KR100262379B1 - Highly dispersible food additive and food composition containing the same - Google Patents

Highly dispersible food additive and food composition containing the same Download PDF

Info

Publication number
KR100262379B1
KR100262379B1 KR1019970702896A KR19970702896A KR100262379B1 KR 100262379 B1 KR100262379 B1 KR 100262379B1 KR 1019970702896 A KR1019970702896 A KR 1019970702896A KR 19970702896 A KR19970702896 A KR 19970702896A KR 100262379 B1 KR100262379 B1 KR 100262379B1
Authority
KR
South Korea
Prior art keywords
calcium
weight
ferric pyrophosphate
slurry
powder
Prior art date
Application number
KR1019970702896A
Other languages
Korean (ko)
Other versions
KR970706739A (en
Inventor
히사카즈 호조
가요코 하시모토
나오키 구보타
시로 미나요시
Original Assignee
마루오 기헤이
마루오 칼슘 가부시키가이샤
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 마루오 기헤이, 마루오 칼슘 가부시키가이샤 filed Critical 마루오 기헤이
Publication of KR970706739A publication Critical patent/KR970706739A/en
Application granted granted Critical
Publication of KR100262379B1 publication Critical patent/KR100262379B1/en

Links

Classifications

    • AHUMAN NECESSITIES
    • A23FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
    • A23LFOODS, FOODSTUFFS, OR NON-ALCOHOLIC BEVERAGES, NOT COVERED BY SUBCLASSES A21D OR A23B-A23J; THEIR PREPARATION OR TREATMENT, e.g. COOKING, MODIFICATION OF NUTRITIVE QUALITIES, PHYSICAL TREATMENT; PRESERVATION OF FOODS OR FOODSTUFFS, IN GENERAL
    • A23L29/00Foods or foodstuffs containing additives; Preparation or treatment thereof
    • AHUMAN NECESSITIES
    • A23FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
    • A23CDAIRY PRODUCTS, e.g. MILK, BUTTER OR CHEESE; MILK OR CHEESE SUBSTITUTES; MAKING THEREOF
    • A23C9/00Milk preparations; Milk powder or milk powder preparations
    • A23C9/152Milk preparations; Milk powder or milk powder preparations containing additives
    • A23C9/154Milk preparations; Milk powder or milk powder preparations containing additives containing thickening substances, eggs or cereal preparations; Milk gels
    • A23C9/1544Non-acidified gels, e.g. custards, creams, desserts, puddings, shakes or foams, containing eggs or thickening or gelling agents other than sugar; Milk products containing natural or microbial polysaccharides, e.g. cellulose or cellulose derivatives; Milk products containing nutrient fibres
    • AHUMAN NECESSITIES
    • A23FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
    • A23CDAIRY PRODUCTS, e.g. MILK, BUTTER OR CHEESE; MILK OR CHEESE SUBSTITUTES; MAKING THEREOF
    • A23C9/00Milk preparations; Milk powder or milk powder preparations
    • A23C9/12Fermented milk preparations; Treatment using microorganisms or enzymes
    • A23C9/123Fermented milk preparations; Treatment using microorganisms or enzymes using only microorganisms of the genus lactobacteriaceae; Yoghurt
    • AHUMAN NECESSITIES
    • A23FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
    • A23CDAIRY PRODUCTS, e.g. MILK, BUTTER OR CHEESE; MILK OR CHEESE SUBSTITUTES; MAKING THEREOF
    • A23C9/00Milk preparations; Milk powder or milk powder preparations
    • A23C9/152Milk preparations; Milk powder or milk powder preparations containing additives
    • AHUMAN NECESSITIES
    • A23FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
    • A23CDAIRY PRODUCTS, e.g. MILK, BUTTER OR CHEESE; MILK OR CHEESE SUBSTITUTES; MAKING THEREOF
    • A23C9/00Milk preparations; Milk powder or milk powder preparations
    • A23C9/152Milk preparations; Milk powder or milk powder preparations containing additives
    • A23C9/1522Inorganic additives, e.g. minerals, trace elements; Chlorination or fluoridation of milk; Organic salts or complexes of metals other than natrium or kalium; Calcium enrichment of milk
    • AHUMAN NECESSITIES
    • A23FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
    • A23LFOODS, FOODSTUFFS, OR NON-ALCOHOLIC BEVERAGES, NOT COVERED BY SUBCLASSES A21D OR A23B-A23J; THEIR PREPARATION OR TREATMENT, e.g. COOKING, MODIFICATION OF NUTRITIVE QUALITIES, PHYSICAL TREATMENT; PRESERVATION OF FOODS OR FOODSTUFFS, IN GENERAL
    • A23L29/00Foods or foodstuffs containing additives; Preparation or treatment thereof
    • A23L29/015Inorganic compounds
    • AHUMAN NECESSITIES
    • A23FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
    • A23LFOODS, FOODSTUFFS, OR NON-ALCOHOLIC BEVERAGES, NOT COVERED BY SUBCLASSES A21D OR A23B-A23J; THEIR PREPARATION OR TREATMENT, e.g. COOKING, MODIFICATION OF NUTRITIVE QUALITIES, PHYSICAL TREATMENT; PRESERVATION OF FOODS OR FOODSTUFFS, IN GENERAL
    • A23L29/00Foods or foodstuffs containing additives; Preparation or treatment thereof
    • A23L29/20Foods or foodstuffs containing additives; Preparation or treatment thereof containing gelling or thickening agents
    • A23L29/206Foods or foodstuffs containing additives; Preparation or treatment thereof containing gelling or thickening agents of vegetable origin
    • A23L29/256Foods or foodstuffs containing additives; Preparation or treatment thereof containing gelling or thickening agents of vegetable origin from seaweeds, e.g. alginates, agar or carrageenan
    • AHUMAN NECESSITIES
    • A23FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
    • A23LFOODS, FOODSTUFFS, OR NON-ALCOHOLIC BEVERAGES, NOT COVERED BY SUBCLASSES A21D OR A23B-A23J; THEIR PREPARATION OR TREATMENT, e.g. COOKING, MODIFICATION OF NUTRITIVE QUALITIES, PHYSICAL TREATMENT; PRESERVATION OF FOODS OR FOODSTUFFS, IN GENERAL
    • A23L33/00Modifying nutritive qualities of foods; Dietetic products; Preparation or treatment thereof
    • A23L33/10Modifying nutritive qualities of foods; Dietetic products; Preparation or treatment thereof using additives
    • A23L33/16Inorganic salts, minerals or trace elements

Landscapes

  • Chemical & Material Sciences (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Polymers & Plastics (AREA)
  • Food Science & Technology (AREA)
  • Nutrition Science (AREA)
  • Health & Medical Sciences (AREA)
  • Inorganic Chemistry (AREA)
  • Dispersion Chemistry (AREA)
  • Mycology (AREA)
  • Microbiology (AREA)
  • Coloring Foods And Improving Nutritive Qualities (AREA)
  • General Preparation And Processing Of Foods (AREA)
  • Jellies, Jams, And Syrups (AREA)

Abstract

탄산칼슘, 인산칼슘 및 피로인산제2철로 이루어지는 군에서 선택된 1종 100중량부에 대하여 알긴산프로필렌글리콜에스테르를 1.5∼40중량부 첨가하여 이루어지는 식품첨가제를 제공한다. 본 발명의 식품첨가제는 액 중에서의 재분산성, 장기안정성 및 풍미가 우수하고, 이 첨가제를 함유하여 이루어지는 식품조성물은 중성, 산성 어느 영역에 있어서도 장기간의 보존안정성이 매우 양호하다.Provided is a food additive comprising 1.5 to 40 parts by weight of propylene glycol alginate based on 100 parts by weight of one kind selected from the group consisting of calcium carbonate, calcium phosphate and ferric pyrophosphate. The food additive of the present invention is excellent in redispersibility, long-term stability and flavor in the liquid, and the food composition containing this additive has very good long-term storage stability in both neutral and acidic regions.

Description

고분산성을 갖는 식품첨가제 및 이것을 함유하는 식품조성물{HIGHLY DISPERSIBLE FOOD ADDITIVE AND FOOD COMPOSITION CONTAINING THE SAME}Highly dispersible food additives and food compositions containing them {HIGHLY DISPERSIBLE FOOD ADDITIVE AND FOOD COMPOSITION CONTAINING THE SAME}

최근, 칼슘 섭취량의 부족이 지적되고 있고, 이 경향은 성장기의 어린이와 노인에 있어서 현저하다. 이 칼슘섭취량 부족을 해소하기 위하여 칼슘강화식품이 판매되고 있으며, 일반적으로 칼슘함유량이 많은 것으로 되어 있는 우유에 마저도 다시 칼슘을 첨가하여 칼슘강화우유로서 제공하는 것이 시도되고 있고, 기타, 요구르트, 쥬스, 밀크분말류에도 칼슘강화된 상품이 다수 판매되고 있다.In recent years, a lack of calcium intake has been pointed out, and this tendency is remarkable in the growing children and the elderly. In order to alleviate this lack of calcium intake, calcium fortified foods are sold. In general, it is also attempted to add calcium to milk which has a high calcium content and provide it as calcium fortified milk. Others include yogurt, juice, Milk powder is also sold in a number of calcium-enriched products.

예컨대 요구르트 등의 산성식품에 칼슘을 강화할 목적으로 유산칼슘, 염화칼슘 등의 수용성의 무기 또는 유기산칼슘 형태의 칼슘, 탄산칼슘, 인산칼슘 등의 수불용성의 무기 형태의 칼슘이 첨가되어 사용되고 있다.For example, water-insoluble inorganic forms such as calcium lactate and calcium chloride, or water-insoluble inorganic forms such as calcium carbonate, calcium phosphate, and the like are added to acidic foods such as yogurt for the purpose of strengthening calcium.

그러나, 수용성의 무기 또는 유기산칼슘 형태의 칼슘은 요구르트 중의 단백질의 안정성을 저해하기 쉽기 때문에 일정량 이상의 배합이 곤란하여, 칼슘 원료로서 다량으로 사용할 수 없다는 결점이 있었다.However, water-soluble inorganic or organic calcium calcium forms tend to impair the stability of proteins in yoghurt, so that a certain amount or more of compounding is difficult and cannot be used in large amounts as a calcium raw material.

한편, 수불용성의 무기 형태의 칼슘은 수불용성 때문에 요구르트 중의 단백질의 안정성을 저해하는 일이 없으므로 첨가량의 관점에서는 다량으로 사용하는 것이 가능하나, 이 무기 형태의 칼슘은 전반적으로 비중이 3 전후로 높아서, 요구르트 중에 분산시킬 경우 단시간에 침전하기 때문에 식품으로서의 미관상 바람직하지 않으며, 결국 그 첨가량은 제한되어 다량으로 사용할 수 없다는 결점이 있었다.On the other hand, since the water-insoluble inorganic form of calcium does not impair the stability of the protein in yogurt because of the water insolubility, it is possible to use a large amount from the viewpoint of the added amount. In the case of dispersion in yogurt, it is undesirably desirable as a food because it is precipitated in a short time, and in the end, the amount of addition is limited and cannot be used in large quantities.

식품용도, 예컨대 요구르트 중에 사용하는 무기 형태의 칼슘제 슬러리의 제조방법으로는 결정셀룰로스를 동시에 첨가하여 그 그물망 구조에 의해 탄산칼슘입자를 지지시키는 방법(특개소 56-117753호), 및 슬러리상 탄산칼슘 또는 슬러리상 탄산칼슘에 HLB 10 이상의 친수성 유화제를 첨가한 것에 초음파를 조사하여 탄산칼슘의 분산성을 개량하는 방법(특개소 64-69513호) 등이 제안되어 있다.As a method for preparing an inorganic calcium slurry for use in food, such as yoghurt, a method for supporting calcium carbonate particles by adding crystalline cellulose at the same time (particularly 56-117753), and slurry calcium carbonate Or the method which improves the dispersibility of calcium carbonate by irradiating ultrasonic wave to the addition of the hydrophilic emulsifier of HLB10 or more to slurry calcium carbonate (Patent No. 64-69513), etc. is proposed.

그러나, 상기 특개소 64-117753호와 같이 결정셀룰로스를 첨가하는 방법은 제품 점도가 매우 높아지기 때문에 식감상(食感上) 바람직하지 않다.However, the method of adding crystalline cellulose as in Japanese Patent Laid-Open No. 64-117753 is not preferable because of the high viscosity of the product.

또, 특개소 64-69513호와 같이, 탄산칼슘 슬러리에 자당(蔗糖)지방산에스테르를 첨가제로서 사용하여 분산시키는 방법은 우유와 같은 중성 또는 약산성 제품에 대하여 어느 정도 유효한 효과를 보이는데 불과하고, 예컨대 요구르트와 같은 산성영역을 띄는 제품에 대해서는 자당지방산에스테르가 산에 대하여 불안정한 상태가 되기 쉬워 분산 불량을 일으키는 경향이 있어 그다지 바람직하지 않다.In addition, as disclosed in Japanese Patent Application Laid-Open No. 64-69513, the method of dispersing the sucrose fatty acid ester in the calcium carbonate slurry as an additive shows only a somewhat effective effect on neutral or weakly acidic products such as milk. For products having an acidic region such as sucrose, fatty acid esters are not preferable because they tend to be unstable to acids and cause poor dispersion.

또, 이들 방법의 경우, 수분산액 중의 탄산칼슘 고형분 농도가 10중량% 전후로 매우 낮기 때문에, 우유첨가용 탄산칼슘으로 전국에서 널리 사용될 경우, 그 수송용기비용 및 유통비가 매우 높아질 뿐만아니라, 그 형태가 수분산액이기 때문에 부패되기 쉬워 항상 냉장수송, 냉장보관이 필요하기 때문에 이 방법은 경제적으로 양호한 방법이 못된다.In addition, in the case of these methods, the calcium carbonate solids concentration in the aqueous dispersion is very low, around 10% by weight, so that when used widely in the country as milk carbonate calcium carbonate, the transportation container cost and distribution cost not only become very high, but also the form This method is not economically good because it is easy to rot because it is an aqueous dispersion, and therefore requires refrigeration and storage.

최근, 드링크타입의 요구르트, 우유, 쥬스류 액체식품의 장기간 보존가능한 용기, 보존방법의 진보에 따라 그 식품을 판매점, 자동판매기, 가정내 대형냉장고 등에 장기간 보존하는 케이스가 증가하고 있고, 동종의 액체식품에 칼슘강화 목적으로 첨가되는 무기칼슘염 입자는 해당 식품 중에서의 분산상태가 양호하지 않을 경우, 장기간의 액체식품 보존 동안에 식품용기 저부에 침전되어, 요구르트, 우유, 쥬스류 액체식품을 음용할 때 해당 침전물이 음용자에게 불쾌감, 불청결감을 주는 일이 많다.In recent years, with the advancement of containers for long-term storage of liquid foods such as yogurt, milk, and juices, and the advancement of the preservation method, the case of storing the food for a long time in stores, vending machines, large refrigerators in the home, etc. is increasing. Inorganic calcium salt particles added for the purpose of calcium fortification are precipitated at the bottom of the food container during long-term liquid food preservation if the dispersion state in the food is not good, and the corresponding precipitate when drinking the liquid food of yogurt, milk and juice. There is a lot of unpleasantness and unpleasantness to this drinker.

따라서, 현재 칼슘강화 목적으로 종래기술로 조제된 무기칼슘염 입자를 첨가하여 시판되고 있는 액체식품류는 해당 무기입자 식품 중에서의 분산안정성 기간이 짧기 때문에 해당 무기입자 첨가량은 극소량으로 제한되고, 또 일반소비자가 구입후 1

Figure pct00001
2일간에 반드시 식용해야 하는 액체식품에 제한되는 문제점이 있다.Therefore, liquid foods currently marketed by adding inorganic calcium salt particles prepared in the prior art for the purpose of strengthening calcium have a short dispersion stability period in the inorganic particle foods, and therefore the amount of the inorganic particles added is limited to a very small amount. After purchase 1
Figure pct00001
There is a problem that is limited to liquid food that must be edible in two days.

한편, 최근, 철분부족에 의한 빈혈증상을 일으키는 여성이 다수 발견된다. 이 경향은 여고생이나 젊은 성인여성에 있어서 특히 현저하다. 이 철결핍성 빈혈의 원인은 식생활에서 유래하는 점이 가장 크지만, 여성의 경우는 생리적 출혈, 임신에 따른 철수요증가, 및 다이어트에 의한 섭취부족 등, 철부족에 의한 빈혈이 되기 쉬운 환경하에 있고, 일반적으로 약 반수의 여성은 철이 부족하다고 언급되고 있다. 이 철부족을 해소하기 위하여 철분강화식품이 판매되기에 이르렀고, 우유, 청량음료수 등에 철분을 강화한 상품도 다수 판매되기 시작하고 있다.On the other hand, in recent years, many women who cause anemia symptoms due to iron deficiency have been found. This tendency is particularly pronounced in high school girls and young adult women. The most common cause of iron deficiency anemia is from diet, but in women, it is prone to anemia due to iron deficiency, such as physiological bleeding, increased withdrawal demand due to pregnancy, and insufficient dietary intake. In general, about half of women are said to lack iron. Iron-reinforced foods have been sold to alleviate this iron shortage, and a number of products fortified with iron, such as milk and soft drinks, are also beginning to be sold.

예컨대, 청량음료수 등에 있어서, 철분을 강화할 목적으로 유산철, 구연산철나트륨, 글루콘산제1철 등의 수용성의 유기 또는 무기 형태의 철이나 피로인산제2철 등의 수불용성 또는 난용성의 무기 형태의 철이 첨가 사용되고 있다. 그러나, 수용성의 유기 또는 무기 형태의 철은 철미(鐵味)가 강해서, 식감문제로 한꺼번에 너무 많은 양을 사용할 수 없다는 결점이 있었다. 또, 피로인산제2철 등의 수불용성 또는 난용성의 무기 형태의 철의 분산체를 이용할 경우는, 철취(鐵臭)는 개선되나 비중이 2.75 이상으로 높아서, 청량음료수 등에 분산시킬 경우 단시간에 침전하기 때문에 식품으로서의 미관상 바람직하지 않고, 결국 그 첨가량은 제한되어 다량으로 사용하는 것이 불가능하다는 결점이 있었다.For example, in soft drinks, water insoluble or poorly soluble inorganic forms such as iron or ferric pyrophosphate, or water-soluble organic or inorganic forms of iron lactate, sodium iron citrate, ferrous gluconate, etc., for the purpose of strengthening iron. Iron is added and used. However, water-soluble organic or inorganic forms of iron have a strong iron content, and there is a drawback that too much quantity cannot be used at one time due to texture problems. In addition, in the case of using a water-insoluble or poorly soluble inorganic dispersion such as ferric pyrophosphate, iron odor is improved, but the specific gravity is higher than 2.75. There is a drawback that it is undesirably desirable as a food because of precipitation, and the amount of addition thereof is thus limited and cannot be used in large quantities.

