JPH09157285A - Production of mixed powdery composition of ascorbic acid with maltitol having high fluidity - Google Patents

Production of mixed powdery composition of ascorbic acid with maltitol having high fluidity

Info

Publication number
JPH09157285A
JPH09157285A JP7344312A JP34431295A JPH09157285A JP H09157285 A JPH09157285 A JP H09157285A JP 7344312 A JP7344312 A JP 7344312A JP 34431295 A JP34431295 A JP 34431295A JP H09157285 A JPH09157285 A JP H09157285A
Authority
JP
Japan
Prior art keywords
maltitol
ascorbic acid
aqueous solution
purity
solid content
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Granted
Application number
JP7344312A
Other languages
Japanese (ja)
Other versions
JP3955088B2 (en
Inventor
Masahiro Niimi
匡弘 新見
Fumie Niimi
文江 新見
Kazuaki Kato
和昭 加藤
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Towa Chemical Industry Co Ltd
Original Assignee
Towa Chemical Industry Co Ltd
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Towa Chemical Industry Co Ltd filed Critical Towa Chemical Industry Co Ltd
Priority to JP34431295A priority Critical patent/JP3955088B2/en
Publication of JPH09157285A publication Critical patent/JPH09157285A/en
Application granted granted Critical
Publication of JP3955088B2 publication Critical patent/JP3955088B2/en
Anticipated expiration legal-status Critical
Expired - Lifetime legal-status Critical Current

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  • Furan Compounds (AREA)
  • Saccharide Compounds (AREA)
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Abstract

PROBLEM TO BE SOLVED: To economically advantageously produce a mixed powdery composition of ascorbic acid with maltitol while solving problems such as deviation of components or fluidity. SOLUTION: This method for producing a mixed powdery composition of ascorbic acid with maltitol comprises successively passing through (1) the first step for respectively preparing a maltitol massecuite at 10-70wt.% suspended crystal content from an aqueous solution having 85-99.9wt.% maltitol purity at 70-90wt.% solid concentration and a massecuite from an aqueous solution of ascorbic acid having >=98wt.% purity, (2) the second step for keeping the introduction ratio of the maltitol massecuite at 5-80wt.% expressed in terms of solid content and the introduction ratio of the ascorbic acid massecuite at 20-95wt.% expressed in terms of the solid content, introducing the respective massecuites into a spray dryer and spray-drying the massecuites at 30-75 deg.C air blasting temperature.

Description

【発明の詳細な説明】Detailed Description of the Invention

【0001】[0001]

【発明の属する技術分野】TECHNICAL FIELD OF THE INVENTION

【0002】本発明はアスコルビン酸とマルチトールと
の流動性の高い混合粉末組成物の製造方法に関するもの
である。
The present invention relates to a method for producing a highly fluid mixed powder composition of ascorbic acid and maltitol.

【0003】[0003]

【従来の技術及び発明が解決しようとする課題】2. Description of the Related Art

【0004】マルチトール粉末は、マルトースを接触水
素化し、粉末化することにより製造される糖アルコール
であり、甘味質が砂糖に近く、甘味度も他の糖アルコー
ルに比較して砂糖に近く、口内細菌により資化されにく
いので虫歯の原因にならず、ヒトの消化酵素では消化さ
れにくいなどの特徴があるため、糖尿病患者、肥満や虫
歯を予防したいと考えている人々に広く利用されてい
る。
Maltitol powder is a sugar alcohol produced by catalytically hydrogenating maltose and pulverizing it, and has a sweetness similar to sugar and a sweetness degree similar to sugar as compared with other sugar alcohols, Since it is not easily assimilated by bacteria, it does not cause tooth decay and is not easily digested by human digestive enzymes, so it is widely used by diabetics, people who want to prevent obesity and tooth decay.

【0005】また、マルチトール結晶などに代表される
マルチトール粉末は、非吸湿性、熱などに対する安定
性、インシュリン分泌を促さないことや各種ミネラルの
吸収に好ましい影響を与えることなど、各種の有用な機
能を有することから、前記の特殊な用途に止まらず、一
般の食品や医薬品、化粧品の材料等としても広く利用さ
れつつある。
Maltitol powder represented by maltitol crystals is useful for various purposes such as non-hygroscopicity, stability to heat, not promoting insulin secretion, and having a favorable effect on absorption of various minerals. Since it has various functions, it is not only used for the above-mentioned special applications but also widely used as a material for general foods, pharmaceuticals, cosmetics and the like.

【0006】一方、アスコルビン酸はビタミンCとして
知られ、大量に製造されており、各種酸化防止剤や酸味
量等として食品用途に用いられている他、各種工業用途
や医薬用途にも広く用いられている。
On the other hand, ascorbic acid is known as vitamin C, is produced in large quantities, and is used in various food applications such as various antioxidants and sourness, as well as in various industrial applications and pharmaceutical applications. ing.

【0007】しかし、更に用途を拡大しようとしたとき
に、アスコルビン酸の酸味が強いことや、保存中に酸化
分解してしまい黄色に変色したり、含量が低下すること
等が課題として残されていた。
[0007] However, when the application is further expanded, there remain problems such as the strong sourness of ascorbic acid, the oxidative decomposition during storage, which causes discoloration to yellow and the decrease in content. It was

【0008】また、アスコルビン酸で流通している商品
の殆どは微細な結晶品であり、マルチトールのほうは流
通している商品の殆どは粉末の粒子が鋭角端を有する破
砕品や結晶品であって、共に流動性がやや低いことも課
題とされていた。
Most of the products distributed with ascorbic acid are fine crystal products, and most of the products distributed with maltitol are crushed products or crystal products in which powder particles have sharp edges. Therefore, it was also a problem that the liquidity was rather low.

【0009】従って、砂糖に類似したまろやかな甘味質
のマルチトールとアスコルビン酸との流動性の高い混合
粉末組成物が望まれていた。
Therefore, there has been a demand for a highly fluid mixed powder composition of maltitol and ascorbic acid, which has a mellow sweetness similar to that of sugar.

【0010】更に、そのような混合粉末組成物を調製す
る際には、保存、輸送等している間に成分の偏りが生じ
ないことや保存性を改善することも課題とされていた。
Further, when preparing such a mixed powder composition, it has been a subject to prevent the components from being biased during storage and transportation and to improve the storability.

【0011】従って、成分の偏りや流動性などの課題を
解決しつつ、アスコルビン酸とマルチトールとの混合粉
末組成物を経済的に有利に製造する方法の開発が望まれ
ていたのである。
Therefore, it has been desired to develop a method for economically advantageously producing a mixed powder composition of ascorbic acid and maltitol while solving the problems such as the component bias and the fluidity.

