scholarly journals Structure–Properties Relationship in Waterborne Poly(Urethane-Urea)s Synthesized with Dimethylolpropionic Acid (DMPA) Internal Emulsifier Added before, during and after Prepolymer Formation

Polymers ◽  
2020 ◽  
Vol 12 (11) ◽  
pp. 2478
Author(s):  
Mónica Fuensanta ◽  
Abbas Khoshnood ◽  
José Miguel Martín-Martínez
Keyword(s):  
Particle Size ◽  
Phase Separation ◽  
Ph Value ◽  
Peel Test ◽  
Gravimetric Analysis ◽  
Scanning Calorimetry ◽  
Adhesion Properties ◽  
Structural Differences ◽  
Higher Temperature ◽  
Structure Properties

Dimethylolpropionic acid (DMPA) internal emulsifier has been added before, during and after prepolymer formation in the synthesis of waterborne poly(urethane-urea)s (PUDs) and their structure–properties relationships have been assessed. PUDs were characterized by pH, viscosity and particle size measurements, and the structure of the poly(urethane-urea) (PU) films was assessed by infra-red spectroscopy, differential scanning calorimetry, X-ray diffraction, thermal gravimetric analysis, plate–plate rheology and dynamic mechanical thermal analysis. The adhesion properties of the PUDs were measured by cross-hatch adhesion and T-peel test. The lowest pH value and the highest mean particle size were found in the PUD made by adding DMPA after prepolymer formation, all PUDs showed relatively ample mono-modal particle size distributions. The highest viscosity and noticeable shear thinning were obtained in the PUD made by adding DMPA during prepolymer formation. Depending on the stage of addition of DMPA, the length of the prepolymer varied and the PU films showed different degree of micro-phase separation. Because the shortest prepolymer was formed in the PU made with DMPA added before prepolymer, this PU film showed the lowest storage moduli and early melting indicating higher degree of micro-phase separation. The highest storage modulus, later melting, higher temperature and lower modulus at the cross between the storage and loss moduli corresponded to the PU made by adding DMPA after prepolymer formation, because the longer prepolymer produced during synthesis. The lowest thermal stability corresponded to the PU made by adding DMPA during prepolymer formation and the structures of all PU films were dominated by the soft domains, the main structural differences derived from the hard domains. Whereas DMPA-isophorone diisocyanate (IPDI) urethane and urea hard domains were created in the PU film made by adding DMPA during prepolymer formation, the other PU films showed DMPA-IPDI, polyester-IPDI and two different DMPA-IPDI-polyester hard domains. Finally, the adhesion properties of the PUDs and PU coatings were excellent and they were not influenced by the structural differences caused by adding DMPA in different stages of the synthesis.

scholarly journals Structural and Viscoelastic Properties of Thermoplastic Polyurethanes Containing Mixed Soft Segments with Potential Application as Pressure Sensitive Adhesives

Polymers ◽  
2021 ◽  
Vol 13 (18) ◽  
pp. 3097
Author(s):  
Mónica Fuensanta ◽  
José Miguel Martín-Martínez
Keyword(s):  
Phase Separation ◽  
Potential Application ◽  
Viscoelastic Properties ◽  
Gravimetric Analysis ◽  
Scanning Calorimetry ◽  
Adhesion Properties ◽  
Pressure Sensitive Adhesives ◽  
Thermoplastic Polyurethanes ◽  
Pressure Sensitive ◽  
Soft Segments

