EP1871725A1 - Procede de fabrication de composants - Google Patents

Procede de fabrication de composants

Info

Publication number
EP1871725A1
EP1871725A1 EP06723679A EP06723679A EP1871725A1 EP 1871725 A1 EP1871725 A1 EP 1871725A1 EP 06723679 A EP06723679 A EP 06723679A EP 06723679 A EP06723679 A EP 06723679A EP 1871725 A1 EP1871725 A1 EP 1871725A1
Authority
EP
European Patent Office
Prior art keywords
phases
nanocrystalline
added
mpa
cement
Prior art date
Legal status (The legal status 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 status listed.)
Withdrawn
Application number
EP06723679A
Other languages
German (de)
English (en)
Inventor
Peter Stemmermann
Krassimir Garbev
Günter BEUCHLE
Uwe Schweike
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Karlsruher Institut fuer Technologie KIT
Original Assignee
Forschungszentrum Karlsruhe GmbH
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
Application filed by Forschungszentrum Karlsruhe GmbH filed Critical Forschungszentrum Karlsruhe GmbH
Publication of EP1871725A1 publication Critical patent/EP1871725A1/fr
Withdrawn legal-status Critical Current

Links

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
    • C04B28/186—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 containing formed Ca-silicates before the final hardening step
    • 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
    • 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
    • Y10—TECHNICAL SUBJECTS COVERED BY FORMER USPC
    • Y10S—TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y10S264/00—Plastic and nonmetallic article shaping or treating: processes
    • Y10S264/25—Metallic oxide
    • 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
    • Y10—TECHNICAL SUBJECTS COVERED BY FORMER USPC
    • Y10S—TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y10S264/00—Plastic and nonmetallic article shaping or treating: processes
    • Y10S264/35—Use of CaO with refractories