본 발명은 이러한 실상을 감안하여, 상기와 같은 문제를 해결하여, 유통경제성이 우수하고 또한 액체식품 중에서의 장기간 분산안정성이 양호한 식품첨가물용 칼슘제 및/또는 철분제, 또한 이 식품첨가용 칼슘제 및/또는 철분제를 함유하여 이루어지는 식품조성물을 제공하는 것이다.In view of such a situation, the present invention has solved the above problems and has excellent distribution economy and good long-term dispersion stability in liquid foods, and / or iron additives for food additives, and also calcium additives for food additives and / or It is to provide a food composition containing iron powder.

(발명의 개시)(Initiation of invention)

본 발명자들은 상기 과제를 해결하고자 예의 검토한 결과, 특정의, 또한 특정량의 친수성 유화제를 사용함으로써 용이하게 장기간 분산안정성이 양호한 식품첨가물용 칼슘제 및/또는 철분제가 얻어지는 것을 발견하여 본 발명을 완성하였다.MEANS TO SOLVE THE PROBLEM As a result of earnestly examining in order to solve the said subject, the present inventors discovered that the calcium agent and / or iron powder for food additives which are excellent in long-term dispersion stability can be easily obtained by using a specific and specific amount of hydrophilic emulsifier, and completed this invention. .

즉, 본 발명은 탄산칼슘, 인산칼슘(이하, 칼슘제라 함) 및 피로인산제2철로 이루어지는 군에서 선택된 적어도 1종에 알긴산프로필렌글리콜에스테르(이하, PGA라 함)를 첨가하여 이루어지는 식품첨가제, 및 이 식품첨가제를 함유하여 이루어지는 식품조성물을 내용으로 한다.That is, the present invention is a food additive formed by adding an alginate propylene glycol ester (hereinafter referred to as PGA) to at least one selected from the group consisting of calcium carbonate, calcium phosphate (hereinafter referred to as calcium) and ferric pyrophosphate, and The food composition which contains this food additive is a content.

본 발명은 요구르트, 우유, 쥬스류 등의 식품에 첨가하여 칼슘 및/또는 철을 강화하는데 유효하게 이용되는, 액 중에서의 분산안정성이 양호한 식품첨가제에 관한 것이다.BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to a food additive having good dispersion stability in a liquid, which is added to foods such as yoghurt, milk, juice, and the like and effectively used to strengthen calcium and / or iron.

(발명을 실시하기 위한 최량의 형태)(The best form to carry out invention)

이하, 본 발명을 상술한다.Hereinafter, the present invention will be described in detail.

본 발명에 사용하는 탄산칼슘은 예컨대 탄산칼슘을 50중량% 이상 함유하는 코랄탄산칼슘, 중질탄산칼슘, 합성탄산칼슘을 들 수 있지만, 수산화칼슘의 수현탁액인 석회유와 탄산가스를 반응시키는 탄산가스법으로 대표되는 화학적 합성방법에 의해 조제되는 합성탄산칼슘이 바람직하다. 탄산가스법에 있어서 합성탄산칼슘을 조제할 때의 바람직한 방법으로는 이하에 제시하는 방법을 들 수 있다.Examples of the calcium carbonate used in the present invention include calcium carbonate, heavy calcium carbonate and synthetic calcium carbonate containing 50% by weight or more of calcium carbonate. However, the calcium carbonate is a carbon dioxide gas method in which lime oil, which is an aqueous suspension of calcium hydroxide, is reacted with carbon dioxide gas. The synthetic calcium carbonate prepared by the typical chemical synthesis method is preferable. The method shown below is mentioned as a preferable method at the time of preparing synthetic calcium carbonate in a carbon dioxide gas method.

석회유를 탄산가스를 이용하여 탄산화 반응시키고, 얻어지는 탄산칼슘의 수현탁액 조제공정에 있어서, 탄산화 반응종료하여 조제된 pH값이 K인 탄산칼슘의 수현탁액을 교반, 및/또는 습식분쇄, 및/또는 정치시켜, 해당 탄산칼슘의 수현탁액 pH를 아래 식(a)와 (b)를 만족하는 pH값 L로 상승시킨 후, 수현탁액 중에 존재하는 알칼리물질을 제거 및/또는 알칼리물질의 단위체적당 농도를 저하시키고, 탄산칼슘의 수현탁액 pH를 아래 식(c)를 만족하는 pH값 M으로 조정하여 탄산칼슘을 조제한다.In the step of preparing the aqueous suspension of calcium carbonate obtained by carbonizing the lime oil using carbon dioxide gas, the aqueous suspension of calcium carbonate having a pH value of K prepared by terminating the carbonation reaction is stirred, and / or wet pulverized, and / or After standing still, the aqueous suspension pH of the calcium carbonate is raised to a pH value L satisfying the following formulas (a) and (b), and then the alkali substance present in the aqueous suspension is removed and / or the concentration per unit volume of the alkali substance is determined. It lowers and adjusts the aqueous suspension pH of calcium carbonate to pH value M which satisfy | fills following formula (c), and prepares calcium carbonate.

L

Figure pct00002
8.6 (a)L
Figure pct00002
8.6 (a)

10(L+2)/10K

Figure pct00003
125 (b)10 (L + 2) / 10 K
Figure pct00003
125 (b)

10(M+2)/10L

Figure pct00004
80 (c)10 (M + 2) / 10 L
Figure pct00004
80 (c)

단, K, L은 동일 온도조건하의 pH이다. 또, pH값 M은 M이 8.6 미만일 경우, M은 8.6으로 계산.However, K and L are pH under the same temperature conditions. Moreover, pH value M calculates 8.6 when M is less than 8.6.

본 발명에 사용하는 인산칼슘이란 인산의 칼슘염으로 이루어지는 무기물을 지칭하고, 인산칼슘으로는 인산칼슘을 50중량% 이상 함유하는 천연인산칼슘, 우골(牛骨), 합성인산칼슘 등을 들 수 있고, 수산화칼슘, 탄산칼슘, 염화칼슘 등의 칼슘염과 인산, 인산소다 등의 인산염을 반응시키는 화학적 합성방법에 의해 조제되는 합성인산칼슘이 바람직하고, 그 중에서도 피로인산이수소칼슘, 인산일수소칼슘, 인산삼칼슘으로 이루어지는 군에서 선택되는 적어도 1종의 인산칼슘이 더욱 바람직하다.Calcium phosphate used in the present invention refers to an inorganic substance consisting of calcium salts of phosphoric acid, and examples of calcium phosphate include natural calcium phosphate, right bone, synthetic calcium phosphate containing 50% by weight or more of calcium phosphate, and the like. And synthetic calcium phosphates prepared by a chemical synthesis method in which calcium salts such as calcium hydroxide, calcium carbonate and calcium chloride and phosphates such as phosphoric acid and sodium phosphate are reacted, and among them, pyrohydrogen dihydrogen phosphate, calcium monohydrogen phosphate and phosphate More preferred is at least one calcium phosphate selected from the group consisting of tricalcium.

본 발명의 원료로서 사용하는 칼슘제, 즉 탄산칼슘 및/또는 인산칼슘의 형태에 관해서는 통상의 방법으로 조제되는 칼슘제의 수현탁액이라도 좋고, 또 해당 수현탁액을 통상법에 따라 탈수, 건조, 분쇄를 거쳐 조제되는 칼슘제 분체에, 재차 물을 첨가하여 조제되는 수현탁액도 좋으나, 식품첨가물 규격엄수, 및 위생관리면의 관점에서 후자의 형태를 채용하는 것이 바람직하다.As for the form of the calcium agent used as the raw material of the present invention, namely calcium carbonate and / or calcium phosphate, an aqueous suspension of a calcium agent prepared by a conventional method may be used, and the aqueous suspension is dehydrated, dried, and pulverized according to a conventional method. Although the water suspension prepared by adding water to the calcium powder to be prepared is also good, it is preferable to adopt the latter form in view of food additive standard adherence and hygiene management.

후자의 방법을 채용할 경우, 사용하는 탄산칼슘의 분체 pH에 관해서는 본 발명에 사용하는 친수성 유화제의 기능저하방지, 및 분쇄 및 분급시의 효율상승의 관점에서, 탄산칼슘분체의 고형분 농도가 20중량%인 수현탁액 200cc를 300W, 20kHz로 10분간 초음파 처리한 후의 수현탁액의 25℃에 있어서의 pH가 11.7 이하인 탄산칼슘 분체를 사용하는 것이 바람직하고, 더 바람직하게는 11.5 이하이다.When the latter method is employed, the solids concentration of the calcium carbonate powder is 20 in terms of preventing the degradation of the hydrophilic emulsifier used in the present invention and increasing the efficiency at the time of grinding and classing. It is preferable to use the calcium carbonate powder whose pH at 25 degreeC of the aqueous suspension after sonicating 200 weight% aqueous suspension 200 cc at 300 W and 20 kHz for 10 minutes, More preferably, it is 11.5 or less.

또, 본 발명의 원료로서 사용하는 칼슘제의 질소흡착법(BET법)에 의한 비표면적은 6m2/g∼60m2/g 범위가 바람직하다. 비표면적이 6m2/g 미만인 경우, 우유 등의 액체식품 중에서의 장기간 안정성에 문제가 생기고, 또, 60m2/g을 넘을 경우, 칼슘제 분체의 응집력이 매우 강해지기 때문에 그 분산이 곤란해진다.In addition, it is a specific surface area by nitrogen adsorption method (BET method) of calcium used as a raw material of the present invention is preferably 6m 2 / g~60m 2 / g range. When the specific surface area is less than 6 m 2 / g, there is a problem in long-term stability in liquid foods such as milk, and when it exceeds 60 m 2 / g, the cohesive force of the calcium powder becomes very strong, and its dispersion becomes difficult.

본 발명에 사용하는 피로인산제2철이란 화학적으로 합성하여 얻어지는 합성피로인산제2철이면 된다. 이하에 방법을 예시한다.The ferric pyrophosphate used in the present invention may be a synthetic ferric pyrophosphate obtained by chemical synthesis. The method is illustrated below.

수중에 염화제2철을 용해시키고, 이 용액에 피로인산나트륨을 온수에 녹인 액을 혼합하여 교반을 행한다. 반응종료후, 해당 용액을 필터프레스를 이용하여 탈수하고, 얻어진 탈수 케이크에 재차 물을 가하여 교반하고, 탈수전과 동일 농도의 피로인산제2철 수용액을 얻는다. 이 조작을 2회 반복한 후, 해당 피로인산제2철 수용액을 필터프레스로 탈수하여 그 프레스케이크를 패들드라이어로 건조하고, 건식분쇄기를 이용하여 피로인산제2철 분체를 조제한다. 또한, 본 발명에 사용하는 피로인산제2철 슬러리는 상기와 같이 건조, 분말화하지 않고, 슬러리 상태(피로인산제2철 액)로 사용하여도 상관없다.Ferric chloride is dissolved in water, and the solution in which sodium pyrophosphate is dissolved in warm water is mixed and stirred. After completion of the reaction, the solution was dehydrated using a filter press, water was added to the obtained dewatered cake again and stirred to obtain a ferric pyrophosphate aqueous solution having the same concentration as before dehydration. After repeating this operation twice, the ferric pyrophosphate aqueous solution is dewatered with a filter press, the press cake is dried with a paddle dryer, and ferric pyrophosphate powder is prepared using a dry mill. The ferric pyrophosphate slurry used in the present invention may be used in a slurry state (ferrous pyrophosphate liquid) without drying and powdering as described above.

또, 본 발명의 원료로서 사용하는 피로인산제2철 분체의 질소흡착법(BET법)에 의한 비표면적은 3m2/g∼50m2/g 범위가 바람직하다. 비표면적이 3m2미만인 경우, 우유 등의 액체식품 중에서의 장기간 안정성에 문제가 생기고, 또 50m2/g을 넘을 경우, 피로인산제2철 분체의 응집력이 매우 강해지기 때문에 그 분산이 곤란해진다.The specific surface area by the nitrogen adsorption method (BET method) of ferric pyrophosphate powder used as a raw material of the present invention is preferably from 3m 2 / g~50m 2 / g range. When the specific surface area is less than 3 m 2 , problems arise in the long-term stability in liquid foods such as milk, and when it exceeds 50 m 2 / g, the cohesive force of the ferric pyrophosphate powder becomes very strong, and its dispersion becomes difficult.

다음에, 상기 칼슘제 및 피로인산제2철로 이루어지는 군에서 선택된 적어도 1종과 PGA와 물의 혼합슬러리를 조제한다. 이 조제방법은 이하, (A), (B), (C)에 나타내는 3종류의 방법으로 대별되나, 어느 방법을 채용하거나, 또 조합하여 사용하여도 양호하다.Next, at least one selected from the group consisting of the calcium agent and the ferric pyrophosphate, and a mixed slurry of PGA and water are prepared. Although this preparation method is divided roughly into the three types of methods shown to (A), (B), (C) below, you may employ | adopt and use in combination any method.

(A) 칼슘제 및/또는 피로인산제2철과 물로 이루어지는 식품첨가제의 수현탁액을 화학적 분산방법, 분쇄기 및/또는 분산기를 사용하는 물리적 방법으로 분쇄 및/또는 분리처리 후, PGA를 첨가처리한다.(A) The aqueous suspension of the food additive consisting of calcium and / or ferric pyrophosphate and water is pulverized and / or separated by a physical method using a chemical dispersion method, a pulverizer and / or a disperser, and then PGA is added thereto.

(B) 칼슘제 및/또는 피로인산제2철과 PGA와 물로 이루어지는 식품첨가제의 수현탁액을, 화학적 분산방법, 분쇄기 및/또는 분산기를 사용하여 물리적 방법으로 분쇄 및/또는 분산처리한다.(B) The aqueous suspension of a food additive comprising calcium and / or ferric pyrophosphate, PGA and water is ground and / or dispersed by physical methods using a chemical dispersion method, a pulverizer and / or a disperser.

(C) 칼슘제 및/또는 피로인산제2철과 물로 이루어지는 식품첨가제의 수현탁액을 화학적 분산방법, 분쇄기 및/또는 분산기를 사용하는 물리적 방법으로 분쇄 및/또는 분산처리후, PGA를 첨가처리하고, 다시 분쇄기 및/또는 분산기를 사용하는 물리적 방법으로 분쇄 및/또는 분산처리한다.(C) the water suspension of the food additive consisting of calcium and / or ferric pyrophosphate and water is pulverized and / or dispersed by a physical method using a chemical dispersion method, a pulverizer and / or a disperser, and then PGA is added thereto. The milling and / or dispersing is carried out again by a physical method using a grinder and / or a disperser.

상기, (A), (B), (C)의 방법에 있어서, 칼슘제 및/또는 피로인산제2철과 PGA와 물의 혼합슬러리를 조제하는데 양호한 조건은 해당 혼합슬러리 중의 칼슘제 및/또는 철분제 100중량부에 대하여 PGA가 1.5∼40중량부 첨가되어 있는 것이 필요하고, 요구르트 등의 액체식품에 있어서 식감상의 목으로 넘어가는 맛 등을 고려할 경우, 바람직하게는 PGA가 1.5∼30중량부, 더 바람직하게는 5∼15중량부 첨가되어 있는 것이다.In the above methods (A), (B) and (C), the conditions for preparing a mixed slurry of a calcium agent and / or ferric pyrophosphate, PGA and water are 100 wt% of the calcium agent and / or iron powder in the mixed slurry. It is necessary that 1.5 to 40 parts by weight of PGA is added to the part, and in consideration of the taste that passes over the throat of the texture in liquid food such as yogurt, the PGA is preferably 1.5 to 30 parts by weight, more preferably. Preferably 5 to 15 parts by weight is added.

혼합슬러리 중의 칼슘제 및/또는 철분제의 입도분포에 있어서의 중량(체적)평균경 G(㎛)에 대해서는 하기 (α)의 요건을 구비하는 것이고, 상당히 장기간의 보존분산안정성이 요구되는 식품용도에는 (β)의 요건을 구비하는 것이 바람직하고 더 바람직하게는 (γ)의 요건을 구비하는 것이다.The weight (volume) average diameter G (µm) in the particle size distribution of the calcium agent and / or the iron powder in the mixed slurry has the following requirements (α), and for food applications that require long-term storage and dispersion stability ( It is preferable to satisfy the requirement of β), and more preferably, to satisfy the requirement of (γ).

(α) G

Figure pct00005
0.8(α) G
Figure pct00005
0.8

(β) 0.04

Figure pct00006
G 〈 0.5(β) 0.04
Figure pct00006
G <0.5

(γ) 0.04

Figure pct00007
G 〈 0.3(γ) 0.04
Figure pct00007
G <0.3

PGA의 첨가 중량부가 1.5중량부 미만인 경우, 예컨대 혼합 슬러리 중의 칼슘제 및/또는 철분제 입도분포에 있어서의 중량(체적)평균경을 매우 미세하게 조제했다 하더라도 이들 혼합슬러리, 또는 그 혼합슬러리를 건조분말화하여 얻어지는 칼슘제 및/또는 철분제의 파우더를 예컨대, 쥬스, 드링크 타입의 요구르트 등의 식품에 첨가사용할 경우, 식품 중의 칼슘제 및/또는 철분제의 경시 안정성이 악화되고, 심할 경우 24시간 이내에 식품용기저부에 응집, 침강한다.When the added weight of PGA is less than 1.5 parts by weight, even if the weight (volume) average diameter in the particle size distribution of the calcium and / or iron powder in the mixed slurry is prepared very finely, these mixed slurries or the mixed slurries are dry powdered. When the powder of calcium and / or iron powder obtained by adding to the food, for example, juice, drink type yogurt, etc., is used, the aging stability of the calcium and / or iron powder in food deteriorates, and in severe cases, it aggregates at the bottom of the food container within 24 hours. , Settle.

한편, PGA의 첨가 중량부가 40중량부를 넘을 경우, 혼합슬러리 또는 그 혼합슬러리를 건조분말화하여 얻어지는 칼슘제 및/또는 철분제 파우더를 쥬스, 드링크타입의 요구르트 등의 식품에 첨가사용할 경우, 제품 점도가 상승하여 식감상 바람직하지 않고, 심할 경우 불쾌감을 준다.On the other hand, when the added weight part of PGA exceeds 40 parts by weight, the product viscosity increases when calcium and / or iron powder obtained by dry powdering the mixed slurry or the mixed slurry is added to foods such as juice and drink yogurt. The texture is undesirable, and if it is severe, it gives a discomfort.

또, 예컨대 세트타입의 요구르트 등의 식품에 혼합슬러리, 또는 그 혼합슬러리를 건조분말화하여 얻어지는 칼슘제 및/또는 철분제 파우더를 사용할 경우, PGA의 첨가 중량부가 1.5중량부 미만인 경우, 또는 PGA의 첨가 중량부가 40중량부를 넘을 경우는, 조직적으로 양호한 제품을 얻을 수 없다.In the case of using a mixed slurry or a calcium and / or iron powder obtained by dry powdering the mixed slurry in a food such as a set-type yoghurt, for example, the added weight of PGA is less than 1.5 parts by weight or the added weight of PGA. When the addition exceeds 40 parts by weight, a product that is good in structure cannot be obtained.