【0012】[0012]

【課題を解決するための手段】[Means for Solving the Problems]

【0013】本発明者等は、前述の課題を解決するた
め、鋭意検討した結果、マルチトールマスキットとアス
コルビン酸のマスキットとを各々調製し、特定の割合で
噴霧乾燥装置に導入して噴霧乾燥することにより、従来
品のような成分の偏りが無く、且つ、経済的に有利な、
アスコルビン酸とマルチトールとの流動性の高い混合粉
末を製造する方法を開発することに成功し、更に、マル
チトールとアスコルビン類との高い濃度の混合水溶液を
調製した後、冷却して細かい結晶を発生させ、粘度の低
いマスキットを調製して噴霧乾燥することによって、流
動性が高く、アスコルビン酸の保存性が改善され、従来
品のような成分の偏りが無い、アスコルビン酸とマルチ
トールとの混合粉末を経済的に有利に製造することに成
功し、本発明を完成するに至った。
In order to solve the above-mentioned problems, the inventors of the present invention have conducted extensive studies, and as a result, prepared maltitol maskit and ascorbic acid maskit and introduced them into a spray dryer at a specific ratio and spray-dried them. By doing so, there is no bias in the components as in conventional products, and it is economically advantageous,
We succeeded in developing a method for producing a highly fluid mixed powder of ascorbic acid and maltitol, and further prepared a mixed aqueous solution of high concentration of maltitol and ascorbins, and then cooled to form fine crystals. Mixing of ascorbic acid and maltitol has high fluidity and improved storage stability of ascorbic acid by preparing a musket with low viscosity and spray-drying, and there is no bias of components as in conventional products. The present invention has been completed by succeeding in economically producing the powder.

【0014】本発明の課題を解決するための手段は、下
記の通りである。
Means for solving the problems of the present invention are as follows.

【0015】第一の本発明は、アスコルビン酸とマルチ
トールとの流動性の高い混合粉末組成物を製造する方法
において、1)マルチトール純度が85〜99.9重量
%で固形分濃度が70〜90重量%のマルチトール水溶
液から、懸濁結晶量10〜70重量%のマルチトールマ
スキットを、純度98以上のアスコルビン酸の水溶液か
らマスキットを、それぞれ調製する第一工程、2)マル
チトールマスキットの導入割合を固形分で5〜80重量
%、アスコルビン酸のマスキットの導入割合を固形分で
20〜95重量%の割合に保ち、各々のマスキットを噴
霧乾燥装置に導入し、送風温30〜75℃で噴霧乾燥す
る第二工程、の2工程を逐次的に経由することを特徴と
する、アスコルビン酸とマルチトールとの流動性の高い
混合組成物の製造方法である。
The first aspect of the present invention relates to a method for producing a highly fluid mixed powder composition of ascorbic acid and maltitol, wherein 1) the maltitol purity is 85 to 99.9% by weight and the solid content concentration is 70. The first step of preparing a maltitol mass kit having an amount of suspended crystals of 10 to 70% by weight from an aqueous solution of maltitol of 90% by weight and a mass kit of an aqueous solution of ascorbic acid having a purity of 98 or more, 2) maltitol mass. The introduction rate of the kit is maintained at 5 to 80% by weight in terms of solid content, and the introduction rate of the ascorbic acid maskit is maintained at 20 to 95% by weight in terms of the solid content, and each of the maskits is introduced into the spray dryer, and the blowing temperature is 30 to 30%. Production of a highly fluid mixed composition of ascorbic acid and maltitol, characterized in that the two steps of the second step of spray drying at 75 ° C. are sequentially performed. It is the law.

【0016】第二の本発明は、第一工程において、濃度
20〜35%のアスコルビン酸純度98以上の水溶液か
らアスコルビン酸マスキットを調製し、且つマルチトー
ルマスキットの懸濁結晶量が10〜40重量%に調節さ
れたものである、第一の発明に記載のアスコルビン酸と
マルチトールとの流動性の高い混合粉末組成物の製造方
法。
In the second aspect of the present invention, in the first step, an ascorbic acid mass kit is prepared from an aqueous solution having a concentration of 20 to 35% and a purity of ascorbic acid of 98 or more, and the amount of suspended crystals of maltitol mass kit is 10 to 40. The method for producing a highly powdered mixed powder composition of ascorbic acid and maltitol according to the first invention, wherein the mixed powder composition has been adjusted to have a weight percentage.

【0017】第三の本発明は、アスコルビン酸とマルチ
トールとの流動性の高い混合粉末組成物を製造する方法
において、1)純度90〜99.9重量%のマルチトー
ルを固形分比率で5〜80重量%、純度98%以上のア
スコルビン酸を固形分比率で20〜95重量%含有する
固形分濃度20〜85重量%の水溶液を調製し、温度1
0〜60℃まで冷却し、必要に応じて種結晶の添加及び
希釈をして更に0.5〜10時間程度撹拌し、アスコル
ビン酸とマルチトールとの混合水溶液のマスキットを調
製する第一工程、2)第一工程で得られたアスコルビン
酸とマルチトールとの混合水溶液のマスキットを噴霧乾
燥装置に導入し、送風温30〜75℃で噴霧乾燥する第
二工程、の2工程を逐次的に経由することを特徴とす
る、アスコルビン酸とマルチトールとの流動性の高い混
合粉末組成物の製造方法である。
A third aspect of the present invention relates to a method for producing a highly fluid mixed powder composition of ascorbic acid and maltitol, wherein 1) maltitol having a purity of 90 to 99.9% by weight is added in a solid content ratio of 5%. ˜80% by weight, ascorbic acid having a purity of 98% or more in a solid content ratio of 20 to 95% by weight, and an aqueous solution having a solid content concentration of 20 to 85% by weight is prepared at a temperature of 1%.
A first step of preparing a mass kit of a mixed aqueous solution of ascorbic acid and maltitol, which is cooled to 0 to 60 ° C., seed crystals are added and diluted if necessary, and stirred for about 0.5 to 10 hours, 2) Introduce the mass kit of the mixed aqueous solution of ascorbic acid and maltitol obtained in the first step into a spray drying device, and sequentially pass through the second step of spray drying at a blast temperature of 30 to 75 ° C. The method for producing a highly fluid mixed powder composition of ascorbic acid and maltitol.

【0018】また、第四の本発明は、調製後のマスキッ
トに水、アスコルビン酸の水溶液、マルチトール水溶液
の何れか1種または2種以上の混合液を加えることによ
り、固形分濃度を20〜80%に調整してマスキットの
粘度を低下させる、第三の発明に記載のアスコルビン酸
とマルチトールとの流動性の高い混合粉末組成物の製造
方法である。
In the fourth aspect of the present invention, the solid content concentration is 20 to 20 by adding one or a mixture of water, an aqueous solution of ascorbic acid and an aqueous solution of maltitol to the prepared mask. A method for producing a highly fluid mixed powder composition of ascorbic acid and maltitol according to the third aspect of the invention, wherein the viscosity of the musket is reduced by adjusting it to 80%.

