A convenient route to distannanes, oligostannanes, and polystannanes

2010 ◽  
Vol 88 (10) ◽  
pp. 1046-1052 ◽  
Author(s):  
Aman Khan ◽  
Robert A. Gossage ◽  
Daniel A. Foucher
Keyword(s):  
Molecular Weight ◽  
Gel Permeation Chromatography ◽  
Low Pressure ◽  
Inert Atmosphere ◽  
Major Product ◽  
Molar Ratio ◽  
Reaction Conditions ◽  
Gel Permeation ◽  
Highly Dispersed ◽  
Convenient Route

The quantitative conversion of the tertiary stannane (n-Bu)3SnH (2) into (n-Bu)6Sn2 (4) was achieved by heating the neat hydride material under low pressure or under closed inert atmosphere conditions. A 31% conversion of Ph3SnH (3) to Ph6Sn2 (5) was also observed under low pressure; however, under closed inert atmosphere conditions afforded Ph4Sn (6) as the major product. A mixed distannane, (n-Bu)3SnSnPh3 (7), can also be prepared in good yield utilizing an equal molar ratio of 2 and 3 and the same reaction conditions used to prepare 4. This solvent-free, catalyst-free route to distannanes was extended to a secondary stannane, (n-Bu)2SnH2 (8), which yielded evidence (NMR) for hydride terminated distannane H(n-Bu)2SnSn(n-Bu)2H (9), the polystannane [(n-Bu)2Sn]n (10), and various cyclic stannanes [(n-Bu)2Sn]n=5,6 (11, 12). Further evidence for 10 was afforded by gel permeation chromatography (GPC) where a broad, moderate molecular weight, but highly dispersed polymer, was obtained (Mw = 1.8 × 104 Da, polydispersity index (PDI) = 6.9) and a characteristic UV–vis absorbance (λmax) of ≈370 nm observed.

scholarly journals SILATRANE-CONTAINING POLYMETHACRYLATES

2019 ◽  
Vol 14 (1) ◽  
pp. 82-89 ◽  
Author(s):  
V. V. Istratov ◽  
E. V. Andreeva ◽  
V. I. Gomzyak ◽  
V. A. Vasnev
Keyword(s):  
Molecular Weight ◽  
Thermal Properties ◽  
Three Dimensional ◽  
Gel Permeation Chromatography ◽  
Inert Atmosphere ◽  
Synthetic Methods ◽  
Ir And Nmr Spectroscopy ◽  
Gel Permeation ◽  
Melting And Crystallization Temperatures ◽  
Melting And Crystallization

The possibility of synthesizing silatrane-containing polymers was investigated using three different synthetic methods: the formation of silatrane fragments from polymers with trialkoxysilyl groups, the copolymerization of silatrane-containing monomers, and the reaction of silatranes with functional copolymers. The obtained polymethacrylate copolymers were characterized using gel permeation chromatography, IR and NMR spectroscopy. It was shown that depending on the synthesis scheme used, polymers were obtained in the form of three-dimensional structures or soluble products. It was established that the molecular weight of the synthesized polymers depended significantly on both the content of silatrane fragments and the synthesis technique used. It was shown that the modification of linear carboxyl-containing copolymers by silatranes allows the synthesis of high-molecular polymers with a high content of silatrane fragments. For the synthesized polymers, thermal properties were investigated, and the hydrophobicity of the surface of polymer films was also evaluated. It was found that all the studied polymers did not have clear melting and crystallization temperatures. The polymers were stable in an inert atmosphere up to 270-280 °C, whereas in air they decomposed at lower temperatures with the restructuring of the macromolecular skeleton and the formation of highly heat-resistant silicone structures. An increase in the content of silatrane moieties in the copolymers led to an increase in the hydrophilicity of polymers.

scholarly journals A Greener Enzymatic Oligoesterification of Biobased Renewable Synthons

2021 ◽  
Author(s):  
Juan Villavicencio ◽  
Ferley Orozco ◽  
Ricardo Benitez ◽  
Jaime Martin ◽  
Giovanni Rojas
Keyword(s):  
Molecular Weight ◽  
Molar Mass ◽  
Gel Permeation Chromatography ◽  
Scanning Calorimetry ◽  
Reaction Conditions ◽  
Step Process ◽  
Gel Permeation ◽  
One Step ◽  
First Time ◽  
Temperature Time

Polyesters of xylitol and succinic acid were prepared yielding from 70 to 75% by enzymecatalyzed esterification using a molar mass from 1:1 to 2:5 at 120 and 140 °C employing from 1 to 10% m/m of enzyme. Control over branching degree was achieved by tuning the reaction conditions (temperature, time, comonomer ratio, enzyme content). This one-step process from renewable starting materials avoids protection-deprotection techniques, as well as the use of toxic solvents by introducing limonene as solvent for polyesterification for the first time. All materials were structurally characterized by infrared (IR) and nuclear magnetic resonance (NMR)spectroscopy, their thermal properties were studied by differential scanning calorimetry (DSC)and thermogravimetric analysis (TGA), and the molecular weight of samples were obtained by gel-permeation chromatography (GPC).

