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prof. Ing. Svetozár Katuščák, PhD.
Identifikační číslo: 3934
Univerzitní e-mail: svetozar.katuscak [at] stuba.sk
Externí spolupracovník - Fakulta chemickej a potravinárskej technológie (STU)

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Základní informace

Základní informace o závěrečné práci

Typ práce: Diplomová práce
Název práce:Metódy štúdia procesov modifikácie a degradácie lignocelulózových materiálov
Autor: Ing. Lívia Beňová
Pracoviště: Oddelenie dreva, celulózy a papiera (ÚPSP FCHPT)
Vedoucí práce: prof. Ing. Svetozár Katuščák, PhD.
Oponent:doc. Ing. Katarína Hroboňová, PhD.
Stav závěrečné práce:Závěrečná práce byla úspěšně obhájena

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Jazyk zpracování závěrečné práce:slovenský jazyk

slovenský jazyk        anglický jazyk

Název práce:Studies about Methods of Modification and Degradation Processes in Lognocellulosic Materials
Abstrakt:For the research of modified processes and devices it is needed certain complex of basic methods. For that reason the interdisciplinary team and consortium Kniha SK of STU is continually preparing modernisation of methods -- basic separative, analytical and evaluative. This work follows up to date developed modernisation of evaluation of mechanical qualities (attributes) and that was focused especially on progress: GPC of cellulose HPLC of carbohydrate furaldehyd, carboxyl acids and its salts TA paper changes in modified and degrading processes Assessment of surface polarity The object of the research in dissertation work was degrading, stabilizing, deacidifing and other modification processes of lignocellulose materials. Straight way of cellulose degradation measuring is her fractionation and determining of molecular weight, polydisperse parameters and other solution properties. Cellulose is the most distinguished component of paper and LCM in term of its mechanical properties, also in term of paper and documents life -- cycle. Complex fractionation and characterization of soluble and insoluble pieces / fractions, complicated composite LC polymer materials is ideal goal in field of analytical and others methods currently developed. The following results have been achieved: 1. By the combination of HPLC and GPC, we gained information on the ozonization of cellulose. Per HPLC was analysed aquatic extract of cellulose before and after ozonisation. Low-molecular compounds as for instance sacharides and carboxyl acids are primary product of cellulose oxidation degradation. In pulp samples after ozonization we detected more degradation products such as: sacharides (methyl-D-gluko-pyranose, xylose, alfa -D-arabinose, D- fructose, D-manose, glucose, D-galaktose, celobiose and lactose) and carboxyl acids (acetic acid and formic acid) that in non -- ozonized cellulose. It demonstrates that during cellulose ozonisation comes to cellulose oxidative degradation. Per GPC non-derivative cellulose (dissolved per assistance of solvent system LiCl/DMAc) was proved that secondary oxidative degradation of cellulose, at which comes to fussion glykosidic bonds of polymer chain. We determined changes of molecular weight distribution and polydispersity parameters of cellullose. The degree of polymerisation of the ozonized oxygen delignified hardwood kraft pulp decreased upon longer ozonization processes.(From 3985,52 (non-ozonized pulp) to 1907,59 (pulp ozonized along 657s). Per GPC non-derivated cellulose (dissolved with LiCl/DMAc solvent system) was proved secondary oxidative degradation of cellulose, at which comes to fussion of glykosidic bonds of polymer chain. 2. Wood newspaper samples are insoluble either in LiCL/DMAc solution system nor in solutions used for cellulose solution, therefore it was determined with GPC - CTC fractionation cellulose method derivated with trikarbanilaths. The cause of insolubility of samples may be presence of mechanical wood pulp and also lignin-cellulose and other hardly soluble complexes. We determined samples of wood newspaper: unmodified and modified per accelerated thermic ageing, and modification systems: Bookkeeper Modification suspension and MgO Modification system and metoxy magnesium metyl carbonate (MMMK) at the rate 3:1. We determined the process of changes of polydispersity parameters, during modification and paper ageing. We accomplished the following results: o by accelerated thermic ageing of unmodified wood newspaper is reached the biggest degradation of cellulose in paper and the highest reducement of APS as well as polydispersity degree, o during accelerated thermic ageing of modified wood newspaper is reached the biggest degradation of cellulose -- modification with MgO modification system and metoxy magnesium methyl carbonate (MMMK) at the rate 3:1, the lowest rate of degradation towards the destruction cellulose chain in comparison to modification with Bookkeeper modification suspension. 