Thermoplastic polyurethanes (TPUs) were synthetized with blends of poly(propylene glycol) (PPG) and poly(1,4-butylene adipate) (PAd) polyols, diphenylmethane-4,4′-diisocyanate (MDI) and 1,4-butanediol (BD) chain extender; different NCO/OH ratios were used. The structure and viscoelastic properties of the TPUs were assessed by infrared spectroscopy, differential scanning calorimetry, X-ray diffraction, thermal gravimetric analysis and plate-plate rheology, and their pressure sensitive adhesion properties were assessed by probe tack and 180° peel tests. The incompatibility of the PPG and PAd soft segments and the segregation of the hard and soft segments determined the phase separation and the viscoelastic properties of the TPUs. On the other hand, the increase of the NCO/OH ratio improved the miscibility of the PPG and PAd soft segments and decreased the extent of phase separation. The temperatures of the cool crystallization and melting were lower and their enthalpies were higher in the TPU made with NCO/OH ratio of 1.20. The moduli of the TPUs increased by increasing the NCO/OH ratio, and the tack was higher by decreasing the NCO/OH ratio. In general, a good agreement between the predicted and experimental tack and 180° peel strength values was obtained, and the TPUs synthesized with PPG+PAd soft segments had potential application as pressure sensitive adhesives (PSAs).

scholarly journals New Waterborne Polyurethane-Urea Synthesized with Ether-Carbonate Copolymer and Amino-Alcohol Chain Extenders with Tailored Pressure-Sensitive Adhesion Properties

Materials ◽  
2020 ◽  
Vol 13 (3) ◽  
pp. 627 ◽  
Author(s):  
Mónica Fuensanta ◽  
Abbas Khoshnood ◽  
Francisco Rodríguez-Llansola ◽  
José Miguel Martín-Martínez
Keyword(s):  
Amino Alcohol ◽  
Peel Test ◽  
Waterborne Polyurethane ◽  
Chain Extender ◽  
Gravimetric Analysis ◽  
Scanning Calorimetry ◽  
Adhesion Properties ◽  
Oh Groups ◽  
Pressure Sensitive ◽  
Chain Extenders

New waterborne polyurethane-urea dispersions with adequate adhesion and cohesion properties have been synthesized by reacting isophorone diisocyanate, copolymer of ether and carbonate diol polyol and three amino-alcohols with different number of OH groups chain extenders using the prepolymer method. The waterborne polyurethane-urea dispersions were characterized by pH, particle-size distribution, and viscosity, and the polyurethane-urea films were characterized by attenuated total reflectance infrared (ATR-IR) spectroscopy, differential scanning calorimetry (DSC), thermal gravimetric analysis (TGA), and plate-plate rheology (temperature and frequency sweeps). Polyurethane-urea pressure-sensitive adhesives (PUU PSAs) were prepared by placing the waterborne polyurethane dispersions on polyethylene terephthalate (PET) films and they were characterized at 25 °C by creep test, tack and 180° peel test. The waterborne polyurethane-urea dispersions showed mean particle sizes between 51 and 78 nm and viscosities in the range of 58–133 mPa·s. The polyurethane-urea films showed glass transition temperatures (Tgs) lower than −64 °C, and they showed a cross of the storage and loss moduli between −8 and 68 °C depending on the number of OH groups in the amino-alcohol chain extender. Different types of PUU PSAs (removable, high shear) were obtained by changing the number of OH groups in the amino-alcohol chain extender. The tack at 25 °C of the PUU PSAs varied between 488 and 1807 kPa and the 180° peel strength values ranged between 0.4 and 6.4 N/cm, and their holding times were between 2 min and 5 days. The new PUU PSAs made with amino-alcohol chain extender seemed very promising for designing environmentally friendly waterborne PSAs with high tack and improved cohesion and adhesion property.

The Influence of Calcination Temperature on Quantitative Phase of Hematite from Iron Stone Tanah Laut

2015 ◽  
Vol 1112 ◽  
pp. 489-492
Author(s):  
Ali Mufid ◽  
M. Zainuri
Keyword(s):  
Particle Size ◽  
Calcination Temperature ◽  
Thermo Gravimetric Analysis ◽  
Precipitation Method ◽  
Gravimetric Analysis ◽  
X Ray Diffraction ◽  
Scanning Calorimetry ◽  
X Ray ◽  
Particle Size Analyzer ◽  
Co Precipitation

