scholarly journals Synthesis of Polyurethane/Silica Modified Epoxy Polymer Based on 1,3-Propanediol for Coating Application

2017 ◽  
Vol 17 (3) ◽  
pp. 477 ◽  
Author(s):  
Lutviasari Nuraini ◽  
Evi Triwulandari ◽  
Muhammad Ghozali ◽  
Muhammad Hanafi ◽  
Jumina Jumina

Studies on the synthesis of polyurethane/silica modified epoxy polymer using 1,3-propanediol has been conducted. Synthesis of polymers made by reaction of tolonate and 1,3-propanediol (ratio NCO/OH=2.5) as the building blocks of polyurethane with diglycidyl ether bisphenol A (DGEBA) epoxy and catalyst dibutyltin dilaurate (DBTL).The total weight of the polyurethane used was 20% (w/w) of the total epoxy. Based on Fourier Transform Infrared (FTIR) and 1H-Nuclear Magnetic Resonance (1H-NMR) spectra indicated the existence of a new bond that is formed from the reaction of isocyanate group and hydroxyl group, where the hydroxyl groups derived from epoxy and 1,3-propanediol. The addition of silica (5, 10, and 15% w/w to epoxy) into the epoxy-modified polyurethane has been carried out through sol-gel reaction of tetraethyl orthosilicate (TEOS). The isocyanate conversion rate for the addition of silica 5, 10, and 15% are 95.69; 100, and 100%, respectively. The morphology and element identification by Scanning Electron Microscopy/Energy Dispersive X-Ray Analysis (SEM/EDX), showed that Si element has been successfully added in the polymer. From the tensile strength and elongation analysis, also thermal stability analysis using Thermal Gravimetric Analyzer (TGA), the increase of silica amount into the polyurethane modified epoxy did not significantly affect to thermal properties, but decrease the tensile strength of the polymer.

Author(s):  
Е.И. Костылева ◽  
А.Н. Новиков

В работе изучены способы формирования наночастиц диоксида кремния и диоксида титана золь-гель методом в молекулярной сетке полимера. Для этого проводили гидролиз тетраэтоксисилана и тетрабутоксититана в ультразвуковом поле. Продукты выделяли, термически обрабатывали для удаления побочных продуктов и воды и изучали методами оптической микроскопии, ИК-спектроскопии, совмещенным дифференциально-термическим и термогравиметрическим анализом. В результате получены высокодисперсные, наноразмерные, гидрофобные с высокоразвитой удельной поверхностью частицы. Они содержат на поверхности остаточные алкокси- и гидроксильные группы. Размеры диоксида кремния составляют 10-50 нм, диоксида титана - 50-150 нм. На размер частиц и способность к агломерации существенное влияние оказывает способ смешения компонентов. Проведен гидролиз тетраэтоксисилана и тетрабутоксититана в среде водной эмульсии полидиметилсилоксанового каучука с помощью ультразвукового диспергирования. Из полученных составов удалялась вода, их отверждали и изготавливали образцы для физико-механические испытаний. Прочность при растяжении для резин, наполненных диоксидом кремния, увеличивается с 0,7 до 3,0 МПа, относительное удлинение повышается со 100% до 140 %. Вулканизаты, наполненные диоксидом титана, имеют прочность при разрыве 0,4-2,7 МПа, относительное удлинение 100-160 %.Наилучшие результаты получены при проведении совместного гидролиза тетраэтоксисилана и тетрабутоксититана. Прочность при растяжении у данных образцов составляет 3,5 МПа, относительное удлинение 180 %. Предложенная методика одновременного золь-гель синтеза в ультразвуковом поле диоксида кремния и диоксида титана позволяет улучшать физико-механические показатели вулканизатов на основе низкомолекулярного полидиметилсилоксанового каучука. The methods of formation of silicon dioxide and titanium dioxide nanoparticles by sol-gel method in a polymer molecular grid are studied. For this purpose, hydrolysis of tetraethoxysilane and tetrabutoxytitane was carried out in an ultrasonic field. The products were isolated, thermally treated to remove by-products and water, and studied by optical microscopy, IR spectroscopy, combined differential thermal and thermogravimetric analysis. As a result, highly dispersed, nanoscale, hydrophobic particles with a highly developed specific surface area were obtained. They contain residual alkoxy and hydroxyl groups on the surface. The dimensions of silicon dioxide are 10-50 nm, titanium dioxide - 50-150 nm. The size of the particles and the ability to agglomerate are significantly influenced by the method of mixing the components. Hydrolysis of tetraethoxysilane and tetrabutoxytitane was carried out in an aqueous emulsion of polydimethylsiloxane rubber using ultrasonic dispersion. Water was removed from the obtained compositions, they were cured and samples were made for physico-mechanical tests. The tensile strength for rubbers filled with silicon dioxide increases from 0.7 to 3.0 MPa, the elongation increases from 100% to 140%. Vulcanizates filled with titanium dioxide have a tensile strength of 0.4-2.7 MPa, elongation of 100-160%. The best results were obtained during the joint hydrolysis. The tensile strength of these samples is 3.5 MPa, the elongation is 180%. The proposed method of simultaneous sol-gel synthesis in an ultrasonic field of silicon dioxide and titanium dioxide allows improving the physical and mechanical properties of vulcanizates based on low molecular weight polydimethylsiloxane rubber.


