WO2007017912A1 - Matériau structural en céramique microporeuse - Google Patents

Matériau structural en céramique microporeuse Download PDF

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Publication number
WO2007017912A1
WO2007017912A1 PCT/IT2006/000567 IT2006000567W WO2007017912A1 WO 2007017912 A1 WO2007017912 A1 WO 2007017912A1 IT 2006000567 W IT2006000567 W IT 2006000567W WO 2007017912 A1 WO2007017912 A1 WO 2007017912A1
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range
comprised
weight
polyvinyl alcohol
solid mixture
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PCT/IT2006/000567
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English (en)
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Andrea Mancioli
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Cover Colofificio Ceramico S.R.L.
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Application filed by Cover Colofificio Ceramico S.R.L. filed Critical Cover Colofificio Ceramico S.R.L.
Priority to EP06780597A priority Critical patent/EP1919845A1/fr
Publication of WO2007017912A1 publication Critical patent/WO2007017912A1/fr

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    • C04B33/00—Clay-wares
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    • C04B33/13—Compounding ingredients
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    • E04—BUILDING
    • E04F—FINISHING WORK ON BUILDINGS, e.g. STAIRS, FLOORS
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Definitions

  • the present invention concerns a method for the production of microporous ceramic structural material, the ceramic material obtainable by means of said method and uses thereof.
  • the invention refers to the field of ceramic tiles, used to coat floors or walls.
  • the term tiles is used to indicate plates cut according to different shapes and dimensions.
  • ceramic is used, according to its common meaning, to indicate a product obtained, starting from a mixture of ceramic dusts, mainly based on clays and sand, by means of a production method comprising a formation step (through pressing or extruding) and a subsequent firing step.
  • the formation step task is that of aggregating dusts, having a certaing degree of humidity.
  • the firing step modifies the raw material structure, giving the final product the typical features of ceramic material regarding hardness, mechanical strength, chemical and phisical inertia.
  • Ceramic tiles can be classified according to their capacity of absorbing water.
  • Water absorbtion is a meter of the material porosity; high levels of water absorbtion indicate a porous structure, while low levels of water absorbtion indicate a compact structure.
  • Such a classification allows to directly derive other features of the ceramic material, in particular mechanical strength and modulus of rupture in bending. In fact, generally, the higher the material compatness, the higher its mechanical strength. On the other side, a high porosity generally is to the detriment of the material mechanical strength.
  • ceramic materials are more and more frequently used not only for domestic application, in which the aesthetic aspect is predominant, but also in public spaces, in which cases the ceramic tiles consitute the ideal solution that ⁇ an satisfy at the same time structural neeeds, such as breaking load, mechanical abrasion resistance and chemical resistance, but also aeshetic needs, since they can have different external appearance with regard to colour, luster, auditority or realising surfaces with particular outlinex.
  • the slipping resistance of a material for making floors is improved by increasing its surface roughness, to give an example by realising surface reliefs, which permit the drainage of eventually present liquids.
  • suitable slopes are realised, in order to make easier the deflux of water (due both to precipitations and washing).
