WO2013080456A1 - 不定形組成物 - Google Patents

不定形組成物 Download PDF

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Publication number
WO2013080456A1
WO2013080456A1 PCT/JP2012/007210 JP2012007210W WO2013080456A1 WO 2013080456 A1 WO2013080456 A1 WO 2013080456A1 JP 2012007210 W JP2012007210 W JP 2012007210W WO 2013080456 A1 WO2013080456 A1 WO 2013080456A1
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Prior art keywords
weight
amorphous composition
composition
fiber
amorphous
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PCT/JP2012/007210
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English (en)
French (fr)
Inventor
賢 米内山
浩毅 村松
徹也 三原
智彦 岸木
鉄也 石原
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ニチアス株式会社
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Publication of WO2013080456A1 publication Critical patent/WO2013080456A1/ja

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    • 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
    • C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
    • C04B2235/70—Aspects relating to sintered or melt-casted ceramic products
    • C04B2235/96—Properties of ceramic products, e.g. mechanical properties such as strength, toughness, wear resistance
    • C04B2235/9607—Thermal properties, e.g. thermal expansion coefficient
    • C04B2235/9615—Linear firing shrinkage

Definitions

  • the present invention relates to, for example, a heat-resistant inorganic fiber-containing hardboard processed product, an amorphous composition used as a material for a repair or adhesive of a molded product, and more specifically, a specific biosoluble inorganic fiber is used.
  • the present invention relates to an amorphous composition.
  • amorphous compositions have contained inorganic fibers such as glass fibers, glass wool, ceramic wool, rock wool, alumina fibers, zirconia fibers, silica / alumina fibers as reinforcing fibers.
  • the amorphous composition is usually in the form of a paste, and is inserted into a gap of a tile or the like by, for example, glazing, spraying or pouring to form a joint.
  • the inorganic fibers contained in the amorphous composition become dust and are scattered in the air, and the operator inhales the dust. Since inorganic fibers are in danger of health damage if they are inhaled by humans and enter the lungs, at present, amorphous compositions using biosoluble fibers as inorganic fibers have been developed (for example, Patent Documents 1 to 5). .
  • the amorphous composition is usually stored after production. As described above, after being applied or embedded in repair of a molded product (target molded product) used in a furnace or the like, it is dried. It is then exposed to high temperatures in a furnace. Therefore, different practical performances are required at the time of storage, at the time of construction with equipment, at the time of drying after construction, and further at the time of heating of equipment. Specifically, it has long-term stability during storage, it has an appropriate consistency (viscosity) during construction and excellent paintability, and it adheres to the target molded product during construction and drying. It is excellent in the moldability in which the property and the arranged shape are maintained. At the time of heating, the function as a heat-resistant material and the adhesiveness are maintained, and the performance of the target molded product is not adversely affected.
  • the present inventors have developed a novel biosoluble fiber excellent in fire resistance and biosolubility (Japanese Patent Application No. 2011-59354).
  • One object of the present invention is to provide an amorphous composition having practical properties, including inorganic fibers having excellent fire resistance and biosolubility.
  • an amorphous composition comprising inorganic fibers having the following composition and a chelating agent not containing metal ions.
  • Composition of inorganic fiber SiO 2 66-82% by weight CaO 10-34% by weight MgO 3 wt% or less Al 2 O 3 5 wt% or less The total of SiO 2 , CaO, MgO and Al 2 O 3 is 98 wt% or more.
  • the amorphous composition according to 1, comprising colloidal silica.
  • the amorphous composition according to 2 wherein the colloidal silica has a pH of 8-11. 4). 4.
  • an amorphous composition having practical properties, including inorganic fibers excellent in fire resistance and biosolubility.
  • the amorphous composition of the present invention contains specific inorganic fibers that are excellent in fire resistance and biosolubility as reinforcing fibers.
  • a chelating agent that does not contain metal ions is included to prevent solidification during storage.
  • the composition of the present invention includes inorganic fibers having the following composition. SiO 2 66-82% by weight CaO 10-34% by weight MgO 3 wt% or less Al 2 O 3 5 wt% or less Total of SiO 2 , CaO, MgO, Al 2 O 3 98 wt% or more
  • Biosoluble fibers can be broadly classified into Mg silicate fibers containing a lot of MgO and Ca silicate fibers containing a lot of CaO.
  • Ca silicate fibers are used. Since the biosoluble fiber is easily soluble in water, it is usually dissolved in water contained in the amorphous composition and the contained components are eluted. It may react with other components in the composition, the target molded article to be applied, or the like, causing inconvenience. Accordingly, a composition containing ceramic fibers that are hardly soluble in water may behave differently from a composition containing biosoluble fibers, and among biosoluble fibers, a composition containing Mg silicate fibers and Ca silicate fibers. Since the composition and the amount of the eluted component are different, the composition containing may sometimes show different behavior.
  • Mg silicate fiber When using Mg silicate fiber for the amorphous composition, organic fiber is added as a binder in order to ensure necessary strength, but addition of organic fiber is not necessary for Ca silicate fiber. Moreover, when using Mg silicate fiber, addition of a pH adjuster is required. If a pH adjuster is not added, there is a risk of solidifying during storage, resulting in increased drying shrinkage. However, in the case of Ca silicate fiber, the same addition as that of Mg silicate fiber may or may not be added.
  • the following composition can be illustrated as Ca silicate fiber. Fibers having the following composition are excellent in biosolubility and fire resistance after heating. If such a fiber is used in an amorphous composition that does not contain a specific chelating agent, the amorphous composition will solidify after long-term storage even if it can be used immediately after production. Although the adhesion to the molded article is weakened and peeled off and is difficult to repair, an amorphous composition containing a specific chelating agent as in the present invention is difficult to peel off and is easy to repair.
