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1.
The development of a new process for gentle drying, micronisation and formulation of a high viscous biopoymer
Christian Reibe, 2011, dissertation

Abstract: Biopolymers are characterised by their biodegradable behaviour in certain environments. Especially the development of natural biopolymers from renewable resources is gathering increasing interest in the scientific as well as in the industrial sectors . Since Biopolymers may be tailored to specific requirements, the encapsulation of pharmaceutical compounds or flavours in biopolymers would open wide avenues for the production of controlled- release systems. Most common mechanical pulverisation processes are milling and grinding. With these processes it is not possible to produce specific morphologies like foams or hollow spheres, but always splintered edges. Encapsulation is carried out by common precipitation techniques. Gelatine, as a widely applied biopolymer, represents one example of those substances of large interest, but it is difficult to process. Especially gelatines with high molecular mass are difficult or almost impossible to be pulverized by spray drying techniques, due to their high viscosity. In the frame of this research work, an integrated high-pressure spraying, drying and pulverization process for high viscous gelatine was developed, based on a combination of the water removing effects "Evaporation" and "Gas-solubility". The resulting products were dry, free-flowing gelatine powders, still exhibiting high molecular masses. Due to the new, gentle method of processing, a completely new gelatine product with unique properties was obtained. Even the encapsulation of edible oil in high ratios was found to be possible with this new process. The characterisation was carried out by standard methods for gelatine on the one hand side, and standard procedures for characterising powders on the other hand side. The developed process was patented under the identifier "WO 002009135601 A1".
Keywords: High Pressure Process, Supercritical Fluids, High molecular mass Gelatine, Micronisation, CO-2 - spray drying, Encapsulation, Gelatine Powder
Published: 26.01.2011; Views: 2507; Downloads: 73
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2.
Preparation of enantiomers using high pressure technologies
Paul Thorey, 2010, dissertation

Abstract: The study of two different methods of obtaining chiral alcohols is proposed herein. The requirement of the relatively new paradigm of green chemistry associated with clean technologies such as biocatalysis or non-conventional solvents, dense gases, was focused at. Indeed, the two methods of production of chiral alcohols were: - the conversion of acetophenone into (R)-1-phenylethanol in dense gases catalysed by Lactobacillus brevis alcohol dehydrogenase and its coenzyme, NADP/H; - the resolution of (±)-trans-1,2-cyclohexanediol by cocrystal formation with tartaric acid followed by supercritical extraction. In both cases high enantiopurities were achieved (ee>99%).
Keywords: High-pressure technologies, enantiomers, green chemistry, R-1-phenylethanol, Lactobacillus brevis, alcohol dehydrogenase, NADP, liquid propane, enzyme deactivation, resolution, trans-1, 2-cyclohexanediol, tartaric acid, cocrystal, supercritical carbon dioxide, extraction, X-ray diffraction, differential scanning calorimetry
Published: 02.02.2011; Views: 2088; Downloads: 69
.pdf Full text (6,25 MB)

3.
Particle formation using supercritical fluids
Željko Knez, 2006, review article

Abstract: Particle formation and the design of solid particles and powdery composites with unique properties is at the moment one of major the developments of supercritical fluid (synonyms: dense gases, dense fluids, high pressure) applications. Conventional well-known processes for the particle-size redistribution of solid materials are crushing and grinding (which for some compounds are carried out at cryogenic temperatures), air micronization, sublimation, and recrystallization from solution. There are several problems associated with the above-mentioned processes. Some substances are unstable under conventional milling conditions, in recrysfallization processes the product is contaminated with solvent and waste solvent streams are produced. The application of supercritical fluids may overcome the drawbacks of conventional processes, and powders and composites with special characteristics can be produced. Several processes for the formation and design of solid particles using dense gases have been studied intensively. The unique thermodynamic and fluid-dynamic properties of supercritical fluids can also be used for the impregnation of solid particles, for the formation of solid powderous emulsions, particle coatings, e.g. for the formation of solids with unique properties for use in different applications. This review will focus on the fundamentals and on recent advances of particle formation and design processes using supercritical fluids on their applications and the technological advantages and disadvantages of various processes.
Keywords: chemical processing, high pressure technology, supercritical CO2, proteinase, thermal stability, pressure stability, enzyme activity, water content, dense gases
Published: 31.05.2012; Views: 1372; Downloads: 34
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4.
The lipase-catalyzed synthesis of fatty acid fructose esters in organic media and in supercritical carbon dioxide
Saša Šabeder, Maja Leitgeb, Željko Knez, 2006, original scientific article

