JPH0648848A - Incombustible composite material structure and its production - Google Patents

Abstract

PURPOSE: To easily and safely prevent environmental pollution by drying and curing an intermediate structure obtained by impregnating the dispersed phase of non-combustible continuous fiber or the like with the prescribed continuous phase and forming with lamination.

CONSTITUTION: A liquid soluble silicate of 20.0 parts, and having about 100 centipoise viscosity, pH 11.3 and 1.37 g/cm³ density and 1.0 part rutile grade metal oxide such as TiO are mixed to form 100 pts.wt. of a non-combustible liquid continuous phase matrix 11. On the other hand non-combustible continuous fiber or a fiber strand 10 dispersed with non-combustible inorganic particles of ≤5 μ size is prepared. Subsequently the strand 10 is drawn out from an bobbin package 20 and a non-impregnated strand 22 is introduced via guides 21 and 23 into a pan 24 and is impregnated with the matrix 11. Subsequently an obtd. intermediate structure of a composite material is cured by exposing its surface 15 to a hot air 17 of ≤90% relative humidity and 38-66°C, and a non-combustible composite material structure of glass fiber or the like having 0.5-2.0 mm thickness is produced by forming.

COPYRIGHT: (C)1994,JPO

Description

Detailed Description of the Invention

[0001]

FIELD OF THE INVENTION This invention relates to a noncombustible composite structure comprising particles or a noncombustible dispersed phase such as fiber reinforcement embedded in a noncombustible continuous phase such as a solidifiable inorganic liquid matrix, and The present invention relates to a manufacturing method thereof.

[0002]

BACKGROUND OF THE INVENTION Composite materials are embedded in a continuous phase, such as a liquid binding matrix that can be solidified.
It is composed of more than one kind of dispersed phase (for example, fiber reinforcing material). The composite structure consists of a fiber reinforcement made of glass, carbon or other inorganic material most commonly used as the dispersed phase and a thermosetting organic resin matrix used as the continuous phase. 800 ° F (42
When heated to temperatures above 7 ° C., most thermoset organic matrix materials will decompose, producing smoke and toxic fumes. When heated to temperatures above 1200 ° F (649 ° C), the glass fiber reinforcement melts. Primarily for these reasons, composite structures from prior art using glass fibers as the disperse phase are structures that may be exposed to fire or pipes that store and transport flammable liquids above ground. It was unsuitable for making structures for tanks and tanks. NFPA (National Fire Protection Asso) is a standard for storage and handling of flammable liquids.
ciation, American Fire Protection Code 30 but this provision requires the use of steel or other noncombustible structural materials for aboveground fuel storage tanks, refinery aboveground piping and similar applications. There is. FAA (Federal Aviati
on Administration, Federal Aviation Administration and DOT (Departme
(nt of Transportation) requires aircraft and train interiors to be made of materials that will not burn or produce toxic fumes when exposed to fire temperatures above 750 ° F (399 ° C). . Steel ground tanks are corroded and can cause fires due to lightning strikes or carelessness during maintenance or repair of corroded parts of the tank. Living structures made of wood are very vulnerable to fire, while ordinary plastic and resin impregnated fiberglass structures generate toxic fumes and smoke when exposed to ignition temperatures.

A common matrix material used as the continuous phase of a composite material is a two-part curable thermosetting organic polymer, which is relatively expensive and requires special care in its shipping, storage and handling. When these organic matrix materials are unsaturated polyester or vinyl ester resin, they usually contain as much as 50% by weight of styrene monomer, and must be handled as flammable liquids. Ventilation of the working environment is often necessary because of the strange odor produced by the vaporization of styrene monomer. When an epoxy resin is used as the organic matrix material, care must be taken to prevent the amine curing agent from coming into contact with the worker's skin or being inhaled. In addition, matrix materials of the type described above, which are commonly used in composites, require special solvents and other chemicals to clean the tools and containers used. Soluble silicates have long been considered unsuitable for use as the continuous phase in fiber reinforced composite materials. One reason is that soluble silicates attack glass and are believed to cure by dehydration rather than by polymerization or chemical reaction. The adhesive strength and interlaminar shear strength of the cured soluble silicate are considerably lower than those of many plastics and thermosetting resins. The soluble silicate gradually dissolves in water unless its surface is coated or special heat treatment is performed. In addition, soluble silicates can be cured too rapidly when using microwave energy or exposed to temperatures above 150 ° F (65 ° C),
The resulting composite material structure becomes extremely brittle and unusable.

