JPH09123155A - Method for producing inorganic cured composite - Google Patents

Abstract

(57) 【Abstract】 PROBLEM TO BE SOLVED: To suppress damage to the surface of a cured body when heating and curing a SiO ₂ —Al ₂ O ₃ -based reactive inorganic powder and an inorganic composition slurry containing an alkali metal silicate aqueous solution as a main component. While providing air bubbles in the vicinity of the upper surface of the molding die, a method for producing an inorganic cured product excellent in product appearance quality and mechanical strength is provided. A SiO ₂ -Al ₂ O ₃ -based powder, between the slurry inorganic composition based on alkali metal silicate solution, was injected into a mold, a slurry-like mineral composition top and mold In addition, a lattice-shaped article formed of stainless steel, an organic fiber or an inorganic fiber is heat-cured while scissors to be an inorganic cured body, and the inorganic cured body and the lattice-shaped article are integrated into one body. Body manufacturing method.

Description

Detailed Description of the Invention

[0001]

BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to a method for producing an inorganic cured composite, and more specifically, it is nonflammable and stable in strength, which is useful as a building member such as inner and outer walls of homes and buildings, partitions, roof tiles, floors and the like. The present invention relates to a method for producing a board-shaped inorganic cured composite.

[0002]

_2. Description of the Related Art An inorganic cured product prepared by injecting a slurry inorganic composition containing SiO ₂ -Al ₂ O ₃ powder and an alkali metal silicate aqueous solution as a main component into a molding die and curing it by heating is Because of its excellent non-combustibility and mechanical strength, it is widely used as a building member such as a wall or partition of a house or office building, or a floor.

For example, Japanese Patent Publication No. 3-9060 discloses that
In a hydrated inorganic molding material which is composed of an inorganic solid reaction component and an alkali metal silicate solution and can be cured at a low temperature,
Solid reaction component per 1 part by weight of alkali metal silicate solution:
(a) Electrostatic precipitator ash or (b) ground calcined bauxite or (c) a mixture of (a) and (b) 0.5-4.0
Part by weight, the alkali metal silicate solution is SiO ₂ vs. K ₂ O
Or having a molar ratio of Na ₂ O of 1.2 to 2.5, and a molding material having a water content of 20 to 65% by weight with respect to the solid reaction component, which is a water-curable inorganic molding material curable at low temperature. It is disclosed.

However, in order to heat and harden the SiO ₂ -Al ₂ O ₃ -based powder and the slurry-like inorganic composition containing an alkali metal silicate aqueous solution as a main component, the above-mentioned slurry-like inorganic material is used to prevent water evaporation. After injecting the composition into the mold, it is necessary to heat in a sealed state, and the bubbles generated in the slurry-like inorganic composition are broken in the vicinity of the upper surface of the mold to form a large number of irregularities. Especially, when a thin board is produced, there is a problem that not only the appearance quality of the product is deteriorated but also the mechanical strength is deteriorated.

[0005]

SUMMARY OF THE INVENTION The present invention has been made in view of the above facts, and its object is to provide SiO ₂ —Al ₂ O ₃ -based powder and an alkali metal silicate aqueous solution. When heat-curing the slurry inorganic composition as the main component, removing air bubbles near the upper surface of the mold while suppressing damage to the surface of the cured product, producing an inorganic cured composite excellent in product appearance quality and mechanical strength There is a way to provide.

[0006]

The present invention is directed to SiO ₂ --Al ₂ O ₃
System powder, a slurry inorganic composition containing an alkali metal silicate aqueous solution as a main component is poured into a mold, and stainless steel, organic fiber or inorganic fiber is used between the upper surface of the slurry inorganic composition and the mold. A gist of the method for producing an inorganic cured composite is characterized in that the lattice-shaped product to be formed is heat-cured while scissors to be an inorganic cured product, and the inorganic cured product and the lattice-shaped product are integrated. is there.

