JP2018108958A - Seamless capsule - Google Patents

Abstract

PROBLEM TO BE SOLVED: To provide a relatively large grain diameter seamless capsule.SOLUTION: The diameter of the seamless capsule is set to 5 mm or more, and the ratio T2/T1 of the maximum thickness T2 to the minimum thickness T1 of the film is set to 3.5 or less.SELECTED DRAWING: None

Description

  The present invention relates to a seamless capsule.

  A seamless capsule is a capsule in which an inclusion is seamlessly wrapped with a film (capsule film).

  For example, Patent Document 1 discloses that in the preparation of a seamless soft capsule film, carrageenan, which is a capsule film composition, is decomposed with an acidic pH adjuster, and the decomposition is stopped with a neutralizing agent. A seamless soft capsule manufactured by subjecting alginates to gelation in an aqueous gelling aid solution containing calcium ions as a product, and having at least carrageenan and alginates in the composition of the capsule film A soft capsule is disclosed. This document describes that the capsule has a diameter of 0.5 to 15 mm, preferably 1 to 8 mm, and in the examples, a capsule having a diameter of 4 mm is manufactured.

  Patent Document 2 discloses a method for producing a seamless capsule characterized by including a coating step of coating a seamless capsule separated from a hardening liquid with an adsorbent powder during or after drying. It is described that the capsule has a diameter of 1 mm to 7 mm, and in the examples, a capsule having a diameter of 3.5 mm was obtained.

Japanese Patent No. 4822299 (Claims, Examples, Paragraph 0068) Japanese Patent Laying-Open No. 2015-81249 (Claims, Examples, Paragraph 0051)

  An object of the present invention is to provide a seamless capsule having a relatively large particle size (diameter).

  Although the diameter of the seamless capsule is widely described as in Patent Documents 1 and 2, in practice, the diameter of the seamless capsule is at most 3.5 mm or 4 mm, and has a large particle size (for example, 9 mm or more, 10 mm or more, for example). ) No seamless capsule has been produced.

  On the other hand, according to the study by the present inventors, when a seamless capsule having a large diameter is to be produced by a general method, the capsule itself is actually broken, and the capsule itself is not formed. However, it is difficult to form capsules due to the effect of surface tension when the coating rate and film thickness are large, as well as when the coating rate and film thickness are small. It has been found that there are cases where it is not possible to form seamless capsules that can guarantee practicality. At best, capsules with a diameter of about 3.5 mm or 4 mm and capsules with a large particle size may differ greatly in the aspect of the capsule itself. It was not, and it was thought to be one of the factors that were not actually manufactured.

Under such circumstances, as a result of intensive investigations, the present inventors have controlled the production conditions of seamless capsules (further, by selecting a film and inclusions), etc. Seamless capsules can be obtained, and seamless capsules having properties such as small variations in thickness of the film (uneven thickness) are capsules that can withstand practical use despite having a large particle size, Capsule of desired film can be obtained regardless of coating rate and film thickness, and seamless capsules having gel-like inclusions that are not known at all (especially seamless capsules having a large particle size) can be obtained. I found out.
In addition to the above, the present inventors have obtained various new findings as will be described below, and have made further studies and completed the present invention.

That is, the present invention relates to the following inventions and the like.
[1] A seamless capsule having a diameter of 5 mm or more and a ratio T2 / T1 of the maximum thickness T2 to the minimum thickness T1 of the film being 3.5 or less.
[2] The seamless capsule according to [1], having a diameter of 7 mm or more.
[3] The seamless capsule according to [1] or [2], wherein the diameter is 10 mm or more and the ratio T2 / T1 of the maximum thickness T2 to the minimum thickness T1 of the film is 3 or less.
[4] The seamless capsule according to any one of [1] to [3], wherein a ratio T2 / T1 of the maximum thickness T2 to the minimum thickness T1 of the film is 2.3 or less.
[5] The seamless capsule according to any one of [1] to [4], wherein the sphericity is 80% or more.
[6] Any of [1] to [5], wherein the diameter is 10 mm or more, the ratio T2 / T1 of the maximum thickness T2 to the minimum thickness T1 of the film is 2.1 or less, and the sphericity is 85% or more. Seamless capsule according to crab.
[7] The seamless capsule according to any one of [1] to [6], wherein the coating rate is 3 to 60% by mass.
[8] The seamless capsule according to any one of [1] to [7], wherein the coating rate is 10% by mass or less.
[9] The seamless capsule according to any one of [1] to [8], wherein the coating rate is 15% by mass or more.
[10] The seamless capsule according to any one of [1] to [9], which has a diameter of 13 mm or more.
[11] The seamless capsule according to any one of [1] to [10], which has a diameter of 15 mm or more.
[12] The seamless capsule according to any one of [1] to [11], wherein the inclusion is a gel.
[13] The seamless capsule according to any one of [1] to [12], wherein the value SD / T is 0.2 or less, where SD is the standard deviation of the film thickness and T is the film thickness.
[14] An apparatus comprising a concentric multiple nozzle concentrically provided with an outer nozzle that allows passage of a coating liquid containing constituents of the film and an inner nozzle that supplies a content liquid containing constituents of inclusions, and a forming tube And a seamless capsule manufacturing method including a capsule forming step of forming a capsule in the forming tube by discharging the content liquid from the discharge port of the inner nozzle and the coating liquid from the discharge port of the outer nozzle into the forming tube. And
When the distance between the axis of the concentric multiple nozzle and the axis of the forming tube is X and the diameter of the capsule is D, the value X / D is adjusted to be 3 or less, and
A method for producing a seamless capsule, wherein the value Y / D is adjusted to 0.4 or less, where Y is the width of the discharge port of the inner nozzle and D is the diameter of the capsule.
[15] The production method according to [14], wherein the value X / D is adjusted to 2 or less and the value Y / D is adjusted to 0.28 or less to obtain seamless capsules with a yield rate of 80% or more.
[16] The production method according to [14] or [15], wherein the seamless capsule is the seamless capsule according to any one of [1] to [13].

