JP2010168264A - Inorganic porous body and method for producing the same - Google Patents

Abstract

<P>PROBLEM TO BE SOLVED: To provide an inorganic porous body and a method for producing the same excellent in productivity, capable of widely controlling a pore diameter and its distribution easily, and capable of forming a thin film. <P>SOLUTION: The inorganic porous body is produced by dispersing an inorganic compound in water to obtain a water dispersion of the inorganic compound, dispersing a liquid organic compound in the water dispersion of the inorganic compound to obtain an organic-inorganic water dispersion, and removing the water and the liquid organic compound of the organic-inorganic water dispersion. <P>COPYRIGHT: (C)2010,JPO&INPIT

Description

  The present invention relates to an inorganic porous body and a method for producing the same.

  Conventionally, porous bodies made of various materials such as organic materials have been used as, for example, a substance separation, a carrier supporting a functional material (for example, a catalyst), a battery membrane, a buffer material, and the like. For example, a foam obtained by foaming a polymer material such as polyurethane, polystyrene, polyethylene, polypropylene, and phenol resin is used as the porous body.

On the other hand, with the progress of research on nanocomposites using metal oxides and clay minerals in recent years, for example, a method for producing porous bodies made by combining organic materials such as polymer materials and inorganic materials has been studied. Has been.
For example, after preparing a gel formed by polymerizing a water-soluble organic monomer in a solution containing a water-swellable clay mineral and forming a three-dimensional network, the solvent contained in the solution is then frozen and removed (freeze-dried). ) Has been proposed (see, for example, Patent Document 1).

  According to the method for producing a porous material described in Patent Document 1, it is possible to obtain a porous material that is low in density, has a controlled pore diameter and its distribution over a wide range, and does not contain macro cracks.

JP 2004-359747 A

However, the method for producing a porous material described in Patent Document 1 requires a troublesome process such as preparation of a gel or freeze-drying, and thus has a problem of poor productivity. In addition, since the gel is a gel formed by forming a three-dimensional network, the gel cannot be applied, and therefore, there is a problem that it is difficult to reduce the thickness of the porous material.
An object of the present invention is to provide an inorganic porous body that is excellent in productivity, can easily control the pore diameter and its distribution widely, and can be formed into a thin film, and a method for producing the same.

  In order to achieve the above object, the method for producing an inorganic porous body of the present invention includes an inorganic compound dispersion step of dispersing an inorganic compound in water to obtain an aqueous dispersion of the inorganic compound, and the aqueous dispersion of the inorganic compound, An organic compound dispersion step of dispersing a liquid organic compound to obtain an organic-inorganic water dispersion, and a removal step of removing water and the liquid organic compound of the organic-inorganic water dispersion are provided. .

Moreover, in the manufacturing method of the inorganic porous body of this invention, it is suitable to mix | blend a hydrophobic compound in the said organic compound dispersion | distribution process.
Moreover, in the manufacturing method of the inorganic porous body of this invention, it is suitable in the said organic compound dispersion | distribution process to mix | blend the bulk, needle shape, or plate-shaped hydrophobic inorganic compound.
Moreover, in the manufacturing method of the inorganic porous body of this invention, it is suitable to mix | blend surfactant in the said inorganic compound dispersion | distribution process and / or the said organic compound dispersion | distribution process.

In the method for producing an inorganic porous body of the present invention, a binder is blended into any of the water, the aqueous dispersion of an inorganic compound, the liquid organic compound, and the organic-inorganic aqueous dispersion. Is preferred.
In addition, the inorganic porous body of the present invention is obtained by the above-described method for producing an inorganic porous body.

According to the method for producing an inorganic porous body of the present invention, the pore diameter and the distribution of the inorganic porous body can be widely controlled and thinned by a simple operation. Therefore, the pore diameter and the distribution thereof are widely controlled, and a thin inorganic porous body can be produced with high production efficiency.
As a result, the inorganic porous material of the present invention produced by the method for producing an inorganic porous material of the present invention is produced with high production efficiency, and the pore diameter and its distribution are easily controlled and thinned. .

The image processing figure of the electron micrograph which shows the cross-section of the inorganic porous body of Example 1 is shown. The image processing figure of the electron micrograph which shows the cross-section of the inorganic porous body of Example 2 is shown. The image processing figure of the electron micrograph which shows the cross-section of the inorganic porous body of Example 3 is shown. The image processing figure of the electron micrograph which shows the cross-section of the inorganic porous body of Example 4 is shown. The image processing figure of the electron micrograph which shows the cross-section of the inorganic porous body of Example 9 is shown. The image processing figure of the electron micrograph which shows the cross-section of the inorganic porous body of Example 12 is shown. The image processing figure of the electron micrograph which shows the cross-section of the inorganic porous body of Example 13 is shown. The image processing figure of the electron micrograph which shows the cross-section of the inorganic porous body of Example 16 is shown. The image processing figure of the electron micrograph which shows the cross-section of the inorganic porous body of Example 17 is shown. The image processing figure of the electron micrograph which shows the cross-section of the inorganic porous body of Example 18 is shown. The image processing figure of the electron micrograph which shows the cross-section of the inorganic porous body of Example 19 is shown. The image processing figure of the electron micrograph which shows the cross-section of the inorganic compound of the comparative example 1 is shown.

In the method for producing an inorganic porous body of the present invention, first, an inorganic compound is dispersed in water to obtain an aqueous dispersion of the inorganic compound (inorganic compound dispersion step).
In the present invention, examples of the inorganic compound include bulk inorganic compounds, acicular inorganic compounds, and plate-like inorganic compounds.
Examples of the bulk inorganic compound include inorganic compounds such as a spherical shape, a rectangular parallelepiped shape, or an irregular shape thereof, and examples thereof include silicon oxide (silica), tin oxide (including antimony-doped tin oxide), and titanium oxide. Zinc oxide, aluminum oxide (alumina), calcium carbonate, magnesium hydroxide, barium titanate, silicon nitride, and other metal fine particles.

Examples of the acicular inorganic compound include potassium titanate, wollastonite, sepiolite, acicular tin oxide, acicular magnesium hydroxide, and the like.
Examples of the plate-like inorganic compound include boron nitride, plate-like calcium carbonate, and plate-like aluminum hydroxide.
The plate-like inorganic compound also includes a layered clay mineral.

The layered clay mineral is a clay mineral having a layered structure in which unit crystals are laminated, and examples thereof include a montmorillonite mineral group (smectite group mineral).
Specific examples of the montmorillonite mineral group include montmorillonite (montmorillonite), magnesia montmorillonite (magnesian montmorillonite), tet montmorillonite (tetsu montmorillonite), tetmagnesian montmorillonite (tetsu magnesia montmorillonite). , Beidellite, aluminian beidellite, nontronite (nontronite), aluminian nontronite, saponite (saponite), aluminian saponite (aluminian saponite), hectorite, soconite, stevensite, bentonite and the like. Examples of the layered clay mineral include vermiculite (vermiculite), halloysite, swellable mica, and graphite.