The above-mentioned SiO ₂ —Al ₂ O ₃ powder is SiO ₂ / Al ₂ O ₃
= 1/9 to 9/1 (weight ratio) is preferably used. The above-mentioned SiO ₂ -Al ₂ O ₃ -based powder is the above-mentioned SiO ₂ -Al ₂ O ₃
Ingredients are the main ingredients, and at least 5 in total
It preferably accounts for 0% by weight or more. When the content of the above components is less than 50% by weight, the reactivity with the aqueous solution of alkali metal silicate is lowered, and the mechanical strength of the obtained inorganic cured product is lowered.

The above-mentioned SiO ₂ —Al ₂ O ₃ -based powder can be obtained from various raw material sources and by various processing means. For example, it contains 80% by weight or more of particles having a particle size of 10 μm or less. Fly ash, an inorganic powder obtained by melting fly ash, fly ash, clay or a mixture thereof containing 80% by weight or more of particles having a particle size of 10 μm or less, which is calcined at 400 to 1000 ° C., and sprayed in the air. Inorganic powder obtained by applying mechanical energy of 0.1 to 30 kgh / kg to the body and clay,
In addition, the inorganic powder obtained in the above item is further heated at 100 to 750 ° C.
Inorganic powder obtained by heating to the temperature of
Examples thereof include inorganic powder obtained by applying mechanical energy of 0.1 to 30 kgh / kg to metakaolin, ash of an electrostatic precipitator during corundum or mullite production, ground calcined bauxite, and metakaolin. These SiO ₂ —Al ₂ O ₃ -based powders may be used alone or as a mixture of two or more.

The above-mentioned fly ash is JIS A 6
Fine particle size ash collected by a dust collector from a pulverized coal combustion boiler specified in 201, SiO ₂ 40% or more, moisture 1%
Below, specific gravity 1.95 or more, specific surface area 2700 cm ² / g
As described above, 75% or more passes through the 44 μm standard sieve.

The method for preparing fly ash from the above fly ash is not particularly limited, and examples thereof include wet sedimentation classification, air classification, other classification using specific gravity, jet mill, roll mill, ball mill, and other fine classification. Examples thereof include a system using a crusher and a classifier. The fly ash having a particle size of 10 μm or less less than 80% by weight has a low reactivity with an aqueous solution of an alkali metal silicate, and the mechanical strength of the obtained inorganic cured product is low.
It is not preferable because it may cause curing failure.

As the above fly ash, there is used fly ash obtained by treating the above fly ash at 400 to 1000 ° C. or treating fly ash at 400 to 1000 ° C. in the same manner.
Fly ash is generally black, but if coloring other than black is desired, it is decolorized by firing. If the baking temperature is lower than 400 ° C, decolorization is not sufficient,
If it exceeds, the reactivity with the alkali metal silicate aqueous solution is lowered, so that the above-mentioned firing temperature is preferably used.

As a method for preparing the above-mentioned inorganic powder, it can be obtained by melting fly ash or clay or a mixture thereof and spraying it into the air. The technique of spraying the above-mentioned melt into the gas is ceramic coating. The thermal spray technology used for is applied. This spraying technique is preferably carried out with 2000 of the above fly ash and clay.
It is melted at a temperature of ˜16000 ° C. and sprayed at a speed of 30 to 80 m / s, and specific examples thereof include a plasma spraying method, a high energy gas spraying method, and an arc spraying method. The surface area of the reactive inorganic powder obtained by the thermal spraying technique is generally controlled to 0.1 to 60 m ² / g.

The above clays and clays have the chemical composition
SiO _2: 5 to 85 wt%, Al ₂ O _3: 90~10 clay containing by weight% is used. Examples of the clay having the above composition include kaolinite, dickite, nakrite, kaolin minerals such as halloysite, muscovite, illite, fengite, glaucoma, celadonite, paragonite, blancmalite and other mica clay minerals, montmorillonite, beidellite. , Nontronite, savonite, sauconite, etc., smetite, chlorite, pyrophyllite, talc, shale, etc.

The particle diameters of the above clay and metakaolin are not particularly limited, but an average particle diameter of 0.01 to 5 is required for the mechanical energy to act effectively.
00 μm is preferable, and more preferably 0.1 to 100 μm.
m.

