JP5291922B2 - Lipophilic component-containing powder - Google Patents

Description

  The present invention relates to a lipophilic component-containing powder and a method for producing the same.

  The lipophilic component-containing powder obtained by making the lipophilic component into an emulsion containing an excipient (water-soluble wall material) and then drying the emulsion has a lipophilic component in the powder. Since it is retained / encapsulated in the matrix of the material, even a highly volatile lipophilic component typified by a perfume has little volatilization during storage and excellent flavor sustainability. In addition, even when an external force load such as compaction / molding is applied, the lipophilic component hardly permeates and is excellent in powder processing. Furthermore, since the powder is emulsified when dissolved in water, it is very convenient when spraying a pesticidal active ingredient typified by an agrochemical.

  On the other hand, when the powder is dissolved and used, a stable emulsified state may not be maintained depending on the dissolving environment. For example, fertilizers and the like contain inorganic salts and require salt resistance. In addition, the carbon dioxide generating bath agent is required to be able to withstand the load caused by foaming and pH (weak acidity) change in the hot water bath. In such an environment, a polyoxyalkylene (2 to 3 carbon atoms of alkylene group) -based nonionic surfactant (hereinafter sometimes simply referred to as a polyoxyalkylene-based nonionic surfactant) is mixed with a lipophilic component. It is known that the lipophilic component maintains a stable emulsified state. However, when preparing a lipophilic component-containing powder containing a polyoxyalkylene nonionic surfactant, the emulsion becomes unstable in the presence of an excipient, making it difficult to prepare the powder. As a technique for solving this problem, Patent Document 1 discloses a technique in which a fine emulsified liquid can be produced not only by a simple stirring but also by adding an anionic active agent to an emulsion. ing.

  On the other hand, when the proportion of the lipophilic component containing the polyoxyalkylene nonionic surfactant contained in the powder is increased, particularly when this proportion is 35% by weight or more, external load such as compaction / molding is applied. When applied, there has been a problem that the lipophilic component tends to exude.

JP 2006-77001 A

  A lipophilic component obtained by making a lipophilic component containing a polyoxyalkylene nonionic surfactant as described above into an emulsion containing an excipient (water-soluble wall material) and then drying the emulsion. The contained powder is excellent in powder processing even if it is subjected to external force loads such as compaction / molding, and is excellent in powder processing. However, when the inclusion is in liquid form, these physical properties increase as the ratio increases. Tend to be damaged. On the other hand, there is a desire to increase the content of lipophilic components including polyoxyalkylene-based nonionic surfactants from the viewpoint of production efficiency and design freedom when finishing a powder as an intermediate product.

  In order to solve this problem, attention was paid to the state in which the lipophilic component is retained in the powder. That is, it is known that the strength of a material having voids inside is improved by reducing the size of the voids as much as possible as seen in the honeycomb structure. Therefore, in the powder obtained by spray-drying the O / W emulsion, it is considered preferable to make the dispersion diameter of the lipophilic component retained in the matrix formed by the water-soluble wall material fine. In order to obtain a powder having such a shape, (1) when producing an O / W emulsion, obtaining oil droplets of fine lipophilic components, (2) when spray-drying the O / W emulsion In addition, it is easy to prevent coalescence of the lipophilic component oil droplets and keep them in a matrix formed by the water-soluble wall material while being fine, and the step (1) for obtaining the oil droplets of the fine lipophilic component is simple. It is preferable to be obtained by a simple operation. It is necessary to solve the above two problems.

  As described above, when the lipophilic component containing the polyoxyalkylene-based nonionic surfactant is made into an emulsion containing an excipient (water-soluble wall material) using an anionic surfactant, simple stirring is used. Oil droplets of a stable and fine lipophilic component can be easily obtained. However, it was found that when the emulsion was spray-dried to produce a powder, the oil droplets of the lipophilic component were not kept fine. In such a case, when the content of the lipophilic component including the polyoxyalkylene-based nonionic surfactant in the powder is low, exudation of the liquid material is suppressed when a load is applied, but When the rate is high, the bleeding becomes remarkable due to insufficient strength of the matrix.

  As described above, (1) when making an O / W emulsion, oil droplets of a fine lipophilic component are obtained, and (2) when the O / W emulsion is spray-dried, A powder that satisfies the two conditions of preventing coalescence of oil droplets and maintaining it in a matrix formed of a water-soluble wall material while being fine, and containing a high amount of a lipophilic component containing a polyoxyalkylene nonionic surfactant The technology to manufacture is anxious.

  The problem of the present invention is that the lipophilic component is easily stable and minute even in the excipient-containing state, and even if the content of the lipophilic component including the polyoxyalkylene nonionic surfactant in the powder is high. It can be made into emulsified oil droplets, and when it is pulverized, it can finely hold oil droplets of lipophilic components, and even if it is subjected to external force load such as compaction / molding, it does not easily leak out and contains lipophilic components It is providing the powder and its manufacturing method.

  The present inventors can use a specific anionic surfactant in combination with a lipophilic component containing a polyoxyalkylene-based nonionic surfactant so that it is stable and minute even in an excipient-containing state. O / W emulsion containing fine emulsified oil droplets is obtained, and when O / W emulsion in which lipophilic components are emulsified in fine oil droplets is pulverized by spray drying, coalescence of oil droplets is prevented and fine It was found that a lipophilic component-containing powder having excellent processability can be obtained because it is held in a matrix formed by a water-soluble wall material as it is, and even if an excessive load is applied, the lipophilic component is hardly exuded.

  That is, the present invention comprises (A) a lipophilic component, (B) a polyoxyalkylene (a C2-C3 alkylene group) nonionic surfactant, (C) an alkylpolyester represented by the general formula (I) Oxyethylene acetate (hereinafter referred to as alkylpolyoxyethylene acetate (I)), (D) a lipophilic component-containing powder obtained by drying an O / W emulsion containing an excipient and water, and ( E) A lipophilic component-containing powder containing at least one selected from fatty acids and (F) fatty acid soaps, a method for producing the same, and a tableted product obtained by tableting the powder containing the lipophilic component-containing powder. To do.

R ¹ —O— (CH ₂ CH ₂ O) _n —CH ₂ COOM (I)
[Wherein, R ¹ is a hydrocarbon group having 10 to 25 carbon atoms, M is H or a cation, and n is a number of 1 to 40 indicating the average number of added moles of an oxyethylene group. ]

  According to the present invention, the lipophilic component containing a polyoxyalkylene nonionic surfactant is made into an emulsion containing an excipient (water-soluble wall material) using alkyl polyoxyethylene acetate (I). Therefore, it can be easily made into fine oil droplets. Further, when the emulsion is pulverized by spray drying, coalescence of oil droplets can be prevented, and the lipophilic component can be held in a matrix formed by the water-soluble wall material while being fine. As a result, even if the content of the lipophilic component including the polyoxyalkylene-based nonionic surfactant in the powder is high or an excessive load is applied, the lipophilic component is difficult to ooze out and has excellent processability. An oil component-containing powder can be obtained. In addition, when the lipophilic component is a cosmetic oil component or an agrochemical active component, the lipophilic component becomes stable fine oil droplets when dissolved, so that it is possible to exhibit a transparent appearance and enhance its efficacy.

[(A) component]
The component (A) is a lipophilic component that is pulverized according to the present invention, and the lipophilic component refers to one having a solubility in water at 25 ° C. of less than 10% by weight. The lipophilic component is not particularly limited, but, for example, fragrance, agrochemical activator, fats and oils, waxes, hydrocarbons, higher fatty acids, higher alcohols, aliphatic amines, esters, oily Medicinal ingredients, silicone oils and the like can be mentioned.

  Perfumes include fragrances such as menthol and crocodile, citrus such as orange, lemon and grapefruit, fruits such as apple, teas such as tea and green tea, beans such as coffee, spices such as black pepper and curry , Flavors such as peppermint, spearmint, daily flavors, vanillas, cola nuts, essential oils, and extracts.

