New solid state epoxy resins based on diglycidyl ether of 1,1-dichloro-2,2 bis (4-hydroxyphenyl), ethylene (BPC) and BPA epoxy resins in the reaction with BPC and BPA were developed. Solid epoxy resins were synthesised by the use of two different heating methods: conventional and microwave reactor. The use of microwave radiation as novel heating medium as an alternative to the conventional methods, which provide a quicker and more effective synthesis. The solid epoxies have high melting points higher than 100°C and the polycondensation degree remains between n ϭ 4 -12. Epoxy value stays low and occurs around 0,02-0,1. BPA epoxy resins and diglycidylether of BPC II were compared in terms of reaction speed. It can be seen that the reaction of BPC diglycidylether occurs approximately 20% quicker given the same reaction conditions of temperature, and balance of catalyst.
Solid state epoxy resins were synthesized in the reactions of the systems: 1,1-dichloro--2,2-bis(4-hydroxyphenyl)ethylene (BPC II) and 2,2-bis(4-hydroxyphenyl)propane (bisphenol A), mixed in various weight ratios, with one of two low-molecular weight epoxy resins, Epidian 5 ® or diglycidylether of 1,1-dichloro-2,2-bis(4-hydroxyphenyl)ethylene (DGEBC II). Additionally the series of the samples synthesized with use of DGEBC II but with addition of red phosphorus as flame retardant were prepared. It was found, on the basis of limiting oxygen index (LOI) measurements, that the flammability of the samples decrease (higher values of LOI) with increase in BPC II weight part in the mixture with bisphenol A, for all the series of samples prepared. Solid state resins synthesized with the use of DGEBC II were less flammable than similar samples with bisphenol A. Addition of red phosphorus increased significantly LOI values, however, caused deterioration of optical properties of the resins investigated. The samples characterized with low flammability were selected for the syntheses with addition of zinc stannate (ZS) or zinc hydroxystannate (ZHS) as flame retardants. The values of LOI of the products obtained were determined (Table 2). It was found that the addition of 2-3 wt. % of ZS or ZHS significantly improves LOI values not causing the deterioration of optical properties.
Streszczenie-Opisano dwie metody syntezy karbamoiloetylowanych pochodnych skrobi (CrES) obejmuj¹ce etapy degradacji (chemicznej b¹dŸ enzymatycznej pod wp³ywem α-amylazy) oraz etap reakcji addycji z akryloamidem. Zbadano wp³yw warunków degradacji enzymatycznej (biodegradacji) na rozpuszczalnooeae w wodzie CrES, lepkooeae jej roztworów wodnych, stopieñ podstawienia (DS) i ciê¿ar cz¹steczkowy. Scharakteryzowano wp³yw opisanej modyfikacji skrobi na zmiany struktury jej powierzchni. S³owa kluczowe: skrobia, karbamoiloetylowanie, stopieñ podstawienia, degradacja enzymatyczna, α-amylaza, rozpuszczalnooeae w wodzie, ciê¿ar cz¹steczkowy, struktura powierzchni. WATER-SOLUBLE CARBAMOYLETHYLATED DERIVATIVES OF POTATO STARCH. PART I. SYNTHESIS AND STRUCTURE Summary-Water-soluble starch derivatives (CrES) containing carbamoylethyl groups were synthesized using two methods. The first based on chemical degradation of native potato starch under the influence of KOH or NaOH and subsequent reaction of addition with acryloamide. The other based on carbamoylethylation of native starch in such reaction and subsequent enzymatic biodegradation of CrES obtained using α-amylase. The effects of biodegradation conditions, namely: catalyst type and concentration [Ca(OH)2, KOH], time and temperature of the process and α-amylase concentration on CrES solubility in the water and viscosity of aqueous solutions obtained (Table 1 and 6) as well as on the degree of substitution (DS, Table 2-5). The lowering of molecular weight of starch products after degradation, either chemical or enzymatic one, positively influences the solubility of CrES in water (results of MALDI-TOF measurements, Fig. 1, 2 and 6). The modification causes also the changes in the surface structure of CrES facilitating its dissolution in water (results of SEM microscopic investigations, Fig. 3 and 7). Chemical structure of CrES was confirmed by FT-IR method (Fig. 4, 5 and 8).
Derivatives of starch, such as graft copolymer of acrylamide onto starch, carbamoylethylated starch, carbamoylethyl-dihydroxypropylated starch, and dihydroxypropylated starch have been tested for their properties as components of drilling fluids used for clay inhibition and for the regulation of their rheology. The influence of modified starch and their blends with tylose as protective agents in the filtration of drilling fluids, as well as replacement of tylose, by modified starch were investigated. The viscosity, flow limit, filtration, pH, and dispersion as factors of the properties of potassium drilling fluids with the addition of starch derivatives were determined.
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