JP3610640B2 - Production method of granulated material containing fine powder - Google Patents

Description

【０００１】
【発明の属する技術分野】
本発明は、微粉体状の素材を含有する造粒物の製造法に関し、特に健康食品として有用な微粉体状の素材を含有する造粒物の製造に応用することができる。
【０００２】
【従来の技術】
近年の我々を取りまく社会環境の変化の中で食生活の多様化は日常的でかつ身近な事象として認識できる。たとえば、食品の形態も固形状、ゲル状、ペースト状、フレーク状、乳化状、ゼリー状、粉状、液状など様々なものが市場に出ている。つまり食品の栄養価、機能、特性はもとより、味覚、臭覚、視覚などの官能特性を引き出す目的で形態が決定されている場合も多い。これらの食品の素材そのものは、一般消費者はもとより、食品加工メーカーでその特性を生かしながら用途、末端消費者の嗜好、年代、性別などに応じて様々に加工し、出来るだけ摂取しやすい形態にされている。
摂餌効率という広い観点からすれば、対象が人間以外の家畜、ペット、養殖魚等であってもよく、摂取させる素材として一般的な食品以外の飼料、栄養強化剤、健康食品、医薬品、食品添加物、飼料添加物、調味料、酵素製剤、生菌類などがあげられる。
【０００３】
上記の素材において、微粉体状のものが数多く存在し、これらは取扱いにくくまた加工しにくい。そのままでは摂取し難い欠点がある。
また、これらの素材の中には、苦味、渋味、えぐみなどを有するものも多くて摂取する際の障害となるため、これらの味のマスキングも必要となってくる。
例えば食品素材の中で、近年の健康志向にともない、イチョウ葉エキス末、ギムネマシルベスタ、茶抽出物等の健康食品素材、あるいはビフィズス菌に代表される有用腸内細菌、あるいはクロレラ、スピルリナ等の藻類乾燥品は、非常に微細な粉体として流通される場合が多い。
また、ガン抑制効果や免疫賦活効果があるといわれているシイタケ、ヒメマツタケ、マイタケ、サルノコシカケ（霊芝）等の菌子体抽出物は、多くは凍結乾燥された微粉体として流通している。
【０００４】
そのほか、凍結乾燥野菜、凍結乾燥果実、魚介類エキスの微粉末、粉末醤油、粉末味噌などの素材も一般的には、微粉体であるために重量あたりの表面積が大きく、非常に吸湿性が高いものが多くて保存性や取り扱いに問題があった。
従来は、上記の微粉体を流動層中で水、油脂類を結合剤として用い、デンプン、糖類、デキストリン等を増量材として用いて造粒または顆粒化する方法（流動層造粒）あるいは予めこれらの増量材と混合したのち蒸気を吹き付けて加熱しながら押し出す方法（押し出し造粒法）が一般的であった。
また、水分を使用する方法では、必ず造粒工程後に乾燥工程が入るため、味や風味を損なう場合が多い。また、生菌類および酵素類等の生体由来の微粉体を用いて造粒する場合には、これらの素材が、死滅あるいは失活するために使用できない。
【０００５】
特開平６−１２５７１７号公報には水を使用しない食品の乾式造粒方法が開示されており、特定の融点をもつ油脂類を粘結剤とし、油脂添加量、造粒方法、工程温度を規定し造粒食品を得ている。
また、特開平６−２２９９６１号公報には、遠心流動層内において球形顆粒を核とし、表面に粉体を吹き付けた後、糖質水溶液等をさらに噴霧被覆してなる多層造粒物の製造方法が提案されている。これらは、いずれの場合も水あるいは溶媒を介在させ被膜材を均一にコーティングし、かつ最終的に乾燥工程を経て造粒物を得るものである。
しかしながら、これらの乾式造粒法では、得られた造粒物の強度が弱くて被覆性が充分でないことが問題であった。
【０００６】
【発明が解決しようとする課題】
本発明の目的は、非常に細かい微粉体状の素材を取り扱い易い粒状物にするとともに、流動性の改善、脂質による被覆を完全にして吸湿性の抑制、臭味改善（マスキング）などの機能を付与する方法を提供することにある。
【０００７】
【課題を解決するための手段】
本発明は、素材である微粉体と核となるそれ以上の粒径と比重をもつ粒状粉体とを攪拌混合し、結合材を一切用いることなく、粒状粉体に微粉体を靜電気力により付着させ、さらに、脂質により被覆して微粉体を含有する造粒物を製造する方法である。本発明においては微粉体を付着さる粒状粉体を用いることが大きな特徴であり、これが核となる。
すなわち、本発明の第１の発明は、（Ａ）微粉体とその微粉体より粒径および比重が大きい粒状粉体とを混合攪拌することによ粒状粉体の表面にこの微粉体を付着せしめて造粒させた後、（Ｂ）溶融状態にある脂質を噴霧することにより、造粒物に脂質を被覆する微粉体含有造粒物の製造法である。本発明の第２の発明は、（Ａ）工程で造粒させた後、粒径が造粒物より小さい脂質粉体と造粒物とを混合攪拌して脂質を造粒物に被覆する微粉体含有造粒物の製造法である。また、本発明の第３の発明は、（Ａ）工程で造粒させた後、（Ｂ）工程で脂質を噴霧することにより脂質を被覆し、さらに（Ｃ）工程でその被覆造粒物より粒径の小さい脂質粉体とその造粒物とを混合攪拌して脂質を造粒物に被覆する微粉体含有造粒物の製造法である。
本発明に用いる粒状粉体は、非常に種類、品種が多く、用途またはその後の加工に併せて選択が可能であり応用範囲が広い。
【０００８】
【発明の実施の形態】
本発明の造粒方法は、（Ａ）工程、（Ｂ）工程と（Ｃ）工程の３工程からなり、（Ａ）工程は粒状粉体の表面に、微粉体を電気的力で付着せしめる方法であり、（Ｂ）工程は脂質を溶融・噴霧することにより被覆する方法と脂質を物理力で被覆する方法とであり、（Ｃ）工程はさらに脂質を物理力で被覆する方法である。
本発明における（Ａ）工程は粒状粉体の表面に、微粉体を電気的力で付着せしめて造粒させる方法である。
この粒状粉体の粒径は微粉体の粒径の１０〜１０００倍で、比重が微粉体の１．２〜１００倍である。粒状粉体の粒径が微粉体粒径の１０倍未満で、比重が微粉体の１．２倍未満であると微粉体が粒状粉体表面にコーテングできない。粒状粉体の粒径が微粉体粒径の１０００倍を超え、比重が微粉体の１００倍を超えると微粉体が粒状粉体表面にコーテングできない。
次に、（Ｂ）工程で脂質素材を物理力で被覆する方法の場合はその脂質の粒径が（Ａ）工程で得られる造粒物の粒径の０．００１〜０．９９倍である。脂質の粒径が造粒物の粒径の０．００１倍未満であるとコーテングできず、脂質の粒径が造粒物の０．９９を超えると脂質がコーテングできない。
