The Research of Silane Oligomer with Lower Valatilization Rate for Protecting Concrete

2013 ◽  
Vol 357-360 ◽  
pp. 1318-1322 ◽  
Author(s):  
Hong Yao Sun ◽  
Zheng Yang ◽  
Gao Xia Sun ◽  
Xue Feng Xu
Keyword(s):  
Molecular Weight ◽  
Gel Permeation Chromatography ◽  
Chloride Ions ◽  
Polymerization Reaction ◽  
Low Molecular Weight ◽  
Construction Process ◽  
Reaction Conditions ◽  
Hydrophobic Agent ◽  
Ft Ir ◽  
Ft Ir Spectroscopy

As one of the measures to improve the durability of concrete, silane penetrating hydrophobic agents can preserve the properties of respiratory function of concrete and can prevent the penetration from harmful medium such as chloride ions. Because of low molecular weight of the silane penetrating hydrophobic agent such as isobutyl triethoxysilane, high volatilization rate of silane can result in waste of material in construction process. The silane oligomer was obtained by radical polymerization reaction with suitable monomers, initiators and reaction conditions. Furthermore, we verified the structure of the silane oligomer by FT-IR spectroscopy and got its molecular weight by GPC(Gel Permeation Chromatography). The silane oligomer with lower volatilization rate has excellent properties of hydrophobicity, higher penetration depth and resistance to chloride ions penetration.

SYNTHESIS OF ISOTOPICALLY LABELLED OLEFINS VIA THE WITTIG REACTION

1965 ◽  
Vol 43 (5) ◽  
pp. 1614-1624 ◽  
Author(s):  
J. G. Atkinson ◽  
M. H. Fisher ◽  
D. Horley ◽  
A. T. Morse ◽  
R. S. Stuart ◽  
...  
Keyword(s):  
Molecular Weight ◽  
Dimethyl Sulfoxide ◽  
Wittig Reaction ◽  
Low Molecular Weight ◽  
Phosphonium Salts ◽  
Reaction Conditions ◽  
Selective Labelling ◽  
Wittig Reactions

A new application of the Wittig reaction to the preparation of olefins of low molecular weight which allows selective labelling in the vinyl or allyl positions with isotopes of hydrogen and carbon has been developed. Using the modification of the Wittig reaction introduced by E. J. Corey, in which a solution of the methylsulfinyl carbanion in dimethyl sulfoxide serves as the base, a series of olefins from C2 to C8 were synthesized. The synthesis was applied to the preparation of the following labelled compounds: 5-methylene-14C-bicyclo[2.2.1]hept-2-ene; propene-1-14C; 1-butene-1-14C; propene-1-d1; 2-methylpropene-1,1-d2; 2-methyl-d3-propene-3,3,3-d3; 2-methyl-2-butene-4,4,4-d3; 2-methyl-d3-2-butene-1,1,1-d3; methylene-d2-cyclohexane. For the synthesis of carbon-labelled olefins the reaction has few limitations since the intermediates and products are isotopically stable under the reaction conditions. Deuterium-labelled olefins can be obtained from deuterated formaldehyde or β-deuterated phosphonium salts, but α-deuteroketones and aldehydes and α-deuterophosphonium salts lose the isotope to the solvent.In all the Wittig reactions, benzene was formed as a by-product in 10–15% yield. The mechanism of benzene formation is probably analogous to that proposed by Seyferth involving the decomposition of a pentacovalent phosphorous intermediate.

scholarly journals Characterisation of Sequential Solvent Fractionation and Base-catalysed Depolymerisation of Treated Alkali Lignin

BioResources ◽  
2015 ◽  
Vol 10 (3) ◽  
pp. 4137-4151 ◽  
Author(s):  
Aikfei Ang ◽  
Zaidon Ashaari ◽  
Edi Suhaimi Bakar ◽  
Nor Azowa Ibrahim
Keyword(s):  
Molecular Weight ◽  
Chemical Structure ◽  
Average Molecular Weight ◽  
Gel Permeation Chromatography ◽  
Solubility Parameters ◽  
Low Molecular Weight ◽  
Sequential Fractionation ◽  
Weight Average Molecular Weight ◽  
Solvent Fractionation ◽  
Alkali Lignin