[0004]

SUMMARY OF THE INVENTION An object of the present invention is to solve the above-mentioned problems of the prior art, to prevent smoke and toxic gas from being generated by heat, and to safely and without polluting the working environment. It is to provide a non-combustible composite material structure that can be easily manufactured.

[0005]

The present inventor has generally used a continuous phase matrix of a fiber reinforced composite structure if it is modified by adding a metal oxide and clay in a liquid soluble silicate. It has been found that structural as well as chemical properties may be expected over and above the conventional chemical compositions used. For example, unimpregnated woven and non-woven fabrics of glass fiber strands used in the dispersed phase to combine with a liquid organic binder matrix that cures to form a composite material are 1300 ° F (70 ° F).
It melts when heated to 4 ° C. Also, when a glass fiber filament is impregnated with a certain type of liquid soluble silicate and bonded to it, even if the composite material structure obtained is heated above the melting point of the glass fiber filament, it remains as it is. there were. Also, when the continuous phase of the composite material comprises a liquid soluble silicate modified by the addition of a small amount of a metal oxide, the resulting composite material structure has a liquid continuous phase of 215 ° F.
Even when cured at an excessive dehydration rate such as exposure to a temperature of (102 ° C.) or higher, the solubility in water was sufficiently low.

Further, certain low viscosity soluble silicates are
Since it is easily impregnated with glass or carbon fiber and coated with it, it can be used for filament winding molding of a tube-shaped composite material structure. Soluble silicate is cheaper and less toxic than thermosetting resin,
Tools and molding equipment can be easily cleaned with water, environmentally safe, there is no environmental pollution during processing, shipping and handling is safe, and it can be easily and safely stored for many years. It can be easily cured by a specific dehydration technique. To the inventor, prior to the inventor, there was no practical way of utilizing the desirable properties of soluble silicates as the non-combustible continuous phase of composites containing non-combustible fibers or particles as the dispersed phase. I haven't found it. The present invention has been made based on such findings, and provides an economical and effective method of using a liquid soluble silicate as a continuous phase matrix material of a noncombustible composite material.

The first aspect of the present invention is to form a non-combustible liquid continuous phase by mixing a metal oxide and a liquid soluble silicate, and a dispersion comprising at least essentially non-combustible continuous fibers or non-combustible inorganic particles. A method of providing a cured, non-combustible composite structure by preparing a phase, impregnating a continuous phase with a dispersed phase to form an intermediate structure of the composite, and drying the intermediate structure. The second aspect of the present invention is a composite material structure obtained by the above method. As will be described later, the term "composite material structure" as used herein includes a filament winding structure, a plate material, a foam insulation material, and a coating material that can be used for paint coating.

The liquid soluble silicate used in the present invention is a silicic acid sodium having a silicic acid ratio (SiO ₂ / Na ₂ O weight ratio) of 2 to 4, and a specific gravity at room temperature (20 ° C.) of 40 to 42. It is an aqueous solution of 2 baume (1.37 to 1.41 g / cm ³ ). Metal oxides include zinc oxide, titanium oxide,
It is suitable to add iron oxide or the like to the liquid soluble silicate in a weight ratio of 1 to 10%, preferably 4 to 8%. Further, examples of the non-combustible continuous fibers constituting the non-combustible dispersed phase, glass fibers, carbon fibers, mineral fibers such as basalt fibers, etc., and non-combustible particles, such as mineral powder of clay or Examples include foamed particles of minerals such as expanded perlite and expanded vermiculite.
Further, the mixing ratio of the continuous phase and the dispersed phase may be appropriately determined depending on the properties of the raw materials used, the type of the target composite material structure, the manufacturing conditions, and the like. To some extent, the proportion of the dispersed phase in the mixture is 30 to 70% by volume when the dispersed phase is fibrous, and when the dispersed phase is powdered like a coating material. Is preferably in the range of 5 to 40% by weight.

