JP4605665B2 - Solid milk and method for producing the same - Google Patents
Solid milk and method for producing the same Download PDFInfo
- Publication number
- JP4605665B2 JP4605665B2 JP2007292818A JP2007292818A JP4605665B2 JP 4605665 B2 JP4605665 B2 JP 4605665B2 JP 2007292818 A JP2007292818 A JP 2007292818A JP 2007292818 A JP2007292818 A JP 2007292818A JP 4605665 B2 JP4605665 B2 JP 4605665B2
- Authority
- JP
- Japan
- Prior art keywords
- milk
- solid
- solid milk
- milk powder
- fat
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Active
Links
Images
Description
本発明は，温水に溶かして飲用する固形乳，及びその製造方法に関する。より詳しくは，本発明は，好適な溶解性と強度とを有する固形乳，及びその製造方法に関する。 The present invention relates to a solid milk that is dissolved in warm water for drinking and a method for producing the same. More specifically, the present invention relates to solid milk having suitable solubility and strength, and a method for producing the same.
粉乳は，牛乳などから微生物の成育に必要な水分をほとんど取り除くことによって，保存性を高めた食品である。水分を除去すると容積及び重量が減るので，粉乳を容易に輸送できる。このように粉乳は，保存性，輸送の面で利点が多い。粉乳は，粉乳同士の間に隙間があるので，粉乳の空隙率は，一般に６０％〜７０％であり，温水に容易に溶ける。しかし，粉乳は，温水などに溶かす際に，その都度適量を計量しなければならない。また，粉乳を計量する際や，粉乳を取り出す際などに，粉乳が散らかることがある。そこで，粉乳を固形状態にした固形乳が提案されている（実開昭４９−１３０１８９号公報，及び実開昭６１−１１８２８０号公報参照）。しかし，粉乳を実際に固形状態にし，強度と溶解性とを両立させることは，容易ではなかった。つまり，粉乳を固形状態にしても，容易に壊れ，扱いにくかった。さらに固形乳は，粉乳に比べて表面積が少ないので，温水に溶けにくかった。 Powdered milk is a food that has been preserved by removing most of the water necessary for the growth of microorganisms from milk. Since removing the water reduces the volume and weight, milk powder can be transported easily. Thus, milk powder has many advantages in terms of storage stability and transportation. Since powdered milk has a gap between powdered milk, the porosity of the powdered milk is generally 60% to 70% and easily dissolves in warm water. However, when milk powder is dissolved in warm water, an appropriate amount must be measured each time. In addition, milk powder may be scattered when measuring milk powder or taking out milk powder. Therefore, solid milk in which milk powder is in a solid state has been proposed (see Japanese Utility Model Publication Nos. 49-130189 and 61-118280). However, it was not easy to make milk powder into a solid state and achieve both strength and solubility. In other words, even when milk powder was in a solid state, it was easily broken and difficult to handle. Furthermore, since solid milk has a smaller surface area than powdered milk, it was difficult to dissolve in warm water.
実際に粉乳に圧力を加えて固形状態にする場合，粉乳が乳化物であるため，圧力により乳化状態が壊れる。すると，粉乳から脂肪がしみ出す（この脂肪は，「遊離脂肪」と呼ばれる）。この遊離脂肪は，酸化しやすく，粉乳の風味を損なう。また，粉乳を温水に溶かした際に，過剰の遊離脂肪は，水面に浮き凝集するという問題がある（この現象は,「オイルオフ」と呼ばれる）。一方，特公昭４９−４９４８号には，「団粒化粉乳」が開示されている。そして，「団粒化粉乳は，その内部組織が多孔質になっているため，浸水し易く，したがって，温湯中に投入すると容易に崩壊し，分散して溶解する」点が開示されている。しかしながら，同公報における「団粒化粉乳」は，シュガー又はグルコースとの混合物であり，「コーヒー紅茶等に添加して使用するのにも適している」というものである。すなわち，粉乳のみを原料とするものではないし，乳幼児に母乳の代わりに与えるものでもない。特公昭４９−４９４８号公報では，粉乳のみを原料とする場合の遊離脂肪の問題などから，顆粒状態の粉乳と，シュガー又はグルコースとの混合物を用いて「団粒化粉乳」としたのである。顆粒状態の粉乳であれば固形化状態に比べ表面積が広くなるので，顆粒自体の空隙率が小さくても溶解性は高い。 When pressure is applied to powdered milk to make it into a solid state, the powdered milk is an emulsion, so the emulsified state is broken by the pressure. The fat then oozes from the milk powder (this fat is called “free fat”). This free fat is easily oxidized and impairs the flavor of milk powder. In addition, when powdered milk is dissolved in warm water, there is a problem that excess free fat floats and aggregates on the water surface (this phenomenon is called “oil-off”). On the other hand, Japanese Patent Publication No. 49-4948 discloses “aggregated milk powder”. Further, it is disclosed that “aggregated powdered milk has a porous internal structure, so that it is easy to be submerged, and therefore easily disintegrates, disperses and dissolves when poured into hot water”. However, the “aggregated milk powder” in the publication is a mixture with sugar or glucose and is “suitable to be added to coffee tea or the like”. In other words, it does not use only powdered milk as a raw material, nor does it give infants instead of breast milk. In Japanese Examined Patent Publication No. 49-4948, due to the problem of free fat when only powdered milk is used as a raw material, a “aggregated powdered milk” is made using a mixture of granular powdered milk and sugar or glucose. Since powdered milk powder in a granular state has a larger surface area than a solidified state, the solubility is high even if the porosity of the granule itself is small.
特公昭４５−３９０１８号公報には，上記特公昭４９−４９４８号公報と同様の技術が開示されている。すなわち，溶け易い固形乳を得るためには，空隙容積を大きくすれば良い点や，粉乳を固形化する際に遊離脂肪の問題がある点が開示されている。しかし，同文献では，「粉乳の単一粒子の増大化には限度がある」ので（同文献第２欄第３０行目），「糖類に粉乳を付着させて，造粒した後成形乾燥すること」により「遊離脂肪の少ない易溶性固形乳」を得ている（同文献第３欄第１３行目〜第１５行目）。すなわち，同文献も粉乳のみを固形状態とした固形乳を得ることはできないとされている。
Japanese Patent Publication No. 45-39018 discloses a technique similar to that of the above Japanese Patent Publication No. 49-4948. That is, in order to obtain easily meltable solid milk, it is disclosed that the void volume should be increased and that there is a problem of free fat when solidifying milk powder. However, in the same document, “There is a limit to the increase of single particles of milk powder” (the second column,
特開昭５３−５９０６６号公報には，「固形ミルクタブレット」が開示されている。この固形ミルクタブレットは，脂肪分を表面に浸出させ，脂肪の被膜により外気と遮断された高密度のタブレットである。同文献の固形ミルクは，高密度のタブレットが望ましいので，その空隙率は低い。 Japanese Patent Laid-Open No. 53-59066 discloses a “solid milk tablet”. This solid milk tablet is a high-density tablet in which fat is leached to the surface and is blocked from the outside air by a fat coating. The solid milk of this document is preferably a high-density tablet, so its porosity is low.
特許第３０４４６３５号公報には，「冷凍ミルク」が開示されている。この冷凍ミルクは，凍らせるために水分を多く含んでおり，空隙は殆どない。 Japanese Patent No. 3044635 discloses “frozen milk”. This frozen milk contains a lot of water for freezing and has almost no voids.
また，ス−プなど食品の分野において，熱水をかけて溶かす固形状の食品が知られている（特開平１１−１２７８２３号公報，特開２００４−４９２２０号公報，及び特開２００４−４９２２１号公報）。これらは，一般に崩壊剤などが添加されている。また，これらの原料は，粉乳ではないため，粉乳特有の遊離脂肪などの問題はない。すなわち，固形状のスープなどが知られているが，これらの技術を単に固形乳を製造する際に転用しても，固形乳の原料である粉乳には脂肪が多いので，固形乳を得ることはできない。 Further, in the field of foods such as soup, solid foods that are dissolved by applying hot water are known (Japanese Patent Laid-Open Nos. 11-127823, 2004-49220, and 2004-49221). Publication). These are generally added with disintegrants. Moreover, since these raw materials are not milk powder, there are no problems such as free fat peculiar to milk powder. In other words, solid soups are known, but even if these techniques are simply used to produce solid milk, the milk powder, which is the raw material for solid milk, contains a lot of fat, so that solid milk can be obtained. I can't.
また，医薬の分野においては，口の中で容易に溶ける様々な「口腔内速崩壊錠」が開発されている（例えば，特開平５−２７１０５４号公報，特開平８−２９１０５１号公報，特開２０００−９５６７４号公報，特開２０００−４４４６３号公報，特開２００１−８９３９８号公報，及び特許第２６５０４９３号公報）。しかしながら，一般的に医薬の組成においては，有効成分が占有する重量割合が少ない。よって，医薬では，有効成分以外である賦形剤などの添加剤を多く配合することができ，比較的容易に組成を設計できる。また，医薬は，粉乳のような脂肪を多く含むものではない。したがって，「口腔内速崩壊錠」における「速崩壊」技術をそのまま，固形乳に転用することはできない。また，「口腔内速崩壊錠」は，口腔内のわずかな水分により，迅速に溶けなければならない。一方，固形乳は，一般には温水に溶かし飲用するものであって，直接口にするものではないので，「口腔内速崩壊錠」程の速溶解性は必要とされない。
本発明は，好適な溶解性と強度とを有する固形乳及びその製造方法を提供することを目的とする。 An object of this invention is to provide the solid milk which has suitable solubility and intensity | strength, and its manufacturing method.
本発明は，運搬などの取り扱いが容易であり，計量が容易である固形乳及びその製造方法を提供することを別の目的とする。 Another object of the present invention is to provide a solid milk that can be easily handled such as transport and can be easily metered, and a method for producing the same.
本発明は，風味の劣化やオイルオフなど遊離脂肪に起因する経時劣化の少ない固形乳及びその製造方法を提供することを別の目的とする。 Another object of the present invention is to provide a solid milk that is less deteriorated with time due to free fat such as flavor deterioration and oil-off, and a method for producing the same.
本発明は，成分組成を栄養成分だけで制御できる固形乳及びその製造方法を提供することを別の目的とする。 Another object of the present invention is to provide a solid milk whose component composition can be controlled only by nutritional components and a method for producing the same.
本発明は，粉乳に滑沢剤などの添加剤を添加せずに，そのまま固形乳を製造できる固形乳の製造方法を提供することを別の目的とする。 Another object of the present invention is to provide a method for producing solid milk that can produce solid milk as it is without adding additives such as a lubricant to powdered milk.
本発明は，製造工程において，打錠機の杵やうすに粉乳が付着する事態を防止できる固形乳の製造方法を提供することを別の目的とする。 Another object of the present invention is to provide a method for producing solid milk that can prevent a situation in which powdered milk adheres to the punches and thins of a tableting machine in the production process.
本発明は，粉乳を製造した後，粉乳のみならず，その粉乳に基づく固形乳をも製造できる粉乳及び固形乳の製造方法を提供することを別の目的とする。 Another object of the present invention is to provide a milk powder and a method for producing the solid milk that can produce not only the milk powder but also the solid milk based on the milk powder after the milk powder is produced.
本発明は，基本的には，粉乳のみを原料として空隙率及び遊離脂肪を一定範囲に制御した状態で圧縮成形した後，加湿及び乾燥処理することにより，充分な強度と溶解性と兼ね備える固形乳を得ることができるとの知見に基づくものである。上記の課題のうち少なくとも一つは，以下の固形乳及び固形乳の製造方法によって解決される。 Basically, the present invention is a solid milk having sufficient strength and solubility by compression-molding with only powdered milk as a raw material in a state where the porosity and free fat are controlled within a certain range, followed by humidification and drying treatment. It is based on the knowledge that can be obtained. At least one of the above problems is solved by the following solid milk and solid milk production method.
空隙率が，３０％〜５０％であり，粉乳のみを原料とする固形乳。 Solid milk having a porosity of 30% to 50% and using only powdered milk as a raw material.
脂肪として，乳化した脂肪と遊離脂肪とを含み，前記遊離脂肪の含有率が０．５重量％〜４重量％であり，
脂肪の含有率が，５重量％以上である，
上記に記載の固形乳。
The fat includes emulsified fat and free fat, and the content of the free fat is 0.5 wt% to 4 wt%,
The fat content is 5% by weight or more,
Solid milk as described above.
水の含有率が，１重量％〜４重量％である上記に記載の固形乳。 The solid milk as described above, wherein the water content is 1% by weight to 4% by weight.
体積が，１ｃｍ３〜５０ｃｍ３である上記に記載の固形乳。 Volume, above solid milk according a 1 cm 3 to 50 cm 3.