【0019】本発明に用いるマルチトールは、本発明の
条件下で良好な状態のマルチトールマスキットを生成す
る品質が要求されるが、澱粉液化液に通常の糖化条件を
施して調製した高純度マルトースを還元して得たマルチ
トール純度が85〜99.9%で固形分濃度が70〜9
0%、更に好ましくは73〜80%、最も好ましくは7
5〜78%の水溶液であれば、おおむね本発明に要求さ
れる品質を満足するが、分子量が近いマルトトリイトー
ルやマルトテトライトール等はマルチトールの結晶生成
を阻害する傾向があるので、それらの成分が少ないもの
が好ましい。
The maltitol used in the present invention is required to have a quality capable of producing a maltitol mass kit in a good condition under the conditions of the present invention, but a high purity prepared by subjecting a starch liquefaction liquid to ordinary saccharification conditions. Maltitol obtained by reducing maltose has a purity of 85 to 99.9% and a solid content of 70 to 9
0%, more preferably 73 to 80%, most preferably 7
An aqueous solution of 5 to 78% generally satisfies the quality required for the present invention, but maltotriitol, maltotetriitol and the like having similar molecular weights tend to inhibit the crystal formation of maltitol. Those having a small amount of the component are preferable.

【0020】しかし、本発明の中のマルチトールとアス
コルビン酸との混合水溶液からマスキットを調製する方
法にあっては、結晶の析出が困難になるなどの理由から
やや高い純度のマルチトールが要求され、好ましくは純
度90〜99.9%、更に好ましくは純度95〜99.
9%のマルチトールが採用されるべきである。
However, in the method of preparing the musket from the mixed aqueous solution of maltitol and ascorbic acid in the present invention, maltitol having a slightly high purity is required because the precipitation of crystals becomes difficult. , Preferably 90 to 99.9%, and more preferably 95 to 99.
9% maltitol should be adopted.

【0021】また、本発明に用いるアスコルビン酸は、
本発明実施の際にアスコルビン酸マスキットを生成し易
い品質の、高純度のものが好ましいが、市販の食品又は
食品添加用途に調製されている製品は99%以上と純度
が極めて高いので、本発明に有利に採用することができ
る。
The ascorbic acid used in the present invention is
In the practice of the present invention, a high-purity product having a quality that easily produces an ascorbic acid mass kit is preferable, but a commercially available product or a product prepared for use as a food additive has an extremely high purity of 99% or more. Can be advantageously used for

【0022】本発明を実施する際に重要な点の一つは、
マルチトールのマスキットとアスコルビン酸のマスキッ
トをそれぞれ調製する点であり、特に、本発明を実施す
る上で有利なマルチトールのマスキットを調製するに
は、マルチトール水溶液を一度100℃以上に加熱する
などの手段で結晶のエンブリオが残らないように0.8
未満の低い飽和度にした後、濃度70〜90%、更に好
ましくは76〜79%に調整して、必要に応じて種結晶
を加え、冷却しながら撹拌するなどの方法で微細なマル
チトール結晶を生成させ、水溶液中に結晶が10〜70
%更に好ましくは10〜35%の範囲になった時にそれ
以上結晶が生成、成長しないように温度を調節して飽和
度を1.0程度に保持しながら5〜10時間程度撹拌す
ることによって本発明に有利に用いられるマルチトール
マスキットが得られる。
One of the important points in carrying out the present invention is that
The point is to prepare a maltitol musket and an ascorbic acid musket, and in particular, in order to prepare an advantageous maltitol musket for carrying out the present invention, the maltitol aqueous solution is heated once to 100 ° C. or higher. By the means of 0.8
After making the degree of saturation low, the concentration is adjusted to 70 to 90%, more preferably 76 to 79%, and seed crystals are added if necessary, and fine maltitol crystals are added by stirring while cooling. And crystals are formed in the aqueous solution in an amount of 10 to 70
% More preferably, by adjusting the temperature so as to prevent further crystal formation and growth when the content is in the range of 10 to 35% and maintaining the saturation degree at about 1.0, stirring is performed for about 5 to 10 hours. A maltitol mass kit is obtained which is advantageously used in the invention.

【0023】また、マルチトールマスキットを調製する
際に徐冷するなどの影響で細長い結晶が多く析出してし
まうことがあるが、懸濁する結晶が多すぎたり、結晶が
小さ過ぎて粘度が高くなった場合には、十分に撹拌しな
がら水又はマルチトール水溶液を加えて固形分濃度を下
げることも、マスキットの輸送や品質の優れた噴霧乾燥
品を得るうえで有利に採用することができる。
In addition, although a large number of elongated crystals may be precipitated due to the effect of slow cooling when preparing the maltitol mass kit, there are too many suspended crystals or the crystals are too small to increase the viscosity. When the temperature becomes high, addition of water or a maltitol aqueous solution with sufficient stirring to reduce the solid content concentration can also be advantageously used in transporting the mass kit and obtaining a spray-dried product with excellent quality. .

【0024】また、アスコルビン酸のマスキットを調製
する際には、アスコルビン酸は結晶速度が速いので、固
形分濃度20〜35%に調製したアスコルビン酸水溶液
に必要に応じて種結晶を加え、急冷して撹拌するなどの
方法で微細なアスコルビン酸結晶を生成させ、水溶液中
に懸濁している結晶の量が5〜30%の範囲になった時
にそれ以上結晶が生成、成長しないように温度を調節し
て飽和度を1.0程度に保持することによって本発明に
有利に用いられるアスコルビン酸のマスキットが得られ
る。
When preparing a mass kit of ascorbic acid, since ascorbic acid has a high crystallization rate, seed crystals are added to the ascorbic acid aqueous solution prepared to a solid concentration of 20 to 35% as needed, and the mixture is rapidly cooled. Fine ascorbic acid crystals are generated by stirring, etc., and when the amount of crystals suspended in the aqueous solution is in the range of 5 to 30%, the temperature is adjusted so that crystals do not grow and grow further. By maintaining the saturation at about 1.0, the ascorbic acid maskit which is advantageously used in the present invention can be obtained.

【0025】次に、アスコルビン酸とマルチトールとの
混合水溶液からマスキットを調製する方法について説明
する。
Next, a method for preparing a musket from a mixed aqueous solution of ascorbic acid and maltitol will be described.

【0026】この方法の場合は純度90〜99.9%、
更に好ましくは95〜99.9%のマルチトールを採用
するが、マルチトールとアスコルビン酸との固形分比率
が5:95〜80:20の範囲の混合水溶液を調製し、
濃度20〜85%に調節してから温度10〜60℃、好
ましくは12〜40℃まで急速に冷却し、やや強く撹拌
しながら必要に応じてアスコルビン酸及び/又はマルチ
トールの種結晶添加や希釈をして更に0.5〜10時間
穏やかに撹拌し、微細な結晶を析出させることにより混
合液のマスキットを得ることができる。
In the case of this method, the purity is 90 to 99.9%,
More preferably, 95 to 99.9% of maltitol is adopted, but a mixed aqueous solution having a solid content ratio of maltitol and ascorbic acid in the range of 5:95 to 80:20 is prepared,
After the concentration is adjusted to 20 to 85%, the temperature is rapidly cooled to 10 to 60 ° C, preferably 12 to 40 ° C, and ascorbic acid and / or maltitol seed crystals are added or diluted as needed with moderately strong stirring. Then, the mixture is gently stirred for 0.5 to 10 hours to precipitate fine crystals, whereby a mass kit of the mixed solution can be obtained.

