JP2009084132A - Modified clay mineral powder, and method for producing the same - Google Patents

Abstract

<P>PROBLEM TO BE SOLVED: To provide modified clay mineral powder whose specific surface area is increased for easily achieving the addition of the other substance having functionality by modifying the surface region of clay mineral powder, and to provide a method for producing the modified clay mineral powder. <P>SOLUTION: Clay mineral powder 12 and an alkali agent are heated in a mixed state, thus the surface region of the clay mineral powder 12 is modified, so as to form a porous gelled region 14. Further, the gelled region 14 may be removed by using water or an acidic solution. <P>COPYRIGHT: (C)2009,JPO&INPIT

Description

  In the present invention, by using an alkali agent, the surface condition of clay mineral powder such as mica or talc is modified to greatly improve the specific surface area, and for example, functional substances that express various functions can be easily provided. The present invention relates to a modified clay mineral powder and a method for producing the same.

Clay minerals such as mica (mica), talc, kaolinite (kaolin) and montmorillonite have many reserves near the surface of the earth, and since they are easy to process, they have been used for various purposes since ancient times. The range of use is extremely diverse. Mica is commonly referred to as “thousand peel” and has a specific layered laminated structure that is easily peeled into fine scales and has good characteristics such as slipperiness, elasticity, electrical insulation and heat resistance. In addition, it is known as a physically and chemically stable substance. On the other hand, talc is commonly called “talc” or “soapstone” because it is a very soft mineral with a Mohs hardness of 1 and has good sliding properties. Also, the talc structure is layered, although not as pronounced as mica. Furthermore, kaolinite is a hydrated silicate mineral of aluminum (Al ₂ Si ₂ O ₅ (OH) ₄ ), and is well known as a porcelain material because of its high water absorption and excellent adhesion. In recent years, these clay minerals have been used taking advantage of their respective characteristics as cosmetic materials such as foundations.

Since the main component of these clay minerals is silicon dioxide (SiO ₂ ), as described above, while being physically and chemically very stable, modification with other substances is difficult, that is, physical with other substances.・ There is an inherent problem that chemical bonding is weak. In particular, mica has such a high smoothness that the cleaved surface can be used as an atomic force microscope (AFM) substrate, and it can be used in a wide range of applications by adding other substances. Usage is limited.

  In addition to mica, clay minerals such as talc and kaolinite are generally physically and chemically stable, and as mentioned above, physical and chemical modification is difficult. Since it cannot be said that adsorption and adhesion of substances are easy, its use is limited like mica. As one of the means for adhering such other substances, for example, a titanium oxide thin film is formed on the mica surface to form titanium mica, and the surface of the clay mineral and the other substances are subjected to extremely slow conditions. A chemical reaction method has been implemented. However, since such a process has a problem that costs are very high, it is used only in some fields with high added value such as cosmetics and cannot be said to be a general-purpose means.

  For example, muscovite powder is suitably used as a raw material for cosmetics such as a foundation due to the tactile sensation derived from good slipperiness and high whiteness, but has a problem that foundation molding does not work well due to high elasticity. This problem can be addressed by adding fats and oils, but clay mineral powders such as muscovite are difficult to adsorb and adhere to chemical substances as described above, and therefore fats and oils are required in excess. As a result, the moisturizing (water retaining) property due to the increase in hydrophobicity deteriorates, and because of the high transparency of muscovite, the color tone becomes darker when oil is absorbed, so-called `` mica dullness '' occurs, etc. The problem was inherent.

  That is, the present invention has been proposed in order to suitably solve these problems inherent in the conventional clay mineral powder and the method for producing the same, and modifies the surface area of the clay mineral powder. Thus, to provide a modified clay mineral powder having an increased specific surface area so as to easily impart other substances having functionality, and a method for producing the modified clay mineral powder. Objective.

In order to overcome the above-mentioned problems and achieve the intended purpose, the modified clay mineral powder according to the invention of claim 1 comprises:
The surface region of the clay mineral powder is a porous gelling region.
Therefore, according to the invention according to claim 1, since the surface of the clay mineral powder such as mica or talc is a porous gelation region, the functions such as elasticity and flexibility inherent in the clay mineral are impaired. In addition, a functional substance or the like that exhibits a required function can be suitably imparted.

In order to overcome the above-mentioned problems and achieve the intended purpose, the modified clay mineral powder according to the invention of claim 2 comprises:
By heating the clay mineral powder and the alkaline agent in a mixed state, the surface region of the clay mineral powder is modified to become a porous gelling region.
Therefore, according to the invention of claim 2, since the surface of the clay mineral powder such as mica or talc is modified to form a porous gelled region, the elasticity and flexibility inherent in the clay mineral are obtained. Such a functional substance that does not impair the function and develops the required function can be suitably imparted.

The gist of the invention described in claim 3 is that the alkaline agent is removed after heating.
Therefore, according to the invention of claim 3, the obtained modified clay mineral powder is neutralized, so that the handleability is improved.

In order to overcome the above-mentioned problems and achieve the intended purpose, the modified clay mineral powder according to the invention of claim 4 comprises:
By heating the clay mineral powder and the alkali agent in a mixed state, the surface region of the clay mineral powder is modified to form a gel region, and then the gel region is removed to remove the heated clay mineral powder. The specific surface area of the surface is 1.5 times or more that before heating.
Therefore, according to the invention according to claim 4, since the surface of the clay mineral powder such as mica or talc is uneven, and the specific surface area is increased, the elasticity and flexibility inherent in the clay mineral are obtained. A functional substance or the like that exhibits a required function without impairing the function can be suitably imparted.

The gist of the invention described in claim 5 is that the gelled region is removed together with the alkaline agent by an acidic solution.
Therefore, according to the invention which concerns on Claim 5, since removal of an alkaline agent is achieved simultaneously and the obtained modified clay mineral powder is neutralized, handling property improves.

The gist of the invention described in claim 6 is that a dispersing agent and / or a buffering agent is added after the alkaline agent is removed.
Therefore, according to the invention which concerns on Claim 6, aggregation of the modified clay mineral powder obtained by heating and the fluctuation | variation of pH can be prevented.

The gist of the invention described in claim 7 is that sodium hexametaphosphate or sodium tetrapolyphosphate is used as the dispersant.
Therefore, according to the invention of claim 7, since the buffer action is small and inexpensive sodium hexametaphosphate or sodium tetrapolyphosphate is used, it is preferable and easy to prevent aggregation of the modified clay mineral powder obtained by heating. Can be achieved.

The gist of the invention described in claim 8 is that a phosphate compound is used as the buffer.
Therefore, according to the invention according to claim 8, since a phosphoric acid-based compound that exhibits a buffering action in a wide pH range and is inexpensive is used, the pH variation of the modified clay mineral powder obtained by heating is prevented. Can be achieved suitably and easily.

The gist of the invention according to claim 9 is that the mixed clay mineral powder and alkali agent are heated in a range of 550 to 1300 ° C.
Therefore, according to the invention which concerns on Claim 9, regardless of the kind of clay mineral powder, a clay mineral powder can be modified | reformed suitably.

The gist of the invention described in claim 10 is that the mixing amount of the alkali agent is in the range of 5 to 30 parts by weight when the total amount of the clay mineral powder and the alkali agent is 100 parts by weight. .
Therefore, according to the invention which concerns on Claim 10, the thickness of the gelatinization area | region formed by modification | reformation is controllable.

The gist of the invention described in claim 11 is that an alkali metal hydroxide, carbonate or bicarbonate is used as the alkali agent.
Therefore, according to the invention according to claim 11, since the hydroxide, carbonate or hydrogen carbonate having good handleability is used, the modification of the clay mineral powder can be easily achieved.

The gist of the invention described in claim 12 is that sodium, potassium or lithium is used as the alkali metal.
Therefore, according to the twelfth aspect of the invention, sodium, potassium, or lithium, which is abundant as an alkali metal and is easily available at low cost, is used. Therefore, modification of clay mineral powder can be achieved at low cost. .