５０℃の水１００ｍｌに固形乳を１個入れ，１．５往復／ｓ，振幅３０ｃｍの振とう条件において，固形乳が完全になくなるまでに要する時間が，５秒〜１８０秒である上記に記載の固形乳。 The solid milk is placed in 100 ml of water at 50 ° C., and it takes 5 seconds to 180 seconds until the solid milk is completely removed under a shaking condition of 1.5 reciprocations / s and an amplitude of 30 cm. Solid milk.
試料の破断面の面積が最小となる方向に荷重をかけて破断するときの力が，３０Ｎ〜３００Ｎである上記に記載の固形乳。 The solid milk as described above, wherein the force when the load is broken in a direction in which the area of the fracture surface of the sample is minimized is 30N to 300N.
粉乳を圧縮して固形状の粉乳圧縮物を得るための圧縮工程と，
前記圧縮工程で得られた粉乳圧縮物を湿らせるための加湿工程と，
前記加湿工程で加湿された粉乳圧縮物を乾燥させるための乾燥工程とを含み，
前記粉乳の水分含有率が，１重量％〜４重量％であり，
前記粉乳の脂肪含有率が５重量％以上７０重量％以下であり，
前記粉乳圧縮物の遊離脂肪含有率が０．５重量％〜４重量％であり，前記圧縮工程は，打錠機により粉乳を圧縮し，
前記圧縮工程において，粉乳を圧縮する圧縮力が，１ＭＰａ〜１５ＭＰａであり，
前記加湿工程において，前記粉乳圧縮物に加えられる水分の量が，前記圧縮工程後の粉乳圧縮物の質量の０．５〜３％であり，
前記乾燥工程において，固形乳の水分含有率を原料として用いる粉乳の水分含有率の前後１％以内に制御する固形乳の製造方法により製造された上記に記載の固形乳。
A compression step for compressing the powdered milk to obtain a solid powdered milk compressed product,
A humidifying step for moistening the compressed milk powder obtained in the compression step;
A drying step for drying the compressed milk powder compressed in the humidifying step,
The water content of the milk powder is 1 wt% to 4 wt%,
The fat content of the milk powder is 5 wt% or more and 70 wt% or less,
The free fat content of the compressed milk powder is 0.5 wt% to 4 wt%, and the compressing step compresses the milk powder with a tableting machine,
In the compression step, the compression force for compressing the milk powder is 1 MPa to 15 MPa,
In the humidification step, the amount of water added to the compressed milk powder is 0.5 to 3% of the mass of the compressed milk powder after the compression step,
The solid milk as described above, which is produced by the method for producing solid milk, wherein the moisture content of the solid milk is controlled within 1% before and after the moisture content of the milk powder used as a raw material in the drying step.
本発明によれば，固形乳の空隙率を制御することにより，好適な溶解性と強度とを有する固形乳及びその製造方法を提供できる。 ADVANTAGE OF THE INVENTION According to this invention, the solid milk which has suitable solubility and intensity | strength, and its manufacturing method can be provided by controlling the porosity of solid milk.
本発明によれば，所定の形状や大きさを有する固形乳を提供できるので，運搬などの取り扱いが容易であり，計量が容易である固形乳及びその製造方法を提供できる。 According to the present invention, since solid milk having a predetermined shape and size can be provided, it is possible to provide solid milk that is easy to handle and can be easily metered, and a method for producing the same.
本発明によれば，粉乳の保存中に脂質が酸化劣化して起こる風味低下の原因とされていた遊離脂肪を，支障のない範囲で意図的に発生させる。そして，遊離脂肪を滑沢剤などとして有効に活用することで添加剤を加えることなく，遊離脂肪に起因する経時劣化の少ない固形乳及びその製造方法を提供できる。 According to the present invention, free fat, which has been a cause of flavor reduction caused by oxidative degradation of lipid during storage of powdered milk, is intentionally generated within a range that does not hinder. Further, by effectively utilizing free fat as a lubricant and the like, it is possible to provide solid milk with little deterioration with time due to free fat and a method for producing the same without adding additives.
本発明によれば，粉乳をそのまま固形乳にできるので，粉乳自体の組成を制御することで固形乳の成分組成を栄養成分だけで制御できる固形乳及びその製造方法を提供できる。 According to the present invention, powdered milk can be made into solid milk as it is. Therefore, by controlling the composition of the powdered milk itself, it is possible to provide a solid milk capable of controlling the composition of the solid milk only with the nutritional component and a method for producing the same.
本発明によれば，その圧縮工程において，粉乳の遊離脂肪率，粉乳の空隙率及び水分量（特に遊離脂肪率）を適切な範囲に制御することにより，打錠機の杵やうすに粉乳が付着する事態を防止でき，生産性の高い固形乳の製造方法を提供できる。 According to the present invention, in the compression step, the powdered milk can be added to the straw or thin of the tableting machine by controlling the free fat ratio of the milk powder, the porosity of the milk powder, and the water content (particularly the free fat ratio) to an appropriate range. It is possible to prevent the adhering situation and to provide a method for producing solid milk with high productivity.
本発明によれば，上記のとおり，遊離脂肪を添加剤の代わりとして有効に活用できるので，粉乳に滑沢剤などの添加剤を添加せずに，そのまま固形乳とすることができる固形乳の製造方法を提供できる。 According to the present invention, as described above, free fat can be effectively used as a substitute for an additive, so that solid milk that can be used as a solid milk as it is without adding additives such as a lubricant to powdered milk. A manufacturing method can be provided.
本発明によれば，粉乳を製造した後，粉乳のみならず，その粉乳に基づく固形乳をも製造できる粉乳及び固形乳の製造方法を提供できる。 ADVANTAGE OF THE INVENTION According to this invention, after manufacturing milk powder, the manufacturing method of milk powder and solid milk which can manufacture not only milk powder but solid milk based on the milk powder can be provided.
本発明の固形乳のひとつの側面は，空隙率が，３０％〜５０％である固形乳である。先に説明したとおり，昭和４０年代の終わり頃から，固形乳を製造しようとする提案はあった。しかしながら，硬い固形乳は溶けにくく，溶解性の高い固形乳はもろいという問題がある。そのため，硬度と溶解性の両方を満足する固形乳は，得られなかった。本発明者らは，空隙率（圧縮力）や遊離脂肪の量を制御して固形乳を製造することにより，空隙率が３０％〜５０％である固形乳を初めて製造したのである。そして，このようにして製造した固形乳は，硬度と溶解性とを備えたものであった。すなわち，本発明の固形乳は，好ましくは，空隙率が３０％〜５０％であるので，製造時において必要な硬度と、使用時において必要な溶解性とを得ることができる。 One aspect of the solid milk of the present invention is a solid milk having a porosity of 30% to 50%. As explained earlier, there was a proposal to manufacture solid milk from the end of the Showa 40s. However, there is a problem that hard solid milk is difficult to dissolve and solid milk with high solubility is brittle. Therefore, solid milk satisfying both hardness and solubility could not be obtained. The inventors of the present invention have produced solid milk having a porosity of 30% to 50% for the first time by producing solid milk by controlling the porosity (compression force) and the amount of free fat. And the solid milk manufactured in this way was equipped with hardness and solubility. That is, since the solid milk of the present invention preferably has a porosity of 30% to 50%, it is possible to obtain the hardness required at the time of manufacture and the solubility required at the time of use.
本発明の固形乳の別の側面は，脂肪の含有率が，５重量％以上である上記に記載の固形乳である。なお，「脂肪の含有率」とは，固形乳全体の重量における脂肪の割合を意味する。そして，脂肪の含有率の「５重量％以上」として，より具体的には後述のとおり５重量％〜７０重量％などがあげられる。 Another aspect of the solid milk of the present invention is the solid milk described above, wherein the fat content is 5% by weight or more. “Fat content” means the proportion of fat in the weight of the whole solid milk. And more specifically, as described later, “5 wt% or more” of the fat content is 5 wt% to 70 wt%.
本発明の固形乳の別の側面は，脂肪として，乳化した脂肪と遊離脂肪とを含み，前記遊離脂肪の含有率（固形乳全体の重量における遊離脂肪の割合）が０．５重量％〜４重量％である上記に記載の固形乳である。後に説明するように，本発明の固形乳は，従来発生させないことが望ましいとされた遊離脂肪を積極的に含むことにより，所定の空隙を有する固形乳を得るものである。 Another aspect of the solid milk of the present invention includes, as fat, emulsified fat and free fat, and the content of the free fat (ratio of free fat in the weight of the whole solid milk) is 0.5% by weight to 4%. It is a solid milk as described above which is weight%. As will be described later, the solid milk of the present invention is intended to obtain solid milk having a predetermined gap by positively containing free fat, which is conventionally desired not to be generated.
本発明の固形乳の別の側面は，水の含有率が，１重量％〜４重量％である上記に記載の固形乳である。本発明の固形乳の別の側面は，体積が，１ｃｍ３〜５０ｃｍ３である上記に記載の固形乳である。本発明の固形乳は，固形乳であるので従来の粉乳に比べ大きな体積を持ち，容易に適量を計量でき，又運搬も便利である。 Another aspect of the solid milk of the present invention is the above-described solid milk having a water content of 1% by weight to 4% by weight. Another aspect of the solid milk of the present invention, the volume is the solid milk according to the above is a 1 cm 3 to 50 cm 3. Since the solid milk of the present invention is a solid milk, it has a larger volume than conventional powdered milk, can easily measure an appropriate amount, and is convenient to transport.
本発明の固形乳の別の側面は，原料として粉乳を用い，固形乳の組成が均一である上記に記載の固形乳である。原料として遊離脂肪を含むなど所定の粉乳を用いるので，糖による核などを形成しなくとも，粉乳のみからなる固形乳を製造できる。本発明の固形乳の別の側面は，粉乳のみを原料とする上記に記載の固形乳である。粉乳のみを原料とすれば，容易に均一な組成の固形乳を得ることができる。本発明の固形乳の別の側面は，５０℃の水１００ｍｌに固形乳を１個入れ，１．５往復／s，振幅３０ｃｍの振とう条件において，固形乳が完全になくなるまでに要する時間が５秒〜１８０秒である上記に記載の固形乳である。本発明の固形乳は，所定の空隙率を有するので，速溶解性を有するものであり，商品として市場の要求を満足できる。本発明の固形乳の別の側面は，試料の破断面の面積が最小となる方向に荷重をかけて破断するときの力が，３０Ｎ〜３００Ｎである上記に記載の固形乳である。本発明の固形乳は，ある程度の硬度を有するので，運搬の際に壊れる事態などをある程度防止し得る。なお，本発明の固形乳の別の側面は，３０％〜５０％の空隙率を有し，脂肪の含有率が５重量％〜７０重量％であり，遊離脂肪の含有率が固形乳全体の０．５重量％〜４重量％であり，水の含有率が，１重量％〜４重量％であり，体積が１ｃｍ３〜５０ｃｍ３であり，原料として粉乳のみを用いた固形乳である。このような構成を採用する固形乳は，上記で表される速溶解性や上記の硬度を有するものである。 Another aspect of the solid milk of the present invention is the solid milk described above, wherein powdered milk is used as a raw material and the composition of the solid milk is uniform. Since a predetermined powdered milk containing free fat as a raw material is used, a solid milk consisting only of the powdered milk can be produced without forming a sugar core or the like. Another aspect of the solid milk of the present invention is the solid milk described above using only powdered milk as a raw material. If only powdered milk is used as a raw material, solid milk having a uniform composition can be easily obtained. Another aspect of the solid milk of the present invention is that it takes one solid milk in 100 ml of water at 50 ° C., and the time required for the solid milk to completely disappear under shaking conditions of 1.5 reciprocations / s and an amplitude of 30 cm. It is solid milk as described in the above which is 5 seconds to 180 seconds. Since the solid milk of the present invention has a predetermined porosity, it has fast solubility and can satisfy the market demand as a product. Another aspect of the solid milk of the present invention is the solid milk described above, wherein the force when the load is broken in a direction in which the area of the fracture surface of the sample is minimized is 30N to 300N. Since the solid milk of the present invention has a certain degree of hardness, it can prevent to some extent the situation that it breaks during transportation. In addition, another aspect of the solid milk of the present invention has a porosity of 30% to 50%, a fat content of 5% to 70% by weight, and a free fat content of the whole solid milk. 0.5 wt% to 4 wt%, water content is 1% to 4%, volume is 1 cm 3 to 50 cm 3, a solid milk using only powdered milk as a raw material. The solid milk adopting such a configuration has the fast solubility and the hardness described above.