The mechanical energy applied to the above clay and metakaolin means compression force, shearing force, impact force, etc., which may be acted alone or in combination of two or more kinds. Good. These mechanical energies are, for example, ball mills, vibration mills, planetary mills,
It is provided by a medium stirring type mill, a roller mill, a mortar, a jet pulverizer, or the like.

The above mechanical energy is 0.1 kwh / k
If it is less than g, the reactivity with the aqueous solution of alkali metal silicate decreases, and if the mechanical energy exceeds 30 kwh / kg, the load on the crushing device increases and the wear and other damage of the device increase. Not only this, but problems such as impurities in the clay and the like occur, so the mechanical energy is 0.1 to 30 kwh / kg, preferably 1.0 to 2
Act at 6 kwh / kg.

When the above mechanical energy is applied, a grinding aid may be added if necessary. The grinding aid, when applying mechanical energy, clay or metakaolin powder adheres to the inside of the device,
Agents for preventing remarkable aggregation, for example, alcohols such as methyl alcohol and ethyl alcohol, alcohol amines such as triethanolamine, metal soaps such as sodium stearate and calcium stearate, acetone vapor, etc. Is mentioned. These may be used alone or in combination of two or more.

In preparing the above-mentioned inorganic powder, after applying the above mechanical energy to the clay, 10
This is because the heat treatment is performed at a temperature of 0 to 750 ° C., and the improvement in mechanical strength of the obtained inorganic cured product is recognized by the heating. When the heating temperature is less than 100 ° C,
No improvement in the mechanical strength of the obtained inorganic cured product is observed, and when the heating temperature exceeds 750 ° C., crystallization occurs in the inorganic powder, and the reactivity with the alkali metal silicate aqueous solution decreases. The heating temperature is 100 to 750 ° C, preferably 200 to 600 ° C. Further, if the heating time is too short, the mechanical strength of the obtained inorganic cured product is not improved so much, and if it is long, the energy cost is increased. Therefore, the heating time is appropriately set in the range of about 1 minute to 5 hours.

The above-mentioned inorganic powders have
It is a powder as described in Japanese Patent No. 9060 and Japanese Patent Publication No. 4-45471. The above metakaolin is
It is not particularly limited and, for example, commercially available metakaolin is preferably used.

The above aqueous solution of alkali metal silicate includes
_{SiO 2 / M 2 O (M} : an alkali metal, the molar ratio) = 0.05-8
Is preferable, and a more preferable molar ratio (SiO ₂ / M ₂
O) = 0.5 to 2.5. Alkali metal (M)
Examples of the type include sodium, potassium, lithium and the like, and an alkali metal silicate of one kind or two or more kinds thereof is used. When the above molar ratio is less than 0.05,
The content of the alkali metal with respect to the SiO ₂ component serving as the binder component increases, and the water resistance of the resulting inorganic cured product decreases. When the molar ratio exceeds 8, the gelling time becomes short, the storage stability of the inorganic composition decreases, and the molding workability of the inorganic cured product decreases.

The concentration of the alkali metal silicate in the alkali metal silicate aqueous solution is preferably about 10 to 60% by weight. If the concentration of the alkali metal silicate is less than 10% by weight, the water resistance of the resulting inorganic cured product will decrease. On the other hand, if the concentration of the alkali metal silicate exceeds 60% by weight, the viscosity of the alkali metal silicate aqueous solution increases, and the workability of mixing the inorganic composition and the molding workability of the inorganic hardened product deteriorate.

The amount of the aqueous alkali metal silicate solution to be added is 10 to 1300 parts by weight, preferably 10 to 10 parts by weight, relative to 100 parts by weight of the SiO ₂ —Al ₂ O ₃ based reactive inorganic powder.
The amount is 00 parts by weight, more preferably 10 to 550 parts by weight. If the blending amount is less than 10 parts by weight, it is difficult to mix the inorganic composition, and a uniform mixture cannot be obtained.
If it exceeds 300 parts by weight, the resulting inorganic cured product may have a quality defect such as cracking.

