JPS609851B2 - Method for manufacturing hollow porous powder - Google Patents

Description

DETAILED DESCRIPTION OF THE INVENTION The present invention provides a hollow porous powder, in particular, a powder having an average particle size of Approximately 1 to 100 Buddhas, preferably 1 to 20
The present invention relates to a method for producing a hollow porous powder of the same size as a flower.

Conventionally used powders often have defects when the structure is formed by crystallization due to the complicated crystal growth process. Especially in natural minerals, for example, the disorder of atomic arrangement, There are very few crystals that exhibit an ideal arrangement and exhibit a structure consisting of a discontinuous collection of blocks due to dropout of atoms and lack of homogeneity within the crystal.

Powders made of natural minerals have the physical properties of ordinary powders, such as elasticity, specific heat, specific gravity, transparency, hardness, electromagnetic properties,
It has unique characteristics such as ductility, heat resistance, masculinity, and elasticity, and it has various properties depending on its crystal structure, its fineness, and crystal shape. For example, a mineral with a three-layered structure in the shape of a scale has weak bonds between the layers and has a fully developed penis, giving it a slippery feel and being highly elastic. The lack of filling properties is one of the causes of manufacturing troubles. In addition, only some powders with a two-layer structure have excellent virility, and
Because the crystals are amorphous, it is difficult to obtain a close-packed structure due to the bendability of the powder and the fineness of the crystallinity. Can not. On the other hand, natural minerals contain water and impurities, and there are some sensitive minerals that are affected by the production conditions and non-sensitive minerals that are not affected. There are three types of water in a crystal structure: free water, attached water, adsorbed water, and bound water. Free water, attached water, and adsorbed water are easily desorbed, attached, or adsorbed depending on external conditions, and especially bound water When desorbed, the crystal structure changes. As can be understood from the above, natural minerals have low heat retention properties. Viewed from a structural perspective, natural minerals are proven to have the disadvantage of having poor retention of moisture and fragrance, and the smell of fragrance weakens over a short period of time. In addition, most natural minerals have a one-, two-, or three-layer structure, but since they do not have porosity, they have poor breathability, so they cannot be mixed into cosmetics and applied to the skin. When exposed to skin, it tends to inhibit the skin's ability to breathe, causing stress on the skin. The present invention was invented for the purpose of solving the above-mentioned problems and providing a hollow porous powder with excellent physical properties.

That is, in order to achieve the above object, the present invention provides a fine powder having an average particle size of 1 to 50 and made of one or more of anhydrous silicate mineral, alumina silicate mineral, and magnesium silicate mineral as a coating material; and an inner core. Fine powder with an average particle size of 1 to 50 particles consisting of one or more types of volatile substances as substances, and a mixture with a mixing weight ratio of 0 to about 8:2 to 4:5 in an aqueous system or inert The coating substance is attached and aggregated to the surface of the inner core material by soaking it in a solvent to form particles with an average particle size of 1 to 100.
The first feature is to make a Buddha powder, then heat the powder to volatilize and remove the inner core material.

The present invention also provides metal carbonate minerals and (
or) an average particle size of 1 to 50 made of one or more types of anhydrous alumina silicate mineral containing volatile substances other than water
The second feature is that the metal carbonate mineral and/or anhydrous alumina silicate mineral are eluted by adding a fine powder of Buddha and washing the obtained powder with an acid solution.

Next, to explain the details of the present invention in detail, first, the natural minerals constituting the coating material and preferred specific examples thereof are as shown in the following table.

However, it goes without saying that the present invention is not limited to the substances listed in the specific examples.

Next, the volatile substances that make up the inner core substance include menthol, camphor, methyl/graben, ethyl/graben, and fluorine.