A liquid composition obtained by adding and mixing 5% by weight of zinc oxide powder to a certain soluble silicate was prepared at 250 ° F. (1
When heated to 20 ° C. and dehydrated, it was found that the obtained cured product was very brittle, but its solubility in water was sufficiently low. It has been found that this liquid composition can be used as a binder to make high temperature resistant, non-combustible, water resistant insulation from expanded perlite and vermiculite. Such insulation has commercial applications such as fire doors, ground pipes and tanks. Furthermore, when a liquid soluble silicate (continuous phase) is impregnated into a laminate or ribbon containing glass fibers (dispersed phase) and its surface is exposed to hot air, the fibers bond to each other and consist of multiple layers. Non-combustible composite structures can be formed. It has been found that such structures can be used as components of filament winding pipes, pressure vessels and tanks for storing or transporting non-flammable or flammable liquids or gases.

Further, since a certain liquid soluble silicate has a sufficiently low viscosity, it can be easily impregnated into a continuous fiber twine or a yarn constituting a tightly woven glass cloth. Such a silicate was filed by the inventor on February 26, 1992, which is pending in the US patent.
It can also be used as the continuous phase constituting the composite material structure disclosed in Serial No. 07 / 838,463 "Double-walled composite material pipe and joint structure and its manufacturing method and manufacturing apparatus". The disclosure of the patent application is added here for reference. In particular, certain low-viscosity liquid soluble silicates have been described in the referenced patent application as non-combustible, eg, 100
It is an ideal matrix material that provides a permeable annular structure for composite pipes that exhibits an ignition point above 0 ° F (538 ° C). This soluble silicate matrix can also be used with carbon fibers at 2,000 ° F.
A non-combustible composite material structure capable of withstanding a high temperature (1,076 ° C.) or higher is obtained. Further, when a liquid soluble silicate matrix material is dehydrated and slowly cured at temperatures below 150 ° F (65 ° C), the fiber reinforced composite structure retains a substantial portion of the fiber reinforcement's tensile strength. I was also found to do. When constructed as a composite material structure of the type described in the inventor's U.S. Pat. No. 3,784,441 "Composite Material Structure", granted on Jan. 8, 1974, By using this soluble silicate, it becomes possible to construct a high tensile strength electrical insulator that does not generate a carbonized short circuit path even when an arc is generated on the surface.

When an aqueous solution of a soluble silicate is exposed to air, it hardens by dehydration. By adding Dow Silicon 200 liquid having a viscosity of approximately 10 centistokes to liquid soluble silicate, its shelf life and usable "pot life"
Will increase for months. This is because, in this case, the oil-like film of the silicon liquid floats on the surface of the liquid matrix mixture mainly composed of the liquid soluble silicate and serves as a barrier against air. This air barrier prevents dehydration and prevents the formation of a hardened silicate film or coating. Otherwise, the viscosity of the liquid soluble silicate will change and the wetting and impregnation properties of the fibers will also change.

The many advantages of using a silicate-based matrix in a reinforced composite include the following: formation of a non-combustible composite having a melting point greater than twice that of glass fiber; any conventional thermoset. Reduces the price of liquid matrix to a lower price than organic resins; provides a completely non-toxic working environment; simplifies the treatment of all liquid matrix material wastes; odorless, non-polluting, environmentally safe and non-flammable matrix material Providing a quick and easy cleaning of the matrix coater and equipment handling the matrix using just water; using a one-part matrix system that does not require mixing; providing a matrix that cures in dry hot air or at room temperature.

