JP5180880B2 - Salty seasoning and method for producing the same - Google Patents
Salty seasoning and method for producing the same Download PDFInfo
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- JP5180880B2 JP5180880B2 JP2009052891A JP2009052891A JP5180880B2 JP 5180880 B2 JP5180880 B2 JP 5180880B2 JP 2009052891 A JP2009052891 A JP 2009052891A JP 2009052891 A JP2009052891 A JP 2009052891A JP 5180880 B2 JP5180880 B2 JP 5180880B2
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- Prior art keywords
- sodium chloride
- potassium chloride
- chloride
- spray
- coating layer
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- 235000011194 food seasoning agent Nutrition 0.000 title claims description 25
- 238000004519 manufacturing process Methods 0.000 title claims description 13
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 claims description 225
- WCUXLLCKKVVCTQ-UHFFFAOYSA-M Potassium chloride Chemical compound [Cl-].[K+] WCUXLLCKKVVCTQ-UHFFFAOYSA-M 0.000 claims description 204
- 239000011780 sodium chloride Substances 0.000 claims description 111
- 235000011164 potassium chloride Nutrition 0.000 claims description 102
- 239000001103 potassium chloride Substances 0.000 claims description 102
- 239000007921 spray Substances 0.000 claims description 53
- 239000002245 particle Substances 0.000 claims description 51
- 239000010410 layer Substances 0.000 claims description 45
- 239000011247 coating layer Substances 0.000 claims description 42
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- 235000019643 salty taste Nutrition 0.000 claims description 10
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- 239000003795 chemical substances by application Substances 0.000 description 3
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Description
本発明は、従来の食塩に代わる塩味料およびその製造方法に関する。詳しくは、低ナトリウム塩及びその製造方法に関する。 The present invention relates to a salt flavoring agent replacing conventional salt and a method for producing the same. In detail, it is related with a low sodium salt and its manufacturing method.
従来からナトリウムを過剰摂取することによって、高血圧などの生活習慣病を招くことが知られている。また、ナトリウムはナトリウムイオンと塩素イオンが結合した食塩の形で摂取され、現在成人１人当たりの食塩摂取量は、約１２ｇ／ｄａｙである。しかし、近年における消費者の健康志向、厚生労働省の食塩摂取量１０ｇ／ｄａｙ未満の推奨及び食塩感受性の高い患者の事を考慮した食生活の改善が必要となってきている。食生活の改善方法としては、カリウムにナトリウムを排泄する作用がある塩化カリウムが昭和５７年に食品添加物に指定されてからは、塩化ナトリウムの一部を塩化カリウムに替えた低ナトリウム塩が多数開発されている。しかし、塩化カリウムは、独特のエグ味を有しているので、食品の味が損なわれるという課題がある。そのため、かかる課題の解決が望まれている。 Conventionally, it is known that excessive intake of sodium causes lifestyle-related diseases such as hypertension. Sodium is ingested in the form of sodium chloride combined with chloride ions, and the amount of sodium intake per adult is currently about 12 g / day. However, in recent years, it has become necessary to improve the dietary habits in consideration of consumer health, recommendations from the Ministry of Health, Labor and Welfare of less than 10 g / day of salt intake, and patients with high salt sensitivity. As a method for improving dietary habits, since potassium chloride, which has the effect of excreting sodium into potassium, was designated as a food additive in 1982, there are many low sodium salts in which some sodium chloride is replaced with potassium chloride. Has been developed. However, since potassium chloride has a unique taste, there is a problem that the taste of food is impaired. Therefore, the solution of such a problem is desired.
例えば、塩化カリウムのエグ味を抑制するために、クエン酸塩、コンブエキス、ポリ−γ−グルタミン酸等の成分を添加する方法が開示されている（特許文献１〜３）。しかし、どの添加剤も異味が添加され、本来の塩化ナトリウムとは異なる味となる。また、塩化ナトリウムと塩化カリウムの単なる混合物に各添加剤を添加又はコーティングしているだけなので、粒径比及び比重差により偏析が生じ、料理で使用する際には毎回異なる味を有する。特に、固形物として使用（ゆで卵にふりかけて食べる等）する際には、塩化ナトリウムと塩化カリウムと各添加剤が口の中で同時に溶解するので、先味及び後味において塩化カリウムのエグ味を抑制することはできない。 For example, in order to suppress the taste of potassium chloride, a method of adding components such as citrate, kombu extract, poly-γ-glutamic acid, etc. has been disclosed (Patent Documents 1 to 3). However, any additive has a different taste and has a different taste from the original sodium chloride. Moreover, since each additive is only added or coated to a simple mixture of sodium chloride and potassium chloride, segregation occurs due to the difference in particle size ratio and specific gravity, and each tastes different when used in cooking. In particular, when used as a solid (e.g., sprinkled on a boiled egg), sodium chloride, potassium chloride, and each additive dissolve simultaneously in the mouth. It cannot be suppressed.
また、塩化カリウムと溶解速度の速いフレーク塩との混合によって塩化カリウムのエグ味を抑制する方法が開示されている（特許文献４）。しかし、溶解速度の速いフレーク塩によって、塩味を強くすることは可能であるが、単に塩化ナトリウムと塩化カリウムを混合しただけあるため、上記と同様に先味及び後味において十分に塩化カリウムのエグ味は抑制できない。また、単なる混合物であるため、粒径比及び比重差により偏析が生じ、使用時において毎回異なる味を有する。 In addition, a method for suppressing the taste of potassium chloride by mixing potassium chloride with flake salt having a high dissolution rate is disclosed (Patent Document 4). However, it is possible to enhance the salty taste with flake salt having a high dissolution rate, but since sodium chloride and potassium chloride are simply mixed, the taste of potassium chloride is sufficient in the initial and aftertaste as above. Cannot be suppressed. Moreover, since it is a mere mixture, segregation occurs due to the particle size ratio and the specific gravity difference, and it has a different taste every time it is used.
更に、塩化カリウムと塩化ナトリウムを押出し造粒することにより、塩化カリウムの露出を抑え、塩化カリウムのエグ味を抑制する方法が開示されている（特許文献５）。しかし、造粒物の表面には、塩化カリウムが露出しているので、十分に塩化カリウムのエグ味を抑制できていない。 Furthermore, a method of suppressing the exposure of potassium chloride and suppressing the taste of potassium chloride by extruding and granulating potassium chloride and sodium chloride is disclosed (Patent Document 5). However, since potassium chloride is exposed on the surface of the granulated product, the taste of potassium chloride cannot be sufficiently suppressed.
また、塩化カリウムを胃溶性皮膜剤で薄膜コーティングした後に塩化ナトリウムでコーティングした三層構造により塩化カリウムのエグ味を抑制する方法が開示されている（特許文献６）。この方法は、塩化カリウムの表面を胃溶性皮膜でコーティングしているので、経口摂取においては、最外層の塩化ナトリウムだけを口の中で溶解させ、胃溶性皮膜剤でコーティングした塩化カリウムは口の中で溶出することなく飲み込んで胃で溶出させるＤＤＳ（ドラッグデリバリーシステム）製剤である。しかし、塩化ナトリウムが溶出した後は、口の中に固形物が残り違和感を感じる。更に、塩化ナトリウムは被覆層を形成することが難しいと共に、できたとしても被覆層が脆い。 In addition, a method of suppressing the taste of potassium chloride by a three-layer structure in which potassium chloride is thin-coated with a gastric film and then coated with sodium chloride is disclosed (Patent Document 6). In this method, since the surface of potassium chloride is coated with a gastric film, when taken orally, only the outermost sodium chloride is dissolved in the mouth, and the potassium chloride coated with the gastric film is in the mouth. It is a DDS (drug delivery system) formulation that is swallowed without eluting in the stomach and eluted in the stomach. However, after sodium chloride is eluted, solid matter remains in the mouth, and the user feels uncomfortable. Furthermore, it is difficult for sodium chloride to form a coating layer, and even if possible, the coating layer is brittle.
更に、塩化カリウムの表面を塩基性アミノ酸及び／又は塩基性ペプチドでコーティング（中間層被膜）した後に塩化ナトリウム及び糖類でコーティング（表層被膜）した三層構造により塩化カリウムのエグ味を抑制する方法が開示されている（特許文献７）。この方法では、糖類を用いてコーティングするので、塩化ナトリウムの被覆層を形成することは容易になるが、添加物による異味で本来の塩化ナトリウムとは異なる味となる。 Furthermore, there is a method for suppressing the taste of potassium chloride by a three-layer structure in which the surface of potassium chloride is coated with a basic amino acid and / or basic peptide (intermediate layer coating) and then coated with sodium chloride and sugar (surface coating). It is disclosed (Patent Document 7). In this method, since the saccharide is used for coating, it is easy to form a sodium chloride coating layer, but the taste is different from that of the original sodium chloride due to the additive taste.
上記のような理由から、食塩に近い味を呈する塩味料が望まれている。 For the reasons described above, a salty seasoning that has a taste close to that of salt is desired.
本発明の目的は、塩化ナトリウム及び塩化カリウムを含む低ナトリウム塩において、使用時及び保存時において塩化カリウムと塩化ナトリウムの含量均一性に優れており、塩化カリウムのエグ味を抑制する添加剤を添加しなくとも塩化カリウムのエグ味を感じない塩味料およびその製造方法を提供することにある。 The object of the present invention is to add an additive that suppresses the taste of potassium chloride in a low sodium salt containing sodium chloride and potassium chloride, which is excellent in content uniformity of potassium chloride and sodium chloride during use and storage. It is an object of the present invention to provide a salty seasoning that does not feel the taste of potassium chloride and a method for producing the same.
