JP2018089603A - Method for producing granule - Google Patents

Abstract

PROBLEM TO BE SOLVED: To provide a production method that makes it possible to obtain a granule with excellent strength, excellent flowability, and a reduced occurrence of impalpable powder.SOLUTION: A method for producing a granule has the following steps 1 and 2, where an organic acid content is 30 mass% or more and 70 mass% or less, and the ratio of the organic acid relative to a nonionic surfactant is 5 or more and 25 or less. Step 1: the organic acid and the nonionic surfactant are mixed. Step 2: the mixture obtained by step 1 is mixed with water-soluble binder and the mixture is granulated, to obtain a granule.SELECTED DRAWING: None

Description

  The present invention relates to a method for producing a granulated product, a method for producing a granulated product for a bath agent, and a method for producing a bath agent.

  Conventionally, bathing agents that generate carbon dioxide gas by the reaction of carbonate and organic acid are known. Known forms of bathing agents include powders, tablets, tablets and the like. It is known that a powdered bath agent is produced by mixing a granulated product containing an organic acid and a nonionic surfactant with a carbonate such as sodium carbonate (Patent Documents 1 and 2). In Patent Document 3, a granulated product for bathing agent containing an organic acid, a hydrophilic activator and an oil component is prepared by mixing an organic acid and a hydrophilic activator, and then adding and mixing the oil component. Is disclosed.

JP 2011-021004 A JP 2012-158588 A JP 2012-1469 A

A granulated product containing an organic acid and a nonionic surfactant is suitable as a granulated product for a bathing agent, and can be mixed with carbonate to produce a bathing agent. The granules need to have sufficient strength for transportation and the like. In addition, it is desirable to have good fluidity and little generation of fine powder during mixing with carbonate.
The present invention provides a production method capable of obtaining a granulated product having excellent strength, good fluidity and little generation of fine powder.

The present invention includes the following steps 1 and 2, granulation wherein the organic acid content is 30% by mass or more and 70% by mass or less, and the mass ratio of the organic acid to the nonionic surfactant is 5 or more and 25 or less. The present invention relates to a method for manufacturing a product.
Step 1: Step of mixing an organic acid and a nonionic surfactant Step 2: Step of mixing a water-soluble binder with the mixture obtained in Step 1, granulating the mixture, and obtaining a granulated product

Moreover, this invention has the following process A and B, the process A regarding the manufacturing method of a bath agent composition: By the manufacturing method of the granulated material of the said this invention, an organic acid and a nonionic surfactant are contained, It is obtained in Step B: Step A for producing a granulated product having an organic acid content of 30% by mass to 70% by mass and a mass ratio of the organic acid to the nonionic surfactant of 5 to 25. Mixing the granulated product and carbonate

  ADVANTAGE OF THE INVENTION According to this invention, the manufacturing method which is excellent in intensity | strength, has good fluidity | liquidity, and can obtain a granulation suitable as a granulation for bathing agents etc. with little generation | occurrence | production of fine powder is provided.

[Production method of granulated product]
The method for producing a granulated product of the present invention includes the following steps 1 and 2, wherein the organic acid content is 30% by mass or more and 70% by mass or less, and the mass ratio of the organic acid to the nonionic surfactant is 5%. A granulated product having a particle size of 25 or less is produced.
Step 1: Step of mixing an organic acid and a nonionic surfactant Step 2: Step of mixing a water-soluble binder with the mixture obtained in Step 1, granulating the mixture, and obtaining a granulated product

  The method for producing a granulated product of the present invention comprises mixing an organic acid, a nonionic surfactant, and a water-soluble binder so that the content of the organic acid is 30% by mass or more and 70% by mass or less. A method for producing a granulated product having a mass ratio of organic acid to 5 to 25 inclusive, wherein an organic acid and a nonionic surfactant are mixed, and then a water-soluble binder is mixed. A method for producing a granulated product. In this method, all of the organic acid and at least a part of the nonionic surfactant are mixed, and then the entire water-soluble binder can be mixed.

(Process 1)
The organic acid used in the present invention is preferably water-soluble from the viewpoints of solubility in bath water and handling properties. The organic acid is preferably a solid one.
In the case where the organic acid used in the present invention is a solid, one having an oil absorption capacity of 0.02 ml / g or more is preferable from the viewpoint of sufficient supporting performance when an oil component is blended in the granulated product. More than g is more preferable. The oil absorption capacity is a value determined by the method described in the examples. The upper limit of the oil absorption capacity is not particularly limited, but is preferably 1.0 ml / g or less.

