Study on Synthesis of Cyclotriphosphazene Containing Aminopropylsilicone Functional Group as Flame Retardant

2013 ◽  
Vol 683 ◽  
pp. 25-29 ◽  
Author(s):  
Lan Lan He ◽  
Yi Zhang ◽  
Zhao Lu Qin ◽  
Yan Hua Lan ◽  
Ding Hua Li ◽  
...  
Keyword(s):  
Flame Retardant ◽  
Chemical Structure ◽  
Gel Permeation Chromatography ◽  
Molar Ratio ◽  
Reaction Conditions ◽  
Element Analysis ◽  
Fourier Transformed Infrared Spectroscopy ◽  
Industrial Grade ◽  
Distribution Calculation ◽  
Optimum Reaction

A novel non-halogen flame retardant APESP, cyclotriphosphazene containing six aminopropyltriethoxysilicone functional groups N3P3[NH(CH2)3Si(OCH2CH3)3]6, was synthesized by menas of SN2 nucleophilic substitution reaction, using hexachlorocyclotriphosphazene(HCCP) and 3-aminopropyltriethoxy-silane (KH550) as material. Firstly the industrial grade HCCP was purified through recrystallization and sublimation. Then the reaction process was investigated to prompt the yield, and the optimum reaction conditions were as follows: triethylamine as acid-binding agent, tetrahydrofuran as solvent, HCCP/KH550/triethylamine molar ratio 1:7.2:7.2, dripping time: 1 hour, temperature: 67°C and reaction time: 20h. Maximum APESP yield reached 94.3%. The chemical structure and purity was characterized by element analysis, Fourier-transformed infrared spectroscopy (FTIR), mass spectrum, gel permeation chromatography (GPC) and nuclear magnetic resonance (NMR) analysis. The results showed that the structure of synthesized product is consistent with the theoretical structure, in which the chlorine atoms were completely substituted. The charge distribution calculation of HCCP and KH550 confirmed the reaction mechanism.

Study on the Synthesis of Isoamyl Acetate Catalyzed by Strong Acidic Cation Exchange Resin

2011 ◽  
Vol 396-398 ◽  
pp. 2411-2415 ◽  
Author(s):  
Ping Lan ◽  
Li Hong Lan ◽  
Tao Xie ◽  
An Ping Liao
Keyword(s):  
Acetic Acid ◽  
Reaction Time ◽  
Cation Exchanger ◽  
Cation Exchange Resin ◽  
Isoamyl Acetate ◽  
Molar Ratio ◽  
Esterification Reaction ◽  
Reaction Conditions ◽  
Optimum Reaction

Isoamyl acetate was synthesized from isoamylol and glacial acetic acid with strong acidic cation exchanger as catalyst. The effects of reaction conditions such as acid-alcohol ratio, reaction time, catalyst dosage to esterification reaction have been investigated and the optimum reaction conditions can be concluded as: the molar ratio of acetic acid to isoamylol 0.8:1, reaction time 2h, 25 % of catalyst (quality of acetic acid as benchmark). The conversion rate can reach up to 75.46%. The catalytic ability didn’t reduce significantly after reusing 10 times and the results showed that the catalyst exhibited preferably catalytic activity and reusability.

1H-NMR Analysis of Degree of Substitution in N,O-Carboxymethyl Chitosans from Various Chitosan Sources and Types

2012 ◽  
Vol 506 ◽  
pp. 158-161 ◽  
Author(s):  
A. Jaidee ◽  
Pornchai Rachtanapun ◽  
S. Luangkamin
Keyword(s):  
Chemical Structure ◽  
Carboxymethyl Chitosan ◽  
Degree Of Substitution ◽  
Resonance Spectroscopy ◽  
Nmr Analysis ◽  
Reaction Conditions ◽  
H Nmr ◽  
Fourier Transformed Infrared Spectroscopy ◽  
Chitosan Oligomer ◽  
Ft Ir