本発明者等は、上述した課題を解決するために、核粒子である塩化カリウムの表面を塩化ナトリウムの被覆層で覆うことによって、上記の課題が達成される事を見出した。 In order to solve the above-described problems, the present inventors have found that the above-described problems can be achieved by covering the surface of potassium chloride, which is a core particle, with a coating layer of sodium chloride.
即ち、本発明（１）は、核粒子である塩化カリウムの表面が塩化ナトリウムの被覆層で覆われ、該被覆層の表面における塩化ナトリウム結晶の個数平均径が１０〜１００μｍであることを特徴とする塩味料である。 That is, the present invention (1) is characterized in that the surface of potassium chloride as a core particle is covered with a coating layer of sodium chloride, and the number average diameter of sodium chloride crystals on the surface of the coating layer is 10 to 100 μm. It is a salty seasoning.
更に、本発明（２）は、該被覆層がにがりを含む、前記発明(１)記載の塩味料である。 Furthermore, the present invention (2) is the salty taste according to the invention (1), wherein the coating layer contains bittern.
また、本発明（３）は、塩化ナトリウムと塩化カリウムの重量比が９０：１０〜１０：９０である、前記発明（１）または（２）記載の塩味料である。 Further, the present invention (3) is the salty taste according to the invention (1) or (2), wherein the weight ratio of sodium chloride and potassium chloride is 90:10 to 10:90.
更に、本発明（４）は、前記発明（１）〜（３）のいずれか１つに記載の塩味料を含む、調味料および食品である。 Furthermore, this invention (4) is a seasoning and foodstuff containing the salty seasoning as described in any one of said invention (1)-(3).
また、本発明（５）は、下記の工程：
〔１〕塩化カリウム粒子に塩化ナトリウム水溶液をスプレーしながら乾燥造粒し、塩化ナトリウムを含む噴霧層を形成する工程；および
〔２〕過飽和の塩化ナトリウム水溶液を用いて塩化ナトリウムを結晶成長させることにより、塩化ナトリウムを含む晶析層を形成する工程
を含む、塩味料の製造方法
である。
The present invention (5) includes the following steps:
[1] A step of drying and granulating potassium chloride particles while spraying a sodium chloride aqueous solution to form a spray layer containing sodium chloride; and [2] crystal growth of sodium chloride using a supersaturated sodium chloride aqueous solution. A method for producing a salty seasoning, comprising a step of forming a crystallization layer containing sodium chloride.
更に、本発明（６）は、前記発明（５）記載の製造方法によって得られる、塩味料である。 Furthermore, this invention (6) is a salty taste obtained by the manufacturing method of the said invention (5).
本発明に係る塩味料は、核粒子である塩化カリウム表面を塩化ナトリウムの被覆層でコーティングした造粒物にすることによって、含量均一性が極めて良好（例えば、試験例５において、５ｇのサンプリングを４回行ったところほぼ均一な値を示した）であり、塩化カリウムのエグ味を感じない。 The salty seasoning according to the present invention is very good in content uniformity by forming a granulated product in which the surface of potassium chloride as a core particle is coated with a coating layer of sodium chloride (for example, in Test Example 5, sampling of 5 g is performed). It was almost uniform after 4 times) and did not feel the taste of potassium chloride.
また、本発明の製造方法によれば、従来のコーティング方法と比べて被覆層が強固な造粒物となり、造粒工程後の移送、乾燥、充填等で被覆層が剥離して微粉末が発生しないのでハンドリングが極めて優れた効果を奏する。 In addition, according to the production method of the present invention, the coating layer becomes a strong granulated product as compared with the conventional coating method, and the coating layer peels off by transfer, drying, filling, etc. after the granulation process, and fine powder is generated. Because it does not, handling has an excellent effect.
本発明に係る塩味料は、塩化ナトリウム及び塩化カリウムを必須成分として含むものである。但し、この必須成分以外のにがり、固結防止剤、添加物を含有していてもよい。 The salty seasoning according to the present invention contains sodium chloride and potassium chloride as essential components. However, it may contain bittern, anti-caking agent and additives other than the essential components.
本発明に係る塩味料の特徴は、核粒子である塩化カリウムの表面を塩化ナトリウムの被覆層で覆っていることである。 The feature of the salty seasoning according to the present invention is that the surface of potassium chloride which is a core particle is covered with a coating layer of sodium chloride.
先ず、本発明に係る核粒子に関して説明する。核粒子とは、造粒の際に核となる粒子のことをいう。また、該核粒子に使用する塩化カリウムは、特に限定されないが、例えば、通常市販されている食品添加物用の塩化カリウムや日本薬局方用の塩化カリウムで目的は十分達成できる。 First, the core particle according to the present invention will be described. A core particle means the particle | grains used as a nucleus in the case of granulation. The potassium chloride used for the core particles is not particularly limited. For example, potassium chloride for food additives or potassium chloride for Japanese pharmacopoeia which are usually commercially available can sufficiently achieve the object.
次に、被覆層に関して説明をする。被覆層とは、核粒子の表面をコーティングしている層をいい、核粒子の表面をコーティングすることによって、使用時及び保存時における含量均一性に優れた造粒物を調製することができる。また、該コーティングに使用する塩化ナトリウムは、特に限定されないが、例えば、イオン交換膜法、天日製塩、塩浜等の一般的な方法により得られ、通常市販されている塩化ナトリウムで目的を十分達成でき、にがり成分を含有していてもよい。 Next, the coating layer will be described. The coating layer refers to a layer that coats the surface of the core particles. By coating the surface of the core particles, a granulated product having excellent content uniformity during use and storage can be prepared. Further, the sodium chloride used for the coating is not particularly limited. For example, it is obtained by a general method such as an ion exchange membrane method, a salt made from the sun, or a salt beach, and the purpose can be sufficiently achieved by commercially available sodium chloride. And may contain a bittern component.
塩味の強さは塩化ナトリウム濃度（塩化ナトリウム含量）に依存するが、本発明による塩化カリウムの表面を塩化ナトリウムでコーティングした造粒物（例えば、図１又は図２）は、単なる混合により得られる塩化カリウムと塩化ナトリウムの混合物（例えば、図３）や、塩化カリウムと塩化ナトリウムの混合造粒物（例えば、押出し造粒や流動層造粒による凝集造粒物、図４）と比べて、先味において、塩化カリウムとの接触を抑制することができるため、塩化カリウムのエグ味を抑制できる上に、塩味を強く感じることができる。 Although the strength of saltiness depends on the sodium chloride concentration (sodium chloride content), the granulated product (for example, FIG. 1 or FIG. 2) in which the surface of potassium chloride according to the present invention is coated with sodium chloride is obtained by simple mixing. Compared with a mixture of potassium chloride and sodium chloride (for example, FIG. 3) and a mixture granulated product of potassium chloride and sodium chloride (for example, agglomerated granulated material by extrusion granulation or fluidized bed granulation, FIG. 4). In the taste, since contact with potassium chloride can be suppressed, the taste of potassium chloride can be suppressed and the salty taste can be strongly felt.
本発明に係る塩味料は、典型的には、顆粒及び／又は粉末である。そして、その平均粒子径は、約１２５〜１５５０μｍであることが好適である。また、塩味料の形態は、単粒子の核粒子の表面に被覆層が形成された単核コーティング（例えば、図１）であってもよいし、複数の核粒子が被覆層を介して結合した凝集造粒コーティング（例えば、図２）であってもよい。尚、本発明における平均粒子径の測定は、例えばロボットシフター（株式会社セイシン企業製；ＲＰＳ−８５ｃ）を用いて測定できる。 The salty taste according to the present invention is typically granules and / or powder. And it is suitable that the average particle diameter is about 125-1550 micrometers. In addition, the form of the salty seasoning may be a mononuclear coating (for example, FIG. 1) in which a coating layer is formed on the surface of a single particle core particle, or a plurality of core particles are bonded via the coating layer. It may be an agglomerated granulated coating (eg, FIG. 2). In addition, the measurement of the average particle diameter in this invention can be measured, for example using a robot shifter (the Seishin company make; RPS-85c).
本発明による塩味料における塩化ナトリウムと塩化カリウムの重量比は、好ましくは９０：１０〜１０：９０の範囲である。 The weight ratio of sodium chloride and potassium chloride in the salty seasoning according to the present invention is preferably in the range of 90:10 to 10:90.
次に本発明に係る塩味料の必須成分以外のにがり、固結防止剤、添加物について説明する。にがりとは、一般的に、海水からの製塩工程において副産物として分離されるものであり、カルシウム塩（塩化カリウム、硫酸カルシウム）、マグネシウム塩（塩化マグネシウム、硫酸マグネシウム）、カリウム塩（塩化カリウム、硫酸カリウム）、リン、鉄、亜鉛、マンガン等を含む液状物、その乾燥物、又は上記成分を人工的に配合することによって調製されたものである。 Next, the bittern, anti-caking agent and additives other than the essential components of the salty seasoning according to the present invention will be described. In general, bittern is separated as a by-product in the salt-making process from seawater, and calcium salt (potassium chloride, calcium sulfate), magnesium salt (magnesium chloride, magnesium sulfate), potassium salt (potassium chloride, sulfuric acid). Potassium), phosphorus, iron, zinc, manganese and the like, dried products thereof, or those prepared by artificially blending the above components.