Moreover, as an inorganic compound, a commercial item can be used, for example, a commercial item of silicon oxide (silica), a commercial item of titanium oxide, a commercial item of zinc oxide, a commercial item of antimony-doped tin oxide, and barium titanate. Commercial products and commercial products of layered clay minerals are used.
Examples of commercially available silicon oxide (silica) include Aerosil series (manufactured by Nippon Aerosil Co., Ltd.), and more specifically, Aerosil 300 (average diameter of primary particles: about 7 nm), Aerosil 200 (1 Secondary particle average diameter: about 12 nm), Aerosil 130 (primary particle average diameter: about 16 nm), Aerosil 90G (primary particle average diameter: about 20 nm) (Nippon Aerosil Co., Ltd.).

  Moreover, as a commercial item of silicon oxide (silica), the commercial item of the aqueous dispersion of silicon oxide (silica) is also included. Examples of commercially available aqueous dispersions of silicon oxide (silica) include the Snowtech series (manufactured by Nissan Chemical Industries), and more specifically, Snowtex 20 (primary particle diameter: 10 to 20 nm). ), Snowtex 50 (primary particle diameter: 20 to 30 nm), Snowtex 20L (primary particle diameter: 40 to 50 nm) (above, manufactured by Nissan Chemical Industries, Ltd.), and the like.

Examples of commercially available antimony-doped tin oxide include the SN series (manufactured by Ishihara Sangyo Co., Ltd.), and more specifically, SN-100S, SN-100P (powder, primary particle size: 10 to 30 nm). SN-100D (water dispersion, solid content concentration 30% by weight) (above, manufactured by Ishihara Sangyo Co., Ltd.).
Examples of commercially available titanium oxide include TTO series (manufactured by Ishihara Sangyo Co., Ltd.), and more specifically, TTO-51 (A) (primary particle diameter: 10 to 30 nm), TTO-55 ( A) (primary particle diameter: 30 to 50 nm), TTO-55 (B) (primary particle diameter: 30 to 50 nm), TTO-55 (D) (primary particle diameter: 30 to 50 nm), TTO-S -1 (short axis length: 10-20 nm, long axis length: 50-100 nm), TTO-S-3 (short axis length: 10-20 nm, long axis length: 50-100 nm), TTO-V -3 (short axis length: 5 to 15 nm, long axis length: 30 to 90 nm), TTO-F-2 (primary particle diameter: 30 to 50 nm), TTO-F-6 (primary particle diameter: 50) ˜90 nm) (made by Ishihara Sangyo Co., Ltd.).

Examples of commercially available products of zinc oxide include ZnO-310 (primary particle diameter of 15 to 35 nm), ZnO-350 (primary particle diameter: 10 to 30 nm), and ZnO-410 (primary particle diameter: 5 to 15 nm). (Above, manufactured by Sumitomo Osaka Cement Co., Ltd.).
As a commercial item of barium titanate, BT-HP100 (made by Kyoritsu Material Co., Ltd.) etc. are mentioned, for example.

  Commercially available layered clay minerals include, for example, Kunipia series (Montmorillonite, manufactured by Kunimine Kogyo Co., Ltd.), Bengel series (Bentonite, manufactured by Hojun Co., Ltd.), Somasif ME series (Swellable mica, manufactured by Corp Chemical Co., Ltd.) Synthetic products include, for example, smecton (saponite, manufactured by Kunimine Kogyo Co., Ltd.), Lucentite SWN (hectorite, manufactured by Corp Chemical), laponite (hectorite, manufactured by Rockwood Additives), and the like. .

These inorganic compounds can be used alone or in combination of two or more.
The inorganic compound is preferably hectorite.
In the present invention, the average diameter of the primary particles of the inorganic compound (in the case of a needle-like inorganic compound or a plate-like inorganic compound, the maximum length of the inorganic compound) is, for example, 1 to 1000 nm, preferably 5 to 500 nm. Preferably, it is 10-300 nm.

When the average diameter of the primary particles of the inorganic compound (the maximum length of the inorganic compound in the case of a needle-like inorganic compound or a plate-like inorganic compound) exceeds the above range, the organic compound of the target size Oil droplets (described later) may not be obtained.
Further, when a bulk inorganic compound and / or an acicular inorganic compound is used as the inorganic compound, the average diameter of the primary particles (in the case of an acicular inorganic compound, the maximum length of the inorganic compound) is more preferable. Is 1 to 200 nm, particularly preferably 5 to 100 nm.

  Further, when an acicular inorganic compound and / or a plate-like inorganic compound is used as the inorganic compound, the aspect ratio of the inorganic compound (in the case of the acicular inorganic compound, the major axis length / minor axis length, or Expressed by long axis length / thickness, and in the case of a plate-like inorganic compound, expressed by diagonal length / thickness or long side length / thickness) is, for example, 5-200, preferably 10 to 100.

  In the present invention, as the inorganic compound, for example, an inorganic compound that has a certain degree of affinity with water is used. Preferably, an inorganic compound having a good balance between hydrophilicity and hydrophobicity is used. By using an inorganic compound having a good balance between hydrophilicity and hydrophobicity, the inorganic compound can be present (locally distributed) at the interface between the aqueous phase and the oil phase in the organic compound dispersion step described later.

  If the hydrophobicity of the inorganic compound is too high, the inorganic compound is stably present in the oil phase (oil droplets of the organic compound) in the organic compound dispersion step described later, and the interface between the aqueous phase and the oil phase. In some cases, inorganic compounds cannot be present. Even when the hydrophilicity of the inorganic compound is too high, the inorganic compound is stably present in the aqueous phase in the organic compound dispersion step described later, and the inorganic compound is present at the interface between the aqueous phase and the oil phase. It may not be possible to

In the present invention, when the hydrophilicity of the inorganic compound is too high, for example, it is necessary to partially hydrophobize (surface treatment) the surface of the inorganic compound with a surface treatment agent.
Examples of the surface treatment agent include general surface modifiers such as coupling agents and fatty acids.
Examples of the coupling agent include a silane coupling agent, a titanium coupling agent, and an aluminum coupling agent.

  Examples of the silane coupling agent include 3- (meth) acryloxypropyl-trimethoxysilane, 3- (meth) acryloxypropyl-triethoxysilane, 3- (meth) acryloxypropylmethyl-dimethoxysilane, 3 -(Meth) acryloxypropylmethyl-diethoxysilane, vinyltrimethoxysilane, vinyltriethoxysilane, 4-vinylbutyltrimethoxysilane, 4-vinylbutyltriethoxysilane, 8-vinyloctyltrimethoxysilane, 8-vinyl Octyltriethoxysilane, 10- (meth) acryloxydecyltrimethoxysilane, 10- (meth) acryloxydecyltriethoxysilane, methyltrimethoxysilane, butyltrimethoxysilane, hexyltrimethoxysilane, decyl Limethoxysilane, hexadecyltrimethoxysilane, octadecyldimethylmethoxysilane, tetramethoxysilane, tetraethoxysilane, dimethoxydimethylsilane, methoxytrimethylsilane, diethoxydimethylsilane, methyltrimethoxysilane, methyltriethoxysilane, phenyltrimethoxysilane Phenyltriethoxysilane, dimethoxydiphenylsilane, diphenylethoxymethylsilane, dimethoxymethylphenylsilane, hexamethyldisilazane and the like.