2006 ◽  
Vol 312 ◽  
pp. 211-216 ◽  
Author(s):  
Shao Yun Fu ◽  
Qin-Yan Pan ◽  
Chuan Jun Huang ◽  
Guo Yang ◽  
Xin-Hou Liu ◽  
...  

Epoxy blend matrices were prepared by incorporating polyurethane-epoxy into diglycidyl ether of bisphenol-F (DGEBF) type epoxy while SiO2/epoxy nanocomposites were made using DGEBF type epoxy and tetraethylorthosilicate (TEOS) via a sol-gel process. The mechanical properties including tensile and impact properties at 77 K of the matrices and nanocomposites were studied. The mechanical properties at room temperature were also given for the purpose of comparison with the cryogenic mechanical properties. The results showed that the incorporation of polyurethane-epoxy with a proper content into DGEBF type epoxy enhanced the mechanical properties at both room and cryogenic temperatures. Addition of SiO2 nanoparticles to DGEBF type epoxy led to significant increase in tensile strength at cryogenic temperature (77 K) while no evident change in tensile strength at room temperature. In addition, a slight enhancement by the addition of 2 wt % silica while a slight reduction by the addition of 4 wt % silica were observed in impact energy.


2020 ◽  
Vol 301 ◽  
pp. 219-226
Author(s):  
Wahida Abdul Rahman ◽  
Nur Syazwani Anuar ◽  
Noor Aishatun Majid

Natural based film have been studied as a possible replacement for the conventional films because it can be developed from natural sources. The aim of this study is to investigate the effect of acetylation contact time to the physical and mechanical properties of the jackfruit rind based cellulose acetate film. Acetylation of jackfruit rind based cellulose was studied and samples with different degree of substitution were obtained as a function of contact time from 1 hour to 24 hours. The products were characterized by saponification reaction. In this study, saponifcation reaction showed that, more hydroxyl group were substituted with acetyl groups as the contact time of acetylation increased. The Cellulose Acetate (CA) had been mixed in the gelatine matrix film. The addition of jackfruit rind based CA showed that the moisture uptake and solubility of the film decreased compared to Cellulose/Gelatine composite film. This is because acetyl groups are more hydrophobic than hydroxyl groups thus reducing the hydophilic nature of cellulose. Additionally, from the tensile test, it was proven that the film with CA of 24 hours contact time exhibits the highest tensile strength.