  • the surfaces' features that allow to obtain a good slipping resistance (such as high roughness and presence of reliefs) obstruct the possibility to clean them effectively, since they constitute areas that are able to host and retain the dirt.
  • the surface's roughness and the presence of reliefs can be unsuitable for the aesthetic needs typical of the floor in a determined space.
  • the solution according to the present invention is proposed, whose aim is to provide a microporous ceramic structural material having a high drainage capacity, able to prevent the formation of a film of water or of other liquids on its surface.
  • a ceramic material that, notwithstanding its high porosity, at the same time presents high mechanical features and appreciable aesthetic featurex.
  • the provided microporous ceramic material presents a low density opposite to high mechanical capacities and can be used for the construction of ventilated walls having a reduced specific weight.
  • the mixture is allowed to settle for a period of time of about 24 hours.
  • the dimensions of the ceramic dusts used in said mixing step varies and can reach maximum values below 1 mm, and said grains of formulation based on polyvinyl alcohol (FPVA) have dimensions preferably below 0,40 mm.
  • FPVA polyvinyl alcohol
  • grain size of said solid mixture is comprised in a range (defineded in millimetres) selected between 0-0,25; 0-0,30; 0,05-0,30.
  • the grain size distribution and relative percentage of the ceramic dusts (PC) and grains of formulation based on polyvinyl alcohol (FPVA) of said solid mixture have the trend summarised in Table 1 : Table 1 - Grain size distribution and relative ercenta e of PC and FPVA
  • the grain size distribution of the grains of the solid mixture obtained by mixing together ceramic dusts (PC) and grains of formulation based on polyvinyl alcohol (FPVA) during the initial mixing step has the trend summarised in Table 2:
  • said ceramic dusts contain the following amount of oxydes, defined as a percentage by weight relative to the total of ceramic dusts: SiO 2 comprised in the range 50-75%, AI 2 O 3 comprised in the range 12-25%, CaO comprised in the range 0- 10%, MgO comprised in the range 0-6%, Na 2 O comprised in the range 0- 5%, K 2 O comprised in the range 0-4%.
  • said ceramic material presents a compressive breaking load comprised in the range 100-400 kg/cm 2 and a drainage capacity comprised in the range 20-350 L/(m 2 h).
  • said ceramic material presents a compressive breaking load comprised in the range 100-200 kg/cm 2 and a drainage capacity comprised in the range 200-350 l_/(m 2 h).
  • said ceramic material presents a compressive breaking load comprised in the range 250-400 kg/cm 2 and a drainage capacity comprised in the range 20-250 L/(m 2 h).
  • said ceramic material can be used for the production of wall coating tiles, whereas in the second case it can be used for the production of floor tilex.
  • said ceramic dusts (PC) being mixed together with said formulation based on polyvinyl alcohol, in the mixing step of the method previously defined, contain the following amount of oxides, defined in percentage by weight with regard to the whole ceramic dusts: SiO 2 comprised in the range 50-65%, Al 2 ⁇ 3 comprised in the range 12-20%, CaO comprised in the range 3-10%, MgO comprised in the range 2-6%, Na 2 O comprised in the range 0-1%, K 2 O comprised in the range 0-1%.
  • said ceramic dusts contain the following amounts of oxides: SiO 2 comprised in the range 60- 75%, AI 2 O 3 comprised in the range 18-25%, CaO comprised in the range 0-1 %, MgO comprised in the range 0-1 %, Na 2 O comprised in the range 1- 5%, K 2 O comprised in the range 0 ⁇ 5-4%.
  • Table 3 shows the grain size distribution of the grains of the formulation based on polyvinyl alcohol (FPVA)
  • Table 4 the grain size distribution of the ceramic dusts is reported (PC)
  • Table 5 shows the grain size distribution of the solid mixtures obtained by mixing together ceramic dusts (PC) and grains of the formulation based on polyvinyl alcohol (FPVA), with reference to the different examplex.
