dielectric spectroscopy, thermal mechanical relaxation, ultrasonic characterization, transmission electron microscopy, X-ray scattering, and NMR, among others. It also outlines rheological and processing parameters in the multiphase polymer systems with stable microstructures.

Nonionic Surfactants

Nonionic Surfactants
Author: Vaughn Nace
Publisher: CRC Press
Total Pages: 284
Release: 2017-10-19
Genre: Science
ISBN: 135142842X
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Focuses on copolymers made from sequential block polymerizations of ethylene oxide, propylene oxide and 1, 2-butylene oxide. This text presents the latest applications of polyoxyalkylene block copolymers in areas such as medicine, coal and petroleum, plastics, emulsion polymerization, paper, photography, personal care and cleaner systems. It offers in-depth coverage of the subject from synthesis and analysis to toxicology and environmental impact.

Synthesis, Characterization and Self-assembly of Amphiphilic Block Copolymers

Synthesis, Characterization and Self-assembly of Amphiphilic Block Copolymers
Author: Xiaojun Wang
Publisher:
Total Pages: 250
Release: 2012
Genre:
ISBN:
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This dissertation presents a review on state-of-the-art research of well-defined charged block copolymers, including synthesis, characterization, bulk morphology and self-assembly in aqueous solution of amphiphilic block polyelectrolytes. In Chapter 1, as a general introduction, experimental observations and theoretical calculations devoted towards understanding morphological behavior in charged block copolymer systems are reviewed along with some of the new emerging research directions. Further investigation of charged systems is urged in order to fully understand their morphological behavior and to directly target structures for the tremendous potential in technological applications. Following this background, in Chapters 2, 3, 4 and 5 are presented the design and synthesis of a series of well-defined block copolymers composed of charged and neutral block copolymers with full characterization: sulfonated polystyrene-b-fluorinated polyisoprene (sPS-b-fPI) and polystyrene-b-sulfonated poly(1,3-cyclohexadiene) (PS-b-sPCHD). Their bulk morphological behaviors in melts and self-assembly of sPS-b-fPI, PS-b-sPCHD in water were investigated. Some unique behaviors of sPS-b-fPI were discovered. The mechanisms for formation of novel nanostructures in aqueous solution are discussed in details in Chapter 4. Spherical and vesicular structures were formed from strong electrolyte block copolymers, e.g. PS-bsPCHD. Detailed light scattering and transmission electron microscopy were applied to characterize these structures. The abnormal formation of vesicles as well as microstructure effects on self-assembly is discussed in Chapter 5. In Chapter 6, we describe the successful synthesis of a well-defined acid-based block copolymers containing polyisoprene while maintaining the integrity of the functionality (double bonds) of polyisoprene. A general purification method is also presented in order to remove homo polyisoprene, polystyrene, and PS-b-PI in the di-, and tri-block copolymers. The self-assembly of PS-b-PI-b-PAA triblock terpolymers was studied in order to form multicompartmental structures in aqueous environments. In the last Chapter 7, detailed synthesis and characterization of a novel conjugate: poly(L-leucine) grafted hyaluronan (HA) (HA-g-PLeu) are presented. This work describes a new method to synthesize HA-g-PLeu via a "grafting onto" strategy. Due to the amphiphilic nature of this graft copolymers, a "local network" formed by self-assembly which was characterized by atomic force microscopy and light scattering. The secondary structure of the polypeptide was revealed by circular dichroism.

The Synthesis and Characterization of Amphiphilic Poly(ethylene Oxide)-block-poly(octadecyl Acrylate) Block Copolymers

The Synthesis and Characterization of Amphiphilic Poly(ethylene Oxide)-block-poly(octadecyl Acrylate) Block Copolymers
Author: Yi Wang (Polymer engineer)
Publisher:
Total Pages: 0
Release: 2014
Genre: Crystalline polymers
ISBN:
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A series of well-defined poly(ethylene oxide)-block-poly(octadecyl acrylate) (PEO-b-PODA) diblock copolymers were successfully synthesized by reversible addition fragmentation transfer (RAFT) polymerization with low polydispersities (M[subscript w]/M[subscript n] = 1.09-1.13). The crystallization behavior of poly(ethylene oxide)-block-poly(octadecyl acrylate) (PEO-b-PODA) diblock copolymers has been studied by differential scanning calorimetry (DSC), small-angle X-ray scattering (SAXS) and polarized optical microscopy (POM). The melt morphology of PEO455-PODA19 experienced a transition from lamella to cylinder at 130°C. For the double crystalline block copolymer PEO455-PODA19, the micro-phase separation at 55°C created lamellar micro-domains, which confined the PEO blocks as it crystallized. The leading crystallization of PEO blocks then created a space that confined PODA crystallites as they are developed. The spherulites were formed first when PEO started to crystallize, but crystallites with polyhedral shape finally formed. As for the micelle behavior, the transmission electron microscopy (TEM) showed that amphiphilic block copolymers PEO-PODA with different volume fractions of hydrophobic PODA blocks ranging from 21% to 54%, were able to self-assemble in water forming spherical micelles.