  As the organic acid, succinic acid, fumaric acid, malic acid, adipic acid, tartaric acid, benzoic acid, citric acid, pyrrolidone carboxylic acid, salicylic acid and the like are preferable. From the viewpoint of easy handling and economical efficiency, fumaric acid is more preferable. These organic acids can be used alone or in combination of two or more.

  When the organic acid is solid, the average particle diameter is preferably 250 μm or less, more preferably 200 μm or less, and even more preferably 150 μm or less, from the viewpoint of granulation and solubility.

Examples of the nonionic surfactant include glycerin fatty acid ester, propylene glycol fatty acid ester, sorbitan fatty acid ester, polyoxyethylene sorbitan fatty acid ester, polyoxyethylene sorbitol fatty acid ester, polyoxyethylene alkyl ether, polyoxyethylene alkenyl ether, polyoxyethylene Examples include oxyethylene polyoxypropylene glycol, polyoxyethylene polyoxypropylene alkyl ether, polyoxyethylene polyoxypropylene alkenyl ether, polyethylene glycol fatty acid ester, polyoxyethylene castor oil, polyoxyethylene hydrogenated castor oil, polyglycerin fatty acid ester It is done. A nonionic surfactant can be used 1 type or in combination of 2 or more types.
As the nonionic surfactant, polyoxyethylene sorbitol fatty acid ester is preferable from the viewpoint of enhancing the warm bath effect in combination with carbon dioxide gas. The polyoxyethylene sorbitol fatty acid ester preferably has an average added mole number of ethylene oxide of 20 or more and 70 or less. The polyoxyethylene sorbitol fatty acid ester is preferably a fatty acid having 12 to 18 carbon atoms. The fatty acid is preferably oleic acid.

  The granulated product obtained in the present invention has an organic acid content of 30% by mass or more and 70% by mass or less, and a mass ratio of the organic acid to the nonionic surfactant is 5 or more and 25 or less. Considering this, the amount of the organic acid and the nonionic surfactant used in step 1 can be set.

  Step 1 may be a step of mixing 5 parts by mass or more and 25 parts by mass or less of an organic acid with respect to 1 part by mass of the nonionic surfactant and the nonionic surfactant. This is preferable when the entire amount of the nonionic surfactant is used in step 1 from the viewpoint of the fluidity and strength of the granulated product.

The mixing of the organic acid and the nonionic surfactant in step 1 can be performed using a suitable mixer. The mixer is preferably equipped with a heatable jacket, and is preferably heated to a predetermined temperature during and / or after charging.
The mixer may be an apparatus that does not give a large amount of compaction by applying strong shear during mixing. For example, a drum mixer, a ribbon mixer, a nauter mixer, and the like can be given.

  In the case of using a plurality of types of organic acids, it is preferable to perform mixing for 1 minute to 10 minutes after the preparation of the organic acid.

  The mixing of the organic acid and the nonionic surfactant in step 1 is preferably 5 ° C. or higher, more preferably 10 ° C. or higher, more preferably 20 ° C. or higher, from the viewpoint of shortening the heating time in the subsequent step. The temperature is preferably 60 ° C. or lower, more preferably 50 ° C. or lower, and still more preferably 40 ° C. or lower.

  In the case where the nonionic surfactant is a liquid, it is preferable from the viewpoint of shortening the temperature raising time in the subsequent step that the nonionic surfactant is set to a temperature of 40 ° C. or higher and 60 ° C. or lower in advance. When a powdered nonionic surfactant is added, it may be used at room temperature.

  From the viewpoint of uniformly adding and mixing the nonionic surfactant, the mixing machine charged with the organic acid is preferably stirred for 0.5 minutes or more, more preferably 1 minute or more, even more preferably 3 minutes or more, The nonionic surfactant is added preferably over 20 minutes, more preferably over 15 minutes, and even more preferably over 10 minutes. The addition of the nonionic surfactant in step 1 may be performed continuously or intermittently.

  In step 1, it is preferable from the viewpoint of the fluidity and strength of the granulated product that the total amount of the organic acid blended in the granulated product is mixed with the nonionic surfactant.

  In Step 1, among the total amount of the nonionic surfactant blended in the granulated product, it is preferably 50% by mass or more, more preferably 60% by mass or more, still more preferably 70% by mass or more, and 100% by mass. % Or less nonionic surfactant is preferably mixed with the organic acid from the viewpoint of the fluidity and strength of the granulated product. You may use the whole quantity of the nonionic surfactant mix | blended with a granulated material, ie, 100 mass%, at the process 1. FIG.