혼합슬러리 중의 칼슘제 및/또는 철분제의 입도분포에 있어서의 중량(체적)평균경은 0.04∼0.8㎛ 범위가 바림직하다. 해당 평균경이 0.8㎛보다 클 경우는 침강되기 쉽기 때문에, 이들의 혼합슬러리, 또는 그 혼합슬러리를 건조분말하여 얻어지는 칼슘제 및/또는 철분제 파우더는 장기 보존가능한 식품용도에는 사용할 수 없다.The weight (volume) average diameter in the particle size distribution of the calcium agent and / or iron powder in the mixed slurry is preferably in the range of 0.04 to 0.8 µm. If the average diameter is larger than 0.8 mu m, it is easy to settle, and therefore, the mixed slurry or the calcium and / or iron powder obtained by dry powdering the mixed slurry cannot be used for foods that can be stored for a long time.

혼합슬러리 중의 칼슘제 및/또는 철분제의 입도분포에 있어서의 중량(체적)평균경을 0.8㎛이하로 조정하는 방법에 대해서는 상기 (A), (B), (C) 기재의 방법에 따르면 되지만, 물리적 방법에 의한 분쇄 및/또는 분산방법에 대해서는 다이노밀, 샌드밀, 코볼밀 등의 습식분쇄기, 나노마이저, 마이크로플루이타이저, 호모게나이저 등의 유화·분산장치, 초음파분산기, 3축롤밀 등의 롤밀이 바람직하게 사용될 수 있다.The method of adjusting the weight (volume) average diameter in the particle size distribution of the calcium agent and / or the iron powder in the mixed slurry to 0.8 μm or less may be used according to the methods described in the above (A), (B) and (C). For the grinding and / or dispersing method, wet grinding machines such as dynomills, sand mills, and coball mills, emulsifying / dispersing apparatuses such as nanomizers, microfluidizers, homogenizers, ultrasonic dispersers, triaxial roll mills, etc. Roll mills can be preferably used.

식품첨가물 규격의 관점에서, 혼합슬러리의 원료로 칼슘제 분체를 사용할 경우는 상기 습식 분쇄기를 사용하고, 하기 ③, ④, ⑤를 모두 구비하는 분쇄조건으로 분쇄하는 것이 더 바람직하다.From the standpoint of the food additive standard, when using calcium powder as the raw material of the mixed slurry, it is more preferable to use the wet grinder to grind under the grinding conditions including all of the following ③, ④ and ⑤.

Figure pct00008
Figure pct00009
Figure pct00008
Figure pct00009

2

Figure pct00010
P
Figure pct00011
100 ④2
Figure pct00010
P
Figure pct00011
100 ④

Q

Figure pct00012
10 ⑤Q
Figure pct00012
10 ⑤

단,only,

Figure pct00013
Figure pct00013

P: 습식분쇄하는 칼슘제 및/또는 철분제 분체의 질소흡착법(BET법)에 의한 비표면적(m2/g). 또한, 칼슘제 및 철분제를 사용할 경우의 비표면적은 그 혼합비에 의해 비례계산으로 산출한다.P: specific surface area by the wet grinding calcium and / or nitrogen in the powder cheolbunje adsorption method (BET method) to (m 2 / g). In addition, the specific surface area in the case of using a calcium agent and an iron powder is computed by proportional calculation by the mixing ratio.

A: 습식분쇄기에 사용하는 미디어의 충전량이고, 습식분쇄기의 분쇄실(베셀용기)용적 중에 차지하는 미디어의 용적량(체적%)A: The volume of the media (volume%) that is the filling amount of the media used for the wet grinder and occupies in the volume of the grinding chamber (vessel container) of the wet grinder.

B: 습식분쇄기에 사용하는 미디어의 참비중B: True weight of media used in wet grinding machine

C: 습식분쇄기의 디스크 또는 로터의 주변속도(m/초)C: peripheral speed of the disc or rotor of the wet mill (m / s)

D: 습식분쇄하는 칼슘제 및/또는 철분제의 수현탁액의 칼슘제 및/또는 철분제의 고형분 농도(%)D: Solid content concentration (%) of the calcium agent and / or iron powder of the water suspension of the calcium agent and / or iron powder which wet-crushes

E: 습식분쇄하는 칼슘제 및/또는 철분제의 수현탁액의, 습식분쇄기의 분쇄실 중에 체류하는 시간(분)E: Time (minutes) of staying in the grinding chamber of a wet grinding machine of the water suspension of the calcium agent and / or iron powder to be wet-pulverized

F: 습식분쇄기에 사용하는 미디어 입자경(mm)F: Media Grain Size (mm) Used in Wet Grinding Machine

또, 특히 철분만을 대량으로 강화하고자 할 경우에, 특히 양호한 분산상태를 필요로 하는 용도에는 상기 습식분쇄기를 사용하여 이하에 예시하는 특정조건 ①, ②를 모두 구비하는 분쇄조건으로 분쇄하는 것이 더욱 바람직하다.In particular, in the case where only the iron powder is to be strengthened in a large amount, it is more preferable to grind it in a grinding condition having all of the specific conditions ① and ② exemplified below by using the above-mentioned wet grinding machine for applications requiring a particularly good dispersion state. Do.

Figure pct00014
Figure pct00014

W

Figure pct00015
1.26 ②W
Figure pct00015
1.26 ②

X=피로인산제2철분제의 슬러리 분쇄 또는 분산전의 pH값X = pH value before slurry grinding or dispersion of ferric pyrophosphate

Y=피로인산제2철분제의 슬러리 분쇄 또는 분산후의 pH값Y = pH value after slurry grinding or dispersion of ferric pyrophosphate

Z=피로인산제2철분제의 슬러리 철분제 고형분 농도(%)Z = Slurry Iron Concentration Solid Content of Ferric Pyrophosphate (%)

본 발명의 특정 습식분쇄조건 ①, ②식을 만족하지 않은 분쇄조건의 경우는 피로인산제2철의 입자표면이 조금 불안정해지기 쉽고, 따라서 재응집하기 쉬운 상태에 있고, 실질기한이 짧은 액체음료의 상품에 사용하는데에는 하등문제가 없으나, 장기적으로 액 중에서 안정된 분산상태를 유지할 필요가 있는 상품에는 상기 제조방법(B) 또는 (C)와 상기 분쇄조건 ①, ②의 요령을 함께 구비하는 분쇄조건을 사용하는 것이 바람직하다.In the case of the grinding conditions that do not satisfy the specific wet grinding conditions ① and ② of the present invention, the surface of the particles of ferric pyrophosphate tends to be slightly unstable, and thus is easy to reaggregate, and has a short liquid term. There is no problem in using it in the commodity, but commodity which needs to maintain stable dispersion state in the liquid for a long time is the grinding condition which is equipped with the methods of the manufacturing method (B) or (C) and the grinding conditions ① and ② together. Preference is given to using.

본 발명에 있어서의 칼슘제 및/또는 철분제와 PGA와 물의 혼합슬러리 중의 칼슘제 및/또는 철분제의 입도분포에 있어서의 중량평균경은 하기 요령으로 측정계산된 것이다.The weight average diameter in the particle size distribution of the calcium agent and / or the iron agent and the calcium agent and / or the iron agent in the mixed slurry of PGA and water in the present invention is measured and calculated by the following procedure.

측정기종: 시마쯔 제작소 제 SA-CP3Measuring instrument: SA-CP3 manufactured by Shimadzu Corporation

시료조제: 혼합슬러리를 하기 25℃ 용매 중에 적하하고, 입도분포 측정시료로 한다.Sample preparation: The mixed slurry was added dropwise to the following 25 ° C. solvent to obtain a particle size distribution measurement sample.

용매: 이온교환수에 폴리아크릴산소다 0.004중량% 용해시킨 수용액Solvent: Aqueous solution dissolved in 0.004% by weight of sodium polyacrylate in ion-exchanged water

예비분산: SK 디스퍼저(세이신기업제)를 사용하여 초음파분산 100초Pre-dispersion: Ultrasonic dispersion 100 seconds using SK Disperser (manufactured by Seishin Corporation)

측정온도: 27.5℃±2.5℃Measurement temperature: 27.5 ℃ ± 2.5 ℃

이상과 같이 하여 조제된 칼슘제 및/또는 철분제와 PGA와 물의 혼합슬러리를 건조분말화함으로써 본 발명의 식품첨가용 칼슘제 및/또는 철분제 파우더가 조제된다.The powdered calcium agent and / or iron powder of the present invention is prepared by dry powdering the mixed slurry of the calcium agent and / or iron powder, PGA and water prepared as described above.

혼합슬러리 건조에 대하여, 건조기에 특별한 제한은 없으나 친수성 유화제의 변질방지의 관점에서 매우 단시간에 건조를 행하는 것이 바람직하고, 이 관점에서 건조기로서는, 스프레이드라이어, 세라믹매체를 가열유동상태로 사용하는 슬러리드라이어 등의 액적분무형 건조기를 사용하는 것이 바람직하다.There is no particular restriction on the drying of the mixed slurry, but from the viewpoint of preventing the deterioration of the hydrophilic emulsifier, it is preferable to perform drying in a very short time. As a drying machine, a slurry dryer using a spray dryer or a ceramic medium in a heating fluid state can be used. It is preferable to use droplet spray dryers, such as these.

본 발명의 방법으로 조제되는 식품첨가용 칼슘제 및/또는 철분제슬러리 및 파우더는 수중에 있어서의 재분산성이 매우 양호하고, 특수한 분산기, 교반기 등을 사용하지 않아도 쉽게 수중에 분산한다.The food additive calcium and / or iron powder slurry and powder prepared by the method of the present invention have very good redispersibility in water and are easily dispersed in water without using a special disperser, agitator or the like.

따라서, 본 발명의 방법으로 조제되는 식품첨가용 칼슘제 및/또는 철분제슬러리 및 파우더를 이용하여 식품, 예컨대 칼슘 및/또는 철분강화우유를 조제하는데는, 본 발명 방법으로 조제되는 칼슘제 및/또는 철분제 슬러리 및 파우더를 우유에 직접 첨가하여 강력하게 교반하고, 우유 중에 칼슘제 및/또는 철분제를 분산시키는데 충분하지만, 해당 칼슘제 및/또는 철분제 슬러리 및 파우더를 미리 수중에 분산시켜 얻어지는 칼슘제 및/또는 철분제의 수분산액을 우유에 첨가하여도 상관없다. 또 환원유는 본 발명 방법으로 조제되는 칼슘제 및/또는 철분제 슬러리 및 파우더를 60℃정도의 온도로 용해한 버터 또는 버터오일에 가하여 고속교반하여 분산시키고, 이어서 여기에 환원탈지유 또는 탈지유를 첨가하여 균질화하면 된다.Therefore, the preparation of food, such as calcium and / or iron fortified milk, using the food additive calcium and / or iron powder slurry and powder prepared by the method of the present invention, the calcium and / or iron powder slurry prepared by the method of the present invention And the powder is added directly to the milk and stirred vigorously, sufficient to disperse the calcium and / or iron powder in the milk, but an aqueous dispersion of the calcium and / or iron powder obtained by dispersing the calcium and / or iron slurry and powder in water in advance. May be added to milk. Reducing oil is added to a butter or butter oil dissolved in a calcium and / or iron powder slurry and powder prepared by the method of the present invention at a temperature of about 60 ° C., and then dispersed by high speed stirring, and then homogenized by adding reduced skim milk or skim milk. do.

또, 본 발명 방법으로 조제되는 식품첨가용 칼슘제 및/또는 철분제슬러리 및 파우더를 이용하여 칼슘 및/또는 철분강화요구르트를 조제하는 방법에 관해서는 본 발명 방법으로 조제되는 인산칼슘 및/또는 철분제슬러리 및 파우더를 우유에 직접 첨가하여 강력하게 교반하고, 우유 중에 인산칼슘 및/또는 철분제를 분산후, 유산균을 접종하면 된다.In addition, the method for preparing calcium and / or iron fortified yogurt using the food additive calcium agent and / or iron powder slurry and powder prepared by the method of the present invention, and the calcium phosphate and / or iron powder slurry prepared by the method of the present invention and Powder may be added directly to milk, stirred vigorously, and calcium phosphate and / or iron powder may be dispersed in milk, followed by inoculation of lactic acid bacteria.

이들 방법으로 조제한 칼슘 및/또는 철분강화우듀 등은 클래리파이어로 제거되는 칼슘제 및/또는 철분제량이 종래 방법으로 조제되는 칼슘제 및/또는 철분제 슬러리 및 파우더를 첨가한 경우에 비하여 대폭 감소한다.Calcium and / or iron-reinforced wudu prepared in these methods are greatly reduced compared to the case where calcium and / or iron powder slurries and powders prepared by conventional methods are added in the amount of calcium and / or iron powder removed by the clarifier.

즉, 본 발명의 방법으로 조제되는 식품첨가용 칼슘제 및/또는 철분제슬러리 및 파우더를 첨가한 우유, 요구르트, 쥬스류 중에는 탄산칼슘, 인산칼슘 및/또는 피로인산제2철이 매우 안정하게 유지되어 있다. 또, 본 발명 방법으로 조제한 탄산칼슘, 인산칼슘 및/또는 피로인산제2철은, 분산성이 양호하기 때문에 우유등에 첨가할 때의 교반시간이 짧아도 되고, 따라서, 버터 중에서 장시간 교반한 경우에 볼 수 있는 탄산칼슘, 인산칼슘 및/또는 피로인산제2철의 응집은 생기지 않는다.That is, calcium carbonate, calcium phosphate and / or ferric pyrophosphate are very stable in milk, yoghurt and juice to which the calcium additive for food addition and / or iron powder slurry and powder prepared by the method of the present invention are added. In addition, the calcium carbonate, calcium phosphate and / or ferric pyrophosphate prepared by the method of the present invention have a good dispersibility, so that the stirring time when added to milk or the like may be short. No agglomeration of calcium carbonate, calcium phosphate and / or ferric pyrophosphate may occur.

본 발명의 식품첨가제는 상기 용도 이외에 크림, 요구르트, 커피, 홍차, 우롱차 등의 액체식품, 와인, 술 등의 알콜음료 등에 칼슘 및/또는 철분강화 목적으로 사용할 수 있다.The food additive of the present invention may be used for the purpose of strengthening calcium and / or iron in liquid foods such as cream, yogurt, coffee, black tea, oolong tea, alcoholic beverages such as wine, liquor, etc. in addition to the above-mentioned uses.

또, 본 발명의 칼슘제 및/또는 슬러리 및 파우더는 유산칼슘, 염화칼슘 등의 수가용성 칼슘염 및/또는 구연산철나트륨, 글루콘산철 등의 수가용성 철염과 병용하여도 하등 지장이 없다.The calcium agent and / or slurry and powder of the present invention can be used in combination with water-soluble calcium salts such as calcium lactate and calcium chloride and / or water-soluble iron salts such as sodium iron citrate and iron gluconate.

이하에 실시예, 비교예를 나타내어 본 발명을 더 상세히 설명하나, 본 발명은 이들 실시예에 한정되는 것은 아니다.Although an Example and a comparative example are shown to the following and this invention is demonstrated in detail, this invention is not limited to these Examples.

본 실시예와 비교예에서 사용할 칼슘제를 이하 방법으로 조제하였다.The calcium agent to be used in this example and a comparative example was prepared by the following method.

(1) 피로인산이수소칼슘(1) calcium dihydrogen phosphate

인산 수용액 중에 탄산칼슘을 첨가교반후, 탈수, 건조하여, 인산수소칼슘을 얻었다. 그 인산수소칼슘을 200℃로 가열, X회절측정에 의해 피로인산이수소칼슘이 생성해 있는 것을 확인후, 건식분쇄하여, 피로인산이수소칼슘의 백색분체를 얻었다.After adding and stirring calcium carbonate in aqueous solution of phosphoric acid, dehydration and drying were performed to obtain calcium hydrogen phosphate. The calcium hydrogen phosphate was heated to 200 ° C., and after confirming that calcium dihydrogen phosphate was produced by X diffraction measurement, dry grinding was performed to obtain a white powder of calcium dihydrogen phosphate.

이 백색분체의 질소흡착법에 의한 비표면적을 시바다 과학기기공업제 표면적 측정장치 SA-1000을 이용하여 측정한 결과, 15m2/g이었다.The specific surface area of this white powder by nitrogen adsorption was measured using a surface area measuring apparatus SA-1000 manufactured by Shivada Scientific Instruments, and found to be 15 m 2 / g.

(2) 인산일수소칼슘(2) calcium dihydrogen phosphate

인산 수용액 중에 수산화칼슘을 첨가교반하여 X회절측정에 의해 인산일수소칼슘이 생성해 있는 것을 확인후 탈수, 건조, 건식분쇄하여, 인산일수소칼슘의 백색분체를 얻었다.After adding and stirring calcium hydroxide in the aqueous solution of phosphoric acid, it was confirmed that calcium monohydrogen phosphate was produced by X diffraction measurement, followed by dehydration, drying and dry grinding to obtain a white powder of calcium monohydrogen phosphate.

이 백색분체의 질소흡착법에 의한 비표면적을 시바다 과학기기공업제 표면적 측정장치 SA-1000을 사용하여 측정한 결과, 20m2/g이었다.The specific surface area of this white powder by nitrogen adsorption was measured using a surface area measuring apparatus SA-1000 manufactured by Shivada Scientific Instruments, and found to be 20 m 2 / g.

(3) 인산삼칼슘(3) tricalcium phosphate

강암모니아성 염화칼슘용액에 제이인산암모늄을 첨가교반후, 탈수하여 얻어지는 케이크를 수차 수세후, 건조, 건식분쇄를 행하여 백색분체를 얻었다. X회절측정에 의해 그 백색분체가 인산삼칼슘임을 확인하였다. 이 백색분체의 질소흡착법에 의한 비표면적을 시바다 과학기기공업제 표면적 측정장치 SA-1000을 이용하여 측정한 결과, 18m2/g이었다.After stirring and adding ammonium diphosphate to the strong ammonia calcium chloride solution, the cake obtained by dehydration was washed with water several times, dried and dried to obtain white powder. The X diffraction measurement confirmed that the white powder was tricalcium phosphate. The specific surface area of this white powder by nitrogen adsorption was measured using a surface area measuring apparatus SA-1000 manufactured by Shivada Scientific Instruments, and found to be 18 m 2 / g.

(4) 탄산칼슘(4) calcium carbonate

비중 1.050으로 온도가 5℃인 석회유 7m3에 탄산가스농도 25중량%의 로(爐)가스(이하 탄산가스라 함)를 25m3/분의 유속으로 도통(導通)하여 탄산화반응을 행하고, pH 7에서 탄산화반응을 완결하여 슬러리상 탄산칼슘을 얻었다.Due to gravity 1.050 temperatures (爐) gas (the carbon dioxide gas &quot;) a conductive (導通) at a flow rate of 25m 3 / min to 25% by weight of the carbon dioxide concentration to 5 ℃ the milk of lime 7m 3 performs the carbonation reaction, pH The carbonation reaction was completed at 7, to obtain slurry calcium carbonate.