  • SiO 2 66-82 wt% (for example, it can be 68-80 wt%, 70-80 wt%, 71-80 wt% or 71-76 wt%)
  • CaO 10-34% by weight (for example, it can be 20-30% by weight or 21-26% by weight)
  • MgO 3 wt% or less eg, 1 wt% or less
  • Al 2 O 3 5% by weight or less eg, 3.5% by weight or less or 3% by weight or less.
  • Other oxides ⁇ 2% by weight
  • the Al 2 O 3 content can be, for example, 3.4% by weight or less or 3.0% by weight or less. Moreover, it can be 1.1 weight% or more or 2.0 weight% or more. The content is preferably 0 to 3% by weight, more preferably 1 to 3% by weight. If Al 2 O 3 is contained within this range, the strength becomes high.
  • the above inorganic fibers include other oxides such as alkali metal oxides (K 2 O, Na 2 O, etc.), Fe 2 O 3 , ZrO 2 , P 2 O 5 , B 2 O 3 , TiO 2 , MnO, R 2 O 3 (R is selected from Sc, La, Ce, Pr, Nd, Sm, Eu, Gd, Tb, Dy, Ho, Er, Tm, Yb, Lu, Y, or a mixture thereof) The above may or may not be included. Other oxides may be 0.2 wt% or less or 0.1 wt% or less, respectively.
  • the alkali metal oxide may contain 0.2% by weight or less of each oxide, and the total of the alkali metal oxides may be 0.2% by weight or less.
  • the total of SiO 2 , CaO, MgO and Al 2 O 3 may be more than 98 wt% or more than 99 wt%.
  • the biologically soluble inorganic fiber is, for example, an inorganic fiber having a physiological saline dissolution rate at 40 ° C. of 1% or more.
  • the physiological saline dissolution rate is measured, for example, as follows. That is, first, 1 g of a sample prepared by pulverizing inorganic fibers to 200 mesh or less and 150 mL of physiological saline are placed in an Erlenmeyer flask (volume: 300 mL) and placed in an incubator at 40 ° C. Next, a horizontal vibration of 120 revolutions per minute is continuously applied to the Erlenmeyer flask for 50 hours.
  • the concentration (mg / L) of each element contained in the filtrate obtained by filtration is measured with an ICP emission analyzer. Then, based on the measured concentration of each element and the content (% by weight) of each element in the inorganic fiber before dissolution, the physiological saline dissolution rate (%) is calculated. That is, for example, when the measurement element is silicon (Si), magnesium (Mg), calcium (Ca), and aluminum (Al), the physiological saline dissolution rate C (%) is calculated by the following equation.
  • C (%) [filtrate amount (L) ⁇ (a1 + a2 + a3 + a4) ⁇ 100] / [weight of inorganic fiber before dissolution (mg) ⁇ (b1 + b2 + b3 + b4) / 100].
  • a1, a2, a3 and a4 are the measured concentrations of silicon, magnesium, calcium and aluminum (mg / L), respectively, and b1, b2, b3 and b4 are respectively in the inorganic fibers before dissolution. It is content (weight%) of silicon, magnesium, calcium, and aluminum.
  • the inorganic fiber has an average fiber diameter of usually 1 to 50 ⁇ m, preferably 2 to 10 ⁇ m, particularly preferably 2 to 5 ⁇ m, and an average fiber length of usually 1 to 200 mm, preferably 2 to 50 mm.
  • the surface of the inorganic fiber may or may not be covered with a coating layer.
  • the coating layer is hardly soluble in water and easily soluble in physiological saline as described above.
  • Examples of substances that form a coating layer on the surface of inorganic fibers include phosphates, molybdenum compounds, polyamidine compounds, and ethyleneimine compounds.
  • Examples of the phosphate include aluminum tripolyphosphate, aluminum dihydrogen tripolyphosphate, aluminum metaphosphate, zinc phosphate, and calcium phosphate.
  • Examples of the molybdenum compound include zinc molybdate, aluminum molybdate, calcium molybdate, calcium phosphomolybdate, and aluminum phosphomolybdate.
  • Examples of the polyamidine compound include acrylamide, acrylonitrile, N-vinylacrylamidine hydrochloride, N-vinylacrylamide, vinylamine hydrochloride, N-vinylformamide copolymer and the like.
  • Examples of ethyleneimine compounds include aminoethylene and dimethyleneimine.
  • the inorganic fiber is preferably contained in the amorphous composition in an amount of 10 to 60% by weight, preferably 10 to 50% by weight, more preferably 10 to 30% by weight, and further preferably 15 to 30% by weight. If it exceeds 60% by weight, the amount of the inorganic binder is lowered, so that the adhesive force may be lowered. If it is less than 10% by weight, moldability may be reduced.
  • Colloidal silica can be included as an inorganic binder.
  • the pH of colloidal silica is preferably 8 or more, more preferably 9-11. Depending on the type of thickener selected to be less than 8, there is a risk that the paste will not have a moderate viscosity.
  • the colloidal silica is preferably contained in an amount of 1 to 60% by weight, more preferably 6 to 42.5% by weight, and still more preferably 8 to 42.5% by weight. More preferably, it is 10 to 42.5% by weight, more preferably 15 to 40% by weight, and still more preferably 20 to 30% by weight. If it exceeds 42.5% by weight, the reinforcing effect of the fiber may be reduced, and the drying shrinkage rate may be increased, or the moldability may be reduced. If it is less than 6% by weight, the bond strength and adhesiveness of the fibers may be lowered.
  • a chelating agent that does not contain metal ions such as alkaline earth metals and alkali metals is used.
