WO2006005783A1 - Method of obtaining insulating materials from waste from thermal processes that use biomass - Google Patents
Method of obtaining insulating materials from waste from thermal processes that use biomass Download PDFInfo
- Publication number
- WO2006005783A1 WO2006005783A1 PCT/ES2005/000383 ES2005000383W WO2006005783A1 WO 2006005783 A1 WO2006005783 A1 WO 2006005783A1 ES 2005000383 W ES2005000383 W ES 2005000383W WO 2006005783 A1 WO2006005783 A1 WO 2006005783A1
- Authority
- WO
- WIPO (PCT)
- Prior art keywords
- waste
- biomass
- mixtures
- thermal
- processes
- Prior art date
Links
- 239000002028 Biomass Substances 0.000 title claims abstract description 21
- 238000000034 method Methods 0.000 title claims abstract description 20
- 239000002699 waste material Substances 0.000 title claims abstract description 16
- 239000011810 insulating material Substances 0.000 title claims abstract description 10
- 239000000203 mixture Substances 0.000 claims abstract description 22
- 239000002956 ash Substances 0.000 claims abstract description 17
- 239000000463 material Substances 0.000 claims abstract description 15
- 239000002893 slag Substances 0.000 claims abstract description 14
- 238000002485 combustion reaction Methods 0.000 claims abstract description 13
- 238000002309 gasification Methods 0.000 claims abstract description 5
- 238000000197 pyrolysis Methods 0.000 claims abstract description 5
- 239000002803 fossil fuel Substances 0.000 claims abstract description 3
- 238000007669 thermal treatment Methods 0.000 claims abstract description 3
- 235000002918 Fraxinus excelsior Nutrition 0.000 claims description 14
- 239000012467 final product Substances 0.000 claims description 9
- 238000010438 heat treatment Methods 0.000 claims description 9
- 238000007596 consolidation process Methods 0.000 claims description 5
- 239000002253 acid Substances 0.000 claims description 2
- 150000007513 acids Chemical class 0.000 claims description 2
- 238000000227 grinding Methods 0.000 claims description 2
- 230000000704 physical effect Effects 0.000 claims description 2
- 238000000926 separation method Methods 0.000 claims description 2
- 230000008030 elimination Effects 0.000 claims 1
- 238000003379 elimination reaction Methods 0.000 claims 1
- 239000010909 process residue Substances 0.000 claims 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 abstract description 9
- 238000009413 insulation Methods 0.000 abstract description 7
- 230000009970 fire resistant effect Effects 0.000 abstract description 6
- 238000002156 mixing Methods 0.000 abstract description 4
- 238000004064 recycling Methods 0.000 abstract description 4
- 238000001311 chemical methods and process Methods 0.000 abstract 1
- 238000007493 shaping process Methods 0.000 abstract 1
- 239000000047 product Substances 0.000 description 16
- 239000000654 additive Substances 0.000 description 14
- 239000000470 constituent Substances 0.000 description 9
- 239000003245 coal Substances 0.000 description 8
- 239000010881 fly ash Substances 0.000 description 5
- 239000000126 substance Substances 0.000 description 4
- 239000000378 calcium silicate Substances 0.000 description 3
- 229910052918 calcium silicate Inorganic materials 0.000 description 3
- OYACROKNLOSFPA-UHFFFAOYSA-N calcium;dioxido(oxo)silane Chemical compound [Ca+2].[O-][Si]([O-])=O OYACROKNLOSFPA-UHFFFAOYSA-N 0.000 description 3
- 230000006835 compression Effects 0.000 description 3
- 238000007906 compression Methods 0.000 description 3
- 239000000446 fuel Substances 0.000 description 3
- 238000004519 manufacturing process Methods 0.000 description 3
- MHAJPDPJQMAIIY-UHFFFAOYSA-N Hydrogen peroxide Chemical compound OO MHAJPDPJQMAIIY-UHFFFAOYSA-N 0.000 description 2
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 2
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 description 2
- 238000010521 absorption reaction Methods 0.000 description 2
- 239000011230 binding agent Substances 0.000 description 2
- 239000006227 byproduct Substances 0.000 description 2
- 238000006243 chemical reaction Methods 0.000 description 2
- 238000010276 construction Methods 0.000 description 2
- 239000007789 gas Substances 0.000 description 2
- 238000007654 immersion Methods 0.000 description 2
- 239000002440 industrial waste Substances 0.000 description 2
- 239000004570 mortar (masonry) Substances 0.000 description 2
- 239000011505 plaster Substances 0.000 description 2
- 239000011148 porous material Substances 0.000 description 2
- 239000002994 raw material Substances 0.000 description 2
- 239000011378 shotcrete Substances 0.000 description 2
- 235000008733 Citrus aurantifolia Nutrition 0.000 description 1
- 240000007594 Oryza sativa Species 0.000 description 1
- 235000007164 Oryza sativa Nutrition 0.000 description 1
- 239000011398 Portland cement Substances 0.000 description 1
- 241000779819 Syncarpia glomulifera Species 0.000 description 1
- 235000011941 Tilia x europaea Nutrition 0.000 description 1
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 description 1
- 230000000996 additive effect Effects 0.000 description 1
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 1
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 1
- 239000004568 cement Substances 0.000 description 1
- 239000000919 ceramic Substances 0.000 description 1
- 238000003889 chemical engineering Methods 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 230000002860 competitive effect Effects 0.000 description 1
- 239000004567 concrete Substances 0.000 description 1
- 239000000975 dye Substances 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 125000004494 ethyl ester group Chemical group 0.000 description 1
- 238000000605 extraction Methods 0.000 description 1
- 239000011152 fibreglass Substances 0.000 description 1
- 239000003517 fume Substances 0.000 description 1
- 239000000499 gel Substances 0.000 description 1
- 239000010440 gypsum Substances 0.000 description 1
- 229910052602 gypsum Inorganic materials 0.000 description 1