固結防止剤とは、湿度の影響によって塩が固結して塊になることを防止する添加剤であり、その成分としては、炭酸カルシウム、炭酸マグネシウム、二酸化ケイ素、でん粉、クエン酸鉄アンモニウムが挙げられる。 Anti-caking agent is an additive that prevents salt from caking due to the influence of humidity, and its components include calcium carbonate, magnesium carbonate, silicon dioxide, starch and ammonium iron citrate. Can be mentioned.
添加剤とは、第一次機能（栄養機能）、第三次機能（健康性機能・生体調節機能）を有した食品のことである。つまり、一次機能とは、生命現象を営むために必要不可欠なエネルギー源や生体構成成分の補給に必要な食品成分（栄養素）としての機能であり、成分としては、糖質、脂質、タンパク質、ビタミンを挙げることができる。また、三次機能とは、体調を整える機能で、病気の予防や健康の維持増進に果す機能であり、成分としては、高血圧予防、糖尿病予防、高脂血症予防、動脈硬化予防、肥満予防、老化予防、抗酸化作用、抗アレルギー作用等を有する成分であれば特に限定されないが、好適には、天然ポリフェノール類、タンパク質、アミノ酸類、糖類、不飽和脂肪酸、テンペン類、オクタコサノール、カプサイシン、セラミド、レシチン、ノビレチン、タンゲレチン、モナコリン、スルフォラファンを挙げることができる。必須成分以外のにがり、固結防止剤、添加物については、単独で乃至は複数組み合わせて用いてもよい。更に、必須成分以外のにがり、添加物については、被覆層中に存在させても、層構造の最外層に存在させても、又は単に混合してもよい。 An additive is a food having a primary function (nutrient function) and a tertiary function (health function / biological regulation function). In other words, the primary function is a function as a food ingredient (nutrient) necessary for supplementing vital constituents and energy sources that are indispensable for carrying out life phenomena, including sugars, lipids, proteins, and vitamins. Can be mentioned. Tertiary function is a function to improve physical condition, and is a function to prevent disease and maintain and promote health. As ingredients, high blood pressure prevention, diabetes prevention, hyperlipidemia prevention, arteriosclerosis prevention, obesity prevention, It is not particularly limited as long as it is a component having aging prevention, antioxidant action, antiallergic action, etc., but preferably natural polyphenols, proteins, amino acids, saccharides, unsaturated fatty acids, tempens, octacosanol, capsaicin, ceramide, Examples include lecithin, nobiletin, tangeretin, monacolin and sulforaphane. Bitterns, anti-caking agents and additives other than essential components may be used alone or in combination. Furthermore, bitterns and additives other than essential components may be present in the coating layer, in the outermost layer of the layer structure, or simply mixed.
次に、本発明に係る塩味料の使用方法につき説明する。本発明に係る塩味料は、食品以外にも、化粧品として用いることができる。ここで、化粧品とは、トイレタリー（例えば、石鹸、歯磨き粉、シャンプー、リンス、シェービングフォーム、口中清涼剤、制汗剤、エステティック用品）及びコスメティック（例えば、洗顔石鹸、化粧水、栄養クリーム、コールドクリーム、乳液、パック等の基礎化粧品、ファンデーション、口紅、頬紅、マスカラ、アイシャドウ、眉墨、マニキュア等の仕上げ化粧品、男性用化粧品、ボディ化粧品、薬用化粧品等の特殊用途化粧品、香水、オーデコロン等のフレグランス、ヘアートリートメント、ポマード、ヘアークリーム、シャンプー、リンス等の頭髪用化粧品、エステティック用品）等を意味する。 Next, the method for using the salty seasoning according to the present invention will be described. The salty seasoning according to the present invention can be used as cosmetics in addition to food. Here, cosmetics include toiletries (for example, soap, toothpaste, shampoo, rinse, shaving foam, mouth freshener, antiperspirant, aesthetic supplies) and cosmetics (for example, facial soap, lotion, nutritional cream, cold cream). Basic cosmetics such as emulsions, packs, foundations, lipsticks, blushers, mascara, eyeshadows, eyebrows, manicures and other finished cosmetics, male cosmetics, body cosmetics, special cosmetics such as medicinal cosmetics, perfumes, eau de cologne fragrances, Hair treatment, pomade, hair cream, shampoo, rinse, etc.
本発明に係る塩味料は、そのまま用いてもよいし、健康食品の加工用や健康食塩として、日常的な食卓塩（例えば、低ナトリウム塩、ゴマ塩、塩胡椒、グルタミン酸ナトリウムを含有した味塩）として使用してもよい。さらには、調味料（例えば、醤油、ソース、ドレッシング、マヨネーズ、味噌）、調味食品（例えば、ふりかけ、インスタント味噌汁、インスタントスープ、レトルト惣菜）、調理済食品（例えば、冷凍食品）、ステープル（例えば、シリアル、パン、即席めん、スナックめん）、農産加工品（例えば、漬物）、水産加工品（例えば、ツナ缶詰、魚介類缶詰、魚肉ハム・ソーセージ、佃煮、魚類の干物）、畜産加工品（例えば、ソーセージ類、ハム類）、乳油製品（例えば、バター、マーガリン、チーズ）、菓子（例えば、スナック菓子）、果実飲料（例えば、野菜飲料）などにおける添加物として使用することも可能である。 The salty seasoning according to the present invention may be used as it is, or as a table salt (eg, low sodium salt, sesame salt, salt and pepper, sodium glutamate salt for daily use as health food processing or health salt. ). Furthermore, seasonings (eg, soy sauce, sauce, dressing, mayonnaise, miso), seasoned foods (eg, sprinkles, instant miso soup, instant soup, retort beet), cooked foods (eg, frozen foods), staples (eg, Cereal, bread, instant noodles, snack noodles), processed agricultural products (eg pickles), processed fishery products (eg canned tuna, canned seafood, fish ham / sausage, boiled fish, dried fish), processed livestock products (eg , Sausages, hams), milk oil products (eg, butter, margarine, cheese), confectionery (eg, snack confectionery), fruit beverages (eg, vegetable beverages), and the like.
次に、本発明の塩味料の製造方法を説明する。詳しくは、塩化カリウムの表面を塩化ナトリウムでコーティングする方法であり、より詳しくは、以下の通りである。 Next, the manufacturing method of the salty seasoning of this invention is demonstrated. Specifically, this is a method of coating the surface of potassium chloride with sodium chloride, and more specifically, as follows.
本発明の塩味料の製造方法は、下記工程：
〔１〕塩化カリウム粒子に塩化ナトリウム水溶液をスプレーしながら乾燥造粒し、塩化ナトリウムを含む噴霧層を形成する工程；および
〔２〕過飽和の塩化ナトリウム水溶液を用いて塩化ナトリウムを結晶成長させることにより、塩化ナトリウムを含む晶析層を形成する工程
を含む。したがって、本発明の被覆層は、噴霧層と晶析層を有する。
The method for producing the salty taste of the present invention includes the following steps
[1] A step of drying and granulating potassium chloride particles while spraying a sodium chloride aqueous solution to form a spray layer containing sodium chloride; and [2] crystal growth of sodium chloride using a supersaturated sodium chloride aqueous solution. And a step of forming a crystallization layer containing sodium chloride. Therefore, the coating layer of the present invention has a spray layer and a crystallization layer.
＜工程〔１〕＞
本発明に係る工程〔１〕の塩化ナトリウムを含む噴霧層を形成する方法について説明する。塩化ナトリウムを含む噴霧層の形成は、遠心流動コーティング造粒装置（例えば、高速攪拌造粒装置）、流動層コーティング装置やパンコーティング装置等を用いて実施することができ、好ましくは、流動層コーティング装置を用いる。
<Process [1]>
A method for forming a spray layer containing sodium chloride in step [1] according to the present invention will be described. The formation of the sprayed layer containing sodium chloride can be carried out using a centrifugal fluidized coating granulator (for example, a high-speed agitation granulator), a fluidized bed coating device, a pan coating device, or the like, preferably fluidized bed coating. Use the device.
流動層コーティング装置は、底部の通気構造から、流動層コーティング装置（一般的なトップスプレー式流動層やサイドスプレー式流動層）、噴流層コーティング装置（ドラフト管付）、攪拌転動流動層（転動流動層型、攪拌転動流動層型、回転円板付流動層型）コーティング装置の三つに分類される。各装置は、調製しようとする造粒物によって適宜選定することができる。例えば、単粒子コーティングであれば、噴流層コーティング装置を使用することが好ましい。 The fluidized bed coating device has a fluidized bed coating device (general top spray type fluidized bed and side spray type fluidized bed), spouted bed coating device (with a draft tube), stirring and rolling fluidized bed (rolling layer) from the bottom ventilation structure. The fluidized bed type, the stirring rolling fluidized bed type, and the fluidized bed type with rotating disk) are classified into three types. Each apparatus can be appropriately selected depending on the granulated product to be prepared. For example, in the case of single particle coating, it is preferable to use a spouted bed coating apparatus.