好ましくは、（Ａ）工程において粒状粉体の粒径が微粉体粒径の２〜５倍で、粒状粉体の比重が微粉体の比重が２〜３倍である。
また、微粉状の素材の粒径としてはできるだけ小さい方が好ましい。
【０００９】
本発明の対象となる微紛体としては、健康食品原料、調味料原料、香辛料原料、生菌、酵素、アミノ酸、ペプタイド、ビタミン、有機酸、医薬品原料等があげられる。
具体的には、健康食品として、イチョウ葉エキス末、茶抽出物粉末、甘草抽出物粉末、ギムネマシルベスタ、菌子体抽出物（シイタケ、ヒメマツタケ、マイタケ、カワラダケ、麗芝等）、プロポリス末、冬虫夏草末、サメ軟骨粉末、朝鮮人参粉末、クロレラ粉末、スピルリナ粉末、ロイヤルゼリー末、花粉、クマザサ末エゾウコギ末、玄米酵素、納豆菌、酵母等があげられる。
また、調味料原料、香辛料原料としては、粉末味噌、粉末醤油、粉末ソース、スパイス、粉末カレー粉等があげられる。また、生菌類としては有用腸内細菌としてのビフィズス菌をはじめとする乳酸菌等、酵素としては、リパーゼ、プロテアーゼ、セルラーゼ、アミラーゼ等の食品工業用酵素があげられる。
これらの微粉体は、一般食品原料、健康食品原料、医薬品原料等として流通する際には吸湿性が高く、また粉立ちがあるため取扱いが難しく、また風味が悪いものも多いので、造粒物として取り扱うことが好ましい。
【００１０】
本発明で使用する、造粒物の核となる粒状粉体としては、例えば、蔗糖、グラニュー糖などの糖；アビセルなどの結晶セルロース；エリスルトールなどの糖アルコール；塩化ナトリウム、炭酸カルシウム、硫酸カルシウム、塩化マグネシウム等の無機塩；アスコルビン酸、クエン酸、リンゴ酸、フマール酸、ソルビン酸、コハク酸、酒石酸、グルコン酸等の有機酸；アスコルビン酸ナトリウム、アスコルビン酸カルシウム、クエン酸ナトリウム、クエン酸カルシウム、クエン酸第一鉄、グルコン酸亜鉛等の有機酸塩などがあげられる。
これらの微粉体と粒状粉体との組合わせにおいて、例えば、イチョウ葉エキス末とグラニュー糖、ビフィズス菌原末とグルコン酸、クロレラパウダーとグラニュー糖、パンクレアチンとアビセル、ギムネマシルベスタとグラニュー糖の組み合わせ等がある。
【００１１】
また本発明の造粒物の最外層となる脂質としては、融点として４０℃以上、望ましくは５０℃以上のものであれば良く、特にその種類を限定するものではない。 例えば、硬化油としては牛脂極度硬化油（融点：５８〜６０℃）、菜種極度硬化油（融点：６８〜６９℃）、パーム極度硬化油（融点：６６〜７０℃）、大豆極度硬化油（融点：６９〜７２℃）、硬化ホホバ油（融点：６８〜７０℃）などがあげられる。
また、ワックスでは、カルナバワックス（融点：８０〜８６℃）、ライスワックス（融点：７０〜８３℃）、キャンデリラワックス（融点：６８〜７２℃）、ミツロウ（融点：６５〜６７℃）などを用いることも可能である。脂肪酸ではステアリン酸（融点：６８〜７０℃）、ミリスチン酸（融点：５３〜５５℃）、パルミチン酸（融点：６２〜６４℃）、エイコサン酸（融点：７５〜７７℃）、ベヘン酸（融点：８０〜８２℃）などを用いることができる。
また、融点が非常に高いものとしては金属石鹸であるステアリン酸カルシウム（融点：１５８〜１６０℃）、パルミチン酸カルシウム（融点：１６５〜１７０℃）等がある。またステロールとしは、コレステロール（融点：１４５〜１４９℃）、フコステロール（融点：１２０〜１２４℃）、カンペステロール（融点：１５５〜１５７℃）、ラノステロール（融点：１３５〜１３９℃）などがあげられる。
さらにグリセリンの部分脂肪酸エステルとしては高融点のグリセリンモノ脂肪酸エステル、グリセリンジ脂肪酸エステル等があげられ、具体的には、ステアリン酸モノグリセリド（「エマルジーＭＳ」理研ビタミン（株）製：融点６８〜６９℃）、ステアリン酸ジグリセリド（「エマルジーＢ−２００」理研ビタミン（株）製：融点６９〜７０℃）などが使用される。これらの硬化油、ワックス、脂肪酸、金属石鹸、グリセリンの部分脂肪酸エステルは目的用途に応じて適宜選択することができる。
【００１２】
つぎに各発明の具体的な製造法の操作について説明する。
第１の発明においては微粉体と粒状粉体とを混合攪拌する方法は通常の混合機を用いて両者を混合攪拌するだけでよく、混合機としては市販の混合機や混合造粒機を用いることができる。この場合に両者を付着させる結合剤は必要とせず、両者は靜電気的に付着する。この際とくに加温する必要もない。
つぎに、この表面にこの微粉体を付着せしめた粒状粉体に溶解した脂質を噴霧して添加する。添加された脂質は付加物表面で固まり、粒状粉体の表面に微粉体の付着した粒子が脂質により被覆される。
第２の発明は、第１の発明の前半の工程で得られた微粉体を表面に付着した粒状粉体を混合攪拌しつつ、粒状粉体より粒径の小さい脂質を加えて粉体混合攪拌して脂質を微粉体が表面に付着した粒状粉体の表面に付着することができる。
第３の発明は、第１の発明で得られた脂質で被覆された微粉体含有造粒物を混合攪拌しつつ、さらにこの粒子より粒径の小さい脂質を加えて粉体混合する。
この粒子より粒径の小さい脂質は第１の発明の造粒物をさらに被覆することになる。
本発明に用いる微粉体と粒状粉体との混合比は、重量基準で、１：５〜１：１００、好ましくは１：１０であり、脂質の使用量は微粉体との比は、重量基準で、１：１〜１０：１、好ましくは１：１〜２：１である。
本発明に用いる粒状粉体は、非常に種類、品種が多く、用途またはその後の加工に併せて選択が可能であり応用範囲が広い。
【００１３】
【実施例】
本発明を実施例および比較例によりさらに詳細に説明する。
比較例Ａ
苦味を有するイチョウ葉エキス末（フランス原産：平均粒径７０μｍ、嵩比重０．５６）５０ｇおよび日本坩糖（株）製のグラニュー糖（平均粒径４６５μｍ：比重１．１）３５０ｇを攪拌型造粒装置（奈良機械（株）製 ＯＭＤ−３型）に投入し、機内温度２０℃、窒素ガス雰囲気下において、主軸回転数５００ｒｐｍ、副軸回転数１０００ｒｐｍで１０分間攪拌して一次造粒物を得た。この段階においてグラニュー糖にイチョウ葉エキス末が均質に付着しており、殆ど未付着のイチョウ葉エキス末は存在しなかった。さらに、この一次造粒物を主軸回転数２００ｒｐｍ、副軸回転数５００ｒｐｍの条件で攪拌しながら、溶融した牛脂硬化油（融点４８℃）１０ｇを噴霧器を用いて５分間かけて流動層内にゆっくりと噴霧した。その後１０分間攪拌を続けた。得られた造粒物は非常に粒径が揃い、かつイチョウ葉エキスの持つ特有の苦味はかなり減少していた。造粒物とイチョウ葉エキス原末のそれぞれについて、３７℃の精製水９００ｍｌにイチョウ葉エキス分として６９０ｍｇを添加し、１００ｒｐｍで６０分間攪拌し、波長３２０ｎｍの吸光度から溶出率を測定した結果、造粒物の溶出率は原末の２０％であった。