  In the present invention, a seamless capsule having a relatively large particle diameter (diameter) can be provided.

  The seamless capsule of the present invention usually does not break during drying or with a small impact. Therefore, according to the present invention, a practical seamless capsule can be provided as well as a large particle size.

  In another aspect of the present invention, a seamless capsule having a clean shape can be obtained even with a large particle size, with few capsule dents and the like.

  According to another aspect of the present invention, even when stored for a long period of time, there is no deformation or breakage of the capsule, leakage of the inclusion, and the like, and a seamless capsule excellent in stability can be obtained.

  In another aspect of the present invention, it is possible to obtain a seamless capsule having desired desired characteristics (for example, touch, disintegration, etc.) despite a relatively large particle size.

  In another aspect of the present invention, a seamless capsule having a large particle diameter can be obtained regardless of the coating rate and the thickness of the coating.

  In another aspect of the present invention, a seamless capsule having a solid (particularly gel) inclusion can be obtained.

FIG. 1 is a schematic diagram showing a manufacturing process (manufacturing apparatus) of a seamless capsule by a dropping method.

[capsule]
The capsule usually has a film (a film, a capsule film) and an inclusion (an inclusion included in the film). In other words, the capsule has an inclusion and a film covering the inclusion.

(Film)
The film may usually contain a film-forming component (film-forming base, film-forming agent). The film-forming component is not particularly limited and can be appropriately selected depending on the use of the capsule. For example, a polysaccharide (or a derivative thereof) {for example, a seaweed-derived polysaccharide [for example, agar, carrageenan, alginic acid or a salt thereof ( For example, alkali metal salts (sodium salt, potassium salt, etc.), alkaline earth metal salts (calcium salt, magnesium salt, etc.), iron salts, tin salts, etc.), ferceleran, curdlan, etc.], resin-derived polysaccharides (Eg, gati gum, gum arabic, etc.), microorganism-derived polysaccharides (eg, pullulan, welan gum, xanthan gum, gellan gum), plant-derived polysaccharides (eg, tragacanth gum, pectin, glucomannan, starch, polydextrose, dextrin, maltodextrin) , Cyclodextrin, indigestible dextst Etc.), seed-derived polysaccharides (eg, guar gum or derivatives thereof (eg, hydroxypropyl guar gum, cationized guar gum, guar gum degradation products (eg guar gum enzyme degradation product), etc.), tara gum, tamarind seed gum, locust bean gum, psyllium Seed gum, ama seed gum, etc.], fermentation polysaccharides (eg, ditan gum), cellulose derivatives (eg, hydroxypropylcellulose, hydroxypropylmethylcellulose, methylcellulose, carboxymethylcellulose, etc.), chitosan}, synthetic resins (eg, polyvinyl alcohol) , Proteins (eg, gelatin, casein, zein), sugar alcohols (eg, sorbitol, maltitol, lactitol, palatinit, xylitol, mannini) Lumpur, galactitol, erythritol) and the like. The film-forming component may function as a plasticizer, sweetener, dietary fiber, bulking agent, or the like depending on the type.

  You may use a film formation component individually or in combination of 2 or more types.

  Among these, agar, carrageenan, gelatin and the like are typical. Therefore, the film forming component may be composed of at least one film forming component (A) selected from agar, carrageenan and gelatin. In particular, the film-forming component may comprise a non-gelatin component such as agar and / or carrageenan.

  The agar is not particularly limited, and examples thereof include powder agar, solid agar, and flake agar. Examples of the raw material for agar include red algae (for example, Amakusa, ogonori) and the like.

The intensity of the agar can be appropriately selected according to the use of the capsule and the texture. For example, in the viewpoint of cracking feeling and touch, jelly strength of agar, 500 g / cm ² or more (e.g., 550~3000g / ^cm 2), preferably 600 g / cm ² or more (e.g., 650~2000g / ^cm 2) , more preferably 700 g / cm ² or more (e.g., 750~1500g / cm ²⁾ may be, it may be 800 g / cm ² or more.
Further, in a case such as that desired soft capsule shell, jelly strength of agar, 500 g / cm ² or less (e.g., 100 to 500 g / ^cm 2), preferably 300 g / cm ² or less (e.g., 100 to 300 g / cm ² ), More preferably 250 g / cm ² or less (for example, 150 to 250 g / cm ² ).
The jelly strength can be measured by the Nissho water method.

Examples of carrageenan include κ (kappa) carrageenan, ι (iota) carrageenan, λ (lambda) carrageenan, μ (mu) carrageenan, ν (new) carrageenan, θ carrageenan, ζ (zeta) carrageenan, and π carrageenan. It is done.
Carrageenan may be derived from, for example, all algae such as red seaweeds such as Sugiori, Myrinaceae, and Ibaranoaceae.
The viscosity of the carrageenan can be appropriately selected according to the use of the capsule and the texture. For example, it may be 5 mPa · s or more in agar such as crack feeling or touch. The upper limit of the viscosity is not particularly limited, but is preferably 500 mPa · s or less. The viscosity can be measured using, for example, a B-type viscometer.