In broad terms, the method of the present invention for making a noncombustible composite structure comprises the steps of: mixing a metal oxide with a liquid soluble silicate to form a noncombustible liquid continuous phase. Preparing a dispersed phase comprising at least essentially non-combustible continuous fibers or non-combustible inorganic particles, impregnating the continuous phase with the dispersed phase to form an intermediate structure of the composite material and drying the intermediate structure. To cure the continuous phase to obtain a cured, non-combustible composite material. The additive mixing step preferably comprises adding about 1.0 to 5% by weight of the continuous phase metal oxide to the liquid soluble silicate. This adding step may also include adding rutile grade titanium oxide powder, zinc oxide powder, and / or iron oxide powder to the liquid soluble silicate. The liquid soluble silicate has a viscosity of about 60 to 400 centipoise and a specific gravity of about 40.0 to 42.2 Baume (about 1.37 to 1.41).
g / cm ³ ) and a pH of about 11.3 are preferred.

A suitable amount (eg, 5 to 40%, preferably 10 to 40% by weight of the liquid soluble silicate) of kaolin clay powder is mixed with one or more prior to mixing with the liquid continuous phase. It can be added to metal oxides to obtain paintable noncombustible composites or coatings with the required viscosity and thixotropy. Such paintable coating materials combine iron oxide and metal oxides,
Can be colored. Kaolin (Al ₂ O ₃ , 2H ₂
O) is a major constituent of many clays, some of which contain lime, alkalis, organic materials and other impurities. When mixed with a liquid soluble silicate, the clay does not dissolve but remains in a colloidal solution. When the liquid soluble silicate hardens, the clay-containing mixture hardens,
Clay exhibits reversible colloidal properties and, therefore, exhibits considerable compressive strength.

In the above preparation step, it is preferable to prepare about 30 to 70% by volume of the composite material of glass or carbon fiber. The glass fibers are preferably about 3 to 25 microns in diameter and 50 to 675 yards of E-glass strand per pound in count. In the drying step, the composite intermediate structure is heated to about 65-150 ° F.
It is preferable to expose to a temperature of (18 ° C to 66 ° C) to accelerate the dehydration hardening of the continuous phase. The step of exposing to heat can also include blowing hot air onto the surface of the composite intermediate material until it is properly cured.

As mentioned above, the method of manufacture can also include adding to the continuous phase an anti-hardening agent having a lower specific gravity than the liquid soluble silicate. A preferred method is to include in the additive mixing step the addition of a sufficient amount of silicone liquid to form a thin, air impermeable layer on the surface of the liquid continuous phase. A preferred silicone fluid is Dow 200 with a viscosity of about 10-100 centistokes.
(Dow Corning Co., Ltd. trade name) Polydimethylsiloxane silicone liquid.

1 and 2 illustrate the commercial application of the method of the present invention in which a plurality of fiber strands 10 are brought together to form a dispersed phase, the individual fibers 12 of which have a liquid matrix ( Impregnation to impregnate 11)
It is intended to form a dispersed phase through an infiltration step. 3-5 illustrate that the method further contemplates placing matrix-impregnated twine strands 13 on a mold to form first layer 14. FIG. 6 shows that the drying step involves exposing at least one surface 15 of the strand 13, preferably impregnated with the matrix, to a curing temperature of about 150 ° F. (66 ° C.).
One way to achieve this is to blow hot air 17 onto the surface 15 of the composite structure using a hot air blower 16 to accelerate the dehydration and hardening of the liquid continuous phase 11 to form the matrix that binds the strands. That is.

Within the scope of the present method, the steps of replenishing the fiber strands and impregnating the matrix as described above are repeated to form a second layer 18 of Twain strands 13 impregnated with the matrix, over the first layer 14. Disposing the second layer 18 to form a multi-layer composite structure 19 as shown in FIGS. 3, 4 and 5. As shown in these figures, the second step 18 includes the first layer 1 in the placement step.
Arranged across 4 and orienting the strands of the first and second layers in two directions relative to each other. More preferably, the disposing step comprises orienting the fiber strands of the first and second layers at least approximately perpendicular to each other.

