WO1996034839A1 - Procede de fabrication de materiaux isolants et produits contenant lesdits materiaux - Google Patents

Procede de fabrication de materiaux isolants et produits contenant lesdits materiaux Download PDF

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Publication number
WO1996034839A1
WO1996034839A1 PCT/GB1996/001033 GB9601033W WO9634839A1 WO 1996034839 A1 WO1996034839 A1 WO 1996034839A1 GB 9601033 W GB9601033 W GB 9601033W WO 9634839 A1 WO9634839 A1 WO 9634839A1
Authority
WO
WIPO (PCT)
Prior art keywords
compound
silica
stabilizing reagent
aqueous mixture
fibrous
Prior art date
Application number
PCT/GB1996/001033
Other languages
English (en)
Inventor
Miodrag Markovic
Original Assignee
Bowman, Paul, Alan
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Priority claimed from YU28195A external-priority patent/YU49145B/sh
Application filed by Bowman, Paul, Alan filed Critical Bowman, Paul, Alan
Priority to AU55067/96A priority Critical patent/AU5506796A/en
Publication of WO1996034839A1 publication Critical patent/WO1996034839A1/fr

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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
    • C04B28/00—Compositions of mortars, concrete or artificial stone, containing inorganic binders or the reaction product of an inorganic and an organic binder, e.g. polycarboxylate cements
    • C04B28/18—Compositions of mortars, concrete or artificial stone, containing inorganic binders or the reaction product of an inorganic and an organic binder, e.g. polycarboxylate cements containing mixtures of the silica-lime type
    • 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
    • C04B40/00—Processes, in general, for influencing or modifying the properties of mortars, concrete or artificial stone compositions, e.g. their setting or hardening ability
    • C04B40/02—Selection of the hardening environment
    • C04B40/024—Steam hardening, e.g. in an autoclave
    • 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