This research aims to form particles of hematite (α-Fe2O3) with a basis of mineral iron ore Fe3O4 from Tanah Laut. Magnetite Fe3O4 was synthesized using co-precipitation method. Further characterization using X-ray fluorescence (XRF) to obtain the percentage of the elements, obtained an iron content of 98.51%. Then characterized using thermo-gravimetric analysis and differential scanning calorimetry (TGA-DSC) to determine the calcination temperature, that at a temperature of 445 °C mass decreased by 0.369% due to increase in temperature. Further Characterization of X-ray diffraction (XRD) to determine the phases formed at the calcination temperature variation of 400 °C, 445 °C, 500 °C and 600 °C with a holding time of 5 hours to form a single phase α-Fe2O3 hematite. Testing with a particle size analyzer (PSA) to determine the particle size distribution, where test results indicate that the α-Fe2O3 phase of each having a particle size of 269.7 nm, 332.2 nm, 357.9 nm, 412.2 nm. The best quantity is shown at a temperature of 500 °C to form the hematite phase. This result is used as the calcination procedure to obtain a source of Fe ions in the manufacture of Lithium Ferro Phosphate.

scholarly journals Balanced Viscoelastic Properties of Pressure Sensitive Adhesives Made with Thermoplastic Polyurethanes Blends

Polymers ◽  
2019 ◽  
Vol 11 (10) ◽  
pp. 1608 ◽  
Author(s):  
Fuensanta ◽  
Vallino-Moyano ◽  
Martín-Martínez
Keyword(s):  
Phase Separation ◽  
Viscoelastic Properties ◽  
Simple Procedure ◽  
Peel Strength ◽  
Similar Degree ◽  
Gravimetric Analysis ◽  
Scanning Calorimetry ◽  
Pressure Sensitive Adhesives ◽  
Thermoplastic Polyurethanes ◽  
Pressure Sensitive

Pressure sensitive adhesives made with blends of thermoplastic polyurethanes (TPUs PSAs) with satisfactory tack, cohesion, and adhesion have been developed. A simple procedure consisting of the physical blending of methyl ethyl ketone (MEK) solutions of two thermoplastic polyurethanes (TPUs) with very different properties—TPU1 and TPU2—was used, and two different blending procedures have been employed. The TPUs were characterized by infra-red spectroscopy in attenuated total reflectance mode (ATR-IR spectroscopy), differential scanning calorimetry, thermal gravimetric analysis, and plate-plate rheology (temperature and frequency sweeps). The TPUs PSAs were characterized by tack measurement, creep test, and the 180° peel test at 25 °C. The procedure for preparing the blends of the TPUs determined differently their viscoelastic properties, and the properties of the TPUs PSAs as well, the blending of separate MEK solutions of the two TPUs imparted higher tack and 180° peel strength than the blending of the two TPUs in MEK. TPU1 + TPU2 blends showed somewhat similar contributions of the free and hydrogen-bonded urethane groups and they had an almost similar degree of phase separation, irrespective of the composition of the blend. Two main thermal decompositions at 308–317 °C due to the urethane hard domains and another at 363–373 °C due to the soft domains could be distinguished in the TPU1 + TPU2 blends, the weight loss of the hard domains increased and the one of the soft domains decreased by increasing the amount of TPU2 in the blends. The storage moduli of the TPU1 + TPU2 blends were similar for temperatures lower than 20 °C and the moduli at the cross over of the moduli were lower than in the parent TPUs. The improved properties of the TPU1 + TPU2 blends derived from the creation of a higher number of hydrogen bonds upon removal of the MEK solvent, which lead to a lower degree of phase separation between the soft and the hard domains than in the parent TPUs. As a consequence, the properties of the TPU1 + TPU2 PSAs were improved because good tack, high 180° peel strength, and sufficient cohesion were obtained, particularly in 70 wt% TPU1 + 30 wt% TPU2 PSA.

scholarly journals Oral Formulations of diclofenac beads and their Characterization