- 239000008240 homogeneous mixture Substances 0.000 description 1
- 238000000265 homogenisation Methods 0.000 description 1
- 239000010903 husk Substances 0.000 description 1
- 150000004679 hydroxides Chemical class 0.000 description 1
- 239000012784 inorganic fiber Substances 0.000 description 1
- 229910052500 inorganic mineral Inorganic materials 0.000 description 1
- 239000012212 insulator Substances 0.000 description 1
- 238000004898 kneading Methods 0.000 description 1
- 239000004571 lime Substances 0.000 description 1
- 239000000395 magnesium oxide Substances 0.000 description 1
- CPLXHLVBOLITMK-UHFFFAOYSA-N magnesium oxide Inorganic materials [Mg]=O CPLXHLVBOLITMK-UHFFFAOYSA-N 0.000 description 1
- GVALZJMUIHGIMD-UHFFFAOYSA-H magnesium phosphate Chemical class [Mg+2].[Mg+2].[Mg+2].[O-]P([O-])([O-])=O.[O-]P([O-])([O-])=O GVALZJMUIHGIMD-UHFFFAOYSA-H 0.000 description 1
- 239000004137 magnesium phosphate Substances 0.000 description 1
- 235000010994 magnesium phosphates Nutrition 0.000 description 1
- AXZKOIWUVFPNLO-UHFFFAOYSA-N magnesium;oxygen(2-) Chemical compound [O-2].[Mg+2] AXZKOIWUVFPNLO-UHFFFAOYSA-N 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 239000011707 mineral Substances 0.000 description 1
- 238000000465 moulding Methods 0.000 description 1
- 239000004006 olive oil Substances 0.000 description 1
- 235000008390 olive oil Nutrition 0.000 description 1
- 238000005192 partition Methods 0.000 description 1
- 235000015927 pasta Nutrition 0.000 description 1
- 239000010451 perlite Substances 0.000 description 1
- 235000019362 perlite Nutrition 0.000 description 1
- 239000001739 pinus spp. Substances 0.000 description 1
- 238000002203 pretreatment Methods 0.000 description 1
- 235000009566 rice Nutrition 0.000 description 1
- 150000003839 salts Chemical class 0.000 description 1
- 239000004576 sand Substances 0.000 description 1
- 238000007873 sieving Methods 0.000 description 1
- 239000000741 silica gel Substances 0.000 description 1
- 229910002027 silica gel Inorganic materials 0.000 description 1
- RMAQACBXLXPBSY-UHFFFAOYSA-N silicic acid Chemical compound O[Si](O)(O)O RMAQACBXLXPBSY-UHFFFAOYSA-N 0.000 description 1
- 235000012239 silicon dioxide Nutrition 0.000 description 1
- 239000011780 sodium chloride Substances 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 238000001228 spectrum Methods 0.000 description 1
- 238000005507 spraying Methods 0.000 description 1
- 239000010936 titanium Substances 0.000 description 1
- 229910052719 titanium Inorganic materials 0.000 description 1
- 229940036248 turpentine Drugs 0.000 description 1
- 239000010455 vermiculite Substances 0.000 description 1
- 229910052902 vermiculite Inorganic materials 0.000 description 1
- 235000019354 vermiculite Nutrition 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B18/00—Use of agglomerated or waste materials or refuse as fillers for mortars, concrete or artificial stone; Treatment of agglomerated or waste materials or refuse, specially adapted to enhance their filling properties in mortars, concrete or artificial stone
- C04B18/02—Agglomerated materials, e.g. artificial aggregates
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B09—DISPOSAL OF SOLID WASTE; RECLAMATION OF CONTAMINATED SOIL
- B09B—DISPOSAL OF SOLID WASTE NOT OTHERWISE PROVIDED FOR
- B09B3/00—Destroying solid waste or transforming solid waste into something useful or harmless
- B09B3/20—Agglomeration, binding or encapsulation of solid waste
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B09—DISPOSAL OF SOLID WASTE; RECLAMATION OF CONTAMINATED SOIL
- B09B—DISPOSAL OF SOLID WASTE NOT OTHERWISE PROVIDED FOR
- B09B3/00—Destroying solid waste or transforming solid waste into something useful or harmless
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02W—CLIMATE CHANGE MITIGATION TECHNOLOGIES RELATED TO WASTEWATER TREATMENT OR WASTE MANAGEMENT
- Y02W30/00—Technologies for solid waste management
- Y02W30/50—Reuse, recycling or recovery technologies
- Y02W30/91—Use of waste materials as fillers for mortars or concrete
Definitions
- the present invention relates to obtaining thermal insulation and fire-resistant materials, manufactured with ashes or slags that come from processes such as combustion, pyrolysis or gasification of biomass or mixtures of fossil-biomass fuels, representing the ashes, slags or mixtures of the above, on a dry basis, more than 50% by weight of the constituents of the final product.
- the invention is fundamentally applicable to the field of obtaining insulating materials or for passive fire protection usable in a wide spectrum of the construction of buildings, warehouses and industrial facilities. These materials can be presented in the form of pads, bags, shaped, blankets or felts, coatings, plastering, gunite and panels whether they are flexible, rigid or semi-rigid. Its use can be highlighted in fire-resistant divisions or compartments such as fire doors, partitions, screens, transdos, suspended ceilings, protection of metal structures, etc.
- REPLACEMENT SHEET (Rule 28 ⁇ fossils, in different chemical and thermal processes, by recycling them in the form of materials that can provide significant added value, achieving, at the same time, a reduction in the cost of management and disposal of these by-products.
- thermal insulation and fire resistance are favored, with respect to the products with ashes from the combustion of coal, when ashes or slags are used that come from processes such as combustion, pyrolysis, gasification or other processes of heat treatment using biomass, or mixtures of fossil fuels and biomass, together with various binders and a minor proportion of additives.
- the characteristics of the products obtained from the aforementioned secondary raw materials can make them competitive against other commercial products with thermal insulation or fire resistance properties equal to or less than those of the products presented in this invention. .
