Synthesis and characterization of polysulfides formed by the inverse vulcanisation of cyclosiloxanes with sulfur

Park, Kun Woo; Tafili, Elizabeth; Fan, Flora; Žujović, Zoran D.; Leitao, Erin M.

doi:10.1039/d2py00581f

Cited by 9 publications

(10 citation statements)

References 48 publications

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“…[15,[23][24][25][26][27][28] Moreover, crosslinking agents possessing functional segments have been utilized to integrate the functional segments to polysulfides. [29,30] On the other hand, our previous work demonstrated benzoxazine compounds could react with elemental sulfur to result in the corresponding polybenzoxazine-sulfur materials through SRTC reaction. [10] For the sulfur-involved reactions, formation of hydrogen sulfide (H 2 S) as a byproduct has been reported in some cases.…”

Section: Introductionmentioning

confidence: 99%

Reaction between 1,3,5‐Triisopropylbenzene and Elemental Sulfur Extending the Scope of Reagents in Inverse Vulcanization

Lai

Liu

2023

Macromol. Rapid Commun.

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Inverse vulcanization utilizes an organic compound as reagent for crosslinking elemental sulfur to result in corresponding polymeric material with a high sulfur content. This work, employing 1,3,5-triisopropylbenzene (TIPB) as the reagent, demonstrates the first attempt on extending the scope of crosslinking agents of inverse vulcanization to saturate compounds. Under nuclear magnetic spectroscopic analysis, the reactions between TIPB and elemental sulfur take places through ring-opening reaction of S 8 resulting in sulfur radicals at sulfur chain ends, radicals transferring to isopropyl groups of TIPB, and radical coupling reactions between carbon radicals and sulfur radicals. The obtained products are similar to the sulfur polymers from conventional inverse vulcanization processes and show self-healing property.

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Section: Introductionmentioning

confidence: 99%

Reaction between 1,3,5‐Triisopropylbenzene and Elemental Sulfur Extending the Scope of Reagents in Inverse Vulcanization

Lai

Liu

2023

Macromol. Rapid Commun.

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“…(c) The change of thickness of pSHVDS 170 when exposed to 150 °C. (d)The plot between sulfur content and T g of SCPs without aromatic groups reported previously, and pSHVDS 170 developed in this work 7,13,20,22,26,31,45,65,66.…”

mentioning

confidence: 92%

“…19,24,25 The glass transition temperatures (T g ) of HCSPs prepared through IV are typically low, 24 even in polymers prepared from high functionality comonomers such as tetravinyl tin (T g = 1.31 °C) 21 and pentavinylpentamethyl cyclopentasiloxane (T g = −5.4 °C). 26 Furthermore, thermal properties of many HSCPs are highly sensitive to polymerization 27 and storage conditions. 20 As the sulfur content increases, a trade-off between optical properties (such as refractive index (RI)) and thermal stability becomes apparent, and it extremely challenging to achieve HSCPs exhibiting high RI and high IR transmittance simultaneously with high T g and high thermal stability.…”

Section: Introductionmentioning

confidence: 99%

“…Despite recent progress in improving the optical properties of HSCPs for IR optics, their poor thermal properties remain a significant challenge. ,, The glass transition temperatures ( T g ) of HCSPs prepared through IV are typically low, even in polymers prepared from high functionality comonomers such as tetravinyl tin ( T g = 1.31 °C) and pentavinyl-pentamethyl cyclopentasiloxane ( T g = −5.4 °C) . Furthermore, thermal properties of many HSCPs are highly sensitive to polymerization and storage conditions .…”

Section: Introductionmentioning

confidence: 99%

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Visible, Mid- and Long-Wave Infrared Transparent Sulfur-Rich Polymer with Enhanced Thermal Stability

Jang,

Choi,

Kang

et al. 2023

Chem. Mater.

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High sulfur content polymers (HSCPs) are regarded as promising materials for infrared (IR) optics, especially the long-wave IR range, due to intrinsic properties of sulfur, but the poor thermal stability of HSCPs limits their reliable utilization in wider IR applications. We herein present a new HSCP, poly(sulfur-co-hexavinyl disiloxane) (pSHVDS), prepared directly from elemental sulfur through sulfur vapor chemical deposition (sCVD). By employing hexavinyl disiloxane (HVDS) comonomer with high functionality (f = 12) and weak absorption in the IR range, despite the poor compatibility between sulfur and HVDS, the sCVD process enables the preparation of highly cross-linked HSCP with 68 wt % sulfur. Furthermore, the combination of high refractive index (RI) of 1.842, high glass transition temperature (T g ) of 151 °C, and high transparency in visible, mid- and long-wave IR range is achieved successfully, which is an unprecedentedly unique property compared to HSCPs reported to date. These favorable properties of pSHVDS render the material ideal for antireflection applications in IR optics, and conformal pSHVDS coatings on germanium IR lenses significantly improved the transmittance in mid- and long-wave IR regions. The developed polymer will lead the new possibility for polymer based optical devices, especially in the IR range.

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“…Recently, a cyclosiloxane hybrid polymer (CHP) was fabricated from tetra-functional monomers. CHP has gained much attention due to its molecularly smooth highly cross-linked hybrid network, thermal stability, and hard but elastic nature. − Compared to linear polysiloxane, CHP has better thermal stability due to reduction in “back-biting” of linear siloxane chains . Previous studies have shown the nano-size structure of CHP to be layered but isotropic in bulk due to different orientations of nano-sized layers .…”

Section: Introductionmentioning

confidence: 99%

Anchoring Effect of Hyperbranched Carborane in Highly Cross-Linked Cyclosiloxane Networks toward High-Performance Polymers

Chen

et al. 2023

Macromolecules

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High-performance polymers (HPPs) have good thermal and mechanical properties even under harsh environments and are widely used in aerospace, microelectronics, automobile, and other fields. Traditional employed highly cross-linked HPPs tend to fail in their performance at high temperatures due to the structural defects, which remains a challenge in both scientific investigation and engineering applications for decades. Herein, we employed a cyclosiloxane hybrid polymer (CHP) to investigate a new design strategy to compensate for the structural defects in the highly cross-linked network, which avoids catastrophic failure at high temperatures. Hyperbranched o-carborane was synthesized and used to compensate for structural defects of CHP. The antioxidant ability and toughness of CHP were improved, and it had better mechanical properties over a wide temperature range. Moreover, the anchoring effect of hyperbranched o-carborane in the cyclosiloxane network was systematically investigated. The hyperbranched o-carborane cage could stabilize the CHP network under dynamic thermal stress through anchoring the dangling bonds, and the highly cross-linked network suppressed the disintegration of the o-carborane cage by anchoring boron atoms of the ocarborane cage. Furthermore, the structural evolution mechanism of the o-carborane cage with increasing temperature was proposed. This fundamental research provided new insights into the design of HPPs for harsh environments.

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Synthesis and characterization of polysulfides formed by the inverse vulcanisation of cyclosiloxanes with sulfur

Cited by 9 publications

References 48 publications

Reaction between 1,3,5‐Triisopropylbenzene and Elemental Sulfur Extending the Scope of Reagents in Inverse Vulcanization

Reaction between 1,3,5‐Triisopropylbenzene and Elemental Sulfur Extending the Scope of Reagents in Inverse Vulcanization

Visible, Mid- and Long-Wave Infrared Transparent Sulfur-Rich Polymer with Enhanced Thermal Stability

Anchoring Effect of Hyperbranched Carborane in Highly Cross-Linked Cyclosiloxane Networks toward High-Performance Polymers

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