The invention according to claim 13 is that heating of the mixed clay mineral powder and alkali agent is carried out after kneading and drying the clay mineral powder and alkali agent in the presence of water. To do.
Therefore, according to the invention of claim 13, since the clay mineral powder and the alkaline agent are kneaded prior to heating, the uneven distribution of the alkaline agent is prevented, and the clay mineral powder and the alkaline agent are preferably brought into contact with each other. Can be achieved.

In the invention according to claim 14, the amount of water used when kneading the clay mineral powder and the alkali agent is 70 to 150 with respect to 100 parts by weight of the mixed clay mineral powder and alkali agent. The gist is that it is part by weight.
Therefore, according to the invention which concerns on Claim 14, uneven distribution of the alkaline agent mixed with clay mineral powder can be prevented suitably.

The gist of the invention described in claim 15 is that the alkaline agent contains a salt, oxide or hydroxide of an alkaline earth metal.
Therefore, according to the invention which concerns on Claim 15, since an alkaline-earth metal is hardly soluble in water, it is convenient.

The gist of the invention described in claim 16 is that calcium or magnesium is used as the alkaline earth metal.
Therefore, according to the invention of claim 16, since calcium or magnesium which is abundant as an alkaline earth metal, easily available, and excellent in handleability is used, the modified clay mineral powder can be easily used. Yield can be increased at low cost.

The gist of the invention described in claim 17 is that one or more kinds of natural or synthetic mica, talc or kaolinite powder are used as the clay mineral powder.
Therefore, according to the invention which concerns on Claim 17, various material characteristics with which mica, talc, or kaolinite is provided can be provided to the modified clay mineral powder.

The gist of the invention described in claim 18 is that one kind or two or more kinds of mica, biotite, phlogopite or sericite are used as the natural mica.
Therefore, according to the invention which concerns on Claim 18, the various material characteristic with which various mica is provided to a modified clay mineral powder can be provided.

The gist of the invention described in claim 19 is that a film-like or flake-like substance obtained by crushing the raw ore of the clay mineral powder is used as the clay mineral powder.
Therefore, according to the invention which concerns on Claim 19, the shape characteristic according to a use can be provided to a modified clay mineral powder.

The gist of the invention described in claim 20 is that the raw ore is pulverized by a dry method or a wet method.
Therefore, according to the invention of claim 20, the raw ore can be easily pulverized.

In order to overcome the above-mentioned problems and achieve the intended purpose, a method for producing a modified clay mineral powder according to the invention of claim 21 comprises:
The mixture of the clay mineral powder and the alkali agent is heated to modify the surface region of the clay mineral powder into a porous gelling region.
Therefore, according to the invention of claim 21, since the surface of the clay mineral powder such as mica or talc is modified to form a porous gelling region, the elasticity and flexibility inherent in the clay mineral are obtained. Thus, it is possible to produce a modified clay mineral powder capable of suitably imparting a functional substance or the like that exhibits a required function without impairing the function.

The gist of the invention described in claim 22 is that the alkaline agent is removed by washing the heated mixture.
Therefore, according to the invention of claim 22, since the alkaline agent is removed, a neutral modified clay mineral powder with improved handling properties can be produced.

In the invention described in claim 23, the gelled region and the alkaline agent are removed by washing the heated mixture with an acidic solution, and the specific surface area of the surface is 1.5 compared with that before heating. The gist is that it is more than doubled.
Therefore, according to the invention of claim 23, since the surface of the clay mineral powder such as mica or talc is increased in irregularities and the specific surface area is increased, the elasticity and flexibility inherent in the clay mineral are obtained. It is possible to produce a modified clay mineral powder capable of suitably imparting a functional substance or the like that exhibits a required function without impairing the function.

The gist of the invention described in claim 24 is that after the removal of the alkaline agent, a post-treatment of adding a dispersant and / or a buffering agent is performed.
Therefore, according to the invention which concerns on Claim 24, the modified clay mineral powder which can prevent aggregation and the fluctuation | variation of pH can be manufactured.

The gist of the invention described in claim 25 is that sodium hexametaphosphate or sodium tetrapolyphosphate is used as the dispersant.
Therefore, according to the invention of claim 25, since the buffering action is small and inexpensive sodium hexametaphosphate or sodium tetrapolyphosphate is used, a modified clay mineral powder capable of preventing powder aggregation can be produced at low cost. obtain.

The gist of the invention described in claim 26 is that a phosphate compound is used as the buffer.
Therefore, according to the invention of claim 26, since a phosphoric acid compound that exhibits a buffering action in a wide pH range and is inexpensive is used, a modified clay mineral powder that can prevent pH fluctuation can be easily and inexpensively obtained. Can be manufactured.

The gist of the invention described in claim 27 is that the mixture is heated in a range of 550 to 1300 ° C.
Therefore, according to the invention which concerns on Claim 27, a modified clay mineral powder can be manufactured reliably irrespective of the kind of clay mineral powder.

The gist of the invention according to claim 28 is that the alkali agent is mixed so as to be in the range of 5 to 30 parts by weight when the total amount of the clay mineral powder and the alkali agent is 100 parts by weight. .
Therefore, according to the invention of claim 28, the thickness of the gelled region formed by the modification can be controlled.

The gist of the invention described in claim 29 is that an alkali metal hydroxide, carbonate or bicarbonate is used as the alkali agent.
Therefore, according to the invention of claim 29, a hydroxide, carbonate or hydrogen carbonate having good handleability and low cost is used, so that the modified clay mineral powder can be easily produced.

The gist of the invention of claim 30 is that sodium, potassium or lithium is used as the alkali metal.
Therefore, according to the invention of claim 30, sodium or the like, which is abundant and is easily available as an alkali metal, is used, so that the modified clay mineral powder can be produced at a low cost.

The gist of the invention described in claim 31 is that the mixture is heated after the clay mineral powder and the alkali agent are kneaded and dried in the presence of water.
Therefore, according to the invention of claim 31, since the clay mineral powder and the alkaline agent are kneaded prior to heating, the uneven distribution of the alkaline agent is prevented, and the clay mineral powder and the alkaline agent are preferably brought into contact with each other. Can be achieved.

The gist of the invention of claim 32 is that 70 to 150 parts by weight of water is used with respect to 100 parts by weight of the mixture when the mixture is kneaded.
Therefore, according to the invention which concerns on Claim 32, uneven distribution of the alkaline agent mixed with clay mineral powder can be prevented suitably.

The gist of the invention described in claim 33 is that the alkaline agent contains an alkaline earth metal salt, oxide or hydroxide.
Therefore, according to the 33rd invention, since it is hardly soluble in water, manufacture of a modified clay mineral powder is facilitated.

The gist of the invention described in claim 34 is that calcium or magnesium is used as the alkaline earth metal.
Therefore, according to the invention of claim 34, since calcium or magnesium which is easily available as an alkaline earth metal and has excellent handleability is used, the yield of the modified clay mineral powder can be easily increased at low cost. Can be.

The gist of the invention described in claim 35 is that one or more kinds of natural or synthetic mica, talc or kaolinite powder are used as the clay mineral powder.
Therefore, according to the invention which concerns on Claim 35, the modified clay mineral powder which provided various raw material characteristics with which a mica, a talc, or kaolinite was provided can be manufactured.

The gist of the invention described in claim 36 is that one kind or two or more kinds of muscovite, biotite, phlogopite or sericite are used as the natural mica.
Therefore, according to the invention which concerns on Claim 36, the modified clay mineral powder which provided various material characteristics with which various mica is provided can be manufactured.

The gist of the invention described in claim 37 is that a film-like or flake-like substance obtained by crushing the raw ore of the clay mineral powder is used as the clay mineral powder.
Therefore, according to the invention which concerns on Claim 37, the modified clay mineral powder which provided the shape characteristic according to the use can be manufactured.

The gist of the invention of claim 38 is that the raw ore is pulverized by a dry method or a wet method.
Therefore, according to the invention of claim 38, the raw ore can be easily pulverized.

  According to the modified clay mineral powder and the method for producing the same according to the present invention, the surface area is modified using an alkaline agent to increase the specific surface area of the clay mineral powder. It is possible to obtain a modified clay mineral powder imparted with a variety of functions that are easily imparted with a functional substance and expressed with the functional substance.

