• 专利附录
  • 专利说明
  • 权利要求
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    • 专利摘要:
    INORGANIC BINDING SYSTEM FOR THE PRODUCTION OF CHEMICAL RESISTANT CHEMISTRY PRODUCTS. The present invention relates to a new binder system comprising at least one latent hydraulic binder, at least one amorphous silica, optionally at least one reactive charge and at least one alkali metal silicate. It has surprisingly been found that the binder system according with the invention it hardens in the form of a hybrid matrix, which is acid resistant, water resistant and alkali resistant. The binder system can be used for the production of a mortar that grips hydraulically, which, after the grouting, hardens for seven days and the subsequent storage for three days in acid, base and / or water, has resistance to compression of more than 15 N mm-2, preferably more than 20 N mm-2 and, in particular, more than 25 N mm-2, according to DIN EN 13888.
    公开号:BR112012012648B1
    申请号:R112012012648-2
    申请日:2010-09-13
    公开日:2020-12-29
    发明作者:Florian Ellenrieder；Uwe Gehrig；Mathias Degenkolb；Joachim Riedmiller
    申请人:Construction Research & Technology Gmbh；
    IPC主号:
    专利说明:

    [0001] The present invention relates to a new inorganic bonding system, the use of this bonding system for the production of a mortar that grips hydraulically and a mortar that contains this bonding system.
    [0002] Portland cement was first mentioned in British patent BP 5022 and has since been further developed further. Modern Portland cement contains about 70% by weight of Cao + MgO, about 20% by weight of SiO2 and about 10% by weight of Al2O3 + Fe2O3. Due to this high CaO content, it hardens hydraulically. The hardened Portland cement is resistant to alkali, but it is not resistant to acid.
    [0003] As latent hydraulic binders, certain slags from metallurgical processes can be activated with strong alkalis, such as, for example, soluble glasses, or can be used as mixtures in Portland cement. By mixing with fillers (quartz sand or aggregate having a corresponding grain size) and additives, they can be used as mortar or concrete. Blast furnace slag, a typical latent hydraulic binder, has, in general, 30 to 45% by weight of CaO, about 4 to 17% by weight of MgO, about 30 to 45% by weight of SiO2 and about from 5 to 15% by weight of Al2O3, typically about 40% by weight of CaO, about 10% by weight of MgO, about 35% by weight of SiO2 and about 12% by weight of Al2O3. Hardened products generally have the properties of hydraulically hardened systems.
    [0004] Inorganic binder systems based on reactive water-insoluble oxides based on SiO2 in combination with Al2O3, which harden in an aqueous alkaline medium, are generally known. Such binder systems are also referred to as geopolymers and are described, for example, in US 4,349,386, WO 85/03699 and US 4,472,199. Such systems generally have 50 to 60% by weight of SiO2, 20 to 25% by weight of Al2O3, no CaO and 15 to 30% by weight of M2O (M = Na, K).
    [0005] Metakaolin, slag, ash dust, activated clay or their mixtures can be used as a mixture of reactive oxides. The alkaline medium for activating the binder usually consists of aqueous solutions of alkali metal carbonates, alkali metal fluorides, alkali metal hydroxides and / or soluble glass. Hardened binders have high mechanical stability. Compared to cement, they can be more economical and more resistant and can have a more advantageous CO2 emission balance. Such systems are, in general, more likely to be resistant to acids and less likely to be resistant to alkalis.
    [0006] WO 08/012438 describes an additional geopolymer cement based on ash dust with low CaO class F content, blast furnace slag and aqueous alkali metal silicate having a SiO2: M2O ratio of more than 1 , 28, preferably more than 1.45. In the examples calculated from anhydrous oxides, about 45 to 50% by weight of SiO2, about 20 to 26% by weight of AI2O3, about 9 to 10% by weight of CaO and about 3 to 4% by weight of K2O are present.