The gelatin is not particularly limited, and examples thereof include pork gelatin, beef gelatin, chicken gelatin, fish gelatin and the like.
As gelatin, gelatin derivatives such as succinylated gelatin, gelatin hydrolyzate, hydrolyzed gelatin, and cross-linked gelatin may be used.
If the purpose is to avoid the use of mammals (eg, cows, pigs, etc.) due to religious restrictions, allergies, etc., non-mammal capsules are made by not using mammal-derived gelatin. be able to.
The strength of the gelatin can be appropriately selected according to the use of the capsule and the texture. For example, from the viewpoint of feeling of cracking and touch, the bloom strength of gelatin is 150 or more (for example, 160 to 500), preferably 170 or more (for example, 175 to 450), more preferably 200 or more (for example, 200 to 400). ).
When a soft capsule film is desired, the bloom strength of gelatin may be 150 or less, preferably 130 or less, and more preferably 100 or less.
The Bloom strength is defined by the mass necessary for a cylindrical piston having a diameter of 12.7 mm to be pushed into a 4 mm gel, for example.

  When the film contains a film forming component (A), the ratio (solid content ratio) of the film forming component (A) in the film (or film forming component) is, for example, 10% by mass or more (for example, 10 to 100% by mass). , Preferably 15% by mass or more (for example, 15 to 95% by mass), more preferably 20% by mass or more (for example, 20 to 90% by mass), or 30% by mass or more (for example, 40% by mass or more). , Preferably 50% by mass or more).

  The film may contain a combination of the film forming component (A) and other film forming components. The other film-forming component (film-forming component (B)) may be any component other than the film-forming component (A), and can be selected according to the function required for the capsule. For example, alginic acid or a salt thereof, microorganism Derived polysaccharides (eg gellan gum, etc.), plant derived polysaccharides (eg pectin, starch, dextrin, maltodextrin, cyclodextrin, indigestible dextrin etc.), seed derived polysaccharides (eg guar gum or derivatives thereof (eg Guar gum degradation products etc.)], sugar alcohols (eg sorbitol, xylitol etc.) and the like. The film-forming component (B) may be composed of at least one of these components.

  The film forming component (B) may be used alone or in combination of two or more.

  When a film | membrane contains a film formation component (B), the ratio (solid content ratio) of the film formation component (B) in a film | membrane (or film formation component) is 70 mass% or less (for example, 0.1-65 mass), for example. %), Preferably 60% by mass or less (for example, 0.5 to 55% by mass), more preferably 50% by mass or less (for example, 1 to 45% by mass), or 2% by mass or more (for example, 2 to 40% by mass, preferably 3 to 35% by mass, and more preferably 5 to 30% by mass).

  When the film contains the film forming component (A) and the film forming component (B), these ratios are, for example, the former / the latter (mass ratio) = 99.5 / 0.5 to 10/90 (for example, 99/1 to 15/85), more preferably 98/2 to 20/80 (for example, 95/5 to 25/75), and 99/1 to 30/70 (for example, 95/5 to 95/5). 40/60, preferably 90/10 to 50/50).

  The film-forming component may be either water-soluble or water-insoluble depending on the application, and a combination of a water-soluble component and a water-insoluble (hydrophobic) component may be used.

The film may contain a plasticizer for adjusting the film strength. Examples of the plasticizer include polyhydric alcohols (for example, (poly) alkylene glycols such as ethylene glycol, propylene glycol, polyethylene glycol, and polypropylene glycol; polyols having three or more hydroxyl groups such as glycerin), saccharides [for example, simple substances. Sugar (eg, glucose, fructose, glucose, galactose, etc.), disaccharide (eg, sucrose, maltose, trehalose, coupling sugar, etc.), oligosaccharide (eg, malto-oligosaccharide, etc.)], sugar alcohol (eg, sorbitol, etc.) , Maltitol, lactitol, palatinit, xylitol, mannitol, galactitol, erythritol, and the like sugar alcohols), polysaccharides or derivatives thereof [eg, starch, starch derivatives (eg, Dextrose, dextrin, maltodextrin, indigestible dextrin, cyclodextrin (α, β, or γ, etc.), cellulose derivatives (eg, hydroxypropylcellulose, hydroxypropylmethylcellulose, methylcellulose, carboxymethylcellulose, etc.)], polyvinyl alcohol, And triacetin.
In addition, about 10-90 may be sufficient as DE (starch degradation degree) of a starch derivative, for example.

  You may use a plasticizer individually or in combination of 2 or more types.

  In addition, sugar alcohol, starch, starch derivatives, etc. can also be used as a film forming component as described above.

  Of these, polyhydric alcohols, saccharides, starch, starch derivatives and the like may be suitably used as plasticizers. Therefore, the plasticizer may be composed of at least one of these. On the other hand, in the present invention, capsules can be obtained without using saccharides (for example, sucrose, trehalose, etc.).

  When the film contains a plasticizer, the plasticizer ratio (solid content ratio) in the film is, for example, 70% by mass or less (for example, 0.1 to 65% by mass), and preferably 60% by mass or less (for example, 0.8%). 5 to 55% by mass), more preferably 50% by mass or less (for example, 1 to 45% by mass), or 2% by mass or more (for example, 2 to 60% by mass, preferably 3 to 50% by mass, More preferably, it may be 5 to 40% by mass).