【００１４】
比較例１
比較例Ａで用いたイチョウ葉エキス末５０ｇを比較例Ａで用いた攪拌型造粒装置に投入し、機内温度２０℃、窒素ガス雰囲気下において、主軸回転数２００ｒｐｍ、副軸回転数５００ｒｐｍで攪拌しながら、溶融した牛脂硬化油（融点４８℃）１０ｇを噴霧器を用いて５分間かけて流動層内にゆっくりと噴霧し攪拌造粒した。この段階で、イチョウ葉エキスの苦味は抑制されていなかった。また、流動性は不良であった。
【００１５】
実施例１
ビフィズス菌原末（新扶桑製薬（株）製、５０％殺菌でんぷん希釈品（平均粒径５０μｍ、嵩比重０．５）５０ｇおよびグルコン酸（顆粒品、平均粒径２００μｍ）４００ｇを攪拌型造粒装置（ヘンシルミキサー）に投入し、回転数５００ｒｐｍで１０分間攪拌した。この段階において、投入時のカサが明らかに減り、粉体が落ちついて、ビフィズス菌末がグルコン酸顆粒に付着してきていた。この時の造粒物の平均粒径は２８０μｍであつた。さらに、微粉体の菜種極度硬化油（融点６８℃、平均粒径５μｍ、比重０．３８）を５０ｇ投入し、回転数７００ｒｐｍで約１０分間攪拌した。得られた造粒品の菌数を直後と１ヶ月後（２０℃保管）で比較したところ、ほぼ配合理論値と同じ値を示した。
【００１６】
比較例２
実施例１で用いたビフィズス菌原末５０ｇと実施例１で用いた菜種極度硬化油４００ｇとを実施例１で用いた攪拌型造粒装置に投入し、回転数５００ｒｐｍで１０分間攪拌した。この段階において、粉立ちして粉体の流動性は不良であり、菌数も１ヶ月後（２０℃保管）で、７０％に低下していた。
【００１７】
実施例２
クロレラパウダー（クロレラ工業（株）製：平均粒径２０μｍ、嵩比重０．５５）５０ｇおよび比較例Ａで用いたグラニュー糖４００ｇを攪拌型造粒装置（深江工業（株）製 ハイスピードミキサー）に投入し、主軸回転数５００ｒｐｍ、機内温度２０℃で１０分間攪拌した。この段階で比重の非常に軽いクロレラパウダーは、殆どグラニュー糖に付着しており、投入時のカサは明らかに減少していた。しかしこの段階においては、表面のクロレラの青臭みは感じた。この時の造粒物の平均粒径は５００μｍであつた。つぎに、実施例１で用いた微粉体の菜種極度硬化油５０ｇ投入し、主軸回転数７００ｒｐｍで約１０分間攪拌した。得られたクロレラ造粒物はクロレラの青臭さが明らかに減少していた。
【００１８】
比較例３
実施例２で用いたクロレラパウダー５０ｇと実施例１で用いた微粉体の菜種極度硬化油４００ｇを実施例２で用いた攪拌型造粒装置に投入し、回転数６００ｒｐｍで１０分間攪拌した。この段階において、クロレラの青臭みは消えていなかった。さらに、同じ菜種極度硬化油の微粉体を５０ｇ添加し同様の条件で攪拌を１０分間継続したが、クロレラの青臭みは消えていなかった。
【００１９】
実施例３
パンクレアチン（天野製薬（株）製：平均粒径３０μｍ、比重０．６２）５０ｇとアビセル（旭化成 （株）製：平均粒径１５０μｍ、比重０．８７）３５０ｇを攪拌型造粒装置（奈良機械（株）製ＯＭＤ−１５０型）に投入し、機内温度２０℃、窒素ガス雰囲気下において、主軸回転数５００ｒｐｍ、副軸回転数１０００ｒｐｍで１０分間攪拌した。この際、酵素製剤が非常に水を嫌うため、機内の乾燥状態に留意した。この段階において、仕込み当初のカサが明らかに減り、微粉状パンクレアチンの飛散も減少した。この時の造粒物の平均粒径は２１４μｍであつた。この段階においてはパンクレアチン特有の酸味が認められた。さらに実施例１で用いた微粉体の菜種極度硬化油１００ｇを添加し、主軸回転数７００ｒｐｍ、副軸回転数１５００ｒｐｍで約１０分間攪拌した。得られたパンクレアチン造粒物は酸味が消えており、また良好な流動性を示した。
【００２０】
比較例４
実施例３で用いたパンクレアチン５０ｇと実施例１で用いた微粉体の菜種極度硬化油３５０ｇを実施例３で用いた攪拌型造粒装置に投入し、機内温度２０℃、窒素ガス雰囲気下において、主軸回転数５００ｒｐｍ、副軸回転数１０００ｒｐｍで１０分間攪拌した。この段階において、パンクレアチンの酸味はやや希釈されたものの残っていた。さらに同じ菜種極度硬化油微粉体５０ｇを追加し、攪拌造粒を２０分間継続したが同じ状態で改善は認められなかった。
【００２１】
実施例４
比較例Ａで用いたイチョウ葉エキス末５０ｇと比較例Ａで用いたグラニュー糖３５０ｇを比較例１で用いた攪拌型造粒装置に投入し、機内温度２０℃、窒素ガス雰囲気下において、主軸回転数５００ｒｐｍ、副軸回転数１０００ｒｐｍで攪拌して一次造粒物を得た。この段階においてグラニュー糖にイチョウ葉エキス末が均質に付着しており、殆ど未付着のイチョウ葉エキス末は存在しなかった。さらに、この一次造粒物を主軸回転数２００ｒｐｍ、副軸回転数５００ｒｐｍの条件で攪拌しながら、溶融した牛脂硬化油（融点４８℃）１０ｇを噴霧器を用いて５分間かけて流動層内にゆっくりと噴霧した後１０分間攪拌を続けた。この時の造粒物の平均粒径は６１０μｍであつた。状態が落ちつくまで、約１０分間攪拌を継続し、実施例１で用いた微粉体の菜種極度硬化油の微粉体９０ｇを添加し、主軸回転数７００ｒｐｍ、副軸回転数１５００ｒｐｍの条件で攪拌し１０分間攪拌して目的の造粒物を得た。
【００２２】
比較例５
比較例Ａで用いたイチョウ葉エキス末５０ｇと実施例１で用いた菜種極度硬化油の微粉体３５０ｇを比較例Ａで用いた攪拌型造粒装置に投入し、機内温度２０℃、窒素ガス雰囲気下において、主軸回転数５００ｒｐｍ、副軸回転数１０００ｒｐｍで攪拌して１０分間攪拌して目的の造粒物を得た。この段階で、イチョウ葉エキス末の苦味は非常に強かった。また、流動性についても粉立ちがして不良であつた。
【００２３】
実施例１〜４および比較例Ａ、比較例１〜５で製造した造粒物について被覆性、流動性を下記の評価基準で測定し、その結果を表１および表２に示した。
[被覆性の評価基準]
○：被覆が完全で原末の臭いまたは味が感じられない。
△：被覆が不完全で原末の臭いまたは味がやや感じられる。
×：被覆が不良で原末の臭いまたは味が強く感じられる。
[流動性の評価基準]