本発明の固形乳の製造方法のある側面は，粉乳を圧縮し固形状の粉乳圧縮物を得るための圧縮工程と，前記圧縮工程で得られた粉乳圧縮物を湿らせるための加湿工程と，前記加湿工程で加湿された粉乳圧縮物を乾燥させるための乾燥工程とを含む固形乳の製造方法である。本発明の固形乳の製造方法の別の側面は，前記圧縮工程において，原料に添加剤を実質的に添加しない上記に記載の固形乳の製造方法である。本発明の固形乳の製造方法の別の側面は，前記圧縮工程において，脂肪含有率が５重量％以上の粉乳を用いる上記に記載の固形乳の製造方法である。本発明の固形乳の製造方法の別の側面は，粉乳圧縮物の遊離脂肪含有率が０．５重量％〜４重量％である上記に記載の固形乳の製造方法である。本発明の製造方法においては，従来発生させないことが望ましいとされた遊離脂肪を積極的に含むことにより，所定の空隙を有する固形乳を得ることができる。本発明の固形乳の製造方法の別の側面は，前記圧縮工程において，粉乳圧縮物の空隙率を３０％〜５０％となるように圧縮力を制御する上記に記載の固形乳の製造方法である。本発明の固形乳の製造方法の別の側面は，前記圧縮工程において，粉乳を圧縮する圧縮力が，１ＭＰａ〜１５ＭＰａである上記に記載の固形乳の製造方法である。本発明の固形乳の製造方法の別の側面は，前記加湿工程において，前記粉乳圧縮物に加えられる水分の量が，前記圧縮工程後の粉乳圧縮物の質量の０．５〜３％である上記に記載の固形乳の製造方法である。本発明の固形乳の製造方法の別の側面は，前記乾燥工程において，固形乳の水分含有率を原料として用いる粉乳の水分含有率の前後１％以内に制御する上記に記載の固形乳の製造方法である。 A certain aspect of the method for producing solid milk of the present invention includes a compression step for compressing milk powder to obtain a solid milk powder compressed product, and a humidifying step for moistening the milk powder compressed material obtained in the compression step, It is a manufacturing method of solid milk including the drying process for drying the compressed milk powder humidified in the humidification process. Another aspect of the method for producing solid milk of the present invention is the method for producing solid milk as described above, wherein an additive is not substantially added to the raw material in the compression step. Another aspect of the method for producing solid milk according to the present invention is the method for producing solid milk as described above, wherein milk powder having a fat content of 5% by weight or more is used in the compression step. Another aspect of the method for producing solid milk of the present invention is the method for producing solid milk as described above, wherein the free fat content of the compressed milk powder is 0.5% by weight to 4% by weight. In the production method of the present invention, solid milk having a predetermined gap can be obtained by positively containing free fat, which is conventionally desired not to be generated. Another aspect of the method for producing solid milk of the present invention is the method for producing solid milk as described above, wherein the compression force is controlled so that the porosity of the compressed milk powder is 30% to 50% in the compression step. is there. Another aspect of the method for producing solid milk of the present invention is the method for producing solid milk as described above, wherein the compression force for compressing the milk powder is 1 MPa to 15 MPa in the compression step. In another aspect of the method for producing solid milk of the present invention, in the humidification step, the amount of water added to the compressed milk powder is 0.5 to 3% of the mass of the compressed milk powder after the compression step. It is a manufacturing method of the solid milk as described above. Another aspect of the method for producing solid milk of the present invention is the production of the solid milk as described above, wherein in the drying step, the moisture content of the solid milk is controlled within 1% before and after the moisture content of the powdered milk used as a raw material. Is the method.
本明細書において「空隙率」とは，粉体の嵩体積中空隙が占める体積の割合を意味し（例えば，宮嶋孝一郎編集「医薬品の開発」（第１５巻）廣川書店平成元年（１９８９年）発行，第２４０頁参照），より具体的には後述の試験例における「固形乳の空隙率測定」により測定される値を意味する。 In the present specification, “porosity” means the ratio of the volume occupied by voids in the bulk volume of the powder (for example, edited by Koichiro Miyajima “Development of Drugs” (Vol. 15) Yodogawa Shoten Heisei 1 (1989) , Issued, page 240), more specifically, a value measured by “measurement of porosity of solid milk” in a test example described later.
本明細書において「粉乳」とは，乳脂肪及び植脂などの脂溶性成分と；水，糖類，たん白質（ペプチドやアミノ酸も含む）及びミネラルなどの水溶性成分とを，混合したものを乾燥して粉末状にした調製乳などを意味する。また，粉乳の例として，全脂粉乳，調製粉乳，及びクリーミーパウダーなどがあげられる。 In this specification, “milk powder” means a mixture of fat-soluble components such as milk fat and fat, and water-soluble components such as water, sugars, proteins (including peptides and amino acids) and minerals. It means a milk powder or the like. Examples of powdered milk include whole milk powder, prepared milk powder, and creamy powder.
本明細書において「固形乳」とは，常温にて固形状態に調製した乳類を意味する。固形乳は，より具体的には，粉乳を所定の大きさ，重量に成形したものであり，水に溶かすと，粉乳を水に溶かしたものと同様なものになるものを意味する。 In the present specification, “solid milk” means milk prepared in a solid state at room temperature. More specifically, solid milk means powdered milk formed into a predetermined size and weight, and when it is dissolved in water, it means the same as that of powdered milk dissolved in water.
本明細書において「組成が均一」とは，固形乳の全ての部位において，その組成が実質的に同様であることを意味する。なお，固形化や溶解性の付与を目的としていない成分を添加・混合してから圧縮成型する場合なども「組成が均一」であるとする。ただし、例えば，特許文献３，又は特許文献４のように，粒径の大きな糖類などを核として、粒径の小さい粉乳を付着させた状態は，ここでいう「組成が均一」とはいえない。ただし，固形乳を製造した後，表面にコ−ティング層を設けた場合は，そのコ−ティング層の内部が固形乳であり，その固形乳の「組成が均一」といえる。 As used herein, “uniform composition” means that the composition is substantially the same in all parts of the solid milk. It should be noted that “composition is uniform” also when compression molding is performed after adding and mixing components not intended for solidification or solubility. However, for example, as in Patent Document 3 or Patent Document 4, a state in which powdered milk with a small particle size is adhered using a saccharide with a large particle size as a core is not said to be “uniform in composition” here. . However, when a coating layer is provided on the surface after producing solid milk, the inside of the coating layer is solid milk, and it can be said that the composition of the solid milk is “uniform”.
本明細書において「添加剤」とは，結合剤，崩壊剤，滑沢剤及び膨張剤などの栄養成分以外の剤を意味する。 In the present specification, the “additive” means an agent other than a nutrient component such as a binder, a disintegrant, a lubricant, and a swelling agent.
本明細書において「添加剤を実質的に添加しない」とは，原料として基本的に粉乳のみを用いることを意味し，添加剤が固形乳の栄養成分に影響を与えない量，例えば０．５重量％以下（好ましくは，０．１重量％以下）である場合を意味する。なお，本発明において，原料として粉乳のみを用い，粉乳以外の添加剤を用いないことが好ましい。 In the present specification, “substantially no additive” means that only powdered milk is basically used as a raw material, and the amount of additive that does not affect the nutritional components of solid milk, for example 0.5 It means a case where it is not more than wt% (preferably, not more than 0.1 wt%). In addition, in this invention, it is preferable to use only powdered milk as a raw material and not to use additives other than powdered milk.
１．固形乳
本発明の固形乳は，空隙率が３０％〜５０％の固形乳である。空隙率が大きいほど，溶解性が高くなるが，強度が弱くなる。また，空隙率が小さいと，溶解性が低くなる。この空隙率は，おもに圧縮工程の圧縮力によって制御される。なお，本発明において，好ましい空隙率は，３５％〜５０％であるが，空隙率をその用途などに応じて調整し３０％〜３５％，３０％〜４５％，４０％〜４５％，又は４０％〜５０％としてもよい。これらのような空隙率の範囲となるように調整すれば，後述のとおり，オイルオフなどの問題を解決した良好な固形乳を得ることができる。
1. Solid milk The solid milk of the present invention is a solid milk having a porosity of 30% to 50%. The higher the porosity, the higher the solubility but the lower the strength. In addition, when the porosity is small, the solubility becomes low. This porosity is mainly controlled by the compression force of the compression process. In the present invention, the preferable porosity is 35% to 50%, but the porosity is adjusted according to the application and the like, and 30% to 35%, 30% to 45%, 40% to 45%, or It may be 40% to 50%. If adjusted so that the porosity is within such a range, as described later, it is possible to obtain a good solid milk that solves problems such as oil-off.
それぞれの空隙は，固形乳に複数存在することが好ましい。各空隙（孔）は、好ましくは均一に分散している。空隙が固形乳でほぼ一様に分布するので，より高い溶解性を得ることができる。空隙が大きいほど水の侵入が容易であり速溶解性を得ることができる。一方，空隙の大きさが大きすぎると強度が弱くなるか，又は固形乳の表面が粗くなる。そこで，空隙の大きさは，１０μm〜５００μmがあげられ，好ましくは５０μm〜３００μmである。この空隙の大きさは，公知の手段，例えば固形乳の表面及び断面を走査型電子顕微鏡を用いて観察することにより測定できる。 It is preferable that a plurality of each void exist in the solid milk. Each void (hole) is preferably uniformly dispersed. Since the voids are distributed almost uniformly in the solid milk, higher solubility can be obtained. The larger the gap, the easier the water can penetrate and the faster solubility can be obtained. On the other hand, if the size of the gap is too large, the strength becomes weak or the surface of the solid milk becomes rough. Therefore, the size of the gap is 10 μm to 500 μm, preferably 50 μm to 300 μm. The size of the void can be measured by a known means, for example, by observing the surface and cross section of the solid milk using a scanning electron microscope.
固形乳の成分は，水分量を除く他，基本的には原料となる粉乳の成分と同様である。固形乳の成分として，脂肪，糖質，たん白質，ミネラル，及び水分があげられる。固形乳の脂肪含有率は，例えば５重量％〜７０重量％があげられ，好ましくは５重量％〜５０重量％であり，より好ましくは１０重量％〜４５重量％である。本発明の固形乳は，脂肪として，乳化した脂肪と遊離脂肪とを含んでいてもよい。すなわち，従来の粉乳や固形乳においては，遊離脂肪が風味を損ねる・温水に溶解した際に水に浮く（オイルオフ）などの問題があり積極的に排除されてきた。本発明の固形乳は，好ましくはこの遊離脂肪を積極的に含有する。そして，この遊離脂肪を，滑沢剤などの代わりに有効活用する。これにより，本発明は添加剤を用いなくても良好な固形乳を製造できる。ただし，遊離脂肪が多すぎるとオイルオフの問題が生ずる。そこで，本発明の固形乳において遊離脂肪の含有率は，０．５重量％〜４重量％があげられ，好ましくは０．７重量％〜３重量％であり，より好ましくは１重量％〜２．５重量％である。これらの範囲であれば，後述の実施例において示されるとおり，好適な硬度，溶解性，及び過度なオイルオフを抑制できるからである。なお，オイルオフが問題となる遊離脂肪の量は，原料として用いる粉乳中の脂肪組成，及び脂肪球径などの物性により異なるので，固形乳に含まれる遊離脂肪の量は，上記の範囲内で適宜修正すればよい。 The components of the solid milk are basically the same as the components of the powdered milk used as a raw material except for the water content. Components of solid milk include fats, sugars, proteins, minerals, and moisture. The fat content of the solid milk is, for example, 5% to 70% by weight, preferably 5% to 50% by weight, and more preferably 10% to 45% by weight. The solid milk of the present invention may contain emulsified fat and free fat as fat. In other words, conventional powdered milk and solid milk have been actively eliminated due to problems such as the loss of flavor of free fat and floating in water (oil off) when dissolved in warm water. The solid milk of the present invention preferably positively contains this free fat. And this free fat is used effectively instead of lubricants. Thereby, this invention can manufacture favorable solid milk, without using an additive. However, if there is too much free fat, the problem of oil-off occurs. Therefore, the content of free fat in the solid milk of the present invention is 0.5 wt% to 4 wt%, preferably 0.7 wt% to 3 wt%, more preferably 1 wt% to 2 wt%. .5% by weight. This is because, within these ranges, suitable hardness, solubility, and excessive oil-off can be suppressed as shown in the examples described later. Note that the amount of free fat for which oil-off is a problem varies depending on the fat composition in the milk powder used as a raw material and physical properties such as the diameter of the fat globules. Therefore, the amount of free fat contained in the solid milk is within the above range. What is necessary is just to correct suitably.
固形乳に含まれる水分が多いと保存性が悪くなり，水分が少ないともろくなる。したがって，固形乳の水分含有率として，１重量％〜４重量％があげられ，好ましくは２重量％〜３．５重量％である。 When there is a lot of water in the solid milk, the shelf life is poor, and it becomes brittle even if the water is low. Accordingly, the water content of the solid milk is 1% to 4% by weight, preferably 2% to 3.5% by weight.