(Process 2)
Step 2 is a step of mixing the water-soluble binder with the mixture obtained in Step 1 and granulating the mixture to obtain a granulated product.

  The water-soluble binder is a component mainly for increasing the strength of the granulated product in the production of the granulated product. In addition, the organic acid is coated with the water-soluble binder, so that the organic acid and the carbonate in the granulated product are prevented from contacting and reacting during storage, and the packaging container expands due to the generation of carbon dioxide gas. Can be prevented.

The water-soluble binder is preferably thermoplastic from the viewpoint of the suitability for production of the granulated product. The water-soluble binder is preferably mixed in a liquid. The water-soluble binder is preferably not mixed with an aqueous solution.
As the water-soluble binder, polyethylene glycol, polypropylene glycol, polyoxyethylene alkyl ether, and polyoxyethylene phenol ether are preferable, and polyethylene glycol and polypropylene glycol are more preferable.

  In addition, the number average molecular weight of the water-soluble binder is preferably 4,000 or more, more preferably 6,000 or more, by the GPC method using polystyrene as a standard from the viewpoints of viscosity adjustment and handling properties when granulating. 7,000 or more, more preferably 20,000 or less, more preferably 13,000 or less, and still more preferably 9,000 or less. When measuring the molecular weight of polyethylene glycol, water / ethanol is used as the solvent.

  When these water-soluble binders are used, two or more water-soluble binders having different average molecular weights may be used in combination.

  In step 2, the water-soluble binder has a mass ratio of the organic acid to the water-soluble binder of preferably 1 or more, more preferably 3 or more, and preferably 6 or less, from the viewpoint of fluidity and strength of the granulated product. More preferably, it is mixed so that it becomes 5.5 or less.

  In step 2, a nonionic surfactant can be mixed. The nonionic surfactant mixed in Step 2 may be the same as or different from Step 1, but is preferably the same. When mixing the nonionic surfactant in the step 2, the ratio of the nonionic surfactant mixed in the step 1 among all the nonionic surfactants blended in the granulated product is preferably 50% by mass or more, More preferably, it is 60 mass% or more, More preferably, it is 70 mass% or more, Preferably it is 100 mass% or less, More preferably, it is 90 mass% or less, More preferably, it is 80 mass% or less.

In step 2, oily components can be mixed. The oil component is preferably not mixed in Step 1.
The oil component is preferably liquid at 40 ° C. from the viewpoint of dispersibility in bath water and the like. This means that even if it contains a solid or semi-solid oily component alone at 40 ° C., the whole oily component may be liquid.

  When the oily component is one having a carbon dioxide oil phase / water phase distribution ratio of 1.1 or more, when the granulated product is used as a granulated product for bathing, the carbon dioxide generated in the bath is the oily component. Since it is present at a higher concentration, it is preferable because a high concentration of carbon dioxide gas can be supplied to the skin and the warming effect after bathing can be further enhanced. A more preferable distribution ratio is 1.3 or more, further preferably 1.5 or more, particularly preferably 1.6 or more, and further preferably 1.7 or more. The distribution ratio of carbon dioxide gas to the oil phase / water phase can be measured by the method described in paragraph [0060] of JP-A-2007-223936.

Oil components include cetyl octanoate, cetyl isooctanoate, myristyl lactate, cetyl lactate, isopropyl myristate, myristyl myristate, isocetyl myristate, octyldodecyl myristate, isopropyl palmitate, isostearyl palmitate, isopropyl adipate, stearin Fatty acid esters such as butyl acid, isocetyl stearate, isostearyl isostearate, isotridecyl isononanoate, decyl oleate, and cholesterol isostearate;
Fatty acid triglycerides such as tri (caprylic acid / capric acid) glycerin and glyceryl tricaprylate;
Soybean oil, nutca oil, jojoba oil, avocado oil, almond oil, olive oil, cacao butter, sesame oil, persic oil, castor oil, coconut oil, mink oil, beef tallow, pork fat and other natural fats and oils, and hydrogenation of these natural fats and oils Hardened oils obtained and glycerides such as myristic acid glyceride and 2-ethylhexanoic acid glyceride;
Hydrocarbon oils such as liquid paraffin, petrolatum, paraffin, microcrystalline wax, ceresin, squalane, squalene, dioctylcyclohexane, bristan;
Higher fatty acids such as lauric acid, myristic acid, palmitic acid, stearic acid, behenic acid, oleic acid, linoleic acid, linolenic acid, lanolinic acid, isostearic acid;
Higher alcohols such as lauryl alcohol, cetyl alcohol, stearyl alcohol, oleyl alcohol, cholesterol, 2-hexyldecanol;
Peppermint oil, jasmine oil, pepper brain oil, cypress oil, spruce oil, ryu oil, turpentine oil, cinnamon oil, bergamot oil, mandarin oil, ginger oil, pine oil, lavender oil, bay oil, clove oil, hiba oil, Rose oil, eucalyptus oil, lemon oil, thyme oil, peppermint oil, rose oil, sage oil, menthol, cineole, eugenol, citral, citronellal, borneol, linalool, gellerall, camphor, thymol, spirantol, pinene, limonene, terpene Essential oils such as compounds;
Silicone oil etc. are mentioned.