If necessary, the above-mentioned reactive inorganic composition may be added with an inorganic filler, a reinforcing fiber, a lightweight aggregate, a coloring agent, a foaming agent, a foaming aid, a foaming agent and the like. As the inorganic filler, those having a low activity with respect to the alkali metal silicate aqueous solution are preferably used, for example, silica sand,
Examples include rock powder, volcanic ash such as shirasu and anti-firestone, wollastonite, calcium carbonate, silica stone powder, diatomaceous earth, mica, silica fume, etc. However, it is not limited to these.

The reason why it is preferred that the inorganic filler has a low activity with respect to the alkali metal silicate aqueous solution is that when the activity is high, gelation of the alkali metal silicate aqueous solution progresses rapidly, and the mixture of the above inorganic compositions is mixed. This is because the workability and the workability of molding the inorganic cured body become difficult. The amount of the inorganic filler added is preferably 900 parts by weight or less based on 100 parts by weight of the SiO ₂ —Al ₂ O ₃ powder. The above addition amount is 900
If the amount is more than parts by weight, the mechanical strength of the obtained inorganic cured product is reduced.

As the above-mentioned reinforcing fibers, those which are usually used in cement products are used. For example, polypropylene fibers, polyethylene fibers, polyester fibers, polyamide fibers, vinylon fibers, rayon, carbon fibers, acrylic fibers, aramid fibers. , Artificial fibers such as acrylonitrile fiber and alkali-resistant glass fiber, and natural fiber such as silk. These organic fibers or inorganic fibers are used alone or as a mixture.

The shape of the reinforcing fiber is as follows: fiber diameter 1 to
It is preferably 500 μm and the fiber length is 1 to 15 mm. When the fiber diameter is less than 1 μm, a fiber ball is formed at the time of addition to the inorganic composition to reduce the mechanical strength of the obtained inorganic cured product, the fiber diameter exceeds 500 μm, and the fiber length is 1 mm. If it is less than the above range, the reinforcing effect such as improvement in tensile strength of the obtained inorganic cured product cannot be obtained. If the fiber length exceeds 15 mm, the dispersibility in the inorganic composition decreases, and the resulting cured inorganic material has a large variation in mechanical strength. The addition amount of the reinforcing fiber made of the organic fiber or the inorganic fiber is preferably 10 parts by weight or less with respect to 100 parts by weight of the SiO ₂ —Al ₂ O ₃ powder. The above addition amount is 10
If it exceeds the weight part, the dispersibility in the above-mentioned inorganic composition decreases.

Examples of the lightweight aggregates include inorganic foams such as pearlite, glass balloons, silica balloons, fly ash balloons, and shirasu foams, organic foams such as phenolic resins, urethane resins, polyethylene foams and polystyrene foams. The body etc. are used. The amount of the lightweight aggregate added is preferably 150 parts by weight or less based on 100 parts by weight of the SiO ₂ —Al ₂ O ₃ -based powder. When the above-mentioned addition amount exceeds 150 parts by weight, the molding workability of the inorganic cured body becomes difficult, and the mechanical strength and surface smoothness of the obtained inorganic cured body also deteriorate.

As the colorant, for example, metal oxide pigments such as iron oxide, titanium oxide and cobalt oxide, carbon black and the like are preferably used. The amount of the colorant added is preferably 50 parts by weight or less with respect to 100 parts by weight of SiO ₂ —Al ₂ O ₃ -based powder. Even if the addition amount exceeds 50 parts by weight,
It is uneconomical because the hiding power of these colorants is not so different.

Examples of the foaming agent include Mg and C
a, Cr, Mn, Fe, Co, Ni, Cu, Zn, A
l, Ga, Sn, Si, metal powder such as ferrosilicon, hydrogen peroxide solution, aqueous solution or powder of peroxide such as sodium peroxide, potassium peroxide, sodium perborate are used.
Above all, Al powder and hydrogen peroxide solution are preferably used because of their cost, safety, availability, and mixing work. The metal-based powder and the peroxide-based powder have a particle size of 1 to
About 200 μm is preferable. When the particle size is less than 1 μm, the dispersibility in the inorganic composition is deteriorated, and rapid foaming occurs, so that fineness and uniformity of cells cannot be obtained. On the other hand, if the particle size exceeds 200 μm, the reactivity of foaming decreases, and it is not possible to provide the obtained inorganic cured product with a sufficient foaming structure. The amount of the foaming agent added is SiO ₂ -Al.
5 parts by weight (or parts by weight of solute in the case of an aqueous solution) is preferable for 100 parts by weight of ₂ O ₃ based powder. When the above-mentioned addition amount exceeds 5 parts by weight, the mechanical strength of the obtained inorganic cured foam decreases, and handling becomes difficult.