The liquid composition mainly composed of the liquid soluble silicate and the metal oxide in the present invention can considerably enhance the heat resistance of ordinary glass fiber and other suitable materials as a composite material matrix. Safe, non-combustible, non-toxic,
It gives an odorless and low viscosity inorganic continuous phase. The composition can be applied with a brush, roller or spray device without the need for ventilation. The composition can be used as a filament winding matrix for making refractory composite pipe or tank structures. In combination with continuous fiber reinforcement or woven fabric reinforcement, compression molding, pultrusion molding is possible, or it can be used as a matrix for laminated molding. It can be used in combination with expanded perlite or vermiculite as a matrix for continuous phase bonding of noncombustible composite insulation. It can be used in combination with finely divided clay, rock or sand particles as a hardenable liquid matrix of a coatable refractory, non-combustible composite coating.

The liquid composition of this invention can be shipped and stored in standard plastic containers. The composition has a shelf life of at least 5 years when covered and stored below 150 ° F (66 ° C). The composition can be used for the production of smoke-free, non-combustible composite material structures for aircraft interiors and interior structures and furniture which do not emit smoke or toxic gases when exposed to fire. The non-combustible composite material of this invention is not degraded by non-polar solvents such as styrene monomers, petroleum-based liquids, uncured polyester and epoxy plastics and methylene chloride. If the non-combustible composite material of the present invention is expected to continue to be in continuous contact with water, acids, alcohols or foods, except for the specific syntactic foam insulation,
It must be wrapped in an impermeable, water resistant coating or structure.

Other industrial applications of the composite structure used as a matrix for this composition also include the following: the path does not carbonize when an electric arc runs on the outer surface, high tensile strength and brittle. Electrical insulation; at least 2000 ° F
Storage structure of refractory insulation that withstands (1093 ° C) and still retains structural strength; mold containing molten metal; barrel, chase for guns and bazooka missiles, rocket booster case, solid fuel rocket Non-combustible carbon fiber composite materials such as those used for nozzles, etc .; Others.

[0022]

The present invention will be described in more detail with reference to the following examples. (Example 1) As shown in FIGS. 1 to 6, various incombustible composite material structures were formed by including a dispersed phase composed of the glass fiber reinforcing material 10. At that time, the dispersed phase was impregnated with a continuous phase composed of a curable liquid matrix 11. The weight composition of the continuous phase was as follows, and the continuous phase was impregnated so that the total amount of the dispersed phase and the continuous phase was 100 parts. 20.0 parts of liquid soluble silicate, its viscosity is 100 centipoise, density is 1.37 g / c
m ³ (40.0 Baume), pH 11.3. (P
Product name “PQ soluble silicate” manufactured by Industrial Chemicals Division of Q Corporation, product name “Soda silicate”
Solution E "), 1.0 part rutile grade titanium oxide powder (trade name" Tioxide ") 0.02 part polydimethylsiloxane, whose viscosity is 10 centistokes. (Dow Corning Cor
Poration's trade name "Dow Corning 200 Fuluid") Following the step of impregnating the glass fiber reinforcement with the liquid matrix, the surface of the composite structure is exposed to less than 80% relative humidity and a temperature of about 75 ° F (23 ° C). ) And exposed to the air to cure. This molding procedure results in a thickness of 0.020
A non-combustible composite panel was made using ˜0.080 inch (0.5-2.0 mm) woven glass fiber fabric.