- the present invention allows, for the first time, to be used in thermal insulation and for passive protection against fire, ashes or slags that come from processes such as combustion, pyrolysis, gasification or other thermal treatment processes that use biomass, or fuel mixtures fossils and biomass, in more than 50% by weight and dry basis, of the constituents of the final product.
- the most suitable ashes or slags are chosen among the different by-products that generate the heat treatment processes mentioned above.
- the ashes and slags are used without previous pretreatments, although depending on their physicochemical properties they can be subjected to separation, grinding, sieving and chemical attacks with acids or bases.
- the scope of these operations is given by the degree of improvement that is desired in the final product with respect to the following properties: fire resistance, thermal conductivity, density, heat capacity, water storage capacity, acoustic absorption coefficient,
- REPLACEMENT SHEET (Rule 28 ⁇ resistance to compression, flexion and impact, product stiffness, hardness and color, or to eliminate unwanted residue components.
- the ashes, slags or their mixtures are used alone or together with:
- the content of the additives or their mixtures does not exceed, on a dry basis, 50% by weight of the constituents of the final product.
- the manufacturing process consists of either mixing the constituents (waste and additives) without agglomerating or obtaining a homogeneous paste by adding the proportion of water required to the mixture of waste and additive, depending on the properties of the materials residuals and the application you want to obtain from the final product.
- mixtures of the non-agglomerated constituents or the kneaded mixtures can be subjected, during or after the setting period, to a series of operations that help to improve some of their insulating or mechanical properties, such as:
- REPLACEMENT SHEET (Rule 28 ⁇ different heating rates, and isothermal plateaus of different duration, between room temperature and 1800 0 C.
- the consolidation consists of the immersion or bath of the piece already set in a solution that is introduced into the pores of the pieces, creating a mesh that improves the mechanical properties (resistance to compression, flexion and impact, stiffness of the products, hardness) and physical properties (density, water storage capacity). This treatment can also be done by bristle brushes or by low pressure spraying (maximum 0.5 bar).
- the process of this invention allows the pastes made by mixing the constituents to be used in different forms of forming or molding, or by projection by dry or wet (gunite) route of the pastes on the elements to be isolated.
- Un agglomerated materials or pastes are prepared by combining waste, additives and water in different mixtures and proportions, according to the characteristics and insulating and mechanical properties of fire resistance, thermal conductivity, density, heat capacity, water storage capacity, coefficient of acoustic absorption, resistance to compression, flexion and impact, rigidity of the products, hardness and color that are desired to obtain.
- REPLACEMENT SHEET (Rule 28 ⁇ These constituents are placed in a planetary kneader, and mixed for five minutes with an average speed of 140 rpm until a homogeneous mixture is obtained, so that 1883.6 g of pasta are obtained.
- 750 ml_ of water are taken; this being the water / solid ratio that optimizes the insulating and mechanical properties for this composition, and is added to the mixture of constituents described above, kneading in the planetary kneader for ten minutes at an average speed of 140 rpm until homogenization.
- a mold is filled with the hydrated paste before it begins to set. In this practical example, a 2 cm thick, 27.5 cm high and 18 cm wide plate has been manufactured. Once the mold is filled, it is allowed to set at room temperature, being demoulded at 24 hours. The demoulded piece obtained is allowed to finish curing at room temperature for a period greater than 28 days. Once the material is cured, the consolidation treatment is carried out on the plate.
- This process consists in impregnating the plate, by immersion, in a solution composed of ethyl esters of the silicic acid dissolved in mineral turpentine, at a temperature between 1O 0 C and 25 0 C, until the rejection of the consolidating product occurs.
- the plate remains for 34 minutes immersed in the bath, and outside the bath the consolidation reaction is allowed to complete for approximately four weeks at a temperature of 2 ° C and a relative humidity between 40 and 50%.
- the plate obtained is subjected to a temperature exposure that significantly reproduces the temperature of the fire resistance test according to UNE-EN 1363-1, as shown in the attached graph.
- the plate has been subjected to the thermal program that appears in said standard, and the temperature has been recorded both on the exposed face and on the unexposed face of the plate.
- the time it takes to reach Ia unexposed face has been measured according to the criteria of Ia standard cited above, the time it takes to reach Ia unexposed face the temperature of 18O 0 C.
- the results obtained for the embodiment of the test show that the time to reach the unexposed face of the plate a temperature of 18O 0 C is 33 minutes and 45 seconds. This time is 25% higher than that recorded in the same test with plates of the same dimensions, whose
- REPLACEMENT SHEET (Rule 28 ⁇ Major constituents are fly ash from the combustion of coal, or with fire-resistant plates based on calcium silicate, currently on the market. In addition, during the performance of the test the emission of gases has not been observed, and the plate has maintained the mechanical stability before, during and after the test.
Landscapes
- Engineering & Computer Science (AREA)
- Chemical & Material Sciences (AREA)
- Civil Engineering (AREA)
- Ceramic Engineering (AREA)
- Environmental & Geological Engineering (AREA)
- Materials Engineering (AREA)
- Structural Engineering (AREA)
- Organic Chemistry (AREA)
- Processing Of Solid Wastes (AREA)
Abstract
The invention relates to a method of obtaining materials with good thermal insulation and fire resistance properties, based on waste (ash and slag) originating from processes such as combustion, pyrolysis, gasification and other thermal treatment processes that use biomass or mixtures comprising biomass and fossil fuels. The materials thus produced are characterised in that ash, slag or mixtures thereof represent, on a dry basis, more than 50 % of the weight of the product as it is used as an insulating material, without agglomerating or mixing same with water for the purpose of mixing and subsequent shaping or guniting. The recycling of the above-mentioned materials provides a novel use for waste from thermal and chemical processes in high-value-added applications as thermal-insulation or fire-resistant elements for use in industrial plants, premises or buildings.