本発明に係る工程〔１〕の塩化カリウム粒子とは、固体状態の塩化カリウムのことであり、平均粒子径は特に限定されるものではないが、ハンドリング面を考慮すると、平均粒子径は１００〜１５００μｍが好ましく、１００〜７００μｍがより好ましく、２００〜７００μｍがさらに好ましい。尚、塩化カリウムの平均粒子径が小さいほど、口中において塩化カリウムの溶解速度が速くなるので塩化カリウムのエグ味を抑制できると推測する。 The potassium chloride particles in the step [1] according to the present invention are solid potassium chloride, and the average particle diameter is not particularly limited. However, in consideration of the handling surface, the average particle diameter is from 100 to 100. 1500 μm is preferable, 100 to 700 μm is more preferable, and 200 to 700 μm is more preferable. In addition, since the dissolution rate of potassium chloride in a mouth becomes quick, so that the average particle diameter of potassium chloride is small, it is estimated that the taste of potassium chloride can be suppressed.
本発明に係る工程〔１〕の塩化ナトリウム水溶液の濃度は、２０〜２８重量％が好ましく、２５〜２７重量％がより好ましい。該水溶液の濃度が低くなると、水溶液の量が多くなるため塩化ナトリウムの噴霧層を形成する時間が長くなる。また、２８重量％以上より高いと塩化ナトリウムが１００℃では溶解しなくなり懸濁液となる。 The concentration of the sodium chloride aqueous solution in step [1] according to the present invention is preferably 20 to 28% by weight, and more preferably 25 to 27% by weight. When the concentration of the aqueous solution is lowered, the amount of the aqueous solution is increased, so that the time for forming the spray layer of sodium chloride is increased. On the other hand, when the content is higher than 28% by weight, sodium chloride does not dissolve at 100 ° C. and becomes a suspension.
工程〔１〕で形成する噴霧層の厚みは、２５μｍ以上が好ましく、２５〜５０μｍがより好ましい。該噴霧層の厚みが２５μｍ未満になると、被覆が不完全であるため、工程〔２〕の操作により噴霧層が剥離・脱落して核粒子の塩化カリウムの溶出率が２０％以上となり、含量均一性や生産コストに問題が生じる。他方、噴霧層の厚みが５０μｍ以上になると、核粒子の塩化カリウムの溶出率を１０％以下に抑制できるが、工程〔１〕における塩化ナトリウムを含む噴霧層を形成する時間が長くなり、やはり生産コストが問題となる。噴霧層とは、工程〔１〕で得られた造粒物の被覆層を意味する。ここで、溶出率とは、工程〔２〕において、塩化カリウムが結晶成長中に溶出する割合のことである。尚、噴霧層の厚みは以下の式より算出する。
噴霧層の厚み［μｍ］＝［｛（Ｘ３×Ｚ×Ｐ／Ｙ×Ｑ）＋Ｘ３｝１／３−Ｘ］／２
Ｘ：ＫＣｌ平均粒子径［μｍ］
Ｙ：工程〔１〕で使用するＫＣｌの重量［ｇ］
Ｚ：ＫＣｌ比重（１．９８）［ｇ／ｃｍ３］
Ｐ：噴霧層中のＮａＣｌ重量［ｇ］
Ｑ：ＮａＣｌ比重（２．１６）［ｇ／ｃｍ３］
尚、Ｐはイオンクロマトグラフで測定した結果である。
The thickness of the spray layer formed in the step [1] is preferably 25 μm or more, and more preferably 25 to 50 μm. When the thickness of the spray layer is less than 25 μm, the coating is incomplete, so that the spray layer is peeled off and dropped by the operation of step [2], and the elution rate of potassium chloride in the core particles becomes 20% or more, and the content is uniform. Problems arise in productivity and production costs. On the other hand, when the thickness of the spray layer is 50 μm or more, the elution rate of potassium chloride in the core particles can be suppressed to 10% or less, but the time for forming the spray layer containing sodium chloride in the step [1] becomes longer, which is also produced. Cost becomes a problem. A spray layer means the coating layer of the granulated material obtained at process [1]. Here, the elution rate is the rate at which potassium chloride is eluted during crystal growth in step [2]. The spray layer thickness is calculated from the following equation.
Spray layer thickness [μm] = [{(X 3 × Z × P / Y × Q) + X 3 } 1/3 −X] / 2
X: KCl average particle diameter [μm]
Y: Weight of KCl used in step [1] [g]
Z: KCl specific gravity (1.98) [g / cm 3 ]
P: NaCl weight in spray layer [g]
Q: NaCl specific gravity (2.16) [g / cm 3 ]
In addition, P is a result measured by an ion chromatograph.
本発明に係る工程〔１〕の運転条件に関して説明する。先ず造粒温度及び乾燥温度は、２５〜２００℃が好ましく、６０〜１００℃がより好ましい。温度が低くなると、コーティング時間が長くなり、１００℃以上になると、排出等のハンドリングが困難となる。 The operating conditions of the process [1] according to the present invention will be described. First, the granulation temperature and the drying temperature are preferably 25 to 200 ° C, more preferably 60 to 100 ° C. When the temperature is low, the coating time is long, and when it is 100 ° C. or higher, handling such as discharge becomes difficult.
次に、風量に関しては、一般的条件の範囲内で目的は充分達成される。ただし、風量が少ないと核粒子同士が凝集しやすくなる。また、多くなると水溶液中の成分がスプレードライ現象を生じやすくなり微粉末が増える。更に、各粒子が受ける衝撃が大きくなるため微粉末が生じやすくなる。 Next, with regard to the air volume, the objective is sufficiently achieved within the range of general conditions. However, if the air volume is small, the core particles tend to aggregate. In addition, when the amount increases, the components in the aqueous solution are liable to cause a spray-drying phenomenon and the fine powder increases. Furthermore, since the impact received by each particle is increased, fine powder is likely to be generated.
＜工程〔２〕＞
本発明に係る工程〔２〕は、工程〔１〕で得られる造粒物の表面に存在する塩化ナトリウム粒子を核として、過飽和の塩化ナトリウム水溶液から塩化ナトリウムの結晶を成長させて晶析層を形成する工程である。大量生産スケールにおいては、工程〔１〕と工程〔２〕で被覆を行うことにより、工程〔１〕のみで被覆を行うよりも短時間で被覆層を形成できる。また、塩化ナトリウムの結晶を成長させることにより、移送、乾燥、充填等で被覆層が剥離して微粉末が発生しない強固な被覆状態となる。このような結晶成長をさせる装置としては、一般的な晶析装置が使用でき、例えば、クリスタル−オスロ型晶析装置、逆円錐型晶析装置、ＤＴＢ型晶析装置、ＤＰ型晶析装置を用いてもよいが、好ましくは、図５の逆循環流動式晶析装置（以下、単に晶析装置ともいう）である。
<Process [2]>
In the step [2] according to the present invention, a crystallization layer is formed by growing sodium chloride crystals from a supersaturated sodium chloride aqueous solution using the sodium chloride particles present on the surface of the granulated product obtained in the step [1] as a nucleus. It is a process of forming. In the mass production scale, the coating layer can be formed in a shorter time by performing the coating in the steps [1] and [2] than in the coating only in the step [1]. Further, by growing crystals of sodium chloride, the coating layer is peeled off by transfer, drying, filling, etc., and a strong coating state is produced in which fine powder is not generated. As a crystal growth apparatus, a general crystallizer can be used. For example, a crystal-Oslo crystallizer, an inverted cone crystallizer, a DTB crystallizer, and a DP crystallizer can be used. Although it may be used, the reverse circulation flow crystallizer (hereinafter also simply referred to as a crystallizer) shown in FIG. 5 is preferable.
本発明に係る工程〔２〕の飽和溶液に関して説明する。溶質は工程〔１〕と同じく塩化ナトリウムであり、図５の晶析装置を使用する場合は、槽ａにおいて攪拌モーターｂにより飽和溶液が調製される。また、過剰量の溶質が槽ａにあることが好ましい。槽ａにおける飽和水溶液の温度は、２０〜１２０℃が好ましい。 The saturated solution in step [2] according to the present invention will be described. The solute is sodium chloride as in step [1], and when the crystallizer of FIG. 5 is used, a saturated solution is prepared by the stirring motor b in the tank a. Moreover, it is preferable that the excess amount of solute exists in the tank a. The temperature of the saturated aqueous solution in the tank a is preferably 20 to 120 ° C.
本発明に係る工程〔２〕の過飽和溶液に関して説明する。図５の晶析装置を使用する場合は、槽ａで調製された溶液がポンプｃを介して冷却器ｄで冷却されて過飽和溶液が調製される。過飽和溶液の過飽和度の値が大きいほど結晶の成長速度は大きくなる。ここで、過飽和度とは、例えば、９０℃で飽和にした塩化ナトリウム飽和濃度とそれを８０℃に冷却した時の塩化ナトリウム飽和濃度の差である。 The supersaturated solution in step [2] according to the present invention will be described. When the crystallizer of FIG. 5 is used, the solution prepared in the tank a is cooled by the cooler d via the pump c to prepare a supersaturated solution. The larger the supersaturation value of the supersaturated solution, the higher the crystal growth rate. Here, the degree of supersaturation is, for example, the difference between the saturated sodium chloride concentration saturated at 90 ° C. and the saturated sodium chloride concentration when it is cooled to 80 ° C.