N,O-Carboxymethyl chitosans were synthesized by the reaction between shrimp, crab and squid chitosans with monochloroacetic acid under basic conditions at 50°C. The mole ratio of reactants was obtained from various reaction conditions of shrimp chitosan polymer and oligomer types. The mole ratio 1:12:6 of chitosan:sodium hydroxide:monochloroacetic acid was used for preparing carboxymethyl of chitosan polymer types while carboxymethyl of chitosan oligomer types were used the mole ratio 1:6:3 of chitosan:sodium hydroxide:monochloroacetic acid. The chemical structure was analyzed by fourier transformed infrared spectroscopy (FT-IR) and proton nuclear magnatic resonance spectroscopy (1H-NMR). The FT-IR was used for confirm the insertion of carboxymethyl group on chitosan molecules. The 1H-NMR was used for determining the degree of substitution (DS) of carboxymethylation at hydroxyl and amino sites of chitosans. Carboxymethyl chitosan samples had the total DS of carboxymethylation ranging from 1.0-2.2. The highest of DS of carboxymethylation was from shrimp chitosan oligomer type.

scholarly journals Simplified Method to Optimize Enzymatic Esters Syntheses in Solvent-Free Systems: Validation Using Literature and Experimental Data

Catalysts ◽  
2021 ◽  
Vol 11 (11) ◽  
pp. 1357
Author(s):  
Ronaldo Rodrigues de Sousa ◽  
Ayla Sant’Ana da Silva ◽  
Roberto Fernandez-Lafuente ◽  
Viridiana Santana Ferreira-Leitão
Keyword(s):  
Immobilized Lipase ◽  
Solvent Free ◽  
Molar Ratio ◽  
Mathematical Tool ◽  
Enzymatic Esterification ◽  
Reaction Conditions ◽  
Reaction Behavior ◽  
Optimum Reaction ◽  
Interesting Correlation ◽  
Using Data

The adoption of biocatalysis in solvent-free systems is an alternative to establish a greener esters production. An interesting correlation between the acid:alcohol molar ratio and biocatalyst (immobilized lipase) loading in the optimization of ester syntheses in solvent-free systems had been observed and explored. A simple mathematical tool named Substrate-Enzyme Relation (SER) has been developed, indicating a range of reaction conditions that resulted in high conversions. Here, SER utility has been validated using data from the literature and experimental assays, totalizing 39 different examples of solvent-free enzymatic esterifications. We found a good correlation between the SER trends and reaction conditions that promoted high conversions on the syntheses of short, mid, or long-chain esters. Moreover, the predictions obtained with SER are coherent with thermodynamic and kinetics aspects of enzymatic esterification in solvent-free systems. SER is an easy-to-handle tool to predict the reaction behavior, allowing obtaining optimum reaction conditions with a reduced number of experiments, including the adoption of reduced biocatalysts loadings.

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.

A New Technological Study on Synthesis of Bis(2-chloroethoxy)Methane

2014 ◽  
Vol 1033-1034 ◽  
pp. 7-11
Author(s):  
Yan Bai ◽  
Xuan Tang ◽  
Kui Zhou ◽  
Cun She Zhang
Keyword(s):  
Mass Fraction ◽  
Acid Catalysis ◽  
Molar Ratio ◽  
Optimum Conditions ◽  
Reaction Conditions ◽  
Ethylene Chlorohydrin ◽  
Optimum Reaction ◽  
Chromatographic Detection ◽  
Catalyst Dosage ◽  
Technological Study

bis(2-chloroethoxy)methane was synthesized by the reaction of ethylene chlorohydrin and Oligopolyformaldehyde under sulfuric acid catalysis. optimum reaction conditions obtained were as follows: the molar ratio of Oligopolyformaldehyde and ethylene chlorohydrin of 1.2:2, catalyst dosage was 5‰mass fraction of ethylene chlorohydrin, toluene were chose as water-carrying agent, All reactant were refluxed on temperature of 110°C until no water generated. Under the optimum conditions the yield of bis(2-chloroethoxy)methane was 97.7%. The structure of bis(2-chloroethoxy)methane were conformed by ATR IR. The purity of bis(2-chloroethoxy)methane were 99% by gas chromatographic detection.