  Pesticide activators include fenthion, fenitrothion, propaphos, cyanophos, prothiofos, sulprofos, EPN, cyanofenphos, oxydeprofos ), Disulfoton, thiometon, marathion, mecalbam, pirimiphosmethyl, diazinon, etrimfos, isoxathion, pyroxalophos, chlorthiophos ), Isofenphos, EDDP, cyfluthrin, permethrin, cyhalothrin, fenvalerate, flucythrinate, etofenpro Ethofenprox, silaneophane, cycloprothrin, IBP, edifenphos, propiconazole, imazalil, tridemorph, etazol, pyrifenox ( pyrifenox, butachlor, metolachlor, thiobencarb, butylate, EPTC, molinate, sethoxydim, fluazifop-butyl, lactofen ), Piperophos, esprocarb, pyributicarb, benoxazol and the like.

  Examples of the fats and oils include soybean oil, nutka 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. Examples thereof include hardened oil obtained by hydrogenating natural fats and oils and synthetic triglycerides such as myristic acid glyceride and 2-ethylhexanoic acid glyceride. Examples of the waxes include carnauba wax, whale wax, beeswax and lanolin. Examples of the hydrocarbons include liquid paraffin, ceramide, retinoid, petrolatum, paraffin microcrystalline wax, ceresin, squalane and pristane. Examples of higher fatty acids include lauric acid, myristic acid, palmitic acid, stearic acid, arachidic acid, behenic acid, oleic acid, linoleic acid, linolenic acid, lanolinic acid, and isostearic acid. Examples of higher alcohols include lauryl alcohol, cetyl alcohol, stearyl alcohol, oleyl alcohol, lanolin alcohol, cholesterol, 2-hexyldecanol and the like. Examples of aliphatic amines include laurylamine, stearylamine, oleylamine and the like. Examples of the esters include cetyl octanoate, myristyl lactate, isopropyl myristate, octyldodecyl myristate, isopropyl palmitate, isopropyl adipate, butyl stearate, decyl oleate, and isostearyl isostearate. As an oily medicinal ingredient, the following formula (II)

(In the formula, R ² represents a hydroxyl group or a methoxy group, R ³ , R ⁴ and R ⁵ represent a hydrogen atom, and R ⁶ represents an alkyl group.)
And nicotinic acid methyl nicotinate, tocopherol nicotinate, tocopherol, L-menthol, guaiazulene and the like. Examples of silicone oils include dimethylpolysiloxane, decamethylcyclopentasiloxane, methylphenylpolysiloxane, alkyl acrylate copolymer methylpolysiloxane ester, and the like.

  Among these components (A), fragrances, agricultural chemical activators, ceramides, liquid paraffin, ester oils, higher alcohols, cosmetic oily ingredients such as oily medicinal ingredients, higher fatty acids, and silicone oils are preferred. These components (A) may be used in combination of two or more as required.

[Component (B)]
The component (B) is a nonionic surfactant having a polyoxyalkylene chain (alkylene group having 2 to 3 carbon atoms). The polyoxyalkylene chain may be a polyoxyethylene chain, a polyoxypropylene chain, or a polyoxyalkylene chain in which an oxyethylene group and an oxypropylene group are mixed. In this case, the oxyethylene group and the oxypropylene group may be random or block. .

  Examples of the component (B) include polyoxyethylene alkyl aryl ether, polyoxyethylene sorbite tetraoleate, polyoxyethylene sorbitan monoalkylate, polyoxyethylene sorbitan trichelate, polyoxyethylene nonylphenyl ether, polyoxyalkylene ( Examples thereof include C2-C3 alkyl ethers of alkylene groups, polyoxyethylene hydrogenated castor oil, polyoxyethylene polyoxypropylene glycol and the like. In particular, from the viewpoint of dispersion / dissolution in component (A), those having an HLB of 20 or less are preferred, and those having an HLB of 17 or less are more preferred. Moreover, you may use (B) component in combination of 2 or more type as needed.

  The (A) component and the (B) component change to changes such as salt, pH, and temperature when obtaining an O / W emulsion containing stable and fine emulsified oil droplets and when the lipophilic component-containing powder is dissolved. On the other hand, in order to exist as stable fine oil droplets, it is preferable to mix and dissolve in advance. The total content of the component (A) and the component (B) in the powder of the present invention is 20% by weight from the viewpoint of economy, the necessary amount for blending the same amount of lipophilic component, and the degree of freedom of the product form. The above is preferable, 30% by weight or more is more preferable, and 35% by weight or more is further preferable. Further, from the viewpoint of oil retention (preventing oil seepage), it is preferably 80% by weight or less, more preferably 70% by weight or less, and still more preferably 55% by weight or less. Therefore, from the viewpoints of economy, ease of intake, and oil retention, the total content of the component (A) and the component (B) is preferably 20 to 80% by weight, preferably 30 to 70% by weight in the powder of the present invention. % Is more preferable, and 35 to 55% by weight is still more preferable. (A) / (B) = 1-10 are preferable and, as for the weight ratio of (A) component and (B) component, 1.5-4 are more preferable.

[Component (C)]
The component (C) is an emulsifier for emulsifying the component (A) in the fine oil droplets together with the component (B), and is an alkyl polyoxyethylene acetate represented by the general formula (I).

In the general formula (I), R ¹ represents a hydrocarbon group having 10 to 25 carbon atoms, and the hydrocarbon group may be linear or branched, and may be saturated or unsaturated. R ¹ is preferably an alkyl group having 10 to 22 carbon atoms. M represents H or a cation, and examples of the cation include alkali metals such as sodium and potassium, and cations such as ammonium and alkanolamine. n is a number of 1 to 40 indicating the average number of added moles of oxyethylene groups, and a number of 3 to 25 is preferable.

  The content of the component (C) in the powder of the present invention is preferably 0.01% by weight or more, and more preferably 0.05% by weight or more from the viewpoint of emulsion stability. Moreover, from a viewpoint of cost, the freedom degree of a mixing | blending, and emulsion stability, 10 weight% or less is preferable and 5 weight% or less is more preferable. Therefore, from the viewpoint of emulsion stability, the degree of freedom of blending, and cost, the content of the component (C) is preferably 0.01 to 10% by weight and more preferably 0.05 to 5% by weight in the powder.

[(D) component]
The component (D) is a water-soluble wall material used as an excipient for fixing the component (A) and forming particles. As component (D), glucose, fructose, lactose, maltose, sucrose, dextrin, maltodextrin, cyclodextrin, maltose, fructose, trehalose and other monosaccharides, disaccharides and polysaccharides; sorbitol, mannitol, maltitol, lactose, Sugar alcohols such as maltotriitol, xylitol, polyhydric alcohols; thickening polysaccharides such as gum arabic, guar gum, pectin, pullulan and sodium alginate; cellulose derivatives such as methylcellulose and sodium carboxymethylcellulose; esterification and etherification treatment to starch , Starch derivatives subjected to terminal reduction treatment; processed starch, gelatin degradation product, agar, polyvinyl alcohol and the like. Moreover, you may use (D) component in combination of 2 or more type as needed.

  The content of the component (D) in the powder of the present invention is preferably 20% by weight or more, more preferably 30% by weight or more from the viewpoint of preventing the lipophilic component from exuding. Moreover, from a viewpoint of cost and the freedom degree of a mixing | blending, 65 weight% or less is preferable and 60 weight% or less is more preferable. Therefore, the content of the component (D) is preferably 20 to 65% by weight and more preferably 30 to 60% by weight in the powder from the viewpoint of preventing the oleophilic component from bleeding, the degree of freedom of blending, and the cost.

[(E) component]
The component (E) is a fatty acid that is blended for the purpose of eliminating foam generated when the lipophilic component-containing powder is dissolved. In particular, when a lipophilic component-containing powder is used in a carbon dioxide-generating bath, foam derived from the active agent remains on the hot water surface when dissolved, but here, as part or all of the component (A) When the component (E) is used, foam residue can be avoided due to the defoaming effect.

  Component (E) is a fatty acid having a hydrocarbon group having 8 to 24 carbon atoms, preferably an alkyl group or an alkenyl group (lauric acid, myristic acid, palmitic acid, stearic acid, arachidic acid, behenic acid, oleic acid, linol. Acid, linolenic acid, lanolinic acid, isostearic acid, etc.). Of these, saturated fatty acids are preferred. Moreover, you may use (E) component in combination of 2 or more type as needed.

