The Research on the Crystal Structure of Oxidized Starch by Microwave-Liquid Phase Method

2013 ◽  
Vol 634-638 ◽  
pp. 461-466
Author(s):  
Shan Cong ◽  
Hong Wei Zhang

Maize starches and hydrogen-peroxide were used as major raw materials to synthesize oxidized starch by microwave radiation in a few minutes. Its crystal structure was analyzed respectively by X-ray diffraction (XRD), infrared spectroscopy (FT-IR), differential scanning calorimetry(DSC) and the apparent morphology was observed by scanning electron microscope (SEM). The XRD results show that the samples’ crystallinity has declined obviously after microwave radiation for 3.0 min and 6.0 min, and the later sample formes new crystal; The FT-IR results indicate that when microwave radiation time increases, the proportion of the native crystalline structure in the sample declines; The DSC results demonstrate that in microwave radiation, some spiral structure in internal starch granule is destroyed, while the starch-starch crystal structure subjects to a certain degree of destruction; The SEM results show that with the microwave radiation time increasing, the degree of erosion on the sample particle surface increases and expands gradually into the inside.

2011 ◽  
Vol 84-85 ◽  
pp. 514-518
Author(s):  
Hong Yan Zhang ◽  
Jin Hua Wang ◽  
Li Fang Zhang ◽  
Li Li Wang

This paper is researched on SiO2-coated Cr2O3 for the hydrolysis reaction of tetraethyl orthosilicate. The influences of precursors, solid contents of suspension and Si ratio of water on coated particle surface are investigated. The products are characterized and the conclusion shows that the experimental method is feasible.


2014 ◽  
Vol 34 (7) ◽  
pp. 611-616 ◽  
Author(s):  
Shijie Cheng ◽  
Jun Xu ◽  
Yumin Wu

Abstract Oxidized starch-graft-poly(styrene-butyl acrylate) [OS-g-P(St-BA)] latex was synthesized by the graft copolymerization of OS with St and n-butyl acrylate (BA) via emulsion polymerization. The graft copolymers were characterized by Fourier transform infrared (FT-IR), transmission electronic microscopy (TEM), dynamic light scattering, thermogravimetry (TG), and differential scanning calorimetry (DSC). The effects of the amount of OS, monomers, and initiator on graft copolymerization were investigated. Under the optimal conditions, the percentage of graft (PG), grafting efficiency (GE), and ζ potential could reach 256.5%, 41.7%, and -30.1 mV, respectively. The results indicated that the OS grafted onto particles greatly enhanced the colloidal stability of latex. The thermal stability properties of OS-g-P(St-BA) were also improved by the addition of OS. The OS-g-P(St-BA) latex may be used to partly replace the conventional synthetic latex for paper coating.


2014 ◽  
Vol 2014 ◽  
pp. 1-7 ◽  
Author(s):  
Di Li ◽  
Guo-Qing Zhong

The antimony(III) complex [Sb(Hedta)]·2H2O was synthesized with ethylenediaminetetraacetic acid (H4edta) and antimonous oxide as main raw materials in aqueous solution. The composition and structure of the complex were characterized by elemental analysis, infrared spectra, single crystal X-ray diffraction, X-ray powder diffraction, thermogravimetry, and differential scanning calorimetry. The crystal structure of the antimony(III) complex belongs to orthorhombic system, space group Pna2(1), with cell parameters ofa=18.4823(18) Å,b=10.9408(12) Å,c=7.3671(5) Å,V=1489.7(2) Å3,Z=4, andDc=1.993 g cm−3. The Sb(III) ion is five-coordinated by two amido N atoms and three carboxyl O atoms from a single Hedta3−ligand, forming a distorted trigonal bipyramid geometry. The thermal decomposition processes of the complex include dehydration, oxidation, and pyrolysis of the ligand, and the last residue is Sb2O3at the temperature of 570°C.


2012 ◽  
Vol 512-515 ◽  
pp. 207-210
Author(s):  
Quan Wen ◽  
Jian Feng Huang ◽  
Li Yun Cao ◽  
Jian Peng Wu

V2O5 powders were successfully synthesized by the EDTA assistanced ultrasound sol-gel process using NH4VO3 and EDTA, NH3•H2O as raw materials. The synthesized activation energy and the influence of pH values and the calcination temperatures on the phases and microstructures of powders were particularly investigated. The precursor powders and the V2O5 powders were characterized by X-ray diffraction (XRD), fourier transform inelectron microscopy (FT-IR), scanning electron microscopy (SEM) and differential scanning calorimetry-thermal gravimetric (DSC-TG). Results show that the obtained products exhibit good crystallization under the conditions of pH=4, calcination temperature 400~500 °C and calcination time 0.5 h during the synthesizing process. The as-prepared V2O5 powders show preferred growth orientation along (001) plane at the pH=4. By DSC analysis, the ultrasonic cavitation result in the decrease in synthesized activation energy obviously than that was prepared without ultrasonic irradiation.