【0027】次に、本発明の第二工程について説明す
る。
Next, the second step of the present invention will be described.

【0028】マルチトールマスキットとアスコルビン酸
のマスキットとを別々に調製してから噴霧乾燥装置に導
入する場合は、マルチトールマスキットの導入割合を固
形分で5〜80重量%、アスコルビン酸の導入割合を固
形分で20〜95重量%の割合に保ち、噴霧乾燥装置に
入る直前に両方のマスキットを混合させるかまたは各々
のマスキットを噴霧乾燥装置に導入したのちにアトマイ
ザーなどの上で混合させるが、噴霧乾燥装置内の送風温
を30〜75℃の範囲に調節し、各成分の固形分比率を
前記範囲内に調節することが、比較的吸湿性の低い製品
を得ることや、流動性の高い均一な組成などの市場が要
求する品質を満足すること等の理由から好ましい。
When the maltitol musket and the ascorbic acid musket are separately prepared and then introduced into the spray dryer, the maltitol musket is introduced at a solid content of 5 to 80% by weight, and ascorbic acid is introduced. The proportion is kept at 20 to 95% by weight in terms of solid content, and both mass kits are mixed immediately before entering the spray dryer, or each mass kit is introduced into the spray dryer and then mixed on an atomizer or the like. It is possible to obtain a product having a relatively low hygroscopic property and to adjust the air temperature in the spray dryer within the range of 30 to 75 ° C. and the solid content ratio of each component within the above range. It is preferable because it satisfies the quality required by the market such as high uniform composition.

【0029】本発明の第一工程でアスコルビン酸とマル
チトールとの混合水溶液から調製したマスキットを噴霧
乾燥する場合は、予めアスコルビン酸とマルチトールと
の固形分比率が水溶液の段階で適切に調整してあるの
で、マスキットをそのまま装置に導入し、噴霧乾燥装置
内の送風温を30〜75℃の範囲に調節しながら操作す
ることによって本発明を実施することができる。
When spray-drying the mass kit prepared from a mixed aqueous solution of ascorbic acid and maltitol in the first step of the present invention, the solid content ratio of ascorbic acid and maltitol is adjusted beforehand at the aqueous solution stage. Therefore, the present invention can be carried out by introducing the mass kit as it is into the apparatus and operating it while adjusting the blowing temperature in the spray-drying apparatus within the range of 30 to 75 ° C.

【0030】また、マスキットを噴霧乾燥装置に導入す
る方式は通常の噴霧乾燥に採用されている方式であれば
格別の制約を受けないが、噴霧乾燥装置の上部にアトマ
イザーを備えた方式のものがノズル方式のものよりも条
件を調節し易いので好ましく、送風温は30℃未満の場
合には乾燥効果が不十分で水分が残り過ぎる場合が多
く、75℃を超える温度を採用した場合には、アスコル
ビン酸が黄色くなってしまい品質を損なう場合が多い。
The method of introducing the musket into the spray drying apparatus is not particularly limited as long as it is a method adopted in ordinary spray drying, but a method in which an atomizer is provided above the spray drying apparatus is used. The condition is easier to control than the nozzle type, and the blowing temperature is less than 30 ° C., the drying effect is insufficient and water remains too much, and when the temperature exceeds 75 ° C., Ascorbic acid often turns yellow and impairs quality.

【0031】このように本発明の第二工程を実施する際
に、噴霧乾燥装置の底部に落下したときの粉末は十分に
低い水分含量まで乾燥される。
Thus, when carrying out the second step of the present invention, the powder when dropped on the bottom of the spray dryer is dried to a sufficiently low water content.

【0032】しかし、マルチトールの結晶化を高めるた
めには粉末中に残っている水分が有効に働くので、この
時点で必ずしも乾燥を完了させる必要はない。
However, in order to enhance the crystallization of maltitol, the water remaining in the powder works effectively, so that it is not always necessary to complete the drying at this point.

【0033】更に、品質の安定した本発明の製品を得る
うえで、噴霧乾燥した後の粉末を温度25℃前後に保持
して熟成させてから公知の方法で乾燥することも有利に
採用することができる。
Further, in order to obtain the product of the present invention with stable quality, it is also advantageous to employ a method in which the powder after spray drying is kept at a temperature of about 25 ° C. for aging and then dried by a known method. You can

【0034】本発明に採用する噴霧乾燥装置は、本発明
を実施して得られるマスキットの性質が噴霧乾燥困難な
ものであるという事情や、流動性の高い製品を得るうえ
から、直径の大きいものが好ましいが、具体的には直径
が5メートル以上、更に好ましくは8メートル以上のも
のが有利に採用できる。
The spray-drying apparatus adopted in the present invention has a large diameter because the mass kit obtained by carrying out the present invention is difficult to spray-dry, and a product having high fluidity is obtained. However, specifically, those having a diameter of 5 meters or more, and more preferably 8 meters or more can be advantageously used.

【0035】以上に説明したように、本発明の工程は加
熱や乾燥操作の部分が比較的短時間に終了するもので、
強い加熱やニーダー法のような機械的に強い混練をする
必要がないので成分に着色することがなく、複雑な構造
の特殊な機器も要求されないので経済的に有利な方法で
あり、本発明の方法を経由することにより得られる製品
は、極めて流動性が高く、輸送や保管の間に振動等によ
って成分の偏りを生じることがなく、且つ、共存するマ
ルチトールによってアスコルビン酸の分解が抑制される
ので保存性が改善されており、従って、各種用途に用い
た場合に性質や味、効果などにばらつきが出ないという
有利な特徴がある。
As described above, in the process of the present invention, the heating and drying operations are completed in a relatively short time.
It is an economically advantageous method because it does not require strong mechanical kneading such as strong heating or a kneader method to color the components and does not require special equipment having a complicated structure. The product obtained by passing through the method has extremely high fluidity, does not cause component bias due to vibration during transportation and storage, and coexisting maltitol suppresses decomposition of ascorbic acid. Therefore, the storability is improved, and therefore, there is an advantageous feature that the properties, tastes, effects, etc. do not vary when used for various purposes.

【0036】また、本発明により得られる製品は、従来
品に比べて吸湿製が低いので、貯蔵中の固結が生じにく
いなどの有利な性質も備えている。
Further, since the product obtained by the present invention has a lower hygroscopicity than that of the conventional product, it has an advantageous property that it is unlikely to cause solidification during storage.