本発明の固形乳の形状は，ある程度の大きさをもつものであれば，特に限定されない。固形乳の形状として，円柱状，楕円柱状，立方体状，直方体状，板状，球状，多角柱状，多角錐状，多角錐台状，及び多面体状のものがあげられ，持ち運びの便利さなどの観点から円柱状又は四角柱状が好ましい。なお，固形乳が壊れる事態を防止するため，角部分に面取りが施されている固形乳が好ましい。 The shape of the solid milk of the present invention is not particularly limited as long as it has a certain size. Solid milk shapes include cylinders, elliptical cylinders, cubes, rectangular parallelepipeds, plates, spheres, polygonal cylinders, polygonal pyramids, polygonal frustums, and polyhedrons. From the viewpoint, a cylindrical shape or a quadrangular prism shape is preferable. In addition, in order to prevent the situation where solid milk is broken, solid milk with chamfered corners is preferable.
本発明の固形乳は，１個〜数個の固形乳（好ましくは１個の固形乳）を温水に溶解すれば，飲用する際の１回分の乳となるものが好ましい。したがって，固形乳の体積は，１ｃｍ３〜５０ｃｍ３があげられ，好ましくは２ｃｍ３〜３０ｃｍ３であり，より好ましくは４ｃｍ３〜２０ｃｍ３である。 The solid milk of the present invention is preferably one that can be used as a one-time milk for drinking if 1 to several solid milks (preferably one solid milk) are dissolved in warm water. Accordingly, the volume of the solid milk is, 1 cm 3 to 50 cm 3 and the like, preferably 2cm 3 ~30cm 3, more preferably 4 cm 3 to 20 cm 3.
本発明の固形乳は，ある程度の溶解性を持っている必要がある。本発明の固形乳は，後述の溶解性測定条件で，１８０秒以下の溶解性のものがあげられ，好ましくは１２０秒以下であり，より好ましくは６０秒以下である。ただし，時間が短すぎると，均一な液体が得られないため，５秒以上の溶解性のものが好ましい。 The solid milk of the present invention needs to have a certain degree of solubility. The solid milk of the present invention includes those having a solubility of 180 seconds or less under the solubility measurement conditions described below, preferably 120 seconds or less, more preferably 60 seconds or less. However, if the time is too short, a uniform liquid cannot be obtained.
本発明の固形乳は，運搬する際に壊れる事態を極力さけるため，ある程度の強度を持つ必要がある。本発明の固形乳は，後述の錠剤硬度測定条件で，３０Ｎ以上の硬度を有するものが好ましい。一方，溶解性の観点から，３００Ｎ以下の硬度のものが好ましい。 The solid milk of the present invention needs to have a certain degree of strength in order to avoid the situation where it breaks during transportation. The solid milk of the present invention preferably has a hardness of 30 N or more under the tablet hardness measurement conditions described below. On the other hand, from the viewpoint of solubility, those having a hardness of 300 N or less are preferred.
２．製造工程
本発明の固形乳の製造方法は，粉乳を圧縮し固形状の粉乳圧縮物を得るための圧縮工程と，圧縮工程で得られた粉乳圧縮物を湿らせるための加湿工程と，加湿工程で加湿された粉乳圧縮物を乾燥させるための乾燥工程とを含む。
2. Production process The method for producing solid milk of the present invention comprises a compression process for compressing powdered milk to obtain a solid milk powder compressed product, a humidifying process for moistening the compressed milk powder product obtained in the compression process, and a humidification process. And a drying step for drying the compressed milk powder that has been humidified in step (b).
２．１．圧縮工程
圧縮工程は，粉乳を圧縮し固形状の粉乳圧縮物を得るための工程である。圧縮工程では，粉乳を次工程へ移行できる程度の比較的低い圧力で粉乳を打錠することにより，水が侵入するための空隙を確保した粉乳圧縮物を得る。圧縮工程では，適切な空隙を設けた保形性のある粉乳圧縮物を製造するという要件を満たすように粉乳を圧縮する。すなわち，この圧縮工程での空隙率が，固形乳の空隙率と密接に関連する。また，粉乳圧縮物の潤滑性が乏しければ，打錠機などの装置に粉乳圧縮物の一部が付着するという打錠障害の問題を生ずる。さらに，粉乳圧縮物の保形性が悪ければ，固形乳を製造する過程において，形状を保てないものができるという問題を生ずる。
2.1. Compression process The compression process is a process for compressing powdered milk to obtain a solid powdered milk compressed product. In the compression step, the compressed milk powder is compressed with a relatively low pressure so that the milk powder can be transferred to the next step, thereby obtaining a compressed milk powder that has a space for water to enter. In the compression step, the powdered milk is compressed so as to satisfy the requirement of producing a compressed milk powder having shape retention with an appropriate gap. That is, the porosity in this compression process is closely related to the porosity of solid milk. In addition, if the compressed milk powder is poor, a problem of tableting trouble that a part of the compressed milk powder adheres to a device such as a tableting machine is caused. Furthermore, if the compressed form of the compressed milk powder is poor, there is a problem that in the process of producing the solid milk, a product that cannot keep the shape is produced.
圧縮工程における原料として，好ましくは粉乳のみを用い，添加剤を実質的に添加しない。粉乳は，市販のものを購入しても良いし，公知の製造方法（例えば，特開平１０−２６２５５３号公報，特開平１１−１７８５０６号公報，特開２０００−４１５７６号公報，特開２００１−１２８６１５号公報，特開２００３−１８０２４４号公報及び特開２００３−２４５０３９号公報に記載の製造方法など）により製造したものを用いても良い。粉乳の組成は，上記の固形乳と同様のものがあげられる。なお，圧縮工程の原料に，脂肪を添加しても良い。ただし，脂肪を添加すると，この脂肪はオイルオフのもととなる。そして，添加された脂肪は，粉乳の表面に付着するので，臼への充填精度が下がることとなる。したがって，圧縮工程において，好ましくは目標となる遊離脂肪量を含むように製造した粉乳を用いる。 Preferably, only milk powder is used as a raw material in the compression step, and no additive is substantially added. Powdered milk may be purchased commercially, or a known production method (for example, JP-A-10-262553, JP-A-11-178506, JP-A-2000-41576, JP-A-2001-128615). The manufacturing method described in Japanese Patent Laid-Open No. 2003-180244 and Japanese Patent Laid-Open No. 2003-245039, etc.) may be used. The composition of the milk powder is the same as that of the above solid milk. In addition, you may add fat to the raw material of a compression process. However, when fat is added, this fat becomes the source of oil-off. And since the added fat adheres to the surface of the milk powder, the filling accuracy into the die is lowered. Therefore, in the compression step, preferably milk powder produced so as to contain the target free fat content is used.
粉乳の脂肪含有率が大きい場合は，圧縮力が小さくてすむ。一方，粉乳の脂肪含有率が小さい場合は，圧縮力を大きくしなければならない。よって，脂肪含有率が大きい粉乳を用いるほど，適切な空隙を設ける，保形性のある粉乳圧縮物を製造するという要件を満たすことができる。このような観点から，粉乳の脂肪含有率は，例えば５重量％〜７０重量％があげられ，好ましくは５重量％〜５０重量％であり，より好ましくは１０重量％〜４５重量％である。 If the fat content of the milk powder is high, the compression force is small. On the other hand, if the fat content of milk powder is small, the compression force must be increased. Therefore, the requirement that a milk powder compressed product having a shape-retaining property can be satisfied as the powdered milk having a higher fat content is used. From such a viewpoint, the fat content of the milk powder is, for example, 5% to 70% by weight, preferably 5% to 50% by weight, and more preferably 10% to 45% by weight.
粉乳は，上記のとおり遊離脂肪を含んでいるものが好ましい。本発明では，この遊離脂肪を，滑沢剤などの代わりに有効活用する。これにより，本発明は添加剤を添加しなくても良好な固形乳を製造できる。本発明の固形乳において遊離脂肪の含有率は，０．５重量％〜３重量％があげられ，好ましくは０．７重量％〜２．４重量％であり，より好ましくは１重量％〜２重量％である。 The milk powder preferably contains free fat as described above. In the present invention, this free fat is effectively used instead of a lubricant. Thereby, this invention can manufacture favorable solid milk, without adding an additive. In the solid milk of the present invention, the content of free fat is 0.5 to 3% by weight, preferably 0.7 to 2.4% by weight, more preferably 1 to 2%. % By weight.
粉乳に含まれる水分が多いと保存性が悪くなり，水分が少ないともろくなる（保形性が悪くなる）。したがって，粉乳の水分含有率として，１重量％〜４重量％があげられ，好ましくは２重量％〜３．５重量％である。 If the powdered milk contains a lot of water, the preservability will be poor, and if the water content is low, it will become brittle (shape retention will be poor). Therefore, the water content of the powdered milk is 1% to 4% by weight, preferably 2% to 3.5% by weight.
圧縮工程では，粉乳を圧縮し固形状の粉乳圧縮物を得るための圧縮手段により粉乳圧縮物を製造する。圧縮手段は，粉乳を圧縮し固形状の粉乳圧縮物を得ることができるものであれば特に限定されない。圧縮手段として，公知の打錠機，圧縮試験装置などの加圧成形機があげられ，好ましくは打錠機である。なお，打錠機として，例えば，特公昭３３−９２３７号公報，特開昭５３−５９０６６号公報，特開平６−２１８０２８号公報，特開２０００−９５６７４号公報，及び特許第２６５０４９３号公報に記載のものがあげられる。 In the compression step, the compressed milk powder is produced by a compression means for compressing the powdered milk to obtain a solid milk powder compressed product. The compressing means is not particularly limited as long as it can compress milk powder to obtain a solid milk powder compressed product. Examples of the compression means include a known tableting machine and a pressure molding machine such as a compression tester, and a tableting machine is preferred. Examples of the tableting machine are described in, for example, Japanese Patent Publication No. 33-9237, Japanese Patent Publication No. 53-59066, Japanese Patent Publication No. 6-218028, Japanese Patent Publication No. 2000-95674, and Japanese Patent No. 2650493. Things.
なお，打錠機を用いて粉状物を圧縮する場合，粉状物を臼に入れ，杵を打ち付けることにより粉状物に圧縮力を付加し，固形状とする。なお，この際に粉状物が，潤滑性に乏しければ，杵の表面に粉状物が付着する事態が生ずる。これは，製品の品質を悪くするだけではなく，杵の表面を清掃しなければならなくなり，歩留まりが低下する。そこで，滑沢剤を添加することが，特に医薬を製造する際に行われている。しかし，滑沢剤は，水に溶けにくいワックスである。したがって，固形乳のように，温水に溶かした状態で飲用するものについては，滑沢剤を添加することは望ましくない。これは，固形乳を製造困難にさせていた理由のひとつである。本発明は，上記のとおり，これまでできるだけ発生させないことが望ましいとされていた遊離脂肪を滑沢剤として適量用い，これにより粉乳が杵に付着する事態を防止したものである。さらには，上記のとおり，適切な空隙率をもつ粉乳圧縮物を得ることで，溶解しやすく，保形性に優れた固形乳を得ることができたものである。また，崩壊剤を添加すると沈殿物が生ずるなどの事態が起きるが，本発明の固形乳の製造方法では，崩壊剤が不要であるので，このような事態を有効に回避できる。 In addition, when compressing a powdery substance using a tableting machine, the compressive force is applied to the powdery substance by placing the powdery substance in a mortar and hitting a punch to make it a solid form. At this time, if the powder is poor in lubricity, the powder may adhere to the surface of the basket. This not only deteriorates the quality of the product, but also requires cleaning the surface of the bag, which reduces the yield. Therefore, the addition of a lubricant is performed particularly when producing a medicine. However, lubricants are waxes that are difficult to dissolve in water. Therefore, it is not desirable to add a lubricant to those that are drunk in warm water, such as solid milk. This is one of the reasons that made solid milk difficult to manufacture. As described above, the present invention uses an appropriate amount of free fat, which has been desired to be generated as little as possible, as a lubricant, thereby preventing powdered milk from adhering to the straw. Furthermore, as described above, by obtaining a compressed milk powder having an appropriate porosity, it was possible to obtain solid milk that was easily dissolved and excellent in shape retention. In addition, when a disintegrant is added, a situation such as precipitation occurs, but in the method for producing solid milk of the present invention, such a situation can be effectively avoided because a disintegrant is unnecessary.
圧縮工程における環境温度は，特に限定されず室温にて行うことができる。より具体的には，圧縮工程における環境温度として，１０℃〜３０℃があげられる。圧縮工程における湿度は，例えば３０％ＲＨ〜５０％ＲＨがあげられる。圧縮工程において好ましくは，粉乳の圧縮作業を連続的に行う。 The environmental temperature in the compression step is not particularly limited and can be performed at room temperature. More specifically, the environmental temperature in the compression process is 10 ° C to 30 ° C. The humidity in the compression process is, for example, 30% RH to 50% RH. In the compression step, the milk powder compression operation is preferably performed continuously.