Catalytic Synthesis of Isoamyl Acetate Catalyzed by (NH4)6[MnMo9O32]•8H2O Supported Activated Carbon with Waugh Structure

2013 ◽  
Vol 781-784 ◽  
pp. 190-193
Author(s):  
Mei Xu ◽  
Hua Yuan ◽  
Wei Liu ◽  
Jian Wang ◽  
Feng Zhen Yang
Keyword(s):  
Acetic Acid ◽  
Activated Carbon ◽  
Reaction Time ◽  
Conversion Rate ◽  
Isoamyl Alcohol ◽  
Isoamyl Acetate ◽  
Catalytic Synthesis ◽  
Molar Ratio ◽  
Reaction Conditions ◽  
Optimum Reaction

The synthesis of isoamyl acetate with ammonium 9-molybdate manganese heteropolyacid salt supported activated carbon as catalyst was studied. The optimum reaction conditions are obtained as follows: isoamyl alcohol to acetic acid molar ratio = 1.646, the weight of catalyst is 40% of total weigh, m (acidulate catalyst)=0.2g, m (water carrying reagent toluene) = 3ml, reaction time is about 63 minutes. Selectivity is 100% and conversion rate is 89.48%.

scholarly journals Two-Stage Conversion of High Free Fatty AcidJatropha curcasOil to Biodiesel Using Brønsted Acidic Ionic Liquid and KOH as Catalysts

2014 ◽  
Vol 2014 ◽  
pp. 1-9 ◽  
Author(s):  
Subrata Das ◽  
Ashim Jyoti Thakur ◽  
Dhanapati Deka
Keyword(s):  
Ionic Liquid ◽  
Molar Ratio ◽  
Reaction Conditions ◽  
Two Stage ◽  
Second Stage ◽  
Stage Conversion ◽  
Acidic Ionic Liquid ◽  
Brønsted Acidic Ionic Liquid ◽  
Optimum Reaction ◽  
Stage Process

Biodiesel was produced from high free fatty acid (FFA)Jatropha curcasoil (JCO) by two-stage process in which esterification was performed by Brønsted acidic ionic liquid 1-(1-butylsulfonic)-3-methylimidazolium chloride ([BSMIM]Cl) followed by KOH catalyzed transesterification. Maximum FFA conversion of 93.9% was achieved and it reduced from 8.15 wt% to 0.49 wt% under the optimum reaction conditions of methanol oil molar ratio 12 : 1 and 10 wt% of ionic liquid catalyst at 70°C in 6 h. The ionic liquid catalyst was reusable up to four times of consecutive runs under the optimum reaction conditions. At the second stage, the esterified JCO was transesterified by using 1.3 wt% KOH and methanol oil molar ratio of 6 : 1 in 20 min at 64°C. The yield of the final biodiesel was found to be 98.6% as analyzed by NMR spectroscopy. Chemical composition of the final biodiesel was also determined by GC-MS analysis.

Optimization of Chiral Resolution of (+/-)-1-Phenylethanol by Statistical Methods

2011 ◽  
Vol 9 (1) ◽  
Author(s):  
Ganapati D. Yadav ◽  
Jyoti B. Sontakke
Keyword(s):  
Kinetic Resolution ◽  
Batch Reactor ◽  
Immobilized Lipase ◽  
Enantiomeric Excess ◽  
Molar Ratio ◽  
Catalyst Loading ◽  
Acyl Donor ◽  
Reaction Conditions ◽  
Optimum Reaction ◽  
Synthetic Intermediate