【0037】[0037]

【実施例】【Example】

【0038】以下に、実施例、比較例を掲げて更に具体
的に本発明の方法を説明するが、本発明の技術的範囲は
以下の例に制限されるものではない。
Hereinafter, the method of the present invention will be described more specifically with reference to Examples and Comparative Examples, but the technical scope of the present invention is not limited to the following examples.

【0039】また、以下の例において、%は特に断らな
い限り重量%を表わすものとする。
In the following examples,% means% by weight unless otherwise specified.

【0040】(実施例1)(Example 1)

【0041】<第一工程> 純度99.9%の市販のア
スコルビン酸を濃度33%に調整し、撹拌しながら温度
15℃まで急激に冷却して微細な結晶を析出させ、その
まま温度を15℃に保持して、毎分20回転のゆっくり
とした撹拌を5時間続け、アスコルビン酸のマスキット
を得た。
<First Step> Commercially available ascorbic acid having a purity of 99.9% was adjusted to a concentration of 33% and rapidly cooled to 15 ° C. with stirring to precipitate fine crystals, and the temperature was kept at 15 ° C. While maintaining at 20 rpm, slow stirring at 20 rpm was continued for 5 hours to obtain an ascorbic acid mass kit.

【0042】純度95.0%の食品用マルチトール[東
和化成工業(株)製、登録商標アマルティMR]を濃度7
5%に調整し、加熱して温度を100℃にした後、撹拌
しながら30分間で温度15℃まで急激に冷却して微細
な結晶を析出させ、毎分20回転のゆっくりとした撹拌
を10時間続けて懸濁結晶量35%のマルチトールマス
キットを得た。
Maltitol for food having a purity of 95.0% [registered trademark Amarti MR manufactured by Towa Kasei Kogyo Co., Ltd.] at a concentration of 7
After adjusting to 5% and heating to 100 ° C., the temperature was rapidly cooled to 15 ° C. over 30 minutes with stirring to precipitate fine crystals, and a slow stirring at 20 rpm was performed for 10 minutes. Continuously, a maltitol mass kit containing 35% of suspended crystals was obtained.

【0043】<第二工程> 第一工程で得た各々のマス
キットをポンプで噴霧乾燥装置に送入する際に、アスコ
ルビン酸が60、マルチトールが40の固形分比率と
し、噴霧乾燥装置に入る直前に両者の配管が接続して一
本の配管から各マスキットが導入されるよう調整し、送
風温度70℃、排風温度35℃、噴霧乾燥装置の底部に
落下した粉末の温度が35℃で、水分が3%になるよう
に噴霧乾燥して本発明のアスコルビン酸とマルチトール
との流動性の高い混合粉末組成物を得た。
<Second Step> When each of the mass kits obtained in the first step is fed into the spray dryer by a pump, the solid content ratio of ascorbic acid is 60 and maltitol is 40, and the mixture enters the spray dryer. Immediately before, adjust so that both pipes are connected and each mass kit is introduced from one pipe, and the air temperature is 70 ° C, the air temperature is 35 ° C, and the temperature of the powder dropped to the bottom of the spray dryer is 35 ° C. The mixture was spray-dried so that the water content was 3% to obtain a highly fluid mixed powder composition of ascorbic acid and maltitol of the present invention.

【0044】本実施例により得られたアスコルビン酸と
マルチトールとの流動性の高い混合粉末組成物の組成を
液体クロマトグラフ法により測定したところ、マルチト
ール41%、アスコルビン酸59%であった。
The composition of the highly fluid mixed powder composition of ascorbic acid and maltitol obtained in this example was measured by liquid chromatography to find that it was 41% maltitol and 59% ascorbic acid.

【0045】また、本実施例により得られたアスコルビ
ン酸とマルチトールとの流動性の高い混合粉末組成物の
約50メッシュの粉末を安息角測定機具(PT−D型)
により測定した結果、安息角は、30°であり、外観は
白色のサラサラした極めて流動性の優れた粉末であっ
た。
Further, about 50 mesh powder of the mixed powder composition of ascorbic acid and maltitol having high fluidity obtained in this example was used as a repose angle measuring device (PT-D type).
As a result, the angle of repose was 30 ° and the powder was white and had a smooth appearance and was extremely fluid.

【0046】(実施例2)(Example 2)

【0047】<第一工程> 実施例1と同様にしてアス
コルビン酸のマスキットを得た。
<First Step> A mass kit of ascorbic acid was obtained in the same manner as in Example 1.

【0048】純度98%の食品用マルチトール[東和化
成工業(株)製、登録商標レシス]の水溶液を濃度80%
に濃縮し、加熱して温度を100℃にした後、撹拌しな
がら20分間で温度15℃まで急激に冷却してマルチト
ール液の固形分に対して3%の微細なマルチトール粉末
[東和化成工業(株)製、登録商標レシス]を添加して微
細な結晶を析出させ、水を加えて全体の濃度を78%に
調整し、毎分20回転のゆっくりとした撹拌を10時間
続けて懸濁結晶量35%のマルチトールマスキットを得
た。
An aqueous solution of maltitol for food [purity 98%, manufactured by Towa Kasei Kogyo Co., Ltd., registered trademark RESIS] having a purity of 98% is 80% in concentration.
After concentrating to 100 ° C and heating to 100 ° C, the mixture is rapidly cooled to 15 ° C for 20 minutes with stirring, and a fine maltitol powder of 3% relative to the solid content of the maltitol liquid [Towa Kasei Kogyo Co., Ltd., registered trademark Lesis] was added to precipitate fine crystals, water was added to adjust the total concentration to 78%, and slow stirring at 20 rpm was continued for 10 hours. A maltitol mass kit having a turbid crystal amount of 35% was obtained.

【0049】<第二工程> マスキットの導入比率をア
スコルビン酸が90、マルチトールが10とした他は、
実施例1と同様にして各々のマスキットをポンプで噴霧
乾燥装置に送入し、同様の条件で噴霧乾燥して本発明の
アスコルビン酸とマルチトールとの流動性の高い混合粉
末組成物を得た。
<Second Step> In addition to the introduction ratios of the musket being 90 for ascorbic acid and 10 for maltitol,
In the same manner as in Example 1, each mass kit was pumped into a spray dryer and spray dried under the same conditions to obtain a highly fluid mixed powder composition of ascorbic acid and maltitol of the present invention. .

【0050】本実施例により得られたアスコルビン酸と
マルチトールとの流動性の高い混合粉末組成物の組成を
液体クロマトグラフ法により測定したところ、マルチト
ール10.2%、アスコルビン酸89.8%であった。
The composition of the highly fluid mixed powder composition of ascorbic acid and maltitol obtained in this example was measured by liquid chromatography to find that maltitol was 10.2% and ascorbic acid was 89.8%. Met.

