scholarly journals Preparation of Higher Molecular Weight Poly (L-lactic Acid) by Chain Extension

2013 ◽  
Vol 2013 ◽  
pp. 1-6 ◽  
Author(s):  
Chenguang Liu ◽  
Yuliang Jia ◽  
Aihua He
Keyword(s):  
Molecular Weight ◽  
Lactic Acid ◽  
Average Molecular Weight ◽  
Hexamethylene Diisocyanate ◽  
Chain Extension ◽  
Poly Lactic Acid ◽  
Weight Changes ◽  
H Nmr ◽  
Left Handed ◽  
Ft Ir

High molecular weight poly (lactic acid) (PLA) was obtained by chain extending with hexamethylene diisocyanate (HDI). The influences of the amount of chain extender, reaction time, and molecular weight changes of prepolymers on the poly(lactic acid) were investigated. PLA prepolymer with a viscosity, average molecular weight (Mη) of 2 × 104 g/mol was synthesized froml-lactide using stannous octoate as the catalyst. After 20 min of chain extension at 175°C, the resulting polymer hadMwof 20.3 × 104 g/mol andMnof 10.5 × 104 g/mol. Both FT-IR and1H-NMR verified that the structure of PLA did not change either before chain extending or after. The optically active characterized that the chain extending-product was left handed. DSC and XRD results showed that both theTgand the crystallinity of PLA were lowered by chain-extension reaction. The crystalline transformation happened in PLA after chain extending, crystallineα′form toαform.

The Preparation of Poly(lactic acid) via Chain Linked Hydroxy-Terminated Lactic Acid Prepolymer

2011 ◽  
Vol 410 ◽  
pp. 337-340
Author(s):  
Suek Songprateepkul ◽  
Suriyan Rakmae ◽  
C. Deeprasertkul ◽  
Nitinat Suppakarn ◽  
Pranee Chumsamrong
Keyword(s):  
Molecular Weight ◽  
Lactic Acid ◽  
Average Molecular Weight ◽  
Glass Tube ◽  
Acid Value ◽  
Chain Extender ◽  
Hexamethylene Diisocyanate ◽  
Poly Lactic Acid ◽  
Weight Average Molecular Weight ◽  
A Chain

In this work, hydroxyl-terminated lactic acid prepolymer was firstly prepared by adding diethylene glycol in the condensation of lactic acid. Molecular weight, acid value and structure of prepolymer were characterized. The results showed that the prepolymer was hydroxyl-terminated with weight average molecular weight (MW) of 10,000 g/mol. After that, the chain linking polymerization of the prepolymer was carried out in a glass tube at 160 °C for 1 h employing 1,6-hexamethylene diisocyanate (HMDI) as a chain extender. By varying the hydroxyl/isocyanate ratio, it was found that the OH/NCO ratio of 1:2 seemed to be the most suitable ratio which gave PLA with the maximum MW of 93,000 g/mol.

scholarly journals Poly(lactic Acid): A Versatile Biobased Polymer for the Future with Multifunctional Properties—From Monomer Synthesis, Polymerization Techniques and Molecular Weight Increase to PLA Applications

Polymers ◽  
2021 ◽  
Vol 13 (11) ◽  
pp. 1822
Author(s):  
Evangelia Balla ◽  
Vasileios Daniilidis ◽  
Georgia Karlioti ◽  
Theocharis Kalamas ◽  
Myrika Stefanidou ◽  
...  
Keyword(s):  
Molecular Weight ◽  
Lactic Acid ◽  
Chain Extension ◽  
Poly Lactic Acid ◽  
Plastic Pollution ◽  
Practical Applications ◽  
Decomposition Reactions ◽  
Melt Polycondensation ◽  
Polymerization Conditions ◽  
Molecular Weight Increase