Description
TITULOTITLE
Obtención de materiales aislantes a partir de residuos de procesos térmicos que utilizan biomasaObtaining insulating materials from waste from thermal processes that use biomass
OBJETO DE LA INVENCIÓN Se refiere Ia presente invención a Ia obtención de aislamientos térmicos y de materiales resistentes al fuego, fabricados con cenizas o escorias que proceden de procesos como Ia combustión, pirólisis o gasificación de biomasa o de mezclas de combustibles fósiles-biomasa, representando las cenizas, escorias o las mezclas de las anteriores, en base seca, más del 50 % en peso de los constituyentes del producto final.OBJECT OF THE INVENTION The present invention relates to obtaining thermal insulation and fire-resistant materials, manufactured with ashes or slags that come from processes such as combustion, pyrolysis or gasification of biomass or mixtures of fossil-biomass fuels, representing the ashes, slags or mixtures of the above, on a dry basis, more than 50% by weight of the constituents of the final product.
La invención es aplicable fundamentalmente al ámbito de Ia obtención de materiales aislantes o para Ia protección pasiva contra el fuego utilizables en un amplio espectro de Ia construcción de edificios, naves e instalaciones industriales. Estos materiales pueden presentarse en forma de almohadillas, sacos, conformados, mantas o fieltros, revestimientos, enfoscados, gunitados y paneles bien sean flexibles, rígidos o semi-rígidos. Se puede destacar su uso en divisiones o compartimentaciones resistentes al fuego como puertas cortafuego, tabiques, mamparas, trasdosados, falsos techos, protección de estructuras metálicas, etc.The invention is fundamentally applicable to the field of obtaining insulating materials or for passive fire protection usable in a wide spectrum of the construction of buildings, warehouses and industrial facilities. These materials can be presented in the form of pads, bags, shaped, blankets or felts, coatings, plastering, gunite and panels whether they are flexible, rigid or semi-rigid. Its use can be highlighted in fire-resistant divisions or compartments such as fire doors, partitions, screens, transdos, suspended ceilings, protection of metal structures, etc.
ESTADO DE LA TÉCNICASTATE OF THE TECHNIQUE
Algunos de los productos comerciales empleados como aislantes térmicos o para Ia protección pasiva contra el fuego, tienen una composición química y propiedades que pueden esperarse en mezclas inorgánicas a base de cenizas y escorias. En este sentido, los resultados de estudios desarrollados por los investigadores que presentan esta solicitud de patente, en los que se han analizado las posibles aplicaciones de las cenizas de combustión del carbón junto con aglomerantes como el cemento portland y otros residuos industriales, en el campo de Ia protección pasiva contra el fuego, avalan esta hipótesis ('Development of new fire-proof producís made from coal fly ash: the CEFYR project'. Journal of Chemical Technology and Biotechnology, 77 (2003) 361-366 ySome of the commercial products used as thermal insulators or for passive fire protection have a chemical composition and properties that can be expected in inorganic mixtures based on ash and slag. In this sense, the results of studies developed by the researchers who present this patent application, in which the possible applications of coal combustion ashes have been analyzed together with binders such as Portland cement and other industrial waste, in the field of passive fire protection, support this hypothesis ('Development of new fire-proof producís made from coal fly ash: the CEFYR project'. Journal of Chemical Technology and Biotechnology, 77 (2003) 361-366 and
HOJA DE REEMPLAZO (Regla 28)
'Recycling potential of coal fly ash and titanium waste as new fire-proof producís'. Chemical Engineering Journal, 95,(2003) 155-161].REPLACEMENT SHEET (Rule 28) 'Recycling potential of coal fly ash and titanium waste as new fire-proof producís'. Chemical Engineering Journal, 95, (2003) 155-161].
Se ha demostrado en muchos casos que es posible obtener materiales aislantes térmicos y resistentes al fuego a partir de residuos industriales sin valor de mercado (cuando no onerosos para el medio ambiente). Así, por ejemplo, en pastas constituidas mayoritariamente por cenizas volantes de Ia combustión del carbón se suelen dar las características generalmente exigibles a los productos aislantes o resistentes al fuego como son: incombustibilidad, estabilidad a temperaturas elevadas, no generación de humos ni gases en condiciones de incendios y ausencia de características ecotóxicas. Además, cuando se conforman como placas o como pastas proyectadas, dichos morteros poseen, a igualdad de espesores, una capacidad aislante comparable a Ia de productos comerciales a base de silicato calcico, un producto muy utilizado en aislamientos térmicos y para Ia protección pasiva contra el fuego de edificios, naves e instalaciones industriales. Asimismo, como alternativa al vertido de las cenizas procedentes de Ia combustión del carbón, han aparecido en los últimos años aplicaciones de reciclado de las mismas en: productos cerámicos, productos a base de silicato calcico, morteros y hormigones, paneles para Ia construcción y puertas corta fuego (JP Patent 09100153 A2 -1997-, JP Patent 2000086348 A2 -2000-, JP Patent 2001151506-A —2001-, WO Patent 9709283-A -1997-, WO Patent 200035826 B1 -2000-, CN Patent 1264688 A -2000-, JP Patent 11180743-A -1999-, EP Patent 999606-A - 1999-, JP Patent 5279136-A -1993-, JP Patent 10025170 A2 -1998-, WO Patent 200181267-A2 -2002-, CN Patent 1198418-A -1999-, DE Patent 19930653-A1 - 2001-, CN Patent 1280962-A -2001-, TW Patent 402658-A -2001-, NZ Patent 333778-A -2000-).It has been demonstrated in many cases that it is possible to obtain thermal and fire-resistant insulating materials from industrial waste with no market value (when not burdensome for the environment). Thus, for example, in pastes constituted mainly by fly ash of coal combustion, the characteristics generally required of insulating or fire resistant products are usually given, such as: incombustibility, stability at high temperatures, no generation of fumes or gases in conditions of fires and absence of eco-toxic characteristics. In addition, when they are formed as plates or as projected pastes, said mortars have, with equal thickness, an insulating capacity comparable to that of commercial products based on calcium silicate, a product widely used in thermal insulation and for passive protection against fire of buildings, warehouses and industrial facilities. Likewise, as an alternative to the pouring of the ashes from the combustion of coal, recycling applications have appeared in recent years in: ceramic products, products based on calcium silicate, mortars and concretes, construction panels and doors Fire cut (JP Patent 09100153 A2 -1997-, JP Patent 2000086348 A2 -2000-, JP Patent 2001151506-A —2001-, WO Patent 9709283-A -1997-, WO Patent 200035826 B1 -2000-, CN Patent 1264688 A - 2000-, JP Patent 11180743-A -1999-, EP Patent 999606-A - 1999-, JP Patent 5279136-A -1993-, JP Patent 10025170 A2 -1998-, WO Patent 200181267-A2 -2002-, CN Patent 1198418 -A -1999-, DE Patent 19930653-A1 - 2001-, CN Patent 1280962-A -2001-, TW Patent 402658-A -2001-, NZ Patent 333778-A -2000-).