○：粉立ちせず、さらさらとしていて流動性は良好である。
△：粉立ちはしないが、流動性はやや不良である。
×：粉立ちしたり、べとべとしたりして流動性は不良である。
【００２４】
【表１】

【００２５】
【表２】

【００２６】
表１の結果から、実施例１〜４は脂質の被覆が完全であり、苦み、青臭み、酸味の風味は完全にはマスキングされており臭味改善ができたうえに、粉体の流動性改善、吸湿性の抑制、粉立ち防止ができた。これに反し、表２の結果から、比較例１は被覆が完全でなく、イチョウ葉エキスの苦味は抑制できず流動性も不良で、比較例２は被覆が完全でなく、粉体の流動性は改善されず菌数も１ヶ月後で７０％に低下していた。比較例３はクロレラの青臭みは、消えておらずマスキングは不十分であった。また、比較例４は被覆が完全でなく、パンクレアチンの酸味はやや希釈されたものの強く感じられた。比較例５は被覆が完全でなく、イチョウ葉エキスの苦味は抑制できず流動性も不良であつた。
【００２７】
【発明の効果】
本発明の方法により得られた微粉体含有造粒物は、極めて被覆性と流動性に優れ、長期の保存と取り扱いに効果的である。また、本発明の方法においては水や溶媒を一切使用しないため、微粉体素材の変質は極めて少く健康食品や医薬品の造粒化に極めて有用な方法である。[0001]
BACKGROUND OF THE INVENTION
The present invention relates to a method for producing a granulated material containing a fine powder material, and can be applied particularly to the production of a granulated material containing a fine powder material useful as a health food.
[0002]
[Prior art]
Diversification of eating habits can be recognized as a daily and familiar phenomenon in the social environment surrounding us in recent years. For example, various food forms such as solid, gel, paste, flake, emulsified, jelly, powder, and liquid are on the market. In other words, the form is often determined for the purpose of extracting sensory characteristics such as taste, smell, and vision as well as the nutritional value, function, and characteristics of food. These food ingredients themselves are processed by various food processing manufacturers according to their use, end consumer preference, age, gender, etc. while taking advantage of their characteristics, not only for general consumers, but in a form that is as easy to consume as possible. Has been.
From a broad viewpoint of feeding efficiency, the target may be livestock other than humans, pets, farmed fish, etc., and feeds other than general foods, nutrition enhancers, health foods, pharmaceuticals, foods Additives, feed additives, seasonings, enzyme preparations, live fungi and the like.
[0003]
There are many fine powders of the above materials, which are difficult to handle and process. There is a drawback that it is difficult to take as it is.
In addition, some of these ingredients have bitterness, astringency, egumi, etc., which are obstacles to ingestion, so masking of these tastes is also necessary.
For example, among food ingredients, health food ingredients such as ginkgo biloba extract powder, Gymnema sylvestre, tea extract, or useful intestinal bacteria represented by bifidobacteria, or algae such as chlorella and spirulina Dry products are often distributed as very fine powders.
In addition, mycelium extracts such as shiitake mushroom, himematsutake, maitake, and sarcoma mushroom (reishi), which are said to have a cancer suppressing effect and an immunostimulatory effect, are often distributed as lyophilized fine powders.