  Next, the modified clay mineral powder and the method for producing the same according to the present invention will be described below with reference to the accompanying drawings by way of preferred examples. The inventor of the present application modifies (denatures) the surface region of the powder by mixing and heating a clay mineral powder such as mica (mica), talc (talc) or kaolinite and an alkali agent. It has been found that a modified clay mineral powder can be obtained which has a specific surface area increased and can easily impart a functional substance exhibiting various functions such as color development. The mica, talc or kaolinite referred to in the present invention is an example suitable as a clay mineral selected as a base material, and includes clay minerals having other layered structures, such as vermiculite or other clays. It may be a mineral. The clay mineral powder referred to in the present invention is composed of clay mineral particles such as mica, talc or kaolinite, and the expression of the powder includes the meaning of the particles. Furthermore, “mixing” of the clay mineral powder and the alkali agent in the present invention includes “contact” such as applying the alkali agent on the clay mineral powder. Furthermore, “modification” as used in the present invention means that the state (of the surface region) of the clay mineral powder is changed to improve the quality.

(First embodiment)
The modified clay mineral powder 10 according to the first embodiment is a porous gelled region 14 by modifying the surface region of the clay mineral powder 12 such as mica and talc as shown in FIG. The specific surface area is increased by the modification. Since the porous gelled region 14 has a very fine structure with a pore diameter of several nanometers (nm) to several hundreds of nanometers, the specific surface area is improved by at least 1.5 times or more. Here, the surface region refers to a region near the surface of the clay mineral powder before modification and having a thickness of up to about 1 μm. The total thickness of clay mineral powder such as general mica is about 1 μm, and when the surface region of 1 μm or more is modified to the gelled region 14, it becomes substantially only the gelled region 14, and This is because the clay mineral powder 10 cannot be obtained. In addition, as an index representing the degree of adsorption / application of the functional substance (powder) to the surface of the modified clay mineral powder 10, not only the specific surface area but also the oil absorption, water absorption and methylene blue adsorption as described in Experiment 2 below. Use quantity. The oil absorption amount, water absorption amount and methylene blue adsorption amount can all be quantitatively evaluated by using the specific surface area. Therefore, in the present invention, the modified clay mineral powder 10 of the functional substance (powder) is used. The specific surface area is adopted as an index indicating the degree of adsorption / applying to the surface.

  The surface region is modified by (1) mixing the clay mineral powder 12 and the alkali agent 20 (contact with the alkali agent 20), and (2) heating at a predetermined temperature. Specifically, in the surface region of the clay mineral powder 12, the water of crystallization forming the composition of the clay mineral powder 12 is desorbed and replaced with the metal component of the alkaline agent 20, thereby generating the gel region 14. In addition, since only the surface region of the clay mineral powder 12 is modified to become the gel region 14, the clay mineral powder 12 exists under the gel region 14, and thus the resulting modified clay mineral powder 10 is obtained. The useful function expressed by the clay mineral powder 12 is retained (see Experiment 1 below). It should be noted that the thickness of the gelled region 14 depends on the degree of contact with the alkaline agent 20 and the degree of heating (heating temperature and time), as is apparent from the modification conditions (1) and (2) described above. Determined by.

  As shown in FIG. 2, the modified clay mineral powder 10 according to the first embodiment basically undergoes each raw material preparation step S1, mixing step S2, heating step S3, alkali content removal step S4 and final step S5. Manufactured by. Here, in order to contribute to an understanding of the present invention, mica and talc that are suitably used as clay minerals will be described below before each process is described.

  The mica is a hydrous silicate mineral having a layered monoclinic crystal structure as a main component, and the powder obtained by pulverizing the mica is fine but has a scale-like or plate-like similarity and a particle size. In addition to being stable, it exhibits good slipperiness and elasticity. The mica is composed of two or three metal oxides / hydroxides between the four tetrahedral structures 2 formed by the oxide of 3 atoms of silicon (Si) and 1 atom of aluminum (Al). It is a 2: 1 type clay mineral with a sandwiched octahedral structure. In this structure, 1/4 of the tetrahedron is replaced with Al, and the layers of each layer of mica having tetrahedron-octahedron-tetrahedron as one constituent unit have a negative charge. In the center of the 6-membered ring formed by the body, potassium (K), which is a monovalent cation, is incorporated in a 12-coordinate form.

In mica, there are muscovite (mascobite), biotite (biotite), phlogopite (phlogopite), synthetic mica and the like due to the difference in structure. The metal element composing the octahedron of mica is trivalent aluminum (Al ³⁺ ), divalent iron (Fe ²⁺ ), or magnesium (Mg ²⁺ ). The total charge must be +6. That is, when a trivalent cation (Al ^3+, etc.) enters as an octahedral cation, the cation enters 2/3 of the cation site and 1/3 becomes a vacant 2-dihedral shape. In the case of (Mg ²⁺ , Fe ^2+, etc.), it becomes a trioctahedral type in which all octahedral cation seats (3/3) are full. Even if the divalent cation replaces the trivalent cation and enters the octahedron, if 1/3 is vacant, it becomes a 2-octahedron type, and conversely, the trivalent cation replaces the divalent cation. If you are in an octahedron, it becomes a 3-octahedron type if it is full at 3/3. The representative of the 2-octahedral mica is muscovite, and the representative of the 3-octahedral mica is black / biotite.

In addition, special mica such as synthetic phlogopite synthesized artificially is also known in recent years. As described above, the mica tetrahedron sheet is connected in a plane at a ratio of one aluminum to three silicons, but does not contain aluminum and is formed of only silicon. Mica, and sodium mica in which one potassium atom existing between the layers is replaced with two sodium atoms correspond to this. These have excellent characteristics such as swellability as described in the following non-patent literature, but in terms of the surface being smooth and physically and chemically stable, It is the same. Synthetic mica is an artificially fused mica composed of phlogopite (an octahedron consisting only of magnesium (Mg ²⁺ )), which is a biotite containing iron. It is a mica having a chemical structure in which the OH group (crystal water) of light and black-gold mica is substituted with fluorine.
Shunichi Ota (2004) Clay Basic Course I Synthetic Mica and its Applications, Clay Science, Vol. 44, No. 1, 31-36

  In addition, talc is a structure in which an octahedral structure composed of three magnesium (Mg) oxides and hydroxides is sandwiched between four tetrahedral structure 2 layers formed by a four-atom silicon (Si) oxide. It has become. That is, unlike the mica structure, there is no charge between the layers and no interlayer cations. Therefore, each layer is not fixed by electric charges as in mica, and the structure is easy to collapse due to slipping between layers, and the touch is different from mica. Moreover, since it has high whiteness and hardly transmits light, its color tone is different from that of mica having high light transmittance. These mica and talc are both extremely stable chemically, and it is known that it is difficult to bond organic or inorganic chemical substances by chemical bonding to these surfaces.

  Each said raw material preparation process S1 is a process of preparing the clay mineral powder 12 which is a raw material for obtaining the modified clay mineral powder 10, and the alkaline agent 20 for modifying the surface area of the clay mineral powder 12. The pulverization step S11, and the classification step S12 and the drying step S13 that are performed as necessary. The crushing step S11 is a step for obtaining a clay mineral powder 12 adjusted to a predetermined particle size from a clay mineral ore, that is, a clay mineral present as a rock block. If necessary, it is also applied to the alkaline agent 20 as described later. This pulverization step S11 is performed by a pin mill, a hammer mill, a roll mill (roller mill), dry pulverization or wet pulverization, or other known pulverization means. As for the pulverization of the clay mineral powder 12, pulverization by a so-called water pulverizer or an underwater stirrer using a water stream that performs suitable pulverization under wet conditions is preferable. In this pulverization using a water pulverizer or an underwater stirrer, classification is performed at the same time, so classification in the classification step S12 described later is not necessary. The diameter of the clay mineral powder 12 that is the basis of the modified clay mineral powder 10 is substantially determined by the type of pulverization means used, the pulverization time, and the like.

  The clay mineral powder 12 may be in any form such as a film, flakes or powder obtained by pulverizing clay mineral raw ore by a required method according to the intended use. May be. By using such a shape, when the modified clay mineral powder 10 according to the present invention is used, for example, a shape characteristic corresponding to the use of a cosmetic raw material such as a foundation that requires particularly good tactile sensation is exhibited. It becomes possible.