2016 ◽  
Vol 847 ◽  
pp. 241-248 ◽  
Author(s):  
Ya Juan Wang ◽  
Ya Li ◽  
Xin Zhang ◽  
Ning Kun Wu ◽  
Shuang Xi Shao

In order to reduce the pollution of the waste material, the waste leather powder tanned with vegetable tannin was used in this work, and vinyitrimethoxy silane was chosen as coupling agent. Thermogravimetric analysis (TGA) and differential scanning calorimetry (DSC) were used to investigate the thermal properties of the powder sample. Both thermal decomposition temperature and denaturation temperature of the modified sample were higher than those of the raw samples due to the interaction between leather powder and silane, which can be demonstrated by Scanning Electron Microscopy-Energy Dispersive Spectrometer (SEM-EDS) and Fourier Transform Infrared Spectroscopy (FT-IR). Additionally, the flowing property, hydrophilicity and water absorption rate of the powder samples was also examined. The results showed that the hydrophilicity and moisture absorption of the leather powder sample modified with silane was lower than the raw materials. And the flowing properties of the modified samples also decreased because of the coupling reaction of the flexible vinyitrimethoxy silane.


2012 ◽  
Vol 487 ◽  
pp. 714-718 ◽  
Author(s):  
Sheng Kui Zhong ◽  
Ying Mei Zhang ◽  
Wei Li ◽  
Yue Bin Xu

LiMnPO4cathode material for lithium ion batteries was synthesized by high temperature solid-phase method using MnCO3, Li2CO3, NH4H2PO4as raw materials. The structure of samples was identified by XRD analysis and the particle surface morphology was examined by SEM. The results of XRD showed that the LiMnPO4sample sintered at 700°C for 20h had single ordered olivine structure. The SEM pattern showed that spherical particles distributed uniformly. Respectively, it figured out that the initial charge and discharge capacities of the samples at 0.05C rate were 133.9 and 66.4mAh•g-1.


Polymers ◽  
2021 ◽  
Vol 13 (23) ◽  
pp. 4229
Author(s):  
David De Smet ◽  
Madeleine Wéry ◽  
Willem Uyttendaele ◽  
Myriam Vanneste

Polyurethane (PU) coatings are often applied on high added value technical textiles. Key factor to success of PU coatings is its versatility and durability. Up to today most PU textile coatings are solvent-based or water-based. Recent advances are made in applying bio-based PU on textiles. Currently, polymers made from renewable raw materials are experiencing a renaissance, owing to the trend to reduce CO2 emissions, the switch to CO2-neutral renewable products and the depletion of fossil resources. However, the application of bio-based coatings on textiles is limited. The present paper discusses the potential of a bio-based anionic PU dispersion as an environment friendly alternative for petroleum-based PU in textile coating. Coatings were applied on textile via knife over roll. The chemical, thermal and mechanical properties of the bio-based PU coating were characterised via FT-IR, thermogravimetric analysis, differential scanning calorimetry and tensile test. The performance of the coating was studied by evaluating antimicrobial properties, fire retardancy, the resistance to hydrostatic pressure initially and after washing, QUV ageing and hydrolysis test. The developed bio-based PUD coating complied to the fire retardancy test ISO 15025 and exhibited excellent hydrostatic pressure, QUV ageing resistance, hydrolysis resistance, wash fastness at 40 °C.


2017 ◽  
Vol 8 ◽  
pp. 2116-2125 ◽  
Author(s):  
Jilin Wang ◽  
Hejie Liao ◽  
Yuchun Ji ◽  
Fei Long ◽  
Yunle Gu ◽  
...  