  • a mixture was prepared being constituted by atomised ceramic dusts and a granulometric formulation based on polyvinyl alcohol (FPVA) having a grain size distribution of the kind reported in Table 3.
  • the FPVA ⁇ formulation was constituted by 75% by weight of polyvinyl alcohol (PVA) having a molecular weight of 90000 and a hydrolysis rate of 88%, pentaerythritol (12% by weight), a mixture of oxy- ethylene glycols (mono-, di- and tri-oxy-ethylene glycol, 8% by weight), water (2% by weight), process additives (calcium stearate, oligosiloxane, borax and silica, 3% by weight).
  • a fluid solid mixture having a granulometric structure (with grain size distribution of the kind shown in Table 4) having the following composition percentage (defined by weight): white ceramic mixture (45%), black ceramic mixture (20%), blue ceramic mixture (25%), FPVA (10%).
  • the mixture was subsequently put in a press with isostatic buffers, operated by applying a specific pressure of 200 kg/cm 2 , in order to obtain articles with dimensions of 150 x 200 x 10 mm.
  • the formed articles subsequently underwent a quick firing inside a roller kiln, wherein in a first step the temperature was gradually increased, with a temperature gradient of 10°C/min, up to a maximum temperature of 700 0 C, obtaining the complete FPVA removal after 90 minutes. Subsequently, the temperature inside the kiln was increased, with a temperature gradient of 30°C/min, up to the maximum temperature of 121O 0 C, obtaining the complete sintering of the article after 60 minutes.
  • Tiles were obtained having the given dimensions, hourly drainage capacity of 200 L/m 2 and mechanical strength (compressive breaking load) of 190 kg/cm 2 .
  • Example 2 Obtained tiles can be conveniently used for coating floors.
  • Example 2
  • a mixture was prepared which was constituted by atomised ceramic dusts and a granulometric formulation based on polyvinyl alcohol (FPVA) with dimensional distribution of the kind shown in
  • the FPVA formulation was constituted by 80% by weight of PVA having molecular weight of 13.0000, hydrolysis rate of 78%, polyols mixture [tri-methylol propane (10% by weight), beta-cyclodextrine (6% by weight) and glycerol (2% by weight)] and process additives (calcium stearate, oligosiloxane, borax and silica, 2% by weight). From the aforesaid combination a fluid solid mixture is obtained having a granulometric structure (with grain size distribution of the kind shown in
  • Table 4 with the following composition percentage (defined by weight): white ceramic mixture (45%), black ceramic mixture (20%), dark blue ceramic mixture (23%), FPVA (12%).
  • the mixture was subsequently put in a press with isostatic buffers, operated by applying a specific pressure of 180 kg/cm 2 , in order to obtain articles with dimensions of 150 x 200 x 12 mm.
  • the formed articles subsequently underwent a quick firing inside a roller kiln, wherein in a first step .the temperature was gradually increased up to 800 0 C, with a temperature gradient of 7°C/min, obtaining the complete FPVA removal after 110 minutes.
  • the following sintering was obtained in 60 minutes, by increasing the temperature inside the kiln up to the maximum temperature of 1200 0 C, with a temperature gradient of 30°C/min.
  • a mixture was prepared which was constituted by atomized ceramic dusts and a granulometric formulation based on polyvinyl alcohol (FPVA) having dimensional distribution of the kind shown in Table 3.
  • the FPVA formulation was constituted by 70% by weight of
  • PVA having hydrolysis rate of 79% and molecular weight of 100000, polyols mixture [pentaerythritol (7% by weight), glycerol (3% by weight),
  • composition percentage (defined by weight): white ceramic mixture (45%), black ceramic mixture (20%), blue ceramic mixture (25%), FPVA (10%).
  • the mixture was subsequently put in a press with isostatic buffers, operated by applying a specific pressure of of 200 kg/cm 2 , in order to obtain articles with dimensions of 150 x 200 x 10 mm.