  The distribution ratio is a distribution ratio of a mixture of two oily components. Accordingly, even if the oil component alone has a distribution ratio of less than 1.1, it can be mixed with other oil components to make the distribution ratio 1.1 or more.

  Among the oil components, those having a partition ratio of 1.7 or more alone include jojoba oil, squalene, isopropyl myristate, isocetyl myristate, isopropyl palmitate, isocetyl stearate, cetyl isooctanoate, isotridecyl isononanoate and dioctyl. Examples include cyclohexane, tri (caprylic acid / capric acid) glycerin, and glyceryl tricaprylate.

  As the oil component, those having the distribution ratio of 1.7 or more alone and the distribution ratio of 1.1 or more are preferable.

  The oil component is preferably mixed in an amount of 20 to 60 parts by mass of organic acid with respect to 1 part by mass of the oil component.

  Mixing of the mixture obtained in step 1, the oil component, and the water-soluble binder may be performed in the same mixer as in step 1 or may be performed in another mixer. In the same mixer, mixing in step 1 and mixing in step 2 can be performed continuously.

  In the method for producing a granulated product of the present invention, at least one of Step 1 and Step 2, one or more components selected from saccharides and inorganic salts can be mixed. These components can improve the disintegration property of the granulated product, and can improve the solubility in bath water when used as a bath agent.

Saccharides are preferably added after Step 2 or Step 2, and more preferably after Step 2, from the viewpoint of surface modification of the mixture.
Examples of the saccharide include glucose, fructose, lactose, maltose, sucrose, dextrin, maltodextrin, cyclodextrin, and trehalose.
The granulated product produced according to the present invention preferably contains saccharides in an amount of 0.1% by mass or more, more preferably 1% by mass or more, still more preferably 3% by mass or more, and preferably 20% by mass or less. Is contained in an amount of 15% by mass or less, more preferably 10% by mass or less. The amount of sugars to be mixed is adjusted so as to have this content.

The inorganic salt is preferably added in step 1 from the viewpoint of uniform mixing.
As the inorganic salt, an inorganic salt other than carbonate is used. Inorganic salts include inorganic sulfates, inorganic chlorides, inorganic phosphates, inorganic nitrates, and the like. Specific examples include sodium sulfate, magnesium sulfate, sodium chloride, magnesium chloride, potassium chloride, magnesium oxide, sodium thiosulfate, sodium polyphosphate, sodium phosphate, potassium nitrate, and sodium nitrate.
The granulated product produced according to the present invention preferably contains an inorganic salt, preferably 0.1% by mass or more, more preferably 1% by mass or more, still more preferably 3% by mass or more, and preferably 70% by mass or less. Preferably it is 50 mass% or less, More preferably, it contains 30 mass% or less. The amount of the inorganic salt to be mixed is adjusted so as to have this content.

In the granulated product of the present invention, in addition to the saccharides and inorganic salts, components usually used for bath agents may be appropriately contained within a range not impairing the effects of the present invention. Such ingredients include:
Water-soluble polymers such as cellulose derivatives such as polypropylene glycol, polyoxyethylene phenol ether and hydroxyethyl cellulose;
Monohydric alcohols such as ethanol, stearyl alcohol, isopropyl alcohol, cetyl alcohol, hexadecyl alcohol;
Polyhydric alcohols such as glycerin, propylene glycol and sorbitol;
Examples include excipients such as calcium silicate, medicinal ingredients such as herbal medicines, pigments, and fragrances.

  For granulation of a mixture of oily components and water-soluble binder, pelleter double, dome gran, twin dome gran, disc pelleter (Dalton Co., Ltd.), basket type granulator (Kikusui Seisakusho Co., Ltd.) In addition to known extrusion granulators such as), a rolling granulator or the like can be used, but it is preferable to perform extrusion granulation using an extrusion granulator. Further, from the viewpoint of suppressing granulation of the granules, it is preferable to perform extrusion granulation using a dome gran or twin dome gran which is a push-type extrusion granulator.