Illustrative examples include lopyl/ylaben, butyl/ylaben, naphthalene, diosorpic acid, dehydroblastic acid, benzoic acid, salicylic acid, cinnamic acid, t-parachlorobenzoic acid, and paraoxybenzoic acid. In addition, metal carbonate minerals constituting the inner core material used in mixture with volatile substances include magnesium carbonate, beryllium carbonate, calcium carbonate, ferric carbonate, barium carbonate, manganese carbonate, lithium carbonate,
Examples include cobalt carbonate, potassium magnesium hydrogen carbonate, strontium carbonate, lithium hydrogen carbonate, zinc carbonate, and chromium carbonate.Metal carbonate minerals that exist as natural minerals include dolomite, calcite, aralite, strontianite, and munganite. , Dokujodo stone, etc. are exemplified.

Further, as the anhydrous alumina dermatite mineral containing a volatile component other than water, which can be used in combination with the metal carbonate mineral or alone in a mixture with a volatile substance, examples include kakunai stone, biotite, ochite, dumoly chielite, Examples include Zuni stone. These are minerals that lose their volatile components when heated, easily transform into mullite, and shrink in volume; nacre, which expands when heated;
Do not use black gourd stone or pine stone as they are undesirable. Incidentally, volatile substances and metal carbonate minerals constituting the inner core material, and anhydrous alumina silicate minerals containing volatile components other than water, are used by arbitrarily selecting one or more kinds, and each component There is no particular restriction on the mixing ratio when removing all of the inner core material, but when removing a part of the inner core material, the mixing ratio of the latter two and the former may be mixed depending on the extent of removal. The mixing weight ratio of about 8:2 to 2:8
Adjust within the range. Here, there is no particular restriction on the mixing weight ratio of the latter two. Here, in the present invention, the coating material has an average particle diameter of 1 to 50 r, preferably 1 to 2 r.
A fine powder of 0.0 mm is used, and the average particle size is 1 as the inner core material.
A fine powder of ~50 Buddhas, preferably 1 to 15 Buddhas, is used.

That is, if the average particle size of the coating material is 50 mm or more, not only the strength of the obtained hollow porous powder will be reduced, but also the dispersibility will be poor when added to cosmetics, and the powder will have a rough feel when used. In addition, if the average particle size of the inner core material is 50 mm or more, when the resulting hollow porous powder is added to cosmetics, for example, it will become rough and the adhesion to the skin will decrease. Because of the drawbacks, the average particle size was determined to be within the above range. Furthermore, in the present invention, the mixed weight ratio of the coating material and the inner core material is approximately 8:2 to 4:5, but if the coating material is larger than this, the fragrance retention of the hollow porous powder obtained will be reduced. If the strength, heat retention, and air permeability are poor, and on the other hand, if the strength is low, the strength of the hollow porous powder obtained will decrease, and when added to cosmetics, for example, it will be destroyed in the mixing process and become a hollow porous powder. The problem arises that the function of the device is easily lost.

Further, the above-mentioned mixing weight ratio is the same regardless of whether the atmosphere in which the coating material is adhered and coagulated on the surface of the inner core material is aqueous or inert solvent. A mixture of the above-mentioned coating material, a volatile substance as the inner core material, or anhydrous alumina-silicate mineral containing a metal carbonate mineral and/or a volatile component other than water, in the above-mentioned mixed weight ratio, is mixed into an aqueous system. When roped inside at room temperature and under reduced pressure, preferably about 700 to 76 meters Hg, an adsorbed ion layer is formed on the surface of the inner core core material, and the negatively charged minerals that are the coating material are attracted to the inner core. The coating material adheres to the surface of the nuclear material and aggregates, resulting in an average particle size of 1 to 1.
A cored porous powder with a diameter of 0.00 mm is produced.