  The content of the component (E) in the powder of the present invention is preferably 0.05% by weight or more, and more preferably 0.25% by weight or more from the viewpoint of the defoaming effect. Further, from the viewpoint of oil retention (preventing oil seepage), it is preferably 80% by weight or less, more preferably 70% by weight or less, and still more preferably 55% by weight or less.

[(F) component]
(F) component is fatty acid soap mix | blended in order to eliminate the foam produced at the time of melt | dissolution of the lipophilic component containing powder. In particular, when a lipophilic component-containing powder is used in a carbon dioxide-generating bath, foam derived from the active agent remains on the surface of the hot water when dissolved. The rest can be avoided

  As the component (F), for example, a fatty acid soap having a hydrocarbon group having 8 to 24 carbon atoms, preferably an alkyl group or an alkenyl group (lauric acid soap, myristic acid soap, palmitic acid soap, stearic acid soap, behenic acid soap Oleic acid soap, linoleic acid soap, linolenic acid soap, lanolinic acid soap, isostearic acid soap, and the like, and saturated fatty acid soap is more preferable. Examples of the counter ion include sodium, potassium, ethanolamine and the like. It is preferable to combine two or more fatty acid soaps having different alkyl groups or alkenyl groups. Further, the component (F) may be added in the form of a neutralized product, or may be generated by neutralizing part or all of the component (E) during the production process.

  The content of the component (F) in the powder of the present invention is preferably 0.05% by weight or more, and more preferably 0.1% by weight or more from the viewpoint of the defoaming effect. From the viewpoint of emulsion stability, it is preferably 5% by weight or less, more preferably 3% by weight or less. Therefore, from the viewpoint of the defoaming effect and the emulsion stability, the content of the component (F) is preferably 0.05 to 5% by weight and more preferably 0.1 to 3% by weight in the powder of the present invention.

[Other ingredients]
In addition to the (A) component, the (B) component, the (C) component, the (D) component, the (E) component, and the (F) component, the powder of the present invention contains other substances as necessary. May be. For example, emulsification adjuvants, thickeners, preservatives, colorants, disintegration or antioxidants can be used. Moreover, you may contain the water | moisture content derived from the raw material to be used and a manufacturing process.

  The emulsification aid is an agent for further stabilizing emulsification, and examples thereof include nonionic surfactants. This emulsification aid may be part of the components (A) to (F), or may be an agent selected from other than the components (A) to (F). Examples thereof include glycerin fatty acid ester and sorbitan fatty acid ester.

  The content of the emulsification aid in the powder of the present invention is preferably 0.1% by weight or more, more preferably 1% by weight or more, from the viewpoint of emulsion stability. From the viewpoint of cost, it is preferably 15% by weight or less, and more preferably 10% by weight or less.

[Method for producing lipophilic component-containing powder]
The method for producing the lipophilic component-containing powder of the present invention comprises (A) component (including (E) component if necessary), (B) component, (C) component, (D) component and water, and optionally (F). A step of preparing an O / W type emulsion containing components and other components, and a step of drying the emulsion to obtain a lipophilic component-containing powder.

  O / W type emulsion is composed of (A) component (including (E) component if necessary), (B) component, (C) component, (D) component and water, and optionally (F) component and other components. Prepared by mixing. At this time, it is preferable that the component (A) (including the component (E) if necessary) and the component (B), and if necessary, the component (C) are mixed in advance at the melting point of the mixture or higher. The temperature at which the component (A) (including the component (E) if necessary), the component (B), the component (C), the component (D) and water, and the component (F) and other components as necessary is (A It is desirable that the temperature be higher than the melting point of the mixture of the component (B) and the component (B).

The manufacturing method of the lipophilic component-containing powder of the present invention is preferably a manufacturing method including the following step 1, step 2, step 3 and step 4 from the viewpoint of obtaining finer oil droplets. At this time, the component (C) may be added to the oil phase of Step 1 or the aqueous phase of Step 2, but it is preferably added to the aqueous phase of Step 2. Moreover, you may add (D) component, after mixing an oil phase and a water phase.
Step 1: Preparation of an oil phase containing component (A) and component (B) Step 2: Preparation of an aqueous phase containing component (D) and water Step 3: Prepared in steps 1 and 2 Step 2 for preparing an O / W emulsion by mixing the two liquids Step 4: Step for drying the emulsion obtained in Step 3 to obtain a lipophilic component-containing powder

Among the production methods of the present invention, the production method including the following step 1 ′, step 2 ′, step 3 and step 4 is more preferable from the viewpoint of obtaining finer oil droplets.
Step 1 ′: Step (2): Component (A) (including component (E) if necessary), Component (B), and other components as necessary are mixed to prepare an oil phase Step 2 ′: (C) Step 3: Mixing the component, component (D) and water, and other components as necessary to prepare an aqueous phase Step 3: Mixing the two liquids prepared in Steps 1 and 2, O / W type emulsification Step 4: Preparing the product Step of drying the emulsion obtained in Step 3 to obtain a lipophilic component-containing powder

  As the other component in the step 1 ', an emulsification aid is preferable, and as the other component in the step 2', the component (F) is preferable.

  In step 1 ′, an oil phase is formed by dissolving or dispersing component (B) in component (A) (including component (E) if necessary) and other components such as an emulsification aid in advance. In step 3, an aqueous phase is formed by dissolving (D) component, (C) component and other components such as (F) component if necessary, and in step 3, these oil phase component and aqueous phase component are formed. Are preferably mixed with stirring to prepare an O / W emulsion. The component (D) may be added after mixing the oil phase and the aqueous phase. These steps may be performed while venting an inert gas such as nitrogen when the component (A) is a substance that is easily oxidized.

  As the emulsifier used in Step 3, it is preferable to use a static emulsifier / disperser, a general stirrer, a stirrer emulsifier such as a homomixer, or a high-pressure emulsifier such as a homogenizer.

  The average emulsified oil droplet diameter of the O / W type emulsion according to the present invention is preferably 1 μm or less, more preferably 0.5 μm or less, from the viewpoint of obtaining a powder in which the lipophilic component does not easily exude even when an external force is applied. More preferably, it is 0.2 μm or less. Moreover, 0.001 micrometer or more is preferable.

  In step 4, the O / W emulsion obtained in step 3 is dried to obtain a lipophilic component-containing powder having excellent solubility. As a drying method, a general method can be used, and is not particularly limited, and examples thereof include spray drying, freeze drying, vacuum drying, belt drying, shelf drying, drum drying and the like. When dried by a method other than spray drying, pulverization is performed to obtain particles having a desired particle size. Among these drying methods, it is particularly preferable to use the spray drying method from the viewpoints of productivity, heat history, particle shape, and the like.

  In addition, when the lipophilic component-containing powder is formed by the spray drying method, the particle size can be arbitrarily adjusted by the spray nozzle used, but if necessary, the obtained particles may be further aggregated to form aggregated particles. it can.

  In the method of the present invention, the component (B) and the component (C) are used in combination in the emulsification step, so that the component (A) can be easily made into fine oil droplets in the aqueous solution containing the component (D). . When an emulsion containing such component (A) as fine oil droplets is dried, a powder in which the oil droplets are held in a matrix of a water-soluble wall material while being fine is obtained.

[Lipophilic component-containing powder and tablets]
The lipophilic component-containing powder of the present invention comprises (A) component (including (E) component if necessary), (B) component, (C) component and (D) component, and optionally (F) component and other components. It is a powder excellent in the solubility manufactured by the said manufacturing method.

  The average particle size of the lipophilic component-containing powder of the present invention is preferably 10 to 1000 μm, more preferably 10 to 300 μm from the viewpoint of fluidity and solubility. In addition, this average particle diameter can be measured by the method shown in an Example. The lipophilic component-containing powder of the present invention may be single particles, aggregated particles, or pulverized particles.

  Since the lipophilic component-containing powder of the present invention hardly exudes the lipophilic component even when a load is applied, it can be formed into a molded body such as a granule or a tablet by extrusion granulation, briquetting, tableting or the like.