The hole diameter of the screen when using an extrusion granulator is preferably 0.3 mm or more, more preferably 0.5 mm or more, still more preferably 0.7 mm or more, and preferably 2.0 mm or less, more preferably 1 0.0 mm or less. By using such a screen, a cylindrical or noodle-shaped granulated product can be obtained.
The temperature of the mixture charged into the granulator during extrusion granulation is preferably 40 ° C or higher, more preferably 45 ° C or higher, further preferably 50 ° C or higher, and preferably 90 ° C from the viewpoint of granulation capability. Hereinafter, it is more preferably 75 ° C. or less, and further preferably 60 ° C. or less.

  The obtained granulated product can be cooled to suppress coalescence and agglomeration, and then can be sized as necessary. As a machine used for sizing, a known crusher (or crusher) can be used. For example, a high speed mixer (Fukae Powtech Co., Ltd.), Malmerizer (Dalton Co., Ltd.), Examples include Spirer Flow (manufactured by Freund Sangyo Co., Ltd.), Fitzmill (manufactured by Dalton Co., Ltd.), Power Mill (manufactured by Paulek Co., Ltd.), Comil (manufactured by Quadro), and the like.

  The average particle size of the granulated product obtained by the present invention is 0.5 mm or more, preferably 0.6 mm or more, from the viewpoint of granulation property and handling property, and 1.0 mm or less from the viewpoint of solubility in bath water. , Preferably less than 0.9 mm. The average particle diameter of the granulated product is measured by the method described in the examples.

  The bulk density (apparent density) of the granulated product obtained by the present invention is 400 g / L or more, preferably 500 g / L or more, and 900 g / L or less, preferably 800 g, from the viewpoint of solubility in bath water. / L. The bulk density of the granulated product is measured by the method described in the examples.

  The granulated product obtained by the present invention has an organic acid content of 30% by mass or more, preferably 40% by mass or more, more preferably 50% by mass or more, and 70% by mass or less, preferably less than 70% by mass. More preferably, it is 69 mass% or less, More preferably, it is 68 mass% or less.

  In addition, the granulated product obtained by the present invention has a mass ratio of organic acid to nonionic surfactant, that is, a mass ratio of organic acid / nonionic surfactant of 5 or more from the viewpoint of a warm bath effect and a skin care effect. , Preferably 8 or more, more preferably 10 or more, and 25 or less, preferably 22 or less, more preferably 20 or less.

An example of a preferable composition of the granulated product obtained by the present invention is as follows. A granulated product having this composition is preferred as a granulated product for bathing agents.
Content of organic acid: 30% by mass or more, preferably 40% by mass or more, more preferably 50% by mass or more, and 70% by mass or less, preferably less than 70% by mass, more preferably 69% by mass or less, still more preferably Is 68 mass% or less. Mass ratio of organic acid / nonionic surfactant: 5 or more, preferably 8 or more, more preferably 10 or more, and 25 or less, preferably 22 or less, more preferably 20 or less. Content: preferably 5% by mass or more, more preferably 10% by mass or more, and preferably 70% by mass or less, more preferably 30% by mass or less. Content of oily component: preferably 0.5% by mass or more, preferably Is 1% by mass or more, and preferably 2.5% by mass or less, more preferably 3.5% by mass or less. Inorganic salt content: preferably 0.1% by mass or more, More preferably 1% by mass or more, further preferably 3% by mass or more, and preferably 70% by mass or less, more preferably 50% by mass or less, still more preferably 30% by mass or less. Sugar content: 0.1% by mass Or more, preferably 1% by mass or more, and preferably 15% by mass or less, more preferably 10% by mass or less.

As an aspect of this invention, it has following process 1 and 2, content of an organic acid is 30 to 70 mass%, and mass ratio of the organic acid with respect to a nonionic surfactant is 5 or more and 25 or less. The manufacturing method of the granulated material for bath agents is mentioned. The matters described in the method for producing a granulated product of the present invention can be appropriately applied to this production method.
Step 1: Step of mixing an organic acid and a nonionic surfactant Step 2: Step of mixing a water-soluble binder with the mixture obtained in Step 1, granulating the mixture, and obtaining a granulated product For example, a granulated product for bathing agent having excellent strength, good fluidity and little generation of fine powder can be obtained.

[Method of manufacturing bath salt]
The method for producing a bath agent composition of the present invention includes the following steps A and B.
Step A: According to the method for producing a granulated product of the present invention, the organic acid and the nonionic surfactant are contained, the organic acid content is 30% by mass or more and 70% by mass or less, and the nonionic surfactant is used. Step B for producing a granulated product having an organic acid mass ratio of 5 or more and 25 or less: Step of mixing the granulated product obtained in Step A and carbonate

  Process A can be implemented by the manufacturing method of the granulated material of this invention, Preferably the manufacturing method of the granulated material for input agents of this invention.