2019 ◽  
Author(s):  
Bushra Alquadeib
Keyword(s):  
Particle Size ◽  
Sodium Alginate ◽  
Ph Value ◽  
Diclofenac Sodium ◽  
Entrapment Efficiency ◽  
Alginate Beads ◽  
In Vitro Dissolution ◽  
Ulcer Bleeding ◽  
Scanning Calorimetry

Diclofenac sodium (DS) is an effective non-steroidal anti-inflammatory drug (NSAID) agent. However, DS has short half life and adverse effects (e.g., ulcer bleeding or perforation of intestinal wall). The objectives of this study were to improve the oral bioavailability by loading DS in sodium alginate beads. The feasibility of different concentration and stabilizers on the mean particle size (MPS) and entrapment efficiency were also investigated.Materials and methods: DS-floating alginate or pectin beads were prepared by extrusion congealing technique. Physicochemical properties and particle size characterization were evaluated using Fourier Transform Infra-Red spectroscopy (FTIR), differential scanning calorimetry. Moreover, in vitro dissolution profiles were performed for all formulated DS loaded beads. Results: MPS of the prepared spherical beads of DS ranged from 568.3 ± 193 to 1791.3 ± 592 nm. and decreasing in sodium alginate or pectin concentration to the hydroxylpropylmethlycellulose ratio favored DS beads with a smaller MPS. There was a significant reduction in MPS, increment in drug content and drug release, with reduction of sodium alginate or pectin concentrations in the formulated beads. Both DSC and FTIR spectroscopy demonstrated a some sort of interaction between the drug and polymer used. Under conditions mimicking those in the stomach, a small amount of drug was released. The DS beads showed a release behavior dependent on pH value and alginate or pectin to hydroxypropylmethylcellulose ratio.

scholarly journals Preparation, characterization and rheological behavior of chitosan nanocapsule emulsion encapsulated tuberose fragrance

2016 ◽  
Vol 18 (2) ◽  
pp. 1-8 ◽  
Author(s):  
Zuobing Xiao ◽  
Erqin Wang ◽  
Guangyong Zhu ◽  
Rujun Zhou ◽  
Yunwei Niu
Keyword(s):  
Particle Size ◽  
Molecular Mass ◽  
Fourier Transforms ◽  
Ph Value ◽  
Sodium Tripolyphosphate ◽  
Mass Ratio ◽  
X Ray Diffraction ◽  
Scanning Calorimetry ◽  
Thermogravimetric Analyzer ◽  
Preparation Conditions

Abstract In this paper, ionic gelation method was adopted to produce nanocapsules (CNs) encapsulated tuberose fragrance with chitosan (CS) and sodium tripolyphosphate (TPP) as wall materials. The effects of CS/TPP mass ratio, pH value of CS solution, molecular mass of CS and tuberose fragrance (TF) concentration on particle size and particle size distribution (PDI) of chitosan nanocapsules encapsulated tuberose fragrance (CNTs) were investigated systematically. CNTs were characterized by dynamic light scattering (DLS), scanning electron microscopy (SEM), Fourier transforms infrared spectroscopy (FTIR), X-ray diffraction (XRD), thermogravimetric analyzer (TGA) and differential scanning calorimetry (DSC). The results showed that CNTs were successfully prepared. The optimum preparation conditions were as follows: CS/TPP mass ratio 5:1, pH of CS solution 4.0, and molecular mass of CS 150 kda. CNTs emulsions were also systematically investigated by steady-state shear and oscillatory shear measurements respectively. The rheological behaviors of CNTs were obtained.

scholarly journals DEVELOPMENT OF NANOEMULSION CONTAINING PELARGONIUM GRAVEOLENS OIL: CHARACTERIZATION AND STABILITY STUDY

2016 ◽  
Vol 8 (12) ◽  
pp. 271 ◽  
Author(s):  
Janice Luehring Giongo ◽  
Rodrigo De Almeida Vaucher ◽  
Aline Ourique ◽  
MÍriam Steffler ◽  
Clarissa Piccinin Frizzo ◽  
...  
Keyword(s):  
Particle Size ◽  
Storage Temperature ◽  
Thermo Gravimetric Analysis ◽  
Physicochemical Characteristics ◽  
Stability Study ◽  
Gas Chromatography Mass Spectrometry ◽  
Gravimetric Analysis ◽  
Scanning Calorimetry ◽  
Different Temperatures ◽  
The Stability