  Examples of titanium coupling agents include isopropyl tristearoyl titanate, isopropyl tridodecylbenzenesulfonyl titanate, isopropyl tris (dioctylpyrophosphate) titanate, tetraisopropyl bis (dioctyl phosphite) titanate, tetraoctyl bis (ditridecyl phosphite). Titanate, tetra (2,2-diallyloxymethyl-1-butyl) bis (ditridecyl) phosphite titanate, bis (dioctylpyrophosphate) oxyacetate titanate, bis (dioctylpyrophosphate) ethylene titanate, isopropyltri (dioctylphosphate) titanate , Isopropyltricumylphenyl titanate, isopropyltri (N-amidoethylamino) Chill), such as titanate, and the like.

Examples of the aluminum coupling agent include acetoalkoxyaluminum diisopropylate.
Examples of the fatty acid include stearic acid, oleic acid, linoleic acid, linolenic acid, and eleostearic acid.
These surface treatment agents can be used alone or in combination of two or more.

As the surface treatment agent, a coupling agent is preferable, and a silane coupling agent is more preferable.
As a method for surface-treating an inorganic compound with a surface treatment agent, for example, a method of adding an alcohol aqueous solution, an organic solution or an aqueous solution of a surface treatment agent while stirring the inorganic compound in a mixer (dry method), an inorganic compound is alcohol Examples thereof include a method of adding a surface treatment agent after being dispersed in an aqueous solution or water (wet method), a method of spraying the surface treatment agent on an inorganic compound (spray method), and the like.

In addition, as an inorganic compound, the commercial item (for example, above-mentioned TTO series etc.) by which the surface treatment was performed previously on the surface of an inorganic compound can also be used.
The blending ratio of water and inorganic compound (excluding layered clay mineral) is, for example, 0.1 to 50 parts by weight of inorganic compound (excluding layered clay mineral), preferably 0, per 100 parts by weight of water. .2 to 40 parts by weight, more preferably 0.5 to 30 parts by weight.

When the blending ratio of the inorganic compound (excluding the layered clay mineral) exceeds the above range, the viscosity of the aqueous dispersion of the inorganic compound (excluding the layered clay mineral) becomes excessively high, and handling properties may be deteriorated.
In the case where a layered clay mineral is used as the inorganic compound, the mixing ratio of water and the layered clay mineral is, for example, 0.01 to 11 parts by weight, preferably 0.01 to 11 parts by weight with respect to 100 parts by weight of water. 0.5 to 5 parts by weight.

When the blending ratio of the layered clay mineral exceeds the above range, the viscosity of the aqueous dispersion of the layered clay mineral becomes excessively high and the fluidity is excessively lowered, so that the layered clay mineral cannot be uniformly and sufficiently swollen. There is a case.
In order to disperse the inorganic compound in water, water and the inorganic compound are mixed in the above-described mixing ratio, and the mixture is stirred using a known stirrer such as a disper or an ultrasonic homogenizer (described later).

  Moreover, when using a layered clay mineral as an inorganic compound, Preferably, after mix | blending water and an inorganic compound by the above-mentioned mixing | blending ratio, before stirring, for example, for 12 to 48 hours, Preferably, it is 24-36. Let stand for hours. By allowing the water containing the layered clay mineral to stand still, the layered clay mineral can be swollen. Therefore, after standing, by mixing and stirring, each layer of the layered clay mineral can be peeled off and dispersed well in water.

In this method, a liquid organic compound (hereinafter sometimes simply referred to as an organic compound) is then dispersed in the obtained aqueous dispersion of the inorganic compound, and the oil droplets of the organic compound and the inorganic compound are dispersed in water. An organic-inorganic aqueous dispersion is obtained (organic compound dispersion step).
The organic compound is not particularly limited as long as it is an organic compound that is not freely mixed with water. For example, aliphatic hydrocarbons, aromatic hydrocarbons, halogenated hydrocarbons, esters, ketones, alcohols, Examples include ethers and ethylenically unsaturated monomers.

Examples of the aliphatic hydrocarbons include n-hexane, isohexane, heptane, isoheptane, octane, isooctane, nonane, isononane, decane, dodecane, cyclopentane, cyclohexane, cyclopentane, methylcyclopentane, and methylcyclohexane. .
Examples of aromatic hydrocarbons include benzene, toluene, ethylbenzene, isopropylbenzene, butylbenzene, amylbenzene, dodecylbenzene, xylenes, diethylbenzenes, diisopropylbenzenes, cymenes, dimethylnaphthalenes, mesitylene, triethylbenzene, Examples include cyclohexylbenzene, tetralin and naphthalene.

  Examples of the halogenated hydrocarbon include methyl chloride, methylene chloride, chloroform (trichloromethane), carbon tetrachloride, 1,1-dichloroethane, 1,2-dichloroethane, hexachloroethane, trichloroethylene, tetrachloroethylene, isopropyl chloride, butyl chloride, Amyl chloride, hexyl chloride, 2-ethylhexyl chloride, dichloropropanes, dichlorobutanes, dichlorobenzenes, chlorobenzene, chlorotoluenes, dichlorotoluenes (for example, 1,2-dichlorotoluene, 2,3-dichlorotoluene, 2 , 4-dichlorotoluene, 2,5-dichlorotoluene, 2,6-dichlorotoluene, 3,4-dichlorotoluene, 3,5-dichlorotoluene, etc.), trichlorobenzenes (for example, 1,2,3-trichloroben) , 1,2,5-trichlorobenzene, etc.), naphthalene chlorides, methyl bromide, ethyl bromide, propyl bromide, isopropyl bromide, butyl bromide, octyl bromide, lauryl bromide, bromonaphthalene, bromobenzene , Dibromoethanes, dibromopropanes, dibromopentanes, dibromobenzenes, tetrabromoethane, bromochloroethane, tetramethylenechlorobromide, pentamethylenechlorobromide and the like.