An alkali lignin (OL) with a weight-average molecular weight (Mw) of 11646 g/mol was used to prepare low-molecular weight lignin for resin synthesis. The low-molecular weight lignin feedstock was obtained via base-catalysed depolymerisation (BCD) treatments at different combined severity factors. Sequential fractionation of the OL and BCD-treated lignins using organic solvents with different Hildebrand solubility parameters were used to alter the homogeneity of the OL. The yield and properties of OL itself and OL and BCD-treated OL dissolved in propan-1-ol (F1), ethanol (F2), and methanol (F3) were determined. Regardless of the treatment applied, a small amount of OL was dissolved in F1 and F2. The BCD treatment did not increase the yield of F1 but did increase the yields of F2 and F3. Gel permeation chromatography (GPC) showed that the repolymerization reaction occurred in F3 for all BCD-treated OL, so these lignins were not suitable for use as feedstocks for resin production. The GPC, 13Carbon-nuclear magnetic resonance, and Fourier transform infrared spectroscopy analyses confirmed that the F3 in OL exhibited the optimum yield, molecular weight distribution, and chemical structure suitable for use as feedstocks for resin synthesis.

Preparation of hybrid cyanate ester resin in the presence of polysilazane and its properties

2020 ◽  
pp. 095400832095161
Author(s):  
Xiaomeng Huo ◽  
Kangkang Guo ◽  
Fan Wang ◽  
Yaping Zhu ◽  
Huimin Qi
Keyword(s):  
Ir Spectroscopy ◽  
Flexural Modulus ◽  
Cyanate Ester ◽  
Curing Temperature ◽  
Polymerization Reaction ◽  
Polymerization Temperature ◽  
Cyanate Ester Resin ◽  
Short Period ◽  
Ft Ir ◽  
Ft Ir Spectroscopy

A hybrid cyanate ester resin containing polysilazane was prepared via the prepolymerization of bisphenol-A dicyanate ester monomer (BADCy) in the presence of polysilazane (PSZ) under low temperature conditions in a short period of time. Fourier transform-infrared (FT-IR) spectroscopy and nuclear magnetic resonance (NMR) spectroscopy reveal that the polymerization reaction of BADCy can be carried out in the presence of PSZ to obtain a hybrid resin below 100°C and polymethylsilazane (PHS) exhibits an improved prepolymerization effect when compared to polydimethylsilazane (PMS). FT-IR spectroscopy and gel permeation chromatography (GPC) showed that the prepolymerization degree of the PHS/BADCy resin increased upon increasing PHS mass fraction from 0 to 12 wt%, polymerization temperature from 60 to 100°C and polymerization time from 0 to 4 h. The PHS/BADCy hybrid resins samples were prepared and their process properties were investigated by rheometry and Differential scanning calorimetry (DSC). The results indicated that their viscosity was <10 Pa.s in the temperature range of 60–130°C, and the initial curing temperature and curing exothermic enthalpy were 121.9°C and 358.9 J/g, respectively. Furthermore, the cured PHS/BADCy resin possesses excellent thermal and mechanical properties, the 5% weight loss temperature (Td5) and glass transition temperature (Tg) were 424–441°C and 273–282°C, respectively. The cured PHS/BADCy resin with 4 wt% PHS showed the highest flexural strength of 146 MPa and flexural modulus of 4.1 GPa.

scholarly journals Synthesis, Structures, Electrochemistry, and Catalytic Activity towards Cyclohexanol Oxidation of Mono-, Di-, and Polynuclear Iron(III) Complexes with 3-Amino-2-Pyrazinecarboxylate