[0004]
In addition, materials such as freeze-dried vegetables, freeze-dried fruits, seafood extract fine powder, powdered soy sauce, and powdered miso are generally fine powder, so they have a large surface area per weight and are extremely hygroscopic. There were many things and there was a problem in storage stability and handling.
Conventionally, the above-mentioned fine powder is granulated or granulated using water, fats and oils as binders in the fluidized bed, and starch, saccharides, dextrin, etc. as extenders (fluidized bed granulation) or these in advance. A method of extruding while heating with spraying steam after mixing with the above extender (extrusion granulation method) was common.
Moreover, in the method using water, since a drying process is always performed after the granulation process, the taste and flavor are often impaired. Moreover, when granulating using fine powder derived from living organisms such as live fungi and enzymes, these materials cannot be used because they are killed or inactivated.
[0005]
JP-A-6-125717 discloses a dry granulation method for foods that does not use water, and fats and oils having a specific melting point are used as a binder, and the amount of fat and oil added, the granulation method, and the process temperature are specified. A granulated food is obtained.
Japanese Patent Application Laid-Open No. 6-229961 discloses a method for producing a multilayer granulated product in which a spherical granule is used as a nucleus in a centrifugal fluidized bed, a powder is sprayed on the surface, and then an aqueous solution of sugar is further spray-coated. Has been proposed. In these cases, in any case, water or a solvent is interposed to uniformly coat the film material, and finally a granulated product is obtained through a drying process.
However, in these dry granulation methods, there is a problem that the strength of the obtained granulated product is weak and the covering property is not sufficient.
[0006]
[Problems to be solved by the invention]
The purpose of the present invention is to make the material of very fine fine powder form easy to handle, improve fluidity, completely cover with lipid, suppress hygroscopicity, improve odor (masking), etc. It is to provide a method of granting.
[0007]
[Means for Solving the Problems]
The present invention stirs and mixes a fine powder as a raw material and a granular powder having a larger particle size and specific gravity as a core, and attaches the fine powder to the granular powder by electric force without using any binder. And a granulated product containing fine powder by coating with lipid. In the present invention, the use of granular powder to which fine powder adheres is a major feature, which is the core.
That is, according to the first aspect of the present invention, (A) a fine powder and a granular powder having a particle size and specific gravity larger than that of the fine powder are mixed and stirred to adhere the fine powder to the surface of the granular powder. (B) A method for producing a granulated product containing fine powder in which the granulated product is coated with lipid by spraying the lipid in a molten state. The second invention of the present invention is a fine powder for coating a granulated product by mixing and stirring the lipid powder and the granulated product having a particle size smaller than the granulated product after granulation in the step (A). It is a manufacturing method of a body containing granulated material. In addition, the third invention of the present invention is to coat the lipid by spraying the lipid in the step (B) after granulating in the step (A), and further from the coated granulated product in the step (C). This is a method for producing a granulated product containing fine powder in which a lipid powder having a small particle diameter and a granulated product thereof are mixed and stirred to coat the granulated product with lipid.
The granular powder used in the present invention has many types and varieties, and can be selected according to the use or subsequent processing, and has a wide range of applications.
[0008]
DETAILED DESCRIPTION OF THE INVENTION
The granulation method of the present invention comprises three steps of (A) step, (B) step and (C) step, and (A) step is a method of attaching fine powder to the surface of the granular powder by electric force. Step (B) is a method of coating by melting and spraying lipids and a method of coating lipids with physical force, and step (C) is a method of further coating lipids with physical force.
Step (A) in the present invention is a method in which fine powder is adhered to the surface of the granular powder by electric force and granulated.
The particle size of the granular powder is 10 to 1000 times that of the fine powder, and the specific gravity is 1.2 to 100 times that of the fine powder. When the particle size of the granular powder is less than 10 times the particle size of the fine powder and the specific gravity is less than 1.2 times that of the fine powder, the fine powder cannot be coated on the surface of the granular powder. When the particle size of the granular powder exceeds 1000 times that of the fine powder and the specific gravity exceeds 100 times that of the fine powder, the fine powder cannot be coated on the surface of the granular powder.
Next, in the method of coating the lipid material with physical force in the step (B), the particle size of the lipid is 0.001 to 0.99 times the particle size of the granulated product obtained in the step (A). . If the particle size of the lipid is less than 0.001 times the particle size of the granulated product, coating cannot be performed, and if the particle size of the lipid exceeds 0.99 of the granulated product, lipid cannot be coated.
Preferably, in step (A), the particle size of the granular powder is 2 to 5 times the particle size of the fine powder, and the specific gravity of the granular powder is 2 to 3 times that of the fine powder.
Further, the particle size of the fine powder material is preferably as small as possible.
[0009]
Examples of the fine powder targeted by the present invention include health food raw materials, seasoning raw materials, spice raw materials, live bacteria, enzymes, amino acids, peptides, vitamins, organic acids, pharmaceutical raw materials, and the like.
Specifically, as health foods, ginkgo biloba extract powder, tea extract powder, licorice extract powder, Gymnema sylvestre, mycelium extract (Shiitake, Himematsutake, Maitake, Kawarada, Reishi), propolis powder, cordyceps Shark cartilage powder, ginseng powder, chlorella powder, spirulina powder, royal jelly powder, pollen, kumaza powder, elephant powder, brown rice enzyme, natto, yeast and the like.
Examples of the seasoning material and spice material include powdered miso, powdered soy sauce, powdered sauce, spices, and powdered curry powder. Examples of live fungi include lactic acid bacteria such as bifidobacteria as useful intestinal bacteria, and examples of enzymes include food industry enzymes such as lipase, protease, cellulase, and amylase.
These fine powders are highly hygroscopic when distributed as general food raw materials, health food raw materials, pharmaceutical raw materials, etc., and are difficult to handle because they are powdered, and many of them have poor flavor. It is preferable to handle as
[0010]
The granular powder used as the core of the granulated product used in the present invention includes, for example, sugar such as sucrose and granulated sugar; crystalline cellulose such as Avicel; sugar alcohol such as erythritol; sodium chloride, calcium carbonate, calcium sulfate, Inorganic salts such as magnesium chloride; organic acids such as ascorbic acid, citric acid, malic acid, fumaric acid, sorbic acid, succinic acid, tartaric acid, gluconic acid; sodium ascorbate, calcium ascorbate, sodium citrate, calcium citrate, And organic acid salts such as ferrous citrate and zinc gluconate.