  The classification step S12 is a step in which the clay mineral powder 12 obtained by the execution of the pulverization step S11 is made to have a particle size according to the intended use. For the classification performed in the classification step S12, a conventionally known method such as classification using a normal sieve having a mesh corresponding to the particle size of the clay mineral powder 12 used as the base material can be appropriately employed. Note that, for example, when the pulverization step S11 is performed, the particle size is sufficiently obtained as a product, and the classification is not necessarily performed when the clay mineral powder 12 does not need to have the same particle size.

  Further, the drying step S13 is a step of performing drying for removing water used for pulverization when pulverization is performed by a wet pulverization method, and a conventional hot-air circulating constant temperature drying furnace or the like that is generally used. It is carried out by using a known means, for example, a conventionally known dryer such as a fluidized bed dryer or a normal dehydration / drying method such as dry heat drying or spray drying after filter pressing. The drying temperature and time are set within a range in which the clay mineral powder 12 is sufficiently dried and the properties of the clay mineral powder 12 are not affected. For example, the temperature at which this drying is performed is set to about 105 to 160 ° C. When this temperature is too high, especially in the case of talc, it is necessary to pay attention because useful physical properties such as hydrophilicity of the talc raw ore may be lost. Further, the drying time is appropriately set within a range of about 90 to 180 minutes so as not to greatly deteriorate the production efficiency. In addition, drying is unnecessary when the dry pulverization method is adopted in the pulverization step S11.

  In each raw material preparation step S1, not only the clay mineral powder 12 but also an alkaline agent 20 that is mixed with the clay mineral powder 12 and modifies its surface region is prepared. Examples of the alkali agent 20 used here include generally known alkali metal hydroxides such as sodium, potassium or lithium, carbonates or bicarbonates, and these may be used alone or in combination of several kinds. Use. Here, as the alkali metal, sodium, potassium or lithium which is inexpensive and easily available is preferably used.

  The alkali agent 20 may contain a salt, oxide or hydroxide of an alkaline earth metal such as calcium or magnesium. When alkaline earth metal is contained in the alkaline agent 20 in this manner, the clay mineral powder 12 is more efficiently produced than the case where the alkaline earth metal is not used due to the extender function that the alkaline earth metal develops. The gel region 14 can be formed by modifying the surface region. By using easily available calcium or magnesium as the alkaline earth metal, the modified clay mineral powder 10 can be produced at low cost.

  The alkaline agent 20 is prepared in the form of powder or liquid so that it can be easily mixed with the clay mineral powder 12. This is for suitably achieving the modification condition (1) of the surface region of the clay mineral powder 12 (the formation condition of the gelation region 14). As the alkali agent 20, a fine powder or liquid material is used. By using this, the gelled region 14 can be efficiently formed. When using a powdery substance as the alkali agent 20, it prepares by implementing the grinding | pulverization step S11 mentioned above and the classification step S12 and the drying step S13 as needed, or is prepared from a commercial item. When using a liquid substance as the alkali agent 20, it prepares by dissolving the solid alkali agent 20 in solvents, such as water, or it prepares from a commercial item similarly to a powdery material. Needless to say, wet pulverization is not suitable when a powder is obtained using sodium hydroxide having deliquescence as the alkali agent 20.

  The mixing amount of the alkali agent 20 is set to a range of 5 to 30 parts by weight with respect to 100 parts by weight of the total amount of the clay mineral powder 12 and the alkali agent 20. When the mixing amount is less than 5 parts by weight, the surface region of the clay mineral powder 12 is modified to the gelation region 14 regardless of the mixing (contact) state of the clay mineral powder 12 and the alkaline agent 20 and the heating temperature. Is almost never done. On the other hand, when the amount exceeds 30 parts by weight, the modification by the alkali agent 20 is not limited to the surface region regardless of the mixed (contacted) state of the clay mineral powder 12 and the alkali agent 20, and the entire clay mineral powder 12 Thus, almost all of the clay mineral powder 12 is modified into the gelled region 14. The modified clay mineral powder 10 according to the present invention is superior to the basic clay mineral powder 12 by controlling so that the modification by the alkali agent 20 and heating does not reach the entire area of the clay mineral powder 12. Thus, a modified clay mineral powder 10 having a high specific surface area and an easy adsorption and application of a functional substance or the like is obtained. That is, the mixing ratio of the alkaline agent 20 needs to be 30 parts by weight or less so that the entire clay mineral powder 12 does not become the gel region 14.

  Further, since the gelling region 14 is formed by replacing the crystal water of the clay mineral powder 12 with the metal component of the alkali agent 20, the amount of the alkali agent 20 mixed is at least the surface of the clay mineral powder 12 to be modified. It is set to be equal to or more than the chemical equivalent of crystal water to be substituted in the region. That is, the chemical equivalent of the metal component of the alkaline agent 20 is set to be larger than the chemical equivalent of crystal water calculated from the composition of the clay mineral powder 12 mixed with the alkaline agent 20.

  The mixing step S2 is a step of obtaining the mixture 16 by mixing the clay mineral powder 12 and the alkaline agent 20. This mixing step S2 is performed by a ribbon type, paddle type, screw type mixer, kneader or other known mixing means. The mixing in the mixing step S2 is related to the above-described modification condition (1) and greatly affects the formation of the gelled region 14. If the mixing of the clay mineral powder 12 and the alkali agent 20 is insufficient, the alkali agent 20 is present inhomogeneously, the surface area of the clay mineral powder 12 is unevenly modified, and the gelled region 14 is formed. As a result, the surface region of the clay mineral powder 12 may not be suitably modified. The mixing / kneading time varies depending on factors such as the particle size of the clay mineral powder 12 and the amount of the alkali agent 20 mixed, but is appropriately set so that the clay mineral powder 12 and the alkali agent 20 are homogeneously mixed. .

  The heating step S3 is a step of heating the mixture 16 of the clay mineral powder 12 and the alkaline agent 20. That is, it is a process for achieving the above-mentioned reforming condition (2), and the heating temperature is set in the range of 550 to 1300 ° C. This temperature is determined according to the type of the clay mineral powder 12, and at least the crystal water of the clay mineral powder 12 can be replaced with the metal component of the alkaline agent 20. The temperature is set to be equal to or higher than the dehydration temperature that can be removed from the composition and not higher than the temperature at which the clay mineral powder 12 can maintain its shape without dissolving.

  For example, in the case of mica, it is at least 650 ° C. or more, preferably 800 ° C., and muscovite suitably used as a cosmetic raw material is about 1 hour at a heating temperature of 800 ° C. and about 3 to 4 hours at 700 ° C. At 650 ° C., a heating time of 15 hours or longer is required. Further, it is about 1 hour at 900 ° C. for phlogopite and biotite, and about 3 to 4 hours at 750 to 800 ° C. In talc, a temperature higher than this is required, and heating at 950 to 1000 ° C. for about 1 hour is required. For kaolinite, a temperature of about 800 ° C. for about 1 hour is suitable. In general, clay minerals have low thermal conductivity, and it is difficult to uniformly heat the inside of the clay mineral. Therefore, a heating condition considering this point is necessary.

  The heating in the heating step S3 is performed by using a conventionally known means such as a commonly used hot-air circulating constant temperature drying furnace. In addition, a conventionally known dryer such as a fluidized bed dryer is also used. obtain. In addition, the heating time is set to be equal to or longer than the length at which the water of crystallization of the clay mineral powder 12 can replace the metal component of the alkaline agent 20, as with the heating temperature. Specifically, the setting in the range of about 90 to 180 minutes, which is within the range not impeding the production efficiency, is suitable, but the above-mentioned crystallization water of the clay mineral powder 12 is suitably removed depending on the production equipment and other conditions. If the temperature cannot be set, a process such as 24 hours may be performed at a low temperature.