    [0007] The inventors have set themselves the objective of substantially avoiding at least some of the disadvantages of the prior art discussed above. In particular, it was the aim of the invention to provide an inorganic binder system that, in the hardened state, had high mechanical strength and was water resistant, acid resistant and alkali resistant. In particular, the hardened system would have these properties even at a relatively early stage, in particular after only 7 days, and would harden even at room temperature, preferably as low as 10 ° C.
    [0008] EP 1236702 describes a mixture of construction material containing soluble glass for the production of chemical-resistant mortars and based on a latent hydraulic binder, soluble glass and a metal salt as a control agent. The crushed slag can also be used as a latent hydraulic component. Alkali metal salts, in particular lithium salts, are mentioned and used as the metal salt.
    [0009] EP 1081114 describes a mixture of construction material for the production of chemical-resistant mortars, a mixture of construction material containing soluble glass powder and at least one soluble glass hardener. In addition, more than 10% by weight of at least one latent hydraulic binder is present, and the construction material mixture has at least one inorganic filler.
    [0010] EP 0457516 describes acid-resistant, waterproof, fireproof binders, comprising alkali metal silicates, metal oxides and metal carbonates and, optionally, inter alia, microsilica. In these systems, metal oxides are used as handle accelerators.
    [0011] The objective mentioned above is achieved by the characteristics of the independent claims. Dependent claims refer to preferred embodiments.
    [0012] It has surprisingly been found that the inorganic binder system according to the invention hardens in the form of a hybrid matrix, which is acid resistant, water resistant and alkali resistant.
    [0013] The present invention provides an inorganic binder system comprising at least one latent hydraulic binder, at least one amorphous silica, optionally at least one reactive charge and at least one alkali metal silicate.
    [0014] The inorganic binder system of the invention preferably comprises 10 to 30 parts by weight of latent hydraulic binder, 5 to 22 parts by weight of amorphous silica, 0 to 15 parts by weight of reactive load and 3 to 20 parts by weight of silicate of alkali metal.
    [0015] More preferably, it comprises 10 to 30 parts by weight of latent hydraulic binder, 5 to 20 parts by weight of amorphous silica, 0 to 15 parts by weight of reactive charge and 3 to 20 parts by weight of alkali metal silicate .
    [0016] Particularly and preferably, it comprises 15 to 25 parts by weight of the latent hydraulic binder, 5 to 17 parts by weight of amorphous silica, 0 to 10 parts by weight of the reactive load and 4 to 15 parts by weight of metal silicate alkali.
    [0017] In the context of the present invention, a latent hydraulic binder is preferably to be understood as meaning a binder in which the molar ratio of (CaO + MgO): SiO2 is between 0.8 and 2.5 and, particularly and preferably, between 1.0 and 2.0. In particular, the latent hydraulic binder is selected from blast furnace slag, crushed slag, ground slag, electrothermal phosphor slag and steel slag.
    [0018] Blast furnace slag is a residual product of the blast furnace process. The crushed slag is granulated blast furnace slag and the ground slag is finely pulverized blast furnace slag. The ground slag varies in its fineness of grinding and particle size distribution according to the origin and form of preparation, the fineness of grinding having an influence on the reactivity. The so-called Blaine value, which is typically in the order of magnitude 200 to 1000, preferably between 300 and 500 m2kg-1, is used as a characteristic for grinding fineness. A typical blast furnace slag composition was mentioned above.
    [0019] An electrothermal phosphor slag is a waste product of electrothermal phosphorus production. It is less reactive than blast furnace slag and contains about 45 to 50% by weight of CaO, about 0.5 to 3% by weight of MgO, about 38 to 43% by weight of SiO2, about from 2 to 5% by weight of AI2O3 and about 0.2 to 3% by weight of Fe2O3, as well as fluoride and phosphate. Steel slag is a residual product of several steel production processes with a highly varied composition (compare with Caijun Shi, Pavel V. Krivenko, Della Roy, Alkali-Activated Cements and Concretes, Taylor and Francis, London and New York, 2006 , pages 42-51).