  • This invention relates to a process for producing thermal insulating materials which are resistant to high temperatures . More particularly it relates to a process for producing thermal insulating materials in the form of calcium hydrosilicate compounds. The invention also relates to products of the process.
  • the properties of the products obtained using these processes depend mostly upon the crystal form of the so produced hydrosilicate, the shape and size of crystals and the distribution and size of pores.
  • inorganic fibres for example asbestos, glass or mineral
  • organic fibres for example cellulose
  • USA Patent No 3,988,419 describes a process of C-S-H synthesis from an aqueous solution of very fine amorphous Si0 2 (from waste dust out of a furnace for the production of Si, FeSi or SiC) and lime.
  • the solution is heated for some time at a temperature of 100 °C under normal pressure while stirring to form a gel.
  • the gel is then transferred into a rotary press where it is mashed slowly under pressure of saturated water steam of about 8kP/cm 2 until the gel is transformed into a viscous-elastic material which is poured into moulds .
  • the moulds are then introduced into an autoclave and exposed to hydrothermal processing by means of saturated water steam under a pressure of about 20kP/cm 2 to form crystals.
  • the material is then treated with overheated steam in order to allow the crystals to grow and also to dry the said crystals.
  • French Patent 2,505,814 describes a process which comprises the mixing of slaked lime, ground and ultra fine Si0 2 and synthetic fibres (allumosilicates, carbon) in an aqueous suspension. Moulds are then filled with the mixture which is then treated in an autoclave by means of saturated water steam under a pressure of about 12 bars and then dried for several days ' at the temperature of 330"C.
  • YU Patent 44,495 describes a process of synthesizing C-S-H to obtain a product which consists of the mineral tobermorite.
  • This product has good mechanical and thermal insulation properties but includes asbestos and linen fibres.
  • South African Patent 94/5548 describes a process of synthesizing C-S-H which contains the mineral xonotlite C 6 S 6 H. Due to the selection of raw materials, the ratios thereof and proper reaction conditions, the formed xonotlite provides finished products with higher rigidity and lower linear shrinkage at high temperatures and consequently higher thermal stability. The finished products are also free from asbestos fibres which are not desired and even forbidden lately because of harmful effects on human health.
  • a xonotlite molecule contains only one crystal water molecule and this differs, for example, from 11YA tobermorite (C 5 S 6 H S ) which contains five molecules of crystal bound water per molecule.
  • C 5 S 6 H S 11YA tobermorite
  • the phase transformation of C-S-H compound containing more crystal water molecules starts at a considerably lower temperature.
  • the presence of the mineral xonotlite decreases linear deformation and increases mechanical properties of the product due to high temperatures.
  • the addition of a fibrous component and a surfactant affects the formation of a microstructure which increases the viscosity of the porous material and makes the product resistant to sudden temperature changes.
  • thermoinsulating calcium hydrosilicate compound comprising:
  • the source of calcium ions may comprise lime.
  • the lime may comprise slaked lime preferably with a CaO content of not less than 72% by weight.
  • it may comprise quicklime preferably containing not less than 95% CaO.
  • the silica compound may comprise a compound selected from the group consisting of amorphous silica, silica sand, quartz, quartzite, diatomite and mixtures thereof.
  • it may comprise quartz and the quartz may be quartz which was previously treated at a temperature of not higher than 1000 * C and preferably between 800 and lOOO'C.
  • the silica compound contains not less than 98% (by weight) Si0 2 .
  • the silica compound has a particle size of below 63 ⁇ m and preferably at least 90% of the silica compound has a particle size of below 45 ⁇ m.
  • the silica compound and source of calcium ions may have a mole ratio of Ca 2+ /Si0 2 of between 0,91 and 1.2.
  • the amount of water in the aqueous mixture is 3 to 4 times higher by weight than the total dry substance.
  • the fibrous compound may comprise alkali stable fibres.
  • the fibres may be organic, inorganic, natural, synthetic or mixtures of such fibres.
  • Examples of fibres are mineral fibres, alkaline resistant glass fibres, cellulose fibres, polypropylene fibres, polyethylene fibres, polyester fibres, polyamide fibres, polyacrylonitrile fibres etc.
  • the fibres comprise sulphate fir white cellulose.
