Designer poly(urea-siloxane) microspheres with controlled modulus and size: Synthesis, morphology, and nanoscale stiffness by AFM

Gojżewski, Hubert; Obszarska, Jagoda; Harlay, Agnes; Hempenius, Mark A.; Vancso, Gyula J.

doi:10.1016/j.polymer.2018.07.034

Cited by 12 publications

(10 citation statements)

References 57 publications

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“…As mentioned above, functionalized siloxanes are important building blocks, in particular, in syntheses of copolymers from organic and organosilicon monomers . For example, our attention was attracted by the potential possibility of synthesizing a siloxane analogue of PET, a polymer produced on a large scale and used for the production of various materials, such as fibers, films for food packaging, and plastics used in building, medicine, electronics, etc…”

Section: Results and Discussionmentioning

confidence: 99%

Aerobic Co-/N-Hydroxysuccinimide-Catalyzed Oxidation of p-Tolylsiloxanes to p-Carboxyphenylsiloxanes: Synthesis of Functionalized Siloxanes as Promising Building Blocks for Siloxane-Based Materials

et al. 2019

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Synthesis of organosilicon products with a "polar" functional group within organic substituents is one of the most fundamentally and practically important challenges in today's chemistry of silicones. In our study, we suggest a solution to this problem, viz., a high-efficiency preparative method based on aerobic Co-/N-hydroxysuccinimide (NHSI) catalyzed oxidation of p-tolylsiloxanes to p-carboxyphenylsiloxanes. This approach is based on "green", commercially available, simple, and inexpensive reagents and employs mild reaction conditions: Co(OAc) 2 /NHSI catalytic system, O 2 as the oxidant, process temperature from 40 to 60 °C, atmospheric pressure. This reaction is general and allows for synthesizing both mono-and di-, tri-, and poly(p-carboxyphenyl)siloxanes with p-carboxyphenyl groups at 1,1-, 1,3-, 1,5-, and 1,1,1-positions. All the products were obtained and isolated in gram amounts (up to 5 g) and in high yields (80−96%) and characterized by NMR, ESI-HRMS, GPC, IR, and X-ray data: p-carboxyphenylsiloxanes in crystalline state form HOF-like structures. Furthermore, it was shown that the suggested method is applicable for the oxidation of organic alkylarene derivatives (Ar−CH 3 , Ar−CH 2 −R) to the corresponding acids and ketones (Ar−C(O)OH and Ar−C(O)−R), as well as hydride silanes ([Si]−H) to silanols ([Si]−OH). The possibility of synthesizing monomeric (methyl) and polymeric (siloxane-containing PET analogue, Sila-PET) esters based on 1,3-bis(p-carboxyphenyl)disiloxane was studied. These processes occur with retention of the organosiloxane frame and allow to obtain the corresponding products in 90 and 99% yields.

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Section: Results and Discussionmentioning

confidence: 99%

Aerobic Co-/N-Hydroxysuccinimide-Catalyzed Oxidation of p-Tolylsiloxanes to p-Carboxyphenylsiloxanes: Synthesis of Functionalized Siloxanes as Promising Building Blocks for Siloxane-Based Materials

et al. 2019

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“…This latter parameter was calculated as the slope of the approached part of the force-curve distance by a linear fit. To obtain PF-QNM quantitative maps, the relative calibration method proposed by Bruker and recently used in the literature was followed. ,, All samples were probed using Tap 150AI-G probes by BudgetSensors (tip radius <10 nm, as estimated from a tip-checker sample provided by Bruker). The deflection sensitivity of the detector was obtained using a sapphire sample provided by Bruker.…”

Section: Methodsmentioning

confidence: 99%

Volatile Organic Compound-Free Synthesis of Waterborne Poly(hydroxy urethane)–(Meth)acrylic Hybrids by Miniemulsion Polymerization

Bizet

Grau

Cramail

et al. 2020

ACS Appl. Polym. Mater.