２．２．加湿工程
加湿工程は，圧縮工程で得られた粉乳圧縮物を湿らせるための工程である。粉乳圧縮物を湿らせることにより，粉乳圧縮物の表面近傍の粒子が一部溶解し，架橋する。これにより，粉乳圧縮物の表面近傍の強度が増大することとなる。
2.2. Humidification process The humidification process is a process for moistening the compressed milk powder obtained in the compression process. By moistening the compressed milk powder, some particles near the surface of the compressed milk powder are dissolved and crosslinked. As a result, the strength in the vicinity of the surface of the compressed milk powder is increased.
加湿工程では，粉乳圧縮物を湿らせるための加湿手段により粉乳圧縮物を湿らせることができる。加湿手段として，高湿度室，スプレー，及びスチームなど公知の加湿手段があげられる。また，加湿方法として，高湿度環境下に置く方法，スプレーにより水を噴霧する方法，蒸気を吹き付ける方法など公知の加湿方法を採用できる。なお，高湿度環境における湿度として，例えば６０％ＲＨ〜１００％ＲＨがあげられ，好ましくは８０％ＲＨ〜１００％ＲＨであり，より好ましくは９０％ＲＨ〜１００％ＲＨである。また，高湿度環境下に置く時間として，例えば５秒〜１時間があげられ，好ましくは１０秒〜２０分であり，より好ましくは１５秒〜１５分である。高湿度環境下に置く方法における温度として，たとえば３０℃〜１００℃があげられ，好ましくは４０℃〜８０℃である。 In the humidification step, the compressed milk powder can be moistened by a humidifying means for moistening the compressed milk powder. Examples of the humidifying means include known humidifying means such as a high humidity chamber, spray, and steam. Further, as a humidifying method, a known humidifying method such as a method of placing in a high humidity environment, a method of spraying water with a spray, a method of spraying steam, or the like can be employed. The humidity in the high humidity environment is, for example, 60% RH to 100% RH, preferably 80% RH to 100% RH, and more preferably 90% RH to 100% RH. Further, the time for placing in a high humidity environment is, for example, 5 seconds to 1 hour, preferably 10 seconds to 20 minutes, and more preferably 15 seconds to 15 minutes. Examples of the temperature in the method of placing in a high humidity environment include 30 ° C. to 100 ° C., preferably 40 ° C. to 80 ° C.
加湿工程で，粉乳圧縮物に加えられる水分の量（以下，「加湿量」ともいう。）は，適宜調整すればよい。しかし，本発明では，基本的には，原料として粉乳のみを用いているので，後述の実施例（実施例５）及び図３により示されるとおり，加湿量として，以下の範囲が望ましい。すなわち，加湿量を０．５％とすると，錠剤硬度が増大し，加湿量を１％とすると錠剤硬度が約２倍となる。このように，加湿量が増えるにつれ錠剤硬度も大きくなる傾向にある。一方，加湿量が，２．５％以上で，錠剤硬度の増加は止まった。また，加湿量が３％以上では，粉乳圧縮物が溶解し，変形するものや，移送中に装置に付着するものがでた。そこで，粉乳圧縮物に加えられる水分の量として，粉乳圧縮物の質量の０．５％〜３％が好ましく，１％〜２．５％がより好ましい。 What is necessary is just to adjust suitably the quantity (henceforth the "humidification amount") of the water | moisture content added to a powdered milk compact in a humidification process. However, in the present invention, basically only powdered milk is used as a raw material, so that the following range is desirable as the humidification amount as shown in Examples (Example 5) and FIG. That is, when the humidification amount is 0.5%, the tablet hardness is increased, and when the humidification amount is 1%, the tablet hardness is approximately doubled. Thus, the tablet hardness tends to increase as the amount of humidification increases. On the other hand, the increase in tablet hardness stopped when the humidification amount was 2.5% or more. In addition, when the amount of humidification was 3% or more, the compressed powdered milk was dissolved and deformed, or it adhered to the device during transfer. Therefore, the amount of water added to the compressed milk powder is preferably 0.5% to 3%, more preferably 1% to 2.5% of the mass of the compressed milk powder.
２．３．乾燥工程
乾燥工程は，加湿工程で加湿された粉乳圧縮物を乾燥させるための工程である。乾燥工程により，加湿工程で加湿された粉乳圧縮物が乾燥するので，表面タック（べとつき）がなくなり，固形乳を製品として扱うことができるようになる。乾燥工程における乾燥方法として，加湿工程で加湿された粉乳圧縮物を乾燥させることができる公知の方法を採用でき，例えば，低湿度・高温度条件下に置く方法，乾燥空気・高温乾燥空気を接触させる方法などがあげられる。
2.3. Drying process The drying process is a process for drying the compressed milk powder that has been humidified in the humidification process. By the drying process, the powdered milk compressed in the humidification process is dried, so that there is no surface tack (stickiness) and solid milk can be handled as a product. As a drying method in the drying step, a known method that can dry the compressed milk powder compressed in the humidification step can be adopted, for example, a method of placing the product in a low humidity / high temperature condition, contact with dry air / high temperature dry air The method of making it.
低湿度・高温度条件下に置く方法おける「湿度」として，０％ＲＨ〜３０％ＲＨがあげられ，好ましくは０％ＲＨ〜２５％ＲＨであり，より好ましくは０％ＲＨ〜２０％ＲＨである。このように，湿度はできるだけ低く設定することが好ましい。低湿度・高温度条件下に置く方法おける「温度」として，２０℃〜１５０℃があげられ，好ましくは３０℃〜１００℃であり，より好ましくは４０℃〜８０℃である。低湿度・高温度条件下に置く方法おける「乾燥時間」として，０．２分〜２時間があげられ，好ましくは０．５分〜１時間であり，より好ましくは１分〜３０分である。 “Humidity” in the method of placing under low humidity and high temperature conditions includes 0% RH to 30% RH, preferably 0% RH to 25% RH, more preferably 0% RH to 20% RH. is there. Thus, it is preferable to set the humidity as low as possible. “Temperature” in the method of placing under low humidity and high temperature conditions is 20 ° C. to 150 ° C., preferably 30 ° C. to 100 ° C., more preferably 40 ° C. to 80 ° C. “Drying time” in the method of placing under low humidity and high temperature is 0.2 minutes to 2 hours, preferably 0.5 minutes to 1 hour, more preferably 1 minute to 30 minutes. .
先に説明したとおり，固形乳に含まれる水分が多いと保存性が悪くなり，水分が少ないともろくなる。したがって，乾燥工程においては，乾燥温度や乾燥時間などの条件を制御することによって，固形乳の水分含有率を原料として用いる粉乳の水分含有率の前後１％以内（好ましくは前後０．５％以内）に制御することが好ましい。 As explained above, when the water content in the solid milk is large, the storage stability is deteriorated and the water content is fragile. Therefore, in the drying process, by controlling conditions such as drying temperature and drying time, the moisture content of solid milk is within 1% before and after the moisture content of milk powder used as a raw material (preferably within 0.5% before and after) ) Is preferably controlled.
３．粉乳及び固形乳の製造方法
本発明の粉乳及び固形乳の製造方法は，粉乳を製造する工程と，その粉乳を原料として固形乳を製造する工程とを含む。なお，粉乳を製造する工程で製造された粉乳の一部を，そのまま粉乳として容器に充填し，製品としても良い。このようにすることにより，粉乳及び固形乳を得ることができる。
3. The manufacturing method of milk powder and solid milk The manufacturing method of milk powder and solid milk of this invention includes the process of manufacturing powdered milk, and the process of manufacturing solid milk from the powdered milk as a raw material. A part of the milk powder produced in the process of producing the milk powder may be directly filled into a container as a milk powder to produce a product. By doing in this way, milk powder and solid milk can be obtained.
３．１．粉乳の製造方法
粉乳の製造工程は全粉乳、脱脂粉乳、育児用粉乳に代表される調製粉乳など製品の種類によって詳細は異なる。しかし，基本的には，「原料（調整）→清澄化→殺菌→濃縮→（均質化）→噴霧乾燥→篩過→充填」の工程により，粉乳を製造できる。なお，噴霧乾燥後の粉乳の大きさは，５μm〜１５０μm程度であり，粉乳の造粒物の大きさは，１００μm〜５００μm程度である。また，粉乳とその造粒物とが混ざり合った状態では，その空隙は５μm〜１５０μm程度である。
3.1. Manufacturing method of milk powder The details of the manufacturing process of milk powder vary depending on the type of product such as whole milk powder, skim milk powder, prepared milk powder represented by infant formula. However, basically, milk powder can be produced by the process of “raw material (adjustment) → clarification → sterilization → concentration → (homogenization) → spray drying → sieving → filling”. The size of the milk powder after spray drying is about 5 μm to 150 μm, and the size of the granulated product of the milk powder is about 100 μm to 500 μm. Further, in the state where the milk powder and the granulated product are mixed, the gap is about 5 μm to 150 μm.
粉乳の原料として，乳があげられる。乳として，生乳があげられ，より具体的には，牛（ホルスタイン，ジャ−ジ−種その他），山羊，羊，水牛などの乳があげられる。これらを遠心分離等の方法により，脂肪分の一部を取り除くことにより脂肪含量を調節することができる。また，下記の栄養成分などを添加することもできる。一方，調製粉乳を製造する場合は，水に下記の栄養成分を加え，混合して用いる。 Milk is a raw material for powdered milk. Examples of milk include raw milk, and more specifically, milk from cows (Holstein, jersey, etc.), goats, sheep, and buffalos. The fat content can be adjusted by removing a part of the fat content by a method such as centrifugation. The following nutritional components can also be added. On the other hand, when preparing formula milk, add the following nutritional components to water and mix.
上記の原料液を公知の製造方法である「清澄化」，「殺菌」，「均質化」，「濃縮」，「噴霧乾燥」，「篩過」，及び「充填」の工程で処理することにより粉乳を製造することができる。 By processing the above-mentioned raw material liquid in the steps of “clarification”, “sterilization”, “homogenization”, “concentration”, “spray drying”, “sieving”, and “filling”, which are known production methods. Milk powder can be produced.
粉乳の原料となるたん白質として，カゼイン，乳清たん白質（α−ラクトアルブミン，β−ラクトグロブリンなど），乳清たん白質濃縮物（ＷＰＣ），乳清たん白質分離物（ＷＰＩ）などの乳たん白質及び乳たん白質分画物；卵たん白質などの動物性たん白質；大豆たん白質，小麦たん白質などの植物性たん白質；これらのたん白質を酵素などにより種々の鎖長に分解したペプチド；及びさらにタウリン，シスチン，システィン，アルギニン及びグルタミンなどのアミノ酸；を単独又は混合して用いることができる。 Proteins used as the raw material for powdered milk include casein, whey protein (α-lactalbumin, β-lactoglobulin, etc.), whey protein concentrate (WPC), whey protein isolate (WPI), etc. Protein and milk protein fractions; animal proteins such as egg protein; plant proteins such as soybean protein and wheat protein; peptides obtained by degrading these proteins into various chain lengths using enzymes, etc. And further amino acids such as taurine, cystine, cystine, arginine and glutamine can be used alone or in combination.
粉乳の原料となる油脂として，乳脂肪，ラ−ド，牛脂および魚油などの動物性油脂や大豆油，ナタネ油，コ−ン油，ヤシ油，パ−ム油，パ−ム核油，サフラワ−油，綿実油，アマニ油，ＭＣＴなどの植物性油脂，又は，これらの分別油，水素添加油及びエステル交換油を単独又は混合してできる。 As fats and oils that are used as raw materials for milk powder, animal fats such as milk fat, lard, beef tallow and fish oil, soybean oil, rapeseed oil, corn oil, coconut oil, palm oil, palm kernel oil, safflower -Vegetable oils such as oil, cottonseed oil, linseed oil, MCT, or these fractionated oils, hydrogenated oils and transesterified oils can be used alone or in combination.
粉乳の原料となる糖質として，乳糖，ショ糖，ブドウ糖，麦芽糖やガラクトオリゴ糖，フルクトオリゴ糖，ラクチュロ−スなどのオリゴ糖，デンプン，可溶性多糖類，デキストリンなどの多糖類，また，人工甘味料などを単独又は混合して使用できる。 Sugars used as raw materials for milk powder include lactose, sucrose, glucose, maltose and galactooligosaccharides, fructooligosaccharides, oligosaccharides such as lactulose, starches, soluble polysaccharides, polysaccharides such as dextrin, and artificial sweeteners. Can be used alone or in combination.
その他，水溶性，脂溶性のビタミン類，ミネラル類や香料，矯味料などを粉乳の原料として添加することができる。 In addition, water-soluble and fat-soluble vitamins, minerals, fragrances, flavoring agents and the like can be added as raw materials for milk powder.