  By carrying out the main heating step S3, a modified clay mineral powder 10 whose surface region is modified into a gelled region 14 is obtained from the clay mineral powder 12. That is, the surface region of the clay mineral powder 12 is modified by the alkali agent 20 and heating to become a porous gelling region 14, and the gelling region 14 increases the specific surface area. Due to the increase in the specific surface area, a modified clay mineral powder 10 capable of suitably imparting various functional substances such as a coloring material is obtained. Here, in the modified clay mineral powder 10, the composition of the surface region of the clay mineral powder 12 is slightly substituted and the property is only gelled, and the clay mineral powder 12 exists under the gelled region 14. Therefore, various characteristics of the clay mineral powder 12, such as slipperiness, elasticity, electrical insulation and heat resistance, if mica, keeps good characteristics such as good hydrophilicity, if talc. It has become a state.

  The alkali removal step S4 is performed by using an alkali component (the alkali agent 20 and the alkali agent 20 by heating) from the heated mixture (the modified clay mineral powder 10 and the alkali agent 20) that has undergone the above-described steps S1 to S3. Is a step of neutralizing the modified clay mineral powder 10 by removing the alkali component removal step S41, a neutralization step S42 performed as necessary, and drying. Step S43. The removal of the alkali agent 20 and the like in the alkali removal step S41 is basically carried out by washing with water, but any other known method can be adopted, and if necessary, neutralization can be ensured after washing with water. In order to achieve this, a neutralization step S42 by acid neutralization is carried out. In particular, since the metal oxide generated from the alkali agent 20 by heating exhibits high alkalinity, in order to improve the handleability such as safety of the resulting modified clay mineral powder 10 to the human body, the alkali content removal step S4 is performed. Implementation is encouraged.

  In addition, this alkali content removal process S4 becomes unnecessary when the use application of the modified clay mineral powder 10 permits the presence of the alkaline agent 20 or the like. The drying step S43 is a step of drying the modified clay mineral powder 10 wet by the water washing in the alkali removal step S41, and is performed by using various devices used in the drying step S13. The drying temperature and time are set in such a range that the modified clay mineral powder 10 is sufficiently dried and the properties of the modified clay mineral powder 10 are not affected.

  The final step S5 is a step of performing measurement, packaging, and other various inspections necessary for shipment on the modified clay mineral powder 10 manufactured through the above-described steps S1 to S4. And after completion | finish of this final process S5, the modified clay mineral powder 10 is shipped. Since clay mineral powder such as mica is a chemically stable substance, it is difficult to bond chemical substances, but in the present invention, it is mixed with an alkaline agent 20 to modify the surface area and increase the specific surface area. By doing so, it becomes a surface state to which a functional substance such as a coloring material can be suitably imparted.

  Since the modified clay mineral powder 10 according to the present invention has an increased specific surface area, the adsorption and adhesion of various functional substances are improved. When the modified clay mineral powder 10 having such characteristics is used as a filler for resins such as plastics, for example, the adsorption and adhesion of resin molecules are compared to the case of using a normal clay mineral powder 12. This improves the physical properties of the resin, including the resin strength. Further, with respect to the clay mineral powder 12 obtained from the muscovite mineral, the modified clay mineral powder 10 in which the gelled region 14 is formed by modification increases the specific surface area of the surface and the amount of scattered light, so that the oil absorption increases. By doing so, it can be well harmonized with other ingredients blended in cosmetics such as fats and oils, and as a result, the amount of fats and oils used can be reduced, and the problem of “dullness of mica” that reduces transparency is also reduced. That is, the modified clay mineral powder 10 according to the present invention solves the various problems described above (see [0005]) when employed as a cosmetic raw material such as a foundation in order to improve the touch and whiteness. As a result, it is possible to express characteristics that can be suitably used.

  In addition, by adsorbing and adhering various functional substances having functions such as coloring materials, insecticides or fungicides, surfactants, etc., it is possible to produce clay mineral powders that easily express these functions. can do. Further, the modified clay mineral powder 10 is obtained from the film-like or flaky clay mineral powder 12, and various functional materials are adsorbed and imparted thereto, thereby providing various film-like or flaky clay minerals. It is also possible to produce a powder.

(Second embodiment)
In the first embodiment described above, the clay mineral powder 12 is heated in the presence of the alkaline agent 20 to form a porous gelled region 14 in the surface region of the clay mineral powder 12 to increase the specific surface area. However, the present invention is not limited to this. Since the gelled region 14 formed by heating is soluble in an acidic solution, the obtained modified clay mineral powder 10 may be washed with an acidic solution to remove the gelled region 14. Good.

  As described above, the thickness of the gelled region 14 is determined by the degree of contact with the alkaline agent 20 and the degree of heating (heating temperature and time). That is, the degree of mixing of the clay mineral powder 12 and the alkaline agent 20 can be made almost the same even though it can be made nearly uniform by selecting the mixing method and setting the mixing time. Further, the heating temperature generally cannot be the same regardless of what heating device is used. That is, the thickness of the gelled region 14 is not the same depending on the portion of the modified clay mineral powder 10 but is different. Therefore, in the modified clay mineral powder 11 of the second embodiment obtained in this way, the gelled region 14 formed in a non-uniform thickness on the surface region of the clay mineral powder 12 is removed, so that FIG. As shown in FIG. 5, the surface irregularity is increased as compared with the clay mineral powder 12 before the treatment, and at least the specific surface area is increased by 1.5 times or more. Thus, the specific surface area becomes 1.5 times, so that the modified clay mineral powder 10 obtained can be adsorbed / provided with a functional substance or the like as compared with the clay mineral powder 12 as a base. (Experiment 3 described later).

  The mixing amount of the alkali agent 20 is set in the range of 5 to 30 parts by weight with respect to 100 parts by weight of the total amount of the clay mineral powder 12 and the alkali agent 20 as in the first embodiment. When the mixing amount is less than 5 parts by weight, the surface region of the clay mineral powder 12 is modified to the gelation region 14 regardless of the mixing (contact) state of the clay mineral powder 12 and the alkaline agent 20 and the heating temperature. As a result, the specific surface area of the resulting modified clay mineral powder 10 does not become 1.5 times the specific surface area of the clay mineral powder 12 as a base. On the other hand, when the amount exceeds 30 parts by weight, the modification by the alkali agent 20 is not limited to the surface region regardless of the mixed (contacted) state of the clay mineral powder 12 and the alkali agent 20, and the entire clay mineral powder 12 As a result, almost all of the clay mineral powder 12 is modified into the gelled region 14, and the clay mineral powder 12 according to the second embodiment cannot be obtained.

  As shown in FIG. 4, the modified clay mineral powder 11 according to the second embodiment is a gel region removal step instead of the alkali removal step S4 in the production process of the modified clay mineral powder 10 according to the first embodiment. Manufactured by performing S6. Here, since each process S1-S3 and S5 is the same as that of the above-mentioned 1st Example, description is abbreviate | omitted.

  In the second embodiment, the gelation region removal step S6 performed in place of the alkali removal step S4 includes a gelation region 14 formed by modifying the surface region of the clay mineral powder 12 and an alkali component (alkaline agent). 20 and the metal oxide generated from the alkali agent 20 by heating), the gelation region removal step S61, the neutralization step S62 performed as necessary, and the drying step S63. It consists of. The removal of the gelation region 14 and the alkali in the gelation region removal step S61 is performed by adjusting the pH to 3.5 or less with an acidic solution.

  When this pH exceeds 3.5, there is little melt | dissolution of the gelation area | region 14, and the melt | dissolved gelation area | region 14 will also gelatinize again. This phenomenon occurs even when a strong acid having a pH of about 1 is used when the pH exceeds 3.5 during dissolution of the gelled region 14. The washing time required for removal varies depending on the pH of the acidic solution to be used, but is several hours for a strong acidic solution (about pH 1) and about 24 hours for a weak acidic solution (about pH 3.5). Basically, the clay mineral powder 12 existing under the gelled region 14 is physically and chemically stable as described above and does not dissolve in the acidic solution. It may be longer than time.