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A volatile organic compound (VOC)-free method for the synthesis of poly(hydroxyurethane)−(meth)acrylic waterborne hybrid dispersions was developed. Poly(hydroxyurethane) (PHU) synthesized by bulk aminolysis of cyclic-carbonate derivatives using biosourced vegetable oil-based diamines was dissolved in (meth)acrylate monomers; the solution was dispersed in water and polymerized in a miniemulsion. Hybrid particles exhibiting core−shell morphology with the PHU in the shell were obtained. The performance of the coating cast from these dispersions was studied, finding that by simply varying the PHU content and the casting conditions, widely different mechanical properties of PHU−(meth)acrylic hybrids could be obtained. The versatility of the synthetic method that is not limited to the type of (meth)acrylic monomers opens the way for obtaining a broad range of environmentally friendly VOC-and isocyanate-free waterborne urethane−acrylic coatings and adhesives.

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“…This approach has been used extensively in recent literature to evaluate nanomechanical contrast in polymer systems. [36][37][38] PF-QNM allows the simultaneous mapping of topographical and nanomechanical features, being the latter related to the surface elastic modulus, tip-sample adhesion force and surface deformation. Briefly, in this operation method the probe performs force-distance curves on each pixel, at a 2 kHz sinusoidal modulation frequency (fm).…”

Section: Methodsmentioning

confidence: 99%

“…This approach has been used extensively in recent literature to evaluate nanomechanical contrast in polymer systems. [36][37][38] Based on the PF-QNM maps, on fixed zones of the samples' surfaces we performed force spectroscopy measurements. In force spectroscopy, the cantilever approaches, "pokes…”

Section: Molecularmentioning

confidence: 99%

Wrinkling Poly(trimethylene 2,5-Furanoate) Free-standing Films: Nanostructure Formation and Physical Properties

Soccio

Lotti

Munari

et al. 2020

Preprint

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<p>Nanostructured wrinkles were developed on fully bio-based poly(trimethylene furanoate) (PTF) films by using the technique of Laser Induced Periodic Surface Structures (LIPSS). We investigated the effect of irradiation time on wrinkle formation using an UV pulsed laser source, at a fluence of 8 mJ/cm2. It was found that the pulse range between 600 and 4800 pulses allowed formation of periodic nanometric ripples. The nanostructured surface was studied using a combined macro- and nanoscale approach. We evaluated possible physicochemical changes taking place on the polymer surface after irradiation by infrared spectroscopy, contact angle measurements and atomic force microscopy. The macroscopic physicochemical properties of PTF showed almost no changes after nanostructure formation, differently from the results previously found for the terephthalic counterparts, as poly(ethyleneterephthalate), PET, and poly(trimethyleneterephthalate), PTT. The surface mechanical properties of the nanostructured PTF were found to be improved, as evidenced by nanomechanical force spectroscopy measurements. In particular, an increased Young’s modulus and higher stiffness for the nanostructured sample were measured. <br></p>

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Designer poly(urea-siloxane) microspheres with controlled modulus and size: Synthesis, morphology, and nanoscale stiffness by AFM

Cited by 12 publications

References 57 publications

Aerobic Co-/N-Hydroxysuccinimide-Catalyzed Oxidation of p-Tolylsiloxanes to p-Carboxyphenylsiloxanes: Synthesis of Functionalized Siloxanes as Promising Building Blocks for Siloxane-Based Materials

Aerobic Co-/N-Hydroxysuccinimide-Catalyzed Oxidation of p-Tolylsiloxanes to p-Carboxyphenylsiloxanes: Synthesis of Functionalized Siloxanes as Promising Building Blocks for Siloxane-Based Materials

Volatile Organic Compound-Free Synthesis of Waterborne Poly(hydroxy urethane)–(Meth)acrylic Hybrids by Miniemulsion Polymerization

Wrinkling Poly(trimethylene 2,5-Furanoate) Free-standing Films: Nanostructure Formation and Physical Properties

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