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- Alkali-activation (3)
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Eingeladener Vortrag
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Reaction products and strength development of wastepaper sludge ash and the influence of alkalis
(2014)
Wastepaper sludge ash (WSA) from a newsprint paper mill was investigated for its mineralogical composition and its reaction products and strength development after activation with water and sodium and potassium hydroxide solutions. The results showed the WSA to consist of calcite, free lime, gehlenite, tricalcium aluminate, belite, talc, quartz and probably a glassy phase. The principle reaction product was monocarboaluminate (CO3–AFm) for the water- as well as for the alkali-activated WSA. Formation of monocarboaluminate and strength gain was more rapid for the alkali-activated WSA until 1 day of curing. However, afterwards reactions proceeded much slower when alkali solutions were used, leading to an about twice as high compressive strength for water-activated WSA mortars after 28 days of curing. The observed behavior is tentatively ascribed to a less uniform microstructure of the alkali-activated WSA. Significant differences between NaOH- and the KOH-activated WSA were not observed.
Zeolite synthesis was studied using two silica rich filtration residues (FR 1 and FR 2) as Si-source
and sodium aluminate in a direct synthesis at 60°C at strong alkaline conditions (8 M - 16 M NaOH).
In addition to these one-pot syntheses, a two-step process was investigated. Here, an alkaline digestion
of FR at 60°C was followed by gel precipitation with sodium aluminate and gel crystallization
under usual conditions of 80°C - 90°C. The results show that the substitution of chemical
reagent sodium silicate by a waste material like FR as Si-source is possible but requires fine tuning
of the reaction conditions as zeolite crystallization is a process under kinetic control. The
solubility behaviour and impurities of the inserted filtration residues strongly influenced the
course of reaction. Thus zeolites like hydrosodalite or intermediate zeolite between cancrinite
and sodalite, or zeolite NaA or Z-21 in cocrystallization with hydrosodalite could be observed in
the one pot syntheses already in a short time interval between 1 - 4 h depending on the alkalinity.
The two step process yield to zeolites NaA and NaX in very good quality. The reaction process of FR
in both reaction methods was characterized by chemical analyses, X-ray powder diffraction,
Fourier transform infrared spectroscopy as well as scanning electron microscopy. Surface area
and water content of selected products were further characterized by the BET-method and by
thermogravimetry. Summing up the results, we can show that zeolite formation from filtration residues
is possible by several reaction procedures as model cases for a re-use of industrial waste
materials. Beside the importance for environmental protection, the reactions are of interest for
zeolite chemistry as the re-use of FR is possible under economically conditions of low energy consumption
at 60°C and short reaction periods.
In paper recycling several types of waste sludges are produced, which contain organics as well as inorganic fillers of the recycled paper, e.g. kaolinite, calcite, talc, or titanium dioxide [1,2]. Part of these sludges is incinerated to recover energy and to reduce the volume of waste to be handled. The ashes generated in this process are commonly referred to as wastepaper sludge ash (WSA). The quantities of WSA produced are large and at present much of it is still landfilled or otherwise handled entailing costs.
Depending on the composition of the recycled paper and the conditions during processing and incineration, WSA can have cementitious properties. In the present investigation a CaC03-rich WSA was analyzed for reaction products and strength development after hydration with water, 2 M NaOH solution and 8 M NaOH solution. The rationale for activating the WSA with NaOH was to assess the behaviour of the WSA when alkalis are introduced to the System or when the WSA is used as addition in alkali-activated binders.
In paper recycling large amounts of waste sludge, containing organics as well as inorganic fillers of the recycled paper, are produced. A large fraction of these sludges is incinerated; the ashes generated in this process, often referred to as wastepaper sludge ash (WSA), have the potential to be used as binder material, either alone or as supplementary cementitious material. However, ashes from different paper mills differ in their Chemical and mineralogical composition, thus, the reaction products and the properties of the hardened binders may vary s i gn i fi cantley.
In the present study, a calcite-rich WSA was analyzed for reaction products and strength development. The WSA contained, besides calcite, hydraulic phases such as tricalcium aluminate (C3A) and belite (C2S), lime as well as inert phases. When activated with water, the WSA yielded a compressive strength of up to 12.3 MPa and the major hydration product was monocarboaluminate (C4A CO2 IIH2O or C4ACH11). Activation with 2M NaOH or 2M KOH solution caused a more rapid strength gain until one day of curing, but afterwards the strength development slowed down and the strength afiter 28 days was significantly lower than for the water-activated pastes. From TG analyses it is apparent that the higher strength of the alkaliactivated pastes after one day of curing was caused by a more rapid consumption of calcite and associated formation of C4ACH11. At later curing times the amount of calcite did not change substantially and consequently strength development almost ceased.
The results demonstrate the complex influence of alkaline conditions on the hydration of WSA and show that the reaction products, which determine the durability properties of the hardened pastes (and materials made from it), of the calcite-rich WSA differ from the products of other WS As, as discussed in the article.