Synthesis and Characterization of Well-defined, Amphiphilic, Ionic Copolymers

Synthesis and Characterization of Well-defined, Amphiphilic, Ionic Copolymers
Author: Yuqing Liu (Polymer engineer)
Publisher:
Total Pages: 208
Release: 2011
Genre: Addition polymerization
ISBN:
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Amphiphilic ionic block copolymers are promising materials for the fabrication of ion-exchange membranes in fuel cells, water purification and advanced molecular engineering applications, such as nanotemplating. For example, block copolymer architectures provide a route to fabricate membranes with tunable transport properties through polymer self assembly. A significant challenge in this field is the synthesis of amphiphilic copolymers, where the intrinsic immiscibility of the hydrophobic and hydrophilic monomers complicates polymerization. To address the immiscibility between sodium p-styrenesulfonate and styrene monomers, styrenesulfonate monomers were neutralized by hydrophobic trialkyl ammonium salts via ion-exchange reactions, and synthesized successfully by RAFT polymerization with low polydispersity (PDI). Diblock or triblock copolymers with well-defined architectures were obtained by sequential RAFT polymerization with styrene. These sulfonate groups were then converted to the sodium salt form via ion-exchange to obtain amphiphilic ionic block copolymers. It was observed that dimethyl n-alkyl ammonium salts of polystyrenesulfonate displayed thermo-reversible gelation behavior in low polarity organic solvents. The investigation of the gelation behavior as a function of temperature, concentration, and solvent was consistent with gelation driven by the ionic aggregation of the polymer as would be expected for polyelectrolyte surfactant complexes in non-polar solvents. Cationic amphiphilic block/graft copolymers containing quaternary ammonium salts were prepared by the RAFT polymerization of polystyrene-b-poly(vinylbenzyl chloride) (PS-b-PVBC) copolymers, and sequential post-polymerization quaternization of the PVBC blocks. PS-b-PVBEA-b-PS triblock copolymers with well-defined architectures were obtained and the ion conductivity of the corresponding membranes, as well as the morphology of the membranes, was investigated. To improve the mechanical properties of the membranes, different architectures, such as pentablock, heptablock and graft copolymers, were designed and synthesized by RAFT polymerization, and chemical crosslinking was employed to improve the mechanical properties and control the swelling in water. Lastly, a new method to prepare multiblock copolymers via a facile route was developed. Polytrithiocarbonates were prepared by condensation polymerization of a dicarboxylic acid functional trithiocarbonate and a diol, and the trithiocarbonate group was controlled by tuning the amount of acid catalyst and reaction time. The polytrithiocarbonate RAFT agents were used to polymerize PS, polystyrene-b-poly (tert-butylstyrene) (PS-b-PtBS), and PS-b-PVBC. The PDI of the polymers toward 2, but the PDI of the polymer blocks between two trithiocarbonate groups was narrow (1.1-1.3 for PS and PS-b-PtBS, and 1.46 for PS-b-PVBC). The PVBC segments were quaternized to achieve anionic amphiphilic multiblock copolymers.

Synthesis and Characterization of Ionically Bonded Diblock Copolymers

Synthesis and Characterization of Ionically Bonded Diblock Copolymers
Author: Lei Feng (Chemical engineer)
Publisher:
Total Pages: 0
Release: 2013
Genre: Diblock copolymers
ISBN:
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Block copolymers consist of two or more incompatible polymer chains linked by covalent bonds. These block copolymer can separate into nanometer sized domains whose morphology depends upon the size of the block and interactions between them. The properties of block copolymers can be modified and potentially improved by introducing noncovalent interactions to replace covalent linkages between blocks to form supramolecular block copolymers. These kinds of materials combine the microphase separation inherent to block copolymers with the facile synthesis of supramolecular materials thereby affording new and unique materials. This dissertation focuses on synthesis and characterization of PS-b-PMA block copolymers with ion-pair junctions.Firstly, the chain-end sulfonated polystyrene ([omega]-sulfonated PS) was synthesized by reversible addition fragmentation chain transfer (RAFT) polymerization and postpolymerization modification. In the postpolymerization modification two methods were investigated: in the first one, the polymer was converted to a thiol-terminated polymer by aminolysis. Then a sulfonic acid end-group was produced then by oxidation of the thiol end-group with m-chloroperoxybenzoicacid (m-CPBA); in the second method, the RAFT-polymerized polymer was directly sulfonated by oxidation with m-CPBA. After purification by column chromatography, [omega]-sulfonated PS was obtained by both methods with greater than 95% end-group functionality as measured by titration. The sulfonic acid end-group could be neutralized with various ammonium or imidazolium counter ions through acid-base or ionic metathesis reactions. These polymers with ionic end-group can be used as model supramolecular building blocks.Secondly, ammonium end functionalized polymethylacrylate (PMA) was synthesized directly by RAFT polymerization using functional RAFT agent. Then chain-end sulfonated polystyrene and ammonium end functionalized polymethylacrylate (PMA) were used to synthesize A-B block copolymers by two different methods: the first method was by mixing two oppositely charged end group functionalized polymers; the second method was to ionically bond a RAFT agent to the chain end of an end sulfonated polymer to generate a supramolecular macro RAFT agent then an A-B block copolymer was prepared by RAFT polymerization using supramolecular macro-RAFT agent. The polymerization kinetics were investigated and the molecular weight and the chemical structure of the block copolymers were characterized by 1H-NMR and SEC. The results show that the ion-bonded supramolecular block copolymer, PS-PMA, have been successfully prepared with controlled molecular weight and narrow distribution.Thirdly, the morphology of the ion-bonded supramolecular PS-PMA diblock copolymers were investigated by small-angle X-ray scattering (SAXS) and rheological techniques. Several covalently bonded PS-PMA block copolymers were synthesized by RAFT polymerization and their micro domain structures and rheology behaviors were also investigated. The results showed that the electrostatic interactions between the end ion groups are able to overcome the thermodynamic repulsion of two blocks result in the formation of diblock copolymers with similar behaviors and morphology of traditional covalent bonded diblock copolymers and their micro domain structures remain to high temperatures.