３．１．１．清澄化工程
清澄化工程は，遠心分離機またはフィルタ−など公知の手段によって，牛乳などに含まれる微細な異物を除去するための工程である。
3.1.1. Clarification process The clarification process is a process for removing fine foreign substances contained in milk or the like by a known means such as a centrifuge or a filter.
３．１．２．殺菌工程
殺菌工程は，牛乳などに含まれる細菌などの微生物を死滅させるための工程である。殺菌工程での殺菌温度と保持時間は，粉乳の種類によって様々であり，公知の殺菌処理に関する条件を採用できる。
3.1.2. Sterilization process The sterilization process is a process for killing microorganisms such as bacteria contained in milk. The sterilization temperature and holding time in the sterilization process vary depending on the type of milk powder, and known conditions relating to sterilization can be employed.
３．１．３．濃縮工程
濃縮工程は，後述の噴霧乾燥工程の前に牛乳などを予備的に濃縮するための任意の工程であり，真空蒸発缶など公知の手段と条件を採用できる。
3.1.3. Concentration step The concentration step is an optional step for preliminarily concentrating milk or the like before the spray drying step described below, and can employ known means and conditions such as a vacuum evaporator.
３．１．４．均質化工程
均質化工程は，牛乳などに分散している脂肪球などの固形成分を一定以下の大きさに均質化するための任意の工程であり，処理液に高圧を加えて狭い間隙を通過させるなど公知の手段と条件を採用できる。
3.1.4. Homogenization process The homogenization process is an optional process for homogenizing solid components such as fat globules dispersed in milk to a certain size or less. Well-known means and conditions can be employed.
３．１．５．噴霧乾燥工程
噴霧乾燥工程は，濃縮乳中の水分を蒸発させて粉体を得るための工程であり，噴霧乾燥機など公知の手段や，公知の条件を採用できる。
3.1.5. Spray drying process The spray drying process is a process for evaporating the water in the concentrated milk to obtain a powder. Known means such as a spray dryer and known conditions can be employed.
３．１．６．篩過工程
篩過工程は，噴霧乾燥工程で得られた粉体を篩に通すことで，固まり粉など粒径が大きなものを除去し，整粒するための工程である。
3.1.6. Sifting process The sieving process is a process for removing particles having a large particle size such as lump powder by passing the powder obtained in the spray drying process through a sieve, and sizing.
３．１．７．充填工程
充填工程は，粉乳を袋や缶などに充填するための工程である。
本発明の粉乳及び固形乳の製造方法では，上記のとおり粉乳を製造した後，上記の固形乳製造方法を採用できる。すなわち，上記の篩過工程を経た粉乳を原料として，上記の圧縮工程を行えばよい。
3.1.7. Filling process The filling process is a process for filling milk powder into bags or cans.
In the manufacturing method of the milk powder and solid milk of this invention, after manufacturing milk powder as mentioned above, said solid milk manufacturing method is employable. That is, the above compression process may be performed using the milk powder that has undergone the above sieving process as a raw material.
４．固形乳の利用方法
本発明の固形乳は，一般的には温水に溶かして，飲用する。より具体的には，蓋のできる容器に，温水を入れた後，本発明の固形乳を必要個数投入する。そして，好ましくは容器を軽く振ることにより固形乳を早く溶かし，適温の状態で飲用する。
以下に，実施例を示し，本発明の特徴を説明するが，本発明はこれらの実施例に限定されるものではない。以下では，まず実施例における各評価項目の評価方法について説明した後に，参考例及び実施例を説明する。
4). Utilization method of solid milk The solid milk of the present invention is generally dissolved in warm water and drunk. More specifically, after warm water is put into a container that can be covered, the required number of solid milks of the present invention are charged. Preferably, the solid milk is dissolved quickly by gently shaking the container and is drunk at an appropriate temperature.
Examples of the present invention will be described below. However, the present invention is not limited to these examples. Below, after explaining the evaluation method of each evaluation item in an Example first, a reference example and an Example are demonstrated.
［試験例１（固形乳の空隙率測定）］
固形乳の空隙率は，次式により求めた。
空隙率（％）＝（１−Ｗ／ＰＶ）×１００
Ｗ：固形物の重量(g)
Ｐ：ベックマン空気式密度計を用いて測定した固形物の密度(ｇ／ｃｍ３)
Ｖ：固形物の直径，厚みをマイクロメ−タ−で測定して算出した体積（ｃｍ３）
[Test Example 1 (Measurement of porosity of solid milk)]
The porosity of the solid milk was determined by the following formula.
Porosity (%) = (1-W / PV) × 100
W: Weight of solid (g)
P: density of solids measured with a Beckman pneumatic densimeter (g / cm 3 )
V: Volume (cm 3 ) calculated by measuring the diameter and thickness of the solid with a micrometer
［試験例２（遊離脂肪の含有率測定）］
遊離脂肪の含有率は，以下のようにして測定した。まず，固形乳をすり潰さないように留意しながらカッタ−で細かくし粉砕した（粉砕工程）。その後，３２メッシュ篩に粉砕された固形乳を通過させた（篩工程）。篩工程を経たものを試料とし，‘Ｄｅｔｅｒｍｉｎａｔｉｏｎ ｏｆ Ｆｒｅｅ Ｆａｔ ｏｎ ｔｈｅ Ｓｕｒｆａｃｅ ｏｆ Ｍｉｌｋ Ｐｏｗｄｅｒ Ｐａｒｔｉｃｌｅｓ’，Ａｎａｌｙｔｉｃａｌ Ｍｅｔｈｏｄ ｆｏｒ Ｄｒｙ Ｍｉｌｋ Ｐｒｏｄｕｃｔｓ，Ａ／Ｓ ＮＩＲＯ ＡＴＯＭＩＺＥＲ(１９７８)に記載された方法にしたがって遊離脂肪の含有率を測定した。なお，この方法によれば，遊離脂肪の含有率は，一定速度，時間の振とうにより四塩化炭素で抽出された脂肪の重量％で示される。
[Test Example 2 (Measurement of free fat content)]
The content of free fat was measured as follows. First, it was pulverized and pulverized with a cutter, taking care not to crush the solid milk (pulverization step). Thereafter, the crushed solid milk was passed through a 32 mesh sieve (sieving step). The sample after passing through the sieving process was determined according to the method of “Determination of Free Fat on the Surface of Milk Powder Particles”, Analytical Method for Dry Milk Products, A / TO NIRA 19 Was measured. According to this method, the content of free fat is expressed as the weight percentage of fat extracted with carbon tetrachloride by shaking at a constant rate and time.
［試験例３（錠剤硬度測定）］
固形乳の錠剤硬度は，藤原製作所製ハ−ドネステスタ−を使用して測定した。すなわち，試料の破断面の面積が最小となる方向に荷重をかけ，破断したときの荷重を測定した。
[Test Example 3 (Tablet hardness measurement)]
The tablet hardness of the solid milk was measured using a hard tester manufactured by Fujiwara Seisakusho. In other words, a load was applied in the direction in which the area of the fracture surface of the sample was minimized, and the load when it broke was measured.
［試験例４（溶解性測定）］
固形乳の溶解性は，以下のようにして測定した。まず，２００ｍｌの蓋付きのガラス容器に水１００ｍｌ入れ５０℃とした。この水に固形乳を１個入れ，直ちに振とうし，固形乳が完全になくなるまでに要した時間を測定した。なお，振とう条件は，１．５往復／s，振幅３０ｃｍとした。
[Test Example 4 (Solubility Measurement)]
The solubility of the solid milk was measured as follows. First, 100 ml of water was put in a 200 ml glass container with a lid, and the temperature was set to 50 ° C. One solid milk was put into this water, shaken immediately, and the time required until the solid milk disappeared was measured. The shaking conditions were 1.5 reciprocations / s and amplitude 30 cm.
［試験例５（浮遊オイル測定）］
浮遊オイル（オイルオフ）は，以下のようにして測定した。まず，１００ｍｌのビーカーに，５０℃の水５０ｍｌを用意した。その水に固形乳１個を入れ，完全に溶かした。２時間静置後に，油滴の有無を目視により判定した。
[Test Example 5 (Floating oil measurement)]
The floating oil (oil-off) was measured as follows. First, 50 ml of 50 ° C. water was prepared in a 100 ml beaker. One solid milk was put into the water and dissolved completely. After standing for 2 hours, the presence or absence of oil droplets was visually determined.
［試験例６（過酸化物価の測定）］
過酸化物価は，以下のようにして測定した。試料に６０〜７０℃の熱湯を加え，よく混合して溶解し乳化液とする。これにノニオン界面活性剤（ポリオキシオクチルフェノ−ルエ−テル）及びトリポリリン酸ナトリウムの水溶液を加え，乳化を破壊した後，遠心分離により油層と水層に分ける。油層をとり，ヨウ素滴定法（日本油脂化学協会，基準油脂分析試験法，過酸化物価（クロロホルム法））を用いて測定する。本法の測定値は，試料にヨウ化カリウムを加えた場合に遊離されるヨウ素を試料１ｋｇに対するミリ当量数で表したものであり，脂質の酸化劣化の指標に用いられる。
[Test Example 6 (Measurement of Peroxide Value)]
The peroxide value was measured as follows. Add hot water of 60-70 ° C to the sample, mix well and dissolve to make an emulsion. A nonionic surfactant (polyoxyoctylphenol ether) and an aqueous solution of sodium tripolyphosphate are added to this to break up the emulsification, and then the oil layer and the aqueous layer are separated by centrifugation. Take an oil layer and measure using the iodometric titration method (Japan Oil Chemistry Association, standard oil analysis test method, peroxide value (chloroform method)). The measured value of this method represents the iodine liberated when potassium iodide is added to the sample in terms of the number of milliequivalents per 1 kg of the sample, and is used as an index of lipid oxidative degradation.
［試験例７（風味試験）］
風味試験は，試料を１４重量％の濃度となるように５０℃の水に溶かし，パネラ−１０名に飲んでもらい，美味しさの観点で１〜７の７段階（４が中央値で普通の味）に点数をつけてもらい，その平均値で評価した。
[Test Example 7 (flavor test)]
In the flavor test, the sample was dissolved in water at 50 ° C. to a concentration of 14% by weight and drinked by 10 panelists. From the viewpoint of deliciousness, 7 levels (4 is a median value) The taste was given a score, and the average value was evaluated.
［参考例１ （粉乳の製造）］
水に脂肪，糖質，たん白質，乳及びミネラル類を加えて混合した液を，均質化，濃縮，噴霧乾燥の工程の順で処理することにより，様々な成分を含む粉乳を製造した。
[Reference Example 1 (Production of milk powder)]
Powdered milk containing various components was produced by processing a liquid obtained by adding fat, sugar, protein, milk and minerals to water and mixing them in the order of homogenization, concentration, and spray drying.
（圧縮力と空隙率，溶解性，硬度の関係）
参考例の製造法により得た粉乳（脂肪２５重量％，糖質５８．３重量％，たん白質１１．７重量％，その他ミネラル，及び水分を含む）を万能試験機オ−トグラフ（島津製作所製）にて圧縮力０．５〜３０ＭＰａ，杵の降下速度１０ｍｍ／ｍｉｎの条件で圧縮成形した。その後，恒温恒湿器（ＴＡＢＡＩ ＥＳＰＥＣ製）に４０℃・９５％ＲＨの条件で５分間放置した。その後，エアーオーブン（ヤマト科学）により，４０℃で３０分間乾燥した。このようにして，直径２５ｍｍ，重量約５gの固形乳を得た。原料に使用した粉乳及びここで得た固形乳を試験例１〜５により評価した。その結果を表１に示す。また，表１のうち，空隙率と溶解時間の関係を図１に示す。表１のうち，圧縮力と遊離脂肪の関係を図２に示す。
(Relationship between compressive force and porosity, solubility, hardness)
All-purpose testing machine autograph (manufactured by Shimadzu Corporation) with milk powder (25% fat, 58.3% sugar, 11.7% protein, other minerals and moisture) obtained by the production method of Reference Example ) Under the conditions of a compression force of 0.5 to 30 MPa and a drip rate of 10 mm / min. Then, it was left to stand for 5 minutes in a thermo-hygrostat (manufactured by Tabai Espec) under the conditions of 40 ° C. and 95% RH. Then, it dried for 30 minutes at 40 degreeC with the air oven (Yamato Science). In this way, solid milk having a diameter of 25 mm and a weight of about 5 g was obtained. The milk powder used for the raw material and the solid milk obtained here were evaluated by Test Examples 1-5. The results are shown in Table 1. In Table 1, the relationship between the porosity and the dissolution time is shown in FIG. Of Table 1, the relationship between compressive force and free fat is shown in FIG.