  • the formed articles subsequently underwent a slow firing inside an electric muffle kiln, with such a temperature gradient as to reach 250 0 C in 60 minutes, then 45O 0 C in 60 minutes more, 800 0 C after 120 minutes more and 1200 0 C after further 120 minutes. Then, the temperature was maintained constant at 1200 0 C for 10 minutes more. The complete FPVA removal was obtained after 110 minutes.
  • Example 4 In a helical mixer a mixture was prepared which was constituted by atomized ceramic dusts and a granulometric formulation based on polyvinyl alcohol (FPVA) having dimensional distribution of the kind shown in Table 3.
  • FPVA polyvinyl alcohol
  • the FPVA formulation was constituted by 60% by weight of PVA having molecular weight of;60000, hydrolysis rate of 60%, 20% PVA having hydrolysis rate of 79% and molecular weight of 100000, polyols mixture [pentaerythritol (6% by weight), glycerol (4% by weight), PEG 400 (7% by weight)] and process additives (calcium stearate, erucamide, oligosiloxane, borax and silica 3% by weight).
  • a fluid solid mixture having a granulometric structure (grain size distribution of the kind shown in Table 4) and the following composition percentage (defined by weight): white ceramic mixture (45%), superwhite ceramic mixture (25%), dark blue ceramic mixture (22%), FPVA (8%).
  • the mixture was subsequently put in a press with isostatic buffers, operated by applying a specific pressure of 220 kg/cm 2 , in order to obtain articles with dimensions of 150 x 200 x 11 mm.
  • the formed articles subsequently underwent a quick firing inside a roller kiln, wherein in a first step, by increasing the temperature with a temperature gradient of 15°C7min, up to a maximum temperature of 750 0 C, the complete removal of FPVA was obtained in 80 minutes.
  • the temperature inside the kiln was increased, at a temperature gradient of 30°C/min, up to the maximum temperature of 121O 0 C, thus obtaining the complete sintering of the article after 60 minutes.
  • Tiles were obtained having the given dimensions, hourly drainage capacity of 95 L/m 2 and mechanical strength (compressive breaking load) of 300 kg/cm 2 .
  • Example 5 In a helical mixer a mixture was prepared which was constituted by atomized ceramic dusts and a granulometric formulation based on polyvinyl alcohol (FPVA) having.dimensional distribution of the kind shown in Table 3.
  • the FPVA formulation was constituted by 80% by weight di PVA having molecular weight of 205000, hydrolysis rate of 88%, pentaerythritol (12% by weight), PEG 400 (5% by weight)] and process additives (calcium stearate, oligosiloxane, borax and silica 3% by weight).
  • a fluid solid mixture having a granulometric structure (grain size distribution of the kind shown in Table 4) with the following composition percentage (defined by weight): white ceramic mixture (40%), black ceramic mixture (23%), dark blue ceramic mixture (22%), FPVA (15%).
  • An aqueous solution of FPVA (10%) was added to the solid mixture, until the humidity of the mixture reached a value of 10%.
  • a specific pressure of 160 kg/cm 2 was applied to the mixture by means of a press with isostatic buffers, in order to obtain articles with dimensions of 150 x 200 x 8 mm.
  • the formed articles subsequently underwent a quick firing inside a roller kiln, wherein in a first step, by increasing the temperature with a temperature gradient of 6°C7min, up to the maximum temperature of 75O 0 C, the complete removal of FPVA was obtained in 120 minutes.
  • the temperature inside the kiln was increased, with a temperature gradient of 18°C/min, up to the maximum temperature of 113O 0 C, obtaining the complete sintering of the article after 60 minutes.
  • Tiles were obtained having the given dimensions, hourly drainage capacity of 300 L/m 2 and mechanical strength (compressive breaking load) of 130 kg/cm 2 . Obtained tiles can be used for coating walls.