Study on Synthesis and Properties of Phenols Polymer Syntan Catalyzed by Enzyme

2011 ◽  
Vol 138-139 ◽  
pp. 1072-1077
Author(s):  
Sheng Hua Lv ◽  
Rui Gong ◽  
Yan Fen Ma
Keyword(s):  
Molecular Weight ◽  
Nuclear Magnetic Resonance ◽  
Fourier Transform ◽  
Infrared Spectroscopy ◽  
Average Molecular Weight ◽  
Gel Permeation Chromatography ◽  
Molar Ratio ◽  
Structure And Properties ◽  
Monomer Composition ◽  
Gel Permeation

A phenolic copolymer was synthesized from resorcinol (RSC) and 3,5-dihydroxy benzoic acid (DBA) using horseradish peroxidase (HRP)/H2O2 as the radical copolymerization’s initiateor. It was discussed that the effects of monomer composition on the properties of the copolymer. The best molar ratio was 1:1. The structure and properties of the copolymer was characterized by Fourier Transform Infrared spectroscopy (FTIR) and Nuclear Magnetic Resonance (HNMR), Molecular weight (MW) was determined by gel permeation chromatography (GPC). The result shows that the average molecular weight of the copolymer is about 40000. The effect of dosage of HRP on the properties of the copolymer was investigated. And the mechanism of polymerization of RSC and DBA was advanced. The copolymer was used as tanning agent, applied results show that it has excellent retanning properties. It was realized the applicatiom of HRP on the phenols syntan.

scholarly journals Dispersing Effect of Core Cross-linked Star Polycarboxylate Superplasticizers on the Cement Paste

2021 ◽  
Vol 283 ◽  
pp. 01048
Author(s):  
Jinlong Zhang ◽  
Furen Huang ◽  
Xiaolong Chen ◽  
Kaihong Zhong ◽  
Haijun Xu
Keyword(s):  
Aqueous Solution ◽  
Molecular Weight ◽  
Cement Paste ◽  
Conversion Efficiency ◽  
Gel Permeation Chromatography ◽  
Molar Ratio ◽  
Hydrophobic Core ◽  
Reducing Ability ◽  
Gel Permeation ◽  
Dispersing Ability

Researches on topological modification of polycarboxylate superplasticizers to improve the water-reducing or slump-retainning properties have been a hot topic in rencent years. Herein, a core crosslinked star polycarboxylate superplasticizers (SPCE) were synthesized by crosslinking the comb polycarboxylate superplasticizers (CPCE) in aqueous solution. Crosslinkers and spacing monomers were added into the polymerization to promote the formation of hydrophobic core. A larger molecular weight with 75% of yields of the SPCE were observed by gel permeation chromatography (GPC). The dispersing effect of SPCE on the cement paste was then investigated by varying the dosage of crosslinkers and spacing monomers. It was found that the dispersing ability of SPCE became weakened compared to the CPCE. More of the crosslinkers led to smaller flow spread, as revealed by cement paste experiments. Introduction of the spacing monomers contributed to the formation of SPCE. However, the dispersing ability was also weakened. Best conversion efficiency and water-reducing ability was obtained when the molar ratio of crosslinker and spacing monomer to CPCE was set as 3:5:1.

Study on Structure and Tanning Properties of Copolymer of Resorcinol and 3,5-Dihydroxyl Benzoic Acid

2012 ◽  
Vol 487 ◽  
pp. 48-52
Author(s):  
Sheng Hua Lv ◽  
Gong Rui ◽  
Di Li
Keyword(s):  
Molecular Weight ◽  
Nuclear Magnetic Resonance ◽  
Fourier Transform ◽  
Infrared Spectroscopy ◽  
Gel Permeation Chromatography ◽  
Radical Copolymerization ◽  
Mass Ratio ◽  
Monomer Composition ◽  
Chrome Tanning ◽  
Gel Permeation

The radical copolymerization of resorcinol (RSC) and 3,5-dihydroxyl benzoic (DHBA) was carried out in water by the initiator of horseradish (HRP)/H2O2. It was discussed that the effects of monomer composition on the properties of the copolymer. The best monomer mass ratio of RSC:DHBA was 60:40 and the shrink temperature can reached to 88.5oC. The tanning result indicated that the copolymer of RSC and DHPA has particularly excellent tanning properties and can be served as leather tannage substitute for chrome tanning materials. And also the mechanism of the HRP initiated copolymerization was proposed. The structure and molecular weight of the copolymer was characterized by Fourier Transform Infrared spectroscopy (FTIR), Nuclear Magnetic Resonance (NMR) and Gel Permeation Chromatography (GPC). The copolymer can be as tannage and retannage in making leather process. The results showed that it has excellent tanning properties and retanning effects.

scholarly journals Correlations between retention volume and molecular size parameters in gel permeation chromatography of small molecules

1975 ◽  
Vol 28 (1) ◽  
pp. 189 ◽  
Author(s):  
RA Shanks
Keyword(s):  
Molecular Weight ◽  
Small Molecules ◽  
Organic Molecules ◽  
Retention Volume ◽  
Molecular Size ◽  
Gel Permeation Chromatography ◽  
Molar Volumes ◽  
Small Organic Molecules ◽  
Molecular Dimension ◽  
Gel Permeation

Gel permeation columns of Bio Beads S-X8 have been used to provide separation of oligomers and other small organic molecules. Results show successful separations up to molecular weight c. 600. The retention times of compounds have been correlated with the largest molecular dimension of the molecules and also with molar volumes.

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