<p><strong>Objective: </strong>To develop, characterize and evaluate the stability of nanoemulsions containing geranium oil (NEG) at different temperatures (4 °C, 25 °C and 45 °C) for 90 d.</p><p><strong>Methods: </strong>The quantification of oil in the nanostructure was performed by <a href="https://www.google.com.br/url?sa=t&amp;rct=j&amp;q=&amp;esrc=s&amp;source=web&amp;cd=1&amp;cad=rja&amp;uact=8&amp;ved=0ahUKEwiYjL3Niv7OAhVJI5AKHZ-_AeUQFggfMAA&amp;url=https%3A%2F%2Fen.wikipedia.org%2Fwiki%2FGas_chromatography%25E2%2580%2593mass_spectrometry&amp;usg=AFQjCNE3N9EyqMTXtw7u0lxolSlnU5zJfQ">gas chromatography–mass spectrometry</a> (GC-MS). The NEG was prepared in Ultra-Turrex and characterized by determining the particle size, polydispersity indices and pH. The thermo gravimetric analysis (TGA), differential scanning calorimetry (DSC) and transmission electron microscopy (TEM) to evaluate the thermal stability of the compounds, the thermal events and morphological analyses of NEG, respectively.<strong></strong></p><p><strong>Results: </strong>The results allow us to suggest that the use the ultra-turrax method is a strategy good to NEG preparation. The stability of the NEG was strongly influenced by storage temperature, with droplet size increasing rapidly at higher temperatures (45 °C), which was attributed to coalescence near the phase inversion temperature. The NEG submitted the low temperatures (4±2 °C) remained with the same particle size value (164 nm). However, the citronellol and geraniol showed a significant reduction throughout the test even in these conditions of temperature. Thermogram of NEG shows the crystallization peak at the cooling cycle in-20.1 °C and a melting was observed at 1.5 °C. TEM images indicated that NEG was spherical and nanometric.</p><p><strong>Conclusion: </strong>The proposed Ultra-Turrax method is simple which prevents volatilization of GO for the production of NEG. The formulations presented good physicochemical characteristics and stability for 90 d was only achieved in 4 °C.</p>

A Stepwise Control Route for the Preparation of Mg-Al, Zn-Al, and Mg-Fe Layered Double Hydroxides (LDHs)

2008 ◽  
Vol 368-372 ◽  
pp. 1820-1822
Author(s):  
Zhao Hui Liu ◽  
Xiao Hua Gu ◽  
Zhao Cai Zhang ◽  
Dan Wang ◽  
Cui Yu Yin ◽  
...  
Keyword(s):  
Aqueous Solution ◽  
Particle Size ◽  
Size Distribution ◽  
Layered Double Hydroxides ◽  
Room Temperature ◽  
Ph Value ◽  
Constant Ph ◽  
Double Hydroxides ◽  
Aqueous Complexes ◽  
Structure Properties

Mg-Al, Zn-Al, and Mg-Fe layered double hydroxides (LDHs) have been synthesized through a stepwise control route. In the stepwise control route, we controlled the state of Al or Fe composition as Al or Fe hydroxyl aqueous complexes in aqueous solution first, then dropwise Mg2+ or Zn2+ and OH - and keep procedure at constant pH value simultaneously at room temperature. The textural and structure properties of the resulting samples were characterized by XRD and TG-DTG. The results showed that products obtained by the stepwise control route were pure and highly crystalline LDHs. The particle size and size distribution was measured by DLLS.