As the foaming aid, for example, porous powder such as silica gel, zeolite, activated carbon and alumina gel, and metal soap such as metal stearate and metal palmitate are preferably used. The addition amount of the foaming aid is Si
It is desirable that the amount is 10 parts by weight or less based on 100 parts by weight of O ₂ —Al ₂ O ₃ powder. When the above-mentioned addition amount exceeds 10 parts by weight, the foaming reaction is adversely affected, for example, the number of foam breakage increases in the foaming process.

Examples of the foaming agent include various foaming agents of higher alcohol sulfate ester type, alkyl ether sulfate ester type, aromatic derivative sulfonate type, imidazoline derivative type, fatty acid amide type and animal protein type. Agents are preferably used. The amount of the foaming agent added is SiO ₂ --Al ₂ O.
10 parts by weight or less is desirable for 100 parts by weight of the ₃ series powder. If the amount added is more than 10 parts by weight, the resulting cured inorganic material may be defective in curing.

The means for mixing the foamable inorganic composition is not particularly limited, but, for example, a paddle rotation type mixer, a rocking type mixer, a screw type mixer or the like is used. The procedure for mixing the inorganic composition is not particularly limited, but for example, various solid raw materials may be dry-mixed, and an alkali metal silicate aqueous solution may be added and mixed thereto, or all raw materials may be mixed. You can mix them all at once,
Alternatively, a method may be employed in which some solid raw materials are mixed with the alkali metal silicate aqueous solution and then the remaining solid raw materials are sequentially mixed. In the procedure of mixing the foamable inorganic composition, it is preferable to add and mix the foaming agent at the end of the above mixing from the viewpoint of mixing workability and stability of bubbles. When using a foaming agent,
A foaming agent is added at the end of the above mixing, or a slurry is prepared with a raw material other than the foaming agent, and the foaming agent and water are mixed therewith to mix an aqueous solution in which bubbles are generated. You may be asked. When the foaming agent is used as an aqueous solution, the concentration of the foaming agent is preferably 0.1 to 5% by weight. When the concentration of the foaming agent is less than 0.1% by weight, the stability of the bubbles is poor and the number of foam breakage increases, and when the concentration of the foaming agent exceeds 5% by weight, curing failure of the obtained inorganic cured product may occur. It may occur.

The slurry-like inorganic composition obtained as described above is filled in a mold. The filling means is as follows.
The filling may be performed by a free fall method, but may be performed by a pump or the like. During or after filling the slurry inorganic composition, vibration may be applied to the slurry inorganic composition in the mold for leveling and defoaming the slurry inorganic composition.

The stainless steel grid-shaped product used in the present invention has a width and thickness of the stainless steel portion forming the grid of 0.025 to 2 mm, preferably 0.025.
.About.1.2 mm, and the minimum aperture for forming the lattice is 0.
It is 026 to 10 mm, preferably 0.026 to 5 mm. If the wire diameter of the above stainless steel is less than 0.025 mm or the opening is less than 0.026 mm, it becomes difficult to produce a stainless steel lattice-shaped product, and if the wire diameter exceeds 2 mm, stainless steel is produced. The steel lattice-shaped product becomes hard and it becomes difficult to stack it on the molded body, the smoothness of the back surface of the stainless steel lattice-shaped product laminated part is lost, and moreover,
Adhesion to the inorganic cured body to be laminated may be reduced and the reinforcing effect may be lost. On the other hand, if the opening exceeds 10 mm, bubbles will remain between the eyes of the stainless steel lattice-shaped product, and the effect of eliminating bubbles will be insufficient.