  In particular, the film may contain at least glycerin. When the film contains glycerin, the ratio of glycerin in the film is, for example, 70% by mass or less (for example, 0.1 to 65% by mass), preferably 60% by mass or less (for example, 2 to 55% by mass), and more preferably. 50 mass% or less (for example, 3-45 mass%) may be sufficient, and 5 mass% or more (for example, 7-50 mass%) may be sufficient.

  The film may contain other components depending on the application. Examples of other components include colorants (pigments, pigments), flavoring agents, sweeteners, antioxidants, preservatives, seasonings, spices, acidulants (for example, citric acid or salts thereof), bitterness agents, and the like. , Salts, umami components, and other components described in the section of inclusions (for example, physiologically active substances, biologically active substances, etc.) and the like. Depending on the type of sweetener, it can be used as a film-forming component or a plasticizer as described above.

  You may use another component individually or in combination of 2 or more types.

  When a film | membrane contains another component, the ratio of the other component in a film | membrane is 30 mass% or less (for example, 0.01-25 mass%), for example, Preferably it is 20 mass% or less (for example, 0.05-15). % By mass), more preferably 10% by mass or less (for example, 0.1 to 8% by mass).

  The film may contain a solvent component (for example, water). The ratio of the solvent component in the film is, for example, 30% by mass or less (for example, 0.1 to 25% by mass), preferably 20% by mass or less (for example, 1 to 18% by mass), and more preferably 15% by mass or less ( For example, about 3-12 mass%) may be sufficient.

(Included)
The inclusion of the capsule can be appropriately selected according to the use and the like, and is not particularly limited.
The inclusion may be an oily component (oil-soluble component, lipophilic component) or a water-soluble component (hydrophilic component), depending on the type and use of the film. Also good. Moreover, the inclusions may be either liquid or solid, and may contain a combination of these. Usually, the inclusions often contain at least a liquid.

  The inclusions may typically be liquid. Such a liquid inclusion may be liquid as a whole, and may be composed of only a liquid component (one or two or more liquid components), or a liquid component (or a liquid component as a solvent or a dispersion medium). ), Other components (another liquid component, gas component, and / or solid component) may be dissolved or dispersed (to form a liquid inclusion as a whole).

  Liquid forms include colloidal forms, emulsion forms, jelly forms, and the like.

  In another embodiment of the present invention, the capsule inclusion may be solid. The solid state includes a state having substantially no fluidity, for example, a gel [gel shape (gummy shape)]. The solid inclusion may be solid as a whole, and may be composed of only a solid component (one or two or more solid components), or a solid component (or a solid component). As the dispersion medium, other components (liquid component, gas component, and / or another solid component) may be mixed or dispersed (to form a solid inclusion as a whole).

  The inclusions are not particularly limited, and include, for example, fragrances, cosmetics, surfactants, detergents, bathing agents, surfactants, cooling agents, physiologically active substances (for example, vitamins, amino acids, collagen, collagen peptides, lipids) , Isoflavones, minerals, enzymes, hormones, etc.), biologically active substances (medicine, etc.), microorganisms (eg, bacteria such as lactic acid bacteria, bifidobacteria, natto bacteria, yeasts; fungi such as yeast), food and drink (Or an extract thereof), a plant (or an extract thereof), a sweetener, a sour agent, a seasoning, a tonic, and the like. These components may be either solid or liquid, and may be used alone or in combination of two or more.

  As described above, in one embodiment of the present invention, the inclusion is in a liquid state. The liquid component (or liquid inclusion) constituting the liquid inclusion may be either hydrophilic or oleophilic, but, as will be described later, usually for the film (or the part in contact with the film) And may be non-soluble (non-erodible).

  Specific liquid components (lipophilic liquid components) include, for example, fatty acids (for example, caprylic acid, capric acid, eicosapentaenoic acid, docosahexaenoic acid, oleic acid, linoleic acid, etc.), fatty acid esters [for example, triglycerides (medium Glycerin esters (fats) such as chain fatty acid triglycerides (MCT, etc .; non-glycerin fatty acid esters such as isopropyl myristate), etc.], vegetable oils (eg olive oil, sunflower oil, corn oil, peanut oil, grape seed oil, wheat (Germ oil, rapeseed oil, jojoba oil, safflower oil), hydrogenated oil, mineral oil, silicone oil, sucrose fatty acid ester, liquid paraffin, squalane, fragrance (for example, esters, alcohols, aldehydes, ketones, phenols) , Ethers, lactones, hydrocarbons, Nitrogen compounds, sulfur-containing compounds, such as acids), and the like.

  The liquid inclusion may be composed only of the liquid component as described above, and other components (for example, another liquid component and / or solid component) are dissolved in the liquid component (liquid component as a dispersion medium). Or it may be dispersed.

  In another aspect of the present invention, the inclusion may be in a solid form (such as a gel). The solid component constituting the solid inclusion may be either hydrophilic or lipophilic. In addition, the solid component may be soluble (erodible) or insoluble (non-erodible) with respect to the film (or a portion that comes into contact with the film), and particularly may be insoluble.

  Heretofore, seamless capsules whose inclusions are solid (such as gummy) (and have a large particle size) have not been known. Since seamless capsules can usually be produced only in a liquid state, this is considered to be one of the factors for which seamless capsules having a solid inclusion are not known.