  The acidic solution can be used without any problem as long as the mixture 16 after heating can be adjusted to pH 3.5 or lower. However, an acid that forms a metal complex (chelate) such as citric acid can be used. In the case of the solution used, it is possible to efficiently remove not only the gelation region 14 and the alkali content but also foreign matters such as iron contained in the modified clay mineral powder 10. In order to remove foreign substances using an acidic solution, it is more effective to use an acidic solution obtained by mixing an acid that forms a metal complex and an inorganic acid (mineral acid) such as hydrochloric acid, nitric acid, or sulfuric acid. Thus, when foreign matter such as iron is removed from the modified clay mineral powder 10, when muscovite is used as the clay mineral powder 12, iron or the like as a foreign matter that becomes a subtle coloring base of the muscovite is suitable. Therefore, the whiteness of the resulting modified clay mineral powder 10 can be further increased. If the acidic solution is neutralized with the alkaline agent 20 and the pH exceeds 3.5, the gelation region 14 cannot be sufficiently removed. It is preferable to calculate in advance from the amount of the mixed alkali agent 20.

  The neutralization step S62 is a step for completely removing the acidic solution used for removing the gelation region 14 and the like to neutralize the modified clay mineral powder 11, and the acidic solution is sufficiently removed. More specifically, it is carried out using water that is about 10 times or more the volume of the modified clay mineral powder 11 used for washing. This neutralization step S62 becomes unnecessary when the use application of the modified clay mineral powder 11 permits acidity. Further, the drying step S63 is a step of drying the modified clay mineral powder 11 that has been wetted by the washing in the neutralization step S62, and is performed in the same manner as the drying step S13 described above. The drying temperature and time are set in such a range that the modified clay mineral powder 11 is sufficiently dried and the properties of the modified clay mineral powder 11 are not affected. Note that the neutralization step S62 can be eliminated by calculating the chemical equivalent of the acidic solution necessary for the removal of the gelation region 14 and the alkali and performing the gelation region removal step S61.

  The modified clay mineral powder 11 thus obtained has more irregularities and at least a specific surface area of 1.5 times that of the clay mineral powder 12 whose surface is the basis. That is, the modified clay mineral powder 11 according to the second example also has improved adsorption and adhesion of various functional substances, like the modified clay mineral powder 10 of the first example. In addition, since the porous gelled region 14 does not exist on the surface, the “gritty” tactile feel derived from the porosity is weakened, and the good result derived from the properties of the clay mineral powder 12 as a material. The tactile sensation (especially in the case of mica) is strongly expressed.

  Instead of removing the gelation region 14 and the alkali content simultaneously with the acidic solution, in addition to all the steps S1 to S5 in the production process of the modified clay mineral powder 10 of the first embodiment, the alkali content removing step You may make it manufacture the modified clay mineral powder 11 by implementing the gelatinization area | region removal process S6 between S4 and the last process S5. In this case, since the alkali content can be sufficiently removed in the alkali content removal step S4, the ability to remove the alkali content is not considered in the acidic solution used in the subsequent gelation region removal step S6. May be. Further, since the gelation region removal step S61 by the acidic solution is performed subsequent to the alkali removal step S41 performed by washing with water, the drying step S43 performed after the alkali removal step S41 is not necessary.

(Example of change)
The present invention is not limited to the configuration of the embodiment, and can be modified as follows.
(1) In the above-described embodiment, the clay mineral powder 12 and the alkaline agent 20 are heated as the mixture 16. However, the present invention is not limited to this, and as shown in FIG. You may make it implement kneading | mixing process S7 between heating process S3. This kneading step S7 further enhances the degree of mixing of the clay mineral powder 12 and the alkali agent 20 performed in the mixing step S2, in order to homogenize the clay mineral powder 12 and the alkali agent 20 at a high level. To be implemented. The kneading step S7 is performed by adding water to the mixture 16 of the clay mineral powder 12 and the alkaline agent 20 and then using a known kneading apparatus. The amount of water used is 70 to 150 parts by weight with respect to 100 parts by weight of the mixture 16. When the amount used is less than 70 parts by weight, the amount of water is small and kneading cannot be suitably performed. When the amount exceeds 150 parts by weight, it takes time to remove the used water and the production efficiency is lowered, which is not realistic. . Further, there is an optimum value depending on the kind of the clay mineral powder 12, and when the clay mineral powder 12 is mica such as muscovite or phlogopite, it is 70 to 80 parts by weight with respect to 100 parts by weight of the mixture 16. When the clay mineral powder 12 is kaolinite or talc, it is about 100 parts by weight with respect to 100 parts by weight of the mixture 16. In addition, when performing this kneading | mixing process S7, when the alkali agent 20 is water-soluble, since this alkali agent 20 will melt | dissolve in the water used at the time of kneading | mixing, in each said raw material preparation process S1 Grinding, classification and drying are unnecessary. Moreover, in FIG. 5, each process after heating process S3 is abbreviate | omitted.
(2) In the above-described embodiment, the final step S5 is performed after the alkali removal step S4 or the gelled region removal step S6. However, the present invention is not limited to this, and as shown in FIG. You may make it implement post-processing process S8 which improves the property etc. of the modified clay mineral powder 10 and 11 between this alkali content removal process S4 or the gelatinization area | region removal process S6, and the last process S5. In the post-processing step S8, for example, a dispersant, a buffering agent, and the like are mixed with the modified clay mineral powders 10, 11. The dispersant is used when the obtained modified clay mineral powders 10 and 11 are fine and may aggregate, and examples thereof include sodium hexametaphosphate and sodium tetrapolyphosphate. Moreover, the said buffering agent is used when it wants to suppress the fluctuation | variation of pH at the time of use of the modified clay mineral powders 10 and 11, and well-known substances, such as a phosphoric acid type compound, are used. Note that the post-processing step S8 described here can also be applied to the above-described modified example (1). Moreover, in FIG. 6, each process before alkali content removal process S4 or gelatinization area | region removal process S6 is abbreviate | omitted.

(Experimental example)
Hereinafter, with respect to the modified clay mineral powder according to the present invention, the following experiments were performed, and the obtained modified clay mineral powder was measured and observed for evaluation, and the production method was evaluated.

(Experiment 1: About the mixing amount of the alkali agent and the amount of the modified clay mineral powder obtained (gelation region formed))
Basically, in accordance with the method for producing the modified clay mineral powder described in the second embodiment, powder A (white mica (trade name Y-3000; manufactured by Yamaguchi Mica Industry Co., Ltd.)) is used as the clay mineral powder. , Powder B (phlogopite powder (trade name NCR-300; manufactured by Yamaguchi Mica Industry Co., Ltd.)), powder C (talc powder (trade name FK-300S; manufactured by Yamaguchi Mica Industry Co., Ltd.)) or powder D (Kaori) Night powder (trade name: ASP-170; manufactured by Engelhard) is used, and general-purpose sodium carbonate is used as an alkaline agent, and this clay mineral powder and the alkaline agent are mixed (Experimental example 1: clay mineral powder: alkali Agent = 65: 35, Experimental Example 2: Clay mineral powder: Alkaline agent = 70: 30, Experimental example 3: Clay mineral powder: Alkaline agent = 90: 10, Experimental example 4: Clay mineral powder: Alkaline agent = 95: 5 Experimental Example 5: Clay mineral powder: Lukali agent = 96: 4, Experimental Example 6: Clay mineral powder: Alkaline agent = 99: 1 (both weight ratios)), and then 100 parts by weight of the mixture of powder A and powder B, 80 parts by weight The powder C and the powder D were kneaded using 100 parts by weight of water. And after heating a kneaded material, after wash | cleaning and suction filtration about 10 times the amount of the combined volume of the obtained modified clay mineral powder and an alkali agent, and repeating suction filtration 3 times, an alkali content is removed, Neutralization was performed, and suction filtration and dry heat drying were performed to obtain a modified clay mineral powder (with a gelled region). Furthermore, this modified clay mineral powder was adjusted to pH 2 with an acidic solution to obtain a modified clay mineral powder from which the gelled region was removed. Then, the residual ratio (%) due to the modification of the clay mineral powder was calculated from the weight of the first clay mineral powder and the weight of the finally modified clay mineral powder (no gelation region).