Definitions

  • the invention relates to a process for the preparation of components based on calcium silicate hydrates, which are also referred to as C-S-H phases.
  • This mixture which is referred to as cement paste, fresh mortar or fresh concrete, is poured into a mold and usually compressed mecha ⁇ nisch by shaking.
  • the mixture is composed so that a suitable consistency during processing and a sufficiently long processability are guaranteed.
  • the mixture must be so composed or post-treated so that after completion of the reaction with water, the required final strength is achieved.
  • CEM I portland cement
  • Minera ⁇ each perform a function:
  • Calcium aluminates, calcium aluminate ferritates and calcium sulfates which control processability and early strength.
  • the final strength is reduced by high porosity, small particle binding and reduced amount of the strength determ ⁇ Menden phases.
  • fly ash-belit low-calcium fly ash by a two-stage process. For this purpose, first a hydrothermal treatment of flyashes under saturated water vapor partial pressure at 200 0 C and then a roast at 700 ° C. After production, fly ash-belite cement is conventionally dressed and processed with water.
  • MDF macro defect free cement
  • Hot-Pressed Cement Paste by hardening conventionally water-treated and processed cement pastes at elevated pressure (3-5 kbar) and elevated temperature (150-250 0 C) known.
  • DE 28 32 125 C2 describes a method in which CaO and SiO 2 -containing materials with a synthetic calcium silicate, (CaO: SiO 2 - ratio of 0.8 to 1.1) and fibers are mixed with water. After a waiting period of at least 5 hours (“pre-reaction"), since the sedimentation tendency is prevented by stirring, a pumpable slurry is formed, which is poured into plate-like molds and dehydrated under pressure After autoclave hardening and drying, "fire-resistant dimensionally accurate lightweight building boards” in front. The calcium silicate synthetic origin, which ⁇ by autoclave curing is made.
  • DE 33 02 729 A1 discloses the reaction of aqueous-dispersed
  • the present invention is based on the synthesis of calcium silicate hydrates (C-S-H phases) in aqueous solution or suspension with a layered structure.
  • C-S-H phases calcium silicate hydrates
  • the fact that the method according to the invention actually produces such a layer structure can be observed by X-ray structure analysis, since such a structure, as soon as it has a regular spacing, leaves a so-called basal reflex in the X-ray diffractogram.
  • a line in the range of 9 ⁇ to 20 ⁇ forms, which indicates the formation of this layer structure.
  • the present invention utilizes the formation of an electric double layer at the interface between a solid and a liquid phase.
  • a star ⁇ re layer of ions behind which a diffuse charge cloud of ions accumulates.
  • the electric potential is referred to as zeta potential or electron-trokineticians, falls of its magnitude by first strongly within the rigid layer from to fall in the liquid thereto at ⁇ closing phase either slightly further (positive zeta potential) or slightly higher (negative zeta potential)
  • ⁇ is the viscosity of the liquid, v its velocity, ⁇ r its relative permittivity and E the electric field, is a measure of the mobility of the ions.
  • the surface of the solid preferably consists of negatively charged 0 2 ⁇ ions, so that a rigid layer of Ca 2+ ions is formed in the solution adjacent thereto. Here, a diffused layer of 0H ⁇ and Ca 2+ ions is deposited.
  • the surface-distant solution is electrically neutral.
  • Suitable additives modify the interfaces or layers, especially by acting as nuclei for self-assembly of aggregates in the size range up to 1 micron with controllable properties. This process was detected by surface analyzes.
  • an aqueous solution of calcium oxide CaO and silicon dioxide SiO 2 is provided in accordance with method step a).
  • the molar ratio of calcium to silicon (Ca: Si) takes a value in the range between 0.5: 1.0 to 2.5: 1.0, preferably from 0.5: 1.0 to 1.0: 1, 0, with the boundaries included.
  • calcium hydroxide Ca (OH) 2 forms simultaneously in the system CaO-SiO 2 -H 2 O, as a result of which an otherwise inventively produced component no longer has sufficient strength.
  • the water to solid ratio in the preparation of the C-S-H phases is freely selectable within wide limits.
  • the proportion of water is 4-20 times, more preferably approximately 10 times the total weight of the solids.
  • the raw material used is preferably lime CaO or calcium hydroxide-containing sludges.
  • the silicate source used is preferably Aerosil, silicic acid (pyrogenic or precipitated), kieselguhr, waterglass solutions, technical by-products such as microsilica from the production of ferrosilicum, slags from waste incineration or blast furnace processes, granulated blastfurnace or fly ash.
  • aqueous phase according to process step c) is separated off (eg filtered off), leaving behind nanocrystalline material which is removed according to process step d) and dried to a powder.
  • the solid product is thus separated from the suspension water and dried, resulting in a free-flowing, storage-resistant powder, which is not subjected to any further temperature or steam pressure treatment.
  • This dry powder is then filled immediately or after intermediate storage according to process step e) in a prepared form.
  • pressure preferably between 50 MPa and 500 MPa, more preferably between 100 MPa and 200 MPa, the dry powder compacts into a solid component without subsequent temperature treatment.
  • the nanocrystalline C-S-H phases are connected by a self-healing process.
  • the pores which are larger than about I ⁇ m, are closed.
  • this method step can also be carried out several times. For this purpose, it is advantageous to dry powder z. B. fill in layers in the provided form.
  • the mold is removed according to method step f).
  • the component remains either locally or if applicable, for its use elsewhere entnom ⁇ men.
  • the solution during or after process step a) or the powder according to process step d) with blended and homogenized with various additives and / or additives are on the one hand minerals such as calcite, wollastontite or corundum and fiber materials. This possible addition of fillers serves to optimize the mechanical properties or, in the case of heat-insulating materials, to influence the insulating properties of the component. On the other hand, it is also possible to use organic and inorganic additives which change the surface charge of the phases involved, in particular of the CSH phases.
  • a particularly suitable additive is aluminum hydroxide Al (OH) 3 , which can be added in excess and leads to the self-assembly of CSH phases with negative zeta potential and Al (OH) 3 (positive zeta potential).
  • Further suitable additives are sulfur-containing compounds such as CaSO 4 modifications (gypsum) or ettringite, and hydroxides such as brucite or portlandite.
  • the binder produced by the process according to the invention from C-S-H phases or C-S-H phases with additives includes the additives firmly.
  • the bond between binder and aggregates can be adjusted by adjusting the surface charge of the aggregates, e.g. by prior chemical treatment e.g. improve with acid. This process step can be supplemented by a temperature application.
  • the shaping is done simply by applying an external pressure.
  • the components made with it are immediately fixed and allow immediate stripping.
  • the density of the material according to the invention can be adjusted by selecting the substances according to process step a), the drying conditions according to process step d) and the amount of pressure applied to the powder during process step e).
  • the splitting tensile strength of the product produced by the process according to the invention corresponds already at a density of 1.2 g / cm 3 to the splitting tensile strength of self-compacting concrete which has a density of 2.3 g / cm 3 .
  • composition, conditions of synthesis may be due to requirements for the component such. As to its chemical resistance and need not be determined due to the required reaction conditions. This advantage causes a considerable saving of material.
  • the component shape is determined by its function and the requirements of its strength and not by flow and reaction conditions.
  • the density of the material can also be adjusted by selecting suitable additives and / or additives, so that values between 0.5 and 3.0 g / cm 3 are achieved.
  • the material can also be used as a lightweight construction material.
  • the inventive method is used for the synthesis of nanocrystalline Cementhydratphasen or mixtures of nanocrystalline Zementhydratphasen with tuned surface charge, in particular with a positive zeta potential. Furthermore, this method is used for the preparation and use of fully hydrated CSH phases with a defined composition and surface charge as a raw material for binder production. Finally, this Ver ⁇ will go to the production and use of fully hydratisier ⁇ th, dried cement hydrates used as starting material for bonding a cementitious component. The invention will be explained below with reference to exemplary embodiments.
  • the synthesis was carried out by mecha- the further treatment of an aqueous suspension of CaO and SiO 2 in an agate ball mill.
  • HERGÉ in this way ⁇ introduced substance (slurry) was 4 days at 60 0 C dried.
  • drying may be preceded by a filtration step. All process steps, ie weighing, mixing, loading and Entla ⁇ the mills and drying, carried out under N 2 atmosphere in a so-called. "Glove box" to create controlled environmental conditions and in particular to exclude CO 2 .
  • SiO 2 / Al 2 O 3 and water / solid change Likewise, other additives such. As Mg (OH) 2 or CaSO 4 are added.
  • phase composition of the samples was characterized by the consistency of the powder material, by X-ray diffraction to determine the qualitative and quantitative composition of the samples, and by thermogravimetry to determine the water content of the samples. Production of the component
  • components (specimens) in the form of tablets with a diameter of about 1.3 cm were subsequently produced from the powders.
  • masses of 300 to 500 mg were weighed.
  • the powder was applied in each case in a vacuum pressing tool with a force of 20 kN (values between 10 kN and 120 kN are possible), which corresponds to a pressure of about 140 MPa for said diameter.
  • Table 3 shows the data of series of pressed tablets of pure CSH phases with different CaO / SiO 2 ratio or after additional addition of Al (OH) 3 , which significantly increases the strength:
  • the splitting tensile strength was measured by means of the so-called Brazilian Disk TestSr, ie on a disk. If the material is exceeded As a result, failure is caused by cracking.