  The solid component (or the solid component constituting the solid inclusion) is not particularly limited, for example, the components exemplified in the section of the film [for example, film-forming components (gelatin, agar, carrageenan, etc.), Plasticizers, etc.].

  The solid inclusion may be composed of only such a solid component, and other components (for example, another solid component and / or a solid component as a dispersion medium or a matrix). Liquid component) may be mixed or dispersed.

  These components may be used alone or in combination of two or more.

  When the inclusion includes a liquid component and a solid component, these ratios are not particularly limited, and can be appropriately selected depending on whether the form of the inclusion is liquid or solid. For example, the former / The latter (mass ratio) = 99.99 / 0.01 to 0.01 / 99.99, preferably 99.9 / 0.1 to 0.1 / 99.9, more preferably 99.5 / 0. It may be about 5 to 0.5 / 95.5, and 99.99 / 0.01 to 10/90 (for example, 99.9 / 0.1 to 20/80, preferably 99.5 / 0. 5-30 / 70, more preferably 99 / 1-50 / 50), 0.01 / 99.99-90 / 10 (e.g., 0.01 / 99.9-80 / 20, preferably 0.5 / 99.5 to 70/30, more preferably 1/99 to 50/50).

(Capsule form)
The capsule has a film (shell) as an outermost layer, and includes inclusions in the film (inside). Such capsules may usually be seamless capsules (seamless capsules).

  The film may be a single layer or a plurality of layers. In addition, when formed with a plurality of layers, the thickness ratio between one layer and the other layer is not particularly limited, and is, for example, 100/1 to 0.01 / 1 (for example, 50/1 to 0.00). 02/1), preferably 20/1 to 0.05 / 1 (for example, 10/1 to 0.1 / 1), more preferably about 5/1 to 0.2 / 1.

  The diameter (diameter, average diameter) of the capsule (or film) is relatively large, for example, 5 mm or more (for example, 6 to 50 mm), preferably 7 mm or more (for example, 7.5 to 40 mm), more preferably 8 mm or more. (E.g., 9 to 35 mm), particularly 10 mm or more (e.g., 10 to 30 mm), more than 10 mm (e.g., 10.5 mm or more), 11 mm or more (e.g., 11.5 mm or more, 12 mm or more, 13 mm or more) 15 mm or more, 16 mm or more, 17 mm or more, 18 mm or more, 19 mm or more).

  The capsule of the present invention usually has a small thickness unevenness. For example, the ratio T2 / T1 of the maximum thickness T2 to the minimum thickness T1 of the capsule (or film) can be selected from a range of 3.5 or less (for example, 3.2 or less), preferably 3 or less (for example, 2.8). Or less), more preferably 2.5 or less (for example, 2.3 or less), particularly preferably 2.1 or less (for example, 2.0 or less), most preferably 1.8 or less (for example, 1.6 or less). It may be 1.2 or less.

  The thickness of the film (average thickness, the total thickness in the case where it is formed of a plurality of layers, the same applies hereinafter) is not particularly limited and can be appropriately selected according to the use etc., for example, 20 μm to 5 mm, preferably 30 μm. May be about 3 mm, more preferably about 40 μm to 1 mm, and may be relatively small [eg, 1 mm or less (eg, 800 μm or less, 500 μm or less, 300 μm or less, etc.)] or relatively large. [For example, 1 mm or more (for example, 1.5 mm or more, 2 mm or more, 3 mm or more, 4 mm or more, 5 mm or more, 7 mm or more, etc.)].

  When the diameter (average diameter) of the film is D and the thickness (average thickness) of the film is T, the value [T / D] × 100 (%) is, for example, 0.1 to 95%, preferably 0.2. -90%, more preferably about 0.3-80%, and relatively large (for example, 5% or more, 10% or more, 15% or more, 20% or more, 25% or more, 30% or more, 35% or more, 40% or more) or relatively small (for example, 5% or less, 4% or less, 3% or less, 2.5% or less, 2% or less, 1.5% or less, 1% or less).

  In the present invention, a capsule with relatively small variation can be provided. For example, when the standard deviation of the film thickness is SD and the film thickness (average thickness) is T, the value SD / T is 0.5 or less, preferably 0.4 or less, more preferably 0.3 or less, In particular, it may be 0.2 or less (for example, 0.16 or less), or 0.15 or less (for example, 0.14 or less, 0.13 or less, 0.12 or less, 0.11 or less, 0.10 or less). , 0.090 or less, 0.080 or less).

  When the thickness of the film or its ratio to the film thickness is small, it depends on the thinness of the film, and when the ratio of the film thickness or its film thickness is large, it is caused by the influence of surface tension in the capsule manufacturing process. Although it is difficult to obtain good capsules in each case, the present invention can provide capsules in any case.

  In the capsule of the present invention, the film ratio (ratio of the film to the whole capsule (total amount of film and inclusion)) is, for example, 0.1 to 99% by mass (for example, 0.5 to 95% by mass), preferably 1 ~ 90% by mass, more preferably 2 to 80% by mass (for example, 2.5 to 70% by mass), usually 3 to 60% by mass (for example, 3 to 50% by mass), which is relatively large. [For example, 10 mass% or more (for example, 12 to 90 mass%), preferably 15 mass% or more (for example, 18 to 80 mass%), more preferably 20 mass% or more (for example, 22 to 70 mass%), Usually, it can be 10 to 50% by mass (for example, 15 to 45% by mass) or relatively small [for example, 20% by mass or less (for example, 0.1 to 18% by mass), preferably 15% by mass. The following (for example, 0.5 to 2 mass%), more preferably 10 wt% or less (e.g., 1-8 wt%), particularly 8% by weight or less (for example, may be] a 2-7 wt% or less).