그후 교반하여 슬러리상 탄산칼슘의 pH 가 11.5에 도달한 시점에서 필터프레스를 사용하여 탈수하고, 얻어진 탈수케이크에 재차 물을 가하여 탈수전의 슬러리상 탄산칼슘과 동일 농도의 슬러리상 탄산칼슘을 얻었다. 해당 슬러리상 탄산칼슘의 pH는 11.0이었다. 이 슬러리상 탄산칼슘에 재차 탄산가스를 도통하고, 슬러리상 탄산칼슘의 pH를 7.0으로 저하시켜, 슬러리상 탄산칼슘을 얻었다. 해당 슬러리상 탄산칼슘을 필터프레스로 탈수하고, 그 프레스케이크를 패들드라이어로 건조하여, 건식분쇄기를 이용하여 탄산칼슘분체를 조제하였다.Thereafter, the mixture was stirred and dehydrated using a filter press when the pH of the slurry calcium carbonate reached 11.5. Water was added again to the obtained dehydrated cake to obtain slurry calcium carbonate having the same concentration as the slurry calcium carbonate before dehydration. The pH of this slurry calcium carbonate was 11.0. Carbon dioxide gas was again made conductive to this slurry calcium carbonate, pH of slurry calcium carbonate was reduced to 7.0, and slurry calcium carbonate was obtained. The slurry calcium carbonate was dehydrated with a filter press, the press cake was dried with a paddle dryer, and calcium carbonate powder was prepared using a dry mill.

이 백색분체의 질소흡착법에 의한 비표면적을 시바다 과학기기공업제 표면적 측정장치 AS-1000을 이용하여 측정한 결과, 48m2/g이었다.The specific surface area of this white powder by nitrogen adsorption was measured using a surface area measuring device AS-1000 manufactured by Shibada Scientific Instruments, and was 48 m 2 / g.

(5) 피로인산제2철 액(5) Ferric Pyrophosphate Liquid

1m3의 물중에 염화제2철 307kg을 용해시켜, 이 용액에 피로인산나트륨 233kg을 2.5m3의 온수에 녹인 액을 혼합하고, 약 1시간 교반한다. 반응종료후, 해당 용액을 필터프레스를 이용하여 탈수하고, 얻어진 탈수케이크에 재차 물을 가하여 교반하고, 탈수전과 동일 농도의 피로인산제2철 수용액을 얻었다. 이 조작을 2회 반복후, 그 피로인산제2철액을 조제하였다.307 kg of ferric chloride are dissolved in 1 m 3 of water, and a solution in which 233 kg of sodium pyrophosphate is dissolved in 2.5 m 3 of warm water is mixed with this solution and stirred for about 1 hour. After the completion of the reaction, the solution was dehydrated using a filter press, water was added to the obtained dehydrated cake again and stirred to obtain a ferric pyrophosphate aqueous solution having the same concentration as before dehydration. After repeating this operation twice, the ferric pyrophosphate solution was prepared.

(6) 피로인산제2철 분체(6) ferric pyrophosphate powder

1m3의 물중에 염화제2철 307kg을 용해시켜, 이 용액에 피로인산나트륨 233kg을 2.5m3의 온수에 녹인 액을 혼합하고, 약 1시간 교반한다. 반응종료후, 해당 용액을 필터프레스를 이용하여 탈수하고, 얻어진 탈수케이크에 재차 물을 가하여 교반하고, 탈수전과 동일 농도의 피로인산제2철 수용액을 얻었다. 이 조작을 2회 반복후, 그 피로인산제2철 수용액을 필터 프레스로 탈수하여, 그 프레스케이크를 패들드라이어로 건조하여, 건식분쇄기를 이용하여 피로인산제2철 분체를 조제하였다.307 kg of ferric chloride are dissolved in 1 m 3 of water, and a solution in which 233 kg of sodium pyrophosphate is dissolved in 2.5 m 3 of warm water is mixed with this solution and stirred for about 1 hour. After the completion of the reaction, the solution was dehydrated using a filter press, water was added to the obtained dehydrated cake again and stirred to obtain a ferric pyrophosphate aqueous solution having the same concentration as before dehydration. After repeating this operation twice, the ferric pyrophosphate aqueous solution was dehydrated with a filter press, the press cake was dried with a paddle dryer, and ferric pyrophosphate powder was prepared using a dry grinding machine.

얻어진 피로인산제2철의 질소흡착법에 의한 비표면적은 23m2/g이었다.The specific surface area of the obtained ferric pyrophosphate by nitrogen adsorption was 23 m 2 / g.

(실시예 1)(Example 1)

인산삼칼슘 분체에 물을 첨가하여, 인산삼칼슘 고분형 농도가 22중량%인 수현탁액을 조제하고, 습식분쇄기 다이노밀 KD-PILOT형(WAB사제)을 사용하여 습식분쇄를 행하여, 인산삼칼슘의 수분산체를 얻었다. 그후, 해당 인산삼칼슘의 수분산체에 PGA(기미즈 화학공업사제)를 인산삼칼슘고형분 100중량부에 대하여 13중량부 및 물을 첨가하여 강력하게 교반혼합하여, 인산삼칼슘고형분 농도가 10중량%인 혼합물을 조제후, 재차 이 혼합물을 습식분쇄기 다이노밀 KD-PILOT형을 사용하여 습식분쇄하고, 인산삼칼슘슬러리 중의 인산삼칼슘의 입도분포에 있어서의 중량(체적)평균경이 표 1과 같이 0.15㎛에 도달한 시점에서 습식분쇄를 완료하고, 식품첨가용 칼슘제 슬러리를 얻었다. 또한, PGA는 미리 물에서 용해시킨후, 첨가하였다.Water was added to the tricalcium phosphate powder to prepare an aqueous suspension having a tricalcium phosphate solid concentration of 22% by weight, and wet grinding was performed using a wet mill Dinomil KD-PILOT (manufactured by WAB) to produce tricalcium phosphate. An aqueous dispersion of was obtained. Subsequently, 13 parts by weight of PGA (manufactured by Kimizu Chemical Co., Ltd.) and 100 parts by weight of water were added to the aqueous dispersion of tricalcium phosphate, and the mixture was vigorously stirred, and the tricalcium phosphate solid concentration was 10 wt. After preparing a% mixture, the mixture was wet-pulverized again using a wet mill Dinoyl KD-PILOT, and the weight (volume) average diameter in the particle size distribution of tricalcium phosphate in tricalcium phosphate slurry was shown in Table 1. The wet grinding was completed at the time point of reaching 0.15 탆 to obtain a calcium slurry for food addition. In addition, PGA was previously dissolved in water and then added.

(실시예 2)(Example 2)

피로인산이수소칼슘분체에 물을 첨가하여, 피로인산이수소칼슘고형분 농도가 22중량%인 수현탁액을 조제하고, 습식분쇄기 다이노밀 KD-PILOT형을 사용하여 습식분쇄하여, 피로인산이수소칼슘의 수분산체를 얻었다. 그후, 해당 피로인산이수소칼슘의 수분산체에 PGA를 피로인산이수소칼슘 고형분 100중량부에 대하여 10중량부 및 물을 첨가하여 강력하게 교반혼합하여, 피로인산이수소칼슘 고형분 농도가 10중량%인 혼합물을 조제후, 재차 이 혼합물을 습식분쇄기 다이노밀 KD-PILOT형을 사용하여 습식분쇄하고, 피로인산이수소칼슘 슬러리 중의 피로인산이수소칼슘의 입도분포에 있어서의 중량(체적)평균경이 표 1과 같이 0.27㎛에 도달한 시점에서 습식분쇄를 완료하고, 식품첨가용 칼슘제 슬러리를 얻었다. 또한 PGA는 미리 물로 용해시킨후, 첨가하였다.Water was added to the calcium dihydrogen phosphate powder to prepare an aqueous suspension having a calcium dihydrogen phosphate solids concentration of 22% by weight, and wet grinding using a wet mill Dinoyl KD-PILOT to produce calcium dihydrogen phosphate dihydrogen phosphate. An aqueous dispersion of was obtained. Subsequently, 10 parts by weight of PGA was added to the aqueous dispersion of calcium dihydrogen phosphate pyrophosphate and 100 parts by weight of calcium dihydrogen phosphate solid and water were mixed with vigorous stirring, and the concentration of calcium dihydrogen phosphate solid was 10% by weight. After preparing the phosphorus mixture, the mixture was again pulverized using a wet mill Dinoyl KD-PILOT, and the weight (volume) average diameter in the particle size distribution of calcium dihydrogen phosphate in the calcium dihydrogen phosphate slurry was prepared. When it reached 0.27 micrometer like 1, wet grinding was completed and the calcium slurry for food addition was obtained. In addition, PGA was previously dissolved in water and then added.

(실시예 3)(Example 3)

인산일수소칼슘 분체에 물을 첨가하여, 인산일수소칼슘 고형분 농도가 22중량%인 수현탁액을 조제하고, 습식분쇄기 다이노밀 KD-PILOT형을 사용하여 습식분쇄하여, 인산일수소칼슘의 수분산체를 얻었다. 그 후, 해당 인산일수소칼슘의 수분산체에, PGA를 인산일수소칼슘 고형분 100중량부에 대하여 6중량부 및 물을 첨가하여 강력하게 교반혼합하고, 인산일수소칼슘 고형분 농도가 10중량%인 혼합물을 조제후, 재차 이 혼합물을 습식분쇄기 다이노밀 KD-PILOT형을 사용하여 습식분쇄하고, 인산일수소칼슘 슬러리 중의 인산일수소칼슘의 입도분포에 있어서의 중량(체적)평균경이 표 1과 같이 0.36㎛에 도달한 시점에서 습식분쇄를 완료하고, 식품첨가용 칼슘제 슬러리를 얻었다. 또한, PGA는 미리 물로 용해시킨후, 첨가하였다.Water was added to the calcium dihydrogen phosphate powder to prepare an aqueous suspension having a calcium dihydrogen phosphate solid concentration of 22% by weight, followed by wet grinding using a wet mill Dinoyl KD-PILOT, and an aqueous dispersion of calcium dihydrogen phosphate. Got. Subsequently, 6 parts by weight of PGA was added to the aqueous dispersion of calcium monohydrogen phosphate and 100 parts by weight of calcium monohydrogen phosphate and water were mixed with vigorous stirring, and the concentration of calcium monohydrogen phosphate was 10% by weight. After the mixture was prepared, the mixture was again pulverized using a wet mill Dinoyl KD-PILOT, and the weight (volume) average diameter in the particle size distribution of calcium dihydrogen phosphate in the calcium dihydrogen phosphate slurry was shown in Table 1. At the time point of reaching 0.36 mu m, the wet grinding was completed, and a calcium slurry for food addition was obtained. In addition, PGA was previously dissolved in water and then added.

(실시예 4)(Example 4)

인산삼칼슘고형분 100중량부에 대한 PGA첨가량을, 9중량부로 변경한 것, 및 인산삼칼슘 슬러리 중의 인산삼칼슘의 입도분포에 있어서의 중량(체적)평균경이 표 1과 같이 0.22㎛에 도달한 시점에서 습식분쇄를 완료한 것을 제외하고는 실시예 1과 동일한 방법으로 식품첨가용 칼슘제 슬러리를 얻었다.The amount of PGA added to 100 parts by weight of tricalcium phosphate solids was changed to 9 parts by weight, and the weight (volume) average diameter in the particle size distribution of tricalcium phosphate in the tricalcium phosphate slurry reached 0.22 μm as shown in Table 1. A calcium slurry for food addition was obtained in the same manner as in Example 1 except that the wet grinding was completed.

(실시예 5)(Example 5)

피로인산이수소칼슘 고형분 100중량부에 대한 PGA첨가량을 4중량부로 변경한 것, 및 피로인산이수소칼슘 슬러리 중의 피로인산이수소칼슘의 입도분포에 있어서의 중량(체적)평균경이 표 1과 같이 0.24㎛에 도달한 시점에서 습식분쇄를 완료한 것을 제외하고는 실시예 2와 동일한 방법으로 식품첨가용 칼슘제 슬러리를 얻었다.The weight (volume) average diameter in the particle size distribution of calcium dihydrogen phosphate in the dicalcium dihydrogen phosphate slurry was changed to 4 parts by weight of PGA added to 100 parts by weight of dihydrogen pyrophosphate solids. A calcium slurry for food addition was obtained in the same manner as in Example 2 except that the wet grinding was completed at the time point of reaching 0.24 μm.

(실시예 6)(Example 6)

인산삼칼슘고형분 100중량부에 대한 PGA첨가량을 21중량부로 변경한 것, 및 인산삼칼슘 슬러리 중의 인산삼칼슘의 입도분포에 있어서의 중량(체적)평균경이 표 1과 같이 0.18㎛에 도달한 시점에서 습식분쇄를 완료한 것을 제외하고는 실시예 1과 동일한 방법으로 식품첨가용 칼슘제 슬러리를 얻었다.When the PGA addition amount was changed to 21 parts by weight based on 100 parts by weight of tricalcium phosphate solids, and the weight (volume) average diameter in the particle size distribution of tricalcium phosphate in the tricalcium phosphate slurry reached 0.18 μm as shown in Table 1. A calcium slurry for food additives was obtained in the same manner as in Example 1 except that the wet grinding was completed.

(실시예 7)(Example 7)

인산삼칼슘고형분 100중량부에 대한 PGA첨가량을 36중량부로 변경한 것, 및 인산삼칼슘 슬러리 중의 인산삼칼슘의 입도분포에 있어서의 중량(체적)평균경이 표 1과 같이 0.26㎛에 도달한 시점에서 습식분쇄를 완료한 것을 제외하고는 실시예 3과 동일한 방법으로 식품첨가용 칼슘제 슬러리를 얻었다.The point where the amount of PGA added to 100 parts by weight of tricalcium phosphate solid was changed to 36 parts by weight, and the weight (volume) average diameter in the particle size distribution of tricalcium phosphate in the tricalcium phosphate slurry reached 0.26 μm as shown in Table 1. A calcium slurry for food additives was obtained in the same manner as in Example 3 except that the wet grinding was completed.

(실시예 8)(Example 8)

피로인산이수소칼슘 고형분 100중량부에 대한 PGA 첨가량을 28중량부로 변경한 것, 및 피로인산이수소칼슘 슬러리 중의 피로인산이수소칼슘의 입도분포에 있어서의 중량(체적)평균경이 표 1과 같이 0.18㎛에 도달한 시점에서 습식분쇄를 완료한 것을 제외하고는 실시예 2와 동일한 방법으로 식품첨가용 칼슘제 슬러리를 얻었다.The weight (volume) average diameter in the particle size distribution of calcium dihydrogen phosphate in the calcium dihydrogen phosphate slurry was changed to 28 parts by weight of PGA added to 100 parts by weight of dihydrogen pyrophosphate solids. A calcium slurry for food additives was obtained in the same manner as in Example 2 except that the wet grinding was completed at the time point of reaching 0.18 μm.

(실시예 9)(Example 9)

인산삼칼슘 분체 및 피로인산제2철 분체를 30:1의 비율로 혼합후, 물을 첨가하여, 인산삼칼슘 및 피로인산제2철 고형분 농도가 22중량%인 수현탁액을 조제하고, 습식분쇄기 다이노밀 KD-PILOT형을 이용하여 습식분쇄하고, 인산삼칼슘 및 피로인산제2철의 수분산체를 얻었다. 그후, 해당 인산삼칼슘 및 피로인산제2철의 수분산체에 PGA를 인산삼칼슘 및 피로인산제2철 고형분 100중량부에 대하여 14중량부 및 물을 첨가하여 강력하게 교반혼합하여, 인산삼칼슘 및 피로인산제2철 고형분 농도가 10중량%인 혼합물을 조제후, 재차 이 혼합물을 습식분쇄기 다이노밀 KD- PILOT형을 이용하여 습식분쇄를 행하고, 인산삼칼슘 및 피로인산제2철 슬러리 중의 인산삼칼슘 및 피로인산제2철의 입도분포에 있어서의 중량(체적)평균경이 표 1과 같이 0.25㎛에 도달한 시점에서 습식분쇄를 완료하고, 식품첨가용 칼슘제 및 피로인산제2철 슬러리를 얻었다. 또한, PGA는 미리 물에서 용해시킨 후, 첨가하였다.After mixing tricalcium phosphate powder and ferric pyrophosphate powder in a ratio of 30: 1, water was added to prepare a water suspension having a concentration of tricalcium phosphate and ferric pyrophosphate solids by 22% by weight, and a wet mill. Wet grinding was performed using a Dynomil KD-PILOT type to obtain an aqueous dispersion of tricalcium phosphate and ferric pyrophosphate. Subsequently, 14 parts by weight of PGA was added to the aqueous dispersion of tricalcium phosphate and ferric pyrophosphate and 100 parts by weight of solid ferric pyrophosphate solids and water, followed by vigorous stirring and mixing. And after preparing a mixture having a ferric pyrophosphate solid concentration of 10% by weight, the mixture was again subjected to wet grinding using a wet grinding machine Dynomil KD-PILOT, followed by phosphoric acid in tricalcium phosphate and ferric pyrophosphate slurry. The wet grinding was completed when the weight (volume) average diameter in the particle size distribution of tricalcium and ferric pyrophosphate reached 0.25 µm as shown in Table 1 to obtain a calcium food additive and ferric pyrophosphate slurry. . In addition, PGA was previously dissolved in water and then added.

(실시예 10)(Example 10)

피로인산제2철 분체에 PGA를 피로인산제2철 100중량부에 대하여 13중량부 및 물을 첨가하여 강력하게 교반혼합함으로써 피로인산제2철 고형분 농도가 10중량%인 혼합슬러리를 조제하였다. 해당 혼합슬러리를 습식분쇄기 다이노밀 KD-PILOT형을 이용하여 습식분쇄하고, 피로인산제2철분제 슬러리 분산체를 얻었다. 또한, 그 피로인산제2철분제 슬러리 중의 피로인산제2철의 입도분포에 있어서의 중량(체적)평균경이 표 1과 같이 0.29㎛에 도달한 시점에서 습식분쇄를 완료하였다.To the ferric pyrophosphate powder, 13 parts by weight of PGA was added to 100 parts by weight of ferric pyrophosphate and water, followed by vigorous stirring, thereby preparing a mixed slurry having a ferric pyrophosphate solid content of 10% by weight. The mixed slurry was wet milled using a wet mill Dynomil KD-PILOT to obtain a slurry dispersion of ferric pyrophosphate. The wet grinding was completed when the weight (volume) average diameter in the particle size distribution of ferric pyrophosphate in the ferric pyrophosphate slurry reached 0.29 µm as shown in Table 1.