  • it comprises alkali resistant glass fibres which preferably have a 10% by weight Zr0 2 content and 5 - 8% by weight Ti0 2 content and preferably with a thickness of approximately 0,025 ⁇ m and a length of 15 to 25 ⁇ m.
  • the fibrous component may be introduced in an amount of 2 to 8% by weight of the total dry substance. Preferably it is introduced in an amount of 5 to 7% by weight of the total dry substance.
  • the stabilizing reagent is used to stabilize the aqueous mixture and may comprise a surfactant such as alkylphenolpolyglycol ether or a cellulose derivative.
  • a surfactant such as alkylphenolpolyglycol ether or a cellulose derivative.
  • it comprises a compound selected from the group consisting of carboxymethylcellulose (including salts thereof) , metasilicilic acid, active starch, gelatine, alkylhydroxyalkyl cellulose and glass fibres.
  • the carboxymethylcelllulose may comprise Na-carboxymethylcellulose and the alkylhydroxyalkyl- cellulose may comprise ethylhydroxyethylcellulose.
  • the stabilizing reagent comprises metasilicilic acid or Na-carboxymethylcellulose.
  • the stabilizing reagent is introduced in an amount of 0,2 to 1%, preferably 0,4 to 0,6% by weight of the total dry substance .
  • the lime, silica and stabilizing reagent are mixed with water to form an aqueous mixture; the fibrous compound is also mixed with water to form a separate aqueous mixture; and the two aqueous mixtures are then mixed together.
  • This mixture may then be introduced into moulds which are then subjected to hydrothermal treatment at a pressure above 12,5 bars but not above 15 bars.
  • the hydrothermal treatment may be carried out in an autoclave.
  • the hydrothermal treatment is carried out for a period of 10 to 25 hours.
  • the hydrothermally treated product may then be dried, preferably at a temperature of between 60 to 120 * C.
  • the calcium hydrosilicate compound includes the mineral xonotlite.
  • the product may comprise calcium hydrosilicate and preferably it includes xonotlite.
  • the slaked lime with a CaO content of 72% by weight was suspended in 2000 1 of water and stirred for 45 minutes. To this was added 513 1 of water with 8kg metasilicilic acid and 640kg of quartz.
  • the metasilicilic acid is a stabilizing reagent which stabilizes the mixtures of the components.
  • the quartz comprised pulverized quartz sand, containing 98% Si0 2 and the particle size was below 63 ⁇ m with at least 90% of the quartz having particle size of below 45 ⁇ m.
  • the sulphate fir white cellulose was suspended in 1770 1 of water.
  • the quartz, metasilicilic acid and lime suspension was added to the aqueous suspension of the cellulose.
  • the resulting slurry was stirred for 60 minutes, and then poured in moulds of dimensions 3 ,Omxl, 2mx0, 3m.
  • the moulds were then transferred to an autoclave and was hydrothermally treated by the introduction of saturated water steam. The treatment was carried out at a temperature of 198 "C.
  • a pressure of 14,9 bars was obtained in the autoclave within 50 minutes and maintained for 14 hours.
  • the autoclave was cooled in order that the pressure was reduced to 7 bars within 3 hours . Within a further 4 hours the pressure was reduced to atmospheric pressure.
  • the moulds were removed from the autoclave, the blocks were released and then dried at a temperature of not higher than 120 * C to have a moisture content of 10-20%.
  • the product obtained had a bulk density of 321 to 355kg/m 3 a bending strength to 2,7 MPa, with the mineral xonotlite in its structure.
  • Components 1 to 4 were the same as the components described in example 1.
  • Glass fibres were aklkali resistant, contained 10% (by weight) Zr0 2 and 5-8%Ti0 2 (by weight) and had a thickness of about 0.025 ⁇ m and a length of about 15-25 ⁇ m.
  • the quicklime contained 96% CaO.
  • the quartz and the rest of the components were the same as the components described in example 1.
  • a pressure of 14 bars was obtained within 90 minutes and maintained for 14 hours. After that the autoclave was cooled in order that the pressure was reduced to 8 bars within one hour. Within a further 4 hours the pressure was reduced to atmospheric pressure.
  • the product obtained had the following properties: a bulk density of 335 to 373kg/m 3 a bending strength of 2,5 mPa.
  • the product mainly consisted of cross-linked crystals of xonotlite.
  • the quicklime contained 97% CaO.
  • Ultra fine amorphous silica was used and it had a silica content and particle size as set out in example 1.
  • the stabilizing reagent was Na-carboxymethylcellulose.
  • the product obtained had the following properties: a bulk density of 320-340kg/m 3 , a bending strength of 3MPa.
  • the product mainly consisted of cross-linked crystals of xonotlite.