(Example 2) A non-combustible pipe structure was manufactured by the same procedure as shown in FIG. The strand 10 of glass continuous fiber roving is pulled out from the internal package 20 and passed through the strand guide 21 to pass the strand 22 which is not yet impregnated and further to the strand guide 23.
Of the liquid matrix 11 into the coater pan 24, where the strands were impregnated with the liquid matrix. The liquid matrix used was the same as in Example 1 above in the same proportions. Further, the strand is passed under the coater-impregnated rod 25, combined with the strand which is not impregnated, and passed through the ribbon forming and squeeze rods 26 and 27, and further under the ribbon width control rod 28 to be formed. The formed ribbon 30 was guided and laminated on the molding surface. Prior to being laminated on the molding surface, the strand ribbon 30 is passed in front of the hot air blower 16 in which the outlet temperature of heated air is approximately 450 ° F (196.7 ° C), and the upper and lower surfaces of the ribbon are exposed to hot air for a short time. I was exposed. The surface temperature of the ribbon is 15 so that the liquid matrix does not boil or dehydrate too quickly.
Do not exceed 0 ° F (65.6 ° C). The thickness of the strand ribbon 30 is approximately 0.020 inch (0.5 m).
m). Ten layers of strand ribbon were laminated to give a composite cylinder thickness of about 0.20 inches (5 mm). By using a hot air blower to dehydrate and cure the liquid matrix composition, the multilayer composite material was sufficiently cured immediately after molding and processing, and could be released from the surface of the cylindrical mold.

Example 3 A non-combustible composite syntactic foam structure was produced using expanded perlite as the dispersed phase and a mixture having the following weight composition as the liquid continuous phase. 20.0 parts of liquid soluble silicate, its viscosity is 100 centipoise, density is 1.37 g / c
m ³ (40.0 Baume), pH 11.3. (P
Product name “PQ soluble silicate” manufactured by Industrial Chemicals Division of Q Corporation, product name “Soda silicate”
Solution E "), 1.0 part zinc oxide powder (trade name" Dow Corning 200 Fuluid "by Dow Corning Corporation) In this example, the preferred expanded perlite for use in non-combustible syntactic foam materials is" coarse agricultural grade uncoated ". The dry perlite was added to the liquid matrix and mixed in a suitable mixer until uniform bread seeds were formed. The mixture was cast into a mold and 275 °.
It was placed in a furnace heated to F (135 ° C). At least 2
Non-combustible syntactic that does not melt or disintegrate even after soaking in water for many days when placed in air heated to 50 ° F (121 ° C) for 2 hours. A foam was obtained. This non-combustible composite insulation can be used to make roofing boards, furnace fillings, steam pipes, but also for sound insulation and fire protection of glass fiber gas transport and air conditioning ducts. can do. When sandwiched between plywood and glass fiber panels, it can also be used for fire walls and fire doors.

Example 4 A white coatable noncombustible composite material structure or coating material was produced by using clay powder as a dispersed phase and a mixture having the following weight composition as a continuous phase. 14.0 parts of liquid soluble silicate, its viscosity is 100 centipoise, its density is 1.37 g / c
m ³ (40.0 Baume), pH 11.3. (P
Product name “PQ soluble silicate” manufactured by Industrial Chemicals Division of Q Corporation, product name “Soda silicate”
Solution E "), 1.0 part rutile grade titanium oxide powder (trade name" Tioxide ") 0.02 part polydimethylsiloxane, the viscosity of which is 10 centistokes. (Dow Corning Cor)
Poration's trade name "Dow Corning 200 Fuluid") The dispersed phase of this composite coating material is kaolin clay with a particle size of 200 micro inches (trade name "Thiele manufactured by John K. Bice Co.
RC 32 "). About 4.0 parts by weight of the dry dispersed phase was added to 15.02 parts of the liquid continuous phase and mixed well. 2000 ° F of butane gas torch applied on clean wood surface
A white undercoat was obtained which protected the wood surface from ignition against a (1093 ° C) flame. It has been found that this non-combustible basecoat swells upon heating, which improves the flame resistance of the wood surface. This non-combustible basecoat is also paintable over it and has been found to be compatible with many indoor and outdoor waterborne alkyd paints.