  • chelating agents include EDTA (Ethylene Diamine Tetraacetic Acid) ⁇ H ⁇ 3 (NH 4 ) chelating agent, EDTA ⁇ 2H ⁇ 2 (NH 4 ) composition, which does not contain metal ions.
  • chelating agents include chelating agents.
  • the adverse effect during storage caused by alkaline earth metal can be prevented by capturing the alkaline earth metal eluted from the inorganic fiber by the chelating agent and simultaneously forming a protective layer. Since the chelating agent has two or more electron donating groups, a metal chelate compound can be produced. Examples of the electron donating group include a carboxy group and a hydroxyl group.
  • the chelating agent is preferably contained in the amorphous composition in an amount of 0.01 to 3.0% by weight, preferably 0.02 to 2.5% by weight, and 0.05 to 1.5% by weight. More preferably, it is more preferably 0.1 to 1.0% by weight. If the amount is too large, the amorphous composition may solidify. If the amount is too small, the amorphous composition may solidify.
  • the composition of the present invention usually contains a solvent.
  • the solvent is not particularly limited, and examples thereof include water and a polar organic solvent.
  • the polar organic solvent include monovalent alcohols such as ethanol and propanol, and divalent alcohols such as ethylene glycol.
  • water is preferable in that there is no deterioration of the working environment and there is no burden on the environment. Moreover, it does not restrict
  • the content of the solvent is preferably 10 to 80% by weight, more preferably 15 to 68% by weight, more preferably 20 to 68% by weight, when the amorphous composition is 100% by weight. More preferably, it is 25 to 68% by weight. If the content is too small, the fluidity is lowered, so that the workability is deteriorated, and the mechanical strength, particularly the bending strength is lowered. Moreover, since the consistency of an amorphous composition will become high when there is too much content, a composition dripped at the time of construction, and the shrinkage
  • a solvent may be added independently as a solvent, and may be added with a material as a solvent contained in a material (for example, colloidal silica). The amount of the solvent is the sum of the amount added independently and the amount contained in the material. The amount of the solvent can be reduced so that the solvent is only the solvent contained in the colloidal silica.
  • composition of the present invention can contain a binder, a thickener, a dispersant, a preservative, a pH adjuster and the like as additives.
  • examples of the inorganic binder include colloidal silica, alumina sol, zirconia sol, titania sol, aluminum phosphate, and the like.
  • examples of the organic binder include organic fiber, acrylic emulsion, starch and the like.
  • Organic fiber acts as a protective film for inorganic fiber.
  • the organic fiber is not particularly limited and may be any of natural fiber or hydrophobic treated synthetic fiber.
  • Examples of the natural fiber include pulp, cotton, hemp and the like.
  • Examples of the synthetic fiber include vinylon and rayon. , Polypropylene, polyethylene and the like. Of these, pulp is preferable in that it easily incorporates inorganic fibers.
  • the average fiber diameter of the organic fibers is usually 1 to 30 ⁇ m, preferably 2 to 10 ⁇ m, particularly preferably 2 to 5 ⁇ m. When the average fiber diameter is less than 1 ⁇ m, the strength of the joint becomes low, and when it exceeds 30 ⁇ m, it is difficult to take in inorganic fibers.
  • the content of the organic fiber is preferably 5 to 50 parts by weight with respect to 100 parts by weight of the inorganic fiber.
  • Hydrophobic treatment refers to treatment for improving the hydrophobicity of the fiber.
  • Examples of the hydrophobic treatment method include a method of coating the periphery of the fiber with a hydrophobic drug.
  • the thickener is not particularly limited, and known ones can be used. Specific examples include hydroxyethyl cellulose, sodium acrylate polymer, polyether polyol, acrylic polymerized polymer polyesteramine, and ethylene oxide. Moreover, a nonionic thickener can be used. The content of the thickener is not particularly limited, but is preferably 0.01 to 10% by weight, more preferably 0.01 to 8% by weight, and still more preferably 0.01 to 5% by weight in the amorphous composition. It is.
  • the dispersant is not particularly limited, and known ones can be used. Specific examples include carboxylic acids, polyhydric alcohols, amines and the like.
  • the content of the dispersant is not particularly limited, but is preferably 0.01 to 3% by weight with respect to 100% by weight of the amorphous composition.
  • the preservative is not particularly limited, and examples thereof include an inorganic compound or an organic compound having a nitrogen atom or a sulfur atom.
  • the content of the preservative is not particularly limited, but is preferably 0.01 to 3% by weight with respect to 100% by weight of the amorphous composition.
  • the composition of the present invention contains a pH adjuster because dissolution of inorganic fibers in the solution can be further suppressed.
  • the pH adjuster include a buffer solution and an acid.
  • the buffer solution include a phthalate standard solution (Selensen buffer solution) that is a pH 4 standard solution, and a neutral phosphate standard solution that is a pH 7 standard solution, and examples of the acid include acetic acid and formic acid.
  • the pH is preferably about 4 to 8.5.
  • the composition of the present invention may or may not contain an inorganic powder. It may be added as a raw material to produce a composition, or may be added after obtaining the composition.
  • an inorganic powder one or more (mixtures) selected from silica, alumina, mullite, zircon, zirconia, kaolin, clay mineral, titania, calcia, and magnesia can be used.
  • the amorphous composition according to the present invention can be produced by mixing and stirring each component.
  • the molded body according to the present invention can be obtained by molding an amorphous composition and drying / heating. Since the composition of the present invention is pasty (stucco), it can be applied with a trowel, hardened by hand, or sprayed with a pressure gun.
  • the amorphous composition of the present invention is difficult to solidify even if stored for a long time. Moreover, it is easy to apply to a target molded article having an appropriate consistency and is deficient, and is excellent in adhesiveness after being applied and dried. In addition, even during heating, it is difficult to adversely affect the performance of the target molded product.