또, 그 피로인산제2철분제 슬러리의 습식분쇄전의 pH값은 2.0이고, 습식분쇄후의 pH값은 2.8이었다.Moreover, the pH value before the wet milling of the ferric pyrophosphate slurry was 2.0, and the pH value after the wet milling was 2.8.

(실시예 11)(Example 11)

피로인산제2철 고형분 100중량부에 대한 PGA첨가량을 3중량부로 변경하는 것, 및 피로인산제2철 슬러리 중의 피로인산제2철의 입도분포에 있어서의 중량(체적)평균경이 표 1과 같이 0.38㎛에 도달한 시점에서 습식분쇄를 완료하는 것을 제외하고는 실시예 10과 동일한 방법으로, 식품첨가용 피로인산제2철분제 슬러리를 얻었다.The amount of PGA added to 100 parts by weight of ferric pyrophosphate solids was changed to 3 parts by weight, and the weight (volume) average diameter in the particle size distribution of ferric pyrophosphate in the ferric pyrophosphate slurry was shown in Table 1. A slurry of ferric pyrophosphate for food additives was obtained in the same manner as in Example 10 except that the wet grinding was completed at the time point of reaching 0.38 μm.

또, 그 피로인산제2철분제 슬러리의 습식분쇄전의 pH값은 1.9이고, 습식분쇄후의 pH값은 2.6이었다.Moreover, the pH value before the wet grinding of the ferric pyrophosphate slurry was 1.9, and the pH value after the wet grinding was 2.6.

(실시예 12)(Example 12)

피로인산제2철 고형분 100중량부에 대한 PGA첨가량을 28중량부로 변경하는 것, 및 피로인산제2철 슬러리 중의 피로인산제2철의 입도분포에 있어서의 중량(체적)평균경이 표 1과 같이 0.28㎛에 도달한 시점에서 습식분쇄를 완료하는 것을 제외하고는 실시예 10과 동일한 방법으로, 식품첨가용 피로인산제2철분제 슬러리를 얻었다.The PGA addition amount was changed to 28 parts by weight based on 100 parts by weight of the ferric pyrophosphate solids, and the weight (volume) average diameter in the particle size distribution of the ferric pyrophosphate in the ferric pyrophosphate slurry was shown in Table 1. A ferric pyrophosphate slurry for food addition was obtained in the same manner as in Example 10 except that the wet grinding was completed at the time point of reaching 0.28 μm.

또, 그 피로인산제2철분제 슬러리의 습식분쇄전의 pH값은 2.1이고, 습식분쇄후의 pH값은 3.1이었다.Moreover, the pH value before wet grinding of the ferric pyrophosphate slurry was 2.1, and the pH value after wet grinding was 3.1.

(실시예 13)(Example 13)

피로인산제2철 분체에 물을 첨가하여, 피로인산제2철 고형분 농도가 20중량%인 피로인산제2철 분체의 수현탁액을 조제하고, 습식분쇄기 다이노밀 KD-PILOT형을 이용하여 습식분쇄하였다.Water was added to the ferric pyrophosphate powder to prepare a water suspension of the ferric pyrophosphate powder having a concentration of 20% by weight of ferric pyrophosphate solids, and wet grinding using a wet grinder type Dinomil KD-PILOT. It was.

습식분쇄완료후, 조제된 물슬러리 중의 피로인산제2철 100중량부에 대하여 PGA를 20중량부 및 물을 첨가하여 강력하게 교반혼합함으로써 피로인산제2철 고형분 농도가 10중량%인 피로인산제2철분제 슬러리 분산체를 얻었다.After wet grinding, pyrophosphate having a concentration of 10% by weight of ferric pyrophosphate solids was prepared by vigorously stirring and mixing 20 parts by weight of PGA and water to 100 parts by weight of ferric pyrophosphate in the prepared water slurry. A ferric slurry slurry dispersion was obtained.

해당 피로인산제2철분제 슬러리 중의 피로인산제2철의 입도분포에 있어서의 중량(체적)평균경은 표 1과 같이 0.45㎛이었다.The weight (volume) average diameter in the particle size distribution of ferric pyrophosphate in the ferric pyrophosphate slurry was 0.45 μm as shown in Table 1.

또 그 피로인산제2철 슬러리의 습식분쇄전의 pH값은 1.9이고, 습식분쇄후의 pH값은 2.2이었다.Moreover, the pH value before the wet grinding of the ferric pyrophosphate slurry was 1.9, and the pH value after the wet grinding was 2.2.

(실시예 14)(Example 14)

피로인산제2철 고형분 100중량부에 대한 PGA첨가량을 39중량부로 변경한 것 및 피로인산제2철 슬러리 중의 피로인산제2철의 입도분포에 있어서의 중량(체적)평균경이 표 1과 같이 0.26㎛에 도달한 시점에서 습식분쇄를 완료한 것을 제외하고는 실시예 10과 동일한 방법으로 식품첨가용 피로인산제2철 슬러리를 얻었다.The PGA addition amount was changed to 39 parts by weight based on 100 parts by weight of the ferric pyrophosphate solids, and the weight (volume) average diameter in the particle size distribution of the ferric pyrophosphate in the ferric pyrophosphate slurry was 0.26 as shown in Table 1. A ferric pyrophosphate slurry for food addition was obtained in the same manner as in Example 10, except that the wet grinding was completed at the point when the micron was reached.

또, 그 피로인산제2철분제 슬러리의 습식분쇄전의 pH값은 2.2이고 습식분쇄후의 pH값은 3.3이었다.Moreover, the pH value before the wet grinding of the ferric pyrophosphate slurry was 2.2, and the pH value after the wet grinding was 3.3.

(실시예 15)(Example 15)

피로인산제2철 고형분 100중량부에 대한 PGA첨가량을 11중량부로 변경한 것 및 피로인산제2철 슬러리 중의 피로인산 제2철의 입도분포에 있어서의 중량(체적)평균경이 표 1과 같이 0.22㎛에 도달한 시점에서 습식분쇄를 완료한 것을 제외하고는 실시예 10과 동일한 방법으로 식품첨가용 피로인산제2철 슬러리를 얻었다.The PGA addition amount was changed to 11 parts by weight based on 100 parts by weight of ferric pyrophosphate solids, and the weight (volume) average diameter in the particle size distribution of ferric pyrophosphate in the ferric pyrophosphate slurry was 0.22 as shown in Table 1. A ferric pyrophosphate slurry for food addition was obtained in the same manner as in Example 10, except that the wet grinding was completed at the point when the micron was reached.

또, 그 피로인산제2철분제 슬러리의 습식분쇄전의 pH값은 2.0이고 습식분쇄후의 pH값은 3.3이었다.Moreover, the pH value before the wet grinding of the ferric pyrophosphate slurry was 2.0, and the pH value after the wet grinding was 3.3.

(실시예 16)(Example 16)

피로인산제2철 고형분 100중량부에 대한 PGA첨가량을 30중량부로 변경한 것 및 피로인산제2철 슬러리 중의 피로인산제2철의 입도분포에 있어서의 중량(체적)평균경이 표 1과 같이 0.24㎛에 도달한 시점에서 습식분쇄를 완료한 것을 제외하고는 실시예 10과 동일한 방법으로 식품첨가용 피로인산제2철 슬러리를 얻었다.The PGA addition amount was changed to 30 parts by weight based on 100 parts by weight of the ferric pyrophosphate solids, and the weight (volume) average diameter in the particle size distribution of the ferric pyrophosphate in the ferric pyrophosphate slurry was 0.24 as shown in Table 1. A ferric pyrophosphate slurry for food addition was obtained in the same manner as in Example 10, except that the wet grinding was completed at the point when the micron was reached.

또, 그 피로인산제2철분제 슬러리의 습식분쇄전의 pH값은 2.1이고 습식분쇄후의 pH값은 3.3이었다.Moreover, the pH value before the wet grinding of the ferric pyrophosphate slurry was 2.1, and the pH value after the wet grinding was 3.3.

(실시예 17)(Example 17)

피로인산제2철 액에 PGA를 피로인산제2철 100중량부에 대하여 9중량부 및 물을 첨가하여 강력하게 교반혼합함으로써 피로인산제2철 고형분 농도가 3중량%인 혼합슬러리를 조제하였다. 그 혼합슬러리를 습식분쇄기 다이노밀 KD-PILOT형을 이용하여 습식분쇄하고, 피로인산제2철분제 슬러리 분산체를 얻었다. 또한 그 피로인산 제2철분제 슬러리 분산체 중의 피로인산제2철 입도분포에 있어서의 중량(체적)평균경은 표 1과 같이 0.27㎛이었다.To the ferric pyrophosphate solution, 9 parts by weight of PGA was added to 100 parts by weight of ferric pyrophosphate and water, followed by vigorous stirring to prepare a mixed slurry having a ferric pyrophosphate solid content of 3% by weight. The mixed slurry was wet milled using a wet mill Dinomil KD-PILOT to obtain a slurry dispersion of ferric pyrophosphate. In addition, the weight (volume) average diameter in the ferric pyrophosphate particle size distribution in the slurry of the ferric pyrophosphate powder was 0.27 μm as shown in Table 1.

또, 그 피로인산제2철분제 슬러리의 습식분쇄전의 pH값은 3.0이고, 습식분쇄후의 pH값은 3.5이었다.Moreover, the pH value before the wet grinding of the ferric pyrophosphate slurry was 3.0, and the pH value after the wet grinding was 3.5.

(실시예 18)(Example 18)

실시예 1에서 얻은 식품첨가물용 칼슘제 슬러리를 스프레이드라이어를 이용하여 건조하여 식품첨가물용 칼슘제 파우더를 얻었다.The calcium additive slurry for food additives obtained in Example 1 was dried using a spray dryer to obtain a calcium additive powder for food additives.

(실시예 19)(Example 19)

실시예 2에서 얻은 식품첨가물용 칼슘제 슬러리를 스프레이드라이어를 이용하여 건조하여 식품첨가물용 칼슘제 파우더를 얻었다.The calcium additive slurry for food additives obtained in Example 2 was dried using a spray dryer to obtain a calcium additive powder for food additives.

(실시예 20)(Example 20)

실시예 3에서 얻은 식품첨가물용 칼슘제 슬러리를 스프레이드라이어를 이용하여 건조하여 식품첨가물용 칼슘제 파우더를 얻었다.The calcium additive slurry for food additives obtained in Example 3 was dried using a spray dryer to obtain a calcium additive powder for food additives.

(실시예 21)(Example 21)

실시예 4에서 얻은 식품첨가물용 칼슘제 슬러리를 스프레이드라이어를 이용하여 건조하여 식품첨가물용 칼슘제 파우더를 얻었다.The calcium additive slurry for food additives obtained in Example 4 was dried using a spray dryer to obtain a calcium additive powder for food additives.

(실시예 22)(Example 22)

실시예 5에서 얻은 식품첨가물용 칼슘제 슬러리를 스프레이드라이어를 이용하여 건조하여 식품첨가물용 칼슘제 파우더를 얻었다.The calcium additive slurry for food additives obtained in Example 5 was dried using a spray dryer to obtain a calcium additive powder for food additives.

(실시예 23)(Example 23)

실시예 6에서 얻은 식품첨가물용 칼슘제 슬러리를 스프레이드라이어를 이용하여 건조하여 식품첨가물용 칼슘제 파우더를 얻었다.The calcium additive slurry for food additives obtained in Example 6 was dried using a spray dryer to obtain a calcium additive powder for food additives.

(실시예 24)(Example 24)

실시예 7에서 얻은 식품첨가물용 칼슘제 슬러리를 스프레이드라이어를 이용하여 건조하여 식품첨가물용 칼슘제 파우더를 얻었다.The calcium additive slurry for food additives obtained in Example 7 was dried using a spray dryer to obtain a calcium additive powder for food additives.

(실시예 25)(Example 25)

실시예 8에서 얻은 식품첨가물용 칼슘제 슬러리를 스프레이드라이어를 이용하여 건조하여 식품첨가물용 칼슘제 파우더를 얻었다.The calcium additive slurry for food additives obtained in Example 8 was dried using a spray dryer to obtain a calcium additive powder for food additives.

(실시예 26)(Example 26)

실시예 9에서 얻은 식품첨가물용 칼슘제 및 피로인산제2철분제 슬러리를 스프레이드라이어를 이용하여 건조하여 식품첨가물용 칼슘제 및 피로인산제2철분제 파우더를 얻었다.The slurry for calcium additive and ferric pyrophosphate for food additives obtained in Example 9 was dried using a spray dryer to obtain a calcium for food additive and ferric pyrophosphate powder.

(실시예 27)(Example 27)

실시예 10에서 얻은 식품첨가물용 피로인산제2철분제 슬러리를 스프레이드라이어를 이용하여 건조하여 식품첨가물용 피로인산제2철분제 파우더를 얻었다.The ferric pyrophosphate slurry for food additives obtained in Example 10 was dried using a spray dryer to obtain ferric pyrophosphate powder for food additives.

(실시예 28)(Example 28)

실시예 11에서 얻은 식품첨가물용 피로인산제2철분제 슬러리를 스프레이드라이어를 이용하여 건조하여 식품첨가물용 피로인산제2철분제 파우더를 얻었다.The ferric pyrophosphate pyrophosphate slurry for food additives obtained in Example 11 was dried using a spray dryer to obtain ferric pyrophosphate powder for food additives.

(실시예 29)(Example 29)

실시예 12에서 얻은 식품첨가물용 피로인산제2철분제 슬러리를 스프레이드라이어를 이용하여 건조하여 식품첨가물용 피로인산제2철분제 파우더를 얻었다.The ferric pyrophosphate slurry for food additives obtained in Example 12 was dried using a spray dryer to obtain ferric pyrophosphate powder for food additives.

(실시예 30)(Example 30)

실시예 13에서 얻은 식품첨가물용 피로인산제2철분제 슬러리를 스프레이드라이어를 이용하여 건조하여 식품첨가물용 피로인산제2철분제 파우더를 얻었다.The ferric pyrophosphate powder for food additives obtained in Example 13 was dried using a spray dryer to obtain ferric pyrophosphate powder for food additives.

(실시예 31)(Example 31)

실시예 14에서 얻은 식품첨가물용 피로인산제2철분제 슬러리를 스프레이드라이어를 이용하여 건조하여 식품첨가물용 피로인산제2철분제 파우더를 얻었다.The ferric pyrophosphate slurry for food additives obtained in Example 14 was dried using a spray dryer to obtain ferric pyrophosphate powder for food additives.

(실시예 32)(Example 32)

실시예 15에서 얻은 식품첨가물용 피로인산제2철분제 슬러리를 스프레이드라이어를 이용하여 건조하여 식품첨가물용 피로인산제2철분제 파우더를 얻었다.The ferric pyrophosphate slurry for food additives obtained in Example 15 was dried using a spray dryer to obtain ferric pyrophosphate powder for food additives.

(실시예 33)(Example 33)

실시예 16에서 얻은 식품첨가물용 피로인산제2철분제 슬러리를 스프레이드라이어를 이용하여 건조하여 식품첨가물용 피로인산제2철분제 파우더를 얻었다.The ferric pyrophosphate slurry for food additives obtained in Example 16 was dried using a spray dryer to obtain ferric pyrophosphate powder for food additives.

(실시예 34)(Example 34)

실시예 17에서 얻은 식품첨가물용 피로인산제2철분제 슬러리를 스프레이드라이어를 이용하여 건조하여 식품첨가물용 피로인산제2철분제 파우더를 얻었다.The ferric pyrophosphate slurry for food additives obtained in Example 17 was dried using a spray dryer to obtain ferric pyrophosphate powder for food additives.

(비교예 1)(Comparative Example 1)

인산삼칼슘 고형분 100중량부에 대한 PGA의 첨가량을 50중량부로 변경한 것, 및 인산삼칼슘 슬러리 중의 인산삼칼슘의 입도분포에 있어서의 중량(체적)평균경이 표 2와 같이 0.13㎛에 도달한 시점에서 습식분쇄를 완료하는 것을 제외하고는 실시예 1과 동일한 방법으로 식품첨가물용 칼슘제 슬러리를 얻었다.The amount of PGA added to 100 parts by weight of tricalcium phosphate solids was changed to 50 parts by weight, and the weight (volume) average diameter in the particle size distribution of tricalcium phosphate in the tricalcium phosphate slurry reached 0.13 µm as shown in Table 2. A calcium slurry for food additives was obtained in the same manner as in Example 1 except that the wet grinding was completed.

(비교예 2)(Comparative Example 2)

피로인산이수소칼슘 고형분 100중량부에 대한 PGA 첨가량을 1.4중량부로 변경한 것을 제외하고는 실시예 2와 동일한 방법으로 표 2와 같이 식품첨가물용 칼슘제 슬러리를 얻었다.A calcium slurry for food additives was obtained in the same manner as in Example 2 except that the amount of PGA added to 100 parts by weight of calcium dihydrogen phosphate solid was changed to 1.4 parts by weight.

(비교예 3)(Comparative Example 3)

인산일수소칼슘 고형분 100중량부에 대한 PGA첨가량을 42중량부로 변경한 것, 및 인산일수소칼슘의 입도분포에 있어서의 중량(체적)평균경이 표 2와 같이 0.32㎛에 도달한 시점에서 습식분쇄를 완료한 것을 제외하고는 실시예 3과 동일한 방법으로 식품첨가물용 칼슘제 슬러리를 얻었다.The wet grinding was performed when the amount of PGA added to 100 parts by weight of calcium dihydrogen phosphate was changed to 42 parts by weight, and the weight (volume) average diameter in the particle size distribution of calcium dihydrogen phosphate reached 0.32 μm as shown in Table 2. A calcium slurry for food additives was obtained in the same manner as in Example 3 except for completing the following.

(비교예 4)(Comparative Example 4)

인산삼칼슘 고형분 100중량부에 대한 PGA첨가량을 1중량부로 변경한 것을 제외하고는 실시예 4와 동일한 방법으로 표 2와 같이 식품첨가용 칼슘제 슬러리를 얻었다.A calcium slurry for food additives was obtained in the same manner as in Example 4 except that the amount of PGA added to 100 parts by weight of tricalcium phosphate solid content was changed to 1 part by weight.