図１から，空隙率と溶解時間とが相関していることがわかる。また，図１から，空隙率３０％付近で溶解時間が急激に変化することがわかる。溶解して飲用する固形乳の実用的な溶解時間として，１２０秒以内が好ましく，更に６０秒以内が好ましい。空隙率が２５．７％（圧縮力２０ＭＰａ）の固形乳は，溶解するのに２７８秒（約４．６分）を要した。したがって，この固形乳は，実用的ではない。空隙率が３０．１％（圧縮力１５ＭＰａ）の固形乳は，１１０秒で溶解した。また空隙率３１．８％（圧縮力１０ＭＰａ）の固形乳は，５０秒で溶解した。したがって，溶解性の観点からは，空隙率３０％以上，圧縮力１５ＭＰａ以下が好ましいことがわかる。
FIG. 1 shows that the porosity and the dissolution time are correlated. Further, it can be seen from FIG. 1 that the dissolution time changes abruptly around a porosity of 30%. The practical dissolution time of the solid milk to be dissolved and drunk is preferably within 120 seconds, and more preferably within 60 seconds. The solid milk having a porosity of 25.7% (
また，表１から圧縮力が２０ＭＰａを超えると，油滴が水面に観察されオイルオフの問題があることがわかった。オイルオフは，圧縮力１５ＭＰａ以下であれば実用上問題とならないことがわかった。すなわち，オイルオフの観点からも空隙率３０％以上，圧縮力１５ＭＰａ以下が好ましいことがわかる。なお，図２から，圧縮力と発生する遊離脂肪の量とは相関しており，圧縮力を制御することにより遊離脂肪の量を制御できることがわかる。また，空隙率５０％以上では，加湿・乾燥処理前の圧縮成形物の硬度が低く，次の工程への移行が困難であった。 Also, from Table 1, it was found that when the compressive force exceeded 20 MPa, oil droplets were observed on the water surface and there was a problem of oil off. It turned out that oil-off does not become a problem practically if the compression force is 15 MPa or less. That is, it can be seen that a porosity of 30% or more and a compressive force of 15 MPa or less are preferable from the viewpoint of oil-off. FIG. 2 shows that the compression force and the amount of free fat generated are correlated, and the amount of free fat can be controlled by controlling the compression force. When the porosity was 50% or more, the hardness of the compression molded product before the humidification / drying treatment was low, and it was difficult to shift to the next step.
圧縮成形物も加湿，乾燥工程により，錠剤硬度は増大した。流通，利用者での取扱に必要な錠剤硬度は３０Ｎ程度であり，圧縮力１ＭＰａで成形し，加湿，乾燥処理することで達成された。 The compression hardness of the compression molded product also increased due to the humidification and drying process. The tablet hardness required for distribution and handling by users is about 30 N, and it was achieved by molding with a compressive force of 1 MPa, humidifying and drying.
溶解性，加湿・乾燥前後の錠剤硬度及びオイルオフの評価項目において，空隙率３０〜５０％，圧縮力１〜１５ＭＰａの圧縮条件が適していることがわかる。 It can be seen that compression conditions with a porosity of 30 to 50% and a compression force of 1 to 15 MPa are suitable for the evaluation items of solubility, tablet hardness before and after humidification and drying, and oil-off.
（脂肪含量の異なる，粉末，顆粒の粉乳使用）
脂肪含量５〜４０％の粉乳を，圧縮力５ＭＰａで成形した他は，実施例１と同じ工程，条件により直径２５ｍｍ，重量約５gの固形乳を得た。これらを試験例１〜５により評価した。この結果を表２に示す。なお，オイルオフの評価項目は，実施例１と同様である。
(Use of powdered and granular milk powder with different fat content)
Solid milk having a diameter of 25 mm and a weight of about 5 g was obtained by the same process and conditions as in Example 1 except that milk powder having a fat content of 5 to 40% was molded at a compression force of 5 MPa. These were evaluated by Test Examples 1-5. The results are shown in Table 2. The oil off evaluation items are the same as in Example 1.
脂肪含量５％の粉乳を用いたものは，加湿・乾燥処理前の圧縮成形物（遊離脂肪０．１１％）の硬度は著しく低く，次工程への移行が困難であった。脂肪含量１０％以上の粉乳を用いたものは，顆粒化の有無を問わず良好な性能を有した圧縮成形物が得られた。 In the case of using powdered milk having a fat content of 5%, the hardness of the compression-molded product (free fat 0.11%) before humidification / drying treatment was remarkably low, and it was difficult to shift to the next step. When using milk powder having a fat content of 10% or more, a compression molded product having good performance was obtained regardless of granulation.
このように，ある程度の脂肪を含んだ粉乳は，本発明で限定した圧縮力，空隙率，遊離脂肪の量に調整することで，特別な添加剤を加えることなく，硬さと速溶解性の相反する要素を兼ね備えた圧縮成形物を得ることができる。 In this way, milk powder containing a certain amount of fat can be adjusted to the compression force, porosity, and free fat content limited in the present invention, and the contradiction between hardness and fast solubility without adding special additives. Thus, a compression-molded product having the elements to be obtained can be obtained.
（遊離脂肪の効果）
実施例２において，脂肪含量５％の粉乳を用いたものは，加湿・乾燥処理前の圧縮成形物の硬度が著しく低い結果となった。この脂肪５％を含んだ粉乳にバタ−油（Ｃｏｒｍａｎ製）をそれぞれ，（ｉ）０．５重量％，（ｉｉ）１．０重量％，及び(ｉｉｉ)２．０重量％加えてよく混合した後，実施例２に示した条件で圧縮成形することにより，遊離脂肪の硬度増強効果を調べた。その結果を表３に示す。
(Effect of free fat)
In Example 2, those using powdered milk with a fat content of 5% resulted in a remarkably low hardness of the compression molded product before the humidification / drying treatment. To this milk powder containing 5% fat, butter oil (manufactured by Corman) was added (i) 0.5% by weight, (ii) 1.0% by weight, and (iii) 2.0% by weight, and mixed well. After that, the effect of enhancing the hardness of free fat was examined by compression molding under the conditions shown in Example 2. The results are shown in Table 3.
バタ−油を加えた直後に圧縮成形したものは，何れも硬度が著しく低いが，２日経過した後に圧縮成形したものは約７Ｎの硬度が得られた。バタ−油を添加していないものは放置時間に関係なく硬度が著しく低い結果となった。これらの圧縮成形物の空隙率に大きな差がないことから，油脂の添加が保形性の増強に働いたことがわかる。 Any of those compression-molded immediately after adding butter oil had a remarkably low hardness, but those compression-molded after 2 days had a hardness of about 7N. In the case where no butter oil was added, the hardness was remarkably low regardless of the standing time. Since there is no significant difference in the porosity of these compression-molded products, it can be seen that the addition of fats and oils has increased the shape retention.
上記の結果から，単に脂肪を添加すれば硬度増大に寄与するのではなく，時間の経過とともに粉乳粒子の表面から内部に入り込んだ状態で存在する脂肪が硬度増強に働くものと推測される。なお，室温で液体であるバタ−油の替わりに，室温でロウ状の固体脂（パ−ム硬化油，融点５８℃，太陽油脂製）を添加したものでは硬度増大の効果は得られなかった。 From the above results, it is presumed that if fat is simply added, it does not contribute to the increase in hardness, but the fat existing in the state of entering from the surface of the milk powder particles with time elapses works to increase the hardness. In addition, the effect of increasing the hardness was not obtained by adding wax-like solid fat (palm hardened oil, melting point 58 ° C., manufactured by Taiyo Oil) at room temperature instead of butter oil which is liquid at room temperature. .
一般的に固体脂（ワックス）は，圧縮成形時の摩擦を低減する滑沢作用を有していることが知られており，この目的で広く使用されている。しかし，本発明のように空隙を確保するために低圧力での圧縮成形が要求される場合，滑沢・潤滑の付与と保形性増強の両方の作用を有するものが有用である。これには室温で液体の脂肪の添加が有効であるが，添加する工程が増えること及び液体の脂肪を添加した粉は流動性が低下し，臼への充填精度が低くなることから，元々粉乳が有している脂肪を圧縮成形の際に必要な量だけ乳化物から遊離させることは極めて合理的な方法である。 Solid fats (waxes) are generally known to have a lubrication action that reduces friction during compression molding, and are widely used for this purpose. However, when compression molding at a low pressure is required to secure the air gap as in the present invention, it is useful to have both functions of providing lubrication and lubrication and enhancing shape retention. The addition of liquid fat at room temperature is effective for this, but the powder added with liquid fat is reduced in fluidity and the accuracy of filling into the mortar is reduced. It is a very reasonable method to release the fat contained in the emulsion from the emulsion in an amount necessary for compression molding.
（生産性の確認）
参考例の製造法により得た粉乳（脂肪２５％，糖質５８．３％，たん白質１１．７％，その他ミネラル，水分）を単発式打錠機（岡田精工製）にて圧縮力５ＭＰａ，２０個／ｍｉｎ（１２００個／ｈ）の条件で１時間連続して圧縮成形した。その後，恒温恒湿器（ＴＡＢＡＩ ＥＳＰＥＣ製）に４０℃・９５％ＲＨの条件で５分間放置し，エアーオーブン（ヤマト科学）にて４０℃で３０分間乾燥することにより直径２５ｍｍ，重量約４．２gの固形乳を得た。
(Productivity check)
Milk powder (fat 25%, sugar 58.3%, protein 11.7%, other minerals, moisture) obtained by the production method of the reference example was compressed with a single-type tableting machine (manufactured by Okada Seiko Co., Ltd.), Compression molding was continuously performed for 1 hour under the condition of 20 pieces / min (1200 pieces / h). After that, it is left in a thermo-hygrostat (TABAI ESPEC) for 5 minutes under conditions of 40 ° C. and 95% RH, and dried in an air oven (Yamato Scientific) for 30 minutes at 40 ° C., and has a diameter of 25 mm and a weight of about 4. 2 g of solid milk was obtained.
連続打錠１時間で，粉が杵臼に付着して起こる打錠障害は認められなく，運転を中断するようなことはなかった。連続打錠実験の結果を表４に示す。圧縮成形物は１０Ｎの硬度を有しており，加湿工程への移行の際，形が壊れるなどのトラブルはなかった。乾燥工程を得て製造された乳固形物の溶解性は３０秒以内で，９２．５Ｎの充分な錠剤硬度を有していた。また，オイルオフは認めらなく，風味についても原料に使用した粉乳と差がなかった。なお，この乳固形物の空隙率は３６．３％，遊離脂肪は０．５４％であった。 In 1 hour of continuous tableting, there was no tableting failure caused by the powder adhering to the tool and the operation was not interrupted. Table 4 shows the results of the continuous tableting experiment. The compression molded product had a hardness of 10N, and there was no trouble such as breakage of the shape during the transition to the humidification process. The solubility of the milk solids produced by the drying process was within 30 seconds and had a sufficient tablet hardness of 92.5N. Also, no oil-off was observed, and the flavor was not different from the milk powder used as a raw material. This milk solid had a porosity of 36.3% and free fat of 0.54%.
（加湿条件の検討）
粉乳（脂肪２５％，糖質５８．３％，たん白質１１．７％，ミネラル，水分）を万能試験機オ−トグラフ（島津製作所製）にて，圧縮力５ＭＰａ，圧縮速度１０ｍｍ／ｍｉｎの条件で得た圧縮成形物（直径２７ｍｍ，重量約７ｇ）を試料に用いて加湿の条件について調べた。
(Examination of humidification conditions)
Powdered milk (25% fat, 58.3% sugar, 11.7% protein, mineral, moisture) on a universal testing machine autograph (manufactured by Shimadzu Corporation) under conditions of a compression force of 5 MPa and a compression speed of 10 mm / min The compression molded product (diameter: 27 mm, weight: about 7 g) obtained in the above was used as a sample and examined for humidification conditions.
試料を８０℃・１００％ＲＨ（コンビオ−ブン，フジマック製）または４０℃・９５％ＲＨ（恒温恒湿器，ＴＡＢＡＩ ＥＳＰＥＣ製）に一定時間置き，加湿前後の重量を測定することにより，加湿により増えた水分重量を求めた。その後，エアーオーブン（ヤマト科学）にて４０℃で３０分間乾燥し，錠剤硬度を測定した。また，実施例５における加湿時間と錠剤硬度との関係を図３に示し，実施例５における加湿水分量と錠剤硬度との関係を図４に示す。また，８０℃・１００％ＲＨ（コンビオ−ブン），及び４０℃・９５％ＲＨ（恒温恒湿器）における加湿時間，加湿重量(％)，及び乾燥後の硬度(Ｎ)の関係を，それぞれ表５−１，及び表５−２に示す。 Place the sample at 80 ° C / 100% RH (Combibiobun, manufactured by Fujimac) or 40 ° C / 95% RH (constant temperature and humidity chamber, manufactured by TABI ESPEC) for a certain period of time, and measure the weight before and after humidification. The increased water weight was determined. Then, it dried for 30 minutes at 40 degreeC with the air oven (Yamato Science), and measured tablet hardness. Moreover, the relationship between the humidification time in Example 5 and tablet hardness is shown in FIG. 3, and the relationship between the humidification water content in Example 5 and tablet hardness is shown in FIG. Also, the relationship between humidification time, humidification weight (%), and hardness after drying (N) at 80 ° C and 100% RH (combination) and 40 ° C and 95% RH (constant temperature and humidity chamber), The results are shown in Tables 5-1 and 5-2.