  • Example 1 Manufacture of amorphous composition
  • Inorganic fiber A 23.9% by weight containing 73% by weight of SiO 2 , 24% by weight of CaO, 0.3% by weight of MgO and 2 % by weight of Al 2 O 3
  • Colloidal silica Snowtex 30, manufactured by Nissan Chemical Industries, pH 9-11, suspension having a solid content of 30%) 75.8 wt% (22.7 wt% (solid content), 53.1 wt% (solvent) amount)
  • EDTA ⁇ H ⁇ 3 (NH 4 ) chelating agent not containing metal ions
  • Thickener (himetroise, manufactured by Shin-Etsu Chemical Co., Ltd.) 0.8% by weight
  • weight% is the quantity when the whole composition is 100 weight%.
  • the ceramic fiber is a fiber containing 40 to 60% by weight of silica and 60 to 40% by weight of alumina.
  • NTA is NTA (Nitrilo Triacetic Acid) ⁇ 3Na ⁇ H 2 O
  • NTB is NTA ⁇ H ⁇ 2Na.
  • the composition containing ceramic fibers can be used without containing a chelating agent that does not contain metal ions, but the composition containing inorganic fibers A does not contain metal ions. It can be seen that it cannot be used unless it contains a chelating agent. Further, it can be seen from Comparative Examples 2, 3 and 4 that the effect of the present invention cannot be achieved with a chelating agent or citric acid containing a metal ion.
  • the amorphous composition of the present invention can be used as an inorganic fiber-containing hardboard processed product or a molded product repair agent or adhesive material.

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Ceramic Engineering (AREA)
  • Manufacturing & Machinery (AREA)
  • Materials Engineering (AREA)
  • Structural Engineering (AREA)
  • Organic Chemistry (AREA)
  • Inorganic Chemistry (AREA)
  • Chemical Kinetics & Catalysis (AREA)
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  • Curing Cements, Concrete, And Artificial Stone (AREA)
  • Inorganic Fibers (AREA)

Abstract

ＳｉＯ２６６～８２重量％、ＣａＯ１０～３４重量％、ＭｇＯ３重量％以下、Ａｌ２Ｏ３５重量％以下、ＳｉＯ２、ＣａＯ、ＭｇＯ、Ａｌ２Ｏ３の合計９８重量％以上の組成を有する無機繊維と、金属イオンを含まないキレート剤とを含む不定形組成物。

Description

不定形組成物
　本発明は、例えば、耐熱性無機繊維含有ハードボード加工品、モールド品の補修剤や接着剤の材料と使用される不定形組成物に関し、より具体的には、特定の生体溶解性無機繊維を含む不定形組成物に関する。
　従来、不定形組成物は、ガラス繊維、グラスウール、セラミックウール、ロックウール、アルミナ質繊維、ジルコニア質繊維、シリカ・アルミナ質繊維等の無機繊維を、強化繊維として含有していた。不定形組成物は通常ペースト状であり、例えば、鏝塗り、スプレー塗り又は注入施工等により、タイル等の隙間に挿入され、目地を形成する。その際、不定形組成物に含有されている無機繊維は粉塵となって空気中に飛散し、作業者が該粉塵を吸入することとなる。無機繊維は、人に吸入されて肺に侵入すると健康被害が懸念されるため、現在、無機繊維として生体溶解性繊維を用いる不定形組成物が開発されている（例えば、特許文献１～５）。
特開２００６－３０６７１３号公報 特開２００６－２８２４０４号公報 特開２００５－２８１０７９号公報 特表２００２－５２４３８４号公報 国際公開第２０１１／０８３６９６号パンフレット