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Ceramic Engineering (AREA)
  • Structural Engineering (AREA)
  • Organic Chemistry (AREA)
  • Materials Engineering (AREA)
  • Manufacturing & Machinery (AREA)
  • Inorganic Chemistry (AREA)
  • Dispersion Chemistry (AREA)
  • Architecture (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Civil Engineering (AREA)
  • Environmental & Geological Engineering (AREA)
  • Compositions Of Oxide Ceramics (AREA)
  • Finishing Walls (AREA)

Abstract

L'invention concerne un procédé de production d’un matériau structural en céramique microporeuse, en particulier destiné à la production de tuiles, comprenant les étapes suivantes : - mélanger des poussières de céramique avec une quantité, comprise dans la gamme de 1 à 30 % du poids total du mélange solide obtenu, de grains d'une formulation à base de poly(alcool vinylique) (FPAV) ; - augmenter le degré d'humidité dudit mélange solide avec une quantité d'eau comprise dans la gamme de 3 à 15 % en poids, du mélange solide, fournie sous la forme d’une solution aqueuse contenant de 0,5 à 30 % en poids de FPAV ; - comprimer les grains dudit mélange solide au moyen de l'application d'une pression spécifique comprise dans la gamme de 50 à 350 kg/cm2 ; - mettre en inertie les grains comprimés, au moyen d’un chauffage progressif jusqu'à une température maximale comprise dans la gamme de 150 à 8000 °C ; - fritter les grains, au moyen d’un autre chauffage progressif jusqu'à une température maximale comprise dans la gamme de 1000 à 12500 °C ; et - refroidir le matériau fritté. L’invention concerne en outre un matériau structural en céramique microporeuse pouvant être obtenu au moyen dudit procédé et leurs utilisations.
PCT/IT2006/000567 2005-08-05 2006-07-27 Matériau structural en céramique microporeuse WO2007017912A1 (fr)

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IT000423A ITRM20050423A1 (it) 2005-08-05 2005-08-05 Materiale ceramico strutturale microporoso.
ITRM2005A000423 2005-08-05

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CN110734277A (zh) * 2019-08-23 2020-01-31 福建贝迪陶瓷科技有限公司 一种人造珊瑚石的配方及制作工艺

Citations (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPS5113810A (en) * 1974-07-24 1976-02-03 Choichiro Hasumi Keiryogawarano seizohoho
GB1506728A (en) * 1975-06-24 1978-04-12 Poroton Ag Ceramics
GB1587766A (en) * 1977-12-01 1981-04-08 Socri Int Sa Method of manufacturing porous water-permeable and not frost-susceptible terra cotta pavings usable as ground coating and pavings thus obtained
US4954460A (en) * 1984-02-24 1990-09-04 Mino Yogyo Co., Ltd. Water-permeable ceramic material
DE4021627A1 (de) * 1990-07-06 1992-01-09 Wmf Wuerttemberg Metallwaren Verfahren zur herstellung von poroesen, keramischen formkoerpern und zugehoeriger formkoerper-rohling
JP2000282666A (ja) * 1999-03-30 2000-10-10 National House Industrial Co Ltd 床構造および耐磨耗性調湿タイル
DE10347356A1 (de) * 2003-10-11 2005-05-19 Wienerberger Ziegelindustrie Gmbh Verfahren u. Mischung zur Herstellung von Produkten der keramischen Industrie, insbesondere zur Herstellung von Mauerziegeln

Patent Citations (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPS5113810A (en) * 1974-07-24 1976-02-03 Choichiro Hasumi Keiryogawarano seizohoho
GB1506728A (en) * 1975-06-24 1978-04-12 Poroton Ag Ceramics
GB1587766A (en) * 1977-12-01 1981-04-08 Socri Int Sa Method of manufacturing porous water-permeable and not frost-susceptible terra cotta pavings usable as ground coating and pavings thus obtained
US4954460A (en) * 1984-02-24 1990-09-04 Mino Yogyo Co., Ltd. Water-permeable ceramic material
DE4021627A1 (de) * 1990-07-06 1992-01-09 Wmf Wuerttemberg Metallwaren Verfahren zur herstellung von poroesen, keramischen formkoerpern und zugehoeriger formkoerper-rohling
JP2000282666A (ja) * 1999-03-30 2000-10-10 National House Industrial Co Ltd 床構造および耐磨耗性調湿タイル
DE10347356A1 (de) * 2003-10-11 2005-05-19 Wienerberger Ziegelindustrie Gmbh Verfahren u. Mischung zur Herstellung von Produkten der keramischen Industrie, insbesondere zur Herstellung von Mauerziegeln

Non-Patent Citations (1)

* Cited by examiner, † Cited by third party
Title
DATABASE WPI Week 197612, Derwent World Patents Index; AN 1976-21484X, XP002407168 *

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