  As in the case of the thickness, it is usually difficult to obtain a capsule with a large diameter when the coating rate is large or small, but in the present invention, both when the coating rate is large and small. Good capsules can be obtained.

  In the capsule of the present invention, the moisture content of the film can be selected according to the use of the capsule and the like, for example, 50% by mass or less (for example, 0.1 to 40% by mass), preferably 30% by mass or less (for example, 0.5 to 25% by mass), more preferably 20% by mass or less (for example, 1 to 15% by mass).

  The strength (average strength) of the capsule (coating) of the present invention is not particularly limited. For example, the maximum load value when the capsule is pushed in by 5 mm is 0.1 N or more, preferably 0.2 N to 50 N, more preferably It may be about 0.3N to 30N. Although the capsule of the present invention has a relatively large particle size, it is not broken by a small impact and has practicality.

  The shape of the capsule (or film) of the present invention may be non-spherical (ellipsoidal, flat, etc.), but may be usually spherical.

  In the spherical capsule, the sphericity (average sphericity) may be, for example, 50% or more, preferably 60% or more, more preferably 70% or more, particularly 80% or more, and 85% or more (for example, 90% or more).

  In the present invention, in particular, when the particle size is relatively large, when the coating rate is small or large, when the coating thickness is small or large, when the coating thickness is small or large with respect to the coating diameter, the inclusion is a gel. Even in the case of a shape (gummy shape), a capsule with high sphericity can be obtained.

  The capsule of the present invention is usually stable and can retain its shape over a long period of time. For example, in the capsule of the present invention, when the diameter (average diameter) before storage is D1, and the diameter (average diameter) after storage for 6 months at 35 ° C. (sealed state) is D2, the value of D1 / D2 (average Value) is 0.5 to 2 (for example, 0.6 to 1.7), preferably 0.65 to 1.5 (for example, 0.7 to 1.4), and more preferably 0.8 to 1. .3 (e.g. 0.85-1.2), especially 0.9-1.1 (e.g. 0.95-1.05), substantially 1 (change in diameter before and after storage) None).

As described above, the capsule of the present invention has a coating (shell) and an inclusion (core) in the coating (inside).
The inclusion may form a plurality of layers (multilayers). That is, such a capsule may have a film and an inclusion (core) composed of a plurality of layers. The plurality of layers may be two or more layers, and may be, for example, 2 to 5 layers, preferably 2 to 4 layers, and more preferably 2 to 3 layers.

  The inclusion (inside the capsule, inside the film) may include a capsule (second capsule). Examples of the capsule including the second capsule in the inclusion include, for example, a capsule having a film (first capsule film) and a liquid component and an inclusion including the capsule dispersed in the liquid component. It is done. In such an inclusion, the number of second capsules may be one or more, and may be plural (for example, 2 to 10). Similar to the first capsule, the second capsule may have a film and an inclusion in the film. In such a second capsule, the same components as those described above can be used as the film or inclusion.

  As described above, the capsule of the present invention (first capsule) is usually a seamless capsule, but the second capsule does not necessarily need to be a seamless capsule. Like the first capsule, the capsule is a seamless capsule. There may be.

  In the capsule (first capsule, second capsule), the film and the inclusion may be insoluble (non-erodible) with each other. For example, when the film is water-soluble, the inclusion (or a portion of the inclusion that contacts the film) may be water-insoluble (hydrophobic).

  When the inclusion is a plurality of layers, the contact or adjacent layers may be insoluble in each other (for example, a water-soluble layer and a water-insoluble layer in contact with the water-soluble layer). May be configured). Furthermore, when the inclusion includes a liquid component (for example, a hydrophobic or oil-soluble liquid component) and a capsule (second capsule), at least the surface (film) of the second capsule is in contact with the liquid component. It may be insoluble (eg, water soluble).

  In addition, the capsule of this invention may have a coating layer (layer which coat | covers or coats a membrane | film | coat) as needed. The coating agent constituting the coating layer is not particularly limited and can be appropriately selected depending on the application. For example, cellulose derivatives (hydroxypropylmethylcellulose, methylcellulose, ethylcellulose, etc.), methacrylic acid copolymer, shellac, water-soluble shellac, silicone Examples include oil, carnauba wax and zein. These may be used individually by 1 type, and may be used in combination of 2 or more types as needed.

[Method for producing capsule]
The present invention includes a capsule manufacturing method.

  Capsules can usually be manufactured by a dropping method (seamless capsule method) using multiple nozzles. That is, the capsule can be obtained by filling the film (or the inside of the film) with the inclusion by a dropping method (dropping method).