  The lipophilic component-containing powder of the present invention, for example, in the case of a fragrance in which the oleophilic component is easily volatilized, suppresses volatilization at the time of production, resulting in less fragrance loss and excellent fragrance sustainability. It is suitable for addition to toiletry products such as dishwashing detergents and bath additives. In addition, when the lipophilic component is an agrochemical active agent, a spray solution excellent in solubility and dispersibility can be easily obtained by mixing alone or with a fertilizer. Furthermore, since the lipophilic component-containing powder of the present invention is difficult to ooze out the lipophilic component, it can be easily granulated and tableted, and is highly compatible with diversification of product forms. Illustrative examples include foundations as cosmetics, and pellet-type fertilizers, jumbo agents, solid molding baths and the like as agricultural chemical formulations.

The tableted product of the present invention is obtained by tableting a powder containing the lipophilic component-containing powder of the present invention. The content of the lipophilic component contained in the tableted product of the present invention may be arbitrarily blended according to the amount that the function of the lipophilic component is exhibited, or the lipophilic component-containing powder alone may be used. .
As the components other than the lipophilic component-containing powder in the tableted product, for example, solid-mold bathing agents as shown in the examples are preferable. Tableting is preferably performed by a rotary tableting machine from the viewpoint of productivity.

  The% used in the following examples is% by weight unless otherwise specified. In the following examples, each physical property was measured and evaluated by the following method.

<Average particle size of lipophilic component-containing powder>
The median diameter measured using a laser diffraction / scattering particle size distribution analyzer LA-920 (manufactured by Horiba, Ltd.) was taken as the average particle diameter of the powder. Acetone was used as a dispersion solvent. In the measurement, stirring is set to the middle level (specifically, 4 of 7 stages of the measuring apparatus LA-920), and after adding the sample and adjusting to a predetermined concentration, the intermediate level (specifically, the measuring apparatus LA -920, 7 steps of 4) ultrasonic waves were irradiated for 1 minute, and each diameter was measured.

<Oil droplet holding diameter of lipophilic component-containing powder>
The produced powder was cleaved with a scalpel, 30 were randomly selected from the electron micrograph of the cut section, and the oil droplet retention diameter was determined.

<Absorbance of emulsion>
In the laser diffraction / scattering particle size distribution analyzer LA-920, the emulsified oil droplet diameter was below the lower limit of detection, and could not be detected. The prepared emulsion was directly put into a cell (AB10-UV1.0 manufactured by GL Science Co., Ltd.), and the absorbance at 600 nm was measured with a UV meter (UV-1700 manufactured by Shimadzu Corporation). As a control, ion-exchanged water was put in the same cell. The lower the absorbance, the finer the emulsified oil droplets, and the less the light transmission is inhibited by light scattering.

<Tablet test 1>
As a test to show that the prepared powder has high processability such as granulation and tableting, a filter paper (manufactured by Riken Shokai Co., Ltd.) is placed on a filter paper with 30 g of powder marked with oil-based magic. And observed for magic bleeding when compressed at a pressure of 20 MPa. Less magic blur is preferable in order to avoid troubles such as printing caused by adhesion of lipophilic components and powder to the cocoon in steps such as granulation and tableting.

<Tablet test 2>
When the total content of the component (A) and the component (B) in the lipophilic component-containing powder is large, the tableting resistance was evaluated in the tableting test 2. In a cell of a tableting machine (manufactured by Riken Shokai Co., Ltd.), two No. 5C quantitative filter papers cut to the size of the tableting cell are stacked, two sheets of 31 g of powder kept at 30 ° C. are added, and 10 MPa Compression tableting was performed under pressure. After tableting, the weight of the filter paper on the side not directly in contact with the powder was measured, and the weight of the pre-tested filter paper measured in advance was subtracted to calculate the amount of lipophilic component exuded after tableting. This smaller amount of exudation is preferable in order to avoid troubles such as printing caused by adhesion of lipophilic components and powder to the cocoon in steps such as granulation and tableting, and the standard is preferably 100 mg or less.

<Bathtub dissolution test>
Preparation powder 5.0g, sodium carbonate (made by Central Glass Co., Ltd.) 15.0g, sodium hydrogen carbonate (made by Tosoh Corporation) 15.0g, fumaric acid (made by Nippon Shokubai Co., Ltd.) 31.0g, polyethylene Glycol 6000 (manufactured by Kao Corporation) 6.5 g, citrus fragrance 0.5 g, yellow No. 4 0.015 g, blue No. 1 0.005 g were mixed and tableted at a pressure of 20 MPa. The tableted product was put into a 150 L bath filled with 40 ° C. hot water, and the appearance after dissolution was observed.

Example 1
41.3 g of ECTD-6NEX (polyoxyethylene (6) sodium tridecyl ether acetate manufactured by Nikko Chemicals Co., Ltd.) was added to 2250 g of ion-exchanged water. Thereafter, the mixture was heated to 50 ° C., and 1609 g of H-PDX (reduced water candy manufactured by Matsutani Chemical Industry Co., Ltd.) was added and dispersed / dissolved to prepare an aqueous phase. As an oleophilic component, 550 g of ISIS (isostearyl isostearate manufactured by Higher Alcohol Industry Co., Ltd.), 220 g of Exepal IPP (isopropyl palmitate manufactured by Kao Corporation), and Emulgen 306P (polyoxyethylene stearyl ether manufactured by Kao Corporation, HLB9. 7) 110 g and Nikkor GO-440 (Nikko Chemicals Co., Ltd. tetraoleic acid polyoxyethylene sorbite HLB12.5) 220 g were charged and dispersed / dissolved to prepare an oil phase. An oil phase was added to the obtained aqueous phase, and a stirring operation was performed at 3000 r / min for 30 minutes using a disper stirring blade to obtain an emulsion (50 ° C.). The obtained emulsion was slightly bluish and transparent, and the UV absorbance at 600 nm was 0.0415 ABS.

  The emulsion obtained by the above-described emulsification operation is sprayed using a spray dryer (a spray dryer manufactured by Sakamoto Giken Co., Ltd.) under the conditions of an emulsion supply amount of 7000 g / hr, a blowing temperature of 120 ° C., and an exhaust air temperature of 72 ° C. It dried and obtained ester oil containing powder.

About the ester oil containing powder obtained by the said operation, the tableting test 1 and the bath dissolution test were done. As a result, the blur of the magic after pressurization was slight. Moreover, the hot water after dissolution was very transparent although the lipophilic component was dispersed. Bubbles remained on the bath surface after dissolution.
When the cut surface of the prepared powder was observed with an electron microscope, the oil droplets of the lipophilic component were held very finely as shown in FIG. The holding diameter was 0.05 μm to 0.2 μm.

Example 2
2.69 g of sodium hydroxide (purity 96% manufactured by Kishida Chemical Co., Ltd.) was added to 2000 g of ion-exchanged water, and the temperature was raised to 80 ° C. or higher, and then 10 g of LUNAC S-98 (stearic acid manufactured by Kao Corporation) and LUNAC BA 10 g (behenic acid manufactured by Kao Corporation) was added and neutralized. Then, it cooled to 70 degreeC, ECTD-6NEX (Nikko Chemicals Co., Ltd. polyoxyethylene (6) tridecyl ether sodium acetate) 45g, H-PDX (Matsutani Chemical Industry Co., Ltd. reduced water candy) 1290g and Treha ( 430 g of Hayashibara Co., Ltd. Trehalose) was added and dispersed / dissolved to prepare an aqueous phase. As an oleophilic component, 600 g of ISIS (isostearyl isostearate manufactured by Higher Alcohol Industry Co., Ltd.) and 240 g of Exepal IPP (isopropyl palmitate manufactured by Kao Corporation), 15 g of LUNAC SO-90L (Oleic acid manufactured by Kao Corporation) and Emulgen Charge and disperse / dissolve 120 g of 306P (Polyoxyethylene stearyl ether, HLB 9.7 manufactured by Kao Corporation) and 240 g of Nikkor GO-440 (Tetraoleic acid polyoxyethylene sorbite HLB 12.5 manufactured by Nikko Chemicals Co., Ltd.) An oil phase was prepared. An oil phase was added to the obtained aqueous phase, and an emulsion was obtained by stirring for 30 minutes at 3000 r / min using a disper stirring blade (50 ° C.). The resulting emulsion was very clear and the UV absorbance at 600 nm was 0.0105 ABS.