(비교예 5)(Comparative Example 5)

인산삼칼슘 분체에 물을 첨가하여, 인산삼칼슘 고형분 농도가 22중량%인 수현탁액을 조제하고, 습식분쇄기 다이노밀 KD-PILOT형을 사용하여 습식분쇄하여, 인산삼칼슘의 수분산체를 얻었다. 그후, 해당 인산삼칼슘의 수분산체에 HLB가 16인 자당스테아르산에스테르를 인산삼칼슘 고형분 100중량부에 대하여 19중량부 및 물을 첨가하여, 강력하게 교반혼합하고, 인산삼칼슘 고형분 농도가 10중량부%인 혼합물을 조제후, 재차 이 혼합물을 습식분쇄기 다이노밀 KD-PILOT형을 사용하여 습식분쇄하고, 인산삼칼슘 슬러리 중의 인산삼칼슘의 입도분포에 있어서의 중량(체적)평균경이 표 2와 같이 0.20㎛에 도달한 시점에서 습식분쇄를 완료하고, 식품첨가용 칼슘제 슬러리를 얻었다. 또한 자당스테아르산에스테르는 미리 65℃의 온수에 용해후 20℃로 냉각하여 첨가하였다.Water was added to the tricalcium phosphate powder to prepare an aqueous suspension having a tricalcium phosphate solid concentration of 22% by weight, and wet grinding using a wet mill Dinoyl KD-PILOT to obtain an aqueous dispersion of tricalcium phosphate. Thereafter, 19 parts by weight of water and water were added to the aqueous dispersion of tricalcium phosphate sucrose stearic acid ester having a HLB of 16 to 100 parts by weight of tricalcium phosphate solids, and vigorously stirred and mixed, and the concentration of tricalcium phosphate solids was 10. After preparing the mixture in parts by weight, the mixture was pulverized again using a wet mill Dinoyl KD-PILOT, and the weight (volume) average diameter in the particle size distribution of tricalcium phosphate in the tricalcium phosphate slurry was shown in Table 2. As described above, the wet grinding was completed at the time point of reaching 0.20 µm to obtain a calcium slurry for food addition. Sucrose stearic acid ester was dissolved in hot water at 65 ° C in advance and cooled to 20 ° C and added.

(비교예 6)(Comparative Example 6)

피로인산이수소칼슘 분체에 물을 첨가하여, 피로인산이수소칼슘 고형분 농도가 22중량%인 수현탁액을 조제하여, 습식분쇄기 다이노밀 KD-PILOT형을 사용하여 습식분쇄하고, 피로인산이수소칼슘의 수분산체를 얻었다. 그후, 해당 피로인산이수소칼슘의 수분산체에 HLB가 16인 자당스테아르산에스테르를 피로인산이수소칼슘 고형분 100중량부에 대하여 25중량부 및 물을 첨가하여, 강력하게 교반혼합하고, 피로인산이수소칼슘 고형분 농도가 10중량%인 혼합물을 조제후, 재차 이 혼합물을 습식분쇄기 다이노밀 KD-PILOT형을 사용하여 습식분쇄하고, 피로인산이수소칼슘 슬러리 중의 피로인산이수소칼슘의 입도분포에 있어서의 중량(체적)평균경이 표 2와 같이 0.33㎛에 도달한 시점에서 습식분쇄를 완료하고, 식품첨가용 칼슘제 슬러리를 얻었다. 또한 자당스테아르산에스테르는 미리 65℃의 온수에 용해후 20℃로 냉각하여 첨가하였다.Water was added to the calcium dihydrogen phosphate powder to prepare an aqueous suspension having a calcium dihydrogen phosphate solids concentration of 22% by weight, and wet pulverized using a wet mill Dinoyl KD-PILOT. An aqueous dispersion of was obtained. Subsequently, 25 parts by weight of water and water are added to the aqueous dispersion of calcium dihydrogen dihydrogen phosphate to HLB 16 sucrose stearate with respect to 100 parts by weight of calcium dihydrogen dihydrogen phosphate, and vigorously stirred and mixed. After preparing a mixture having a calcium solids concentration of 10% by weight, the mixture was wet-pulverized again using a wet grinding machine Dinoyl KD-PILOT, and the particle size distribution of calcium dihydrogen phosphate in the calcium dihydrogen phosphate slurry was obtained. The wet grinding was completed when the weight (volume) average diameter of the resin reached 0.33 µm as shown in Table 2 to obtain a calcium slurry for food addition. Sucrose stearic acid ester was dissolved in hot water at 65 ° C in advance and cooled to 20 ° C and added.

(비교예 7)(Comparative Example 7)

인산삼칼슘 및 피로인산제2철 고형분 100중량부에 대한 PGA 첨가량을 0.8중량부로 변경한 것을 제외하고는 실시예 9와 동일한 방법으로 표 2와 같이 식품첨가용 칼슘제 및 피로인산제2철분제 슬러리를 얻었다.A calcium-added food additive and a ferric pyrophosphate slurry were prepared in the same manner as in Example 9, except that the amount of PGA added to 100 parts by weight of tricalcium phosphate and ferric pyrophosphate solids was changed to 0.8 parts by weight. Got it.

(비교예 8)(Comparative Example 8)

피로인산제2철 고형분 100중량부에 대한 PGA첨가량을 1중량부로 변경한 것, 및 피로인산제2철 슬러리 중의 피로인산제2철의 입도분포에 있어서의 중량(체적)평균경이 표 2와 같이 0.24㎛에 도달한 시점에서 습식분쇄를 완료한 것을 제외하고는 실시예 10과 동일한 방법으로 식품첨가용 피로인산제2철분제 슬러리를 얻었다.The PGA addition amount was changed to 1 part by weight based on 100 parts by weight of the ferric pyrophosphate solids, and the weight (volume) average diameter in the particle size distribution of the ferric pyrophosphate in the ferric pyrophosphate slurry was shown in Table 2. A slurry of ferric pyrophosphate for food additives was obtained in the same manner as in Example 10 except that the wet grinding was completed at the time point of reaching 0.24 μm.

또, 그 피로인산제2철분제 슬러리의 습식분쇄전의 pH값은 1.9이고, 습식분쇄후의 pH값은 3.1이었다.Moreover, the pH value before the wet milling of the slurry of the ferric pyrophosphate powder was 1.9, and the pH value after the wet milling was 3.1.

(비교예 9)(Comparative Example 9)

피로인산제2철 고형분 100중량부에 대한 PGA첨가량을 45중량부로 변경한 것, 및 피로인산제2철 슬러리 중의 피로인산제2철의 입도분포에 있어서의 중량(체적)평균경이 표 2와 같이 0.25㎛에 도달한 시점에서 습식분쇄를 완료한 것을 제외하고는 실시예 10과 동일한 방법으로 식품첨가용 피로인산제2철분제 슬러리를 얻었다.The PGA addition amount was changed to 45 parts by weight based on 100 parts by weight of the ferric pyrophosphate solids, and the weight (volume) average diameter in the particle size distribution of the ferric pyrophosphate in the ferric pyrophosphate slurry was shown in Table 2. A slurry of ferric pyrophosphate for food additives was obtained in the same manner as in Example 10 except that the wet grinding was completed at the time point of reaching 0.25 탆.

또, 그 피로인산제2철분제 슬러리의 습식분쇄전의 pH값은 2.3이고, 습식분쇄후의 pH값은 3.4이었다.Moreover, the pH value before the wet grinding of the ferric pyrophosphate slurry was 2.3, and the pH value after the wet grinding was 3.4.

(비교예 10)(Comparative Example 10)

시판의 피로인산제2철(요네야마 화학공업사제)분체에 물을 첨가하여, 피로인산제2철 고형분 농도가 20중량%인 피로인산제2철 분체의 수현탁액을 조제하고, 습식분쇄기 다이노밀 파일롯형을 사용하여 습식분쇄하고, 피로인산제2철의 수분산 슬러리를 얻었다. 그 수분산 슬러리를 물로 희석하고, 교반함으로써 피로인산제2철 고형분 농도가 10중량%인 피로인산제2철분제 슬러리를 얻었다. 또한, 그 피로인산제2철 슬러리 중의 피로인산제2철의 입도분포에 있어서의 중량(체적)평균경이 표 2와 같이 0.78㎛이었다.Water was added to commercially available ferric pyrophosphate (manufactured by Yoneyama Chemical Co., Ltd.) powder to prepare a water suspension of ferric pyrophosphate powder having a ferric pyrophosphate solid concentration of 20% by weight. Wet grinding using a pilot type gave a water dispersion slurry of ferric pyrophosphate. The aqueous dispersion slurry was diluted with water and stirred to obtain a ferric pyrophosphate slurry with a ferric pyrophosphate solid content concentration of 10% by weight. In addition, the weight (volume) average diameter in the particle size distribution of ferric pyrophosphate in the ferric pyrophosphate slurry was 0.78 µm as shown in Table 2.

또, 그 피로인산제2철분제 슬러리의 습식분쇄전의 pH값은 1.9이고, 습식분쇄후의 pH값은 2.2였다.Moreover, the pH value before the wet milling of the slurry of the ferric pyrophosphate powder was 1.9, and the pH value after the wet milling was 2.2.

(비교예 11)(Comparative Example 11)

피로인산제2철 분체에 HLB가 16인 자당스테아르산에스테르를 피로인산제2철 100중량부에 대하여 20중량부 및 물을 첨가하여 강력하게 교반혼합함으로써 피로인산제2철 고형분 농도가 10중량%인 혼합슬러리를 조제하였다. 해당 혼합슬러리를 습식분쇄기 다이노밀 파일롯형을 사용하여 습식분쇄하고, 피로인산제2철분제 슬러리 분산체를 얻었다. 또한, 그 피로인산제2철분제 슬러리 중의 피로인산제2철의 입도분포에 있어서의 중량(체적)평균경이 표 2와 같이 0.28㎛에 도달한 시점에 습식분쇄를 완료하였다.The ferric pyrophosphate solids concentration was 10% by weight by vigorously stirring and mixing 20 parts by weight of water and water with 100 parts by weight of ferric pyrophosphate to the ferric pyrophosphate powder. Phosphorus mixed slurry was prepared. This mixed slurry was wet-pulverized using the wet grinder dynomil pilot type, and the slurry dispersion of ferric pyrophosphate powder was obtained. The wet grinding was completed when the weight (volume) average diameter in the particle size distribution of ferric pyrophosphate in the ferric pyrophosphate slurry reached 0.28 μm as shown in Table 2.

또, 그 피로인산제2철분제 슬러리의 습식분쇄전의 pH값은 2.0이고, 습식분쇄후의 pH값은 2.9였다.Moreover, the pH value before the wet milling of the slurry of the ferric pyrophosphate powder was 2.0, and the pH value after the wet milling was 2.9.

(비교예 12)(Comparative Example 12)

비교예 1에서 얻은 식품첨가물용 칼슘제 슬러리를 스프레이드라이어를 이용하여 건조하고, 표 2와 같이 식품첨가물용 칼슘제 파우더를 얻었다.The calcium additive slurry for food additives obtained in Comparative Example 1 was dried using a spray dryer, and as shown in Table 2, a calcium powder for food additives was obtained.

(비교예 13)(Comparative Example 13)

비교예 2에서 얻은 식품첨가물용 칼슘제 슬러리를 스프레이드라이어를 이용하여 건조하여 표 2와 같이 식품첨가물용 칼슘제 파우더를 얻었다.The calcium additive slurry for food additives obtained in Comparative Example 2 was dried using a spray dryer to obtain a calcium powder for food additives as shown in Table 2.

(비교예 14)(Comparative Example 14)

비교예 3에서 얻은 식품첨가물용 칼슘제 슬러리를 스프레이드라이어를 이용하여 건조하여 표 2와 같이 식품첨가물용 칼슘제 파우더를 얻었다.The calcium slurry for food additives obtained in Comparative Example 3 was dried using a spray dryer to obtain a calcium powder for food additives as shown in Table 2.

(비교예 15)(Comparative Example 15)

비교예 4에서 얻은 식품첨가물용 칼슘제 슬러리를 스프레이드라이어를 이용하여 건조하여 표 2와 같이 식품첨가물용 칼슘제 파우더를 얻었다.The calcium additive slurry for food additives obtained in Comparative Example 4 was dried using a spray dryer to obtain a calcium powder for food additives as shown in Table 2.

(비교예 16)(Comparative Example 16)

비교예 5에서 얻은 식품첨가물용 칼슘제 슬러리를 스프레이드라이어를 이용하여 건조하여 표 2와 같이 식품첨가물용 칼슘제 파우더를 얻었다.The calcium additive slurry for food additives obtained in Comparative Example 5 was dried using a spray dryer to obtain a calcium additive powder for food additives as shown in Table 2.

(비교예 17)(Comparative Example 17)

비교예 6에서 얻은 식품첨가물용 칼슘제 슬러리를 스프레이드라이어를 이용하여 건조하여 표 2와 같이 식품첨가물용 칼슘제 파우더를 얻었다.The calcium slurry for food additives obtained in Comparative Example 6 was dried using a spray dryer to obtain a calcium powder for food additives as shown in Table 2.

(비교예 18)(Comparative Example 18)

비교예 7에서 얻은 식품첨가물용 칼슘제 및 피로인산제2철분제 슬러리를 스프레이드라이어를 사용하여 건조하여 표 2와 같이 식품첨가물용 칼슘제 및 피로인산제2철분제의 파우더를 얻었다.The slurry of the calcium additive for food additives and the ferric pyrophosphate powder obtained in Comparative Example 7 was dried using a spray dryer to obtain a powder of the calcium additive for food additives and the ferric pyrophosphate powder as shown in Table 2.

(비교예 19)(Comparative Example 19)

비교예 8에서 얻은 식품첨가물용 피로인산제2철분제 슬러리를 스프레이드라이어를 이용하여 건조하여 표 2와 같이 식품첨가물용 피로인산제2철분제 파우더를 얻었다.The ferric pyrophosphate slurry for food additives obtained in Comparative Example 8 was dried using a spray dryer to obtain ferric pyrophosphate powder for food additives as shown in Table 2.

(비교예 20)(Comparative Example 20)

비교예 9에서 얻은 식품첨가물용 피로인산제2철분제 슬러리를 스프레이드라이어를 이용하여 건조하여 표 2와 같이 식품첨가물용 피로인산제2철분제 파우더를 얻었다.The ferric pyrophosphate slurry for food additives obtained in Comparative Example 9 was dried using a spray dryer to obtain ferric pyrophosphate powder for food additives as shown in Table 2.

(비교예 21)(Comparative Example 21)

비교예 10에서 얻은 식품첨가물용 피로인산제2철분제 슬러리를 스프레이드라이어를 이용하여 건조하여 표 2와 같이 식품첨가물용 피로인산제2철분제 파우더를 얻었다.The ferric pyrophosphate slurry for food additives obtained in Comparative Example 10 was dried using a spray dryer to obtain ferric pyrophosphate powder for food additives as shown in Table 2.

(비교예 22)(Comparative Example 22)

비교예 11에서 얻은 식품첨가물용 피로인산제2철분제 슬러리를 스프레이드라이어를 이용하여 건조하여 표 2와 같이 식품첨가물용 피로인산제2철분제 파우더를 얻었다.The ferric pyrophosphate powder for food additives obtained in Comparative Example 11 was dried using a spray dryer to obtain ferric pyrophosphate powder for food additives as shown in Table 2.

다음에 실시예 18∼실시예 34에서 얻은 본 발명의 식품첨가용 칼슘제 및/또는 피로인산제2철분제 파우더를 65℃의 온수에 첨가하여, 호모믹서에 의해 12000rpm으로 15분간 교반하여 각 칼슘제 및/또는 피로인산제2철 고형분 농도가 10중량%인 재분산액을 조제하였다. 재분산액 중의 각 칼슘제 및/또는 피로인산제2철의 입도분포에 있어서의 중량(체적)평균경을 표 1에 나타낸다.Next, the calcium food additive and / or ferric pyrophosphate powder of the present invention obtained in Examples 18 to 34 were added to hot water at 65 ° C, and stirred at 12000 rpm for 15 minutes by a homomixer to make each calcium and / or Alternatively, a redispersion liquid having a ferric pyrophosphate solid content concentration of 10% by weight was prepared. Table 1 shows the weight (volume) average diameter in the particle size distribution of each calcium agent and / or ferric pyrophosphate in the redispersion.

또, 비교예 12∼비교예 22에서 얻은 식품첨가용 칼슘제 및/또는 피로인산제2철분제 파우더를 상기와 같이하여 각 칼슘제 및/또는 피로인산제2철 고형분 농도가 10중량%인 재분산액을 조제하였다. 그 재분산액 중의 각 칼슘제 및/또는 피로인산 제2철의 입도분포에 있어서의 중량(체적)평균경을 표 2에 나타낸다.In addition, a calcium hydroxide for food additive and / or ferric pyrophosphate powder obtained in Comparative Examples 12 to 22 were prepared as described above to prepare a redispersion having a concentration of 10% by weight of each calcium and / or ferric pyrophosphate solid content. It was. Table 2 shows the weight (volume) average diameter in the particle size distribution of each calcium agent and / or ferric pyrophosphate in the redispersion.

중량평균입자경(㎛)Weight average particle diameter (㎛) 표면처리제Surface treatment agent 표면처리제중량부Surface treatment weight part 재분산액의중량평균경(㎛)Weight average diameter of redispersion (㎛) 실시예 1Example 1 0.150.15 PGAPGA 1313 실시예 18Example 18 0.150.15 실시예 2Example 2 0.270.27 PGAPGA 1010 실시예 19Example 19 0.280.28 실시예 3Example 3 0.360.36 PGAPGA 66 실시예 20Example 20 0.360.36 실시예 4Example 4 0.220.22 PGAPGA 99 실시예 21Example 21 0.240.24 실시예 5Example 5 0.240.24 PGAPGA 44 실시예 22Example 22 0.250.25 실시예 6Example 6 0.180.18 PGAPGA 2121 실시예 23Example 23 0.200.20 실시예 7Example 7 0.260.26 PGAPGA 3636 실시예 24Example 24 0.270.27 실시예 8Example 8 0.180.18 PGAPGA 2828 실시예 25Example 25 0.190.19 실시예 9Example 9 0.250.25 PGAPGA 1414 실시예 26Example 26 0.260.26 실시예 10Example 10 0.290.29 PGAPGA 1313 실시예 27Example 27 0.290.29 실시예 11Example 11 0.380.38 PGAPGA 33 실시예 28Example 28 0.390.39 실시예 12Example 12 0.280.28 PGAPGA 2828 실시예 29Example 29 0.280.28 실시예 13Example 13 0.450.45 PGAPGA 2020 실시예 30Example 30 0.460.46 실시예 14Example 14 0.260.26 PGAPGA 3939 실시예 31Example 31 0.260.26 실시예 15Example 15 0.220.22 PGAPGA 1111 실시예 32Example 32 0.240.24 실시예 16Example 16 0.240.24 PGAPGA 3030 실시예 33Example 33 0.250.25 실시예 17Example 17 0.270.27 PGAPGA 99 실시예 34Example 34 0.290.29 주) PGA: 알긴산프로필렌글리콜에스테르PGA: Alginate propylene glycol ester

중량평균입자경(㎛)Weight average particle diameter (㎛) 표면처리제Surface treatment agent 표면처리제중량부Surface treatment weight part 재분산액의중량평균경(㎛)Weight average diameter of redispersion (㎛) 비교예 1Comparative Example 1 0.130.13 PGAPGA 5050 비교예 12Comparative Example 12 0.140.14 비교예 2Comparative Example 2 0.270.27 PGAPGA 1.41.4 비교예 13Comparative Example 13 0.290.29 비교예 3Comparative Example 3 0.320.32 PGAPGA 4242 비교예 14Comparative Example 14 0.320.32 비교예 4Comparative Example 4 0.220.22 PGAPGA 1One 비교예 15Comparative Example 15 0.230.23 비교예 5Comparative Example 5 0.200.20 S.ES.E 1919 비교예 16Comparative Example 16 0.200.20 비교예 6Comparative Example 6 0.330.33 S.ES.E 2525 비교예 17Comparative Example 17 0.340.34 비교예 7Comparative Example 7 0.250.25 PGAPGA 0.80.8 비교예 18Comparative Example 18 0.270.27 비교예 8Comparative Example 8 0.240.24 PGAPGA 1One 비교예 19Comparative Example 19 0.260.26 비교예 9Comparative Example 9 0.250.25 PGAPGA 4545 비교예 20Comparative Example 20 0.250.25 비교예 10Comparative Example 10 0.780.78 -- 00 비교예 21Comparative Example 21 4.954.95 비교예 11Comparative Example 11 0.280.28 S.ES.E 2020 비교예 22Comparative Example 22 0.290.29 주) PGA: 알긴산프로필렌글리콜에스테르S.E: 자당지방산에스테르PGA: Alginate propylene glycol ester S.E: Sucrose fatty acid ester

또, 상기 실시예 10∼17 및 비교예 8∼11의 결과를 표 3에 나타낸다.Moreover, the result of the said Examples 10-17 and Comparative Examples 8-11 is shown in Table 3.