Dado el previsible aumento del uso de Ia biomasa como fuente de energía o como materia prima de otros procesos, en el futuro se van a generar nuevos tipos de cenizas y escorias en grandes cantidades, por Io que diferentes esfuerzos tecnológicos se van a orientar hacia Ia búsqueda de nuevas alternativas de utilización de estos residuos, distintas a su eliminación en vertederos. Por tanto, con Ia presente invención se disminuyen los problemas medioambientales que previsiblemente ocasionarán las cenizas y escorias procedentes de Ia utilización de Ia biomasa o mezclas de biomasa y combustiblesGiven the foreseeable increase in the use of biomass as a source of energy or as a raw material for other processes, in the future new types of ashes and slags will be generated in large quantities, so that different technological efforts will be directed towards search for new alternatives for using this waste, other than its disposal in landfills. Therefore, with the present invention, the environmental problems that the ashes and slags caused by the use of biomass or mixtures of biomass and fuels are expected to be reduced
HOJA DE REEMPLAZO (Regla 28}
fósiles, en diferentes procesos químicos y térmicos, mediante su reciclado en forma de materiales que puedan aportarle un valor añadido importante, consiguiéndose, al mismo tiempo, una reducción en el coste de gestión y vertido de dichos subproductos.REPLACEMENT SHEET (Rule 28} fossils, in different chemical and thermal processes, by recycling them in the form of materials that can provide significant added value, achieving, at the same time, a reduction in the cost of management and disposal of these by-products.
Además, las características de aislamiento térmico y de resistencia al fuego se ven favorecidas, con respecto a los productos con cenizas de Ia combustión del carbón, cuando se utilizan cenizas o escorias que proceden de procesos como Ia combustión, pirólisis, gasificación u otros procesos de tratamiento térmico que utilizan biomasa, o mezclas de combustibles fósiles y biomasa, junto con diversos aglomerantes y una proporción minoritaria de aditivos.In addition, the characteristics of thermal insulation and fire resistance are favored, with respect to the products with ashes from the combustion of coal, when ashes or slags are used that come from processes such as combustion, pyrolysis, gasification or other processes of heat treatment using biomass, or mixtures of fossil fuels and biomass, together with various binders and a minor proportion of additives.
Asimismo, las características de los productos obtenidos a partir de las materias primas secundarias antes mencionadas, pueden hacerlos competitivos frente a otros productos comerciales con propiedades de aislamiento térmico o de resistencia al fuego iguales o inferiores a las de los productos que se presentan en esta invención.Likewise, the characteristics of the products obtained from the aforementioned secondary raw materials, can make them competitive against other commercial products with thermal insulation or fire resistance properties equal to or less than those of the products presented in this invention. .
DESCRIPCIÓN DE LA INVENCIÓNDESCRIPTION OF THE INVENTION
La presente invención permite utilizar, por primera vez, en aislamientos térmicos y para Ia protección pasiva contra el fuego, cenizas o escorias que proceden de procesos como Ia combustión, pirólisis, gasificación u otros procesos de tratamiento térmico que utilizan biomasa, o mezclas de combustibles fósiles y biomasa, en más del 50 % en peso y base seca, de los constituyentes del producto final.The present invention allows, for the first time, to be used in thermal insulation and for passive protection against fire, ashes or slags that come from processes such as combustion, pyrolysis, gasification or other thermal treatment processes that use biomass, or fuel mixtures fossils and biomass, in more than 50% by weight and dry basis, of the constituents of the final product.
Para mejorar las propiedades aislantes y de resistencia al fuego de los productos fabricados, se escogen las cenizas o escorias más adecuadas entre los distintos subproductos que generen los procesos de tratamiento térmico citados anteriormente.To improve the insulating and fire resistance properties of the manufactured products, the most suitable ashes or slags are chosen among the different by-products that generate the heat treatment processes mentioned above.