Environmental problems, such as global warming and plastic pollution have forced researchers to investigate alternatives for conventional plastics. Poly(lactic acid) (PLA), one of the well-known eco-friendly biodegradables and biobased polyesters, has been studied extensively and is considered to be a promising substitute to petroleum-based polymers. This review gives an inclusive overview of the current research of lactic acid and lactide dimer techniques along with the production of PLA from its monomers. Melt polycondensation as well as ring opening polymerization techniques are discussed, and the effect of various catalysts and polymerization conditions is thoroughly presented. Reaction mechanisms are also reviewed. However, due to the competitive decomposition reactions, in the most cases low or medium molecular weight (MW) of PLA, not exceeding 20,000–50,000 g/mol, are prepared. For this reason, additional procedures such as solid state polycondensation (SSP) and chain extension (CE) reaching MW ranging from 80,000 up to 250,000 g/mol are extensively investigated here. Lastly, numerous practical applications of PLA in various fields of industry, technical challenges and limitations of PLA use as well as its future perspectives are also reported in this review.

scholarly journals Synthesis of polylactic acid-diol (PLA-diol) from lactic acid and 1,4-butanediol

2016 ◽  
Vol 19 (4) ◽  
pp. 58-65
Author(s):  
Ha Thi Thai La
Keyword(s):  
Molecular Weight ◽  
Lactic Acid ◽  
Polyethylene Glycol ◽  
1H Nmr ◽  
Biodegradable Polymer ◽  
Average Molecular Weight ◽  
Chain Extension ◽  
Structure And Properties ◽  
Chain Reaction ◽  
A Chain

In this research, the PLA-diol were synthesized from lactic acid (LA) and 1.4 butanediols (BD) with a tin octoate Sn(Oct)2 catalyst at a temperature of 180 °C and the pressure 5 mmHg. The structure and properties of PLA-diol are analyzed by the following methods: GPC, 1H-NMR and DSC. As a result, with the change in the content of Sn (Oct)2 from 0.1 to 1.0%, the molecular weight Mn of PLA - diol increased gradually from 4.119,2 to 7.359,6 g / mol . In addition, the BD content increased from 2.0% to 5.0%, the average molecular weight of the product decreased gradually from 7.536,9 g / mol to 4.735 g / mol, respectively. This change will affect the ability to use PLA-diol in the next denaturation research to apply in the field of biodegradable polymer such as copolymer with polyurethane, copolymer with polyethylene glycol diacid, or chain extension with other polymer in a chain reaction,...

A New Green Process for Synthesising High Quality PLLA Materials

2013 ◽  
Vol 750-752 ◽  
pp. 1377-1380 ◽  
Author(s):  
Hui Li Shao ◽  
Xian Jue Zhou ◽  
Xue Chao Hu
Keyword(s):  
Molecular Weight ◽  
Ring Opening ◽  
Average Molecular Weight ◽  
Gel Permeation Chromatography ◽  
Ring Opening Polymerization ◽  
Green Process ◽  
Weight Average Molecular Weight ◽  
H Nmr ◽  
Ft Ir ◽  
C Nmr

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.

Preparation and Characterization of Poly(lactic acid) with Different Molecular Weights by Thermal Hydrolysis

2013 ◽  
Vol 440 ◽  
pp. 19-24 ◽  
Author(s):  
Jun Yan Yao ◽  
Loogn Tak Lim ◽  
Yu Jie Li
Keyword(s):  
Molecular Weight ◽  
Lactic Acid ◽  
Hydroxyl Group ◽  
Poly Lactic Acid ◽  
Thermal Hydrolysis ◽  
Molecular Weights ◽  
Hydrolytic Reaction ◽  
Structures And Properties ◽  
Ft Ir

A feasible and effective method of thermal hydrolysis to prepare poly (lactic acid) (PLA) oligomers with different controlled molecular weight from PLA is presented in this paper. The thermal hydrolytic reaction was carried out by immerging PLA resin pellets in boiling distilled water for a certain period of time. Ester groups in PLA chains are hydrolytically degraded in the presence of water and thermal, so PLA oligomers with different molecular weight were prepared. The structures and properties of PLA oligomers were characterized by FT-IR, GPC, DSC, etc. The results showed that thermal hydrolytic reaction could effectively reduce the molecular weight of PLA, which declines with the increase of the thermal hydrolytic reaction time. Meanwhile, the content of terminal hydroxyl group, glass transition temperature, melting point of PLA oligomers prepared from thermal hydrolytic reactions exhibit gradual changes with the extension of the thermal hydrolytic time.