  Examples of the esters include methyl formate, ethyl formate, propyl formate, butyl formate, isobutyl formate, isoamyl formate, hexyl formate, benzyl formate, methyl acetate, ethyl acetate, propyl acetate, isopropyl acetate, butyl acetate (n-butyl acetate). ), Isobutyl acetate, s-butyl acetate, amyl acetate, isoamyl acetate, 2-ethylhexyl acetate, allyl acetate, cyclohexyl acetate, methyl cyclohexyl acetate, benzyl acetate, methyl propionate, ethyl propionate, butyl propionate, isoamyl propionate, Benzyl propionate, methyl butyrate, ethyl butyrate, isopropyl butyrate, butyl butyrate, isoamyl butyrate, ethyl isovalerate, isoamyl isovalerate, ethyl stearate, butyl stearate, amyl stearate, dioxalate Chill, dibutyl oxalate, diamyl oxalate, dimethyl malonate, diethyl malonate, isopropyl malonate, dibutyl sebacate, octyl sebacate, methyl benzoate, ethyl benzoate, propyl benzoate, butyl benzoate, isoamyl benzoate, Benzyl benzoate, dimethyl phthalate, diethyl phthalate, dibutyl phthalate, dioctyl phthalate, methyl salicylate, isoamyl salicylate, benzyl salicylate, methyl lactate, ethyl lactate, butyl lactate, tributyl citrate, amyl lactate, silicate ester, maleate Dibutyl acid, dioctyl maleate, diethyl adipate, dioctyl adipate, diethyl tartrate, dibutyl tartrate, methyl acetoacetate, ethyl acetoacetate, allyl acetoacetate, triethyl acetylcitrate, acetate Rukuen acid tributyl methyl abietic acid, .gamma.-butyrolactone, dimethyl carbonate, diethyl carbonate, diphenyl carbonate, boric acid esters, and phosphoric acid esters.

  Examples of the ketones include methyl ethyl ketone, methyl-n-propyl ketone, methyl-n-butyl ketone, methyl isobutyl ketone, methyl-n-amyl ketone, methyl-n-hexyl ketone, methyl-n-heptyl ketone, ethyl butyl ketone, Examples include diethyl ketone, dipropyl ketone, diisopropyl ketone, diisobutyl ketone, cyclohexanone, and methylcyclohexanone.

  Examples of alcohols include alcohols having 4 or more carbon atoms such as n-butanol, s-butanol, n-amyl alcohol, isoamyl alcohol, s-amyl alcohol, t-amyl alcohol, 2-methyl-1-butanol, 3 -Methyl-2-butanol, n-hexanol, 2-ethylbutanol, n-heptanol, 2-heptanol, 3-heptanol, n-octanol, 2-octanol, 2-ethylhexanol, nonanol, n-decanol, undecanol, 3 , 5-dimethyl-1-hexyn-3-ol, cyclohexanol, methylcyclohexanol and the like.

Examples of ethers include diisopropyl ether, diisoamyl ether, ethyl isoamyl ether, anisole, phenetole, butyl phenyl ether, ethyl benzyl ether, cresyl methyl ether, diphenyl ether, dibenzyl ether, furan, methyl furan, and monochlorodiethyl ether. Is mentioned.
Examples of the ethylenically unsaturated monomer include (meth) acrylic acid alkyl esters (for example, methyl (meth) acrylate, ethyl (meth) acrylate, propyl (meth) acrylate, isopropyl (meth) acrylate, ( (Meth) butyl acrylate (butyl acrylate, etc.), vinyl ester group-containing monomers (eg vinyl acetate, etc.), aromatic unsaturated monomers (eg styrene, vinyl toluene, etc.), (meth) acrylic alicyclic hydrocarbons Ester monomers (for example, cyclopentyl di (meth) acrylate, isobornyl (meth) acrylate, etc.), alkoxy group-containing unsaturated monomers (for example, methoxyethyl (meth) acrylate, ethoxyethyl (meth) acrylate), olefin monomers (Eg, ethylene, pro Ene, isoprene, butadiene, isobutylene, etc.), vinyl ether monomers (for example, vinyl ether), halogen atom-containing unsaturated monomers (for example, vinyl chloride, etc.), acrylic acid ester monomers that contain heterocycles and / or halogen atoms ( For example, (meth) acrylic acid tetrahydrofurfuryl, fluorine (meth) acrylate, and the like.

Moreover, as an organic compound, the mixture (for example, petroleum-based solvent (mineral spirit) etc.) mentioned above is also contained.
These organic compounds can be used alone or in combination of two or more.
Preferred examples of the organic compound include aliphatic hydrocarbons, aromatic hydrocarbons, esters, ketones, and ethylenically unsaturated monomers.

By appropriately selecting the organic compound, the size of the pores in the obtained inorganic porous material can be controlled.
That is, when an organic compound having a large polarity (for example, ethyl acetate, methyl isobutyl ketone, etc.) is used, since the interfacial tension between the organic compound and water is small, oil droplets generated by the organic compound can be reduced. The pores in the resulting inorganic porous body can be reduced. In addition, when an organic compound having a small polarity (for example, toluene, xylene, chloroform, etc.) is used, since the interfacial tension between the organic compound and water is large, oil droplets generated by the organic compound can be enlarged and thus obtained. The pores in the inorganic porous body can be enlarged.

In the organic compound dispersion step, the inorganic compound in the aqueous dispersion of the inorganic compound is, for example, 0.1 to 300 parts by weight, preferably 1 to 200 parts by weight, more preferably 100 parts by weight of the organic compound. The aqueous dispersion of the inorganic compound and the organic compound are blended at a ratio of 10 to 100 parts by weight.
In the organic compound dispersion step, in order to disperse the organic compound in the aqueous dispersion of the inorganic compound, the organic compound and the aqueous dispersion of the inorganic compound are blended at the blending ratio described above and stirred using a stirrer.

  Examples of the stirrer include an ultrasonic homogenizer (for example, GSCVP-600, manufactured by Ginsen), a high-pressure homogenizer (for example, PANDA 2K, manufactured by NIRO-SOAVI), a microfluidizer (manufactured by Microfluidics), and a nanomizer (Yoshida Machine). Kogyo Co., Ltd.), TK homomixer (Primics Co., Ltd.), TK film mix (Primics Co., Ltd.), etc. can be used.

When an ultrasonic homogenizer is used as the stirring device, oil droplets of the organic compound are refined by a cavitation effect caused by ultrasonic irradiation.
When an ultrasonic homogenizer is used as the stirring device, the frequency of the ultrasonic wave used is not particularly limited, and is, for example, 20 to 40 kHz.
When a high-pressure homogenizer, microfluidizer or nanomizer is used as an agitator, the aqueous dispersion of the inorganic compound is pressurized while being discharged from the micropores. Oil droplets are refined.

When a high-pressure homogenizer, microfluidizer, or nanomizer is used as the stirring device, the pressure at the time of pressurization is not particularly limited, and is, for example, 10 to 300 MPa, preferably 50 to 150 MPa.
As a stirring device, a TK homomixer or a TK fill mix is a stirring device that utilizes the high-speed rotation of a rotating body. When the rotating body rotates at a high speed in a mixed solution, a high shearing force is applied to the mixed solution, and organic The oil droplets of the compound are refined.