Optically active 1-phenylethanol is used as a chiral building block and synthetic intermediate in pharmaceutical and fine-chemical industries. Lipase - catalyzed kinetic resolution of (R,S)-1-phenylethanol with vinyl acetate as an acyl donor and Candida antarctica immobilized lipase as a biocatalyst in a batch reactor was optimized using Response Surface Methodology (RSM). Four-factor-five-level central composite rotatable design (CCRD) was employed to evaluate the effect of synthesis parameters such as speed of agitation, enzyme loading, temperature and acyl donor/alcohol molar ratio, on conversion, enantiomeric excess (ee), enantioselectivity and initial rate. Optimum reaction conditions obtained were; mole ratio of acyl donor: ester of 2:1, temperature of 42.5 °C, catalyst loading of 1.6x10-3 g.cm-3 and speed of agitation of 336 rpm. Analysis of variance was performed to determine significantly affecting variables and interactions between the process parameters.

scholarly journals A novel betaine type asphalt emulsifier synthesized and investigated by online FTIR spectrophotometric method

2015 ◽  
Vol 21 (1-1) ◽  
pp. 113-121 ◽  
Author(s):  
Laishun Shi ◽  
Meijie Sun ◽  
Na Li ◽  
Bochen Zhang
Keyword(s):  
Experimental Data ◽  
Lauric Acid ◽  
Chemical Structure ◽  
Ftir Analysis ◽  
Mass Ratio ◽  
Optimum Conditions ◽  
Reaction Conditions ◽  
Optimum Reaction ◽  
Ftir Technique ◽  
Online Ftir

A novel betaine type asphalt emulsifier 3-(N,N,N-dimethyl acetoxy ammonium chloride)-2-hydroxypropyl laurate was synthesized after three steps by the reaction of lauric acid, epichlorohydrin, dimethylamine and sodium chloroacetate. The optimum reaction conditions were obtained for the synthesis of the first step of 3-chloro-2-hydroxypropyl laurate. The esterification yield reaches 97.1% at the optimum conditions of reaction temperature 80?C, reaction time 6 h, feedstock mole ratio of epichlorohydrin to lauric acid 1.5, mass ratio of catalyst to lauric acid 2%. The chemical structure of the product was characterized by FTIR and 1H NMR. The first synthesis step of 3-chloro-2-hydroxypropyl laurate was monitored by online FTIR technique. The by-product was detected by the online FTIR analysis. Based upon the experimental data, a plausible reaction mechanism was proposed for the reaction. The CMC of the objective product has a lower value of 7.4?10-4 mol/L. The surface tension at CMC is 30.85 mN/m. The emulsifier is a rapid-set asphalt emulsifier.

Synthesis of Graft Copolymers of Acrylamide and Comonomers on to Cellulose: A Study of the Effect of Comonomer on Polymer Yields, Structure and Properties

2003 ◽  
Vol 11 (1) ◽  
pp. 19-29 ◽  
Author(s):  
Ghanshyam S. Chauhan ◽  
Lalit Guleria ◽  
Harinder Lal
Keyword(s):  
Graft Copolymers ◽  
Thermal Studies ◽  
Molar Ratio ◽  
Structure And Properties ◽  
Reaction Conditions ◽  
Synthetic Strategy ◽  
Grafting Reactions ◽  
Optimum Reaction ◽  
Ft Ir ◽  
Graft Chain

Cellulose extracted from pine needles was graft copolymerized with acrylamide using benzoyl peroxide as initiator. Following a novel synthetic strategy and using the optimum reaction conditions evaluated for the grafting of acrylamide, some comonomers viz: glycidyl methacrylate, 2-hydroxyethyl methacrylate, acrylic acid and acrylonitrile have been grafted along with acrylamide using five different concentrations of the comonomers. SEM, FT-IR and thermal studies of graft copolymers were carried to obtain evidence of the incorporation of acrylamide and comonomers into cellulose. Reactivity of acrylamide in grafting reactions alone and in the presence of comonomers has been studied. The molar ratio of acrylamide and comonomers, and hence the structure of the graft chain remains independent of the comonomer concentration in the feed. It has also been observed that compared to acrylamide, less acrylonitrile was incorporated while far higher amount of the methacrylates were incorporated in the graft chain.

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