When using an inert solvent instead of an aqueous solvent, the mixing weight ratio of the coating material and inner core material to the inert solvent is 9:
The ratio is 1 to 6:4, preferably 8.3 to 1.7. Examples of inert solvents include silicone oil, polybran, polyoxyethylene tall oil derivatives, etc. The above mixture is added to these inert solvents and brought to room temperature, preferably at 70%
When strongly applied under reduced pressure of about 0 to 760 Hg, the coating material and the inner core material are surrounded by an inert solvent and become one, and when they are subjected to suction, particles with an average particle size of about 1 to 100 Fg are formed. A cored porous powder can be obtained. Next, the powdered material made in the above manner is taken out and fired in an oxidizing air stream at a temperature of about 50 to 15,000° for about 1-2 hours, first forming an inner core at a relatively low heating temperature. Volatile substances contained in it evaporate and it becomes completely hollow or semi-hollow,
By heating and baking at a higher temperature than this, the fine powder particles constituting the coating material are firmly bound to each other.

When the inner core material contains metal carbonate minerals and anhydrous alumina silicate minerals, these fine powder particles also bind strongly to each other during firing, and at the same time, they also firmly bind to the fine powder particles that make up the coating material Z. This leads to the conclusion that Furthermore, if the inner core material contains metal carbonate minerals and/or anhydrous alumina silicate minerals, after firing, it is washed with a Z acid solution such as hydrochloric acid, nitric acid, or sulfuric acid with a concentration of 1 to 2% by weight. The core material is eluted to form a hollow porous powder.

As described above, the hollow porous powder obtained by volatilization and further elution of the inner core material shows, according to electron microscopic observation (omitted), that the natural mineral 2, which is a fine coating material, has an average particle size of 1 to 100. It is an aggregate that is stuck to each other in a shape similar to a mountain-like sphere or an elliptical sphere, and there are countless voids of various sizes between each coating material, and these voids and the voids or voids in the inner core form an aggregate that is bonded to each other. It was found that the material had excellent gas absorption and dissipation ability. The surface layer forms a high-strength film due to permanent shrinkage of the coating material and partial conversion to crystalline material.
In addition, since the hollow porous powder obtained by the present invention is composed of inorganic substances, it has excellent heat resistance and light resistance, has a light apparent specific gravity in aqueous and non-aqueous systems, and has good affinity with solvents. Therefore, in a mixed system, it has non-sedimenting properties, behaves as a single body, has excellent dispersion flexibility, and when used as a powder, for example in cosmetics, it has a moist feel unlike conventional powders. This makes it possible to provide products with a smooth feel and good adhesion.Also,
When filled into a container, it is easy to create a close-packed structure and has excellent packing properties. Furthermore, the hollow porous powder obtained according to the present invention has no skin irritation or skin irritation, and in a patch test on the maekatsube of 102 women with healthy skin, the powder showed no skin irritation after 24 hours and 7 hours. No abnormalities were found in the evaluation. In other words, the cosmetics containing the hollow porous powder according to the present invention are moist and smooth without putting any burden on the skin, have excellent adhesion, and have a fragrance-retaining ability that lasts for a long time and emits a fragrance, resulting in excellent cosmetic effects. In addition to this, the filling properties are greatly improved.

Furthermore, when blended into paints, etc., it can improve fluidity as well as heat resistance and light resistance, and when applied as a filler to synthetic resins, it can help reduce the weight of the product. In addition, when the inner core core material contains metal carbonate minerals or anhydrous alumina silicate minerals, grain protrusions can be coated by changing the mixing weight ratio of both when combining the coating material and the partially remaining inner core core material. The strength of the material layer can be adjusted freely.

Next, the results of a sensory test of fragrance retention by 10 sea bream perfumers are shown.

Sample A: A pressed powder containing 65% by weight of the hollow porous powder according to Example 1 was added with 0.0% lemon flavor. Tortoise weight% perfumed sample B: 0.6% by weight of lemon flavor added to pressed powder containing 65% by weight of normal natural mineral fine powder (1) Room temperature evaluation (Otsu 0-25℃) 40℃ evaluation Note Indicates the volatilization intensity of ±.