Examples of the carbonate used in the step B include sodium carbonate, potassium carbonate, and sodium hydrogen carbonate from the viewpoint of refining the generated carbon dioxide bubbles, and sodium carbonate (Na ₂ CO ₃ ) is preferable. From the viewpoint of generating fine bubbles, the content of sodium carbonate in the carbonate is preferably 70% by mass or more, more preferably 80% by mass or more, still more preferably 85% by mass or more, and 100% by mass or less. It is preferable. It may be 100% by mass. In addition, when the amount of sodium hydrogen carbonate in the carbonate is increased, the carbon dioxide gas is not preferable because it tends to increase without becoming fine bubbles that are cloudy.
The average particle diameter of the carbonate is preferably 100 μm or more, more preferably 200 μm or more, still more preferably 250 μm or more, and preferably 750 μm or less, from the viewpoints of finer foam, duration of foam, sedimentation and the like. Preferably it is 500 micrometers or less, More preferably, it is 400 micrometers or less.

The content of the granulated product in the bath agent obtained by the present invention is preferably 30% by mass or more, more preferably 40% by mass or more, and still more preferably 50% by mass from the viewpoint of obtaining carbon dioxide generation amount and fine bubbles. % Or more, and preferably 80% by mass or less, more preferably 70% by mass or less.
Further, the content of carbonate in the bath agent obtained by the present invention is preferably 20% by mass or more, more preferably 30% by mass or more, and preferably from the point of obtaining carbon dioxide generation amount and fine bubbles. It is 70 mass% or less, More preferably, it is 60 mass% or less, More preferably, it is 50 mass% or less.
The granulated product and carbonate are mixed so as to have these contents.

  In the method for producing a bath agent of the present invention, components other than the carbonate can be mixed.

  When the granulated product and carbonate are mixed to produce the bath agent, any method may be used as a mixing method as long as the granulated product and carbonate can be mixed substantially uniformly. For example, the above-mentioned mixer may be used for mixing, a V-type blender (manufactured by Paulex Co., Ltd.), a double cone mixer (manufactured by Tokuju Kogyo Co., Ltd.), and a ribbon blender (Hosokawa Micron Co., Ltd.). May be used.

  The bathing agent produced by mixing the granulated product obtained by the production method of the present invention and a carbonate preferably has a 0.01 mass% aqueous solution pH at 25 ° C. of preferably 5 or more, more preferably 5. 5 or more, and preferably 7 or less, more preferably 6.5 or less. If the pH is within this range, the generated carbon dioxide gas is easily dissolved in the bath water, and the effect of promoting blood circulation is enhanced.

  The bath agent produced using the granulated product obtained by the production method of the present invention is a foamable powder bath agent. The bath agent generates a large amount of fine bubbles when dissolved in bath water, and the duration of the bubble generation is long. The generation of fine bubbles can be confirmed from the fact that the bath water rapidly becomes cloudy due to the generated bubbles when 40 to 60 g of bathing agent is dissolved in 180 liters of bath water.

  The foaming powder bath agent is used by dissolving in bath water and generating bubbles of carbon dioxide gas. It can be used as a partial bath such as foot bath and arm bath as well as full body bath such as bath.

The foaming powder bathing agent of the present invention may appropriately contain components usually used in bathing agents as long as the effects of the present invention are not impaired. Such ingredients include:
Inorganic salts such as sodium sulfate, magnesium sulfate, sodium chloride, magnesium chloride, potassium chloride, magnesium oxide, sodium thiosulfate, sodium sulfate, sodium polyphosphate, sodium phosphate, potassium nitrate, sodium nitrate;
Sugars such as glucose, fructose, lactose, maltose, sucrose, dextrin, maltodextrin, cyclodextrin, trehalose;
Water-soluble polymers such as polypropylene glycol, polyoxyethylene phenol ether, cellulose derivatives such as hydroxyethyl cellulose;
Monohydric alcohols such as ethanol, stearyl alcohol, isopropyl alcohol, cetyl alcohol, hexadecyl alcohol;
Polyhydric alcohols such as glycerin, propylene glycol and sorbitol;
Examples include excipients such as calcium silicate, medicinal ingredients such as herbal medicines, pigments, and fragrances.