The material of the above-mentioned lattice-shaped stainless steel is
Stainless steel wire specified in JIS G 4309, J
A hot rolled stainless steel plate and steel strip defined by IS G 4304, a cold rolled stainless steel plate defined by JIS G 4305, and the like can be used.

As the stainless steel lattice-shaped product,
For example, standard products include woven wire mesh specified in JIS G3555 and industrial woven wire mesh specified in JIS G3556. In addition, expanded metal and other welding,
A lattice-shaped product having the lattice openings, thickness and width of the lattice-shaped product of the present invention as described above can be appropriately prepared and used by means of bonding or weaving.

The mesh of the lattice-shaped product formed of the organic fiber or the inorganic fiber used in the present invention has a size of 1 cm ^2.
1 to 3000 pieces, preferably 1 to 2500 pieces are used. When the number of openings is less than 1 per 1 cm ^{2, the} number of remaining bubbles increases and the reinforcing effect decreases. On the contrary, when the number of openings is more than 3000 per 1 cm ² , the adhesiveness to the slurry inorganic composition becomes small, and the reinforcing effect of the cured inorganic material decreases.

The above-mentioned organic fiber or inorganic fiber is not particularly limited as long as it has alkali resistance. For example, polypropylene fiber, polyethylene fiber, polyester fiber, polyamide fiber, vinylon fiber, rayon, carbon fiber. , Artificial fibers such as acrylic fibers, aramid fibers, acrylonitrile fibers, and alkali-resistant glass fibers, and natural fibers such as silk. These organic fibers or inorganic fibers are used alone or as a mixture.

The mold used in the method for producing an inorganic cured composite of the present invention is composed of a male mold including a female mold having a mold cavity and a lid mold for sealing the upper surface of the mold cavity. As a method for sandwiching the lattice-shaped product between the upper surface of the slurry inorganic composition filled in the mold and the mold lid mold, as shown in FIG. 1, the lattice-shaped product 1 is slurried. It suffices to place it on the upper surface of the inorganic composition 2 so that the mold is closed, and as shown in FIG. 2, the grid-shaped product 1 is attached to the lid 31 of the mold 3 with a wire or other string-like material. Even if the lattice-shaped product 1 is brought into close contact with the upper surface of the slurry-like inorganic composition 2 in a mold-closed state by tightening at 4, or by detachably fixing with hooks, pins, bolts or other fixtures. Of course, as shown in FIG. 4, a locking step portion 33 is provided on the upper surface of the mold 3 on the side of the mold cavity 32, and the lattice-shaped article 1 is locked to the locking step portion 33. May adhere to the upper surface of the slurry inorganic composition 2. In addition, in the figure, the portion indicated by the reference numeral 34 is an injection port and a deaeration hole of the slurry inorganic composition 2 of the mold 3 lid 31.

The inorganic composition filled in the mold cavity as described above is heat-cured after the mold is closed as shown in FIGS. 3 and 4. The conditions for the heat curing include:
Hold at an ambient temperature of 50 to 300 ° C. for about 5 minutes to 12 hours. Needless to say, the higher the heating temperature, the shorter the curing time, but when using organic fibers with low heat resistance, select a heating temperature that is suitable for the raw materials used and do not cause thermal deterioration of these raw materials. Should be noted. After the above-mentioned heat-curing is completed, the mold is removed and heat-dried. The heating and drying conditions are 30 to 150 ° C. and 5 minutes to 12 hours.

The method for producing an inorganic cured composite of the present invention is as follows:
Since it is configured as above, SiO ₂ -Al ₂ O ₃ based powder,
When a slurry inorganic composition containing an alkali metal silicate aqueous solution as a main component is poured into a mold and cured by heating, bubbles generated in the molding die do not make the surface of the obtained inorganic cured product uneven. The degassed and used lattice-shaped product can be embedded and integrated in the inorganic cured body to produce an inorganic cured composite body excellent in strength and impact resistance by a simple apparatus.