철분제고형분농도중량% ZIron Solid Concentration Weight% Z 표면처리제첨가량중량부Surface treatment additive weight part 분쇄 또는분산전의pH값 XPH value before grinding or dispersing X 분쇄 또는분산후의pH값 YPH value after grinding or dispersing Y WW 중량평균입자경 ㎛Weight average particle diameter μm 실시예 10Example 10 1010 1313 2.02.0 2.82.8 1.111.11 0.290.29 실시예 11Example 11 1010 33 1.91.9 2.62.6 1.061.06 0.380.38 실시예 12Example 12 1010 2828 2.12.1 3.13.1 1.201.20 0.280.28 실시예 13Example 13 1010 2020 1.91.9 2.22.2 0.900.90 0.450.45 실시예 14Example 14 1010 3939 2.22.2 3.33.3 1.251.25 0.260.26 실시예 15Example 15 1010 1111 2.02.0 3.33.3 1.311.31 0.220.22 실시예 16Example 16 1010 3030 2.12.1 3.33.3 1.281.28 0.240.24 실시예 17Example 17 33 99 3.03.0 3.53.5 1.071.07 0.270.27 비교예 8Comparative Example 8 1010 1One 1.91.9 3.13.1 1.271.27 0.240.24 비교예 9Comparative Example 9 1010 4545 2.32.3 3.43.4 1.251.25 0.250.25 비교예 10Comparative Example 10 1010 00 1.91.9 2.22.2 0.900.90 0.780.78 비교예 11Comparative Example 11 1010 2020 2.02.0 2.92.9 1.151.15 0.280.28

X: 피로인산제2철분제의 슬러리의 분쇄 또는 분산전의 pH값X: pH value before grinding or dispersing the slurry of ferric pyrophosphate powder

Y: 피로인산제2철분제의 슬러리의 분쇄 또는 분산후의 pH값Y: pH value after grinding or dispersing the slurry of ferric pyrophosphate powder

Z: 피로인산제2철분제의 슬러리의 철분제 고형분 농도(%)Z: Iron powder solid concentration (%) of the slurry of ferric pyrophosphate powder

Figure pct00016
Figure pct00016

다음에 실시예 1∼9, 비교예 1∼7 및 실시예 18∼26, 비교예 12∼18로 조제된 식품첨가용 칼슘제 및/또는 피로인산제2철분제의 슬러리, 재분산슬러리를 물로 12배 희석하고, 다시 해당 용액에 유산을 첨가하여, 유산농도로서, 0.2% 용액농도로 조정하고, 100ml의 메스실린더에 취하여, 10℃에서 정치하고, 인산칼슘 및/또는 피로인산제2철의 침전으로 생기는 상징(上澄) 투명부분과 인산칼슘 및/또는 피로인산제2철의 분산부분의 착색부분의 계면높이의 경시변화, 침강물의 양의 경시변화를 육안판단하여, 각 칼슘제 및/또는 피로인산제2철의 수중에 있어서의 안정성을 조사하였다. 메스실린더에 새겨진 ml단위의 표시를 판독하여 그 결과를 하기 5단계 표시로 표 4에 나타낸다.Next, the slurry and redispersion slurry of food additive calcium agent and / or ferric pyrophosphate powder prepared in Examples 1 to 9, Comparative Examples 1 to 7 and Examples 18 to 26 and Comparative Examples 12 to 18 were subjected to 12 times with water. Dilute, add lactic acid to the solution again, adjust to 0.2% solution concentration as lactic acid concentration, take in 100 ml of measuring cylinder, stand at 10 ° C, and precipitate precipitate of calcium phosphate and / or ferric pyrophosphate Visually determine the change in the interfacial height of the transparent portion and the colored portion of the dispersed portion of calcium phosphate and / or ferric pyrophosphate and the change of the amount of sediment over time to visually determine the calcium and / or pyrophosphate. The stability in the water of ferric iron was investigated. The mark of ml unit engraved on the measuring cylinder was read and the result is shown in Table 4 by the following five-step display.

또, 실시예 10∼17, 비교예 8∼11 및 실시예 27∼34, 비교예 19∼22로 조제된 피로인산제2철분제 슬러리, 재분산 슬러리를 피로인산제2철 고형분 농도가 0.06중량% 농도로 되도록 물로 희석하고, 다시 해당 용액에 유산을 첨가하여 유산농도로서 0.2%용액 농도로 조정하고, 100ml의 메스실린더에 취해, 10℃에서 정치하고, 피로인산제2철의 침전으로 생긴 상징 투명부분과 피로인산제2철의 분산부분의 착색부분의 계면높이의 경시변화, 침전물양의 경시변화를 육안판단하여, 각 피로인산제2철의 수중에 있어서의 안정성을 조사하였다. 메스실린더에 새겨진 ml단위 표시를 판독하여 그 결과를 하기 5단계 표시로 표 5에 나타낸다.Further, the ferric pyrophosphate solids concentration and the redispersion slurry prepared in Examples 10 to 17, Comparative Examples 8 to 11, Examples 27 to 34, and Comparative Examples 19 to 22 were 0.06% by weight of ferric pyrophosphate solids concentration. Dilute with water to a concentration, add lactic acid to the solution, adjust it to 0.2% solution concentration as lactic acid concentration, take in 100 ml of measuring cylinder, stand at 10 ° C, and become transparent due to precipitation of ferric pyrophosphate The change in the interfacial height of the colored portion of the portion and the dispersed portion of ferric pyrophosphate over time and the change of sediment amount over time were visually judged, and the stability of each ferric pyrophosphate in water was investigated. The ml unit mark engraved on the measuring cylinder is read and the results are shown in Table 5 as the following five-step display.

계면높이Interface height 계면이 존재하지 않는다Interface does not exist 55 계면이 97이상 100미만이다Interface is more than 97 and less than 100 44 계면이 90이상 97미만이다Interface is more than 90 and less than 97 33 계면이 50이상 90미만이다The interface is more than 50 and less than 90 22 계면이 50미만이다The interface is less than 50 1One

침전물의 양Amount of sediment 거의 확인할 수 없다Hardly confirmed 55 약간 침전을 확인할 수 있다Some precipitation can be confirmed 44 0.5mm정도의 침전이 있다There is precipitation about 0.5mm 33 0.5mm이상 2mm미만의 침전이 있다There is precipitation more than 0.5mm and less than 2mm 22 2mm이상의 침전이 있다There is more than 2mm of precipitation 1One

계면높이Interface height 침전물의 양Amount of sediment 1일후1 day later 3일후3 days later 7일후7 days later 1일후1 day later 3일후3 days later 7일후7 days later 실시예 1실시예 2실시예 3실시예 4실시예 5실시예 6실시예 7실시예 8실시예 9실시예 18실시예 19실시예 20실시예 21실시예 22실시예 23실시예 24실시예 25실시예 26비교예 1비교예 2비교예 3비교예 4비교예 5비교예 6비교예 7비교예 12비교예 13비교예 14비교예 15비교예 16비교예 17비교예 18Example 1 Example 2 Example 3 Example 4 Example 5 Example 6 Example 7 Example 8 Example 9 Example 18 Example 19 Example 20 Example 21 Example 22 Example 23 Example 24 Example 25 Example 26 Comparative Example 1 Comparative Example 2 Comparative Example 3 Comparative Example 4 Comparative Example 5 Comparative Example 6 Comparative Example 7 Comparative Example 12 Comparative Example 13 Comparative Example 14 Comparative Example 15 Comparative Example 16 Comparative Example 17 Comparative Example 18 5555555555555555555251122525111155555555555555555552511225251111 5445454555545455555141111514111154454545555454555551411115141111 5435354545445354545141111513111154353545454453545451411115131111 5555555555555555555251122525111155555555555555555552511225251111 5445454555445454555241111514111154454545554454545552411115141111 5334354545434354545131111513111153343545454343545451311115131111

계면높이Interface height 침전물의 양Amount of sediment 1일후1 day later 3일후3 days later 7일후7 days later 1일후1 day later 3일후3 days later 7일후7 days later 실시예 10실시예 11실시예 12실시예 13실시예 14실시예 15실시예 16실시예 17실시예 27실시예 28실시예 29실시예 30실시예 31실시예 32실시예 33실시예 34비교예 8비교예 9비교예 10비교예 11비교예 19비교예 20비교예 21비교예 22Example 10 Example 11 Example 12 Example 13 Example 14 Example 15 Example 16 Example 17 Example 27 Example 28 Example 29 Example 30 Example 31 Example 32 Example 33 Example 34 Comparative Example 8 Comparative Example 9 Comparative Example 10 Comparative Example 11 Comparative Example 19 Comparative Example 20 Comparative Example 21 Comparative Example 22 555554555555545525122511555554555555545525122511 545453355454533525111511545453355454533525111511 544352255353522515111511544352255353522515111511 555554555554545525122511555554555554545525122511 545452355454523515111511545452355454523515111511 535252355352523515111411535252355352523515111411

(실시예 35)(Example 35)

실시예 1에서 조제한 식품첨가물용 칼슘제 슬러리의 분산액 450g을, 시판우유 2.5kg, 버터 120g, 탈지유 800g을 물 4kg에 첨가교반하여 균질화하고, 통상법에 따라 살균냉각후, 미리 조정한 스타터 160g 접종하여 180cc의 컵에 충전하고, 38℃에서 5시간 발효시켜 칼슘강화 요구르트를 얻었다.450 g of the dispersion of calcium slurry for food additives prepared in Example 1 was homogenized by adding and stirring 2.5 g of commercial milk, 120 g of butter, and 800 g of skim milk to 4 kg of water. Cup was filled and fermented at 38 ° C. for 5 hours to obtain calcium fortified yogurt.

각 시료를 남녀 각 10명으로 이루어지는 관능시험을 행하여 각각 하기 4단계로 판정하여 그 평균치를 표 6에 나타낸다.Each sample was subjected to a sensory test consisting of 10 men and women, each of which was determined in the following four steps, and the average is shown in Table 6.

식감(食感)Texture 양호한 조직을 가져 혀감촉 양호하다Good texture with good texture 44 점도 다소 높고, 또는 다소 조직이 나쁘고다소 까칠하다Viscosity is somewhat high, or the organization is bad, somewhat rough 33 점도가 상당히 높고, 또는 상당히 조직이나쁘고, 상당히 까칠하다Highly viscous, or very organized, very rough 22 과농후, 또는 이수(離水)가 보이고 상당히까칠하다Overrich or diarrhea visible and quite rough 1One

풍미zest 풍미가 양호하다The flavor is good 44 풍미가 다소 나쁘다(다소 불쾌감 있음)Flavor is a little bad (somewhat unpleasant) 33 풍미가 상당히 나쁘다(상당한 불쾌감 있음)The flavor is quite bad (with significant discomfort) 22 풍미가 매우 나쁘다(매우 불쾌감 강함)Flavor is very bad (very unpleasant) 1One

(실시예 36∼43, 비교예 23∼29, 실시예 52∼60, 비교예 34∼40)(Examples 36-43, Comparative Examples 23-29, Examples 52-60, Comparative Examples 34-40)

실시예 2∼9, 비교예 1∼7 및 실시예 18∼26, 비교예 12∼18로 조제한 식품첨가물용 칼슘제 및 피로인산제2철분제 슬러리, 또는 식품첨가물용 칼슘제 및 피로인산제2철분제 파우더의 재분산액을 사용한 것을 제외하고는 실시예 35와 동일한 방법으로 칼슘과 철분강화 요구르트를 얻었다.Of the calcium additive for food additives and ferric pyrophosphate slurry prepared in Examples 2 to 9, Comparative Examples 1 to 7 and Examples 18 to 26 and Comparative Examples 12-18, or the calcium for food additives and ferric pyrophosphate powder Calcium and iron powdered yoghurt were obtained in the same manner as in Example 35 except that the redispersion was used.

또, 이들 요구르트의 관능시험을 실시예 35의 방법과 동일하게 행하였다. 그 결과를 표 6에 나타낸다.Moreover, the sensory test of these yoghurts was performed similarly to the method of Example 35. The results are shown in Table 6.

(실시예 44)(Example 44)

실시예 1에서 조제한 식품첨가물용 칼슘제 슬러리 대신 실시예 10에서 조제한 피로인산제2철분제 슬러리를 사용한 것, 및 분산액 첨가량을 40g으로 변경한 것을 제외하고는 실시예 35와 동일한 방법으로 철분강화 요구르트를 얻었다.Iron-reinforced yoghurt was obtained in the same manner as in Example 35, except that the ferric pyrophosphate slurry prepared in Example 10 was used instead of the calcium additive slurry prepared in Example 1, and the amount of dispersion was added to 40 g. .

또, 이들 요구르트의 관능시험을 실시예 35의 방법과 동일하게 행하였다. 그 결과를 표 7에 나타낸다.Moreover, the sensory test of these yoghurts was performed similarly to the method of Example 35. The results are shown in Table 7.

(실시예 45∼50, 비교예 30∼33, 실시예 61∼68, 비교예 41∼44)(Examples 45-50, Comparative Examples 30-33, Examples 61-68, Comparative Examples 41-44)

실시예 11∼16, 비교예 8∼11, 실시예 27∼34, 비교예 19∼22에서 조제한 식품첨가물용 피로인산제2철분제 슬러리, 또는 식품첨가물용 피로인산제2철분제 파우더의 재분산액을 사용하는 것을 제외하고는 실시예 44와 동일 방법으로 철분강화 요구르트를 얻었다.The redispersion liquid of the ferric pyrophosphate slurry for food additives prepared in Examples 11-16, Comparative Examples 8-11, Examples 27-34, and Comparative Examples 19-22, or the ferric pyrophosphate powder for food additives is used. Except that the iron-reinforced yogurt was obtained in the same manner as in Example 44.

또, 이들 요구르트의 관능시험을 실시예 35와 동일한 방법으로 행하였다. 그 결과를 표 7에 나타낸다.Moreover, the sensory test of these yoghurts was performed by the method similar to Example 35. The results are shown in Table 7.

(실시예 51)(Example 51)

실시예 17에서 조제한 식품첨가물용 피로인산제2철분제 슬러리를 사용한 것과 분산액 첨가량을 134g으로 변경한 것을 제외하고는 실시예 35와 동일한 방법으로 철분강화 요구르트를 얻었다.Iron-reinforced yogurt was obtained in the same manner as in Example 35, except that the ferric pyrophosphate slurry for food additives prepared in Example 17 was used, and the amount of dispersion added to 134 g was changed.

또, 이들 요구르트의 관능시험을 실시예 35와 동일한 방법으로 행하였다.Moreover, the sensory test of these yoghurts was performed by the method similar to Example 35.

그 결과를 표 7에 나타낸다.The results are shown in Table 7.

사용한 칼슘제 및철분제 슬러리 또는파우더의 재분산액Redispersion of Used Calcium and Iron Slurry or Powder 식감Texture 풍미zest 실시예 35실시예 36실시예 37실시예 38실시예 39실시예 40실시예 41실시예 42실시예 43실시예 52실시예 53실시예 54실시예 55실시예 56실시예 57실시예 58실시예 59실시예 60비교예 23비교예 24비교예 25비교예 26비교예 27비교예 28비교예 29비교예 34비교예 35비교예 36비교예 37비교예 38비교예 39비교예 40Example 35 Example 36 Example 37 Example 38 Example 39 Example 40 Example 41 Example 42 Example 43 Example 52 Example 53 Example 54 Example 55 Example 56 Example 57 Example 58 Example 59 Example 60 Comparative Example 23 Comparative Example 24 Comparative Example 25 Comparative Example 26 Comparative Example 27 Comparative Example 28 Comparative Example 29 Comparative Example 34 Comparative Example 35 Comparative Example 36 Comparative Example 37 Comparative Example 38 Comparative Example 39 Comparative Example 40 실시예 1에 의한 조제품실시예 2에 의한 조제품실시예 3에 의한 조제품실시예 4에 의한 조제품실시예 5에 의한 조제품실시예 6에 의한 조제품실시예 7에 의한 조제품실시예 8에 의한 조제품실시예 9에 의한 조제품실시예 18에 의한 조제품실시예 19에 의한 조제품실시예 20에 의한 조제품실시예 21에 의한 조제품실시예 22에 의한 조제품실시예 23에 의한 조제품실시예 24에 의한 조제품실시예 25에 의한 조제품실시예 26에 의한 조제품비교예 1에 의한 조제품비교예 2에 의한 조제품비교예 3에 의한 조제품비교예 4에 의한 조제품비교예 5에 의한 조제품비교예 6에 의한 조제품비교예 7에 의한 조제품비교예 12에 의한 조제품비교예 13에 의한 조제품비교예 14에 의한 조제품비교예 15에 의한 조제품비교예 16에 의한 조제품비교예 17에 의한 조제품비교예 18에 의한 조제품Preparation according to Example 1 Preparation according to Example 2 Preparation according to Example 3 Preparation according to Example 5 Preparation according to Example 5 Preparation according to Example 7 Preparation according to Example 8 Preparation according to Example 9 Preparation according to Example 18 Preparation according to Example 19 Preparation according to Example 20 Preparation according to Example 21 Preparation according to Example 22 Preparation According to Example 23 According to Preparation Example 24 to Example 25 Preparation preparation according to Example 26 Preparation preparation according to Example 1 Preparation preparation example according to Example 2 Preparation preparation example according to Example 3 Preparation preparation example according to example 4 Preparation preparation example according to example 5 Preparation preparation example according to example 6 Preparation example 7 Preparation Example of Comparative Example 12 Preparation Example of Comparative Example 14 Preparation Example of Comparative Example 15 Preparation Example of Comparative Example 16 Preparation Example of Comparative Example 16 Preparation Example of Comparative Example 18 Production 4444332344444332341111111111111144443323444443323411111111111111 4444332344444432341313331131333144443323444444323413133311313331