Abstract: Sugar fatty acid esters are biodegradable surface active compounds in foodstuffs and cosmetics or pharmaceuticals. They have potential in replacing pollutant chemically synthesized surfactants. The enzymatic synthesis of fructose palmitate catalyzed by Candida antarctica B lipase was performed in different organic media in a batch react at atmospheric pressure. The influence of the organic solvent and temperature on the esterification was studied. Since supercritical carbon dioxide (SC CO2) has several advantages over organic solvents, such as high reaction rate, high mass transfer, non-toxicity, non flammability and low price, it was also chosen as a reaction medium for fructose palmitate production. The influence of temperature on immobilized lipase activity was studied at 10 MPa and the results were compared to the results obtained from reactions performed at atmospheric pressure under the same reaction conditions. The highest conversion (67%) was obtained after 24 hours of reaction in SC C02 at 80°C. A change of the particle size distribution and morphology of the untreated lipase and lipase treated with 2-methyl 2-butanol and SC C02 was observed. This article was presented at 1st SEECChE, held in Belgrade, September 25-28, 2005
Keywords: chemical processing, high pressure technology, supercritical CO2, lipase catalyzed syntheses, esterification, fructose palmitate, biocatalysts, lipase, Candida antarctica B
Published: 31.05.2012; Views: 1502; Downloads: 222
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5.
Enzyme-catalyzed reactions in different types of high-pressure enzymatic reactors
Mateja Primožič, Maja Leitgeb, Muzafera Paljevac, Željko Knez, 2006, original scientific article

Abstract: The enzyme-catalyzed hydrolysis of carboxy-methyl cellulose (CMC) was performed in three different types of reactors; in a batch stirred-tank reactor (BSTR) operating at atmospheric pressure, in a high-pressure batch stirred-tank reactor (HP BSTR) and in a high-pressure continuous tubular-membrane reactor (HP CTMR). In the high-pressure reactors aqueous SC C02 was used as the reaction medium. The aim of our research was optimization of the reaction parameters for reaction performance. All the reactions were catalyzed by cellulase from Humicola insolens. Glucose production in the high-pressure batch stirred-tank reactor was faster than in the BSTR at atmospheric pressure. The optimal temperature for the reaction performed in the BSTR at atmospheric pressure was 30°C, while the optimal temperature for the reaction performed in SC C02 was 32°C. The influence of the application of tubular ceramic membranes in the high-pressure reaction system was studied on the model reaction of CMC hydrolysis at atmospheric pressure and in SC C02. The reaction was catalyzed by cellulase from Humicola insolens covalently linked to the surface of the ceramic membrane. The hydrolysis of CMC in SC C02 and at atmospheric pressure was performed for a long time period. The reaction carried out in SC C02 was more productive than the reaction performed at atmospheric pressure.
Keywords: chemical processing, enzymatic reaction, cellulase, supercritical carbon dioxide, high-pressure batch reactor, high-pressure membrane reactor
Published: 31.05.2012; Views: 1190; Downloads: 190
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6.
Proteinase-catalyzed hydrolysis of casein at atmospheric pressure and in supercritical media
Mateja Primožič, Maja Leitgeb, Željko Knez, 2006, original scientific article

