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

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.

In the present study, the influence of dextransucrase of Weissella cibaria NITCSK4 (DSWc4), sucrose concentration, and reaction temperature on the yield of low molecular weight dextran (LMWD-DexWc4) was investigated using mixed level Taguchi design and back propagation neural network (BPNN). BPNN model with three neurons in a hidden layer generated a low mean squared error (MSE). The determination coefficients (R2 -value) for ANN and Taguchi models were 0.991 and 0.998, respectively. Considering absolute average deviation (AAD) and MSE, Taguchi model is more adequate. Among three factors, the percentage yield of low molecular weight of dextran is invariably dependent on the sucrose concentration. The study suggested that a low sucrose concentration (3% w/v), DSWc4 (0.25 IU/ml) and slightly high temperature (35°C) ultimately favored the production of LMWD-DexWc4 (91.639%). LMW-DexWc4 produced by DSWc4 at optimized conditions was analyzed. The weight average molecular weight of LMW-DexWc4 was calculated using M-H expression, found to be 85775 (≈90 kDa). The relative percentage error between the number and weight average molecular weight was found to be less (4.42%). The polydispersity (PD) index of the LMW-DexWc4 was found to be 0.9576 and the value is close to 1. The PD value depicted that the molecular weight distribution of dextran was narrowly dispersed.


1976 ◽  
Vol 49 (5) ◽  
pp. 1290-1304
Author(s):  
M. Kurata ◽  
H. Okamoto ◽  
M. Iwama ◽  
M. Abe ◽  
T. Homma

Abstract An iterative computer method was proposed for estimating the degree of branching and molecular weight distribution simultaneously from a pair of measurements on intrinsic viscosity and gel-permeation chromatography. The validity of the method as applied to randomly branched polymers was tested by using both fractionated and unfractionated samples of branched polystyrenes. It was experimentally concluded that the average number of branch points per unit molecular weight, λ, can be determined by this method with an accuracy of about 15%, and the weight-average molecular weight with accuracy of about 10%.


2016 ◽  
Vol 54 (3) ◽  
pp. 340 ◽  
Author(s):  
Le Duc Giang ◽  
Dinh Long Mong Thao ◽  
Hoang Thi Huong ◽  
Le Thi Thu Hiep

Hydroxyl terminated liquid natural rubber (HTLNR) was prepared by the depolymerization of deproteinized natural rubber (DPNR) in mixture of toluene and water at 60oC for 24 hours in the presence of ammonium persulfate as an initiator and tetrahydrofuran (THF) as a homogenizing agent. GPC analysis revealed that the number-average molecular weight (Mn) and weight-average molecular weight (Mw) of HTLNR were found to be 4.334×103 g/mol and 11.702×103 g/mol, respectively, with polydispersity index (PDI) of  2.7. The chemical structure of HTLNR was determined by FTIR and 1H-NMR and 13C-NMR spectroscopic analysis. The mechanism of depolymerization and hydroxylation of NR to form HTNR based on the analytical data is also suggested in this study.


2013 ◽  
Vol 750-752 ◽  
pp. 1377-1380 ◽  
Author(s):  
Hui Li Shao ◽  
Xian Jue Zhou ◽  
Xue Chao Hu

Synthesis of Poly(L-lactide) (PLLA) by the ring-opening polymerization (ROP) of L-lactides in supercritical carbon dioxide (SC-CO2) with co-solvent were studied. Effects of kinds of co-solvent on the molecular weight (MW) and the molecular weight distribution (MWD) of the resultant polymers were investigated by the gel permeation chromatography (GPC). The resultant polymers were also characterized with1H NMR,13C NMR and FT-IR. It was found that PLLA with high purity and almost without racemization could be obtained by this technology and the acetone is the best co-solvent for this kind of polymerization. By using stannous octoate as initiator and acetone as co-solvent, PLLA having a weight-average molecular weight (Mw) near to 9×104and polydispersity index (PDI) of 1.7 was successfully synthesized.


2021 ◽  
Vol 50 (6) ◽  
pp. 1767-1773
Author(s):  
Manjusha Elizabeth Mathew ◽  
Ishak Ahmad ◽  
Sabu Thomas ◽  
Muhammad Kassim ◽  
Rusli Daik

Polyvinyl benzyl chloride (PVBC) was synthesized by free radical polymerization of 4-vinylbenzyl chloride using benzoyl peroxide initiator at 60 °C. PVBC was synthesised in different solvents such as toluene, xylene, 1,4-dioxane, and tetrahydrofuran. The polymers were structurally characterized by 1H NMR and FTIR spectroscopic techniques. The thermal property of the polymer was investigated by thermogravimetric analysis (TGA) and differential thermogravimetric analysis (DTA).The number average molecular weight, weight average molecular weight and polydispersity index of PVBC synthesised in different solvents were determined and compared by gel permeation chromatography technique.


2015 ◽  
Vol 2015 ◽  
pp. 1-6 ◽  
Author(s):  
Tianming Gao ◽  
Ruihong Xie ◽  
Linghong Zhang ◽  
Hongxing Gui ◽  
Maofang Huang

The aim of this work is to introduce a simple and rapid method for characterizing the molecular weight parameters and other molecular structure parameters of natural rubber (NR) using a rubber process analyzer (RPA). In this work, NR of different molecular weights was prepared by milling. Molecular weight parameters were measured by gel permeation chromatography coupled with laser light scattering (GPC-LLS) for comparison with RPA results. It was verified that increasing of milling time leads to a decrease of the number-average molecular weight (M-n), weight-average molecular weight (M-w), and molecular weight distribution (MWD). The dynamic and rheological properties were evaluated on RPA by tests of strain sweep, frequency sweep, and stress relaxation. These results were used to characterize the average molecular weight, MWD, and viscosity of NR and were found to agree with those from GPC-LLS. This convenient and rapid technology for characterizing NR molecular weight parameters would be especially useful in the elastomer industry.


1995 ◽  
Vol 60 (3) ◽  
pp. 489-497 ◽  
Author(s):  
Hynek Balcar ◽  
Jan Sedláček ◽  
Marta Pacovská ◽  
Vratislav Blechta

Catalytic activity of the tungsten aryloxo complexes WCl5(OAr) and WOCl3(OAr), where Ar = 4-t-C4H9C6H4, 2,6-(t-C4H9)2C6H3, 2,6-Cl2C6H3, 2,4,6-Cl3C6H2, and 2,4,6-Br3C6H2 in polymerization of phenylacetylene (20 °C, monomer to catalyst molar ratio = 1 000) was studied. The activity of WCl5(OAr) as unicomponent catalysts increases with increasing electron withdrawing character of the -OAr ligand. Addition of two equivalents of organotin cocatalysts (Me4Sn, Bu4Sn, Ph4Sn, Bu3SnH) to WCl5(O-C6H2Cl3-2,4 ,6) has only slight positive effect (slightly higher polymer yield and/or molecular weight of poly(phenylacetylene)s was achieved). However, in the case of WOCl3(O-C6H3Cl2-2, 6) catalyst, it enhances the activity considerably by eliminating the induction period. Poly(phenylacetylene)s prepared with the catalysts studied have weight-average molecular weight ranging from 100 000 to 200 000. They are trans-prevailing and have relatively low molar fraction of monomer units comprised in cyclohexadiene sequences (about 6%).


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