In this work, a reaction coupling self-propagating high-temperature synthesis (RC-SHS) method was developed for the in situ controlled synthesis of novel, high activity TiB2/(TiB2–TiN) hierarchical/heterostructured nanocomposites using TiO2, Mg, B2O3, KBH4 and NH4NO3 as raw materials. The as-synthesized samples were characterized using X-ray diffraction (XRD), scanning electron microscope (SEM), X-ray energy dispersive spectroscopy (EDX), transition electron microscopy (TEM), high-resolution TEM (HRTEM) and selected-area electron diffraction (SAED). The obtained TiB2/TiN hierarchical/heterostructured nanocomposites demonstrated an average particle size of 100–500 nm, and every particle surface was covered by many multibranched, tapered nanorods with diameters in the range of 10–40 nm and lengths of 50–200 nm. In addition, the tapered nanorod presents a rough surface with abundant exposed atoms. The internal and external components of the nanorods were TiB2 and TiN, respectively. Additionally, a thermogravimetric and differential scanning calorimetry analyzer (TG-DSC) comparison analysis indicated that the as-synthesized samples presented better chemical activity than that of commercial TiB2 powders. Finally, the possible chemical reactions as well as the proposed growth mechanism of the TiB2/(TiB2–TiN) hierarchical/heterostructured nanocomposites were further discussed.


1999 ◽  
Vol 55 (6) ◽  
pp. 947-952 ◽  
Author(s):  
J. J. Criado ◽  
A. Jiménez-Sánchez ◽  
F. H. Cano ◽  
R. Sáez-Puche ◽  
E. Rodríguez-Fernández

Tetrachlorocobaltates(II) of diprotonated α,ω-diaminoalkanes with the formula [NH3(CH2) n NH3]CoCl4, where n = 5 (cadaverine; 1,5-pentanediammonium tetrachlorocobaltate), 8 (1,8-octanediammonium tetrachlorocobaltate) and 10 (1,10-decanediammonium tetrachlorocobaltate), were prepared. The compounds were studied by mass spectrometry, FT-IR and visible spectroscopy, magnetic susceptibility techniques and thermal analysis. The compounds contain the tetrahedral tetrachlorocobaltate(II) ion and the corresponding diprotonated diamine (cadaverine, 1,8-octamethylenediamine and 1,10-decamethylenediamine). The compound corresponding to cadaverine crystallizes in the monoclinic space group P21/c, with lattice parameters a = 7.1633 (7), b = 15.940 (3), c = 11.137 (2) Å, β = 98.44 (1)° and Z = 4. Its crystal structure contains slightly distorted tetrahedral CoCl_4^{2-} ions: the largest difference in Co—Cl bond lengths is 0.029 Å and the largest difference in Cl—Co—Cl angles is 7.76°. The compound also contains diprotonated cadaverine ions. An extensive hydrogen-bonding network connects these ions. The slightly positive deviations of the magnetic susceptibility from the Curie–Weiss law are in agreement with the 4 A 2 ground state for the tetrachlorocobaltate anion. The compounds with eight and ten C atoms show phase transitions in the solid state and a greater complexity is observed in their differential scanning calorimetry curves. Unfortunately, no suitable single crystals of these could be obtained.


Author(s):  
Nehemiah Harris ◽  
Jubilee Benedict ◽  
Diane A. Dickie ◽  
Silvina Pagola

Quinine (an antimalarial) and aspirin (a nonsteroidal anti-inflammatory drug) were combined into a new drug–drug salt, quininium aspirinate, C20H25N2O2 +·C9H7O4 −, by liquid-assisted grinding using stoichiometric amounts of the reactants in a 1:1 molar ratio, and water, EtOH, toluene, or heptane as additives. A tetrahydrofuran (THF) solution of the mechanochemical product prepared using EtOH as additive led to a single crystal of the same material obtained by mechanochemistry, which was used for crystal structure determination at 100 K. Powder X-ray diffraction ruled out crystallographic phase transitions in the 100–295 K interval. Neat mechanical treatment (in a mortar and pestle, or in a ball mill at 20 or 30 Hz milling frequencies) gave rise to an amorphous phase, as shown by powder X-ray diffraction; however, FT–IR spectroscopy unambiguously indicates that a mechanochemical reaction has occurred. Neat milling the reactants at 10 and 15 Hz led to incomplete reactions. Thermogravimetry and differential scanning calorimetry indicate that the amorphous and crystalline mechanochemical products form glasses/supercooled liquids before melting, and do not recrystallize upon cooling. However, the amorphous material obtained by neat grinding crystallizes upon storage into the salt reported. The mechanochemical synthesis, crystal structure analysis, Hirshfeld surfaces, powder X-ray diffraction, thermogravimetry, differential scanning calorimetry, FT–IR spectroscopy, and aqueous solubility of quininium aspirinate are herein reported.


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