[0042]

BEST MODE FOR CARRYING OUT THE INVENTION Embodiments of the present invention will be described below with reference to examples.

[0043] (1) SiO ₂ -Al ₂ O ₃ -based preparation of powder SiO ₂ -Al ₂ O ₃ -based powder A fly ash (KANDEN Chemical Co. Ltd., average particle size 20 [mu] m, J
Classify IS A 6201) with a classifier (manufactured by Nisshin Engineering Co., Ltd., trade name: TC-15),
A SiO ₂ —Al ₂ O ₃ -based powder A having a particle size of 10 μm or less was prepared. SiO ₂ -Al ₂ O ₃ -based powder B kaolin (composition: SiO ₂ 45.7 wt%, Al ₂ O ₃ 38.8
% By weight, average particle size 5 μm, BET specific surface area: 5.8 m ²
/ G) at 3000 ° C. and then sprayed in the air at a speed of 80 m / s to give an average particle size of 5 μm and a BET specific surface area of 9.5.
The SiO ₂ -Al ₂ O ₃ -based powder B of m ² / g was prepared. SiO ₂ -Al ₂ O ₃ based powder C metakaolin (manufactured by Engelhart, trade name: SATE
NTONE SP33, average particle size 3.3 μm, BET specific surface area: 5.8 m ² / g) 100 parts by weight, 0.5 parts by weight of a mixed solution of 25% by weight triethanolamine and 75% by weight ethanol was added to an ultrafine mill ( Made by Mitsubishi Heavy Industries, using zirconia ball 100 mm, ball filling rate 8
5% by volume) and mechanical energy of 10 kwh / kg was applied to obtain SiO ₂ —Al ₂ O ₃ -based powder C. The mechanical energy applied is a value obtained by dividing the electric power supplied to the ultrafine mill by the unit weight of the treated powder.

(2) Preparation of Alkaline Metal Silicate Aqueous Solution Alkali metal silicate aqueous solution JIS No. 1 shown in Table 1 Sodium silicate aqueous solution (Nippon Kagaku Kogyo Co., Ltd.), 1K potassium silicate aqueous solution (Nippon Kagaku Kogyo Co., Ltd.) and sodium silicate An aqueous potassium solution (prepared using sodium hydroxide / potassium hydroxide manufactured by Wako Pure Chemical Industries, Ltd.) was prepared. In the table, M represents an alkali metal.

[0045]

[Table 1]

(3) Iron Lattice-Like Plates Stainless steel lattice-shaped products shown in Table 2 [abbreviated as lattice-shaped products (SUS) in Table 2] All manufactured by Sakakura Metal Co., Ltd.] were prepared.

[0047]

[Table 2]

Lattice-shaped products made of organic fibers and inorganic fibers shown in Table 3 [abbreviated as Lattice-shaped products (Senii) in Table 2]. 4-7
Are manufactured by Kurashiki Spinning Co., Ltd., and 8-11 are manufactured by NBC Kogyo Co., Ltd.].

[0049]

[Table 3]

(4) Inorganic Composition Table 4 shows the composition of the inorganic composition used in the following Examples. The specifications of other additives are as follows. Silica powder: manufactured by Marubeni Textile Materials Co., Ltd. Talc: manufactured by Nippon Talc Co., Ltd., product name: Talc S Vinylon fiber: manufactured by Kuraray Co., Ltd., product name: RM182-4

[0051]

[Table 4]

[0052] (Example 1) SiO ₂ -Al ₂ O ₃ system powder A100
By weight, 30 parts by weight of an alkali metal silicate aqueous solution are mixed for 2 minutes using an omni mixer (manufactured by Chiyoda Giken Co., Ltd.) to prepare a reactive inorganic composition a, which is filled in a mold,
As shown in FIG. 1, the grid 1 was placed on the upper surface of the slurry-like reactive inorganic composition a, and the mold was closed. Then, the grid 1 was heated in a hot air oven at 85 ° C. for 8 hours and demolded to obtain a stainless steel grid-shaped product. 10mm by further drying for 16 hours at 60 ℃ with the embedded
An inorganic cured body of × 250 mm × 50 mm was produced.