  The emulsion obtained by the above-described emulsification operation is sprayed using a spray dryer (a spray dryer manufactured by Sakamoto Giken Co., Ltd.) under the conditions of an emulsion supply amount of 7000 g / hr, an air blowing temperature of 150 ° C., and an exhaust air temperature of 95 ° C. It dried and obtained ester oil containing powder.

About the ester oil containing powder obtained by the said operation, the tableting test 1 and the bath dissolution test were done. As a result, there was no oozing of the magic after pressurization, and no exudation of the lipophilic component was observed. Moreover, the hot water after dissolution was very transparent although the lipophilic component was dispersed. Furthermore, no bubbles remained on the bath surface after dissolution.
When the fractured surface of the prepared powder was observed with an electron microscope, the oil droplets of the lipophilic component were kept very fine as shown in FIG. The holding diameter was 0.05 μm to 0.2 μm.

Example 3
2.69 g of sodium hydroxide (purity 96% manufactured by Kishida Chemical Co., Ltd.) was added to 2000 g of ion-exchanged water, and the temperature was raised to 80 ° C. or higher, and then 10 g of LUNAC S-98 (stearic acid manufactured by Kao Corporation) and LUNAC BA 10 g (behenic acid manufactured by Kao Corporation) was added and neutralized. Then, it cooled to 70 degreeC, ECTD-6NEX (Nikko Chemicals Co., Ltd. polyoxyethylene (6) sodium tridecyl ether acetate) 90g, H-PDX (Matsutani Chemical Industry Co., Ltd. reduced water candy) 1491g, and Granu MG 184 g (Dainippon Meiji Sugar Co., Ltd. granulated sugar) was added and dispersed / dissolved to prepare an aqueous phase. As an oleophilic component, 600 g of ISIS (isostearyl isostearate manufactured by Higher Alcohol Industry Co., Ltd.) and 240 g of Exepal IPP (isopropyl palmitate manufactured by Kao Corporation), 15 g of LUNAC SO-90L (Oleic acid manufactured by Kao Corporation) and Emulgen Charge and disperse / dissolve 120 g of 306P (Polyoxyethylene stearyl ether, HLB 9.7 manufactured by Kao Corporation) and 240 g of Nikkor GO-440 (Tetraoleic acid polyoxyethylene sorbite HLB 12.5 manufactured by Nikko Chemicals Co., Ltd.) An oil phase was prepared. An oil phase was added to the obtained aqueous phase, and a stirring operation was performed at 3000 r / min for 30 minutes using a disper stirring blade to obtain an emulsion (50 ° C.). The resulting emulsion was very clear and the UV absorbance at 600 nm was 0.0057 ABS.

  The emulsion obtained by the above-described emulsification operation is sprayed using a spray dryer (a spray dryer manufactured by Sakamoto Giken Co., Ltd.) under the conditions of an emulsion supply amount of 7000 g / hr, an air blowing temperature of 150 ° C., and an exhaust air temperature of 96 ° C. It dried and obtained ester oil containing powder.

About the ester oil containing powder obtained by the said operation, the tableting test 1 and the bath dissolution test were done. As a result, there was no oozing of the magic after pressurization, and no exudation of the lipophilic component was observed. Moreover, the hot water after dissolution was very transparent although the lipophilic component was dispersed. Furthermore, no bubbles remained on the bath surface after dissolution.
When the fractured surface of the prepared powder was observed with an electron microscope, the oil droplets of the lipophilic component were retained very finely as shown in FIG. The holding diameter was 0.05 μm to 0.2 μm.

Comparative Example 1
6.02 g of sodium hydroxide (purity 96% manufactured by Kishida Chemical Co., Ltd.) was added to 2250 g of ion-exchanged water, and the temperature was raised to 80 ° C. or higher, and then 41.25 g of Lunac S-98 (stearic acid manufactured by Kao Corporation) was added. Charged and neutralized. Thereafter, the mixture was cooled to 70 ° C., and 1595 g of H-PDX (reduced water candy manufactured by Matsutani Chemical Industry Co., Ltd.) was added to disperse / dissolve to prepare an aqueous phase. As the lipophilic component, 550 g of ISIS (isostearyl isostearate manufactured by Higher Alcohol Industry Co., Ltd.) and 220 g of Exepal IPP (isopropyl palmitate manufactured by Kao Corporation) and 13.75 g of Lunac SO-90L (Oleic acid manufactured by Kao Corporation) And Emulgen 306P (Polyoxyethylene stearyl ether, HLB 9.7 manufactured by Kao Corporation) and 220 g of Nikkor GO-440 (Tetraoleic acid polyoxyethylene sorbite HLB 12.5 manufactured by Nikko Chemicals Co., Ltd.) were dispersed / dissolved. Thus, an oil phase was prepared. An oil phase was added to the obtained aqueous phase, and a stirring operation was performed at 3000 r / min for 30 minutes using a disper stirring blade to obtain an emulsion (50 ° C.). The obtained emulsion was slightly bluish and transparent, and the UV absorbance at 600 nm was 0.0343 ABS.

  The emulsion obtained by the above-described emulsification operation is sprayed using a spray dryer (a spray dryer manufactured by Sakamoto Giken Co., Ltd.) under the conditions of an emulsion supply amount of 7000 g / hr, a blowing temperature of 120 ° C., and an exhaust air temperature of 73 ° C. It dried and obtained ester oil containing powder.

About the ester oil containing powder obtained by the said operation, the tableting test 1 and the bath dissolution test were done. As a result, the bleeding of the magic after pressing was very large, and the exudation of lipophilic components was observed. Moreover, the hot water after dissolution was very transparent although the lipophilic component was dispersed. Furthermore, no bubbles remained on the bath surface after dissolution.
When the cut surface of the produced powder was observed with an electron microscope, the oil droplets of the lipophilic component were held very large as shown in FIG. The holding diameter was 0.5 μm to 5 μm.

Comparative Example 2
55 g of Amisoft HS21P (N-stearoyl-L-glutamate sodium manufactured by Ajinomoto Co., Inc.) was added to 2250 g of ion-exchanged water. Thereafter, the mixture was heated to 40 ° C., 1595 g of H-PDX (reduced water candy manufactured by Matsutani Chemical Industry Co., Ltd.) was added and dispersed / dissolved to prepare an aqueous phase. As an oleophilic component, 550 g of ISIS (isostearyl isostearate manufactured by Higher Alcohol Industry Co., Ltd.), 220 g of Exepal IPP (isopropyl palmitate manufactured by Kao Corporation), and Emulgen 306P (polyoxyethylene stearyl ether manufactured by Kao Corporation, HLB9. 7) 110 g and Nikkor GO-440 (Nikko Chemicals Co., Ltd. tetraoleic acid polyoxyethylene sorbite HLB12.5) 220 g were charged and dispersed / dissolved to prepare an oil phase. An oil phase was added to the obtained aqueous phase, and a stirring operation was performed at 3000 r / min for 30 minutes using a disper stirring blade to obtain an emulsion (40 ° C.). The resulting emulsion was very clear and the UV absorbance at 600 nm was 0.0010 ABS.

  The emulsion obtained by the above-described emulsification operation is sprayed using a spray dryer (a spray dryer manufactured by Sakamoto Giken Co., Ltd.) under the conditions of an emulsion supply amount of 7000 g / hr, a blowing temperature of 120 ° C., and an exhaust air temperature of 75 ° C. It dried and obtained ester oil containing powder.

About the ester oil containing powder obtained by the said operation, the tableting test 1 and the bath dissolution test were done. As a result, there was a lot of magic blur after pressurization. Moreover, the hot water after dissolution had many bubbles and became turbid. In addition, oil floating was observed over time.
When the cut surface of the produced powder was observed with an electron microscope, oil droplets of the lipophilic component were largely retained as shown in FIG. The holding diameter was 0.2 μm to 0.5 μm.