In combination of these fine powders and granular powders, for example, a combination of ginkgo biloba extract powder and granulated sugar, bifidobacteria raw powder and gluconic acid, chlorella powder and granulated sugar, pancreatin and avicel, gymnema sylvestre and granulated sugar Etc.
[0011]
In addition, the lipid to be the outermost layer of the granulated product of the present invention may have a melting point of 40 ° C. or higher, desirably 50 ° C. or higher, and the type is not particularly limited. For example, as the hardened oil, beef tallow extremely hardened oil (melting point: 58-60 ° C), rapeseed extremely hardened oil (melting point: 68-69 ° C), palm extremely hardened oil (melting point: 66-70 ° C), soybean hardened oil ( Melting point: 69-72 ° C.), hardened jojoba oil (melting point: 68-70 ° C.) and the like.
In addition, as the wax, carnauba wax (melting point: 80 to 86 ° C.), rice wax (melting point: 70 to 83 ° C.), candelilla wax (melting point: 68 to 72 ° C.), beeswax (melting point: 65 to 67 ° C.), etc. It is also possible to use it. Among fatty acids, stearic acid (melting point: 68-70 ° C), myristic acid (melting point: 53-55 ° C), palmitic acid (melting point: 62-64 ° C), eicosanoic acid (melting point: 75-77 ° C), behenic acid (melting point) : 80-82 ° C.).
Moreover, as a thing with very high melting | fusing point, there exist calcium stearate (melting point: 158-160 degreeC) which is a metal soap, calcium palmitate (melting point: 165-170 degreeC), etc. Examples of sterols include cholesterol (melting point: 145 to 149 ° C.), fucosterol (melting point: 120 to 124 ° C.), campesterol (melting point: 155 to 157 ° C.), lanosterol (melting point: 135 to 139 ° C.), and the like. .
Furthermore, examples of the partial fatty acid ester of glycerin include a high melting point glycerin monofatty acid ester and glycerin difatty acid ester. Specifically, stearic acid monoglyceride ("Emulsy MS" manufactured by Riken Vitamin Co., Ltd .: melting point 68-69 ° C) ), Stearic acid diglyceride (“Emulsy B-200” manufactured by Riken Vitamin Co., Ltd .: melting point 69-70 ° C.) and the like. These hardened oils, waxes, fatty acids, metal soaps, and partial fatty acid esters of glycerin can be appropriately selected according to the intended use.
[0012]
Next, the operation of the specific production method of each invention will be described.
In the first invention, the method of mixing and stirring the fine powder and the granular powder only needs to mix and stir both using a normal mixer, and a commercially available mixer or mixing granulator is used as the mixer. be able to. In this case, there is no need for a binder to attach the two, and the two are electrically attached. At this time, it is not necessary to heat.
Next, the lipid dissolved in the granular powder having the fine powder adhered to the surface is added by spraying. The added lipid hardens on the surface of the adduct, and the particles having fine powder adhered to the surface of the granular powder are coated with the lipid.
The second aspect of the invention is to mix and agitate the granular powder obtained by attaching the fine powder obtained in the first half of the first aspect to the surface, while adding and stirring the powder with a smaller particle size than the granular powder. Thus, the lipid can be attached to the surface of the granular powder having the fine powder attached to the surface.
In the third invention, the fine powder-containing granule coated with the lipid obtained in the first invention is mixed and stirred, and a lipid having a smaller particle diameter than this particle is further added and mixed by powder.
The lipid having a smaller particle diameter than this particle further coats the granulated product of the first invention.
The mixing ratio of the fine powder and the granular powder used in the present invention is 1: 5 to 1: 100, preferably 1:10 on a weight basis, and the amount of lipid used is the weight basis. And 1: 1 to 10: 1, preferably 1: 1 to 2: 1.
The granular powder used in the present invention has many types and varieties, and can be selected according to the use or subsequent processing, and has a wide range of applications.
[0013]
【Example】
The present invention will be described in more detail with reference to examples and comparative examples.
Comparative Example A
50 g of ginkgo biloba extract powder having a bitter taste (origin of France: average particle size 70 μm, bulk specific gravity 0.56) and 350 g of granulated sugar (average particle size 465 μm: specific gravity 1.1) manufactured by Nippon Sucrose Co., Ltd. Put into a granulator (OMD-3 type, manufactured by Nara Machinery Co., Ltd.) and stir for 10 minutes at a spindle speed of 500 rpm and a counterspindle speed of 1000 rpm under an in-machine temperature of 20 ° C. and a nitrogen gas atmosphere. Obtained. At this stage, ginkgo biloba extract powder was uniformly attached to the granulated sugar, and almost no ginkgo biloba extract powder was present. Further, while stirring the primary granulated product under the conditions of the main shaft rotation speed of 200 rpm and the counter shaft rotation speed of 500 rpm, 10 g of melted beef tallow oil (melting point: 48 ° C.) is slowly put into the fluidized bed over 5 minutes using a sprayer. And sprayed. Thereafter, stirring was continued for 10 minutes. The obtained granulated product was very uniform in particle size, and the characteristic bitterness of the ginkgo biloba extract was considerably reduced. As a result of adding 690 mg as a ginkgo biloba extract to 900 ml of purified water at 37 ° C. for each granulated product and ginkgo biloba extract powder, stirring at 100 rpm for 60 minutes, and measuring the elution rate from absorbance at a wavelength of 320 nm. The elution rate of the granules was 20% of the bulk powder.
[0014]
Comparative Example 1
Comparative Example was placed in a stirred granulator using a ginkgo leaf extract powder 50g in Comparative Example A used in A, internal temperature 20 ° C., stirred under a nitrogen gas atmosphere, spindle speed 200 rpm, at 500rpm countershaft rotational speed Then, 10 g of the melted beef tallow oil (melting point: 48 ° C.) was slowly sprayed into the fluidized bed for 5 minutes using an atomizer and stirred and granulated. At this stage, the bitter taste of the ginkgo biloba extract was not suppressed. Moreover, the fluidity was poor.