These stirring devices can be used singly or in combination of two or more kinds (multistage).
As an agitator, Preferably, an ultrasonic homogenizer, a nanomizer, and TK homomixer are mentioned.
In the method for producing an inorganic porous body of the present invention, a hydrophobic compound and / or a hydrophobic inorganic compound having a bulk shape, a needle shape, or a plate shape (excluding a layer shape) is blended in the organic compound dispersion step. be able to.

  Hydrophobic compounds are, for example, hydrophobic organic compounds that are not readily compatible with water, such as higher alkanes having 8 to 30 carbon atoms (for example, dodecane, hexadecane, octadecane, etc.), alkyl groups having 8 to 30 carbon atoms. Higher alcohols (eg, lauryl alcohol, cetyl alcohol, stearyl alcohol), alkyl (meth) acrylates having an alkyl group having 8 to 30 carbon atoms (eg, lauryl (meth) acrylate, stearyl (meth) acrylate, etc.) ), Thiols having an alkyl group having 8 to 30 carbon atoms (for example, lauryl mercaptan, cetyl mercaptan, stearyl mercaptan, etc.), hydrophobic polymers and oligomers (for example, polystyrene, polymethyl (meth) acrylate, polybutadiene, poly (α − Methylstyrene), butadiene - styrene block copolymer, rosin ester), and the like.

These hydrophobic compounds can be used alone or in combination of two or more.
The hydrophobic compound is preferably higher alkanes, more preferably hexadecane.
A hydrophobic compound is mix | blended with the organic compound before mix | blending with the aqueous dispersion liquid of an inorganic compound, for example. The compounding ratio of the hydrophobic compound is, for example, 1 to 80 parts by weight, preferably 1 to 60 parts by weight with respect to 100 parts by weight of the organic compound.

By blending the hydrophobic compound, the oil droplets of the organic compound can be adjusted to an appropriate size by suppressing the oil droplets from becoming too fine.
Hydrophobic inorganic compounds exhibit a hydrophobic property that is not readily compatible with water.
The bulk-form hydrophobic inorganic compound includes, for example, a spherical inorganic shape, a rectangular parallelepiped shape, or a hydrophobic inorganic compound having an irregular shape thereof. Examples of the bulk-form hydrophobic inorganic compound include silica, calcium carbonate, titanium oxide, tin oxide (including antimony-doped tin oxide), alumina, magnesium hydroxide, barium titanate, zinc oxide, silicon nitride, and metal fine particles. Etc.

Examples of the needle-shaped hydrophobic inorganic compound include potassium titanate, wollastonite, sepiolite, acicular tin oxide, acicular magnesium hydroxide, and the like.
The plate-shaped hydrophobic inorganic compound is a plate-shaped hydrophobic inorganic compound excluding the layer-shaped hydrophobic inorganic compound, and examples thereof include boron nitride, plate-like calcium carbonate, and plate-like aluminum hydroxide.

As the hydrophobic inorganic compound, for example, commercially available products can be generally used. Specifically, as silica, Aerosil series (manufactured by Nippon Aerosil Co., Ltd.) and the like, for example, as titanium oxide, TTO series (manufactured by Ishihara Sangyo Co., Ltd.) Etc.
Examples of the Aerosil series include Aerosil R8200 (fumed silica, primary particle diameter 12 nm, hexamethyldisilazane treatment), Aerosil R104 (fumed silica, primary particle diameter 12 nm, octamethylcyclotetrasiloxane treatment), Aerosil R974. (Fumed silica, primary particle diameter 12 nm, dimethyldichlorosilane treatment), Aerosil R812 (fumed silica, primary particle diameter 7 nm, hexamethyldisilazane treatment) or the like is used. Examples of the TTO series include TTO-51 (C) (primary particle diameter of 10 to 30 nm, aluminum hydroxide / stearic acid treatment), TTO-55 (C) (primary particle diameter of 30 to 50 nm, aluminum hydroxide / Stearic acid treatment), TTO-55 (D) (primary particle diameter 30-50 nm, aluminum hydroxide / zirconium oxide treatment), etc. are used.

The size of the hydrophobic inorganic compound is, for example, 1 to 200 nm, preferably 5 to 150 nm, as the primary average particle diameter (the maximum length in the case of needles or plates).
When the size exceeds the above range, the hydrophobic inorganic compound may not be completely encapsulated in the oil droplets.
The hydrophobic inorganic compound is blended, for example, in the organic compound before blending in the aqueous dispersion of the inorganic compound. The blending ratio of the hydrophobic inorganic compound is, for example, 0.1 to 15 parts by weight, preferably 0.5 to 10 parts by weight with respect to 100 parts by weight of the organic compound. When the blending ratio of the hydrophobic inorganic compound exceeds the above range, the viscosity of the organic-inorganic aqueous dispersion may increase excessively and viscosity adjustment may be required.

By blending the hydrophobic inorganic compound, the hydrophobic inorganic compound can be encapsulated inside the basic skeleton of the inorganic compound in the inorganic porous body.
Moreover, in the manufacturing method of the inorganic porous body of this invention, surfactant can be mix | blended in an inorganic compound dispersion | distribution process and / or an organic compound dispersion | distribution process.
Examples of the surfactant include a dispersant (for example, a polymer dispersant) and an emulsifier (for example, an anionic non-reactive emulsifier).

These surfactants can be used alone or in combination of two or more.
In the inorganic compound dispersion step, preferably, the dispersant is water (water before blending the inorganic compound or water before blending after the inorganic compound is blended) and / or inorganic compound. It can mix | blend with an aqueous dispersion liquid.
By mixing the dispersant in water, the primary particles of the inorganic compound can be dispersed.

Also, by blending the dispersant into the aqueous dispersion of the inorganic compound, the dispersibility of the inorganic compound in the aqueous dispersion of the inorganic compound can be improved, so that the viscosity of the aqueous dispersion of the inorganic compound is reduced. The solid concentration of the organic-inorganic aqueous dispersion can be easily adjusted within a certain range.
In the organic compound dispersion step, preferably, an emulsifier can be added to the organic compound and / or the organic-inorganic aqueous dispersion.

A stable organic-inorganic aqueous dispersion can be obtained by blending the emulsifier into the organic compound and / or the organic-inorganic aqueous dispersion.
The compounding ratio of the surfactant is, for example, 0.01 to 20 parts by weight, preferably 0.05 to 15 parts by weight with respect to 100 parts by weight of the inorganic compound.
In the method for producing an inorganic porous body of the present invention, for example, a binder such as a polymer or an oligomer is added to any of water, an aqueous dispersion of an inorganic compound, an organic compound, and an organic-inorganic aqueous dispersion. be able to.

When the binder is blended with the aqueous dispersion of the inorganic compound, the binder is preferably added to the aqueous dispersion of the inorganic compound and dissolved.
In such a case, the binder preferably includes a water-soluble polymer, a water-soluble oligomer, an emulsion of a water-insoluble polymer, and the like. More preferably, a water-soluble polymer is mentioned, and an emulsion of a water-insoluble polymer is also mentioned.