Comparative Example 3
16.5 g of TCP-5 (Tri-POE (5) cetyl ether phosphoric acid manufactured by Nikko Chemicals Co., Ltd.) was added to 2250 g of ion-exchanged water. Thereafter, the mixture was heated to 60 ° C., and 1633.5 g of H-PDX (reduced water candy manufactured by Matsutani Chemical Industry Co., Ltd.) was added and dispersed / dissolved to prepare an aqueous phase. As an oleophilic component, 550 g of ISIS (isostearyl isostearate manufactured by Higher Alcohol Industry Co., Ltd.), 220 g of Exepal IPP (isopropyl palmitate manufactured by Kao Corporation), and Emulgen 306P (polyoxyethylene stearyl ether manufactured by Kao Corporation, HLB9. 7) 110 g and Nikkor GO-440 (Nikko Chemicals Co., Ltd. tetraoleic acid polyoxyethylene sorbite HLB12.5) 220 g were charged and dispersed / dissolved to prepare an oil phase. An oil phase was added to the obtained aqueous phase, and a stirring operation was performed for 30 minutes at 3000 r / min using a disper stirring blade, but a stable emulsion was not obtained. The mixture was processed at 10,000 r / min for 30 minutes using a mixer to obtain an emulsion (60 ° C.). The obtained emulsion was slightly cloudy, and the UV absorbance at 600 nm was 0.708 ABS.

  The emulsion obtained by the above-described emulsification operation is sprayed using a spray dryer (a spray dryer manufactured by Sakamoto Giken Co., Ltd.) under the conditions of an emulsion supply amount of 7000 g / hr, a blowing temperature of 120 ° C., and an exhaust air temperature of 72 ° C. It dried and obtained ester oil containing powder.

About the ester oil containing powder obtained by the said operation, the tableting test 1 and the bath dissolution test were done. As a result, there was a lot of magic blur after pressurization. Moreover, the hot water after dissolution had many bubbles and became turbid. In addition, oil floating was observed over time.
When the cut surface of the produced powder was observed with an electron microscope, oil droplets of the lipophilic component were largely retained as shown in FIG. The holding diameter was 0.2 μm to 0.7 μm.

Comparative Example 4
1.84 g of sodium hydroxide (purity 96% manufactured by Kishida Chemical Co., Ltd.) was added to 2250 g of ion-exchanged water and the temperature was raised to 60 ° C. or higher, and then DDP-8 (DiPOE (8) C12- manufactured by Nikko Chemicals Co., Ltd.) 41.25 g of C15 alkyl ether phosphoric acid) was added and neutralized. Thereafter, 1608.8 g of H-PDX (reduced water candy manufactured by Matsutani Chemical Industry Co., Ltd.) was added and dispersed / dissolved to prepare an aqueous phase. As an oleophilic component, 550 g of ISIS (isostearyl isostearate manufactured by Higher Alcohol Industry Co., Ltd.), 220 g of Exepal IPP (isopropyl palmitate manufactured by Kao Corporation), and Emulgen 306P (polyoxyethylene stearyl ether manufactured by Kao Corporation, HLB9. 7) 110 g and Nikkor GO-440 (Nikko Chemicals Co., Ltd. tetraoleic acid polyoxyethylene sorbite HLB12.5) 220 g were charged and dispersed / dissolved to prepare an oil phase. An oil phase was added to the obtained aqueous phase, and a stirring operation was performed for 30 minutes at 3000 r / min using a disper stirring blade, but a stable emulsion was not obtained. The treatment was performed at 10,000 r / min for 30 minutes using a mixer to obtain an emulsion (60 ° C.). The obtained emulsion was slightly cloudy, and the UV absorbance at 600 nm was 0.180 ABS.

  The emulsion obtained by the above-described emulsification operation is sprayed using a spray dryer (a spray dryer manufactured by Sakamoto Giken Co., Ltd.) under the conditions of an emulsion supply amount of 7000 g / hr, an air blowing temperature of 120 ° C., and an exhaust air temperature of 74 ° C. It dried and obtained ester oil containing powder.

About the ester oil containing powder obtained by the said operation, the tableting test 1 and the bath dissolution test were done. As a result, there was a lot of magic blur after pressurization. Moreover, the hot water after dissolution had many bubbles and became turbid. In addition, oil floating was observed over time.
When the cut surface of the produced powder was observed with an electron microscope, oil droplets of the lipophilic component were largely retained as shown in FIG. The holding diameter was 0.2 μm to 0.5 μm.

  The composition of the powder obtained in Examples 1-3 and Comparative Examples 1-4, the properties of the emulsion, the average particle diameter of the powder, the oil droplet retention diameter of the powder, the tableting test 1 and the results of the bath dissolution test are summarized. Table 1 shows.

  From the results of Table 1, the emulsion obtained in Example 1 can easily make the lipophilic component into fine oil droplets, and the emulsion obtained by pulverizing the emulsion by the spray drying method has excellent tableting resistance and is very transparent. It was found that the appearance of the bath was very good. Furthermore, the emulsions obtained in Examples 2 and 3 can easily make the lipophilic component into fine oil droplets, and those obtained by pulverizing the emulsion by the spray drying method are very excellent in tableting resistance. The appearance was very transparent and there was no bubble residue.

Example 4
56.3 g of ECTD-6NEX (manufactured by Nikko Chemicals Co., Ltd., polyoxyethylene (6) sodium tridecyl ether acetate) was added to 1500 g of ion-exchanged water. Then, it heated to 50 degreeC and prepared the water phase.
As lipophilic components, 562.5 g of ISIS (isostearyl isostearate manufactured by Higher Alcohol Industry Co., Ltd.), 225 g of Exepal IPP (isopropyl palmitate manufactured by Kao Corporation) and Emulgen 306P (polyoxyethylene stearyl ether manufactured by Kao Corporation), 112.5 g of HLB 9.7) and 225 g of Nikkor GO-440 (Nikko Chemicals tetraoleic acid polyoxyethylene sorbite HLB 12.5) were added. Thereafter, the temperature was raised to 50 ° C. and dispersed / dissolved to prepare an oil phase.
The oil phase was added to the aqueous phase, and a stirring operation was performed at 3000 r / min using a disper stirring blade for 10 minutes (50 ° C.). Further, 1068.8 g of H-PDX (reduced water candy manufactured by Matsutani Chemical Industry Co., Ltd.) was added and dispersed / dissolved to prepare an emulsion. The obtained emulsion was slightly pale and transparent.

  The emulsion obtained by the above-described emulsification operation is sprayed using a spray dryer (a spray dryer manufactured by Sakamoto Giken Co., Ltd.) under the conditions of an emulsion supply amount of 7000 g / hr, a blowing temperature of 150 ° C., and an exhaust air temperature of 90 ° C. It dried and obtained ester oil containing powder.

About the ester oil containing powder obtained by the said operation, the tableting test 2 and the bathtub dissolution test were done. As a result, the amount of exudation after pressurization was 12 mg. Moreover, the hot water after dissolution was very transparent although the lipophilic component was dispersed. Bubbles remained on the bath surface after dissolution.
When the fractured surface of the prepared powder was observed with an electron microscope, the oil droplets of the lipophilic component were held very finely as shown in FIG. The holding diameter was 0.05 μm to 0.2 μm.

Example 5
To 1687.5 g of ion-exchanged water, 51.6 g of ECTD-6NEX (polyoxyethylene (6) sodium tridecyl ether acetate manufactured by Nikko Chemicals Co., Ltd.) was added. Then, it heated to 50 degreeC and prepared the water phase.
As lipophilic components, 515.7 g of ISIS (isostearyl isostearate manufactured by Higher Alcohol Industry Co., Ltd.), 206.2 g of Exepal IPP (isopropyl palmitate manufactured by Kao Corporation) and Emulgen 306P (polyoxyethylene stearyl manufactured by Kao Corporation) 103.1 g of ether, HLB 9.7) and 206.2 g of Nikkor GO-440 (Nikko Chemicals tetraoleic acid polyoxyethylene sorbite HLB 12.5) were added. Further, 15.4 g of Lunac BA (behenic acid manufactured by Kao Co., Ltd.) was added. Thereafter, the temperature was raised to 65 ° C., dispersed / dissolved, and then cooled to 50 ° C. to prepare an oil phase.
The oil phase was added to the aqueous phase, and a stirring operation was performed at 3000 r / min using a disper stirring blade for 10 minutes (50 ° C.). Furthermore, 964.3 g of H-PDX (manufactured by Matsutani Chemical Industry Co., Ltd.) was added and dispersed / dissolved to prepare an emulsion. The obtained emulsion was slightly pale and transparent.