Storage Problems of Poplar Chips from Short Rotation Plantations with Special Emphasis on Fungal Development

2012 ◽  
Vol 8 (1) ◽  
pp. 123-132 ◽  
Author(s):  
Zsuzsanna Horváth ◽  
Béla Marosvölgyi ◽  
Christine Idler ◽  
Ralf Pecenka ◽  
Hannes Lenz
Keyword(s):  
Particle Size ◽  
Health Risk ◽  
Dry Matter ◽  
Ph Value ◽  
Wood Chips ◽  
Raw Material ◽  
Special Focus ◽  
Fungal Development ◽  
Short Rotation ◽  
Fungal Particles

Abstract - There are several problems in storing wood chips freshly harvested from short rotation plantations, which result in quality losses as well as in dry matter and energy losses. The factors influencing the degradation of raw material are examined in this paper with special focus on fungal development. An excessive growth of fungi is connected to dry matter losses and also to an increased health risk during raw material handling. The following factors were measured during 6 months storage of poplar wood chips depending on particle size: box temperature, moisture content, pH-value, appearance of fungi in the storage and the concentration of fungal particles in the air. The results show a close connection between particle size, temperature and attack of fungi. During the storage mesophilic and termophilic species of the genera Alternaria, Aspergillus, Cladosporium, Mucor and Penicillium appeared. The concentration of fungal particles is the highest for fine chips and decreases in bigger particles. There was a special focus on the investigation of the properties of coarse chips (G 50), which represent a good compromise between handling, storage losses and health risk due to fungal development.

Optimasi Proses Pembuatan dan Karakterisasi Fisik Niosom Sinkonin

2019 ◽  
Vol 16 (2) ◽  
pp. 178
Author(s):  
Hariyanti Hariyanti ◽  
Sophi Damayanti ◽  
Sasanti Tarini
Keyword(s):  
Differential Scanning Calorimetry ◽  
Particle Size ◽  
Hair Follicle ◽  
Scanning Calorimetry ◽  
Span 60

Sinkonin praktis tidak larut dalam air, sedikit larut dalam kloroform dan alkohol. Hal ini berdampak pada rendahnya penetrasi transfollicular sinkonin, karena hanya bahan aktif hidrofilik yang mampu melewati hair follicle. Dengan demikian dibutuhkan satu sistem penghantaran yang mampu menurunkan hidrofobisitas sinkonin untuk meningkatkan penetrasi sinkonin ke follicle. Niosom merupakan vesikel ampifilik dengan struktur lapisan rangkap yang terbentuk dari hidrasi kombinasi surfaktan nonionik dan kolesterol yang mampu menurunkan hidrofobisitas sinkonin. Penelitian ini bertujuan untuk menentukan proses pembuatan niosom sinkonin yang optimum. Pembuatan niosom sinkonin diawali dengan menentukan temperatur gelasi (Tg) dari span 60 dengan Differential Scanning Calorimetry (DSC), kemudian dilanjutkan dengan optimasi proses meliputi: optimasi kecepatan rotavapor pembentukan film lapis tipis, temperatur hidrasi, kecepatan rotavapor hidrasi, waktu hidrasi, dan waktu sonikasi. Karakteristik vesikel niosom yang optimal meliputi: ukuran partikel dan indeks polidispersitas dengan menggunakan Particle Size Analized (PSA) serta efisiensi penjeratan sinkonin dengan menggunakan KCKT. Temperatur gelasi (Tg) span 60 45±2 oC, kecepatan rotavapor pembentukan film lapis tipis niosom 210 rpm, temperatur hidrasi 55±2 oC, kecepatan rotavapor hidrasi 210 rpm, waktu hidrasi 20 menit, waktu sonikasi suspensi niosom 1 menit. Ukuran vesikel yang diperoleh adalah 100–200 nm, indeks polidispersitas 0,2–0,4 dan efisiensi penjeratan niosom sinkonin 84,49±0,0025%. Proses pembuatan niosom sinkonin memiliki pengaruh besar terhadap hasil ukuran vesikel dan efisiensi penjeratan niosom sinkonin.

Sign in / Sign up

Export Citation Format

Share Document