Las cenizas y escorias se usan sin pretratamientos previos, aunque en función de sus propiedades físico-químicas pueden ser sometidas a tratamientos de separación, molienda, tamizado y ataques químicos con ácidos o bases. El alcance de estas operaciones viene dado por el grado de mejora que se desee conseguir en el producto final con respecto a las siguientes propiedades: resistencia al fuego, conductividad térmica, densidad, capacidad calorífica, capacidad de almacenamiento de agua, coeficiente de absorción acústico,The ashes and slags are used without previous pretreatments, although depending on their physicochemical properties they can be subjected to separation, grinding, sieving and chemical attacks with acids or bases. The scope of these operations is given by the degree of improvement that is desired in the final product with respect to the following properties: fire resistance, thermal conductivity, density, heat capacity, water storage capacity, acoustic absorption coefficient,
HOJA DE REEMPLAZO (Regla 28}
resistencia a compresión, flexión e impacto, rigidez de los productos, dureza y color, o bien eliminar componentes del residuo indeseados. Para Ia fabricación del producto final, las cenizas, escorias o sus mezclas se utilizan solas o junto con:REPLACEMENT SHEET (Rule 28} resistance to compression, flexion and impact, product stiffness, hardness and color, or to eliminate unwanted residue components. For the manufacture of the final product, the ashes, slags or their mixtures are used alone or together with:
• Aditivos con propiedades aglomerantes (yeso, cal, cemento, escayola, cenizas volantes procedentes de Ia combustión del carbón, óxido de magnesio, alúmina, fosfatos de magnesio, arena , gravilla o similares) • Aditivos con Ia capacidad de producir reacciones endotérmicas (sales hidratadas, hidróxidos)• Additives with binding properties (gypsum, lime, cement, plaster, fly ash from the combustion of coal, magnesium oxide, alumina, magnesium phosphates, sand, gravel or similar) • Additives with the ability to produce endothermic reactions (salts hydrated, hydroxides)
• Aditivos que aumentan Ia capacidad de almacenamiento de agua (silica gel, vermiculita, perlita, arlita, geles super-absorbentes de agua)• Additives that increase water storage capacity (silica gel, vermiculite, perlite, arlite, water-absorbing gels)
• Aditivos con Ia capacidad de producir poros en el material (polvo de aluminio, agua oxigenada)• Additives with the ability to produce pores in the material (aluminum powder, hydrogen peroxide)
• Aditivos que mejoran Ia resistencia mecánica (fibras orgánicas o inorgánicas)• Additives that improve the mechanical resistance (organic or inorganic fibers)
• Aditivos que alteran Ia presentación de los productos finales (colorantes)• Additives that alter the presentation of the final products (dyes)
• Aditivos que alteran el tiempo de fraguado del material (cloruro sódico, aditivos fluidificantes, aditivos plastificantes)• Additives that alter the setting time of the material (sodium chloride, fluidizing additives, plasticizing additives)
El contenido de los aditivos o de sus mezclas no supera, en base seca, el 50 % en peso de los constituyentes del producto final.The content of the additives or their mixtures does not exceed, on a dry basis, 50% by weight of the constituents of the final product.
El proceso de elaboración consiste bien en Ia mezcla de los constituyentes (residuo y aditivos) sin aglomerar o bien en Ia obtención de una pasta homogénea añadiendo Ia proporción de agua requerida a Ia mezcla de residuo y aditivo, en función de las propiedades de los materiales residuales y de Ia aplicación que se desee obtener del producto final.The manufacturing process consists of either mixing the constituents (waste and additives) without agglomerating or obtaining a homogeneous paste by adding the proportion of water required to the mixture of waste and additive, depending on the properties of the materials residuals and the application you want to obtain from the final product.
Adicionalmente, las mezclas de los constituyentes sin aglomerar o las mezclas amasadas, pueden ser sometidas, durante o tras el periodo de fraguado, a una serie de operaciones que ayudan a mejorar alguna de sus propiedades aislantes o mecánicas, como:Additionally, the mixtures of the non-agglomerated constituents or the kneaded mixtures can be subjected, during or after the setting period, to a series of operations that help to improve some of their insulating or mechanical properties, such as:
El tratamiento térmico del material sin aglomerar o de las piezas obtenidas. Dicho tratamiento consiste en rampas de calentamiento, conThe heat treatment of un agglomerated material or of the pieces obtained. Said treatment consists of heating ramps, with
HOJA DE REEMPLAZO (Regla 28}
distintas velocidades de calentamiento, y mesetas isotérmicas de distinta duración, entre Ia temperatura ambiente y 18000C. La utilización de consolidantes. La consolidación consiste en Ia inmersión o baño de Ia pieza ya fraguada en una solución que se introduce en los poros de las piezas, creando una malla que mejora las propiedades mecánicas (resistencia a compresión, flexión e impacto, rigidez de los productos, dureza ) y las propiedades físicas (densidad, capacidad de almacenamiento de agua). Este tratamiento puede hacerse igualmente mediante brochas de cerdas o mediante un rociado a baja presión (máximo de 0,5 bar).REPLACEMENT SHEET (Rule 28} different heating rates, and isothermal plateaus of different duration, between room temperature and 1800 0 C. The use of consolidants. The consolidation consists of the immersion or bath of the piece already set in a solution that is introduced into the pores of the pieces, creating a mesh that improves the mechanical properties (resistance to compression, flexion and impact, stiffness of the products, hardness) and physical properties (density, water storage capacity). This treatment can also be done by bristle brushes or by low pressure spraying (maximum 0.5 bar).
El procedimiento de esta invención permite que las pastas elaboradas por mezcla de los constituyentes se utilicen en distintas formas de conformado o moldeado, o mediante proyección por vía seca o húmeda (gunitado) de las pastas sobre los elementos que se van aislar.The process of this invention allows the pastes made by mixing the constituents to be used in different forms of forming or molding, or by projection by dry or wet (gunite) route of the pastes on the elements to be isolated.
Los materiales sin aglomerar o las pastas se preparan combinando los residuos, aditivos y agua en diferentes mezclas y proporciones, según las características y propiedades aislantes y mecánicas de resistencia al fuego, conductividad térmica, densidad, capacidad calorífica, capacidad de almacenamiento de agua, coeficiente de absorción acústico, resistencia a compresión, flexión e impacto, rigidez de los productos, dureza y color que se desean obtener.Un agglomerated materials or pastes are prepared by combining waste, additives and water in different mixtures and proportions, according to the characteristics and insulating and mechanical properties of fire resistance, thermal conductivity, density, heat capacity, water storage capacity, coefficient of acoustic absorption, resistance to compression, flexion and impact, rigidity of the products, hardness and color that are desired to obtain.