  The emulsion obtained by the above-described emulsification operation is sprayed using a spray dryer (a spray dryer manufactured by Sakamoto Giken Co., Ltd.) under the conditions of an emulsion supply amount of 7000 g / hr, a blowing temperature of 150 ° C., and an exhaust air temperature of 90 ° C. It dried and obtained ester oil containing powder.

About the ester oil containing powder obtained by the said operation, the tableting test 2 and the bathtub dissolution test were done. As a result, the exudation amount after pressurization was 58 mg. Moreover, the hot water after dissolution was very transparent although the lipophilic component was dispersed. No foam residue was seen on the bath surface after dissolution.
When the fractured surface of the prepared powder was observed with an electron microscope, the oil droplets of the lipophilic component were retained very finely as shown in FIG. The holding diameter was 0.05 μm to 0.2 μm.

Example 6
56.3 g of ECTD-6NEX (manufactured by Nikko Chemicals Co., Ltd., polyoxyethylene (6) sodium tridecyl ether acetate) was added to 1500 g of ion-exchanged water. Then, it heated to 50 degreeC and prepared the water phase.
As lipophilic components, 562.5 g of ISIS (isostearyl isostearate manufactured by Higher Alcohol Industry Co., Ltd.), 225 g of Exepal IPP (isopropyl palmitate manufactured by Kao Corporation) and Emulgen 306P (polyoxyethylene stearyl ether manufactured by Kao Corporation), 112.5 g of HLB 9.7) and 225 g of Nikkor GO-440 (Nikko Chemicals tetraoleic acid polyoxyethylene sorbite HLB 12.5) were added. Furthermore, 11.3 g of Lunac S-98 (Kao Co., Ltd. stearic acid) and 11.3 g of Lunac BA (Kao Co., Ltd. behenic acid) were added, heated to 65 ° C., and dispersed / dissolved. Then, it cooled to 50 degreeC and prepared the oil phase.
The oil phase was added to the aqueous phase, and a stirring operation was performed at 3000 r / min using a disper stirring blade for 10 minutes (50 ° C.). Furthermore, 1046.3 g of H-PDX (manufactured by Matsutani Chemical Co., Ltd.) was added and dispersed / dissolved to prepare an emulsion. The obtained emulsion was slightly pale and transparent.

  The emulsion obtained by the above-described emulsification operation is sprayed using a spray dryer (a spray dryer manufactured by Sakamoto Giken Co., Ltd.) under the conditions of an emulsion supply amount of 7000 g / hr, a blowing temperature of 150 ° C., and an exhaust air temperature of 90 ° C. It dried and obtained ester oil containing powder.

About the ester oil containing powder obtained by the said operation, the tableting test 2 and the bathtub dissolution test were done. As a result, the amount of exudation after pressurization was 64 mg. Moreover, the hot water after dissolution was very transparent although the lipophilic component was dispersed. No foam residue was seen on the bath surface after dissolution.
When the fractured surface of the produced powder was observed with an electron microscope, the oil droplets of the lipophilic component were retained very finely as shown in FIG. The holding diameter was 0.05 μm to 0.2 μm.

Example 7
56.3 g of ECTD-6NEX (manufactured by Nikko Chemicals Co., Ltd., polyoxyethylene (6) sodium tridecyl ether acetate) was added to 1500 g of ion-exchanged water. Then, it heated to 50 degreeC and prepared the water phase.
As lipophilic components, 562.5 g of ISIS (isostearyl isostearate manufactured by Higher Alcohol Industry Co., Ltd.), 225 g of Exepal IPP (isopropyl palmitate manufactured by Kao Corporation) and Rheodor TWS106V (polyoxyethylene monostearate manufactured by Kao Corporation) Sorbitan, HLB 9.6) 112.5g and Nikkor GO-440 (Nikko Chemicals Co., Ltd. Tetraoleic acid polyoxyethylene sorbit HLB12.5) 225g were added, heated to 50 ° C, dispersed / dissolved. An oil phase was prepared.
The oil phase was added to the aqueous phase, and a stirring operation was performed at 3000 r / min using a disper stirring blade for 10 minutes (50 ° C.). Further, 1068.8 g of H-PDX (reduced water candy manufactured by Matsutani Chemical Industry Co., Ltd.) was added and dispersed / dissolved to prepare an emulsion. The obtained emulsion was slightly pale and transparent.

  The emulsion obtained by the above-described emulsification operation is sprayed using a spray dryer (a spray dryer manufactured by Sakamoto Giken Co., Ltd.) under the conditions of an emulsion supply amount of 7000 g / hr, a blowing temperature of 150 ° C., and an exhaust air temperature of 90 ° C. It dried and obtained ester oil containing powder.

About the ester oil containing powder obtained by the said operation, the tableting test 2 and the bathtub dissolution test were done. As a result, the amount of seepage after pressurization was 5 mg. Moreover, the hot water after dissolution was very transparent although the lipophilic component was dispersed. Bubbles remained on the bath surface after dissolution.
When the cut surface of the produced powder was observed with an electron microscope, the oil droplets of the lipophilic component were held very finely as shown in FIG. The holding diameter was 0.05 μm to 0.2 μm.

Example 8
56.3 g of ECTD-6NEX (manufactured by Nikko Chemicals Co., Ltd., polyoxyethylene (6) sodium tridecyl ether acetate) was added to 1500 g of ion-exchanged water. Then, it heated to 50 degreeC and prepared the water phase.
As lipophilic components, 562.5 g of ISIS (isostearyl isostearate manufactured by Higher Alcohol Industry Co., Ltd.), 225 g of Exepearl IPP (isopropyl palmitate manufactured by Kao Corporation), and Leodol SP-S10V (Sorbitan monostearate manufactured by Kao Corporation) , HLB4.7) 112.5g and Nikkor GO-440 (Nikko Chemicals Co., Ltd. Tetraoleic acid polyoxyethylene sorbite HLB12.5) 225g was charged, heated to 50 ° C, dispersed / dissolved and oiled A phase was prepared.
The oil phase was added to the aqueous phase, and a stirring operation was performed at 3000 r / min using a disper stirring blade for 10 minutes (50 ° C.). Further, 1068.8 g of H-PDX (reduced water candy manufactured by Matsutani Chemical Industry Co., Ltd.) was added and dispersed / dissolved to prepare an emulsion. The obtained emulsion was slightly pale and transparent.

  The emulsion obtained by the above-described emulsification operation is sprayed using a spray dryer (a spray dryer manufactured by Sakamoto Giken Co., Ltd.) under the conditions of an emulsion supply amount of 7000 g / hr, a blowing temperature of 150 ° C., and an exhaust air temperature of 90 ° C. It dried and obtained ester oil containing powder.

About the ester oil containing powder obtained by the said operation, the tableting test 2 and the bathtub dissolution test were done. As a result, the amount of seepage after pressurization was 3 mg. Moreover, the hot water after dissolution was very transparent although the lipophilic component was dispersed. There was no foam residue on the bath surface after dissolution.
When the fractured surface of the produced powder was observed with an electron microscope, the oil droplets of the lipophilic component were held very finely as shown in FIG. The holding diameter was 0.05 μm to 0.2 μm.