2020 ◽  
Vol 10 (8) ◽  
pp. 2692
Author(s):  
Anirban Karmakar ◽  
Luísa M.D.R.S. Martins ◽  
Yuliya Yahorava ◽  
M. Fátima C. Guedes da Silva ◽  
Armando J. L. Pombeiro
Keyword(s):  
Coordination Polymer ◽  
Heterogeneous Catalysts ◽  
Saturated Calomel Electrode ◽  
Two Dimensional ◽  
Reaction Conditions ◽  
Ability To Act ◽  
Tert Butyl Hydroperoxide ◽  
Ft Ir ◽  
Ft Ir Spectroscopy

The synthesis and characterization of a set of iron(III) complexes, viz. the mononuclear [Fe(L)3] (1) and [NHEt3][Fe(L)2(Cl)2] (2), the dinuclear methoxido-bridged [Fe(L)2(μ-OMe)]2.DMF.1.5MeOH (3), and the heteronuclear Fe(III)/Na(I) two-dimensional coordination polymer [Fe(N3)(μ-L)2(μ-O)1/2(Na)(μ-H2O)1/2]n (4), are reported. Reactions of 3-amino-2-pyrazinecarboxylic acid (HL) with iron(III) chloride under different reaction conditions were studied, and the obtained compounds were characterized by elemental analysis, Fourier Transform Infrared (FT-IR) spectroscopy, and X-ray single-crystal diffraction. Compound 1 is a neutral mononuclear complex, whereas 2 is mono-anionic with its charge being neutralized by triethylammonium cation. Compounds 3 and 4 display a di-methoxido-bridged dinuclear complex and a two-dimensional heterometallic Fe(III)/Na(I) polynuclear coordination polymer, respectively. Compounds 3 and 4 are the first examples of methoxido- and oxido-bridged iron(III) complexes, respectively, with 3-amino-2-pyrazinecarboxylate ligands. The electrochemical study of these compounds reveals a facile single-electron reversible Fe(III)-to-Fe(II) reduction at a positive potential of 0.08V vs. saturated calomel electrode (SCE), which is in line with their ability to act as efficient oxidants and heterogeneous catalysts for the solvent-free microwave-assisted peroxidative oxidation (with tert-butyl hydroperoxide) of cyclohexanol to cyclohexanone (almost quantitative yields after 1 h). Moreover, the catalysts are easily recovered and reused for five consecutive cycles, maintaining a high activity and selectivity.

scholarly journals Fractionation of lignosulphonates released during the early stages of delignification

1983 ◽  
Vol 61 (2) ◽  
pp. 416-420 ◽  
Author(s):  
Norman G. Lewis ◽  
David A. I. Goring ◽  
Alfred Wong
Keyword(s):  
Molecular Weight ◽  
High Performance ◽  
Black Spruce ◽  
Gel Permeation Chromatography ◽  
Bimodal Distribution ◽  
High Yield ◽  
Low Molecular Weight ◽  
Lower Yield ◽  
Spruce Wood ◽  
Gel Permeation

High-yield spent bisulphite liquor (HY-SBL) from sulphonated black spruce wood (Piceamariana) was fractionated by gel permeation chromatography (GPC) and by high-performance liquid chromatography (HPLC). The GPC fractionation gave a wide bimodal distribution, whereas with HPLC, a more detailed resolution was seen with the bulk of the fraction giving several clearly defined peaks. The paucidisperse material was further concentrated by a bulk fractionation of the crude SBL which included complexing the lignosulphonates with dicyclohexylamine. The isolated paucidisperse material was found to be dialyzable and to constitute 90% of the lignosulphonate in the sample of SBL. If the bisulphite pulp obtained was recooked in fresh acid sulphite liquor to a lower yield, most of the lignosulphonate dissolved was widely polydisperse with no indication of the discrete components resolvable by HPLC. However, 25% of the lignin made soluble was in the form of the paucidisperse fractions. In all, we were able to obtain about 50% of the lignin in spruce wood as a relatively low molecular weight lignosulphonate resolvable into discrete fractions by HPLC.

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.

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