(- none, 10) Next, examples of the present invention will be shown. Example 1 15 parts by weight of kaolin with an average particle size of 3 to 5 and an average particle size of 2 to 5 parts by weight
Add 31 parts by weight of purified water to 15 parts by weight of potash feldspar and 7 parts by weight of naphthalene having an average particle size of 5 to 10, milled in a centrifugal rotary ball mill for 1 time, and then take out the mixture.
The temperature was raised in an electric furnace for 4 hours to volatilize naphthalene, which is the inner core material, and then fired at 100,000 ℃ for 8 hours to obtain 20 parts by weight of hollow porous powder with an average particle size of 7 to 15 mm. Ta.

Example 2 15 parts by weight of pentonite with an average particle size of 1 to 2 particles, 15 parts by weight of kaolin with an average particle size of 3 to 5 particles, and 10 parts by weight of butylparaben with an average particle size of 4 to 7 particles were dispersed in purified water. After being heated for 5 hours, it was sucked with an aspirator, heated in an electric furnace from room temperature to 400 oo over 4 hours to volatilize the inner core material, butylparaben, and then fired at 1000 qo for 5 hours to give an average Two parts by weight of hollow porous powder having a particle size of 8 to 15 particles were obtained.

Example 3 Parts by weight of pentonite 1 with an average particle size of 1 to 2 mm and parts by weight of butyl paraben 1 with an average particle size of 3 to 7 mm were adjusted to ZIO ratio pS
was gradually added to 50 parts by weight of dimethylsiloxane, stirred for 30 minutes at room temperature, taken out, filtered with a suction aspirator, and placed in an electric furnace at 2,000 to 13 parts by weight.
000 in 3 hours to volatilize the inner core material, butylparaben, and further calcined at 900Z℃ for 3 hours to obtain 8.5 parts by weight of hollow porous powder with an average grain size of 5 to 9 mm. Ta.

Example 4 3 parts by weight of kaolin with an average particle size of 3 to 5 μm, 2 parts by weight of naphthalene with an average particle size of 5 to 10 μm, and 2 parts by weight of naphthalene with an average particle size of 5 to 5 μm
Add purified water 31 to 5 parts by weight of biotite from No. 28, mill it in a centrifugal rotary ball mill for 12 hours, and then take it out.
0,000 in 4 hours in an electric furnace to volatilize naphthalene, which is the inner core material, and then fired at 900 qo for 1 time to form semi-hollow porous 2 powders with an average particle size of 6 to 14 mm. Parts by weight were obtained.

Next, add 2 parts by weight of this semi-hollow porous powder to 50% of 7% hydrochloric acid.
After soaking in water for 10 hours, take it out and suck it with a suction aspirator and dry it with a hollow pore with an average particle size of 5-12.
Parts by weight of powder 2 were obtained.
3 Example 5 Average particle size 3-5 parts by weight of Buddha's Kaolin 3 and average particle size 5-5
Add 31 parts by weight of purified water to 15 parts by weight of camphor of 8 degrees Fahrenheit and 15 parts by weight of biotite with an average particle size of 5 to 8A, grind the mixture in a centrifugal rotary ball mill for 1 hour, take it out, and add 30 parts by weight of 5% hydrochloric acid.
After soaking in water for 10 hours, the mixture was taken out and dried by suction with a suction aspirator to obtain 4 parts by weight of semi-hollow porous powder with an average particle size of 7 to 15 r.

Next, the temperature was raised to 30,000°C in an electric furnace for 4 hours to volatilize camphor, which is the inner core material, and then baked at 1,000°C for 8 hours to obtain a hollow porous powder with an average particle size of 5 to 12 particles. Parts by weight were obtained. Example 6 Kaolin second base weight part with an average particle size of 3 to 6 and an average particle size of 5 to 6
Add 40% of purified water to 3 parts by weight of menthol of 11 grams and 6 parts of calcium carbonate with an average particle size of 5 to 8A, grind for 1 hour in a far-D rotary ball mill, and then take out the mixture.
qo in an electric furnace for 4 hours to volatilize the inner core material, menthol, and further calcined at 900 oo for 1 hour to obtain 20 parts by weight of semi-hollow porous powder with an average particle size of 6 to 14 r. Obtained.