(Example 2) Using the inorganic composition b and the lattice-shaped product 2 shown in Table 5, the molding method shown in FIG. After adhering to the upper surface of the water-soluble inorganic composition b, an inorganic cured body was prepared in the same manner as in Example 1.

Example 3 Using the inorganic composition c and the lattice-shaped product 3 shown in Table 5, an inorganic cured product was produced in the same manner as in Example 2 by the molding method shown in FIG.

(Example 4) Using the inorganic composition d and the lattice-shaped product 4 shown in Table 5, the molding method shown in FIG. 4 was used to form the lattice-shaped step on the upper surface of the mold on the mold cavity side. After locking the product 4 and bringing it into close contact with the upper surface of the above-mentioned slurry-like reactive inorganic composition b, an inorganic cured body was produced in the same manner as in Example 1.

(Examples 5 to 8) Inorganic cured products were prepared in the same manner as in Examples 1 to 4 by using the inorganic compositions, lattice-shaped products and molding methods shown in Table 5.

Comparative Examples 1 to 6 Inorganic compositions were prepared in the same manner as in Example 1 using the inorganic compositions and molding methods used in the Examples as shown in Table 6 except that the lattice-shaped products were not used. Was cured and dried to prepare an inorganic cured body.

The following evaluations were carried out on the inorganic cured products obtained in the above Examples and Comparative Examples. The evaluation results are also shown in Tables 5 and 6. 1. Removal of Air Bubbles The presence or absence of air bubbles on the surface of the inorganic cured body on the side where the lattice-shaped product is laminated was evaluated by visual observation. It should be noted that the evaluation was made in two stages: ◯: one having a smooth surface without bubbles on the surface of the inorganic cured body, and ×: one having a surface with unevenness that was cured while bubbles were attached to the surface of the inorganic cured body.

2. Bending Strength Using an Autograph AGS-1000B manufactured by Shimadzu Corporation, the bending strength was measured under the measurement conditions of three-point bending, span: 200 mm, crosshead speed: 2 mm / min.

[0060]

[Table 5]

[0061]

[Table 6]

[0062]

EFFECT OF THE INVENTION Since the method for producing an inorganic cured composite of the present invention is constructed as described above, it is a slurry containing SiO ₂ --Al ₂ O ₃ powder and an alkali metal silicate aqueous solution as a main component. When the inorganic composition is poured into the molding frame and cured by heating, a lattice-shaped product made of stainless steel or organic fibers or inorganic fibers is set between the upper surface of the molding frame and the slurry inorganic composition. As a result, the air bubbles generated in the molding frame are degassed without making the surface of the obtained inorganic cured body uneven, and an inorganic cured body having high mechanical strength and a beautiful smooth surface is produced by a simple apparatus. be able to.

[0063]

[Brief description of the drawings]

FIG. 1 is a cross-sectional view for explaining an example of a molding frame using a main part of the method for producing an inorganic cured composite body of the present invention.

FIG. 2 is a cross-sectional view showing a closed state of the molding die shown in FIG.

FIG. 3 is a cross-sectional view for explaining another embodiment of a molding die that uses the main part of the method for producing an inorganic cured composite body of the present invention.

FIG. 4 is a cross-sectional view for explaining another embodiment of the molding die that uses the main part of the method for producing an inorganic cured composite body of the present invention.

[Explanation of symbols]

 DESCRIPTION OF SYMBOLS 1 Lattice-shaped product 2 Slurry inorganic composition 3 Molding form 31 Lid type (male) 32 Female type 33 Locking step part 34 Degassing hole 4 Wire

Claims (1)

[Claims] 1. A SiO ₂ —Al ₂ O ₃ -based powder and a slurry-like inorganic composition containing an alkali metal silicate aqueous solution as a main component are injected into a mold to form a top surface of the slurry-like inorganic composition and the mold. In between, a lattice-shaped product formed of stainless steel, an organic fiber or an inorganic fiber is heat-cured while scissors to be an inorganic cured product, and the inorganic cured product is integrated with the above-mentioned lattice-shaped product. Method for producing composite.