MODO DE REALIZACIÓN DE LA INVENCIÓNEMBODIMENT OF THE INVENTION
Para Ia fabricación del material ejemplo de realización práctica, se toman 1300 g de residuo procedente de Ia combustión de Ia biomasa residual presente en el residuo de extracción de aceite de oliva (orujillo), 18,8 g de residuo procedente de Ia combustión de Ia biomasa residual presente en Ia cascarilla de arroz, 546 g de yeso y 18 gramos de fibra de vidrio, Io cual lleva a una composición como Ia mostrada en Ia Tabla 1.For the manufacture of the example material of practical embodiment, 1300 g of waste from the combustion of the residual biomass present in the olive oil extraction residue (orujillo), 18.8 g of waste from the combustion of the Ia are taken residual biomass present in the rice husk, 546 g of plaster and 18 grams of fiberglass, which leads to a composition as shown in Table 1.
HOJA DE REEMPLAZO (Regla 28}
Estos constituyentes se colocan en una amasadora planetaria, y se mezclan durante cinco minutos con una velocidad media de 140 rpm hasta conseguir una mezcla homogénea, de forma que se obtienen 1883,6 g de pasta.REPLACEMENT SHEET (Rule 28} These constituents are placed in a planetary kneader, and mixed for five minutes with an average speed of 140 rpm until a homogeneous mixture is obtained, so that 1883.6 g of pasta are obtained.
Se toman 750 ml_ de agua; siendo ésta Ia relación agua/sólido que optimiza las propiedades aislantes y mecánicas para esta composición, y se añaden a Ia mezcla de constituyentes antes descrita, amasándose en Ia amasadora planetaria durante diez minutos a velocidad media de 140 rpm hasta su homogeneización. Una vez mezclados, se rellena un molde con Ia pasta hidratada antes de que comience su fraguado. En este ejemplo de realización práctica, se ha fabricado una placa de 2 cm de espesor, 27,5 cm de altura y 18 cm de ancho. Una vez relleno el molde, se deja fraguar a temperatura ambiente, siendo desmoldada a las 24 horas. La pieza desmoldada obtenida se deja que finalice su curado a temperatura ambiente durante un periodo superior a 28 días. Finalizado el periodo de curado del material, se realiza sobre Ia placa obtenida un tratamiento de consolidación. Este proceso consiste en impregnar Ia placa, por inmersión, en una solución compuesta por esteres etílicos del ácido silícico disueltos en aguarrás mineral, a una temperatura entre 1O0C y 250C, hasta que se produce el rechazo del producto consolidante. En este ejemplo, Ia placa permanece durante 34 minutos inmersa en el baño, y fuera del baño se deja completar Ia reacción de consolidación durante aproximadamente cuatro semanas a una temperatura de 2O0C y una humedad relativa entre el 40 y el 50 %. Finalizado el periodo de consolidación, se somete Ia placa obtenida a una exposición de temperatura que reproduce significativamente Ia temperatura del ensayo de resistencia al fuego según norma UNE-EN 1363-1 , como se muestra en el gráfico que se adjunta. Para ello, se ha sometido Ia placa al programa térmico que aparece en dicha norma, y se ha registrado Ia temperatura tanto en Ia cara expuesta como en Ia cara no expuesta de Ia placa. Para analizar Ia capacidad aislante de Ia placa, se ha medido, de acuerdo con los criterios de Ia norma citada anteriormente, el tiempo que tarda en alcanzar Ia cara no expuesta Ia temperatura de 18O0C. Los resultados obtenidos durante Ia realización del ensayo muestran que el tiempo en alcanzar Ia cara no expuesta de Ia placa una temperatura de 18O0C es de 33 minutos y 45 segundos. Este tiempo es un 25% superior al registrado en el mismo ensayo con placas de las mismas dimensiones, cuyo750 ml_ of water are taken; this being the water / solid ratio that optimizes the insulating and mechanical properties for this composition, and is added to the mixture of constituents described above, kneading in the planetary kneader for ten minutes at an average speed of 140 rpm until homogenization. Once mixed, a mold is filled with the hydrated paste before it begins to set. In this practical example, a 2 cm thick, 27.5 cm high and 18 cm wide plate has been manufactured. Once the mold is filled, it is allowed to set at room temperature, being demoulded at 24 hours. The demoulded piece obtained is allowed to finish curing at room temperature for a period greater than 28 days. Once the material is cured, the consolidation treatment is carried out on the plate. This process consists in impregnating the plate, by immersion, in a solution composed of ethyl esters of the silicic acid dissolved in mineral turpentine, at a temperature between 1O 0 C and 25 0 C, until the rejection of the consolidating product occurs. In this example, the plate remains for 34 minutes immersed in the bath, and outside the bath the consolidation reaction is allowed to complete for approximately four weeks at a temperature of 2 ° C and a relative humidity between 40 and 50%. At the end of the consolidation period, the plate obtained is subjected to a temperature exposure that significantly reproduces the temperature of the fire resistance test according to UNE-EN 1363-1, as shown in the attached graph. For this, the plate has been subjected to the thermal program that appears in said standard, and the temperature has been recorded both on the exposed face and on the unexposed face of the plate. To analyze the insulating ability of the plate, has been measured according to the criteria of Ia standard cited above, the time it takes to reach Ia unexposed face the temperature of 18O 0 C. The results obtained for the embodiment of the test show that the time to reach the unexposed face of the plate a temperature of 18O 0 C is 33 minutes and 45 seconds. This time is 25% higher than that recorded in the same test with plates of the same dimensions, whose
HOJA DE REEMPLAZO (Regla 28}
constituyente mayoritario son cenizas volantes de Ia combustión del carbón, o con placas resistentes al fuego a base de silicato calcico, actualmente en el mercado. Además, durante Ia realización del ensayo no se ha observado Ia emisión de gases, y Ia placa ha mantenido Ia estabilidad mecánica antes, durante y después del ensayo.REPLACEMENT SHEET (Rule 28} Major constituents are fly ash from the combustion of coal, or with fire-resistant plates based on calcium silicate, currently on the market. In addition, during the performance of the test the emission of gases has not been observed, and the plate has maintained the mechanical stability before, during and after the test.