[0026]

INDUSTRIAL APPLICABILITY The noncombustible composite material structure of the present invention has a melting point that is at least twice as high as the melting point of glass fiber. It is a material that does not generate toxic gas and is useful as various structural materials and heat insulating materials. Further, according to the method of the present invention, since non-toxic, odorless and environmentally-unfriendly materials are used as raw materials, the manufacturing work is safe and easy, and the equipment used is easily washed. Further, there is a great advantage that it can be cured at room temperature depending on the composition of raw materials. Such a material has never been used before, and its industrial utility value is extremely high.

[Brief description of drawings]

FIG. 1 is a schematic diagram showing a plurality of Twain fiber strands impregnated with a curable liquid continuous phase and used as the dispersed phase of a non-combustible composite structure.

FIG. 2 is a schematic diagram showing a plurality of Twain fiber strands with a longitudinally flexible center structure.

FIG. 3 is an isometric view showing a partial cross-section of a non-combustible composite material structure formed into a multi-layer laminated pipe.

FIG. 4 is a schematic cross-sectional view showing a joining structure for mechanically joining adjacent ends of a set of composite material pipes.

5 is an enlarged isometric view partially showing the longitudinally oriented, matrix-impregnated twine strands of the bonded structure of FIG. 4. FIG.

FIG. 6 is a diagram schematically showing an apparatus for forming and curing the twine strands that are oriented in the circumferential direction and impregnated with the matrix, which constitutes the bonding structure of FIG.

[Explanation of symbols]

 10. Fiber strand 11. Matrix (continuous phase) 12. Fiber 13. Twain Strand 14. First layer 15. Surface 16. Hot air blower 17. Hot air 18. Second layer 19. Composite material structure 20. Package 21, 23. Strand guide 22. Strand 24. Coater bread 25. Coater impregnated rod 26, 27. Ribbon forming squeeze bar 28. Ribbon width control rod 30. ribbon

Claims (32)