  In the dropping method, for example, as shown in FIG. 1, a composite nozzle device arranged in a substantially concentric manner is used. The composite nozzle device includes, for example, an inner nozzle 4 that allows the content liquid supplied from the inlet A (liquid containing the constituents of the inclusions, and the inclusion liquid) to pass through, and the coating liquid supplied from the inlet B (the configuration of the coating). The inner nozzle 4 and the outer nozzle 5 are arranged substantially concentrically and are provided with a composite nozzle (concentric multiple nozzles). Then, using this composite nozzle device, the inner solution 1 supplied to the inner nozzle 4 is discharged from the discharge port of the inner nozzle 4 to the forming tube 7, and the coating liquid 2 supplied to the outer nozzle 5 is discharged from the outer nozzle 5. It is discharged to the forming tube 7 from the discharge port (width Y). The inner solution 1 and the coating liquid 2 are simultaneously discharged from the inner nozzle 4 and the outer nozzle 5 into the oil liquid or gas, forming a coaxial flow in the carrier flow 6 flowing downstream, Force is applied, the discharged liquid is cut at regular intervals, the cut portion is made spherical by the interface or surface tension between the oil liquid or gas and the film liquid, the film layer is gelled by cooling, and the capsule (wet capsule) ). The coating layer 2 surrounds the extruded inclusion 1 to form a capsule 3. The obtained capsule 3 may be recovered and dried to obtain a seamless capsule (dried capsule) in the final form.

  A seamless capsule typically includes a nozzle unit (concentric multiple nozzles) having an outer nozzle that allows the coating liquid to pass therethrough and an inner nozzle that supplies the content liquid concentrically, and a forming tube (on the downstream side or on the axis of the nozzle unit). Forming a capsule in the forming tube by discharging the content liquid from the discharge port of the inner nozzle and the coating liquid from the discharge port of the outer nozzle into the forming tube. It is manufactured through the process of making it.

Here, in this invention, it is preferable to adjust the conditions in this series of manufacturing processes.
For example, the distance between the center line (center line) of the concentric multi-nozzle and the center line (center line) of the forming tube (ie, the deviation from the center of the forming tube of the concentric multi-nozzle) is X, and the capsule (film) ), The value X / D is 3.5 or less (for example, 3.2 or less), preferably 3 or less (for example, 2.5 or less), more preferably 2.4 or less (for example, 2.35 or less), particularly preferably 2.3 or less (for example, 2.2 or less), usually 2 or less (for example, 1.9 or less), and 1.8 or less (for example, 1.7 or less), 1.5 or less, 1 or less, 0.7 or less, 0.5 or less.

  In addition, when the width of the discharge port of the inner nozzle (that is, the nozzle interval) is Y and the diameter of the capsule (film) is D, the value Y / D is 0.4 or less (for example, 0.001 to 0.00). 37), preferably 0.35 or less (for example, 0.005 to 0.34), more preferably 0.3 or less (for example, 0.01 to 0.29), particularly preferably 0.28 or less (for example, 0.03 to 0.26), and most preferably 0.25 or less (for example, 0.05 to 0.25).

By adjusting (selecting) such conditions, seamless capsules, particularly seamless capsules having a relatively large particle size as described above, can be obtained efficiently. Moreover, by adjusting such conditions, it is easy to obtain seamless capsules with a small deviation in film thickness and seamless capsules with small variations among a plurality of capsules.
In addition, the moldability itself of the capsule is high, and the raw material can be encapsulated relatively easily.
For example, in the method of the present invention, the yield rate (mass ratio of the encapsulated raw material among the raw materials) is 20% or more (for example, 30% or more), preferably 40% or more (for example, 50% or more), more preferably May be 60% or more (for example, 70% or more), particularly 80% or more (for example, 85% or more).

The film liquid and the content liquid are liquids (liquid components) containing the constituent components of the film and the inclusion, respectively. Such a liquid may be liquefied by warming (heating) melting and may contain a solvent.
For example, the film solution may be a solution in which a film-forming component (such as agar) is dissolved in a solvent (for example, water, alcohol such as ethanol, particularly water). In addition, when the inclusion is a liquid component, the inclusion liquid may be the content liquid. When the inclusion is in a solid state (such as a gel), the inclusion liquid is liquefied with a solvent. Alternatively, the inclusion liquid heated and melted may be used as the content liquid.

  The viscosity of the coating liquid and the content liquid can be selected as appropriate. For example, the viscosity of the coating liquid may be, for example, 50 mPa · s or more (for example, 70 to 500 mPa · s, preferably 80 to 300 mPa · s). Moreover, the viscosity of the content liquid should just be a range which can ensure fluidity | liquidity, and can be suitably selected according to the kind of inclusion, etc.

  In addition, other manufacturing conditions (temperature of coating liquid, temperature of contents liquid, cooling temperature, cooling time, drying temperature, drying time, etc.) depend on the type of coating liquid and inclusion, the thickness of the coating, the coating rate, etc. Can be appropriately selected.

  EXAMPLES Next, the present invention will be described more specifically with reference to examples. However, the present invention is not limited to these examples at all, and many variations are within the technical idea of the present invention. This is possible by those with ordinary knowledge.

  Various physical properties were measured or evaluated as follows.

[Diameter of film (outer diameter of capsule), thickness, SD value, sphericity]
Using a caliper (Mitutoyo Digital Caliper CD-10CX), the major axis and minor axis of the capsule were measured.
And the diameter (average diameter) was calculated | required as an arithmetic average of a major axis and a minor axis.
The sphericity was [minor axis / diameter] × 100 (%).
In addition, the capsule was cut vertically and horizontally, and the maximum thickness and the minimum thickness were measured using the same caliper. The capsule thickness (average thickness) was the arithmetic average of these, and the ratio T2 / T1 of the maximum thickness T2 to the minimum thickness T1 of the film was calculated based on these thicknesses.
Note that the number of measurements was 10 (n = 10), and the arithmetic average of these values was taken as each value.
SD value is the standard deviation.