[0015]
Example 1
Bifidobacteria raw powder (manufactured by Shin Fuso Pharmaceutical Co., Ltd., 50% sterilized starch diluted product (average particle size 50 μm, bulk specific gravity 0.5) 50 g and gluconic acid (granular product, average particle size 200 μm) 400 g with stirring granulation The mixture was put into the apparatus (Hensyl mixer) and stirred for 10 minutes at a rotation speed of 500 rpm.At this stage, there was a clear decrease in the bulk at the time of addition, the powder settled down, and the Bifidobacterium powder had adhered to the gluconic acid granules. At this time, the average particle size of the granulated product was 280 μm, and 50 g of fine rapeseed extremely hardened oil (melting point 68 ° C., average particle size 5 μm, specific gravity 0.38) was added and rotated at 700 rpm. When the number of bacteria in the obtained granulated product was compared immediately after and after 1 month (20 ° C. storage), it was almost the same as the theoretical value of the blend.
[0016]
Comparative Example 2
Was charged and rapeseed extremely hardened oil 400g used in bifidobacteria KinHara end 50g of Example 1 used in Example 1 in a stirred granulator used in Example 1, was stirred rpm 500rpm for 10 minutes. At this stage, powder flow was poor and the fluidity of the powder was poor, and the number of bacteria was reduced to 70% after one month (20 ° C. storage).
[0017]
Example 2
Chlorella powder (manufactured by Chlorella Kogyo Co., Ltd .: average particle size 20 μm, bulk specific gravity 0.55) 50 g and granulated sugar 400 g used in Comparative Example A were added to a stirring granulator (high speed mixer manufactured by Fukae Kogyo Co., Ltd.). The mixture was stirred and stirred for 10 minutes at a spindle speed of 500 rpm and an in-machine temperature of 20 ° C. At this stage, the chlorella powder, which has a very low specific gravity, was almost attached to the granulated sugar, and the bulk at the time of input was clearly reduced. At this stage, however, the blue odor of the surface chlorella was felt. The average particle size of the granulated product at this time was 500 μm. Next, 50 g of rapeseed extremely hardened oil of fine powder used in Example 1 was added and stirred for about 10 minutes at a spindle rotation speed of 700 rpm. The obtained chlorella granule had a clear decrease in the blue odor of chlorella.
[0018]
Comparative Example 3
50 g of chlorella powder used in Example 2 and 400 g of rapeseed extremely hardened oil of fine powder used in Example 1 were put into the stirring granulator used in Example 2 , and stirred at a rotation speed of 600 rpm for 10 minutes. At this stage, the blue odor of Chlorella was not gone. Furthermore, 50 g of the same rapeseed extremely hardened oil fine powder was added and stirring was continued for 10 minutes under the same conditions, but the blue smell of chlorella was not gone.
[0019]
Example 3
50 g of pancreatin (Amano Pharmaceutical Co., Ltd .: average particle size 30 μm, specific gravity 0.62) and 350 g of Avicel (Asahi Kasei Co., Ltd .: average particle size 150 μm, specific gravity 0.87) were mixed with a stirring granulator (Nara Machinery). (OMD-150 manufactured by Co., Ltd.), and stirred for 10 minutes at a spindle rotation speed of 500 rpm and a countershaft rotation speed of 1000 rpm under an in-machine temperature of 20 ° C. and a nitrogen gas atmosphere. At this time, since the enzyme preparations dislike water very much, attention was paid to the dry state in the machine. At this stage, there was a clear decrease in the initial bulk and the amount of finely divided pancreatin scattered. The average particle size of the granulated product at this time was 214 μm. At this stage, a sour taste peculiar to pancreatin was observed. Further, 100 g of rapeseed extremely hardened oil of fine powder used in Example 1 was added, and the mixture was stirred for about 10 minutes at a spindle rotation speed of 700 rpm and a countershaft rotation speed of 1500 rpm. The obtained pancreatin granulated product had disappeared acidity and showed good fluidity.
[0020]
Comparative Example 4
50 g of pancreatin used in Example 3 and 350 g of rapeseed extremely hardened oil of fine powder used in Example 1 were introduced into the stirring granulator used in Example 3 , and the temperature in the apparatus was 20 ° C. under a nitrogen gas atmosphere. The mixture was stirred for 10 minutes at a main shaft rotation speed of 500 rpm and a sub-shaft rotation speed of 1000 rpm. At this stage, the acidity of pancreatin remained slightly diluted. Furthermore, 50 g of the same rapeseed extremely hardened oil fine powder was added and stirring granulation was continued for 20 minutes, but no improvement was observed in the same state.
[0021]
Example 4
The ginkgo biloba extract powder 50 g used in Comparative Example A and the granulated sugar 350 g used in Comparative Example A were put into the stirring granulator used in Comparative Example 1 , and the spindle was rotated at an in-machine temperature of 20 ° C. and in a nitrogen gas atmosphere. The mixture was stirred at several 500 rpm and the countershaft rotation number 1000 rpm to obtain a primary granulated product. At this stage, ginkgo biloba extract powder was uniformly attached to the granulated sugar, and almost no ginkgo biloba extract powder was present. Further, while stirring the primary granulated product under the conditions of the main shaft rotation speed of 200 rpm and the counter shaft rotation speed of 500 rpm, 10 g of melted beef tallow oil (melting point: 48 ° C.) is slowly put into the fluidized bed over 5 minutes using a sprayer. And stirring was continued for 10 minutes. The average particle size of the granulated product at this time was 610 μm. Stirring is continued for about 10 minutes until the state settles, 90 g of fine powder of rapeseed extremely hardened oil used in Example 1 is added, and the mixture is stirred under conditions of a main shaft rotation speed of 700 rpm and a countershaft rotation speed of 1500 rpm. The desired granulated product was obtained by stirring for a minute.
[0022]
Comparative Example 5
Comparative Example was charged to the stirred granulator apparatus used in the ginkgo leaf extract powder 50g and comparing fine powder 350g of rapeseed extremely hardened oil used in Example 1 Example A used in A, internal temperature 20 ° C., a nitrogen gas atmosphere Below, stirring was performed at a main shaft rotation speed of 500 rpm and a sub-shaft rotation speed of 1000 rpm, followed by stirring for 10 minutes to obtain a desired granulated product. At this stage, the bitter taste of the ginkgo biloba extract powder was very strong. In addition, the fluidity was poor and was poor.
[0023]
The covering properties and fluidity of the granulated products produced in Examples 1 to 4 and Comparative Example A and Comparative Examples 1 to 5 were measured according to the following evaluation criteria, and the results are shown in Tables 1 and 2.
[Evaluation criteria for coverage]
○: The covering is complete and the smell or taste of the bulk powder is not felt.
(Triangle | delta): Coating is incomplete and the smell or taste of a raw powder is felt a little.