本発明に係る工程〔２〕の晶析条件に関して説明する。先ず、晶析の温度は１０〜５０℃が好ましい。１０℃以下になると、結晶成長速度が小さくなり、核粒子の塩化カリウムの溶出率が高くなる。ポンプの流量はカラムから造粒物が溢流しない程度が好ましいが、流動状態が激しいと結晶が破砕してしまうので、穏やかな流動状態が好ましい。 The crystallization conditions in the step [2] according to the present invention will be described. First, the crystallization temperature is preferably 10 to 50 ° C. When it becomes 10 degrees C or less, the crystal growth rate will become small and the elution rate of the potassium chloride of a core particle will become high. The flow rate of the pump is preferably such that the granulated material does not overflow from the column, but since the crystals are crushed if the flow state is intense, a gentle flow state is preferable.
尚、工程〔２〕で得られた造粒物を乾燥するタイミングについては特に限定しないが、工程〔２〕の直後に乾燥することが好ましい。また、乾燥で使用する乾燥装置としては特に規定しないが、流動層乾燥機が好適である。操作条件は、通常乾燥する一般的条件の範囲内で目的は充分達成される。 In addition, although it does not specifically limit about the timing which drys the granulated material obtained at process [2], It is preferable to dry immediately after process [2]. Moreover, although it does not prescribe | regulate especially as a drying apparatus used by drying, a fluidized bed dryer is suitable. The operating conditions are sufficiently achieved within the general conditions of normal drying.
工程〔２〕後に得られる造粒物の塩化ナトリウム被覆層の量は、工程〔１〕で得られた噴霧層の量と工程〔２〕で得られた晶析層の量の総和となり、塩化ナトリウムと塩化カリウムの重量比が９０：１０〜１０：９０の範囲であればよい。 The amount of the sodium chloride coating layer of the granulated product obtained after step [2] is the sum of the amount of spray layer obtained in step [1] and the amount of crystallization layer obtained in step [2]. The weight ratio of sodium and potassium chloride may be in the range of 90:10 to 10:90.
また、工程〔２〕後に得られる造粒物の被覆層表面における塩化ナトリウム結晶の個数平均径は、１０〜１００μｍであることが好ましい。従来の方法（流動層造粒等）では、造粒物表面の粒子の個数平均径が８μｍ以下となるので、口内での溶解速度が速く非常に塩辛い味となる。しかし、本発明では、得られる造粒物の被覆層表面の結晶は個数平均径が大きいので、口内での溶解速度が遅くなり本来の塩の味に近くなる。なお、本発明による塩化ナトリウムの結晶成長には成長限界があり、その限界値は１００μｍ程度である。従来の被覆層を形成する造粒方法としては、噴霧溶液を核粒子に対して噴霧する方法（流動層造粒）があるが、噴霧溶液を微小液滴として核粒子に付着させて被覆層を形成するので、被覆層表面の塩化ナトリウムを個数平均径が１０μｍ以上の結晶とすることは困難である。さらに、他の従来の方法としては、攪拌転動流動層や表面改質装置に塩化カリウムと塩化ナトリウムを仕込み、水を噴霧しながら塩化カリウムの表面を塩化ナトリウムで被覆する方法もあるが、この方法では核粒子と被覆層粒子の平均粒子径の比率を１０：１にするためには、例えば平均粒子径１００μｍの塩化カリウムを使用する場合、平均粒子径１０μｍの塩化ナトリウムが必要であり、塩化ナトリウムを粉砕して使用しなければならず、本発明のように球から立方形のような結晶にはならない。また、塩化ナトリウムの平均粒子径が１００μｍ以下の場合、塩化ナトリウムが凝集しやすく、造粒時のハンドリングが問題である。 Moreover, it is preferable that the number average diameter of the sodium chloride crystal | crystallization in the coating layer surface of the granulated material obtained after process [2] is 10-100 micrometers. In the conventional method (fluidized bed granulation or the like), the number average diameter of particles on the surface of the granulated product is 8 μm or less. However, in the present invention, the crystals on the surface of the coating layer of the resulting granulated product have a large number average diameter, so that the dissolution rate in the mouth becomes slow and the taste of the original salt is approached. The crystal growth of sodium chloride according to the present invention has a growth limit, which is about 100 μm. As a conventional granulation method for forming a coating layer, there is a method in which a spray solution is sprayed onto the core particles (fluidized bed granulation), but the coating layer is formed by attaching the spray solution to the core particles as fine droplets. Therefore, it is difficult to form sodium chloride on the surface of the coating layer into crystals having a number average diameter of 10 μm or more. Furthermore, as another conventional method, there is a method in which potassium chloride and sodium chloride are charged into a stirring rolling fluidized bed or a surface reformer, and the surface of potassium chloride is coated with sodium chloride while spraying water. In the method, in order to make the ratio of the average particle diameter of the core particles and the coating layer particles 10: 1, for example, when potassium chloride having an average particle diameter of 100 μm is used, sodium chloride having an average particle diameter of 10 μm is required. Sodium must be ground and used, and it does not become a sphere-like crystal like the present invention. Moreover, when the average particle diameter of sodium chloride is 100 micrometers or less, sodium chloride tends to aggregate, and handling at the time of granulation is a problem.
本発明に係る個数平均径とは、走査型電子顕微鏡で倍率１０００倍にて被覆層表面における塩化ナトリウム結晶を観察後、Ｆｅｒｅｔ径を測定し、以下の式より算出した値である。
個数平均径［μｍ］＝Σ（ｎｄ）／Σｎ
ｎ［個］：ある粒子径を有する粒子の個数
ｄ［μｍ］：ある粒子の粒子径
以下に本発明の実施例を示して、本発明を更に具体的に説明する。
The number average diameter according to the present invention is a value calculated from the following formula by measuring the Feret diameter after observing sodium chloride crystals on the surface of the coating layer at a magnification of 1000 with a scanning electron microscope.
Number average diameter [μm] = Σ (nd) / Σn
n [number]: number of particles having a certain particle diameter d [μm]: particle diameter of a certain particle The present invention will be described more specifically with reference to examples of the present invention.
工程〔１〕
塩化ナトリウム（ナイカイ塩業株式会社製；ナイカイ食塩 ＮａＣｌ純度９９．０％以上）３００ｇを精製水９００ｇに溶解して２５重量％水溶液とした。トップスプレー式流動層造粒装置（フロイント産業株式会社製；ＦＬ−ＬＡＢＯ）に、核粒子として塩化カリウム（マナック株式会社製；日本薬局方塩化カリウム）２００ｇ（平均粒子径５３１μｍ；以下、平均粒子径の測定値は、株式会社セイシン企業製のロボットシフターＲＰＳ８５ｃによる）を投入し、給気温度９０℃、風量０．４ｍ３／ｍｉｎ、スプレー圧力０．２ＭＰａ、スプレー流量６０ＮＬ／ｍｉｎの条件下で、前記水溶液を２．３ｇ／ｍｉｎの噴霧速度で５．４ｈｒ噴霧しながら乾燥した。造粒後、目開き１８０μｍのＪＩＳ標準篩（内径φ２００ｍｍ；深さ４５ｍｍ）を用いてスプレードライした粒子を分級した後、イオンクロマトグラフの測定（試験例４の測定方法）により噴霧層中の塩化ナトリウムの重量を測定した結果、１５４．４ｇ（塩化カリウムの仕込み量を２００ｇとして換算）であった。噴霧層の厚みは、５１．８５μｍ（噴霧層の厚み［μｍ］＝［｛（５３１３×１．９８×１５４．４／２００×２．１６）＋５３１３｝１／３−５３１］／２）であった。
工程〔２〕
図５に示される逆循環流動式晶析装置を使用した。１０００ｍＬ四つ口フラスコ（槽ａ）に塩化ナトリウム（ナイカイ塩業株式会社製；ナイカイ食塩 ＮａＣｌ純度９９．０％以上）３８０．５ｇと精製水１０００ｇを仕込んで４５℃に設定したオイルバスで飽和溶液を調製した。次に、晶析槽ｅ（入口口径：５ｍｍ；出口口径：３５ｍｍ；高さ：１６５ｍｍの円筒形で下部が円錐型）に工程〔１〕で得られた造粒物２０ｇを仕込んだ後、冷却器ｄに１８〜２０℃の冷水を循環させると共に、オイルバスの温度を１０５℃に設定して１２０〜２００ｍＬ／ｍｉｎの速度で槽ａの飽和溶液をポンプｃを介して冷却器ｄで冷却して過飽和溶液とし、晶析槽ｅの下部に供給し、晶析槽ｅから溢流した溶液は槽ａに循環させた。この時の槽ａの温度は６０〜７０℃であり、槽ａに戻ってくる水温は冷却器ｄによる熱交換および放熱を伴って１８〜２０℃であった。尚、槽ｅの温度は、槽ａに戻ってくる水溶液の温度と同程度であると推測する。また、上記条件で４ｍｉｎ運転を行った後、ヌッチェ濾過をし、８０℃で乾燥した。得られた造粒物を構成する塩化ナトリウムと塩化カリウムの重量比は、イオンクロマトグラフによる測定値（試験例４の測定方法）より約1：1であった。
Process [1]
300 g of sodium chloride (manufactured by Naikai Shigyo Co., Ltd .; Naikai NaCl NaCl purity of 99.0% or more) was dissolved in 900 g of purified water to obtain a 25 wt% aqueous solution. In a top spray fluidized bed granulator (Freund Sangyo Co., Ltd .; FL-LABO), 200 g of potassium chloride (Manac Co., Ltd .; Japanese Pharmacopoeia Potassium Chloride) as core particles (average particle size 531 μm; hereinafter, average particle size) Is measured by a robot shifter RPS85c manufactured by Seishin Co., Ltd.) under the conditions of an air supply temperature of 90 ° C., an air volume of 0.4 m 3 / min, a spray pressure of 0.2 MPa, and a spray flow rate of 60 NL / min. The aqueous solution was dried while spraying at a spray rate of 2.3 g / min for 5.4 hours. After granulation, the spray-dried particles are classified using a JIS standard sieve (inner diameter φ200 mm; depth 45 mm) with an opening of 180 μm, and then the chlorination in the spray layer is measured by ion chromatography (measurement method of Test Example 4). As a result of measuring the weight of sodium, it was 154.4 g (converted with the amount of potassium chloride charged as 200 g). The thickness of the spray layer is 51.85 μm (the thickness of the spray layer [μm] = [{(531 3 × 1.98 × 154.4 / 200 × 2.16) +531 3 } 1/3 −531] / 2) Met.