2005 ◽  
Vol 3 (4) ◽  
pp. 803-829 ◽  
Author(s):  
Hammed Hassan

AbstractA concise method for a stereocontrolled synthesis of a set of selectively protected disaccharides is reported. Coupling of the donor 11 onto acceptors 23 and 24, promoted by trimethylsilyl triflate-N-iodosuccinimide (TMSOTf-NIS), generated the disaccharides 25 and 26. Under typical conditions, condensation of the fully protected donor 12 onto acceptors 23 and 24 produced the disaccharides 27 and 28. The building blocks 25–28 were prepared in moderate yields having exclusive β-stereoselectivity. A unique pattern of protecting groups distinguished clearly between positions to be sulfated and functional groups remaining as free hydroxyl groups. Acetyl and/or levulinoyl esters temporarily protected the positions to be sulfated, while benzyl ethers were used for permanent protection. The anomeric positions were protected as allyl ethers, whereas the 4′-positions were masked as p-methoxybenzyl (PMB) ethers. The orthogonality of the PMB and allyl groups can then be used for further elongation of the chain by recurrent deprotection and activation steps. The hydroxyl group, OH-6, of glucosamine moieties was protected as a TBDPS ether to avoid oxidation. A five-step deprotection/sulfonation sequence was applied to the disaccharide 27 to generate the corresponding sulfated [β-D-GlcUA-2-OSO3Na-(1→4)-β-D-Glc pNAc]-(1→O-Pro) 34.


2020 ◽  
Author(s):  
Israa Bu Najmah ◽  
Nicholas Lundquist ◽  
Melissa K. Stanfield ◽  
Filip Stojcevski ◽  
Jonathan A. Campbell ◽  
...  

An insulating composite was made from the sustainable building blocks wool, sulfur, and canola oil. In the first stage of the synthesis, inverse vulcanization was used to make a polysulfide polymer from the canola oil triglyceride and sulfur. This polymerization benefits from complete atom economy. In the second stage, the powdered polymer is mixed with wool, coating the fibers through electrostatic attraction. The polymer and wool mixture is then compressed with mild heating to provoke S-S metathesis in the polymer, which locks the wool in the polymer matrix. The wool fibers impart tensile strength, insulating properties, and flame resistance to the composite. All building blocks are sustainable or derived from waste and the composite is a promising lead on next-generation insulation for energy conservation.


Molecules ◽  
2021 ◽  
Vol 26 (8) ◽  
pp. 2131
Author(s):  
Leonardo Dalseno Antonino ◽  
Júlia Rocha Gouveia ◽  
Rogério Ramos de Sousa Júnior ◽  
Guilherme Elias Saltarelli Garcia ◽  
Luara Carneiro Gobbo ◽  
...  

Several efforts have been dedicated to the development of lignin-based polyurethanes (PU) in recent years. The low and heterogeneous reactivity of lignin hydroxyl groups towards diisocyanates, arising from their highly complex chemical structure, limits the application of this biopolymer in PU synthesis. Besides the well-known differences in the reactivity of aliphatic and aromatic hydroxyl groups, experimental work in which the reactivity of both types of hydroxyl, especially the aromatic ones present in syringyl (S-unit), guaiacyl (G-unit), and p-hydroxyphenyl (H-unit) building units are considered and compared, is still lacking in the literature. In this work, the hydroxyl reactivity of two kraft lignin grades towards 4,4′-diphenylmethane diisocyanate (MDI) was investigated. 31P NMR allowed the monitoring of the reactivity of each hydroxyl group in the lignin structure. FTIR spectra revealed the evolution of peaks related to hydroxyl consumption and urethane formation. These results might support new PU developments, including the use of unmodified lignin and the synthesis of MDI-functionalized biopolymers or prepolymers.


Materials ◽  
2021 ◽  
Vol 14 (10) ◽  
pp. 2553
Author(s):  
Yu Tu ◽  
Weihua Ao ◽  
Chunhong Wang ◽  
Tianyu Ren ◽  
Lijuan Zhang ◽  
...  