    [0020] Amorphous silica is preferably an X-ray amorphous silica, i.e., a silica that shows no crystallinity in the powder diffraction method. In particular, it is selected from precipitated silica, pyrogenic silica and microsilica, as well as glass powder, which is also to be considered as amorphous silica in the context of the present invention.
    [0021] The amorphous silica according to the invention suitably has a content of at least 80% by weight, preferably at least 90% by weight, of SiO2. Precipitated silica is obtained industrially through precipitation processes that start from soluble glass. Precipitated silica is also referred to as silica gel, depending on the production process. Pyrogenic silica is produced by reacting chlorosilanes, such as, for example, silicon tetrachloride, in an oxy-hydrogen flame. Pyrogenic silica is an amorphous SiO2 powder having a particle diameter of 5 to 50 nm and a specific surface area of 50 to 600 m2g-1.
    [0022] Microsilica (also referred to as active silica) is a by-product of the production of silicon or ferrosilicon and also mostly comprises amorphous SiO2 powder. The particles have diameters of the order of magnitude of 0.1 μm. The specific surface area is in the order of magnitude of 20 to 25 m2g-1 (compare with Caijun Shi, Pavel V. Krivenko, Della Roy, Alkali-Activated Cements and Concretes, Taylor and Francis, London and New York, 2006, pages 60-61). In contrast, commercially available quartz sand is crystalline, has comparatively large particles and a comparatively small specific surface area. It serves, according to the invention, merely as an inert aggregate.
    [0023] The reactive load is an optional component. It is suitably a substance having pozzolanic activity. The test for pozzolanic activity can be carried out according to DIN EN 196 part 5. An overview of suitable pozzolans according to the invention is to be found in Caijun Shi, Pavel V. Krivenko, Della Roy, Alkali-Activated Cements and Concretes, Taylor and Francis, London and New York, 2006, pages 51-60, and pages 61-63. Preferably, the reactive charge is selected from lignite ash dust, coal ash dust, metakaolin, volcanic ash, tuff, "trass", pozzolan and zeolites. Metakaolin and ash dust from Classes C (lignite ash dust) and F (coal ash dust) are particularly preferred.
    [0024] Metakaolin is formed in the dehydration of kaolin. White kaolin releases water physically bound at 100 to 200 ° C, dehydroxylation occurs at 500 to 800 ° C with a collapse of the reticular structure and formation of metakaolin (Al2Si2O7). The pure metakaolin therefore contains about 54% by weight of SiO2 and about 46% by weight of Al2O3. Ash dust is formed, inter alia, in the combustion of coal in power plants. According to WO 08/012438, class C ash dust contains about 10% by weight of CaO, while class F ash dust contains less than 8% by weight, preferably less than 4% by weight. weight and typically about 2 wt% CaO. The teaching of WO 08/012438 is hereby incorporated by reference in this proportion.
    [0025] When establishing an adequate hybrid matrix, in particular, the choice of raw materials and their weight proportions are of importance. With an appropriate choice, the inorganic binder system according to the invention has, in general, the following oxide composition, calculated according to the solids: 30 to 70% by weight of SiO2, 2 to 30% by weight of AI2O3, 5 to 30% by weight of CaO, and 5 to 30% by weight of M2O, preferably: 30 to 65%, particularly and preferably 45 to 60%, by weight of SiO2, 5 to 30%, particularly and preferably 5 to 15 % by weight of Al2O3, 5 to 30%, particularly and preferably 12 to 28%, by weight of CaO, and 5 to 30%, particularly and preferably 5 to 20%, by weight of M2O.
    [0026] The best results are obtained with 12 to 25% by weight of CaO.