scholarly journals Smart-Urea-Controlled-Release-Nitrogen-Fertilizer Menggunakan Plastik Biodegradable Poli Asam Laktat Sebagai Carrier

2017 ◽  
Vol 1 (2) ◽  
Author(s):  
Mujtahid Kaavessina ◽  
Chitra Husnabilqis ◽  
Meylani Tri Hardiyanti
Keyword(s):  
Molecular Weight ◽  
Lactic Acid ◽  
Controlled Release ◽  
Nitrogen Fertilizer ◽  
Average Molecular Weight ◽  
Urea Concentration ◽  
Poly Lactic Acid ◽  
Heating Process ◽  
Toxic Substances ◽  
The Matrix

<p>Poly lactic acid is a polymer that has been developed as an alternative to substitution of conventional polymers. The properties of this polymer are biodegradable in nature and non-toxic substances. These polymers potentially can be used as a matrix for urea carries. The aim of this research was to synthesize poly lactic acid in a low molecular weight. This product can be used as a matrix that urea release controller during the process of fertilization. The methodology consisted of two stages. The first stage was polycondensation of lactic acid and degradability test. Lactic acid was mixed with SnCl2 catalyst 0.1% and heated to 138oC for 24 hours. The second stage was producing in the form of Smart Urea Controlled Release Nitrogen Fertilizer (CRNF). Urea was dissolved in poly lactic acid through a heating process at 150°C to dissolve urea with variation in urea concentration weight of  0.5%; 0.1%; 0.15%; 0.2%; 0.25%; 0.3% and CRNF granulation processes. Finally, the mixture was granulated in ambient temperature. Chemical analysis was done the molecular weight of poly lactic acid. The relationship between intrinsic viscosity  and  molecular  weight  was  used.  The  IR  spectra  (FTIR)  was  used  to  fine molecular structure. The release testing of urea from the matrix of poly lactic acid uses UV-VIS Spectrophotometer. The results showed that the average molecular weight of poly lactic acid is 1149.49 g /gmol. FTIR spectra of CRNF with variation in urea concentration weight showed the presence of groups owned by poly lactic acid and urea. The peaks are</p><p>1627.03 to 1629.92 cm-1 for the -NH group and 3478.77 to 3498.06 cm-1 for group -OH. The existence of these groups proves the existence of urea in CRNF. The release of urea from poly lactic acid occurs by diffusion. It can be seen, when urea in CRNF form immersed in water, the concentration of urea in water increase as well as the increasing immersed time.</p>

Biodegradation Behavior of PLA/PBS Blends

2013 ◽  
Vol 821-822 ◽  
pp. 937-940 ◽  
Author(s):  
Shi Jie Zhang ◽  
Yi Wen Tang ◽  
Li Hua Cheng
Keyword(s):  
Molecular Weight ◽  
Weight Loss ◽  
Lactic Acid ◽  
Average Molecular Weight ◽  
Poly Lactic Acid ◽  
Degradation Behavior ◽  
Butylene Succinate ◽  
Exponential Decrease ◽  
Degradation Time

Poly (butylene succinate) (PBS) was mixed with Poly (lactic acid) (PLA) in the melt state. The PLA/PBS blends with different constitution were produced. The samples were buried in laterite. Samples were dug out of soil after the burial for 10, 20, 30, 40, 50 and 60 days, respectively. The weight loss and molecular weight of the sample were tested. The analysis showed that the nearly exponential decrease in average molecular weight as a function of degradation time. The PLA and PBS have the similar degradation behavior in the soil.