(Equipment used)
Mixing of clay mineral powder and alkali agent: Using a general-purpose electric mixer, mixing was performed under the following conditions.
Mixing conditions: mixing speed 900 rpm / hour, 1 minute ・ Kneading of the mixture of clay mineral powder and alkali agent: kneader (trade name: Kenmix Metallic KM-800: manufactured by Aikosha Seisakusho) It knead | mixed on conditions.
Kneading conditions: kneading speed 60 revolutions / minute, time 30 minutes-Heating of the mixture of clay mineral powder and alkaline agent: Heating under the following conditions using an electric muffle furnace (trade name FUW-253PA: manufactured by Tokyo Seisakusho) did.
Heating conditions; temperature 800 ° C., time 1 hour, arrival time from room temperature to treatment temperature 1 hour ・ Acid solution used: hydrochloric acid

(Result of Experiment 1)
The results relating to Experiment 1 are shown in Table 1. From Table 1, when the mixing ratio of the alkaline agent is 35 parts by weight, the residual rate becomes almost zero regardless of the type of clay mineral powder, and the obtained powder cannot be said to be a modified clay mineral powder. Was confirmed. When the mixing ratio of the alkaline agent was 30 parts by weight, the lowest residual muscovite was 9% and the highest clay mineral powder was 83% talc. It was confirmed that the higher the residual rate, the higher the residual temperature of crystallization water of each clay mineral powder, the higher the residual rate, that is, the ease of crystallization water detachment. . Furthermore, in Experimental Example 3 in which the mixing ratio of the clay mineral powder and the alkaline agent is 90:10, a high residual rate of 70 to 90% is obtained regardless of the type of the clay mineral powder, that is, the gelation region to be formed. It was confirmed that sufficient clay mineral powder remained below.

In Experimental Example 4 where the mixing ratio of clay mineral powder and alkaline agent is 95: 5, the same numerical value as in Experimental Example 3 is obtained, and the mixing ratio of clay mineral powder and alkaline agent is 96: 4. In Experimental Example 5 and Experimental Example 6 in which the mixing ratio of the clay mineral powder and the alkaline agent is 99: 1, it is confirmed that the residual rate is almost 100% regardless of the type of the clay mineral powder. It was done. That is, it was found that the gelled region 14 is suitably formed when the mixing ratio of the alkaline agent is 5% or more.

(Experiment 2: Difference between clay mineral powder and modified clay mineral powder)
The powder A (clay mineral powder) used in Experiment 1 and the modified clay mineral powder and the gelled area having the gelled areas related to Powder A obtained in Experiment 3 and Experiment 4 of Experiment 1 were removed. The modified clay mineral powder was subjected to (1) measurement of oil absorption, (2) measurement of water absorption, (3) measurement of methylene blue adsorption, and (4) measurement of specific surface area. In addition, the powder for a control | contrast which did not mix an alkaline agent with the powder A but performed only heating was prepared, and the measurement of (1)-(4) was implemented. The conditions relating to mixing, kneading, heating, and acidic solution are the same as in Experiment 1 described above. Furthermore, (5) crystallinity analysis by X-ray diffraction (FIG. 7) and (5) for the modified clay mineral powder having the gelation region related to the powder A and the powder A obtained in Experimental Example 3 of Experiment 1. 6) Appearance observation by scanning electron microscope (SEM) photographs (FIGS. 8 and 9: enlargement magnification 2000 times, FIGS. 10 and 11: enlargement magnification 20000 times) was performed.

(Measurement equipment and measurement method used in Experiment 2)
(1) Oil absorption: linseed oil (manufactured by Sigma-Aldrich Japan) was used as the oil, and the oil absorption was carried out by the method described in JIS K5101.
(2) Water absorption: Distilled water was used and the method described in JIS K5101 was performed.
(3) Methylene blue adsorption amount: Implemented by the method described in JIS K1474 5.1.1.2. Methylene blue is an effective means for confirming the degree of adsorption of cationic molecules.
(4) Specific surface area: Implemented by the BET method.
(5) Crystallinity analysis: Mica crystallinity peak observed for powder A and modified clay mineral powder (with gelation region) by X-ray diffractometer (trade name RINT-2000: manufactured by Rigaku Corporation) Measurements of 2θ (°) = 0 to 70 including the angle to be performed were performed.
(6) Appearance: With a scanning electron microscope (trade name S-2400: manufactured by Hitachi High-Technologies Corporation), powder A and modified clay mineral powder (with gelation region) under magnification of 2000 times and 20000 times under electron microscope observation ) Was observed.

(Result of Experiment 2)
The results according to Experiment 2 are shown in Table 2 and FIGS. Here, FIG. 7A, FIG. 8 and FIG. 10 are data of powder A which is a clay mineral powder, and FIG. 7B, FIG. 9 and FIG. 11 are modified clay mineral powders obtained in Experimental Example 3. The data is (with gelled region). 8 and 9, the total length of the white horizontal line appearing at the lower right portion in the figure is 20 μm, and in FIGS. 10 and 11, the total length of the white horizontal line appearing at the lower right portion in the figure is 2 μm, respectively.

As can be seen from Table 2, it was confirmed that the modified clay mineral powder (with the gelled region) improved the oil absorption and water absorption by at least 1.5 times compared to the powder A. In addition, the modified clay mineral powder (with gelation region) according to Experimental Example 3 in which 10 parts by weight of an alkali agent was mixed was improved by a factor of 2 or more. That is, this modified clay mineral powder (with a gelled region) has a suitable tactile sensation, has properties that can be suitably molded with a small amount of oil absorption, and can be suitably used for cosmetic raw materials such as foundations. I understood.

  In addition, the specific surface area is 2.4 times (5 times in Experimental Example 3) and the adsorption amount of methylene blue is about 2 times (3 times in Experimental Example 3). It has been confirmed that clay mineral powder (with a gelled region) is suitably provided with functional substances including water-soluble substances typified by anionic molecules that are generally difficult to adsorb to mica. It was. Furthermore, with regard to the modified clay mineral powder from which the gelled region has been removed, any of the values (1) to (3) exceeds the value of the powder A as a base, and (4) the specific surface area is 1.5 times ( It was confirmed that Experimental Example 3 was about 3.5 times). Note that the modified clay mineral powder according to the present invention (with or without gelation region) is also applied to the control material obtained by heating only the powder A (1) to (1) It was confirmed that all the indicators in 4) were higher.

  Furthermore, as is clear from FIG. 7, since the powder A and the modified clay mineral powder (with gelation region) draw exactly the same diffraction lines, there is no change in the structure inside the mica. It became clear. That is, it was confirmed that only the surface region of the clay mineral powder was modified. Note that peaks in the vicinity of 2θ = 18 ° and 27 ° in the graph of FIG. 7 indicate the presence of muscovite. In FIG. 7, the horizontal axis represents the angle (2θ), and the vertical axis represents the X-ray intensity.

  8 and FIG. 9 (SEM photograph at an enlargement magnification of 2000 times), no clear difference could be confirmed, but in FIG. 10 and FIG. 11 (SEM photograph at an enlargement magnification of 20000 times), the modified clay of (b) It has been clarified that the surface of the mineral powder is more porous than the powder A (clay mineral powder) of (a). That is, it was confirmed that the modified clay mineral powder according to the present invention was modified only in the surface region while maintaining the compositional characteristics of the clay mineral powder as a base.

(Experiment 3: Adsorption and impartability of functional substances in modified clay mineral powder)
The powder A used in Experiment 1, the modified clay mineral powder from which the gelation region related to the powder A obtained in Experiment 3 of Experiment 1 has been removed, and the gelation related to the powder A obtained in Experiment 4 The modified clay mineral powder from which the region was removed and the processed powder of the powder A obtained in Experimental Example 5 of Experiment 1 were used as substrates, respectively, and iron acetate ( Wako Pure Chemicals / Reagent Special Grade) was added to each solution as a 1 mM solution, kneaded well, dried for 3 hours with a drying device (SANYO CONVECTION OVEN) set at 105 ° C. Washing with 10 times the amount of water and suction filtration were repeated three times. The powder A, the modified clay mineral powder obtained in Experimental Example 3 (no gelation region), the modified clay mineral powder obtained in Experimental Example 4 (no gelation region), and the experimental example 5 were obtained. Test pieces 3-1, 3-2, 3-3, and 3-4 were obtained from the processed powder of powder A, respectively. And the hue was evaluated by visual observation about each test piece 3-1 to 3-4.