　不定形組成物は、通常、製造後保管される。上述したように炉等に使用される成形品（対象成形品）の補修等に塗布されたり埋め込まれた後、乾燥する。その後、炉において高温に晒される。従って、保管時、設備等での施工時、施工後の乾燥時、さらに設備等の加熱時に、それぞれ異なる実用性能が求められる。
　具体的には、保管時は、長期安定性を有することであり、施工時には、ちょう度（粘性）が適切であって塗り性に優れることであり、施工と乾燥時には、対象成形品との接着性や整えた形状が保持される成形性に優れることである。加熱時は、耐熱材としての機能、接着性を維持しつつ、対象成形品の性能に悪影響を示さないことである。
　本発明者らは、耐火性、生体溶解性に優れる新規な生体溶解性繊維を開発した（特願２０１１－５９３５４）。本発明は、このような耐火性、生体溶解性に優れる無機繊維を含む、実用特性を有する不定形組成物を提供することをその目的の一つとする。
　本発明によれば、以下の不定形組成物等が提供される。
１．以下の組成を有する無機繊維と、金属イオンを含まないキレート剤とを含む不定形組成物。
［無機繊維の組成］
　ＳｉＯ２　６６～８２重量％
　ＣａＯ　１０～３４重量％
　ＭｇＯ　３重量％以下
　Ａｌ２Ｏ３　５重量％以下
　ＳｉＯ２、ＣａＯ、ＭｇＯ、Ａｌ２Ｏ３の合計　９８重量％以上
２．コロイダルシリカを含む１記載の不定形組成物。
３．前記コロイダルシリカのｐＨが、８～１１である２記載の不定形組成物。
４．前記キレート剤が、エチレンジアミン四酢酸・Ｈ・３（ＮＨ４）又はエチレンジアミン四酢酸・２Ｈ・２（ＮＨ４）である１～３のいずれか記載の不定形組成物。
５．不定形組成物中、無機繊維を１０～６０重量％、コロイダルシリカを固形分で１～６０重量％、金属イオンを含まないキレート剤を０．０１～３．０重量％含む１～４のいずれか記載の不定形組成物。
６．不定形組成物中、１０～８０重量％の溶媒を含む１～５のいずれか記載の不定形組成物。
７．１～６のいずれか記載の不定形組成物が乾燥した成形物。
　本発明によれば、耐火性、生体溶解性に優れる無機繊維を含む、実用特性を有する不定形組成物を提供することができる。
　本発明の不定形組成物は、強化繊維として耐火性、生体溶解性に優れる特定の無機繊維を含む。さらに、保存中の固化を防ぐために、金属イオンを含まないキレート剤を含む。
　具体的には、本発明の組成物は、以下の組成を有する無機繊維を含む。
　ＳｉＯ２　６６～８２重量％
　ＣａＯ　１０～３４重量％
　ＭｇＯ　３重量％以下
　Ａｌ２Ｏ３　５重量％以下
　ＳｉＯ２、ＣａＯ、ＭｇＯ、Ａｌ２Ｏ３の合計　９８重量％以上
　生体溶解性繊維は、ＭｇＯを多く含むＭｇシリケート繊維と、ＣａＯを多く含むＣａシリケート繊維に大別できるが、本発明では、Ｃａシリケート繊維を用いる。生体溶解性繊維は水に溶けやすいため、通常不定形組成物に含まれる水に溶解し、含有成分が溶出する。それが組成物中の他の成分や、塗布される対象成形品等と反応し不都合をもたらす恐れがある。従って、水に溶けにくいセラミックス繊維を含む組成物は生体溶解性繊維を含む組成物と異なる挙動を示す場合があり、また、生体溶解性繊維の中でも、Ｍｇシリケート繊維を含む組成物とＣａシリケート繊維を含む組成物は溶出する成分の種類や量が異なるため、異なる挙動を示す場合がある。
　不定形組成物に、Ｍｇシリケート繊維を用いるときは、必要な強度を確保するために、バインダーとして有機繊維を添加するが、Ｃａシリケート繊維は有機繊維の添加は必要ではない。また、Ｍｇシリケート繊維を用いるときは、ｐＨ調整剤の添加が必要である。ｐＨ調整剤を添加しないと、保管中に固化する恐れがあり、乾燥収縮が大きくなる。しかし、Ｃａシリケート繊維の場合は、Ｍｇシリケート繊維と同様な添加してもよいし、しなくてもよい。
　Ｃａシリケート繊維として以下の組成を例示できる。以下の組成の繊維は加熱後の生体溶解性、耐火性に優れる。このような繊維を特定のキレート剤を含まない不定形組成物に用いると、製造直後は良好に使用できても、長期保管後には不定形組成物が固化してくるため、施工・乾燥後対象成形品との接着が弱まり剥がれてしまう、また補修しにくいが、本発明のように特定のキレート剤を含む不定形組成物は剥がれ難く、さらには補修しやすい。
　ＳｉＯ２　６６～８２重量％（例えば、６８～８０重量％、７０～８０重量％、７１～８０重量％又は７１～７６重量％とできる）
　ＣａＯ　１０～３４重量％（例えば、２０～３０重量％又は２１～２６重量％とできる）
　ＭｇＯ　３重量％以下（例えば、１重量％以下とできる）
　Ａｌ２Ｏ３　５重量％以下（例えば３．５重量％以下又は３重量％以下とできる。また、１重量％以上又は２重量％以上とできる）
　他の酸化物　２重量％未満
　ＳｉＯ２が上記範囲であると耐熱性に優れる。ＣａＯとＭｇＯが上記範囲であると加熱前後の生体溶解性に優れる。
　Ａｌ２Ｏ３含有量は、例えば、３．４重量％以下又は３．０重量％以下とできる。また、１．１重量％以上又は２．０重量％以上とできる。好ましくは０～３重量％、より好ましくは１～３重量％である。この範囲でＡｌ２Ｏ３を含むと強度が高くなる。
　上記の無機繊維は、他の酸化物として、アルカリ金属酸化物（Ｋ２Ｏ、Ｎａ２Ｏ等）、Ｆｅ２Ｏ３、ＺｒＯ２、Ｐ２Ｏ５、Ｂ２Ｏ３、ＴｉＯ２、ＭｎＯ、Ｒ２Ｏ３（ＲはＳｃ，Ｌａ，Ｃｅ，Ｐｒ，Ｎｄ，Ｓｍ，Ｅｕ，Ｇｄ，Ｔｂ，Ｄｙ，Ｈｏ，Ｅｒ，Ｔｍ，Ｙｂ，Ｌｕ，Ｙ又はこれらの混合物から選択される）等を１以上含んでもよく、含まなくてもよい。他の酸化物は、それぞれ、０．２重量％以下又は０．１重量％以下としてよい。アルカリ金属酸化物は各酸化物を０．２重量％以下としてもよく、アルカリ金属酸化物の合計を０．２重量％以下としてもよい。