As an aspect of the present invention, a method for producing a bath agent composition having the following steps A and B can be mentioned. The matters described in the method for producing a granulated product of the present invention and the method for producing a bathing agent of the present invention can be appropriately applied to this production method.
Step A: According to the method for producing a granulated product for bathing agent of the present invention, the organic acid and the nonionic surfactant are contained, the content of the organic acid is 30% by mass or more and 70% by mass or less, and the nonionic interface. Step B for producing a granulated product for bathing agent in which the mass ratio of the organic acid to the activator is 5 or more and 25 or less: a step of mixing the granulated product for bathing agent obtained in step A and the carbonate.

The raw materials and apparatuses used in Examples and Comparative Examples are as follows.
<Raw material>
Organic acid: fumaric acid, manufactured by Kawasaki Kasei Kogyo Co., Ltd. (effective portion 99% or more), average particle size: 130 μm, oil absorption capacity 0.191 mL / g
(Oil absorption capacity)
The oil absorption capacity of the organic acid was measured by the following method. 45 g of organic acid powder was put into an absorption measuring device (S410, manufactured by Asahi Soken Co., Ltd.) and rotated at a driving blade of 200 rpm. A nonionic surfactant (Kao Co., Ltd. Rheodor 440V HLB = 12.6) was added dropwise at a liquid supply rate of 2 ml / min to determine the point (drop amount) at which the maximum torque was reached. The liquid addition amount at the point where the torque becomes 70% of the point where the maximum torque is reached is divided by the amount of powder input to obtain the oil absorption capacity.

Nonionic surfactant: polyoxyethylene (40) sorbitol tetraoleate, “Leodol 440V” manufactured by Kao Corporation Water-soluble binder: polyethylene glycol, “K-PEG6000LA” manufactured by Kao Corporation, number average molecular weight: about 8500
Inorganic salt: Magnesium sulfate, “Magnesium sulfate (dried)” manufactured by Tomita Pharmaceutical Co., Ltd. (effective content 99% or more)
Excipient: Glucose, “Anhydrous Crystal Glucose # 900” manufactured by Nippon Shokuhin Kako Co., Ltd., average particle size 25 μm

<Device>
Mixer: 100 L Nauter mixer (manufactured by Hosokawa Micron Co., Ltd .: NX-1 / rotation speed 90 rpm, fluid number 1.13 / jacket water temperature 60 ° C.)
Extrusion granulator: Twin Dome Gran (Dalton Co., Ltd .: TDG-110 type, φ0.7 mm screen, rotation speed 36 rpm)
Granulator: Comil (Quadro: QC-194S, φ2.4mm)

<Method of measuring physical properties>
(The bulk density)
The bulk density was measured by a method defined by JIS K3362: 2008.

(Particle diameter, fine powder rate)
The particle diameter and the fine powder ratio are determined by calculating the median diameter and fine powder ratio from the mass fraction according to the size of the mesh after vibrating for 5 minutes using a metal mesh sieve having an opening of 2000 to 125 μm described in JIS K8801-1: 2006. Calculated.
More specifically, using a 9-stage standard sieve with a mesh opening of 125 μm, 180 μm, 250 μm, 355 μm, 500 μm, 710 μm, 1000 μm, 1400 μm, and 2000 μm, and stacking them in order from a sieve with a small mesh on the top, 100 g of particles were added from above the 2000 μm sieve, and the lid was capped and attached to a low-tap sieve shaker (manufactured by HEIKO, tapping 156 times / minute, rolling: 290 times / minute) and allowed to vibrate for 5 minutes. Then, the mass of the particles remaining on each sieve and the saucer was measured, and the mass ratio (%) of the particles on each sieve was calculated. The average particle size was determined by accumulating the mass ratio of the particles on the sieve with small openings in order from the saucer, and the total particle size was 50%.
A total mass ratio (%) of the particles of the 250 μm sieve was calculated from the saucer and used as the fine powder rate. It shows that the one where the fine powder rate is smaller is excellent in the dischargeability from the bottle and the granulation property.

(Liquidity)
A bulk density measuring hopper defined by JIS K3362: 2008, in which a granulated material is poured into a cylindrical container (diameter 4 cm) having a volume of 100 mL using a hopper for measuring bulk density and the granulated material is ground at the upper part of the container. The time from the beginning of the flow until the end of the flow was measured. The shorter the time, the better the fluidity.

(Particle strength)
The particle strength of the granulated product was measured by measuring the particle strength at 15 points of the granulated product in a room temperature environment using a particle hardness measuring apparatus Grano (Okada Seiko Co., Ltd.), and using the average value. The particle strength of the granulated product is preferably 140 gf / mm ² or more from the viewpoint of handling.