Landscapes

  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Ceramic Engineering (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Inorganic Chemistry (AREA)
  • Materials Engineering (AREA)
  • Structural Engineering (AREA)
  • Organic Chemistry (AREA)
  • Curing Cements, Concrete, And Artificial Stone (AREA)
  • Silicates, Zeolites, And Molecular Sieves (AREA)

Abstract

L'invention concerne un procédé de fabrication de composants à base d'hydrates de silicate de calcium (phases CSH), lequel procédé consiste a) à produire une suspension aqueuse de matières solides qui contiennent de l'oxyde de calcium CaO et du dioxyde de silicium SiO<SUB>2</SUB>, une valeur de 0,5:1,0 à 2,5:1,0 étant sélectionnée pour le rapport molaire Ca:Si, b) à moudre la suspension aqueuse sans augmentation de température au-delà de 100 °C, de sorte que des phases CSH nanocristallines se forment, c) à séparer la phase aqueuse, d) à retirer et sécher le résidu contenant des phases CSH nanocristallines jusqu'à l'obtention d'un produit pulvérulent, e) à verser la poudre séchée dans un moule puis à appliquer une pression, de sorte que la poudre se comprime pour former le composant, et f) à retirer le moule. Le procédé selon l'invention permet la synthèse de phases d'hydrates de ciment nanocristallines à charge superficielle ajustée, la production de phases CSH complètement hydratées à composition et charge superficielle définies comme substance de base pour produire des liants et la production d'hydrates de ciment séchés, complètement hydratés, comme substance de départ pour lier un composant lié au ciment.
EP06723679A 2005-04-21 2006-03-24 Procede de fabrication de composants Withdrawn EP1871725A1 (fr)

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
DE200510018423 DE102005018423A1 (de) 2005-04-21 2005-04-21 Verfahren zur Herstellung von Bauteilen
PCT/EP2006/002696 WO2006111241A1 (fr) 2005-04-21 2006-03-24 Procede de fabrication de composants

Publications (1)

Publication Number Publication Date
EP1871725A1 true EP1871725A1 (fr) 2008-01-02

Family

ID=36706932

Family Applications (1)

Application Number Title Priority Date Filing Date
EP06723679A Withdrawn EP1871725A1 (fr) 2005-04-21 2006-03-24 Procede de fabrication de composants

Country Status (5)

Country Link
US (1) US7807078B2 (fr)
EP (1) EP1871725A1 (fr)
JP (1) JP5065245B2 (fr)
DE (1) DE102005018423A1 (fr)
WO (1) WO2006111241A1 (fr)

Families Citing this family (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
DE102007035257B3 (de) * 2007-07-27 2008-11-13 Forschungszentrum Karlsruhe Gmbh Einphasiges hydraulisches Bindemittel, Verfahren zu seiner Herstellung und mit diesem Bindemittel hergestellter Baustoff
JP4902008B1 (ja) * 2011-07-25 2012-03-21 関西保温工業株式会社 無機質バインダー及びこれを用いて製造される成形体
BR112017015445A2 (pt) 2015-01-19 2018-01-16 Cimpor Cimentos De Portugal Sgps S A ligante hidráulico com base em belite dendrítica e métodos para a sua produção
DK3247684T3 (da) 2015-01-19 2021-05-31 Cimpor Portugal Sgps Sa Fremgangsmåder til fremstilling af amorfe hydrauliske silikatbindemidler med lavt calciumindhold
CN113651337A (zh) * 2021-09-27 2021-11-16 浙江加州国际纳米技术研究院台州分院 一种插层改性c-s-h凝胶纳米分散液的制备方法
CN117831871B (zh) * 2024-03-05 2024-05-28 山东恒嘉高纯铝业科技股份有限公司 一种采用ca6、ca2基压敏电阻的压力报警电容器

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Also Published As

Publication number Publication date
DE102005018423A1 (de) 2006-10-26
JP2008536789A (ja) 2008-09-11
US20080093774A1 (en) 2008-04-24
JP5065245B2 (ja) 2012-10-31
WO2006111241A1 (fr) 2006-10-26
US7807078B2 (en) 2010-10-05

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