　また、ＳｉＯ２、ＣａＯ、ＭｇＯ、Ａｌ２Ｏ３の合計を９８重量％超又は９９重量％超としてよい。
　生体溶解性無機繊維は、例えば、４０℃における生理食塩水溶解率が１％以上の無機繊維である。
　生理食塩水溶解率は、例えば、次のようにして測定される。すなわち、先ず、無機繊維を２００メッシュ以下に粉砕して調製された試料１ｇ及び生理食塩水１５０ｍＬを三角フラスコ（容積３００ｍＬ）に入れ、４０℃のインキュベーターに設置する。次に、三角フラスコに、毎分１２０回転の水平振動を５０時間継続して加える。その後、ろ過により得られた濾液に含有されている各元素の濃度（ｍｇ／Ｌ）をＩＣＰ発光分析装置により測定する。そして、測定された各元素の濃度と、溶解前の無機繊維における各元素の含有量（重量％）と、に基づいて、生理食塩水溶解率（％）を算出する。すなわち、例えば、測定元素が、ケイ素（Ｓｉ）、マグネシウム（Ｍｇ）、カルシウム（Ｃａ）及びアルミニウム（Ａｌ）である場合には、次の式により、生理食塩水溶解率Ｃ（％）を算出する；Ｃ（％）＝［ろ液量（Ｌ）×（ａ１＋ａ２＋ａ３＋ａ４）×１００］／［溶解前の無機繊維の重量（ｍｇ）×（ｂ１＋ｂ２＋ｂ３＋ｂ４）／１００］。この式において、ａ１、ａ２、ａ３及びａ４は、それぞれ測定されたケイ素、マグネシウム、カルシウム及びアルミニウムの濃度（ｍｇ／Ｌ）であり、ｂ１、ｂ２、ｂ３及びｂ４は、それぞれ溶解前の無機繊維におけるケイ素、マグネシウム、カルシウム及びアルミニウムの含有量（重量％）である。
　無機繊維は、強度の観点から、平均繊維径は通常１～５０μｍ、好ましくは２～１０μｍ、特に好ましくは２～５μｍであり、平均繊維長は通常１～２００ｍｍ、好ましくは２～５０ｍｍである。
　無機繊維の表面は被覆層で被覆されていてもいなくてもよい。被覆層は、水に難溶であり、且つ前述の如く生理食塩水には溶け易いものである。無機繊維の表面に被覆層を形成することで、保存期間中、無機繊維の溶液中への溶解は抑制される。
　無機繊維の表面に被覆層を形成する物質としては、リン酸塩、モリブデン化合物、ポリアミジン化合物、エチレンイミン化合物等が挙げられる。
　リン酸塩としては、トリポリリン酸アルミニウム、トリポリリン酸ニ水素アルミニウム、メタリン酸アルミニウム、リン酸亜鉛、リン酸カルシウム等が挙げられる。モリブデン化合物としては、モリブデン酸亜鉛、モリブデン酸アルミニウム、モリブデン酸カルシウム、リンモリブデン酸カルシウム、リンモリブデン酸アルミニウム等が挙げられる。ポリアミジン化合物としては、アクリルアミド、アクリロニトリル、Ｎ－ビニルアクリルアミジン塩酸塩、Ｎ－ビニルアクリルアミド、ビニルアミン塩酸塩、Ｎ－ビニルホルムアミド共重合体等が挙げられる。エチレンイミン化合物としては、アミノエチレン、ジメチレンイミン等が挙げられる。これら被覆層を形成する物質は、１種単独又は２種以上を組み合わせて用いることができる。
　無機繊維を、不定形組成物中、１０～６０重量％含むことが好ましく、好ましくは１０～５０重量％、さらに好ましくは１０～３０重量％、さらに好ましくは１５～３０重量％である。６０重量％超であると無機バインダーの量が低下するため接着力が低下する恐れがある。１０重量％未満であると成形性が低下する恐れがある。
　無機バインダーとしてコロイダルシリカを含むことができる。コロイダルシリカのｐＨは８以上が好ましく、９～１１がより好ましい。８未満であると選択された増粘剤の種類によっては適度の粘度を有するペーストにならない恐れがある。　
　コロイダルシリカを、不定形組成物を１００重量％とした場合、固形分として１～６０重量％含むことが好ましく、さらに好ましくは６～４２．５重量％、さらに好ましくは８～４２．５重量％、さらに好ましくは１０～４２．５重量％、さらに好ましくは１５～４０重量％、さらに好ましくは２０～３０重量％である。４２．５重量％超であると繊維の補強効果が低下し乾燥収縮率が大きくなる、又は成形性が低下する恐れがある。６重量％未満であると繊維の結合強度や接着性が低下する恐れがある。
　本発明では、アルカリ土類金属やアルカリ金属等の金属イオンを含まないキレート剤を用いる。このようなキレート剤を用いることにより、保管中の固化を防ぐことができる。
　キレート剤の例として、金属イオンを含まない、ＥＤＴＡ（エチレンジアミン四酢酸（Ethylene　Diamine　Tetraacetic　Acid））・Ｈ・３（ＮＨ４）の組成のキレート剤、ＥＤＴＡ・２Ｈ・２（ＮＨ４）の組成のキレート剤等が挙げられる。本発明では、キレート剤が無機繊維から溶出するアルカリ土類金属を捕獲し同時に保護層を形成することにより、アルカリ土類金属によりもたらされる保管中の悪影響を防ぐことができると推察される。キレート剤は電子供与基が２以上あるので金属キレート化合物を生成できる。電子供与基には、カルボキシ基、水酸基等がある。
　キレート剤を、不定形組成物中、０．０１～３．０重量％含むことが好ましく、０．０２～２．５重量％含むことが好ましく、０．０５～１．５重量％含むことが好ましく、さらに０．１～１．０重量％含むことがより好ましい。量が多すぎと不定形組成物が固化する恐れがある。量が少なすぎても不定形組成物が固化する恐れがある。
　本発明の組成物は通常溶媒を含む。溶媒としては、特に制限されないが、水及び極性有機溶媒が挙げられ、極性有機溶媒としては、エタノール、プロパノール等の１価のアルコール類、エチレングリコール等の２価のアルコール類が挙げられる。これらのうち、水が、作業環境の悪化がなく、環境への負荷がない点で好ましい。また、水としては特に制限されず、蒸留水、イオン交換水、水道水、工業用水等が挙げられる。