図３によれば，０．５重量％の加湿で，錠剤硬度の増大効果があることがわかる。また，約１重量％の加湿で錠剤硬度は約２倍となり，加湿重量の増加とともに錠剤硬度は大きくなる傾向にあった。加湿重量が２．５重量％を超えると錠剤硬度の増加は止まった。また，図４によれば，高温で処理するほど短時間で加湿工程が完了することがわかる。 According to FIG. 3, it can be seen that there is an effect of increasing tablet hardness with humidification of 0.5 wt%. In addition, when the humidification was about 1% by weight, the tablet hardness approximately doubled, and the tablet hardness tended to increase as the humidification weight increased. When the humidified weight exceeded 2.5% by weight, the increase in tablet hardness stopped. Moreover, according to FIG. 4, it turns out that a humidification process is completed in a short time, so that it processes at high temperature.
（長期保存性）
実施例１の５ＭＰａの圧縮力で製造した固形乳、及び原料として用いた粉乳をアルミ製の袋に入れ，３０℃の条件下での３ヶ月間保存し，溶解時間，錠剤硬度，遊離脂肪，過酸化物性，オイルオフ，風味の項目を試験例に従って調べた。この結果を表６に示す。表６から，溶解時間，錠剤硬度，遊離脂肪，オイルオフ，風味の項目は，製造時の初期値と差がないことがわかる。過酸化物価は，原料に用いた粉乳と同程度の値を示した。以上より，本発明の製造方法で得られた乳固形物は長期保存性に優れていることがわかる。
(Long-term storage)
The solid milk produced in Example 1 with a compressive force of 5 MPa and the powdered milk used as a raw material are put in an aluminum bag and stored for 3 months at 30 ° C., and the dissolution time, tablet hardness, free fat, The peroxide, oil-off, and flavor items were examined according to the test examples. The results are shown in Table 6. From Table 6, it can be seen that the items of dissolution time, tablet hardness, free fat, oil-off, and flavor are not different from the initial values at the time of production. The peroxide value was similar to the milk powder used as the raw material. From the above, it can be seen that the milk solid obtained by the production method of the present invention is excellent in long-term storage stability.
本発明の固形乳を実際に製造したところ，商品として製造・販売できることが分ったので，本発明の固形乳及びその製造方法は，粉乳の代替品及びその製造方法などとして食品産業において利用されうる。 Since the solid milk of the present invention was actually manufactured, it was found that it could be manufactured and sold as a product. Therefore, the solid milk of the present invention and its manufacturing method are used in the food industry as a substitute for milk powder and its manufacturing method. sell.
Claims (5)
前記遊離脂肪の含有率が０．７重量％〜３重量％であり，
空隙率が，３０％〜５０％であり，
粉乳のみを原料とする溶解されて飲用される乳幼児用の固形乳。Fat includes emulsified fat and free fat,
The free fat content is 0.7 wt% to 3 wt%,
The porosity is 30% to 50%,
Solid milk for infants that is dissolved and consumed only from powdered milk.
前記圧縮工程で得られた粉乳圧縮物を湿らせるための加湿工程と，
前記加湿工程で加湿された粉乳圧縮物を乾燥させるための乾燥工程とを含み，
前記粉乳の水分含有率が，１重量％〜４重量％であり，
前記粉乳の脂肪含有率が５重量％以上７０重量％以下であり，
前記圧縮工程は，打錠機により粉乳を圧縮し，
前記圧縮工程において，粉乳を圧縮する圧縮力が，１ＭＰａ〜１５ＭＰａであり，
前記加湿工程において，前記粉乳圧縮物に加えられる水分の量が，前記圧縮工程後の粉乳圧縮物の質量の０．５〜３％であり，
前記乾燥工程において，固形乳の水分含有率を原料として用いる粉乳の水分含有率の前後１％以内に制御する固形乳の製造方法により製造された請求項１に記載の固形乳。A compression step for compressing the powdered milk to obtain a solid powdered milk compressed product,
A humidifying step for moistening the compressed milk powder obtained in the compression step;
A drying step for drying the compressed milk powder compressed in the humidifying step,
The water content of the milk powder is 1 wt% to 4 wt%,
The fat content of the milk powder is 5 wt% or more and 70 wt% or less,
In the compression step, the milk powder is compressed by a tableting machine,
In the compression step, the compression force for compressing the milk powder is 1 MPa to 15 MPa,
In the humidification step, the amount of water added to the compressed milk powder is 0.5 to 3% of the mass of the compressed milk powder after the compression step,
Solid milk of Claim 1 manufactured by the manufacturing method of the solid milk which controls in the said drying process within 1% before and behind the moisture content of the powdered milk which uses the moisture content of solid milk as a raw material.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP2007292818A JP4605665B2 (en) | 2004-07-02 | 2007-11-12 | Solid milk and method for producing the same |
Applications Claiming Priority (2)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP2004196744 | 2004-07-02 | ||
| JP2007292818A JP4605665B2 (en) | 2004-07-02 | 2007-11-12 | Solid milk and method for producing the same |
Related Parent Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP2006528985A Division JP4062357B2 (en) | 2004-07-02 | 2005-07-01 | Solid milk and method for producing the same |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JP2008048748A JP2008048748A (en) | 2008-03-06 |
| JP4605665B2 true JP4605665B2 (en) | 2011-01-05 |
Family
ID=39233362
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP2007292818A Active JP4605665B2 (en) | 2004-07-02 | 2007-11-12 | Solid milk and method for producing the same |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JP4605665B2 (en) |
Families Citing this family (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP4603028B2 (en) * | 2004-07-02 | 2010-12-22 | 明治乳業株式会社 | Solid milk and method for producing the same |
| JP4603029B2 (en) * | 2004-07-02 | 2010-12-22 | 明治乳業株式会社 | Solid milk and method for producing the same |
| JP4618813B2 (en) * | 2004-07-02 | 2011-01-26 | 明治乳業株式会社 | Solid milk and method for producing the same |
Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2000095674A (en) * | 1998-09-22 | 2000-04-04 | Sato Pharmaceutical Co Ltd | Production of tablet having shortened intraoral disintegration time and apparatus therefor |
| JP2000316470A (en) * | 1999-04-28 | 2000-11-21 | Soc Prod Nestle Sa | Dry milk product and its production |
| JP2008048747A (en) * | 2004-07-02 | 2008-03-06 | Meiji Milk Prod Co Ltd | Solid milk and method for producing the same |
| JP2008048750A (en) * | 2004-07-02 | 2008-03-06 | Meiji Milk Prod Co Ltd | Solid milk, and method for producing the same |
| JP2008048749A (en) * | 2004-07-02 | 2008-03-06 | Meiji Milk Prod Co Ltd | Solid milk, and method for producing the same |
Family Cites Families (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS494948B1 (en) * | 1970-12-26 | 1974-02-04 | ||
| JPS5359066A (en) * | 1976-06-29 | 1978-05-27 | Tokyo Nourin Kk | Method of producing solid milk tablet |
| JP2919771B2 (en) * | 1995-04-17 | 1999-07-19 | 佐藤製薬株式会社 | Method for producing fast-dissolving tablet and fast-dissolving tablet produced by the method |
| JP3296412B2 (en) * | 1997-04-25 | 2002-07-02 | 田辺製薬株式会社 | Molded preparation and its manufacturing method |
-
2007
- 2007-11-12 JP JP2007292818A patent/JP4605665B2/en active Active
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2000095674A (en) * | 1998-09-22 | 2000-04-04 | Sato Pharmaceutical Co Ltd | Production of tablet having shortened intraoral disintegration time and apparatus therefor |
| JP2000316470A (en) * | 1999-04-28 | 2000-11-21 | Soc Prod Nestle Sa | Dry milk product and its production |
| JP2008048747A (en) * | 2004-07-02 | 2008-03-06 | Meiji Milk Prod Co Ltd | Solid milk and method for producing the same |
| JP2008048750A (en) * | 2004-07-02 | 2008-03-06 | Meiji Milk Prod Co Ltd | Solid milk, and method for producing the same |
| JP2008048749A (en) * | 2004-07-02 | 2008-03-06 | Meiji Milk Prod Co Ltd | Solid milk, and method for producing the same |
Also Published As
| Publication number | Publication date |
|---|---|
| JP2008048748A (en) | 2008-03-06 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| JP4062357B2 (en) | Solid milk and method for producing the same | |
| JP5420722B2 (en) | Solid milk and method for producing the same | |
| JP5744963B2 (en) | Food with a hollow | |
| JP6401334B2 (en) | Method for judging solubility and strength of solid milk and method for producing solid milk | |
| JP4618813B2 (en) | Solid milk and method for producing the same | |
| JP4605665B2 (en) | Solid milk and method for producing the same | |
| JP4603029B2 (en) | Solid milk and method for producing the same | |
| JP4603028B2 (en) | Solid milk and method for producing the same |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| A521 | Written amendment |
Free format text: JAPANESE INTERMEDIATE CODE: A523 Effective date: 20071203 |
|
| A977 | Report on retrieval |
Free format text: JAPANESE INTERMEDIATE CODE: A971007 Effective date: 20100426 |
|
| A131 | Notification of reasons for refusal |
Free format text: JAPANESE INTERMEDIATE CODE: A131 Effective date: 20100430 |
|
| RD13 | Notification of appointment of power of sub attorney |
Free format text: JAPANESE INTERMEDIATE CODE: A7433 Effective date: 20100601 |
|
| A521 | Written amendment |
Free format text: JAPANESE INTERMEDIATE CODE: A523 Effective date: 20100625 |
|
| A521 | Written amendment |
Free format text: JAPANESE INTERMEDIATE CODE: A523 Effective date: 20100629 |
|
| RD14 | Notification of resignation of power of sub attorney |
Free format text: JAPANESE INTERMEDIATE CODE: A7434 Effective date: 20100804 |
|
| TRDD | Decision of grant or rejection written | ||
| A01 | Written decision to grant a patent or to grant a registration (utility model) |
Free format text: JAPANESE INTERMEDIATE CODE: A01 Effective date: 20100924 |
|
| A01 | Written decision to grant a patent or to grant a registration (utility model) |
Free format text: JAPANESE INTERMEDIATE CODE: A01 |
|
| A61 | First payment of annual fees (during grant procedure) |
Free format text: JAPANESE INTERMEDIATE CODE: A61 Effective date: 20100930 |
|
| R150 | Certificate of patent or registration of utility model |
Ref document number: 4605665 Country of ref document: JP Free format text: JAPANESE INTERMEDIATE CODE: R150 Free format text: JAPANESE INTERMEDIATE CODE: R150 |
|
| FPAY | Renewal fee payment (event date is renewal date of database) |
Free format text: PAYMENT UNTIL: 20131015 Year of fee payment: 3 |
|
| FPAY | Renewal fee payment (event date is renewal date of database) |
Free format text: PAYMENT UNTIL: 20131015 Year of fee payment: 3 |
|
| S533 | Written request for registration of change of name |
Free format text: JAPANESE INTERMEDIATE CODE: R313533 |
|
| FPAY | Renewal fee payment (event date is renewal date of database) |
Free format text: PAYMENT UNTIL: 20131015 Year of fee payment: 3 |
|
| R350 | Written notification of registration of transfer |
Free format text: JAPANESE INTERMEDIATE CODE: R350 |
|
| R250 | Receipt of annual fees |
Free format text: JAPANESE INTERMEDIATE CODE: R250 |
|
| R250 | Receipt of annual fees |
Free format text: JAPANESE INTERMEDIATE CODE: R250 |
|
| R250 | Receipt of annual fees |
Free format text: JAPANESE INTERMEDIATE CODE: R250 |
|
| R250 | Receipt of annual fees |
Free format text: JAPANESE INTERMEDIATE CODE: R250 |
|
| S531 | Written request for registration of change of domicile |
Free format text: JAPANESE INTERMEDIATE CODE: R313531 |
|
| R350 | Written notification of registration of transfer |
Free format text: JAPANESE INTERMEDIATE CODE: R350 |
|
| R250 | Receipt of annual fees |
Free format text: JAPANESE INTERMEDIATE CODE: R250 |