HOJA DE REEMPLAZO (Regla 28)
REPLACEMENT SHEET (Rule 28)
Claims
1. Obtención de materiales aislantes a partir de residuos de procesos térmicos que utilizan biomasa caracterizado porque más del 50% en peso y base seca del producto final está constituido por cenizas, escorias o mezclas de las anteriores, procedentes de los residuos de procesos de combustión, pirólisis, gasificación u otros procesos de tratamiento térmico que utilizan biomasa o mezclas de biomasa y combustibles fósiles.1. Obtaining insulating materials from waste from thermal processes that use biomass characterized in that more than 50% by weight and dry base of the final product is constituted by ashes, slags or mixtures of the previous ones, from combustion process residues , pyrolysis, gasification or other heat treatment processes that use biomass or mixtures of biomass and fossil fuels.
2. Obtención de materiales aislantes a partir de residuos de procesos térmicos que utilizan biomasa según reivindicación 1 , caracterizado porque las cenizas, escorias o mezclas de las anteriores empleadas son pretratadas mediante separación, molienda, tratamiento térmico y ataque con ácidos o bases, para Ia eliminación de los componentes de los residuos indeseados.2. Obtaining insulating materials from waste from thermal processes that use biomass according to claim 1, characterized in that the ashes, slags or mixtures of the above used are pretreated by separation, grinding, heat treatment and attack with acids or bases, for Ia Elimination of unwanted waste components.
3. Obtención de materiales aislantes a partir de residuos de procesos térmicos que utilizan biomasa según reivindicaciones anteriores, caracterizado porque el material se somete a un tratamiento térmico que consta de rampas de calentamiento y mesetas isotérmicas con distintas velocidades de calentamiento y duración, desde Ia temperatura ambiente hasta 1800 0C, mejorando las características y propiedades aislantes y mecánicas del producto final.3. Obtaining insulating materials from waste from thermal processes that use biomass according to previous claims, characterized in that the material is subjected to a thermal treatment consisting of heating ramps and isothermal plateaus with different heating rates and duration, from the temperature ambient up to 1800 0 C, improving the characteristics and mechanical and insulating properties of the final product.
4. Obtención de materiales aislantes a partir de residuos de procesos térmicos que utilizan biomasa según reivindicaciones anteriores, caracterizado porque el material se somete a un tratamiento de consolidación, mejorando las características y propiedades aislantes, mecánicas y físicas del producto final.4. Obtaining insulating materials from waste from thermal processes using biomass according to previous claims, characterized in that the material is subjected to a consolidation treatment, improving the characteristics and insulating, mechanical and physical properties of the final product.
5. Utilización del material aislante obtenido según reivindicaciones anteriores, para su uso en elementos destinados a Ia protección pasiva contra el fuego.5. Use of the insulating material obtained according to previous claims, for use in elements intended for passive fire protection.
HOJA DE REEMPLAZO (Regla 28} REPLACEMENT SHEET (Rule 28}
Applications Claiming Priority (2)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| ESP200401702 | 2004-07-08 | ||
| ES200401702A ES2245895B1 (en) | 2004-07-08 | 2004-07-08 | OBTAINING INSULATING MATERIALS FROM RESIDUES OF THERMAL PROCESSES THAT USE BIOMASS. |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| WO2006005783A1 true WO2006005783A1 (en) | 2006-01-19 |
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Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| PCT/ES2005/000383 WO2006005783A1 (en) | 2004-07-08 | 2005-07-05 | Method of obtaining insulating materials from waste from thermal processes that use biomass |
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| Country | Link |
|---|---|
| ES (1) | ES2245895B1 (en) |
| WO (1) | WO2006005783A1 (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| ES2940129A1 (en) * | 2022-12-05 | 2023-05-03 | Univ Madrid Politecnica | Procedure for obtaining a plaster-based construction material (Machine-translation by Google Translate, not legally binding) |
Families Citing this family (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| ES2351451B1 (en) * | 2009-05-27 | 2011-10-24 | Universidad De Sevilla | OBTAINING FIRE RESISTANT MATERIALS FROM WASTE FROM THE PRESERVED INDUSTRY. |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4659679A (en) * | 1985-01-25 | 1987-04-21 | Falk Richard A | Insulative composition and method of making articles therefrom |
| US6342088B1 (en) * | 1997-03-26 | 2002-01-29 | Ricegrower's Cooperative Limited | Insulation material |
Family Cites Families (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| FR2482486A1 (en) * | 1980-05-16 | 1981-11-20 | Daussan & Co | COVER POWDER FOR FUSION METAL BATH |
| JPS6013991B2 (en) * | 1982-10-07 | 1985-04-10 | 工業技術院長 | Manufacturing method of fireproof insulation material |
-
2004
- 2004-07-08 ES ES200401702A patent/ES2245895B1/en active Active
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2005
- 2005-07-05 WO PCT/ES2005/000383 patent/WO2006005783A1/en active Application Filing
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4659679A (en) * | 1985-01-25 | 1987-04-21 | Falk Richard A | Insulative composition and method of making articles therefrom |
| US6342088B1 (en) * | 1997-03-26 | 2002-01-29 | Ricegrower's Cooperative Limited | Insulation material |
Non-Patent Citations (1)
| Title |
|---|
| LEIVA C.: "Influence of the type of ash on the insulating capacity of fly ash mortars used for passive protection against fire", INTERNATIONAL ASH UTILIZATION SYMPOSIUM, PAER #58, 2003, Retrieved from the Internet <URL:http://www.flyash.info> [retrieved on 20050718] * |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| ES2940129A1 (en) * | 2022-12-05 | 2023-05-03 | Univ Madrid Politecnica | Procedure for obtaining a plaster-based construction material (Machine-translation by Google Translate, not legally binding) |
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| Publication number | Publication date |
|---|---|
| ES2245895B1 (en) | 2007-08-16 |
| ES2245895A1 (en) | 2006-01-16 |
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