Process [2]
The reverse circulation flow crystallizer shown in FIG. 5 was used. A saturated solution in an oil bath set at 45 ° C. with 380.5 g of sodium chloride (manufactured by Naikai Shigyo Co., Ltd .; Naikai NaCl NaCl purity 99.0% or more) and 1000 g of purified water in a 1000 mL four-necked flask (tank a) Was prepared. Next, 20 g of the granulated product obtained in the step [1] was charged in the crystallization tank e (inlet port diameter: 5 mm; outlet port diameter: 35 mm; height: 165 mm, conical at the bottom), and then cooled. While circulating cold water of 18-20 ° C. in the vessel d, the temperature of the oil bath is set at 105 ° C., and the saturated solution in the tank a is cooled by the cooler d via the pump c at a rate of 120-200 mL / min. A supersaturated solution was supplied to the lower part of the crystallization tank e, and the solution overflowed from the crystallization tank e was circulated to the tank a. The temperature of the tank a at this time was 60-70 degreeC, and the water temperature which returns to the tank a was 18-20 degreeC accompanying the heat exchange and heat dissipation by the cooler d. The temperature of the tank e is estimated to be approximately the same as the temperature of the aqueous solution returning to the tank a. Moreover, after operating for 4 minutes on the said conditions, Nutsche filtration was carried out and it dried at 80 degreeC. The weight ratio of sodium chloride and potassium chloride constituting the obtained granulated product was about 1: 1 from the measured value by ion chromatography (measurement method of Test Example 4).
工程〔１〕
塩化ナトリウム（ナイカイ塩業株式会社製；ナイカイ食塩 ＮａＣｌ純度９９．０％以上）３００ｇを精製水９００ｇに溶解して２５重量％水溶液とした。トップスプレー式流動層造粒装置（フロイント産業株式会社製；ＦＬ−ＬＡＢＯ）に、核粒子として塩化カリウム（マナック株式会社製；日本薬局方塩化カリウム）２００ｇ（平均粒子径３０９μｍ）を投入し、給気温度９０℃、風量０．４ｍ３／ｍｉｎ、スプレー圧力０．２ＭＰａ、スプレー流量６０ＮＬ／ｍｉｎの条件下で、前記水溶液を２．３ｇ／ｍｉｎの噴霧速度で５．２ｈｒ噴霧しながら乾燥した。造粒後、目開き１８０μｍのＪＩＳ標準篩（内径φ２００ｍｍ；深さ４５ｍｍ）を用いてスプレードライした粒子を分級した後、イオンクロマトグラフの測定（試験例４の測定方法）により噴霧層中の塩化ナトリウムの重量を測定した結果、１５０．８ｇ（塩化カリウムの仕込み量を２００ｇとして換算）であった。噴霧層の厚みは、２９．５７μｍ（噴霧層の厚み［μｍ］＝［｛（３０９３×１．９８×１５０．８／２００×２．１６）＋３０９３｝１／３−３０９］／２）であった。
工程〔２〕
実施例１の工程〔２〕と同様の操作を行った。尚、運転時間は３ｍｉｎとした。また、得られた造粒物を構成する塩化ナトリウムと塩化カリウムの重量比は、イオンクロマトグラフによる測定値（試験例４の測定方法）より約１：１であった。
Process [1]
300 g of sodium chloride (manufactured by Naikai Shigyo Co., Ltd .; Naikai NaCl NaCl purity of 99.0% or more) was dissolved in 900 g of purified water to obtain a 25 wt% aqueous solution. 200 g of potassium chloride (Manac Co., Ltd .; Japanese Pharmacopoeia Potassium Chloride) 200 g (average particle size 309 μm) as the core particles is fed into a top spray fluidized bed granulator (Freund Sangyo Co., Ltd .; FL-LABO). The aqueous solution was dried while spraying for 5.2 hours at a spray rate of 2.3 g / min under the conditions of an air temperature of 90 ° C., an air volume of 0.4 m 3 / min, a spray pressure of 0.2 MPa, and a spray flow rate of 60 NL / min. After granulation, the spray-dried particles are classified using a JIS standard sieve (inner diameter φ200 mm; depth 45 mm) with an opening of 180 μm, and then the chlorination in the spray layer is measured by ion chromatography (measurement method of Test Example 4). As a result of measuring the weight of sodium, it was 150.8 g (converted with the amount of potassium chloride charged as 200 g). The thickness of the spray layer is 29.57 μm (the thickness of the spray layer [μm] = [{(309 3 × 1.98 × 150.8 / 200 × 2.16) +309 3 } 1 / 3−309] / 2) Met.
Process [2]
The same operation as in step [2] of Example 1 was performed. The operation time was 3 min. Moreover, the weight ratio of sodium chloride and potassium chloride which comprises the obtained granulated material was about 1: 1 from the measured value (measurement method of Test Example 4) by an ion chromatograph.
工程〔１〕
粗塩化ナトリウム（ナイカイ塩業株式会社製；ナイカイ並塩 ＮａＣｌ純度９５．０％以上であり、にがりを含む）３００ｇを精製水９００ｇに溶解して２５重量％水溶液とした。トップスプレー式流動層造粒装置（フロイント産業株式会社製；ＦＬ−ＬＡＢＯ）に、核粒子として塩化カリウム（マナック株式会社製；日本薬局方塩化カリウム）２００ｇ（平均粒子径３１２μｍ）を投入し、給気温度９０℃、風量０．４ｍ３／ｍｉｎ、スプレー圧力０．２５ＭＰａ、スプレー流量６５ＮＬ／ｍｉｎの条件下で、前記水溶液を２．３ｇ／ｍｉｎの噴霧速度で５．３ｈｒ噴霧しながら乾燥した。造粒後、目開き１８０μｍのＪＩＳ標準篩（内径φ２００ｍｍ；深さ４５ｍｍ）を用いてスプレードライした粒子を分級した後、イオンクロマトグラフの測定（試験例４の測定方法）により噴霧層中の塩化ナトリウムの重量を測定した結果、１５１．１ｇ（塩化カリウムの仕込み量を２００ｇとして換算）であった。噴霧層の厚みは、２９．９１μｍ（噴霧層の厚み［μｍ］＝［｛（３１２３×１．９８×１５１．１／２００×２．１６）＋３１２３｝１／３−３１２］／２）であった。
工程〔２〕
実施例１の工程〔２〕と同様の操作を行った。尚、粗塩化ナトリウムは、ナイカイ塩業株式会社製のナイカイ並塩を使用した。そして、運転時間は４ｍｉｎとした。また、得られた造粒物を構成する塩化ナトリウムと塩化カリウムの重量比は、イオンクロマトグラフによる測定値（試験例４の測定方法）より約１：１であった。
Process [1]
300 g of crude sodium chloride (manufactured by Naikai Shigyo Co., Ltd .; Naika average salt NaCl purity of 95.0% or more, including bittern) was dissolved in 900 g of purified water to obtain a 25 wt% aqueous solution. 200 g (average particle size 312 μm) of potassium chloride (Manac Co., Ltd .; Japanese Pharmacopoeia Potassium Chloride) as core particles is charged into a top spray fluidized bed granulator (Freund Sangyo Co., Ltd .; FL-LABO) and supplied. The aqueous solution was dried while spraying for 5.3 hr at a spraying rate of 2.3 g / min under the conditions of an air temperature of 90 ° C., an air volume of 0.4 m 3 / min, a spray pressure of 0.25 MPa, and a spray flow rate of 65 NL / min. After granulation, the spray-dried particles are classified using a JIS standard sieve (inner diameter φ200 mm; depth 45 mm) with an opening of 180 μm, and then the chlorination in the spray layer is measured by ion chromatography (measurement method of Test Example 4). As a result of measuring the weight of sodium, it was 151.1 g (converted with the amount of potassium chloride charged as 200 g). The thickness of the spray layer is 29.91 μm (spray layer thickness [μm] = [{(312 3 × 1.98 × 151.1 / 200 × 2.16) +312 3 } 1/3 −312] / 2) Met.
Process [2]
The same operation as in step [2] of Example 1 was performed. In addition, the crude sodium chloride used the Naikai common salt by Naikai salt industry. The operation time was 4 min. Moreover, the weight ratio of sodium chloride and potassium chloride which comprises the obtained granulated material was about 1: 1 from the measured value (measurement method of Test Example 4) by an ion chromatograph.