[Yield rate]
The yield ratio was defined as the mass ratio of the amount that could be encapsulated (the amount that resisted drying and retained the capsule shape) to the amount of raw material used. The raw materials that have not been encapsulated include those that did not form capsules at all, and those that cracked during drying.

[Moldability]
The formability of the seamless capsule was evaluated as follows.
A: Encapsulation was possible at a yield rate of 80% or more.
◯: Encapsulation was possible at a yield rate of 50% or more and less than 80%.
Δ: Encapsulation was possible at a yield rate of less than 50%.
X: Encapsulation was not possible.

[Stability test]
The capsule was put into a No. 6 bottle, capped, and stored at 35 ° C. for 6 months with the cap closed.
The capsules after storage were evaluated according to the following criteria.
(Capsule deformation)
◯: When the diameter of the film before storage is D2, and the diameter of the film after storage is D1, the value of D1 / D2 is 0.9 to 1.1 (1 or almost 1).
X: The value of D1 / D2 is much smaller than 0.9 or much larger than 1.1.
(Capsule breakage / leakage)
The capsules were checked for breakage and leakage.

In the following specifications (prescriptions), the in-liquid dripping method (extruding a fluid liquid from a concentric nozzle while giving vibration at regular intervals to cool the capsule in the liquid as described in the above figure. An attempt was made to produce seamless capsules by a method of molding capsules with
The submerged dropping method was performed under the conditions shown in the following table, and the coating solution and the content solution were prepared as follows.
(Coating fluid)
Prepared by mixing the raw material and an appropriate amount of water, then heated at a predetermined temperature (about 65-90 ° C.) for 2 hours or more with appropriate stirring, and confirming that all the raw material was dissolved. . In addition, deaeration by suction type defoaming using a vacuum pump or centrifugation was performed as needed.
(Content liquid)
It heated as needed and mixed so that a raw material might become uniform. In addition, since it was necessary to be liquid at the time of filling, when gel or fluidity | liquidity was bad, it heated suitably and took out fluidity | liquidity. In mixing, a high-speed stirrer and / or a fine pulverizer was used as necessary.

The results are shown in the table below.

  In the present invention, a seamless capsule having a relatively large particle size can be obtained.

1 Inclusion 2 Film layer (film)
3 Seamless Capsule 4 Inner Nozzle 5 Outer Nozzle 6 Carrier Flow 7 Forming Tube A Inner Fluid Input B B Coating Fluid Input

Claims (16)

  A seamless capsule having a diameter of 5 mm or more and a ratio T2 / T1 of the maximum thickness T2 to the minimum thickness T1 of the film being 3.5 or less.   The seamless capsule according to claim 1, which has a diameter of 7 mm or more.   The seamless capsule according to claim 1 or 2, wherein the diameter is 10 mm or more, and the ratio T2 / T1 of the maximum thickness T2 to the minimum thickness T1 of the film is 3 or less.   The seamless capsule according to any one of claims 1 to 3, wherein a ratio T2 / T1 of the maximum thickness T2 to the minimum thickness T1 of the film is 2.3 or less.   The seamless capsule according to any one of claims 1 to 4, which has a sphericity of 80% or more.   6. The seamless according to any one of claims 1 to 5, wherein the diameter is 10 mm or more, the ratio T2 / T1 of the maximum thickness T2 to the minimum thickness T1 of the film is 2.1 or less, and the sphericity is 85% or more. capsule.   The seamless capsule according to any one of claims 1 to 6, wherein the coating rate is 3 to 60% by mass.   The seamless capsule according to any one of claims 1 to 7, wherein the coating rate is 10% by mass or less.   The seamless capsule according to any one of claims 1 to 8, wherein the coverage is 15% by mass or more.   The seamless capsule according to any one of claims 1 to 9, which has a diameter of 13 mm or more.   The seamless capsule according to any one of claims 1 to 10, which has a diameter of 15 mm or more.   The seamless capsule according to any one of claims 1 to 11, wherein the inclusion is in a gel form.   The seamless capsule according to any one of claims 1 to 12, wherein the value [SD / T] is 0.2 or less, where SD is the standard deviation of the thickness of the coating and T is the thickness of the coating. Using an apparatus comprising a concentric multiple nozzle concentrically provided with an outer nozzle that allows passage of the coating liquid containing the constituents of the film and an inner nozzle that supplies the content liquid containing the constituents of the inclusion, and a forming tube, A seamless capsule manufacturing method including a capsule forming step of forming a capsule in a forming tube by discharging a content liquid from a discharge port of a nozzle and a coating liquid from a discharge port of an outer nozzle, respectively,
When the distance between the axis of the concentric multiple nozzle and the axis of the forming tube is X and the diameter of the capsule is D, the value X / D is adjusted to be 3 or less, and
A method for producing a seamless capsule, wherein the value Y / D is adjusted to 0.4 or less, where Y is the width of the discharge port of the inner nozzle and D is the diameter of the capsule.   The production method according to claim 14, wherein the value X / D is adjusted to 2 or less and the value Y / D is adjusted to 0.28 or less to obtain a seamless capsule at a yield rate of 80% or more.   The manufacturing method according to claim 14 or 15, wherein the seamless capsule is the seamless capsule according to any one of claims 1 to 13.