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Ceramic Engineering (AREA)
  • Materials Engineering (AREA)
  • Structural Engineering (AREA)
  • Organic Chemistry (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Inorganic Chemistry (AREA)
  • Health & Medical Sciences (AREA)
  • Toxicology (AREA)
  • Silicates, Zeolites, And Molecular Sieves (AREA)

Abstract

Cette invention concerne un procédé de fabrication d'un composé d'hydrosilicate de calcium ayant des propriétés d'isolation thermique, lequel procédé comprend les étapes suivantes: disposer d'une source d'ions calcium, d'un composé de silice, d'un réactif de stabilisation et d'un composé fibreux; effectuer un mélange aqueux à partir de la source d'ions calcium, du composé de silice, du réactif de stabilisation et du composant fibreux; et, enfin, soumettre le mélange aqueux à un traitement hydrothermique sous une pression supérieure à 12,5 bars, mais n'excédant pas 20 bars, et en présence de vapeur saturée à une température variant entre 190 et 212 °C afin de produire un composé d'hydrosilicate de calcium.
PCT/GB1996/001033 1995-05-04 1996-04-30 Procede de fabrication de materiaux isolants et produits contenant lesdits materiaux WO1996034839A1 (fr)

Priority Applications (1)

Application Number Priority Date Filing Date Title
AU55067/96A AU5506796A (en) 1995-05-04 1996-04-30 Process for producing insulating materials and products ther eof

Applications Claiming Priority (4)

Application Number Priority Date Filing Date Title
YU281/95 1995-05-04
YU28195A YU49145B (sh) 1995-05-04 1995-05-04 Postupak za proizvodnju termoizolacionog materijala na bazi kalcijum silikata
ZA95/10534 1995-12-12
ZA9510534A ZA9510534B (en) 1995-05-04 1995-12-12 Process for producing insulating materials and products thereof

Publications (1)

Publication Number Publication Date
WO1996034839A1 true WO1996034839A1 (fr) 1996-11-07

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Family Applications (1)

Application Number Title Priority Date Filing Date
PCT/GB1996/001033 WO1996034839A1 (fr) 1995-05-04 1996-04-30 Procede de fabrication de materiaux isolants et produits contenant lesdits materiaux

Country Status (2)

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AU (1) AU5506796A (fr)
WO (1) WO1996034839A1 (fr)

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2008151825A2 (fr) * 2007-06-15 2008-12-18 Acico Industries Co (K.S.C.C) Plaque coupe-feu en céramique et procédé de fabrication correspondant

Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
GB1269960A (en) * 1969-10-06 1972-04-12 Owens Corning Fiberglass Corp Method of making thermal insulation
FR2278647A1 (fr) * 1974-05-20 1976-02-13 Lille Inst Catholique Arts M Beton a haute resistance et son procede de fabrication
NL8100680A (nl) * 1981-02-12 1982-09-01 Warrior Insulation Werkwijze ter bereiding van calciumsilicaat en uit het verkregen calciumsilicaat gevormde structuur.
DE3641823A1 (de) * 1986-12-06 1988-06-16 Csp Chemie Entwicklungsgesells Verfahren und vorrichtung zur herstellung plattenfoermiger bauelemente aus caliciumsilikat
JPH07126083A (ja) * 1993-10-28 1995-05-16 Kuraray Co Ltd 無機質成形物の製造方法

Patent Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
GB1269960A (en) * 1969-10-06 1972-04-12 Owens Corning Fiberglass Corp Method of making thermal insulation
FR2278647A1 (fr) * 1974-05-20 1976-02-13 Lille Inst Catholique Arts M Beton a haute resistance et son procede de fabrication
NL8100680A (nl) * 1981-02-12 1982-09-01 Warrior Insulation Werkwijze ter bereiding van calciumsilicaat en uit het verkregen calciumsilicaat gevormde structuur.
DE3641823A1 (de) * 1986-12-06 1988-06-16 Csp Chemie Entwicklungsgesells Verfahren und vorrichtung zur herstellung plattenfoermiger bauelemente aus caliciumsilikat
JPH07126083A (ja) * 1993-10-28 1995-05-16 Kuraray Co Ltd 無機質成形物の製造方法

Non-Patent Citations (1)

* Cited by examiner, † Cited by third party
Title
DATABASE WPI Section Ch Week 9528, Derwent World Patents Index; Class L02, AN 95-212815, XP002011440 *

Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2008151825A2 (fr) * 2007-06-15 2008-12-18 Acico Industries Co (K.S.C.C) Plaque coupe-feu en céramique et procédé de fabrication correspondant
DE102007027653A1 (de) * 2007-06-15 2008-12-18 Horst Puckelwaldt Keramische Brandschutzplatte und Verfahren zu deren Herstellung
WO2008151825A3 (fr) * 2007-06-15 2009-04-02 Horst Puckelwaldt Plaque coupe-feu en céramique et procédé de fabrication correspondant

Also Published As

Publication number Publication date
AU5506796A (en) 1996-11-21

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