【0051】また、本実施例により得られた水分0.3
%のアスコルビン酸とマルチトールとの流動性の高い混
合粉末組成物の約50メッシュの粉末を安息角測定機具
(PT−D型)により測定した結果、安息角は、33°
であり、外観は白色のサラサラした極めて流動性の優れ
た粉末であった。
Further, the water content of 0.3 obtained in this example.
% Powder of approximately 50 mesh of a highly fluid mixed powder composition of ascorbic acid and maltitol was measured by a repose angle measuring device (PT-D type), the repose angle was 33 °.
It was a powder with a smooth white appearance and excellent flowability.

【0052】(実施例3)(Embodiment 3)

【0053】<第一工程> 純度99.0%のマルチト
ール[東和化成工業(株)製、登録商標レシス]とアスコ
ルビン酸の固形分比率が20:80の濃度39%の混合
水溶液を温度60℃で調製し、撹拌しながら温度15℃
まで急速に冷却し、対混合水溶液の固形分2%の微粉末
状マルチトールを種結晶として添加し、0.5時間撹拌
を続けて微細結晶を十分に生成させて懸濁結晶量23%
のマルチトールとアスコルビン酸ナトリウムとの混合水
溶液のマスキットを得た。
<First Step> A mixed aqueous solution of maltitol having a purity of 99.0% [registered trademark of Towa Kasei Kogyo KK] and a ascorbic acid with a solid content ratio of 20:80 of 39% is prepared at a temperature of 60. Prepared at ℃, temperature 15 ℃ with stirring
The mixture was rapidly cooled to a mixed solution, and fine powdery maltitol with a solid content of 2% of the mixed aqueous solution was added as a seed crystal, and stirring was continued for 0.5 hour to sufficiently generate fine crystals, and the amount of suspended crystals was 23%.
A mass kit of a mixed aqueous solution of maltitol and sodium ascorbate was obtained.

【0054】<第二工程> 第一工程で得たマスキット
を噴霧乾燥装置に導入し、送風温度65℃、排風温度3
8℃、噴霧乾燥装置の底部に落下した粉末の温度が38
℃で、水分が4%になるように噴霧乾燥し、更に、得ら
れた粉末を38℃で1時間保持して熟成してから乾燥し
て本発明のアスコルビン酸ナトリウムとマルチトールと
の流動性の高い混合粉末組成物を得た。
<Second Step> The mass kit obtained in the first step was introduced into a spray dryer, and the air temperature was 65 ° C. and the air temperature was 3
8 ° C, the temperature of the powder dropped to the bottom of the spray dryer is 38
Spray-dried at 4 ° C. to a water content of 4%, and the obtained powder is kept at 38 ° C. for 1 hour for aging and then dried to obtain the fluidity of the sodium ascorbate of the present invention and maltitol. A high-mixture powder composition was obtained.

【0055】本実施例により得られたアスコルビン酸ナ
トリウムとマルチトールとの流動性の高い混合粉末組成
物の約50メッシュの粉末は水分0.2%で、このもの
を実施例1と同様にして測定した結果、安息角は34°
であり、外観は白色のサラサラした極めて流動性の優れ
た粉末であった。
The powder of about 50 mesh of the highly flowable mixed powder composition of sodium ascorbate and maltitol obtained in this example had a water content of 0.2%. As a result of measurement, the angle of repose is 34 °
It was a powder with a smooth white appearance and excellent flowability.

【0056】(実施例4)(Example 4)

【0057】<第一工程> 純度98%のマルチトール
[東和化成工業(株)製、登録商標レシス]と純度99.
8%のアスコルビン酸を固形分比率75:25の割合で
混合した水溶液を調製し、濃度85%まで濃縮した後、
90℃まで加熱してから15℃まで急速に冷却し、混合
水溶液の固形分に対して0.5%の微細なアスコルビン
酸と0.3%のマルチトール結晶[東和化成工業(株)
製、登録商標レシス]を種結晶として添加し、温度を1
5℃に保持しながらゆるやかに5時間撹拌した後に水を
加えて固形分濃度を78%に調整し、更に5時間撹拌し
て懸濁結晶量32%のマルチトールとアスコルビン酸と
の混合水溶液のマスキットを得た。
<First step> Maltitol having a purity of 98% [registered trademark resin, manufactured by Towa Chemical Industry Co., Ltd.] and a purity of 99.
After preparing an aqueous solution in which 8% ascorbic acid was mixed at a solid content ratio of 75:25 and concentrating it to a concentration of 85%,
After heating to 90 ℃, it is cooled rapidly to 15 ℃, 0.5% fine ascorbic acid and 0.3% maltitol crystals based on the solid content of the mixed aqueous solution [Towa Kasei Kogyo Co., Ltd.
Made, registered trademark Lesis] was added as a seed crystal, and the temperature was adjusted to 1
After gently stirring for 5 hours while maintaining at 5 ° C., water was added to adjust the solid content concentration to 78%, and the mixture was further stirred for 5 hours to prepare a mixed aqueous solution of maltitol and ascorbic acid having a suspended crystal content of 32%. I got a mask.

【0058】<第二工程> 第一工程で得たマスキット
を噴霧乾燥装置に導入し、送風温度68℃、排風温度3
8℃、噴霧乾燥装置の底部に落下した粉末の温度が38
℃で、水分が3.4%になるように噴霧乾燥し、更に、
得られた粉末を38℃で15時間保持して熟成してから
乾燥して本発明のアスコルビン酸とマルチトールとの流
動性の高い混合粉末組成物を得た。
<Second Step> The mass kit obtained in the first step was introduced into a spray dryer, and the air temperature was 68 ° C. and the air temperature was 3
8 ° C, the temperature of the powder dropped to the bottom of the spray dryer is 38
At ℃, spray dry so that the water content is 3.4%,
The obtained powder was kept at 38 ° C. for 15 hours to be aged and then dried to obtain a highly fluid mixed powder composition of ascorbic acid and maltitol of the present invention.

【0059】本実施例により得られたアスコルビン酸と
マルチトールとの流動性の高い混合粉末組成物の水分は
0.3%で、約50メッシュの粉末を実施例1と同様に
して測定した結果、安息角は31°であり、外観は白色
のサラサラした極めて流動性の優れた粉末であった。
The highly fluid mixed powder composition of ascorbic acid and maltitol obtained in this example had a water content of 0.3%, and a powder of about 50 mesh was measured as in Example 1. The angle of repose was 31 °, and the powder was white and had a smooth appearance and was extremely fluid.

【0060】[0060]

【比較例】[Comparative example]

【0061】(比較例1)(Comparative Example 1)

【0062】<第一工程> 純度83%のマルチトール
と純度99.9%のアスコルビン酸を固形分比率17:
83の割合で混合した水溶液を調製し、濃度85%まで
濃縮した後、110℃まで加熱してから15℃まで急速
に冷却し、混合水溶液の固形分に対して0.5%の微細
なアスコルビン酸を種結晶として添加し、温度を15℃
に保持しながらゆるやかに12時間撹拌した後に水を加
えて固形分濃度を78%に調整し、更に5時間撹拌して
マルチトールとアスコルビン酸との混合水溶液のマスキ
ットを得た。
<First Step> Maltitol with a purity of 83% and ascorbic acid with a purity of 99.9% were used in a solid content ratio of 17:
Prepare an aqueous solution mixed at a ratio of 83, concentrate it to a concentration of 85%, then heat it to 110 ° C. and then rapidly cool it to 15 ° C. Add the acid as seed crystals and raise the temperature to 15 ° C.
The mixture was stirred for 12 hours while maintaining the temperature at 0.degree. C., water was added to adjust the solid content concentration to 78%, and the mixture was further stirred for 5 hours to obtain a mass kit of a mixed aqueous solution of maltitol and ascorbic acid.