3. The development and the verification of new HPLC - VÚVH 2006104 method of determination carboxyl acids and its salts and furaldehyd in appropriate extracts from paper. By Modification of newspaper samples with propylenoxide we accomplished the following results: o the control sample of non-modified NP by all three types of paper (Větřní, Glejený a Volum) also during the ageing days contains usually more degradation products (acetic acid, formic acid and their saalts and furaldehyd) as samples modified with propylenoxide, o for all three types of modified (with propylenoxide) also non - modified wood news paper (Větřní, Glejený a Volum) increased the concentration of degradation products with number days of fast thermic ageing, o the highest increase of degradation products during days of fast thermic ageing emerged by wood news paper samples with label Volum afterwards Větřní and at least the degradation products emerged at wood newspaper samples labeled Glejený. Modification of samples, sent to international deacidification centres (CSC - Barcelona, Battele - Eschborn, Nitrochemie - Wimmis, CSC - Leipzig, SOBU - Furth, ZFB - Leipzig) was accomplished with following results: (according HPLC - VÚVH 2006104), o generally modified samples NP (by all processes) non - aged also aged contained more carboxyl acids and less furaldehyd against non - modified sample NP, o in calibration of method HPLC - VÚVH 2006104would be continued, because there are needed measurement of acids model compounds and its salts, which are present in analysed paper samples especially RCOOH, Mg (COOH)2, Mg (HCO3) a MgCO3.The goal is to find out, how is the relation of results these HPLC -- VÚVH analyse to real contents of carboxyl acids and its salts, respectively what part carboxyl acids and carboxyl salts will be determined, o the overall evaluation of degradation news paper samples only by HPLC - VÚVH 2006104 method on the ground of concentration particular degradation products as acids and its salts and furaldehyd is not effective assessment of overall degradation of paper. Whereas it is necessary to analyse the sample by complex quality control. 4. TA, Characterization of ozonized pulp by thermogravimetric analysis. The effect of ozonization on the thermal behaviour of oxygen delignified hardwood kraft pulp was studied by thermogravimetric analysis TG and DTG in the temperature range from 25 to 500 °C. The results revealed that the unozonized pulp appeared to be more stable than ozonized samples. Other result indicated that thermal stability of the ozonized hardwood kraft pulp (delignificated with oxygen) decreased with the length the ozonization process, and this thermal stability express as temperature of maximum rate of decomposition vs. ozone consumption is described by relation: Tdec = 335.12 -23.31exp(-1.45.O3 CON), correlation coefficient, R2 = 0.8492. The thermal stability of the ozonized oxygen delignified hardwood kraft pulp decreased upon longer ozonization processes. 5. Correlation TGA and GPC parameters provide the answer to the question: Which relation can be between GPC and TA results, when are used both methods to valuation of the development of degradation the same polymers? It was evaluated the coefficients sequence R2 from diagram - draftsman at the correlation between TA and GPC parameters. The most important are correlation with TA parameters -- temperature of degradation TD1 and TD2 correlate with GPC parameters (R2 =0,876), (R2 =0,874)a PPS (R2 =0,873) Practical importance from correlation TGA and GPC parameters is, that it can be predicate GPC parameters from TA parameters. 6. We developed and verified the new fast method of valuation LCM surfaces polarity changes by measurement of difference of trichomatic elements between modified and non-modified surface after coloration by chosen standard colouring in system of CIE Lab. It was verified that by coloured difference it is possible also to valuate LCM surfaces polarity, that was proved by comparison of method to up to date used methods for polarity changes measurement (water droplet uptake time to LCM surface and contact angle). By this method it is possible to obtain information about hydrofilization resp. hydrophobization of LCM surface. For verification of this method continues, method is in the process of development.
Klíčová slova:GPC, HPLC, TGA, deacidification, stabilization, polarity

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