Examples of the water-soluble polymer include polyacrylic acid, acrylic acid / maleic acid copolymer, polyurethane, polyvinyl alcohol, cellulose (for example, carboxymethyl cellulose), nylon, and the like.
Moreover, a commercial item can also be used as a water-soluble polymer.
Commercially available water-soluble polymers include, for example, Aquaric series (polyacrylic acid or acrylic acid / maleic acid copolymer, manufactured by Nippon Shokubai Co., Ltd.), Aron series (polyacrylic acid, manufactured by Toagosei Co., Ltd.), Roll series (polyacrylic acid, manufactured by Daiichi Kogyo Seiyaku Co., Ltd.), Gohsenol (polyvinyl alcohol, manufactured by Nippon Synthetic Chemical Industry Co., Ltd.), Kuraray Poval (polyvinyl alcohol, manufactured by Kuraray Co., Ltd.), Metroles (Cellroll, manufactured by Shin-Etsu Chemical Co., Ltd.), etc. Is mentioned.

These water-soluble polymers can be used alone or in combination of two or more.
Examples of the water-insoluble polymer include polyurethane, acrylic, polytetrafluoroethylene, and the like.
As the water-insoluble polymer emulsion, for example, a general commercial product can be used. Specifically, as the polyurethane emulsion (polyurethane dispersion), for example, the Superflex series (ether type polyurethane emulsion, water-insoluble , Manufactured by Daiichi Kogyo Seiyaku Co., Ltd.), Hydran series (polyurethane emulsion, water-insoluble, manufactured by DIC) and the like, and polytetrafluoroethylene emulsion such as, for example, Fullon AD938L (produced by Asahi Glass Co., Ltd.). It is done.

The water-insoluble polymer emulsions can be used alone or in combination of two or more.
Moreover, when mix | blending a binder with an organic compound, for example, Preferably, a binder is added and dissolved in an organic compound.
In such a case, the binder is preferably an oil-soluble polymer or an oil-soluble oligomer, and more preferably an oil-soluble polymer.

  Examples of the oil-soluble polymer include polyolefin polymers (eg, polyethylene, polybutylene, polypropylene, poly (α-olefin)), polyvinyl polymers (eg, polyvinyl chloride, polyvinylpyrene, polymethyl methacrylate, polybutyl acrylate, Polybutyl acrylate, polystyrene, diene polymers (eg, polybutadiene, polyisoprene, polychloroprene, etc.), cellulose diacetate, cellulose triacetate, ethyl cellulose, cellulose acetate phthalate, and block copolymers or random copolymers of the above polymers Examples include coalescence.

These oil-soluble polymers can be used alone or in combination of two or more.
When these binders are mix | blended, in an inorganic porous body, joining between inorganic compounds will be strengthened. Therefore, the self-supporting film | membrane of an inorganic porous body can be formed by mix | blending a binder.
The blending ratio of the binder is, for example, 5 to 200 parts by weight, preferably 10 to 80 parts by weight with respect to 100 parts by weight of the inorganic compound.

In this method, water and a liquid organic compound are then removed from the obtained organic-inorganic aqueous dispersion (removal step).
The method for removing water and the liquid organic compound is not particularly limited, and for example, dry removal by heating can be performed. Thereby, an inorganic porous body can be obtained.
In the case of performing drying and removal by heating, the heating temperature is, for example, 40 to 250 ° C., preferably 70 to 200 ° C., and the heating time is, for example, 0.1 to 4 hours, preferably 0.5 ~ 3 hours.

When the heating temperature is less than the above range, evaporation at room temperature proceeds, the composition variation needs to be remarkably adjusted, and workability may be reduced, and the heating temperature exceeds the above range. In some cases, productivity may decrease.
Moreover, it can also bake after the above-mentioned heating according to the objective and a use. A calcination temperature is 250-1300 degreeC, for example, Preferably, it is 260-1200 degreeC, and a calcination time is 1 to 60 minutes, for example, Preferably, it is 1 to 30 minutes.

Hereinafter, the present invention will be described more specifically with reference to examples and comparative examples. However, the present invention is not limited to the examples and comparative examples. In the following description, “parts” and “%” are based on weight unless otherwise specified.
Example 1
(Preparation of organic-inorganic dispersion)
100 parts by weight of decane as an organic compound and 5 parts by weight of hexadecane as a hydrophobic compound were mixed to prepare an oil phase mixture.

  On the other hand, it was added to 50 parts by weight of Lucentite SWN (inorganic compound (layered clay mineral), manufactured by Corp Chemical Co.) and 882 parts by weight of water, and allowed to stand for 24 hours. Here, Charol AN-103P (surfactant (polymer dispersing agent), manufactured by Daiichi Kogyo Seiyaku Co., Ltd.) was added in an amount of 1.25 parts by weight in terms of solid content, and an ultrasonic homogenizer (GSCVP-600, manufactured by Ginsen) Was stirred for 3 minutes to obtain an aqueous dispersion of layered clay mineral.

Next, the oil phase mixture (105 parts by weight) and the aqueous dispersion of layered clay mineral (solid content 50 parts by weight) were mixed and stirred for 1 minute at 6000 min ⁻¹ using a homogenizer (manufactured by Primics). An organic-inorganic composite liquid was prepared.
Thereafter, the organic-inorganic composite liquid was subjected to a 2-pass treatment at a pressure of 100 MPa using a nanomizer (manufactured by Yoshida Kikai Kogyo Co., Ltd.) to prepare an organic-inorganic aqueous dispersion.

(Preparation of inorganic porous material)
The obtained organic-inorganic aqueous dispersion was dropped onto an aluminum container and dried at 100 ° C. for 1 hour in a hot air circulation oven. Thereafter, it was further dried at 180 ° C. for 1 hour, and the oil phase mixture (organic compound and hydrophobic compound) and water were sufficiently removed to obtain an inorganic porous body.
Example 2
Inorganic porous material in the same manner as in Example 1, except that 0.1 part by weight of Lucentite SWN, 593 parts by weight of water, and 0.0025 part by weight of Charol AN-103P in terms of solid content were used. Got.

Example 3
An inorganic porous material was obtained in the same manner as in Example 1 except that Lucentite SWN was 300 parts by weight, water was 4646 parts by weight, and Charol AN-103P was 7.5 parts by weight in terms of solid content. It was.
Example 4
An organic-inorganic aqueous dispersion was prepared in the same manner as in Example 1 except that n-hexane was used in place of decane as the organic compound.

The obtained organic-inorganic water dispersion was dropped on an aluminum container and dried at 70 ° C. for 1 hour in a hot air circulation oven to sufficiently remove the oil phase mixture and water, thereby obtaining an inorganic porous body. .
Example 5
An organic-inorganic aqueous dispersion was prepared in the same manner as in Example 1 except that toluene was used in place of decane as the organic compound.