Example 9
56.3 g of ECTD-6NEX (manufactured by Nikko Chemicals Co., Ltd., polyoxyethylene (6) sodium tridecyl ether acetate) was added to 1500 g of ion-exchanged water. Then, it heated to 50 degreeC and prepared the water phase.
As lipophilic components, 562.5 g of ISIS (isostearyl isostearate manufactured by Higher Alcohol Industry Co., Ltd.), 225 g of Exepal IPP (isopropyl palmitate manufactured by Kao Corporation), and Leodol SP-P10 (Sorbitan monopalmitate manufactured by Kao Corporation) , HLB 6.7) 112.5 g and Nikkor GO-440 (Nikko Chemicals Co., Ltd. Tetraoleic acid polyoxyethylene sorbite HLB 12.5) 225 g, heated to 50 ° C., dispersed / dissolved to oil phase Was prepared.
The oil phase was added to the aqueous phase, and a stirring operation was performed at 3000 r / min using a disper stirring blade for 10 minutes (50 ° C.). Further, 1068.8 g of H-PDX (reduced water candy manufactured by Matsutani Chemical Industry Co., Ltd.) was added and dispersed / dissolved to prepare an emulsion. The obtained emulsion was slightly pale and transparent.

  The emulsion obtained by the above-described emulsification operation is sprayed using a spray dryer (a spray dryer manufactured by Sakamoto Giken Co., Ltd.) under the conditions of an emulsion supply amount of 7000 g / hr, a blowing temperature of 150 ° C., and an exhaust air temperature of 90 ° C. It dried and obtained ester oil containing powder.

About the ester oil containing powder obtained by the said operation, the tableting test 2 and the bathtub dissolution test were done. As a result, the amount of exudation after pressurization was 12 mg. Moreover, the hot water after dissolution was very transparent although the lipophilic component was dispersed. There was no foam residue on the bath surface after dissolution.
When the fractured surface of the prepared powder was observed with an electron microscope, the oil droplets of the lipophilic component were kept very fine as shown in FIG. The holding diameter was 0.05 μm to 0.2 μm.

Comparative Example 5
As oleophilic components, 660 g of ISIS (isostearyl isostearate, manufactured by Higher Alcohol Industry Co., Ltd.) and 264 g of Exepal IPP (isopropyl palmitate, Kao Co., Ltd.) and Emulgen 306P (polyoxyethylene stearyl ether, HLB 9.7 Kao Co., Ltd.) )) 132 g, Nikkor GO-440 (polyoxyethylene sorbitol tetraoleate HLB12.5, manufactured by Nikko Chemical Co., Ltd.) 264 g and Lunac S-98 (stearic acid: manufactured by Kao Corporation) 66.0 g were dispersed. / Dissolved to prepare an oil phase and kept at 40 ° C. 9.8 g of sodium hydroxide (purity 96% manufactured by Kishida Chemical Co., Ltd.) was added to 1760 g of ion-exchanged water, and the temperature was raised to 40 ° C. After adding the aqueous phase to the oil phase under stirring, 1243.4 g of H-PDX (hydrogenated dextrin manufactured by Matsutani Chemical Industry Co., Ltd.) was added. The obtained emulsion was milky white.

  The emulsion obtained by the above-mentioned emulsification operation is sprayed using a spray dryer (spray dryer manufactured by Sakamoto Giken Co., Ltd.) under the conditions of an emulsion supply rate of 7100 g / hr, an air blowing temperature of 170 ° C., and an exhaust air temperature of 90 ° C. Dried. However, it was not powdered and was a paste. When this tablet was subjected to a tableting test 2 similar to the powder, the amount of seepage was 120 mg or more. The powder average particle diameter and the oil droplet retention diameter could not be measured because they were pasty.

  Table 2 summarizes the compositions of the powders obtained in Examples 4 to 9 and the paste obtained in Comparative Example 5, the average particle diameter and oil droplet retention diameter of the powder, the tableting test 2 and the bath dissolution test. .

  From the results of Table 2, the emulsions obtained in Examples 4 to 9 can easily make lipophilic components into fine oil droplets, and those obtained by pulverizing the emulsion by spray drying are excellent in tableting resistance and are very It was clear that the appearance of the hot water bath was very good. Furthermore, the powder obtained in Examples 5, 6, 8, and 9 had no foam residue on the bath surface after the bath dissolution test.

  As shown in Examples 1 to 9, when the (B) component and (C) component of the present invention are contained, the lipophilic component can be finely dispersed by self-emulsification when the preparation is dissolved. It is possible to have a transparent appearance, and it is possible to enhance the efficacy of oily medicinal ingredients and agrochemical active ingredients. In addition, powders pulverized by spray-drying method are powders with less exudation of lipophilic components to compaction and excellent workability.

2 is an electron micrograph of a broken section of a lipophilic component-containing powder obtained in Example 1. FIG. 2 is an electron micrograph of a fractured section of a lipophilic component-containing powder obtained in Example 2. FIG. 3 is an electron micrograph of a fractured section of a lipophilic component-containing powder obtained in Example 3. FIG. 2 is an electron micrograph of a fractured section of a lipophilic component-containing powder obtained in Comparative Example 1. 2 is an electron micrograph of a fractured section of a lipophilic component-containing powder obtained in Comparative Example 2. 4 is an electron micrograph of a fractured section of a lipophilic component-containing powder obtained in Comparative Example 3. 4 is an electron micrograph of a fractured section of a lipophilic component-containing powder obtained in Comparative Example 4. 4 is an electron micrograph of a fractured section of a lipophilic component-containing powder obtained in Example 4. FIG. 4 is an electron micrograph of a fractured section of a lipophilic component-containing powder obtained in Example 5. FIG. 4 is an electron micrograph of a fractured section of a lipophilic component-containing powder obtained in Example 6. FIG. 3 is an electron micrograph of a fractured section of a lipophilic component-containing powder obtained in Example 7. FIG. 2 is an electron micrograph of a fractured section of a lipophilic component-containing powder obtained in Example 8. FIG. 2 is an electron micrograph of a fractured section of a lipophilic component-containing powder obtained in Example 9. FIG.

Claims (9)

(A) a lipophilic component having a solubility in water at 25 ° C. of less than 10% by weight , (B) a polyoxyalkylene (carbon number 2-3 alkylene group) nonionic surfactant, (C) general formula ( alkyl polyoxyethylene acetate represented by I), a lipophilic component-containing powder obtained by spray-drying the O / W type emulsion containing (D) excipients and water, in the powder ( The total content of the component (A) and the component (B) is 35 to 55% by weight, and the weight ratio of the component (A) and the component (B) is (A) / (B) = 1 to 10 in the powder. The lipophilic component-containing powder, wherein the content of the component (C) is 0.05 to 10% by weight .
R ¹ —O— (CH ₂ CH ₂ O) _n —CH ₂ COOM (I)
[Wherein, R ¹ is a hydrocarbon group having 10 to 25 carbon atoms, M is H or a cation, and n is a number of 1 to 40 indicating the average number of added moles of an oxyethylene group. ]   The lipophilic component-containing powder according to claim 1, comprising at least one selected from (E) fatty acids and (F) fatty acid soaps. The lipophilic component-containing powder according to claim 1 or 2 , wherein the component (D) is at least one selected from dextrin, monosaccharide, disaccharide and sugar alcohol. The (A) component is at least one selected from ceramide, liquid paraffin, ester oil, higher alcohol, higher fatty acid, and silicone oil, The lipophilic component-containing powder according to any one of claims 1 to 3 . The lipophilic component-containing powder according to claim 2 or claim 3 or 4 subordinate to claim 2, wherein the component (E) is a fatty acid having a hydrocarbon group having 8 to 24 carbon atoms. (F) Lipophilic component containing powder in any one of Claims 3-5 dependent on Claim 2 or Claim 2 which is a fatty-acid soap which has a C8-C24 hydrocarbon group. Following steps 1, step 2, viewed including the step 3 and step 4, (C) component is added to the oil phase or aqueous phase of step 2 step 1, the lipophilic component according to any of claims 1 to 6 A method for producing the contained powder.
Step 1: Preparation of an oil phase containing component (A) and component (B) Step 2: Preparation of an aqueous phase containing component (D) and water Step 3: Prepared in steps 1 and 2 Step 2 of mixing two liquids to prepare an O / W type emulsion Step 4: Step of spray drying the emulsion obtained in Step 3 to obtain a lipophilic component-containing powder A tableting product obtained by tableting a powder comprising the lipophilic component-containing powder according to any one of claims 1 to 6 . A solid molding bath comprising the tableting product according to claim 8.