(Measurement equipment used in Experiment 3)
・ Iron acetate: Wako Pure Chemicals ・ Reagent special grade ・ Drying equipment: Sanyo ・ CONVECTION OVEN

(Result of Experiment 3)
The test pieces 3-2 and 3-3 obtained in Experiment 3 were sufficiently colored, whereas the test pieces 3-1 and 3-4 were hardly colored. That is, it was confirmed that a general clay mineral powder can adsorb and impart a functional substance by increasing the specific surface area by 1.5 times.

It is a schematic sectional drawing which expands and shows the surface area | region of the modified clay mineral powder which concerns on suitable 1st Example of this invention. It is process drawing which shows an example of the manufacturing method about the modified clay mineral powder of 1st Example. It is a schematic sectional drawing which expands and shows the surface area | region of the modified clay mineral powder which concerns on suitable 2nd Example of this invention. It is process drawing which shows an example of the manufacturing method about the modified clay mineral powder of 2nd Example. It is process drawing which shows an example of the manufacturing method which concerns on the example of a change (1). It is process drawing which shows an example of the manufacturing method which concerns on the example of a change (2). It is a graph which shows the result of the X-ray diffraction about the clay mineral powder which concerns on Experiment 2, and a modified clay mineral powder. It is the scanning electron micrograph which image | photographed the clay mineral powder which concerns on the experiment 2 by 2000 time magnification. 4 is a scanning electron micrograph of the modified clay mineral powder according to Experiment 2 taken at a magnification of 2000 times. It is the scanning electron micrograph which image | photographed the clay mineral powder which concerns on the experiment 2 by 20000 times magnification. It is the scanning electron micrograph which image | photographed the modified clay mineral powder which concerns on Experiment 2 by 20000 times magnification.

Explanation of symbols

12 Clay mineral powder 14 Gelation region 20 Alkaline agent

Claims (38)

A modified clay mineral powder characterized in that the surface region of the clay mineral powder (12) is a porous gelled region (14). By heating the clay mineral powder (12) and the alkaline agent (20) in a mixed state, the surface region of the clay mineral powder (12) is modified to become a porous gelling region (14). Modified clay mineral powder characterized by.   The modified clay mineral powder according to claim 2, wherein the alkaline agent (20) is removed after heating. By heating the clay mineral powder (12) and the alkaline agent (20) in a mixed state, the surface region of the clay mineral powder (12) is modified to form a gel region (14), and then the gel region A modified clay mineral powder characterized in that the specific surface area of the surface of the clay mineral powder (12) after heating by removing (14) is at least 1.5 times that before heating.   The modified clay mineral powder according to claim 4, wherein the gelled region (14) is removed together with the alkaline agent (20) by an acidic solution.   The modified clay mineral powder according to claim 3 or 5, wherein a dispersing agent and / or a buffering agent is added after the alkali agent (20) is removed.   The modified clay mineral powder according to claim 6, wherein sodium hexametaphosphate or sodium tetrapolyphosphate is used as the dispersant.   The modified clay mineral powder according to claim 6, wherein a phosphate compound is used as the buffer.   The modified clay mineral powder according to any one of claims 2 to 8, wherein the mixed clay mineral powder (12) and alkali agent (20) are heated in a range of 550 to 1300 ° C.   The mixing amount of the alkali agent (20) is in the range of 5 to 30 parts by weight when the total amount of the clay mineral powder (12) and the alkali agent (20) is 100 parts by weight. The modified clay mineral powder according to any one of the above.   The modified clay mineral powder according to any one of claims 2 to 10, wherein an alkali metal hydroxide, carbonate or bicarbonate is used as the alkali agent (20).   The modified clay mineral powder according to claim 11, wherein sodium, potassium or lithium is used as the alkali metal.   The heating of the mixed clay mineral powder (12) and the alkali agent (20) is performed after the clay mineral powder (12) and the alkali agent (20) are kneaded and dried in the presence of water. Item 13. The modified clay mineral powder according to any one of Items 2 to 12.   The amount of water used when kneading the clay mineral powder (12) and the alkali agent (20) is 100 parts by weight of the mixed clay mineral powder (12) and the alkali agent (20). The modified clay mineral powder according to claim 13, which is 70 to 150 parts by weight.   The modified clay mineral powder according to any one of claims 2 to 14, wherein the alkaline agent (20) contains an alkaline earth metal salt, oxide or hydroxide.   The modified clay mineral powder according to claim 15, wherein calcium or magnesium is used as the alkaline earth metal.   The modified clay mineral according to any one of claims 1 to 16, wherein one or more kinds of natural or synthetic mica, talc or kaolinite powder are used as the clay mineral powder (12). Powder.   The modified clay mineral powder according to claim 17, wherein one or more of muscovite, biotite, phlogopite, or sericite is used as the natural mica.   The modified clay according to any one of claims 1 to 18, wherein the clay mineral powder (12) is a film-like or flaky substance obtained by crushing the raw ore of the clay mineral powder (12). Mineral powder.   The modified clay mineral powder according to claim 19, wherein the raw ore is pulverized by a dry method or a wet method. By heating the mixture (16) of the clay mineral powder (12) and the alkali agent (20), the surface region of the clay mineral powder (12) is modified into a porous gelling region (14). A method for producing a modified clay mineral powder, characterized in that:   The method for producing a modified clay mineral powder according to claim 21, wherein the alkaline agent (20) is removed by washing the mixture (16) after heating.   The gelled region (14) and the alkali agent (20) are removed by washing the heated mixture (16) with an acidic solution, and the specific surface area of the surface is 1.5 compared to before heating. The method for producing a modified clay mineral powder according to claim 21, wherein the modified clay mineral powder is doubled or more.   The method for producing a modified clay mineral powder according to claim 22 or 23, wherein after the removal of the alkaline agent (20), a post-treatment of adding a dispersant and / or a buffering agent is performed.   The method for producing a modified clay mineral powder according to claim 24, wherein sodium hexametaphosphate or sodium tetrapolyphosphate is used as the dispersant.   The method for producing a modified clay mineral powder according to claim 24, wherein a phosphate compound is used as the buffer.   The method for producing a modified clay mineral powder according to any one of claims 21 to 26, wherein the mixture (16) is heated in a range of 550 to 1300 ° C.   The said alkali agent (20) is mixed so that it may become the range of 5-30 weight part when the whole clay mineral powder (12) and an alkali agent (20) are 100 weight part. The manufacturing method of the modified clay mineral powder as described in any one of these.   The method for producing a modified clay mineral powder according to any one of claims 21 to 28, wherein an alkali metal hydroxide, carbonate or bicarbonate is used as the alkali agent (20).   30. The method for producing a modified clay mineral powder according to claim 29, wherein sodium, potassium or lithium is used as the alkali metal.   The mixture (16) according to any one of claims 21 to 30, wherein the clay mineral powder (12) and the alkali agent (20) are kneaded and dried in the presence of water and then heated. The manufacturing method of the modified clay mineral powder of description.   32. The method for producing a modified clay mineral powder according to claim 31, wherein 70 to 150 parts by weight of water is used for 100 parts by weight of the mixture (16) when the mixture (16) is kneaded.   The method for producing a modified clay mineral powder according to any one of claims 21 to 32, wherein the alkaline agent (20) contains an alkaline earth metal salt, oxide or hydroxide.   The method for producing a modified clay mineral powder according to claim 33, wherein calcium or magnesium is used as the alkaline earth metal.   The modified clay according to any one of claims 21 to 34, wherein one or more kinds of natural or synthetic mica, talc or kaolinite powder are used as the clay mineral powder (12). Manufacturing method of mineral powder.   36. The method for producing a modified clay mineral powder according to claim 35, wherein one or more of muscovite, biotite, phlogopite, or sericite is used as the natural mica.   The modification according to any one of claims 21 to 36, wherein the clay mineral powder (12) is a film-like or flaky substance obtained by crushing the raw ore of the clay mineral powder (12). A method for producing clay mineral powder.   The method for producing a modified clay mineral powder according to claim 37, wherein the raw ore is pulverized by a dry method or a wet method.