    [0027] The amount of water required for the handle is suitably 10 to 50 parts by weight, preferably 20 to 40 parts by weight, based on the total weight of the inorganic (anhydrous) binder system. The amount of water required for the handle is, therefore, not counted as a constituent of the inorganic binding system.
    [0028] Alkali metal silicate is selected from compounds having the empirical formula m SiO2. n M2O, where M represents Li, Na, K or NH4, or a mixture of them, preferably Na or K.
    [0029] The molar ratio of m: n is suitably not more than 3.6, preferably not more than 3.0, and, in particular, not more than 2.0. Even more preferably, it is not more than 1.70 and, in particular, not more than 1.20.
    [0030] The alkali metal silicate is preferably a soluble glass, particularly and preferably a liquid soluble glass and, in particular, a sodium or potassium soluble glass. However, lithium or ammonium soluble glasses and mixtures of said soluble glasses can also be used. In the case of liquid soluble glasses, the parts by weight mentioned above are calculated according to the solids content of these soluble glasses, which, in general, are 20% by weight to 60% by weight, preferably 30 to 50% by weight, of solids.
    [0031] The aforementioned m: n ratios (also referred to as a module) should preferably not be exceeded, since otherwise the full activation of the components may no longer be expected. Considerably smaller modules can also be used, such as, for example, about 0.2. Soluble glasses having larger modules must be adjusted, before use, with a suitable aqueous alkali metal hydroxide. Soluble potassium glasses are commercially available mainly as aqueous solutions in the appropriate range of modules, since they are highly hygroscopic; soluble sodium glasses are also commercially available as solids in the appropriate range of modules.
    [0032] If the alkali metal silicate or soluble glass is solid, the inorganic binder system can conveniently be formulated as a one-component system, which can then be caused to harden by adding water. In this case, the latent hydraulic binder, amorphous silica, optional reactive charge and alkali metal silicate are present together as a component.
    [0033] However, soluble glass can also be used in the form of an aqueous solution. In this case, the inorganic binder system is conveniently formulated as a two-component system, where normally the latent hydraulic binder, amorphous silica and the optional reactive charge are present as a first component, and the soluble glass solution, which contains at least minus the amount of water required for the handle, is present as a second component. At least in the case of soluble potassium glass, this embodiment is preferred.
    [0034] Inert fillers and / or additional additives can additionally be present in the inorganic binder system according to the invention. These optional components can alternatively also be added only when preparing a mortar or concrete.
    [0035] Preferably, between 0 and 80% by weight, particularly and preferably between 30 and 70% by weight, of inert fillers and / or between 0 and 15% by weight of additives may be present or may be added during preparation mortar or concrete. These data by weight are based on the total weight of the solids of the inorganic (anhydrous) binder system. Inert fillers and / or additional additives are therefore not counted as constituents of the inorganic binder system.
    [0036] Gravels, sands and / or powders generally known, for example, based on quartz, limestone, barite or clay, in particular quartz sand, are suitable as inert fillers. Light fillers, such as perlite, diatomite (diatomaceous earth), exfoliated mica (vermiculite) and foamed sand, can also be used.
    [0037] Suitable additives are, for example, draining agents, defoamers, water retention agents, plasticizers, pigments, fibers, dispersion powders, wetting agents, retarders, accelerators, complexing agents, aqueous dispersions and rheology modifiers generally known.
    [0038] Cement may also be present or may be added during the preparation of mortar or concrete as an additional (hydraulic) additive. A proportion of not more than 20%, preferably not more than 10%, by weight of cement is preferred, based on the total weight of the solids of the inorganic (anhydrous) binder system. This cement may preferably be Portland cement and / or cement with a high alumina content.