　溶媒の含有量は、不定形組成物を１００重量％としたとき、好ましくは１０～８０重量％であり、より好ましくは１５～６８重量％であり、より好ましくは２０～６８重量％であり、さらに好ましくは２５～６８重量％である。含有量が少なすぎると流動性が低くなるので施工性が悪くなり、また、機械的強度、特に曲げ強度が低下する。また、含有量が多すぎると不定形組成物のちょう度が高くなるので施工時に組成物がたれ、また、乾燥による収縮が大きくなる。
　また、溶媒は、溶媒として独立して添加してもよいし、材料中に含有される溶媒として材料と共に添加してもよい（例えばコロイダルシリカ）。溶媒の量は、独立して添加した量と材料中に含まれる量を合わせた量である。溶媒量を少なくして溶媒をコロイダルシリカに含まれる溶媒だけとすることができる。
　本発明の組成物は、添加剤として、バインダー、増粘剤、分散剤、防腐剤、ｐＨ調整剤等を含むことができる。
　無機バインダーとして、コロイダルシリカの他、アルミナゾル、ジルコニアゾル、チタニアゾル、リン酸アルミニウム等が挙げられる。有機バインダーとして、有機繊維、アクリルエマルジョン、澱粉等が挙げられる。
　有機繊維は無機繊維の保護膜として作用する。有機繊維としては、特に制限されず、天然繊維又は疎水処理された合成繊維のいずれであってもよく、天然繊維としては、パルプ、綿、麻等が挙げられ、合成繊維としては、ビニロン、レーヨン、ポリプロピレン、ポリエチレン等が挙げられる。これらのうち、パルプが、無機繊維を取り込み易い点で好ましい。有機繊維の平均繊維径は、通常１～３０μｍ、好ましくは２～１０μｍ、特に好ましくは２～５μｍである。平均繊維径が、１μｍ未満だと目地の強度が低くなり、また、３０μｍを超えると無機繊維を取り込み難くなる。有機繊維の含有量は、無機繊維１００重量部に対して、５～５０重量部が好ましい。
　有機繊維及び無機繊維共に、ある程度の疎水性を持たせることが、有機繊維及び無機繊維を水中に投入した際、急激に沈むことなく、ある程度の時間浮遊することになり、互いのあるいは他の混合材料との混合性がよくなる点で好ましい。疎水処理とは、繊維の疎水性を向上させる処理のことを指し、疎水処理の方法としては、例えば、繊維の周りを疎水性の薬剤でコーティングする方法が挙げられる。
　増粘剤としては、特に制限されず、公知のものが使用できる。具体的には、ヒドロキシエチルセルロース、アクリル酸ナトリウム重合物、ポリエーテルポリオール、アクリル系重合高分子ポリエステルアミン、エチレンオキサイド等が挙げられる。また、非イオン性増粘剤を用いることができる。増粘剤の含有量は、特に制限されないが、不定形組成物中に０．０１～１０重量％が好ましく、さらに好ましくは０．０１～８重量％、さらに好ましくは０．０１～５重量％である。
　分散剤としては、特に制限されず、公知のものが使用できる。具体的には、カルボン酸類、多価アルコール、アミン類等が挙げられる。分散剤の含有量は、特に制限されないが、不定形組成物１００重量％に対して０．０１～３重量％が好ましい。
　防腐剤としては、特に制限されないが、例えば、窒素原子又は硫黄原子を有する無機化合物又は有機化合物等が挙げられる。防腐剤の含有量は、特に制限されないが、不定形組成物１００重量％に対して０．０１～３重量％が好ましい。
　本発明の組成物が、ｐＨ調整剤を含んでいると、無機繊維の溶液への溶解を更に抑制することができ好ましい。ｐＨ調整剤としては、例えば緩衝溶液又は酸が挙げられる。緩衝溶液としては、ｐＨ４標準溶液であるフタール酸塩標準溶液（セーレンセン緩衝液）、ｐＨ７標準溶液である中性リン酸塩標準溶液が挙げられ、酸としては、酢酸、蟻酸等が挙げられる。ｐＨは４～８．５程度が好ましい。
　本発明の組成物は、無機粉体を含んでもよいし、含まなくてもよい。原料として添加して組成物を製造してもよいし、組成物を得た後から添加してもよい。
　無機粉体としては、シリカ、アルミナ、ムライト、ジルコン、ジルコニア、カオリン、粘土鉱物、チタニア、カルシア、マグネシアから選択される1種または2種以上（混合物）を用いることができる。
　本発明に係る不定形組成物は、各成分を混合・撹拌して製造できる。本発明に係る成形体は、不定形組成物を成形し乾燥／加熱して得ることができる。本発明の組成物はペースト状（漆喰）であるため、こてで塗ったり、手で固めたり、圧力銃で散布できる。
　本発明の不定形組成物は、長期に保管しても固化し難い。また、適度なちょう度を有し欠損した対象成形品等に塗り易く、塗って乾燥した後は、接着性に優れる。また、加熱の際も、対象成形品の性能に悪影響を及ぼし難い。
実施例１
［不定形組成物の製造］
　以下を混合撹拌して不定形組成物を製造した。
　ＳｉＯ２を７３重量％、ＣａＯを２４重量％、ＭｇＯを０．３重量％、Ａｌ２Ｏ３を２重量％含む無機繊維Ａ　２３．９重量％
　コロイダルシリカ（スノーテックス３０、日産化学工業社製、ｐＨ９～１１、固形分が３０％の懸濁液）　７５．８重量％（２２．７重量％（固形分量）、５３．１重量％（溶媒量））
　ＥＤＴＡ・Ｈ・３（ＮＨ４）（金属イオンを含まないキレート剤）（キレスト社製）　０．５重量％
　増粘剤（ｈｉメトローズ、信越化学工業社製）　０．８重量％
　尚、重量％は組成物全体を１００重量％としたときの量である。
［不定形組成物の評価］
　以下について評価した。結果を表１に示す。表中×は固化したこと又は固化したため測定できなかったことを表わす。
（１）ちょう度
　製造直後（初期）及び一定期間室温で保管した後の不定形組成物のちょう度をちょう度計により測定した。
（２）曲げ強度