【0063】<第二工程> 第一工程で得たマスキット
を噴霧乾燥装置に導入し、送風温度70℃、排風温度4
0℃の条件で噴霧乾燥した結果、噴霧乾燥装置のアトマ
イザーの周囲の壁に黄色いガラス状の固形物が付着、堆
積してしまい、噴霧乾燥操作を継続することができなか
った。
<Second Step> The mass kit obtained in the first step was introduced into a spray dryer, and the blowing temperature was 70 ° C. and the exhaust temperature was 4
As a result of spray-drying under the condition of 0 ° C., yellow glass-like solid matter adhered and accumulated on the wall around the atomizer of the spray-drying apparatus, and the spray-drying operation could not be continued.

【0064】また、堆積したガラス状固形物を掻き落と
したが、塊状であり、安息角は測定できなかった。
The deposited glassy solid was scraped off, but it was lumpy and the angle of repose could not be measured.

【0065】(比較例2)(Comparative Example 2)

【0066】<第一工程> 純度99.9%の市販のア
スコルビン酸を用いて実施例1と同様にしてアスコルビ
ン酸マスキットを得た。
<First Step> A commercially available ascorbic acid having a purity of 99.9% was used to obtain an ascorbic acid mass kit in the same manner as in Example 1.

【0067】純度98%の食品用マルチトール[東和化
成工業(株)製、登録商標レシス]を濃度65%に調整
し、加熱して温度を110℃にした後、撹拌しながら温
度5℃まで急激に冷却して液固形分に対して0.2%の
微細なマルチトール結晶を種結晶として添加し、毎分2
0回転のゆっくりとした撹拌を10時間続けて懸濁結晶
量3%のマルチトールマスキットを得た。
Maltitol for food [purity 98%, manufactured by Towa Kasei Kogyo Co., Ltd., registered trademark Lesis] was adjusted to a concentration of 65%, heated to 110 ° C. and then heated to 5 ° C. with stirring. Cool rapidly and add 0.2% of fine maltitol crystals to the liquid solids as seed crystals.
Slow stirring with 0 rotation was continued for 10 hours to obtain a maltitol mass kit having a suspended crystal amount of 3%.

【0068】<第二工程> 第一工程で得た各々のマス
キットをポンプで噴霧乾燥装置に送入する際に、アスコ
ルビン酸が17、マルチトールが83の固形分比率と
し、噴霧乾燥装置に入る直前に両者の配管が接続して一
本の配管から各マスキットが導入されるよう調整し、送
風温度70℃、排風温度40℃の条件で運転したとこ
ろ、噴霧乾燥装置の壁に液の飛沫が付着して流れ落ち、
噴霧乾燥操作が不可能であった。
<Second Step> When each of the mass kits obtained in the first step is fed into the spray dryer by a pump, the solid content ratio of ascorbic acid is 17 and maltitol is 83, and the mixture enters the spray dryer. Immediately before, both pipes were connected and adjusted so that each mass kit was introduced from one pipe, and when operated under the conditions of a blast temperature of 70 ° C and an exhaust air temperature of 40 ° C, the liquid sprayed on the wall of the spray dryer. Adheres and flows off,
The spray drying operation was impossible.

【0069】(比較例3)(Comparative Example 3)

【0070】<第一工程> 純度99.9%の市販のア
スコルビン酸を濃度32%に調整し、温度100℃まで
加熱した後、撹拌しながら温度15℃まで急激に冷却し
て微細な結晶を析出させ、そのまま温度を15℃に保持
して、毎分20回転のゆっくりとした撹拌を0.5時間
続け、アスコルビン酸マスキットを得た。
<First Step> Commercially available ascorbic acid having a purity of 99.9% was adjusted to a concentration of 32%, heated to a temperature of 100 ° C., and then rapidly cooled to a temperature of 15 ° C. with stirring to form fine crystals. Precipitation was performed, the temperature was kept at 15 ° C., and slow stirring at 20 rpm was continued for 0.5 hours to obtain an ascorbic acid maskit.

【0071】純度98%の食品用マルチトール[東和化
成工業(株)製、登録商標レシス]を濃度84%に調整
し、加熱して温度を110℃にした後、撹拌しながら温
度15℃まで急激に冷却して結晶を析出させ、毎分20
回転のゆっくりとした撹拌を10時間続けた後水を加え
て濃度を82%に調節し、更に3時間撹拌を続けて懸濁
結晶量39%のマルチトールマスキットを得た。
Maltitol for food [purity 98%, Towa Kasei Kogyo Co., Ltd., registered trademark Lesis] was adjusted to a concentration of 84%, heated to 110 ° C., and then stirred to a temperature of 15 ° C. Cool rapidly to precipitate crystals, 20 minutes per minute
After slowly stirring the mixture for 10 hours, water was added to adjust the concentration to 82%, and the mixture was further stirred for 3 hours to obtain a maltitol mass kit with a suspended crystal content of 39%.

【0072】<第二工程> 第一工程で得た各々のマス
キットをポンプで噴霧乾燥装置に送入しようとしたが、
アスコルビン酸マスキットとマルチトールマスキットの
両方が配管内で固化し、噴霧乾燥操作ができなかった。
<Second Step> Each mass kit obtained in the first step was tried to be pumped into the spray dryer.
Both the ascorbic acid maskit and the maltitol maskit solidified in the pipe and the spray drying operation could not be performed.

【0073】[0073]

【発明の効果】【The invention's effect】

【0074】本発明によると、成分の偏りや流動性など
の課題を解決しつつ、アスコルビン酸とマルチトールと
の混合粉末組成物を経済的に有利に製造できる。
According to the present invention, a mixed powder composition of ascorbic acid and maltitol can be produced economically and advantageously while solving the problems of component bias and fluidity.

【0075】すなわち、本発明の方法は、加熱や乾燥操
作の部分が比較的短時間に終了するもので、強い加熱や
ニーダー法のような機械的に強い混練をする必要がない
ので成分に着色することがなく、複雑な構造の特殊な機
器も要求されないので経済的に有利な方法であり、本発
明の方法を経由することにより得られる製品は、極めて
流動性が高く、輸送や保管の間に振動等によって成分の
偏りを生じることがなく、且つ、共存するマルチトール
によってアスコルビン酸の分解が抑制されるので保存性
が改善されており、従って、各種用途に用いた場合に性
質や味、効果などにばらつきが出ないという有利な特徴
がある。
That is, in the method of the present invention, the heating and drying operations are completed in a relatively short time, and there is no need for strong heating or mechanically strong kneading such as the kneader method, so that the components are colored. It is an economically advantageous method because it does not require special equipment with complicated structure, and the product obtained by passing through the method of the present invention has extremely high fluidity and is not easily stored during transportation or storage. Does not cause bias of the components due to vibration, etc., and the storage stability is improved because the decomposition of ascorbic acid is suppressed by the coexisting maltitol, therefore, the properties and taste when used in various applications, It has an advantageous feature that the effects do not vary.