The obtained organic-inorganic aqueous dispersion was dropped onto an aluminum container and dried at 100 ° C. for 1 hour in a hot air circulation oven. Thereafter, it was further dried at 120 ° C. for 1 hour, and the oil phase mixture and water were sufficiently removed to obtain an inorganic porous body.
Example 6
An organic-inorganic aqueous dispersion was prepared in the same manner as in Example 1 except that xylene was used in place of decane as the organic compound.

The obtained organic-inorganic aqueous dispersion was dropped onto an aluminum container and dried at 100 ° C. for 1 hour in a hot air circulation oven. Thereafter, it was further dried at 140 ° C. for 1 hour, and the oil phase mixture and water were sufficiently removed to obtain an inorganic porous body.
Example 7
An organic-inorganic aqueous dispersion was prepared in the same manner as in Example 1 except that dodecane was used in place of decane as the organic compound.

The obtained organic-inorganic aqueous dispersion was dropped onto an aluminum container and dried at 100 ° C. for 1 hour in a hot air circulation oven. Then, it was further dried at 200 ° C. for 1 hour, and the oil phase mixture and water were sufficiently removed to obtain an inorganic porous body.
Example 8
An organic-inorganic aqueous dispersion was prepared in the same manner as in Example 1 except that ethyl acetate was used in place of decane as the organic compound.

The obtained organic-inorganic water dispersion was dropped on an aluminum container and dried at 80 ° C. for 1 hour in a hot air circulation oven to sufficiently remove the oil phase mixture and water, thereby obtaining an inorganic porous body. .
Example 9
An organic-inorganic aqueous dispersion was prepared in the same manner as in Example 1 except that methyl isobutyl ketone was used in place of decane as the organic compound.

The obtained organic-inorganic aqueous dispersion was dropped onto an aluminum container and dried at 100 ° C. for 1 hour in a hot air circulation oven. Thereafter, it was further dried at 120 ° C. for 1 hour, and the oil phase mixture and water were sufficiently removed to obtain an inorganic porous body.
Example 10
An organic-inorganic aqueous dispersion was prepared in the same manner as in Example 1 except that butyl acetate was used in place of decane as the organic compound.

The obtained organic-inorganic aqueous dispersion was dropped onto an aluminum container and dried at 100 ° C. for 1 hour in a hot air circulation oven. Then, it was further dried at 130 ° C. for 1 hour, and the oil phase mixture and water were sufficiently removed to obtain an inorganic porous body.
Example 11
An organic-inorganic aqueous dispersion was prepared in the same manner as in Example 1 except that butyl acrylate was used in place of decane as the organic compound.

The obtained organic-inorganic aqueous dispersion was dropped onto an aluminum container and dried at 100 ° C. for 1 hour in a hot air circulation oven. Thereafter, it was further dried at 180 ° C. for 1 hour, and the oil phase mixture and water were sufficiently removed to obtain an inorganic porous body.
Example 12
An organic-inorganic aqueous dispersion was prepared in the same manner as in Example 1 except that n-hexane was used instead of decane as the organic compound and no hydrophobic compound was added.

The obtained organic-inorganic water dispersion was dropped on an aluminum container and dried at 70 ° C. for 1 hour in a hot air circulation oven to sufficiently remove the oil phase mixture and water, thereby obtaining an inorganic porous body. .
Example 13
(Surface treatment of inorganic compounds)
30 parts by weight of SN-100S (antimony-doped tin oxide aqueous dispersion, solid concentration 17.9% by weight, manufactured by Ishihara Sangyo Co., Ltd.) and 256 parts by weight of water (including water in SN-100S) 4.5 parts by weight of KBM-503 (3-methacryloxypropyl-trimethoxysilane, manufactured by Shin-Etsu Chemical Co., Ltd.), and then adjusted to pH 4.0 with a 5% aqueous acetic acid solution at room temperature. The mixture was stirred for a time to obtain an aqueous dispersion of the surface-treated inorganic compound (surface-treated antimony-doped tin oxide).

Before blending the organic compound, 3 parts by weight of Charol AN-103P (polymer dispersant (polycarboxylic acid dispersant), manufactured by Daiichi Kogyo Seiyaku Co., Ltd.) and Haitenol LA-16 (anionic non-reactive) 0.05 parts by weight of a functional emulsifier (Daiichi Kogyo Seiyaku Co., Ltd.)
(Preparation of organic-inorganic aqueous dispersion)
100 parts by weight of butyl acrylate as an organic compound and 3 parts by weight of hexadecane as a hydrophobic compound were mixed to prepare an oil phase mixture.

Next, an oil phase mixture (103 parts by weight) and a surface-treated inorganic dispersion of an inorganic compound (solid content 30 parts by weight) were mixed, and stirred for 1 minute at 6000 min ⁻¹ using a homogenizer. -An inorganic composite solution was prepared.
Thereafter, the organic-inorganic composite liquid was subjected to a two-pass treatment using a nanomizer at a pressure of 100 MPa to prepare an organic-inorganic aqueous dispersion.

(Preparation of inorganic porous material)
The obtained organic-inorganic aqueous dispersion was dropped onto an aluminum container and dried at 100 ° C. for 1 hour in a hot air circulation oven. Thereafter, it was further dried at 180 ° C. for 1 hour, and the oil phase mixture and water were sufficiently removed to obtain an inorganic porous body.
Example 14
50 parts by weight of BT-HP100 (barium titanate, manufactured by Kyoritsu Material Co., Ltd.) and 886 parts by weight of water were stirred and dispersed with an ultrasonic homogenizer, and 1.8 parts by weight of KBM-503 was added thereto at room temperature. The mixture was stirred for 20 hours to obtain an aqueous dispersion of the surface-treated inorganic compound (surface-treated barium titanate).

Before blending the organic compound, 2.5 parts by weight of Charol AN-103P was added.
(Preparation of organic-inorganic aqueous dispersion)
100 parts by weight of butyl acrylate as an organic compound and 5 parts by weight of hexadecane as a hydrophobic compound were mixed to prepare an oil phase mixture.

Next, an oil phase mixture (105 parts by weight) and a surface-treated inorganic dispersion of an inorganic compound (solid content 50 parts by weight) were mixed, and stirred for 1 minute at 6000 min ⁻¹ using a homogenizer. -An inorganic composite solution was prepared.
Thereafter, the organic-inorganic composite liquid was subjected to a two-pass treatment using a nanomizer at a pressure of 100 MPa to prepare an organic-inorganic aqueous dispersion.

(Preparation of inorganic porous material)
The obtained organic-inorganic aqueous dispersion was dropped onto an aluminum container and dried at 100 ° C. for 1 hour in a hot air circulation oven. Thereafter, it was further dried at 180 ° C. for 1 hour, and the oil phase mixture and water were sufficiently removed to obtain an inorganic porous body.
Example 15
20 parts by weight of carboxymethyl cellulose (CMC) as a water-soluble polymer was dissolved in 780 parts by weight of water to prepare an aqueous solution of the water-soluble polymer.