<Example 1>
The amount of fumaric acid and magnesium sulfate shown in Table 1 was added to a Nauter mixer and mixed for 3.5 minutes.
Polyoxyethylene (40) sorbitol tetraoleate was then added in the amount shown in Table 1 and mixed for 20 minutes (Step 1).
Further, the remaining polyoxyethylene (40) sorbitol tetraoleate and polyethylene glycol were added, mixed for 15 minutes, then glucose was added, mixed for 5 minutes, and the mixture was extracted.
The obtained mixture (input temperature 55 ° C.) was subjected to extrusion granulation using a twin dome gran (manufactured by Dalton: TDG-110 type, φ0.7 mm screen, rotation speed 36 rpm) (step 2).
The extruded granulated product was received in a vat and cooled at 25 ° C., and then granulated with a comil (Quadro: QC-194S, φ2.4 mm) to obtain a granulated product for a bathing agent of Example 1.
The fine granule ratio, fluidity, particle strength, bulk density, and average particle diameter of the obtained granule for bathing agent were measured. The results are shown in Table 1.

<Example 2>
As in Example 1, except that polyoxyethylene (40) sorbitol tetraoleate was used in Step 1 to obtain a granulated product for bathing agents. The fine granule ratio, fluidity, particle strength, bulk density, and average particle diameter of the obtained granule for bathing agent were measured. The results are shown in Table 1.

<Examples 3 and 4>
As in Example 2, except that the composition of the granulated product for bathing agent is as shown in Table 1, a granulated product for bathing agent was obtained. The fine granule ratio, fluidity, particle strength, bulk density, and average particle diameter of the obtained granule for bathing agent were measured. The results are shown in Table 1.

<Comparative Example 1>
As in Example 1, except that polyoxyethylene (40) sorbitol tetraoleate was used in Step 2 to obtain a granulated product for bathing agents. The fine granule ratio, fluidity, particle strength, bulk density, and average particle diameter of the obtained granule for bathing agent were measured. The results are shown in Table 1.

<Comparative example 2>
As in Example 2, except that the composition of the granulated product for bathing agent is as shown in Table 1, a granulated product for bathing agent was obtained. The fine granule ratio, fluidity, particle strength, bulk density, and average particle diameter of the obtained granule for bathing agent were measured. The results are shown in Table 1.

In Examples 1 to 4, a granulated product for bathing agent having excellent strength of the granulated material, good fluidity and little generation of fine powder was obtained.
In Comparative Example 1, since the nonionic surfactant was not added in Step 1, there was no fluidity of the granulated product, and a lot of fine powder was generated.
In Comparative Example 2, since the mass ratio of the organic acid to the nonionic surfactant exceeded 25, the strength of the granulated product was low, there was no fluidity, and many fine powders were generated.

Claims (8)

A method for producing a granulated product having the following steps 1 and 2, wherein the organic acid content is 30% by mass or more and 70% by mass or less, and the mass ratio of the organic acid to the nonionic surfactant is 5 or more and 25 or less. .
Step 1: Step of mixing an organic acid and a nonionic surfactant Step 2: Step of mixing a water-soluble binder with the mixture obtained in Step 1, granulating the mixture, and obtaining a granulated product   The manufacturing method of the granulated material of Claim 1 whose granulated material is the granulated material for bathing agents.   The manufacturing method of the granulated material of Claim 1 or 2 whose mass ratio of the organic acid with respect to a water-soluble binder is 1-6.   The manufacturing method of the granulated material in any one of Claims 1-3 in which a granulated material contains 0.1 mass% or more and 70 mass% or less of inorganic salt.   The method for producing a granulated product according to any one of claims 1 to 4, wherein a nonionic surfactant is mixed in Step 2.   The production of the granulated product according to claim 5, wherein the ratio of the nonionic surfactant mixed in Step 1 is 50% by mass or more and 90% by mass or less among all the nonionic surfactants to be blended in the granulated product. Method.   The manufacturing method of the granulated material of any one of Claims 1-6 which mixes 1 or more types of components chosen from saccharides and an inorganic salt in at least any one of the process 1 and the process 2. The manufacturing method of the bath agent composition which has the following process A and B.
Process A: By the manufacturing method of the granulated material of any one of Claims 1-7, an organic acid and a nonionic surfactant are contained, and content of an organic acid is 30 mass% or more and 70 mass% or less. Step B for producing a granulated product in which the mass ratio of the organic acid to the nonionic surfactant is 5 or more and 25 or less: the step of mixing the granulated product obtained in Step A and the carbonate