X: The coating is poor and the smell or taste of the bulk powder is felt strongly.
[Evaluation criteria for liquidity]
○: No dusting, smooth and fluidity.
Δ: Powdered but not fluid.
X: The fluidity is poor due to powdering or stickiness.
[0024]
[Table 1]

[0025]
[Table 2]

[0026]
From the results of Table 1, Examples 1 to 4 were completely covered with lipid, and the bitterness, blue odor, and sour taste were completely masked to improve the odor and the fluidity of the powder. Improvement, suppression of hygroscopicity, prevention of dusting. On the contrary, the results of Table 2 show that Comparative Example 1 is not completely coated, the bitterness of the ginkgo biloba extract cannot be suppressed and the fluidity is poor, and Comparative Example 2 is not completely coated and the fluidity of the powder. Was not improved and the number of bacteria decreased to 70% after one month. In Comparative Example 3, the blue odor of chlorella did not disappear and masking was insufficient. In Comparative Example 4, the coating was not complete, and the acidity of pancreatin was felt strongly although it was slightly diluted. In Comparative Example 5, the coating was not complete, the bitterness of the ginkgo biloba extract could not be suppressed, and the fluidity was poor.
[0027]
【The invention's effect】
The fine powder-containing granulated product obtained by the method of the present invention is extremely excellent in coverage and fluidity, and is effective for long-term storage and handling. Moreover, since no water or solvent is used in the method of the present invention, the quality of the fine powder material is extremely small, and it is a very useful method for granulating health foods and pharmaceuticals.

Claims (3)

健康食品原料、調味料原料、香辛料原料、生菌、酵素、アミノ酸、ペプタイド、ビタミン、有機酸、医療品原料等の微粉体状の素材を含有する造粒物の製造方法であって、
（Ａ）微粉体と粒径が微粉体の１０〜１０００倍で、比重が１．２〜１０００倍である粒状粉体とを、微粉体と粒状粉体の混合比を重量基準で、１：５〜１：１０として、混合撹拌することにより粒状粉体の表面にこの微粉体を付着せしめて造粒させた後、
脂質の使用量を微粉体に対して重量基準で１：１〜２：１として
（Ｂ）溶融状態にある脂質を噴霧することにより造粒物に脂質を被覆する微粉体含有造粒物の製造方法。 A method for producing a granulated material containing fine powder materials such as health food ingredients, seasoning ingredients, spice ingredients, viable bacteria, enzymes, amino acids, peptides, vitamins, organic acids, medical ingredients,
(A) A fine powder and a granular powder having a particle size of 10 to 1000 times that of the fine powder and a specific gravity of 1.2 to 1000 times, and the mixing ratio of the fine powder and the granular powder is 1: After 5: 1: 10, the fine powder was adhered to the surface of the granular powder by mixing and stirring and granulated,
(B) Manufacture of a granulated product containing fine powder in which the lipid is coated on the granulated product by spraying the lipid in a molten state with the amount of lipid used as a weight basis of 1: 1 to 2: 1 with respect to the fine powder Method. 健康食品原料、調味料原料、香辛料原料、生菌、酵素、アミノ酸、ペプタイド、ビタミン、有機酸、医療品原料等の微粉体状の素材を含有する造粒物の製造方法であって、
（Ａ）微粉体と粒径が微粉体の１０〜１０００倍で、比重が１．２〜１０００倍である粒状粉体とを、微粉体と粒状粉体の混合比を重量基準で、１：５〜１：１０として、混合撹拌することにより粒状粉体の表面にこの微粉体を付着せしめて造粒させた後、
脂質の使用量を微粉体に対して重量基準で１：１〜２：１として
（Ｂ）粒径が造粒物より粒径の小さい粉体である脂質と造粒物とを混合撹拌して脂質を造粒物に被覆する微粉体含有造粒物の製造方法。 A method for producing a granulated material containing fine powder materials such as health food ingredients, seasoning ingredients, spice ingredients, viable bacteria, enzymes, amino acids, peptides, vitamins, organic acids, medical ingredients,
(A) A fine powder and a granular powder having a particle size of 10 to 1000 times that of the fine powder and a specific gravity of 1.2 to 1000 times, and the mixing ratio of the fine powder and the granular powder is 1: After 5: 1: 10, the fine powder was adhered to the surface of the granular powder by mixing and stirring and granulated,
The amount of lipid used is 1: 1 to 2: 1 on a weight basis with respect to the fine powder.
(B) A method for producing a fine-powder-containing granulated product in which a lipid and a granulated product, which are powder having a particle size smaller than that of the granulated product, are mixed and stirred to coat the lipid with the granulated product. 健康食品原料、調味料原料、香辛料原料、生菌、酵素、アミノ酸、ペプタイド、ビタミン、有機酸、医療品原料等の微粉体状の素材を含有する造粒物の製造方法であって、A method for producing a granulated material containing fine powder materials such as health food raw materials, seasoning raw materials, spice raw materials, live bacteria, enzymes, amino acids, peptides, vitamins, organic acids, medical raw materials,
（Ａ）微粉体と粒径が微粉体の１０〜１０００倍で、比重が１．２〜１０００倍である粒状粉体とを、微粉体と粒状粉体の混合比を、重量基準で１：５〜１：１０として、混合撹拌することにより粒状粉体の表面にこの微粉体を付着せしめて造粒させた後、(A) A fine powder and a granular powder having a particle size of 10 to 1000 times that of the fine powder and a specific gravity of 1.2 to 1000 times, and the mixing ratio of the fine powder and the granular powder is 1: After 5: 1: 10, the fine powder was adhered to the surface of the granular powder by mixing and stirring and granulated,
脂質の使用量を微粉体に対して重量基準で１：１〜２：１としてThe amount of lipid used is 1: 1 to 2: 1 on a weight basis with respect to the fine powder.
（Ｂ）溶融状態にある脂質を噴霧することにより、造粒物に脂質を被覆し、(B) By spraying the lipid in the molten state, the granule is coated with the lipid,
（Ｃ）その被覆造粒物より粒径の小さい粉体である脂質とその被覆造粒物とを混合撹拌して脂質をさらに造粒物に被覆する微粉体含有造粒物の製造方法。(C) A method for producing a granulated product containing fine powder, in which a lipid having a particle size smaller than that of the coated granulated product and the coated granulated product are mixed and stirred to further coat the lipid with the granulated product.