  Next, an aqueous solution of a water-soluble polymer was added to the organic-inorganic water dispersion prepared in the same manner as in Example 1, mixed and stirred, and the organic-inorganic water dispersion to which the aqueous solution of the water-soluble polymer was added was converted into an aluminum container. It was dripped on and it was made to dry at 100 degreeC by the hot air circulation type oven for 1 hour. Then, it was further dried at 180 ° C. for 1 hour, and the oil phase mixture and water were sufficiently removed to obtain a self-supporting sheet (self-supporting film) of the inorganic porous material.

Example 16
Polyurethane emulsion as a binder (Superflex 460, emulsion of water-insoluble ester polyurethane, solid concentration 38%, manufactured by Daiichi Kogyo Seiyaku Co., Ltd.) 52.6 wt.% In the organic-inorganic composite liquid before stirring with Nanomizer An inorganic porous material was obtained in the same manner as in Example 1 except that 20 parts by weight (as solid content) was blended.

Example 17
In the preparation of the organic-inorganic dispersion, the organic-inorganic composite liquid before stirring with the nanomizer is added to the polytetrafluoroethylene emulsion as a binder (trade name: Fullon AD938L, solid content concentration 60%, manufactured by Asahi Glass Co., Ltd.) 33.3. Except for blending parts by weight (20 parts by weight as a solid content), an organic-inorganic aqueous dispersion was obtained in the same manner as in Example 1, and in the production of the inorganic porous body, after drying at 180 ° C., Furthermore, an inorganic porous material was obtained in the same manner as in Example 1 except that baking was performed at 260 ° C. for 1 minute and then baking was performed at 360 ° C. for 3 minutes.

Example 18
In preparation of an organic-inorganic dispersion, 100 parts by weight of toluene as an organic compound, 5 parts by weight of hexadecane as a hydrophobic compound, and a styrene block copolymer as a binder (trade name: Kraton G1650, manufactured by Shell) 20 An organic-inorganic aqueous dispersion was prepared in the same manner as in Example 15 except that an oil phase mixture was prepared by mixing with parts by weight, and subsequently an organic-inorganic composite liquid was prepared. Thereafter, an inorganic porous material was obtained in the same manner as in Example 15.

Example 19
In the preparation of the organic-inorganic dispersion, 100 parts by weight of decane as an organic compound and 5 parts by weight of hexadecane as a hydrophobic compound were mixed to prepare a mixed liquid. Aerosil R8200 (fumed silica, 1 Next particle diameter 12 nm, hexamethyldisilazane treatment, manufactured by Nippon Aerosil Co., Ltd.) 10 parts is added and mixed to prepare an oil phase mixture, and then an organic-inorganic composite liquid is prepared in the same manner as in Example 1. Except that, an inorganic porous material was obtained in the same manner as in Example 1.

Comparative Example 1
(Preparation of aqueous dispersion)
50 parts by weight of Lucentite SWN was added to 851 parts by weight of water and allowed to stand for 24 hours. Here, 2.5 parts by weight of Charol AN-103P was added as a solid content and treated with an ultrasonic homogenizer for 3 minutes to obtain an aqueous dispersion of a layered clay mineral.

(Removal process)
The obtained aqueous dispersion of layered clay mineral was dropped onto an aluminum container and dried in a hot air circulation oven at 100 ° C. for 1 hour to sufficiently remove water, thereby obtaining an inorganic compound.
In the obtained inorganic compound, pores were not formed, and it was confirmed that silicate was laminated.

  Tables 1 and 2 show the formulation of each component in each example and comparative example.

The details of the abbreviations and trade names in Table 1 are shown below.
MIBK: organic compound, methyl isobutyl ketone BA: organic compound, butyl acrylate Lucentite SWN: inorganic compound, layered clay mineral (layered silicate), manufactured by Co-op Chemical Co., Ltd. ATO: inorganic compound, antimony-doped tin oxide (solid content)
Charol AN-103P: surfactant, polymer dispersed (polycarboxylic acid polymer dispersant), manufactured by Daiichi Kogyo Seiyaku Co., Ltd. KBM503: surface treatment agent, 3-methacryloxypropyl-trimethoxysilane, Shin-Etsu Chemical Co., Ltd. Manufactured LA-16: Surfactant, Hytenol LA-16, Emulsifier (Anionic non-reactive emulsifier), Daiichi Kogyo Seiyaku CMC: Binder, Water-soluble polymer, Carboxymethylcellulose Aerosil R8200: Hydrophobic inorganic compound, Hume Dosilica, primary particle size 12 nm, hexamethyldisilazane treatment, manufactured by Nippon Aerosil Co., Ltd. polyurethane: binder, polyurethane emulsion (water-insoluble emulsion), trade name: Superflex 460, solid content concentration 38%, Daiichi Kogyo Seiyaku PTFE: Binder, polytetrafluor Loethylene emulsion (non-water-soluble emulsion), trade name: Fullon AD938L, solid content concentration 60%, manufactured by Asahi Glass Co., Ltd. SEBS: binder, styrene block copolymer, trade name: Kraton G1650, manufactured by Shell, Inc. <SEM observation >
After fixing the inorganic porous material obtained by Examples 1-4, 12 and 16-19 to the SEM sample stand with a carbon tape and performing copper vapor deposition by ion sputtering (E101, manufactured by HITACHI), SEM Hitachi The cross section was observed with a scanning electron microscope (S-570, manufactured by HITACHI) at an acceleration voltage of 10 kV.

The inorganic porous body obtained in Examples 9 and 13 and the inorganic compound obtained in Comparative Example 1 were sampled by a direct method after cleaving the inorganic porous body and the inorganic compound at room temperature, and osmium After coating, the cross section was observed with an FE-SEM (JSM-7500F, manufactured by JEOL) at an acceleration voltage of 3 kV.
The image processing figure of the electron micrograph is shown in FIGS.

Claims (6)

An inorganic compound dispersion step of dispersing the inorganic compound in water to obtain an aqueous dispersion of the inorganic compound;
An organic compound dispersion step of dispersing a liquid organic compound in the aqueous dispersion of the inorganic compound to obtain an organic-inorganic aqueous dispersion;
And a removal step of removing the water of the organic-inorganic water dispersion and the liquid organic compound.   The method for producing an inorganic porous body according to claim 1, wherein a hydrophobic compound is blended in the organic compound dispersion step.   The method for producing an inorganic porous body according to claim 1 or 2, wherein in the organic compound dispersing step, a bulk-like, needle-like or plate-like hydrophobic inorganic compound is blended.   In the said inorganic compound dispersion | distribution process and / or the said organic compound dispersion | distribution process, surfactant is mix | blended, The manufacturing method of the inorganic porous body in any one of Claims 1-3 characterized by the above-mentioned.   A binder is blended in any of the water, the aqueous dispersion of an inorganic compound, the liquid organic compound, and the organic-inorganic aqueous dispersion. The manufacturing method of the inorganic porous body of description.   An inorganic porous body obtained by the method for producing an inorganic porous body according to any one of claims 1 to 5.