    [0039] The present invention additionally provides for the use of the inorganic binder system of the invention as, or as a constituent of, formulations of construction materials and / or construction products, such as concrete, finished concrete parts, concrete products, blocks concrete and also concrete on site, spray concrete, premixed concrete, construction glues and glues from composite thermal insulation systems, concrete restoration systems, one-component and two-component sealant pastes, applied concrete strips on the wall, cutting loads and self-leveling compositions, tile adhesives, plasters and first plastering hands, adhesives and sealants, coating systems, in particular for tunnels, wastewater channels, spray protection and condensate lines, dry mortars , thin joint mortars, drainage mortars and / or restoration mortars.
    [0040] For this purpose, the inorganic binder system of the invention is often mixed with additional components, such as fillers, hydraulic substances and additives. The addition of the alkali metal silicate in powder form is preferably carried out before said components are mixed with water. Alternatively, an aqueous alkali metal silicate solution can be added to the other powder components.
    [0041] The present invention additionally provides a mortar, in particular a dry mortar or thin joint mortar, which contains the inorganic binder system of the invention.
    [0042] After setting, hardening for seven days and subsequent storage for three days in acid, base and / or water, this mortar has compressive strengths of more than 15 N mm-2, preferably more than 20 N mm-2 and, in particular, more than 25 N mm-2, as determined according to DIN EN 13888.
    [0043] The present invention is now illustrated in more detail with reference to the following examples: Examples Raw materials: - Metakaolin comprising about 56% by weight of SiO2, 41% by weight of Al2O3 and, in each case, < 1% by weight of CaO and alkali metal oxide; BET surface area> 10,000 m2kg-1; - Microsilica comprising> 90% by weight of SiO2 and, in each case, <1% by weight of Al2O3, CaO and alkali metal oxide; BET surface area> 15,000 m2kg-1; - Ground blast furnace slag comprising 34 wt% SiO2, 12 wt% Al2O3, 43 wt% CaO and <1 wt% alkali metal oxide; Blaine value> 380 m2kg-1; - Soluble aqueous potassium glass having a SiO2: K2O molar ratio of 1.5 or 1.0 and solids contents of 50% by weight or 40% by weight, respectively; - Quartz sand commercially available. Comparative Examples M1, M2 and M3, and Working Examples M4 and M5:
    [0044] Suitably, initially all powdered substances are homogenized and then mixed with the liquid component. All examples are two-component systems, since water-soluble potassium glass is added separately in each case. Cylindrical test samples are produced having a diameter of 25 ± 1 mm and a height of 25 ± 1 mm. The test samples are tested for chemical resistance according to DIN EN 13888, ie, after preliminary storage for 7 days, under standard climatic conditions, the test samples are stored in a test medium. For the classification of mixtures, the compressive strength is determined both before and after storage. The experimental formulations are shown in Table 1 in parts by weight. The oxide compositions of the anhydrous binder systems are shown in Table 2 in% by weight. Table 3 shows the compressive strengths of the test samples before and after storage in the test media; standard climatic conditions are understood to mean 23 ° C and 50% relative humidity.

    [0045] Table 3 shows that, after a short hardening time of seven days, under standard climatic conditions, minimum compressive strengths of 15 N mm-2 required according to DIN EN 13888 are achieved by M2 to M5. Whereas, however, reference systems M1 to M3, after treatment with acid, water and / or alkali, have low compressive strength, very high compressive strengths can be determined in the case of M4 and M5 systems according to the invention, even after storage in the various test media. The systems according to the invention are therefore resistant to acids, water and alkalis.