[Claims] 1. A step of adding and mixing a metal oxide and a liquid soluble silicate to form an incombustible liquid continuous phase, a disperse phase comprising at least essentially incombustible continuous fibers or incombustible inorganic particles. A step of impregnating and infiltrating the dispersed continuous phase with the liquid continuous phase to form an intermediate structure of a composite material, and drying the intermediate structure to cure the continuous phase to form a hardened non-combustible composite material structure. A method of manufacturing a non-combustible composite material structure comprising the steps of forming. 2. The step of adding and mixing comprises adding 1 to 10% by weight of the continuous phase of the powdered metal oxide.
2. The method according to claim 1, further comprising adding to the liquid soluble silicate. 3. The method according to claim 2, wherein the step of adding the metal oxide comprises adding powdery rutile (titanium oxide) grade titanium oxide to the liquid soluble silicate. . 4. The method of claim 1 wherein the step of preparing the dispersed phase comprises preparing the dispersed phase at least essentially consisting of incombustible inorganic particles smaller than about 5 microns. 5. The method according to claim 2, wherein the step of adding the metal oxide comprises adding iron oxide powder to the liquid soluble silicate. 6. The liquid soluble silicate has a pH of about 11.
3. The method according to claim 1, which is a liquid soluble silicate having a viscosity in the range of about 60 to 400 centipoise. 7. The liquid soluble silicate is SiO ₂ / Na
The weight ratio of ₂ O is 2 to 4, and the specific gravity at 68 ° F (20 ° C) is 40 to 42.2 Baume (1.37 to 1.41 g /
2. The method according to claim 1, which is a liquid soluble silicate composed of an aqueous solution of sodium silicate of cm ³ ). 8. The method of claim 2, wherein the step of adding and mixing comprises adding 1 to 10% by weight of zinc oxide of the continuous phase to the liquid soluble silicate. Production method. 9. The disperse phase preparing step comprises preparing a disperse phase of glass, carbon or basalt fibers in an amount by volume of 30 to 70% of the composite structure. The manufacturing method according to claim 1, wherein: 10. The method of claim 9, wherein the step of preparing the dispersed phase comprises preparing the dispersed phase of glass fibers having individual diameters of about 4 to 25 microns. 11. The step of preparing the dispersed phase comprises about 50 to 675 yards per pound in length per weight.
30-9900 tex) strands of glass fiber.
The manufacturing method described. 12. The method according to claim 1, wherein the step of preparing the dispersed phase comprises preparing a dispersed phase composed of noncombustible inorganic particles. 13. The method of claim 12, wherein the step of preparing the dispersed phase comprises preparing a dispersed phase comprising particles of expanded perlite or expanded vermiculite. 14. The step of drying the composite intermediate structure at a temperature of about 250-275 ° F. (12).
The method according to claim 1, which comprises exposing to air having a relative humidity of about 90% or less at 1.1 to 135 ° C). 15. The drying step comprises exposing the wetted surface of the composite intermediate structure to hot air to bring the temperature of the matrix on the surface of the intermediate structure to at least about 1.
The manufacturing method according to claim 1, wherein the temperature is set to 0 to 150 ° F (38 to 66 ° C). 16. The method according to claim 15, wherein the exposing (drying) step comprises blowing hot air onto both surfaces of the composite intermediate structure. 17. The step of adding and mixing as described above, further comprising:
A process according to claim 2, characterized in that kaolin clay powder having a particle size of about 200 microns, which corresponds to 10 to 40% by weight of the liquid soluble silicate, is added to the liquid continuous phase. . 18. The method according to claim 1, wherein the step of adding and mixing comprises adding a surface hardening inhibitor having a specific gravity smaller than that of the liquid soluble silicate to the liquid continuous phase. Production method. 19. The step of adding and mixing comprises adding to said liquid continuous phase an amount of a polymer having a viscosity of about 10 centistokes sufficient to form an air impermeable coating on the surface of said liquid continuous phase. 19. The manufacturing method according to claim 18, further comprising adding a dimethylsiloxane silicon liquid. 20. The step of preparing a dispersed phase is the preparation of a plurality of fiber strands forming a discontinuous phase,
The manufacturing method according to claim 1, wherein the impregnating / infiltrating step comprises impregnating the plurality of fiber strands with the liquid continuous phase. 21. The manufacturing method according to claim 20, further comprising, prior to the step of impregnating / infiltrating, at least three of the fiber strands are brought together to obtain an impregnated Twain strand containing the discontinuous phase. A method for manufacturing a non-combustible composite material structure, which comprises forming the same. 22. The manufacturing method according to claim 21, wherein
Furthermore, the impregnated Twain strand is about 0.5 mm.
A method for producing a non-combustible composite material structure, which comprises forming a flat ribbon having a thickness of 1. 23. The manufacturing method according to claim 21,
Further, the impregnated twine strand is formed into a cord having a diameter of about 0.5 to 12 mm, which is a method for producing a non-combustible composite material structure. 24. The manufacturing method according to claim 21, wherein
Furthermore, the impregnated twine strands are arranged on a molding surface to form a first layer, which is a method for producing a non-combustible composite material structure. 25. The step of drying comprises subjecting the surface of the impregnated twine strands to at least about 65-150.
25. The method of claim 24, which comprises heating to a temperature of ° F (18-65 ° C) to cure the liquid continuous phase and form a bond of the strands with the matrix. 26. The manufacturing method according to claim 24, further comprising repeating the above-mentioned steps of tweening, impregnation and infiltration to laminate-form a second layer on the first layer to form a composite of a plurality of layers. A method for manufacturing a non-combustible composite material structure, which comprises forming a material structure. 27. The laminating step comprises disposing the second layer across the first layer and orienting the strands of the first and second layers in two directions relative to each other. 27. The manufacturing method according to claim 26. 28. The method of claim 27, wherein the step of laminating comprises making the strands of the first and second layers at least substantially orthogonal to each other. 29. A noncombustible composite material structure manufactured by the manufacturing method according to any one of claims 1 to 28. 30. An incombustible, insoluble syntactic foam insulation produced according to the method of claim 14. 31. A liquid non-combustible paint coating material produced according to the production method of claim 4. 32. A non-combustible composite structure as a non-combustible overcoatable coating produced according to the method of claim 4.