工程〔１〕
塩化ナトリウム（ナイカイ塩業株式会社製；ナイカイ食塩 ＮａＣｌ純度９９．０％以上）３００ｇを精製水９００ｇに溶解して２５重量％水溶液とした。トップスプレー式流動層造粒装置（フロイント産業株式会社製；ＦＬ−ＬＡＢＯ）に、核粒子として塩化カリウム（マナック株式会社製；日本薬局方塩化カリウム）２００ｇ（平均粒子径５３１μｍ）を投入し、給気温度９０℃、風量０．４ｍ３／ｍｉｎ、スプレー圧力０．２ＭＰａ、スプレー流量６０ＮＬ／ｍｉｎの条件下で、前記水溶液を２．３ｇ／ｍｉｎの噴霧速度で２．６ｈｒ噴霧しながら乾燥した。造粒後、目開き１８０μｍのＪＩＳ標準篩（内径φ２００ｍｍ；深さ４５ｍｍ）を用いてスプレードライした粒子を分級した後、イオンクロマトグラフの測定（試験例４の測定方法）により噴霧層中の塩化ナトリウムの重量を測定した結果、７５．６ｇ（塩化カリウムの仕込み量を２００ｇとして換算）であった。噴霧層の厚みは、２７．６８μｍ（噴霧層の厚み［μｍ］＝［｛（５３１３×１．９８×７５．６／２００×２．１６）＋５３１３｝１／３−５３１］／２）であった。
工程〔２〕
実施例１の工程〔２〕と同様の操作を行った。尚、運転時間は１１ｍｉｎとした。また、得られた造粒物を構成する塩化ナトリウムと塩化カリウムの重量比は、イオンクロマトグラフによる測定値（試験例４の測定方法）より約１：１であった。
Process [1]
300 g of sodium chloride (manufactured by Naikai Shigyo Co., Ltd .; Naikai NaCl NaCl purity of 99.0% or more) was dissolved in 900 g of purified water to obtain a 25 wt% aqueous solution. 200 g (average particle size 531 μm) of potassium chloride (Manac Co., Ltd .; Japanese Pharmacopoeia Potassium Chloride) as core particles was charged into a top spray fluidized bed granulator (Freund Sangyo Co., Ltd .; FL-LABO) and supplied. The aqueous solution was dried while spraying for 2.6 hr at a spraying rate of 2.3 g / min under the conditions of an air temperature of 90 ° C., an air volume of 0.4 m 3 / min, a spray pressure of 0.2 MPa, and a spray flow rate of 60 NL / min. After granulation, the spray-dried particles are classified using a JIS standard sieve (inner diameter φ200 mm; depth 45 mm) with an opening of 180 μm, and then the chlorination in the spray layer is measured by ion chromatography (measurement method of Test Example 4). As a result of measuring the weight of sodium, it was 75.6 g (converted with the amount of potassium chloride charged as 200 g). The thickness of the spray layer is 27.68 μm (the thickness of the spray layer [μm] = [{(531 3 × 1.98 × 75.6 / 200 × 2.16) +531 3 } 1/3 −531] / 2) Met.
Process [2]
The same operation as in step [2] of Example 1 was performed. The operation time was 11 min. Moreover, the weight ratio of sodium chloride and potassium chloride which comprises the obtained granulated material was about 1: 1 from the measured value (measurement method of Test Example 4) by an ion chromatograph.
工程〔１〕
塩化ナトリウム（ナイカイ塩業株式会社製；ナイカイ食塩 ＮａＣｌ純度９９．０％以上）３００ｇを精製水９００ｇに溶解して２５重量％水溶液とした。トップスプレー式流動層造粒装置（フロイント産業株式会社製；ＦＬ−ＬＡＢＯ）に、核粒子として塩化カリウム（マナック株式会社製；日本薬局方塩化カリウム）２００ｇ（平均粒子径５３１μｍ）を投入し、給気温度９０℃、風量０．４ｍ３／ｍｉｎ、スプレー圧力０．２ＭＰａ、スプレー流量６０ＮＬ／ｍｉｎの条件下で、前記水溶液を２．３ｇ／ｍｉｎの噴霧速度で１．６ｈｒ噴霧しながら乾燥した。造粒後、目開き１８０μｍのＪＩＳ標準篩（内径φ２００ｍｍ；深さ４５ｍｍ）を用いてスプレードライした粒子を分級後、イオンクロマトグラフの測定（試験例４の測定方法）により噴霧層中の塩化ナトリウムの重量を測定した結果、４５．４ｇ（塩化カリウムの仕込み量を２００ｇとして換算）であった。噴霧層の厚みは、１７．２７μｍ（噴霧層の厚み［μｍ］＝［｛（５３１３×１．９８×４５．４／２００×２．１６）＋５３１３｝１／３−５３１］／２）であった。
工程〔２〕
実施例１の工程〔２〕と同様の操作を行った。尚、運転時間は１１ｍｉｎとした。また、得られた造粒物を構成する塩化ナトリウムと塩化カリウムの重量比は、イオンクロマトグラフによる測定値（試験例４の測定方法）より約１：１であった。
Process [1]
300 g of sodium chloride (manufactured by Naikai Shigyo Co., Ltd .; Naikai NaCl NaCl purity of 99.0% or more) was dissolved in 900 g of purified water to obtain a 25 wt% aqueous solution. 200 g (average particle size 531 μm) of potassium chloride (Manac Co., Ltd .; Japanese Pharmacopoeia Potassium Chloride) as core particles was charged into a top spray fluidized bed granulator (Freund Sangyo Co., Ltd .; FL-LABO) and supplied. The aqueous solution was dried while being sprayed for 1.6 hours at a spray rate of 2.3 g / min under the conditions of an air temperature of 90 ° C., an air volume of 0.4 m 3 / min, a spray pressure of 0.2 MPa, and a spray flow rate of 60 NL / min. After granulation, the particles spray-dried using a JIS standard sieve (inner diameter φ200 mm; depth 45 mm) with an opening of 180 μm are classified, and then sodium chloride in the spray layer is measured by ion chromatography (measurement method of Test Example 4). As a result, the weight was 45.4 g (converted with the amount of potassium chloride charged as 200 g). The thickness of the spray layer is 17.27 μm (the thickness of the spray layer [μm] = [{(531 3 × 1.98 × 45.4 / 200 × 2.16) +531 3 } 1/3 −531] / 2) Met.
Process [2]
The same operation as in step [2] of Example 1 was performed. The operation time was 11 min. Moreover, the weight ratio of sodium chloride and potassium chloride which comprises the obtained granulated material was about 1: 1 from the measured value (measurement method of Test Example 4) by an ion chromatograph.
［比較例１−３］
実施例１−３の工程〔１〕において得られた造粒物を、それぞれ比較例１−３とした。
[Comparative Example 1-3]
The granulated product obtained in step [1] of Example 1-3 was referred to as Comparative Example 1-3.
［比較例４］
塩化ナトリウム１００ｇ（平均粒子径３１０μｍ）と塩化カリウム１００ｇ（平均粒子径３２０μｍ）を攪拌混合機（深江パウテック株式会社製；ＬＦＳ−ＧＳ−２Ｊハイスピードミキサー）に仕込み、撹拌混合を行った。
[Comparative Example 4]
Sodium chloride 100 g (average particle size 310 μm) and potassium chloride 100 g (average particle size 320 μm) were charged into a stirring mixer (manufactured by Fukae Pautech Co., Ltd .; LFS-GS-2J High Speed Mixer) and mixed with stirring.
［試験例１］
実施例２で得られた造粒物の走査型電子顕微鏡（株式会社日立製作所製）による被覆層の断面構造を図６に示す。図６により、被覆層を有していることが確認できた。また、核粒子及び被覆層の元素分析結果（エネルギー分散型Ｘ線分析装置（ＥＤＸ））を図７及び図８にそれぞれ示す。これらの図より、核粒子が塩化カリウムであり、被覆層が塩化ナトリウムであることが確認された。
[Test Example 1]
FIG. 6 shows a cross-sectional structure of the coating layer of the granulated product obtained in Example 2 using a scanning electron microscope (manufactured by Hitachi, Ltd.). It has confirmed that it had a coating layer by FIG. Moreover, the elemental analysis results (energy dispersive X-ray analyzer (EDX)) of the core particles and the coating layer are shown in FIGS. 7 and 8, respectively. From these figures, it was confirmed that the core particles were potassium chloride and the coating layer was sodium chloride.
［試験例２］
実施例１、実施例２、実施例３、比較例１、比較例２及び比較例３で得られた造粒物の走査型電子顕微鏡（株式会社日立製作所製）による表面状態を、図９、図１０、図１１、図１２、図１３および図１４にそれぞれ示す。
[Test Example 2]
The surface state of the granulated product obtained in Example 1, Example 2, Example 3, Comparative Example 1, Comparative Example 2 and Comparative Example 3 with a scanning electron microscope (manufactured by Hitachi, Ltd.) is shown in FIG. 10, 11, 12, 13 and 14, respectively.
［試験例３］
試験例２において、走査型電子顕微鏡で倍率１０００倍にて粒子を観察し、２００個の粒子について表面結晶のＦｅｒｅｔ径を測定し、個数平均径を求めた。どのサンプルにおいても、数箇所で結晶形状を観察し、それぞれ２００個の粒子について測定した。結果を表１に示す。
[Test Example 3]
In Test Example 2, the particles were observed with a scanning electron microscope at a magnification of 1000 times, and the Feret diameter of the surface crystal was measured for 200 particles to determine the number average diameter. In each sample, the crystal shape was observed at several locations, and 200 particles were measured for each. The results are shown in Table 1.