    权利要求:
    Claims (12)
    [0001]
    1. Inorganic binder system characterized by the fact that it comprises 10 to 30 parts by weight of at least one latent hydraulic binder, selected from blast furnace slag, crushed slag, ground slag, electrothermal phosphor slag and steel slag, 5 to 22 parts by weight of at least one amorphous silica, selected from precipitated silica, pyrogenic silica, microsilica and glass powder, 0 to 15 parts by weight of at least one reactive charge, selected from lignite ash dust, ash dust from coal, metakaolin, volcanic ash, tuff, "trass", pozzolan and zeolites 3 to 20 parts by weight of at least one alkali metal silicate, selected from compounds having the empirical formula m SiO2. n M2O, where M represents Li, Na, K or NH4, or a mixture of them, where the molar ratio of m: n is <3.6, where the binder system comprises 12 to 25% by weight of CaO, where 10 to 50 parts by weight of water are required for the handle, and where the latent hydraulic binder, amorphous silica and optional reactive charge are present as a first component and the alkali metal silicate together with at least a quantity of water required for pleating are present as a second component under the condition that it contains no metal salt selected from metal hydroxide, metal oxide, metal salt containing carbon, metal salt containing sulfur, metal salt containing nitrogen , metal salt containing phosphorus, and metal salt containing halogen, as a control agent.
    [0002]
    2. Binder system according to claim 1, characterized by the fact that the m: n molar ratio is <3.0.
    [0003]
    3. Binder system according to claim 1, characterized by the fact that the m: n molar ratio is <2.0.
    [0004]
    Binder system according to claim 1, characterized by the fact that the m: n molar ratio is <1.7.
    [0005]
    Binder system according to claim 1, characterized by the fact that the molar ratio of m: n is <1.2.
    [0006]
    Binder system according to any one of claims 1 to 5, characterized in that 20 to 40 parts by weight of water are required for the handle.
    [0007]
    Binder system according to any one of claims 1 to 6, characterized by the fact that M represents Na or K.
    [0008]
    Binder system according to any one of claims 1 to 7, characterized in that it comprises 15 to 25, parts by weight of latent hydraulic binder, 5 to 17, parts by weight of amorphous silica, 0 to 10, parts in reactive load weight, and 4 to 15 parts by weight of alkali metal silicate.
    [0009]
    Binder system according to any of claims 1 to 8, characterized in that the inert fillers and / or additional additives are additionally present.
    [0010]
    Binder system according to any one of claims 1 to 9, characterized by the fact that ≤ 20%, preferably ≤ 10%, by weight of cement are present.
    [0011]
    11. Use of the binder system as defined in any one of claims 1 to 10 characterized by the fact that it is like, or as a constituent of, formulations of construction materials and / or construction products, such as concrete, finished concrete parts , concrete products, concrete blocks and also concrete on site, spray concrete, premixed concrete, building glues and glues from composite thermal insulation systems, concrete restoration systems, one-component and two-component sealing slurries components, strips of concrete applied to the wall, cutting loads and self-leveling compositions, tile adhesives, plasters and first plastering hands, glues and sealants, coating systems, in particular for tunnels, wastewater channels, spray protection and condensate, mortars, in particular dry mortars or thin joint mortars, drainage mortars and / or restoration mortars.
    [0012]
    12. Use according to claim 11, characterized by the fact that, after gripping, hardening for seven days and subsequent storage for three days in acid, base and / or water, the mortar has compressive strengths of more than than 15 N mm-2, preferably more than 20 N mm-2 and, in particular, more than 25 N mm-2, as determined according to DIN EN 13888.
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    法律状态:
    2020-08-04| B06F| Objections, documents and/or translations needed after an examination request according art. 34 industrial property law|
    2020-08-11| B06U| Preliminary requirement: requests with searches performed by other patent offices: suspension of the patent application procedure|
    2020-11-24| B09A| Decision: intention to grant|
    2020-12-29| B16A| Patent or certificate of addition of invention granted|Free format text: PRAZO DE VALIDADE: 10 (DEZ) ANOS CONTADOS A PARTIR DE 29/12/2020, OBSERVADAS AS CONDICOES LEGAIS. |
    优先权:
    申请号 | 申请日 | 专利标题
    EP09177153|2009-11-26|
    EP09177153.5|2009-11-26|
    PCT/EP2010/063386|WO2011064005A1|2009-11-26|2010-09-13|Inorganic binder system for the production of chemically resistant construction chemistry products|
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