Synthesis and Characterizations of PLLA/PEG Block Copolymers

2010 ◽  
Vol 93-94 ◽  
pp. 198-201 ◽  
Author(s):  
Thai Hien Nguyen ◽  
Atitsa Petchsuk ◽  
Pramuan Tangboriboonrat ◽  
Mantana Opaprakasit ◽  
Alice Sharp ◽  
...  
Keyword(s):  
Molecular Weight ◽  
Ring Opening ◽  
Chemical Structure ◽  
Triblock Copolymers ◽  
Hexamethylene Diisocyanate ◽  
Chain Extension ◽  
Poly Lactic Acid ◽  
Multiblock Copolymers ◽  
Molar Ratios ◽  
A Chain

Poly(lactic acid-co-ethylene glycol) (PLLA/PEG) copolymers were synthesized and their properties were characterized. The PLLA/PEG/PLLA triblock copolymers were synthesized by ring-opening polymerization from l-lactide (LLA) and PEG macroinitiator. Stannous octoate, Sn(Oct)2 was used as a catalyst. Effects of molecular weight of PEG (600, 2000 and 4000), LLA/OH molar ratios (95:5, 98:2) and a sequence of addition of the reactants on properties of the copolymers were investigated. The triblock copolymers were subsequently used in a production of multiblock copolymers by reacting with a chain-extending agent, hexamethylene diisocyanate (HMDI). Chemical structure and molecular weight of the copolymers were characterized by 1H-NMR, FTIR and GPC. The results showed that molecular weight of triblock copolymers varied from 4,500 to 10,200. After chain extension, multiblock copolymer with molecular weight of 16,490 was produced. Thermal properties of the copolymers were also examined by DSC.

The Influence of Amount of Succinic Anhydride in Chain Extension Reaction on Increasing Molecular Weight of Poly(lactic acid)

2013 ◽  
Vol 747 ◽  
pp. 148-152
Author(s):  
Chaichana Piyamawadee ◽  
Duangdao Aht-Ong
Keyword(s):  
Molecular Weight ◽  
Lactic Acid ◽  
Succinic Anhydride ◽  
Gel Permeation Chromatography ◽  
Chain Extension ◽  
Proton Nuclear Magnetic Resonance ◽  
Poly Lactic Acid ◽  
Condensation Polymerization ◽  
Scanning Calorimetry ◽  
Molar Ratios

High molecular weight PLA was successfully synthesized by chain extension reaction of hydroxylated prepolymer using succinic anhydride as a chain extender. Hydroxylated prepolymer was prepared by direct condensation polymerization of L-lactic acid in the presence of 1,4-butanediol. Various molar ratios between hydroxylated prepolymer and succinic anhydride (i.e, 1:1, 1:2, 1:3) were investigated. The results showed that succinic anhydride can help increasing molecular weight of hydroxylated prepolymer approximately up to 47% as characterized by gel permeation chromatography (GPC) technique. Proton nuclear magnetic resonance (1H-NMR) was used to investigate structure of chain-extended PLA. Differential scanning calorimetry (DSC) and thermogravimetric analysis (TGA) were used to examine thermal properties while the crystallinity was investigated by X-ray diffraction (XRD).

scholarly journals Reversible Addition-Fragmentation Chain Transfer (RAFT) Polymerization of Poly(ethylmethacrylate) with Pendant Carbazole Groups

KIMIKA ◽  
2018 ◽  
Vol 29 (1) ◽  
pp. 41-50
Author(s):  
Shienna Marie Pontillas ◽  
Florentino C. Sumera ◽  
Rigoberto C. Advincula
Keyword(s):  
Molecular Weight ◽  
Chain Transfer ◽  
Raft Polymerization ◽  
Average Molecular Weight ◽  
Gel Permeation Chromatography ◽  
Chain Extension ◽  
Conversion Characteristic ◽  
Reversible Addition ◽  
Ft Ir ◽  
Carbazole Group

Carbazole containing polymers have captured the interest of researchers for use in optoelectronics. For an important material to exhibit its optoelectronic properties intrinsic uniformity in the molecular level is required. Thus, a monomer of ethyl methacrylate with pendant carbazole group was synthesized and polymerized via Reversible Addition-Fragmentation Chain Transfer (RAFT) to produce polymers with controlled molecular weight distribution and narrow polydispersity index (PDI). This method of polymerization was compared with that of free radical polymerization by gel permeation chromatography (GPC). The RAFT’s polymerization kinetics was observed to follow a plot of number average molecular weight (Mn) versus % conversion, characteristic of living polymerization. It was also shown to possess polymer chain extension capability. The structure of the monomer and the polymers were characterized by Fourier-Transform Infrared Spectroscopy (FT-IR) and Nuclear Magnetic Resonance (NMR).

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