　製造直後（初期）及び一定期間室温で保管した後の不定形組成物を、所定の型に詰め形状を整えてから、約１００℃で乾燥又は室温放置にて自然乾燥した。乾燥したサンプルを所定サイズに切断加工し、これについて曲げ強度を万能試験機により測定した。
（３）加熱収縮率
　製造直後（初期）及び一定期間室温で保管した後の不定形組成物を、所定の型に詰め形状を整えてから、約１００℃で乾燥又は室温放置にて自然乾燥した。乾燥したサンプルを所定サイズに切断加工し、これについて１１００℃で２４時間加熱して辺または長手方向の加熱収縮率を測定した。
（４）施工性
　製造直後（初期）及び一定期間室温で保管した後の不定形組成物を、対象成形品に塗布して、接着性、塗り性、成形性を評価した。全てに問題が無ければ○とした。
（５）加熱反応性
　製造直後（初期）及び一定期間室温で保管した後の不定形組成物を、対象成形品に塗布した後、１３００℃で２４時間加熱した。接着のはがれ、不定形組成物と対象成形品が溶融反応し形状が変形しなければ○とした。
実施例２，３，比較例１～５
　表１に示す成分と組成で、実施例１と同様にして不定形組成物を製造し評価した。尚、表中のコロイダルシリカの量は固形分量である。結果を表１に示す。
　表中、セラミック繊維は、シリカを４０～６０重量％、アルミナを６０～４０重量％含む繊維である。
　ＮＴＡは、ＮＴＡ（Nitrilo　Triacetic　Acid）・３Ｎａ・Ｈ２Ｏ、ＮＴＢは、ＮＴＡ・Ｈ・２Ｎａである。
Figure JPOXMLDOC01-appb-T000001
　比較例１，５の結果から、セラミック繊維を含む組成物は、金属イオンを含まないキレート剤を含まなくても、実用可能であるが、無機繊維Ａを含む組成物は、金属イオンを含まないキレート剤を含まなければ、使用できないことが分かる。
　また、比較例２，３，４から、金属イオンを含むキレート剤又はクエン酸では本発明の効果を奏することができないことが分かる。
　本発明の不定形組成物は、無機繊維含有ハードボード加工品、モールド品の補修剤や接着剤の材料と使用できる。
　上記に本発明の実施形態及び／又は実施例を幾つか詳細に説明したが、当業者は、本発明の新規な教示及び効果から実質的に離れることなく、これら例示である実施形態及び／又は実施例に多くの変更を加えることが容易である。従って、これらの多くの変更は本発明の範囲に含まれる。
　この明細書に記載の文献及び本願のパリ優先の基礎となる日本出願明細書の内容を全てここに援用する。

Claims (7)

  1. 　以下の組成を有する無機繊維と、金属イオンを含まないキレート剤とを含む不定形組成物。
    ［無機繊維の組成］
    　ＳｉＯ２　６６～８２重量％
    　ＣａＯ　１０～３４重量％
    　ＭｇＯ　３重量％以下
    　Ａｌ２Ｏ３　５重量％以下
    　ＳｉＯ２、ＣａＯ、ＭｇＯ、Ａｌ２Ｏ３の合計　９８重量％以上
  2. 　コロイダルシリカを含む請求項１記載の不定形組成物。
  3. 　前記コロイダルシリカのｐＨが、８～１１である請求項２記載の不定形組成物。
  4. 　前記キレート剤が、エチレンジアミン四酢酸・Ｈ・３（ＮＨ４）又はエチレンジアミン四酢酸・２Ｈ・２（ＮＨ４）である請求項１～３のいずれか記載の不定形組成物。
  5. 　不定形組成物中、無機繊維を１０～６０重量％、コロイダルシリカを固形分で１～６０重量％、金属イオンを含まないキレート剤を０．０１～３．０重量％含む請求項１～４のいずれか記載の不定形組成物。
  6. 　不定形組成物中、１０～８０重量％の溶媒を含む請求項１～５のいずれか記載の不定形組成物。
  7. 　請求項１～６のいずれか記載の不定形組成物が乾燥した成形物。
PCT/JP2012/007210 2011-12-01 2012-11-09 不定形組成物 WO2013080456A1 (ja)

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US9944552B2 (en) 2013-07-22 2018-04-17 Morgan Advanced Materials Plc Inorganic fibre compositions
DE112017004988T5 (de) 2016-09-30 2019-09-05 Morgan Advanced Materials Plc. Anorganische Faserzusammensetzungen
DE102021211747A1 (de) 2020-10-23 2022-04-28 Thermal Ceramics Uk Limited Wärmeisolierung
WO2022084655A1 (en) 2020-10-23 2022-04-28 Thermal Ceramics Uk Limited Thermal insulation
DE102021211746A1 (de) 2020-10-23 2022-04-28 Thermal Ceramics Uk Limited Wärmeisolierung
DE102021211745A1 (de) 2020-10-23 2022-04-28 Thermal Ceramics Uk Limited Wärmeisolierung
DE112021005608T5 (de) 2020-10-23 2023-08-24 Thermal Ceramics Uk Limited Wärmeisolierung
DE102021211747B4 (de) 2020-10-23 2024-02-29 Thermal Ceramics Uk Limited Wärmeisolierung

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