Modified microspheres (SiO2-M) were obtained by the hydrolytic modification of silicon dioxide (SiO2) microspheres with Na2SiO3, and then, SiO2-M was used as a carrier to prepare a composite photocatalyst (SiO2-M/TiO2) using the sol-gel method; i.e., nano-TiO2 was loaded on the surface of SiO2-M. The structure, morphology, and photocatalytic properties of SiO2-M/TiO2 were investigated. Besides, the mechanism of the effect of SiO2-M was also explored. The results show that the hydrolytic modification of Na2SiO3 coated the surface of SiO2 microspheres with an amorphous SiO2 shell layer and increased the quantity of hydroxyl groups. The photocatalytic performance of the composite photocatalyst was slightly better than that of pure nano-TiO2 and significantly better than that of the composite photocatalyst supported by unmodified SiO2. Thus, increasing the loading capacity of nano-TiO2, improving the dispersion of TiO2, and increasing the active surface sites are essential factors for improving the functional efficiency of nano-TiO2. This work provides a new concept for the design of composite photocatalysts by optimizing the performance of the carrier.


Polymers ◽  
2021 ◽  
Vol 13 (15) ◽  
pp. 2575
Author(s):  
Smaher M. Elbayomi ◽  
Haili Wang ◽  
Tamer M. Tamer ◽  
Yezi You

The preparation of bioactive polymeric molecules requires the attention of scientists as it has a potential function in biomedical applications. In the current study, functional substitution of alginate with a benzoyl group was prepared via coupling its hydroxyl group with benzoyl chloride. Fourier transform infrared spectroscopy indicated the characteristic peaks of aromatic C=C in alginate derivative at 1431 cm−1. HNMR analysis demonstrated the aromatic protons at 7.5 ppm assigned to benzoyl groups attached to alginate hydroxyl groups. Wetting analysis showed a decrease in hydrophilicity in the new alginate derivative. Differential scanning calorimetry and thermal gravimetric analysis showed that the designed aromatic alginate derivative demonstrated higher thermo-stability than alginates. The aromatic alginate derivative displayed high anti-inflammatory properties compared to alginate. Finally, the in vitro antioxidant evaluation of the aromatic alginate derivative showed a significant increase in free radical scavenging activity compared to neat alginate against DPPH (2,2-diphenyll-picrylhydrazyl) and ABTS free radicals. The obtained results proposed that the new alginate derivative could be employed for gene and drug delivery applications.


1971 ◽  
Vol 24 (3) ◽  
pp. 521 ◽  
Author(s):  
S Ahmed ◽  
M Alauddin ◽  
B Caddy ◽  
M Martin-Smith ◽  
WTL Sidwell ◽  
...  

The preparation of 3α,12α-bisdimethylamino-5β-cholane dimethiodide, 3α,12α-bisdimethylamino-5β-cholane dimethiodide, 3α,12α- bisdimethylamino-24-nor-5β-cholanedimethiodide, and 3α,12α- bisdimethylamino-24-nor-5β-cholanediethiodide, from deoxycholic acid are described. During this work it was found that attempted copper- quinoline decarboxylation of dehydrocholic acid gives rise to lactol formation, and that what had previously been considered to be 3α,12α- dihydroxy-5β-cholane is a mixture of this compound and 12α,24- dihydroxy-5β-cholane. Comparable selectivity of attack by methanesulphonyl chloride and toluene-p-sulphonyl chloride occurs with various polyhydric alcohols derived from bile acids, as evidenced from the products of reduction of the sulphonates with lithium aluminium hydride. With both 5α- and 5β-cholane derivatives, a C 3 equatorial hydroxyl group exhibits comparable reactivity to the terminal primary hydroxyl group, generated from the bile acid carboxylic group, towards both sulphonyl chlorides. With axial hydroxyl groups at C 7 and C 12, toluene-p-sulphonate formation is much more difficult than methane- sulphonate formation. Reduction by means of lithium aluminium hydride of equatorial sulphonate esters at C 7 and C 12 gives rise to a methylene group, but the axial sulphonates under the same conditions give the axial alcohol. The same clear distinction between equatorial and axial sulphonate esters is not observed at C 3 and C 6, but 17α- methanesulphonyloxy-5α-androstane gives 5α-androstane and the 17β- ester gives 17β-hydroxy-5α-androstane. Reduction of 12-oximino groups in both 5α- and 5β-cholanes with sodium and ethanol, hydrogen in the presence of a catalyst, or lithium aluminium hydride gives solely the 12α-amino compound.


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