Next, 20 parts by weight of this semi-hollow porous powder was mixed with 7% nitric acid and 5 parts by weight.
After being immersed in 00' for 7 hours, the powder was taken out and dried by suction using a suction aspirator to obtain a hollow porous powder having an average particle size of 5 to 12 mm. Example 7 Parts by weight of pentonite 3 with an average particle size of 3 to 5, 14 parts by weight of butyl paraben with an average particle size of 5 to 8, and an average particle size of 5 to 8
Add 34M of purified water to 1 part by weight of French ferric carbonate tablet, grind in a centrifugal rotary ball mill for 1 hour, then take out,
After soaking in 50% nitric acid for 10 hours, it was taken out and dried using a suction aspirator to obtain particles with an average particle size of 7 to 16.
43 parts by weight of semi-hollow porous powder was obtained.

Next, the temperature was raised to 30,000 ℃ in an electric furnace for 4 hours to volatilize the inner core substance, butyl paraben, and then baked at 1,000 ℃ for 8 hours to form a hollow porous powder with an average particle size of 5 to 12 F. Three parts by weight of the body were obtained. Example 8 8 parts by weight of biotite and 8 parts by weight of calcium carbonate were used in place of the ferric carbonate in Example 7, and 3 parts by weight of hollow porous powder was obtained in the same manner.

Example 9 15 parts by weight of pentonite with an average particle size of 1 to 12 particles, 15 parts by weight of kaolin with an average particle size of 3 to 5 particles, and 1 part by weight of butyl paraben with an average particle size of 4 to 7 particles were dispersed in purified water. After lighting for 5 hours, it was sucked and filtered with an aspirator, and heated in an electric furnace from room temperature to 40,000 ℃ in 4 hours to volatilize the inner core substance, butyl paraben, and further 1,000 q.
The resulting powder was soaked in 300°C of 5% nitric acid for 3 hours, taken out, passed through a suction aspirator, dried, and had hollow pores with an average particle size of 8 to 15 mounds. 2 parts by weight of a powder was obtained.

Example 10 3 parts by weight of pentonite with an average particle size of 3 to 5, 14 parts by weight of butylparaben with an average particle size of 5 to 8, and 8 parts by weight each of biotite and calcium carbonate with an average particle size of 5 to 8. After adding 34 parts of purified water and grinding for 1 hour in a centrifugal rotary ball mill, the mixture was taken out and dried by suction using a suction aspirator to obtain 4 parts by weight of powder with an average particle size of 7 to 16 mm.

Claims (1)

[Scope of Claims] 1 (a) Fine powder with an average particle size of 1 to 50μ made of one or more of anhydrous silicate mineral, alumina silicate mineral, and magnesium silicate mineral, which is a coating material; and an inner core material. Average particle size 1 consisting of one or more volatile substances
~50μ fine powder; mixed weight ratio approximately 8:2
A mixture of ~4:5 is stirred in an aqueous system or an inert solvent, and the coating material is adhered and aggregated on the surface of the inner core material to form a fine powder with an average particle size of 1 to 100μ, (b) Next. A method for producing a hollow porous powder, comprising heating the fine powder to volatilize and remove the inner core material. 2 (a) A fine powder with an average particle size of 1 to 50 μ made of one or more of anhydrous silicate mineral, alumina silicate mineral, and magnesium silicate mineral, which is a coating material; and one kind of volatile substance, which is an inner core material, or Average particle size 1 consisting of two or more types and one or more types of anhydrous alumina silicate mineral containing a metal carbonate mineral and/or a volatile substance other than water.
~50μ fine powder; mixed weight ratio approximately 8:2
A mixture of ~4:5 is stirred in an aqueous system or an inert solvent, and the coating material is adhered and aggregated on the surface of the inner core material to form a fine powder with an average particle size of 1 to 100μ, (b) Next. A method for producing a hollow porous powder, characterized in that the fine powder is heated to volatilize and remove volatile substances, and further washed with an acid solution to elute metal carbonate minerals and/or anhydrous alumina silicate minerals.