比較例１〜３では被覆層を形成する表面状態は微粒子（約数μｍ）の集合体であるが、実施例１〜３では、粗大粒子（約１０μｍ以上）の集合体であることが確認された。 In Comparative Examples 1 to 3, the surface state on which the coating layer is formed is an aggregate of fine particles (about several μm), but in Examples 1 to 3, it is confirmed to be an aggregate of coarse particles (about 10 μm or more). It was.
［試験例４］
実施例１、２、４及び５の工程〔２〕において塩化カリウムの溶出率を以下の式で算出した。
溶出率［％］＝［[Ａ−｛Ｂ／（１＋Ｃ）｝／Ａ］]×１００
Ａ：工程〔２〕で仕込んだ工程〔１〕の造粒物中のＫＣｌ重量［ｇ］
Ｂ：工程〔２〕の乾燥後の重量［ｇ］
Ｃ：イオンクロマトグラフで測定した工程〔２〕における（ＮａＣｌ重量／ＫＣｌ重量）の割合［ｇ］
その結果を表２に示す。
[Test Example 4]
In step [2] of Examples 1, 2, 4 and 5, the elution rate of potassium chloride was calculated by the following formula.
Elution rate [%] = [[A- {B / (1 + C)} / A]] × 100
A: KCl weight [g] in the granulated product of step [1] charged in step [2]
B: Weight [g] after drying in step [2]
C: (NaCl weight / KCl weight) ratio [g] in step [2] measured by ion chromatography
The results are shown in Table 2.
尚、イオンクロマトグラフの測定方法に関しては、工程〔１〕及び〔２〕のサンプル５．００００ｇを水に溶かして正確に１００ｍｌとし、これを５０倍希釈してＮａ＋、Ｋ＋の各電解質濃度を東ソー株式会社製のイオンクロマトグラフにより測定してＫＣｌ及びＮａＣｌ重量を算出した。イオンクロマトグラフの分析条件を下記に示す。
カチオン測定
装置；ＴＯＳＯＨ ＩＯＮ ＣＨＲＯＭＡＴＯＧＲＡＰＨ
カラム；ＴＳＫｇｕａｒｄｃｏｌｕｍｎ ＳｕｐｅｒＩＣ−Ｃ Ｓｕｐｅｒ ＩＣ−Ｃａｔｉｏｎ
カラム温度；４０℃
サンプル量；３０μＬ
溶離液；２．５ｍｍｏｌ／Ｌ ＨＮＯ３＋０．５ｍｍｏｌ／Ｌ Ｌ−ヒスチジン
流量；０．８０ｍｌ／ｍｉｎ
Regarding the ion chromatograph measurement method, 5.0000 g of the samples of steps [1] and [2] were dissolved in water to make exactly 100 ml, and this was diluted 50 times to adjust the electrolyte concentrations of Na + and K + to Tosoh. The KCl and NaCl weights were calculated by measurement with an ion chromatograph manufactured by Co., Ltd. The analysis conditions of the ion chromatograph are shown below.
Cation measuring device; TOSOH ION CHROMATOGRAPH
Column; TSK guard column Super IC-C Super IC-Cation
Column temperature: 40 ° C
Sample volume: 30 μL
Eluent: 2.5 mmol / L HNO 3 +0.5 mmol / L L-histidine Flow rate: 0.80 ml / min
［試験例５］
実施例２と比較例４で得られた造粒物を１００ｍＬなすフラスコにそれぞれ２２ｇ仕込み、エバポレーターで５分間回転させた後、それぞれ５ｇのサンプリングを４回行い、試験例２と同条件で成分含量について分析した。実施例２の測定結果を表３、比較例４の測定結果を表４に示す。
[Test Example 5]
Each of the granulated products obtained in Example 2 and Comparative Example 4 was charged in a flask made of 100 mL, and after rotating for 5 minutes with an evaporator, 5 g each was sampled four times. Was analyzed. The measurement results of Example 2 are shown in Table 3, and the measurement results of Comparative Example 4 are shown in Table 4.
この変動係数の結果より、単に混合した比較例４よりも実施例２で得られた造粒物の含量均一性が優れていることがわかる。 From the result of this coefficient of variation, it can be seen that the content uniformity of the granulated product obtained in Example 2 is superior to that of Comparative Example 4 which is simply mixed.
［試験例６］
まず、官能評価試験を行うためのパネル（官能評価を行うために選ばれた人）を選定するために、５味の識別テストおよび味の濃度差識別テストを行った。
＜５味の識別テスト＞
５種の基本味である甘味（ショ糖；０．４ｇ／ｄＬ）、塩味（塩化ナトリウム；０．１３ｇ／ｄＬ）、酸味（酒石酸；０．００５ｇ／ｄＬ）、エグ味（硫酸キニーネ；０．０００４ｇ／ｄＬ）およびうま味（グルタミン酸ナトリウム；０．０５ｇ／ｄＬ）、ならびに水の計６種から５味を当てさせた。合格基準は５味中の誤差が１個以下とし、合格者は味の濃度差識別テストを行った。
＜味の濃度差識別テスト＞
エグ味を除く４種の基本味である甘味（ショ糖；５．００ｇ／ｄＬと５．５０ｇ／ｄＬの比較）、塩味（塩化ナトリウム；１．００ｇ／ｄＬと１．０６ｇ／ｄＬの比較）、酸味（酒石酸；０．０２０ｇ／ｄＬと０．０２４ｇ／ｄＬの比較）及びうま味（グルタミン酸ナトリウム；０．２００ｇ／ｄＬと０．２６６ｇ／ｄＬの比較）において濃度の異なる２つの溶液を比較させ、各味の強い方を判断させた。合格基準は４対中の誤差が１個以下として、パネルを選定した。
＜官能評価試験＞
実施例２と比較例４の造粒物を用いて、２点比較法で官能評価試験を行った。官能評価試験方法は、午前と午後に各一回行って、塩化カリウムの味の強い方をパネル１２人に選ばせた。結果を表５示す。
[Test Example 6]
First, in order to select a panel for performing a sensory evaluation test (a person selected to perform a sensory evaluation), a taste discrimination test for five tastes and a density difference discrimination test for taste were performed.
<Five taste identification test>
Sweetness (sucrose; 0.4 g / dL), salty taste (sodium chloride; 0.13 g / dL), acidity (tartaric acid; 0.005 g / dL), and taste (quinine sulfate; 0004 g / dL) and umami (sodium glutamate; 0.05 g / dL), and a total of 6 to 5 tastes of water. The acceptance criteria was that the error in 5 tastes was 1 or less, and the successful person conducted a taste density difference identification test.
<Taste density difference identification test>
Sweetness (sucrose; comparison between 5.00 g / dL and 5.50 g / dL), salty taste (sodium chloride; comparison between 1.00 g / dL and 1.06 g / dL), which are the four basic tastes excluding the taste Two solutions with different concentrations in sourness (tartaric acid; 0.020 g / dL and 0.024 g / dL) and umami (sodium glutamate; 0.200 g / dL and 0.266 g / dL) The person with the strong taste was judged. As the acceptance criteria, the panel was selected on the assumption that the error in 4 pairs was 1 or less.
<Sensory evaluation test>
Using the granules of Example 2 and Comparative Example 4, a sensory evaluation test was conducted by a two-point comparison method. The sensory evaluation test method was performed once each in the morning and in the afternoon, and the panel panel with 12 people with the strong taste of potassium chloride was selected. The results are shown in Table 5.
この結果、本発明の方法に従って塩化カリウムの表面を塩化ナトリウムで被覆することによって、塩化カリウムのニガ味を抑制できたことがわかった。 As a result, it was found that the negative taste of potassium chloride could be suppressed by coating the surface of potassium chloride with sodium chloride according to the method of the present invention.
本発明の塩味料により、高血圧患者及びナトリウムの摂取の抑制を必要とする人に対して、低ナトリウム塩を提供することができる。 The salty seasoning of the present invention can provide a low sodium salt to hypertensive patients and those who need to suppress sodium intake.
Ａ：被覆層
Ｂ：核粒子
Ｃ：塩化カリウムの単粒子
Ｄ：塩化ナトリウムの単粒子
１：塩化カリウム
２：塩化ナトリウム
ａ：飽和溶液を調製する槽
ｂ：攪拌モーター
ｃ：ポンプ
ｄ：冷却器
ｅ：晶析槽
A: Coating layer B: Core particle C: Single particle of potassium chloride D: Single particle of sodium chloride 1: Potassium chloride 2: Sodium chloride a: Tank for preparing saturated solution b: Stirring motor c: Pump d: Cooler e : Crystallization tank
Claims (6)
〔１〕塩化カリウム粒子に塩化ナトリウム水溶液をスプレーしながら乾燥造粒し、塩化ナトリウムを含む噴霧層を形成する工程；および
〔２〕過飽和の塩化ナトリウム水溶液を用いて塩化ナトリウムを結晶成長させることにより、塩化ナトリウムを含む晶析層を形成する工程
を含む、塩味料の製造方法。 The following steps:
[1] A step of drying and granulating potassium chloride particles while spraying a sodium chloride aqueous solution to form a spray layer containing sodium chloride; and [2] crystal growth of sodium chloride using a supersaturated sodium chloride aqueous solution. The manufacturing method of a salty seasoning including the process of forming the crystallization layer containing sodium chloride.
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