【0076】また、本発明を実施することで得られる製
品は、従来品に比べて吸湿性が低いので、貯蔵中の固結
が生じにくいなどの有利な性質も備えている。
Further, the product obtained by carrying out the present invention has a lower hygroscopicity than the conventional product, and therefore has an advantageous property such that it is hard to be solidified during storage.

Claims (3)

【特許請求の範囲】[Claims] 【請求項1】 アスコルビン酸とマルチトールとの流動
性の高い混合粉末組成物を製造する方法において、 1)マルチトール純度が85〜99.9重量%で固形分
濃度が70〜90重量%のマルチトール水溶液から、懸
濁結晶量10〜70重量%のマルチトールマスキット
を、純度98以上のアスコルビン酸の水溶液からマスキ
ットを、それぞれ調製する第一工程、 2)マルチトールマスキットの導入割合を固形分で5〜
80重量%、アスコルビン酸のマスキットの導入割合を
固形分で20〜95重量%の割合に保ち、各々のマスキ
ットを噴霧乾燥装置に導入し、送風温30〜75℃で噴
霧乾燥する第二工程、の2工程を逐次的に経由すること
を特徴とする、アスコルビン酸とマルチトールとの流動
性の高い混合粉末組成物の製造方法。
1. A method for producing a highly fluid mixed powder composition of ascorbic acid and maltitol, comprising: 1) a maltitol purity of 85 to 99.9% by weight and a solid content concentration of 70 to 90% by weight. The first step of preparing a maltitol mass kit having an amount of suspended crystals of 10 to 70% by weight from an aqueous solution of maltitol and a mass kit from an aqueous solution of ascorbic acid having a purity of 98 or more. 5 to 5 solids
80% by weight, the introduction rate of the ascorbic acid maskit is maintained at a proportion of 20 to 95% by weight in terms of solid content, each maskit is introduced into a spray dryer, and a second step of spray drying at a blast temperature of 30 to 75 ° C. The method for producing a mixed powder composition having a high fluidity of ascorbic acid and maltitol, which comprises sequentially passing through the two steps.
【請求項2】 第一工程において、濃度20〜35%の
アスコルビン酸純度98以上の水溶液からアスコルビン
酸マスキットを調製し、且つマルチトールマスキットの
懸濁結晶量が10〜40重量%に調節されたものであ
る、請求項1に記載のアスコルビン酸とマルチトールと
の流動性の高い混合粉末組成物の製造方法。
2. In the first step, an ascorbic acid maskit is prepared from an aqueous solution having a purity of 98 or more with an ascorbic acid concentration of 20 to 35%, and the amount of suspended crystals of the maltitol maskit is adjusted to 10 to 40% by weight. The method for producing a highly flowable mixed powder composition of ascorbic acid and maltitol according to claim 1, wherein
【請求項3】 アスコルビン酸とマルチトールとの流動
性の高い混合粉末組成物を製造する方法において、 1)純度90〜99.9重量%のマルチトールを固形分
比率で5〜80重量%、純度98%以上のアスコルビン
酸を固形分比率で20〜95重量%含有する固形分濃度
20〜85重量%の水溶液を調製し、温度10〜60℃
まで冷却し、必要に応じて種結晶の添加及び希釈をして
更に撹拌し、アスコルビン酸とマルチトールとの混合水
溶液のマスキットを調製する第一工程、 2)第一工程で得られたアスコルビン酸とマルチトール
との混合水溶液のマスキットを噴霧乾燥装置に導入し、
送風温30〜75℃で噴霧乾燥する第二工程、の2工程
を逐次的に経由することを特徴とする、アスコルビン酸
とマルチトールとの流動性の高い混合粉末組成物の製造
方法。
3. A method for producing a highly fluid mixed powder composition of ascorbic acid and maltitol, comprising: 1) maltitol having a purity of 90 to 99.9% by weight in a solid content ratio of 5 to 80% by weight; An aqueous solution having a solid content concentration of 20 to 85 wt% containing 20 to 95 wt% of ascorbic acid having a purity of 98% or more in a solid content ratio was prepared, and the temperature was 10 to 60 ° C.
The first step of preparing a mass kit of a mixed aqueous solution of ascorbic acid and maltitol, which is cooled to 40 ° C., added and diluted with seed crystals as needed, and further stirred, 2) the ascorbic acid obtained in the first step Introduce the mass kit of the mixed aqueous solution of and maltitol into the spray dryer,
A method for producing a highly fluid mixed powder composition of ascorbic acid and maltitol, which comprises sequentially passing through two steps of a second step of spray drying at a blast temperature of 30 to 75 ° C.
JP34431295A 1995-12-06 1995-12-06 Method for producing mixed powder composition of ascorbic acid and maltitol having high fluidity Expired - Lifetime JP3955088B2 (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
JP34431295A JP3955088B2 (en) 1995-12-06 1995-12-06 Method for producing mixed powder composition of ascorbic acid and maltitol having high fluidity

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
JP34431295A JP3955088B2 (en) 1995-12-06 1995-12-06 Method for producing mixed powder composition of ascorbic acid and maltitol having high fluidity

Publications (2)

Publication Number Publication Date
JPH09157285A true JPH09157285A (en) 1997-06-17
JP3955088B2 JP3955088B2 (en) 2007-08-08

Family

ID=18368273

Family Applications (1)

Application Number Title Priority Date Filing Date
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Country Status (1)

Country Link
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Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2018212264A1 (en) * 2017-05-19 2018-11-22 日産化学株式会社 Nano-functional particles including hydrophilic substance and method for producing nano-functional particles
JP2022044833A (en) * 2019-12-27 2022-03-17 三井製糖株式会社 Method for producing granule, and granule
WO2024014033A1 (en) * 2022-07-15 2024-01-18 Dm三井製糖株式会社 Method for producing granules, and granules

Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2018212264A1 (en) * 2017-05-19 2018-11-22 日産化学株式会社 Nano-functional particles including hydrophilic substance and method for producing nano-functional particles
JP2022044833A (en) * 2019-12-27 2022-03-17 三井製糖株式会社 Method for producing granule, and granule
WO2024014033A1 (en) * 2022-07-15 2024-01-18 Dm三井製糖株式会社 Method for producing granules, and granules
JP2024011889A (en) * 2022-07-15 2024-01-25 Dm三井製糖株式会社 Method for producing granules, and granules

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