Abstract: In the presented work, reaction parameters for hydrolysis of casein, catalyzed by Carica papaya latex at atmospheric and high pressure, were optimized. Casein is a remarkably efficient nutrient, supplying not only essential amino acids, but also some carbohydrates, calcium, phosphorus and therefore is very important for the food industry. Different reaction parameters such as temperature, stirring rate, casein and enzyme concentration were studied to found the optimal conditions for the reaction. Reactions were performed at atmospheric pressure; an influence of temperature/pressure on the casein hydrolysis in supercritical carbon dioxide (SC CO2) was also investigated to improve the reaction rates. Higher conversions were achieved when the reactions were performed in SC CO2, even though casein was not soluble in this medium.
Keywords: chemical processing, high pressure technology, supercritical CO2, enzymatic reactions, proteinase, Carica papaya latex
Published: 31.05.2012; Views: 1051; Downloads: 14
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8.
Supercritical fluids as solvents for enzymatic reactions
Maja Leitgeb, Mateja Primožič, Željko Knez, 2007, review article

Abstract: Enzymes may act in different solvent systems. Water as the solvent in vivo may be replaced partially or mostly with other solvents, such as micro-emulsions, organic solvents, reversed micelles, ionic liquids and supercritical fluids (SCFs).Several types of enzymatic reactions were performed in SCFs. Influence of SCFs on enzyme stability and activity is presented on different examples; on different reaction systems (hydrolysis, transesterification...) and on the use of non-immobilized (Subtilisin carlsberg, Aspergillus niger...) as well as immobilized enzymes. Several types of high-pressure enzymatic reactors (batch-, stirred-tank-, extractive semibatch-, recirculating batch-, semicontinuous flow-, continuous packed-bed-, and continuous-membrane reactors) have been used for the performance of enzymatic reactions. In the studies on stability of biocatalysts in a high-pressure batch-stirred tank reactor changes in biocatalysts activity due to pressurization/depressurization steps were observed. Interesting alternative to overcome this inconvenience is the use of the high-pressure continuous membrane reactors, where just single compression and expansion step is necessary.
Keywords: enzymatic reactions, supercritical carbon dioxide, high-pressure, enzyme stability, high-pressure reactors
Published: 31.05.2012; Views: 1360; Downloads: 56
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9.
Supercritical fluid adsorption and desorption of lipids on various adsorbents
Mojca Škerget, Željko Knez, 2007, original scientific article

Abstract: In present work the feasibility of using supercritical fluid chromatography (SFC) for separation of free fatty acids (FFA) and triglycerides has been examined. Lipids such as oleic acid and sunflower oil (containing 96% of triglycerides) were used; adsorption and desorption on adsorbents such as silica gel and neusilin using supercritical $CO_2$ as mobile phase was investigated. The experiments were performed at 40 °C and in the pressure range from 13 to 30 MPa. Adsorption kinetic lines were determined by analysingbreakthrough curves. Several parameters such as rate of adsorption and desorption, loading, desorbed quantity and diffusion coefficients in solid phase were calculated.
Keywords: supercritical fluid chromatography, lipids, oleic acid, triglycerides, adsorption, desorption
Published: 31.05.2012; Views: 1342; Downloads: 44
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10.
Supercritical fluid extraction of chammomile flower head flowers: comparison with conventional extraction, kinetics and scale-up
Petra Kotnik, Mojca Škerget, Željko Knez, 2007, published scientific conference contribution

Abstract: Supercritical fluid extraction of chamomile flower heads was performed on semicontinuous extraction apparatus in the lab scale using carbon dioxide as solvent. The results of high pressure experiments were compared with those obtained with Soxhlet extraction, steam distillation and maceration. The obtained extracts were analysed by HPLC on ?-bisabolol, matricine and chamazulene content and by gravimetrical method on essential oil and waxes content. The highest content of active components in extracts and highest extraction yield were obtained using SFE at 250 bar and 40 °C. At this extraction conditions the two step separation was used to optimize the separation of essential oil from unwanted components. Dynamic behaviour of theSFE with single step separation runs were analysed using two mathematical models for describing the constant rate period and subsequent falling rate period. Based on the experimental data, external mass transfer coefficient, diffusion coefficient and diffusivity in solid phase were estimated. Results showed acceptable agreement of calculated and experimental data. Based on theparameters determined in the lab scale, the extraction process was successfully transferred to pilot scale.
Keywords: chemical processing, high pressure technology, supercritical extraction, chamomile, matricine, chamazulen, scale-up
Published: 31.05.2012; Views: 1182; Downloads: 23
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