사용한 철분제슬러리 또는 철분제파우더의 재분산액Redispersion of Used Iron Slurry or Iron Powder 식감Texture 풍미zest 실시예 44실시예 45실시예 46실시예 47실시예 48실시예 49실시예 50실시예 51실시예 61실시예 62실시예 63실시예 64실시예 65실시예 66실시예 67실시예 68비교예 30비교예 31비교예 32비교예 33비교예 41비교예 42비교예 43비교예 44Example 44 Example 45 Example 46 Example 47 Example 48 Example 49 Example 50 Example 51 Example 61 Example 62 Example 63 Example 64 Example 65 Example 66 Example 67 Example 68 Comparative Example 30 Comparative Example 31 Comparative Example 32 Comparative Example 33 Comparative Example 41 Comparative Example 42 Comparative Example 43 Comparative Example 44 실시예 10에 의한 조제품실시예 11에 의한 조제품실시예 12에 의한 조제품실시예 13에 의한 조제품실시예 14에 의한 조제품실시예 15에 의한 조제품실시예 16에 의한 조제품실시예 17에 의한 조제품실시예 27에 의한 조제품실시예 28에 의한 조제품실시예 29에 의한 조제품실시예 30에 의한 조제품실시예 31에 의한 조제품실시예 32에 의한 조제품실시예 33에 의한 조제품실시예 34에 의한 조제품비교예 8에 의한 조제품비교예 9에 의한 조제품비교예 10에 의한 조제품비교예 11에 의한 조제품비교예 19에 의한 조제품비교예 20에 의한 조제품비교예 21에 의한 조제품비교예 22에 의한 조제품Preparation according to Example 10 Preparation according to Example 11 Preparation according to Example 12 Preparation according to Example 13 Preparation according to Example 14 Preparation according to Example 16 Preparation Example according to Example 16 Preparation according to Example 27 Preparation according to Example 28 Preparation according to Example 29 Preparation according to Example 30 Preparation according to Example 31 Preparation according to Example 32 According to Preparation Example 8 according to Preparation Example 34 according to Example 33 Preparation Comparative Example 9 Preparation Example Comparative Example 10 Preparation Example 11 Preparation Example Comparative Example 19 Preparation Example 21 Preparation Example 21 Preparation Example 21 Preparation Example 21 Preparation Example 22 433423344334233411111111433423344334233411111111 433324344333243431233123433324344333243431233123

(실시예 69)(Example 69)

탄산칼슘분체에 물을 첨가하여, 탄산칼슘 고형분 농도가 22중량%인 수현탁액을 조제하고, 습식분쇄기 다이노밀 KD-PILOT형을 이용하여 습식분쇄하고, 탄산칼슘의 수분산체를 얻었다. 그후, 그탄산칼슘의 수분산체에 PGA를 탄산칼슘 고형분 100중량부에 대하여 11중량부 및 물을 첨가하여 강력하게 교반혼합하여 탄산칼슘 고형분 농도가 10중량%인 혼합물을 조제후, 재차 이 혼합물을 습식분쇄기 다이노밀 KD-PILOT형을 이용하여 습식분쇄하고, 탄산칼슘슬러리 중의 탄산칼슘 입도분포에 있어서의 중량(체적)평균경이 0.20㎛에 도달한 시점에서 습식분쇄를 완료하고, 식품첨가용 칼슘제 슬러리를 얻었다. 또한, PGA는 미리 물로 용해후, 첨가하였다.Water was added to the calcium carbonate powder to prepare an aqueous suspension having a calcium carbonate solid content of 22% by weight, and wet grinding using a wet mill Dinoyl KD-PILOT to obtain an aqueous dispersion of calcium carbonate. Thereafter, 11 parts by weight of PGA was added to the aqueous dispersion of calcium carbonate and 100 parts by weight of calcium carbonate solid and water were mixed with vigorous stirring to prepare a mixture having a calcium carbonate solid concentration of 10% by weight. Wet grinding using the wet grinding machine Dinomil KD-PILOT type, the wet grinding was completed when the weight (volume) average diameter in the calcium carbonate particle size distribution in the calcium carbonate slurry reached 0.20 µm, and the calcium slurry for food addition was added. Got. In addition, PGA was added after dissolving in water previously.

(실시예 70)(Example 70)

실시예 69에서 얻은 식품첨가물용 칼슘제 슬러리를 스프레이드라이어를 사용하여 건조하여, 식품첨가물용 칼슘제 파우더를 얻었다.The calcium additive slurry for food additives obtained in Example 69 was dried using a spray dryer to obtain a calcium additive powder for food additives.

그 파우더를 65℃의 온수에 첨가하여 호모믹서로 12000rpm으로 15분간 교반하고, 칼슘제 고형분 농도가 10중량%인 재분산액을 조제하여 그 탄산칼슘슬러리의 분산체 중의 탄산칼슘 입도분포를 측정한 바, 중량(체적)평균경은 0.20㎛였다.The powder was added to hot water at 65 ° C., stirred for 15 minutes at 12000 rpm with a homomixer, a redispersion with a calcium solids concentration of 10% by weight was prepared, and the particle size distribution of calcium carbonate in the dispersion of the calcium carbonate slurry was measured. The weight (volume) average diameter was 0.20 mu m.

(비교예 45)(Comparative Example 45)

탄산칼슘 분체에 물을 첨가하여, 탄산칼슘 고형분 농도가 22중량%인 수현탁액을 조제하고, 습식분쇄기 다이노밀 KD-PILOT형을 이용하여 습식분쇄하고, 탄산칼슘의 수분산액을 얻었다. 그후, 탄산칼슘의 수분산체에, HLB가 16인 자당스테아르산에스테르를 탄산칼슘 고형분 100중량부에 대해 23중량부와 물을 첨가하여 강력하게 교반혼합하여, 탄산칼슘 고형분 농도가 10중량%인 혼합물을 조제후, 재차 이 혼합물을 습식분쇄기 다이노밀 KD-PILOT형을 이용하여 습식분쇄하고, 탄산칼슘 슬러리 중의 탄산칼슘의 입도분포에 있어서의 중량(체적)평균경이 0.21㎛에 도달한 시점에서 습식분쇄를 완료하여 식품첨가용 칼슘제 슬러리를 얻었다. 또한, 자당스테아르산에스테르는 미리 65℃의 온수에 용해후 20℃로 냉각하여 첨가하였다.Water was added to the calcium carbonate powder to prepare an aqueous suspension having a calcium carbonate solid content of 22% by weight, and wet grinding using a wet mill Dinoyl KD-PILOT to obtain an aqueous dispersion of calcium carbonate. Thereafter, 23 parts by weight of sucrose stearic acid ester having a HLB of 16 and 100 parts by weight of water were added to the aqueous dispersion of calcium carbonate, and mixed with vigorous stirring to give a calcium carbonate solid concentration of 10% by weight. After the preparation, the mixture was wet-pulverized again using a wet mill Dinomil KD-PILOT and wet-pulverized when the weight (volume) average diameter in the particle size distribution of calcium carbonate in the calcium carbonate slurry reached 0.21 µm. Then, the calcium slurry for food addition was obtained. In addition, sucrose stearate ester was melt | dissolved in 65 degreeC warm water previously, and was cooled and added to 20 degreeC.

(비교예 46)(Comparative Example 46)

탄산칼슘 고형분 100중량부에 대한 HLB가 16인 자당스테아르산에스테르 첨가량을 10중량부로 변경한 것을 제외하고는 비교예 45와 동일한 방법으로 식품첨가용 칼슘제 슬러리를 얻었다. 또한, 자당스테아르산에스테르는 미리 65℃의 온수에 용해후 20℃로 냉각하여 첨가하였다.A calcium slurry for food additives was obtained in the same manner as in Comparative Example 45 except that the sucrose stearic acid ester addition amount having HLB of 16 to 100 parts by weight of the calcium carbonate solid content was changed to 10 parts by weight. In addition, sucrose stearate ester was melt | dissolved in 65 degreeC warm water previously, and was cooled and added to 20 degreeC.

(비교예 47)(Comparative Example 47)

탄산칼슘 고형분 100중량부에 대한 PGA첨가량을 1.2중량부로 변경한 것을 제외한 기타는 실시예 69와 동일한 방법으로, 식품첨가용 칼슘제 슬러리를 얻었다. 또한, PGA는 미리 물로 용해시킨후 첨가하였다.A calcium slurry for food addition was obtained in the same manner as in Example 69 except that the amount of PGA added to 1.2 parts by weight of the calcium carbonate solid content was changed. In addition, PGA was added after dissolving in water in advance.

(비교예 48)(Comparative Example 48)

인산삼칼슘 분체에 물을 첨가하여, 인산삼칼슘 고형분 농도가 22중량%인 수현탁액을 조제하고, 습식분쇄기 다이노밀 KD-PILOT형을 이용하여 습식분쇄하고, 인산삼칼슘의 수분산액을 얻었다. 그후, 인산삼칼슘의 수분산체에, HLB가 13인 글리세린지방산에스테르를 인산삼칼슘 고형분 100중량부에 대해 30중량부와 물을 첨가하여 강력하게 교반혼합하여, 인산삼칼슘 고형분 농도가 10중량%인 혼합물을 조제후, 재차 이 혼합물을 습식분쇄기 다이노밀 KD-PILOT형을 이용하여 습식분쇄하고, 인산삼칼슘 슬러리 중의 인산칼슘의 입도분포에 있어서의 중량(체적)평균경이 0.33㎛에 도달한 시점에서 습식분쇄를 완료하여 식품첨가용 칼슘제 슬러리를 얻었다. 또한, 글리세린지방산에스테르는 미리 65℃의 온수에 용해후 20℃로 냉각하여 첨가하였다.Water was added to tricalcium phosphate powder to prepare an aqueous suspension having a tricalcium phosphate solid content concentration of 22% by weight, and wet grinding was performed using a wet grinding machine Dinomil KD-PILOT to obtain an aqueous dispersion of tricalcium phosphate. Thereafter, 30 parts by weight of water and glycerin fatty acid ester having an HLB of 13 were added to 100 parts by weight of tricalcium phosphate solids and water to the aqueous dispersion of tricalcium phosphate. After preparing the phosphorus mixture, the mixture was again pulverized using a wet grinder, Dinomil KD-PILOT, and the weight (volume) average diameter in the particle size distribution of calcium phosphate in the tricalcium phosphate slurry reached 0.33 µm. Wet grinding was completed at to obtain a calcium slurry for food addition. In addition, glycerin fatty acid ester was dissolved in hot water at 65 ° C in advance and cooled to 20 ° C and added.

(비교예 49)(Comparative Example 49)

피로인산제2철 분체에 HLB가 13인 글리세린지방산에스테르를 피로인산제2철 100중량부에 대하여 30중량부 및 물을 첨가하여 강력하게 교반혼합함으로써 피로인산제2철 고형분 농도가 10중량%인 혼합슬러리를 조제하였다. 그 혼합슬러리를 습식분쇄기 다이노밀 파일롯형을 이용하여 습식분쇄하고, 피로인산제2철분제 슬러리의 분산체를 얻었다. 또한, 그 피로인산제2철분제 슬러리 중의 피로인산제2철의 입도분포에 있어서의 중량(체적)평균경이 0.35㎛에 도달한 시점에서 습식분쇄를 완료하였다. 또한 글리세린지방산에스테르는 미리 65℃ 온수에 용해후 20℃로 냉각, 첨가하였다.The ferric pyrophosphate solids concentration was 10% by weight by vigorously stirring and mixing 30 parts by weight of glycerin fatty acid ester having a HLB of 13 with 100 parts by weight of ferric pyrophosphate and water to ferric pyrophosphate powder. Mixed slurry was prepared. This mixed slurry was wet-pulverized using the wet grinder dynomil pilot type, and the dispersion of the ferric pyrophosphate slurry was obtained. The wet grinding was completed when the weight (volume) average diameter in the particle size distribution of the ferric pyrophosphate in the ferric pyrophosphate slurry reached 0.35 m. In addition, glycerin fatty acid ester was previously dissolved in 65 캜 hot water, cooled to 20 캜 and added.

또, 그 피로인산제2철분제 슬러리의 습식분쇄전의 pH값은 2.1이고, 습식분쇄후의 pH값은 3.0이었다.Moreover, the pH value before wet grinding of the ferric pyrophosphate slurry was 2.1, and the pH value after wet grinding was 3.0.

(비교예 50)(Comparative Example 50)

비교예 45에서 얻은 식품첨가물용 칼슘제 슬러리를 스프레이드라이어를 이용하여 건조하여, 식품첨가물용 칼슘제 파우더를 얻었다.The calcium additive slurry for food additives obtained in Comparative Example 45 was dried using a spray dryer to obtain a calcium additive powder for food additives.

해당 파우더를 65℃ 온수에 첨가하여, 호모믹서에 의해 12000rpm으로 15분간 교반하고, 칼슘제 고형분 농도가 10중량%인 재분산액을 조제하여 해당 탄산칼슘 슬러리 중의 탄산칼슘의 입도분포를 측정한바, 중량(체적)평균경은 0.22㎛였다.The powder was added to hot water at 65 ° C, stirred for 15 minutes at 12000 rpm by a homomixer, a redispersion with a calcium solids concentration of 10% by weight was prepared, and the particle size distribution of calcium carbonate in the calcium carbonate slurry was measured. The volume average diameter was 0.22 micrometer.

(비교예 51)(Comparative Example 51)

비교예 46에서 얻은 식품첨가물용 칼슘제 슬러리를 스프레이드라이어를 이용하여 건조하여, 식품첨가물용 칼슘제 파우더를 얻었다.The calcium additive slurry for food additives obtained in Comparative Example 46 was dried using a spray dryer to obtain a calcium additive powder for food additives.

해당 파우더를 65℃ 온수에 첨가하여, 호모믹서에 의해 12000rpm으로 15분간 교반하고, 칼슘제 고형분 농도가 10중량%인 재분산액을 조제하여 해당 탄산칼슘 슬러리 중의 탄산칼슘의 입도분포를 측정한바, 중량(체적)평균경은 0.21㎛였다.The powder was added to hot water at 65 ° C, stirred for 15 minutes at 12000 rpm by a homomixer, a redispersion with a calcium solids concentration of 10% by weight was prepared, and the particle size distribution of calcium carbonate in the calcium carbonate slurry was measured. The volume average diameter was 0.21 micrometer.

(비교예 52)(Comparative Example 52)

비교예 47에서 얻은 식품첨가물용 칼슘제 슬러리를 스프레이드라이어를 이용하여 건조하여, 식품첨가물용 칼슘제 파우더를 얻었다.The calcium additive slurry for food additives obtained in Comparative Example 47 was dried using a spray dryer to obtain a calcium additive powder for food additives.

해당 파우더를 65℃ 온수에 첨가하여, 호모믹서에 의해 12000rpm으로 15분간 교반하고, 칼슘제 고형분 농도가 10중량%인 재분산액을 조제하여 해당 탄산칼슘 슬러리 중의 탄산칼슘의 입도분포를 측정한바, 중량(체적)평균경은 0.21㎛였다.The powder was added to hot water at 65 ° C, stirred for 15 minutes at 12000 rpm by a homomixer, a redispersion with a calcium solids concentration of 10% by weight was prepared, and the particle size distribution of calcium carbonate in the calcium carbonate slurry was measured. The volume average diameter was 0.21 micrometer.

(비교예 53)(Comparative Example 53)

비교예 48에서 얻은 식품첨가물용 칼슘제 슬러리를 스프레이드라이어를 이용하여 건조하여, 식품첨가물용 칼슘제 파우더를 얻었다.The calcium additive slurry for food additives obtained in Comparative Example 48 was dried using a spray dryer to obtain a calcium additive powder for food additives.

해당 파우더를 65℃ 온수에 첨가하여, 호모믹서에 의해 12000rpm으로 15분간 교반하고, 칼슘제 고형분 농도가 10중량%인 재분산액을 조제하여 해당 인산삼칼슘 슬러리 중의 인산삼칼슘의 입도분포를 측정한바, 중량(체적)평균경은 0.30㎛였다.The powder was added to hot water at 65 ° C., stirred at 12000 rpm for 15 minutes by a homomixer, a redispersion with a calcium solids concentration of 10% by weight was prepared, and the particle size distribution of tricalcium phosphate in the tricalcium phosphate slurry was measured. The weight (volume) average diameter was 0.30 mu m.

(비교예 54)(Comparative Example 54)

비교예 49에서 얻은 식품첨가물용 피로인산제2철분제 슬러리를 스프레이드라이어를 이용하여 건조하여, 식품첨가물용 피로인산제2철분제 파우더를 얻었다.The ferric pyrophosphate slurry for food additives obtained in Comparative Example 49 was dried using a spray dryer to obtain ferric pyrophosphate powder for food additives.

해당 파우더를 65℃ 온수에 첨가하여, 호모믹서에 의해 12000rpm으로 15분간 교반하고, 피로인산제2철분제 고형분 농도가 10중량%인 재분산액을 조제하여 해당 피로인산제2철 슬러리 중의 피로인산제2철의 입도분포를 측정한바, 중량(체적)평균경은 0.36㎛였다.The powder was added to hot water at 65 ° C., stirred for 15 minutes at 12000 rpm by a homomixer, and a redispersion solution having a solid content of 10% by weight of ferric pyrophosphate was prepared. When the particle size distribution of iron was measured, the weight (volume) average diameter was 0.36 mu m.

(실시예 71)(Example 71)

실시예 1에서 조제한 식품첨가물용 칼슘제 슬러리 분산액 450g을 60℃에서 용해시킨 파우더 400g중에 분산시켜, 이것을 탈지분 8kg중에 첨가 교반하고, 이어서 살균하여 칼슘강화우유를 얻었다.450 g of the calcium slurry dispersion for food additives prepared in Example 1 was dispersed in 400 g of powder dissolved at 60 ° C, which was added and stirred in 8 kg of skim powder, and then sterilized to obtain calcium fortified milk.

해당 칼슘강화우유를 100ml의 메스실린더에 취해, 5℃로 보존하고, 정기적으로 메스실린더 중의 우유를 조심스럽게 폐기하고, 메스실린더 저부에 잔재해 있는 침전물 양의 경시변화를 육안관찰하였다. 그 결과를 하기 3단계 표시에 의해 표 8에 나타낸다. 또, 그 칼슘강화우유의 남녀 각 10명에 의한 관능시험을 행하여, 각각 풍미에 관하여 4단계로 판정하여 그 평균치도 표 8에 나타낸다.The calcium-enriched milk was taken in 100 ml of a measuring cylinder, stored at 5 ° C, and the milk in the measuring cylinder was periodically discarded, and the change in the amount of sediment remaining in the bottom of the measuring cylinder was visually observed. The results are shown in Table 8 by the following three-step display. In addition, a sensory test was carried out by ten men and women of the calcium fortified milk, and the flavors were determined in four stages, respectively, and the average values thereof are also shown in Table 8.

침전량Sedimentation 거의 확인할 수 없다Hardly confirmed 33 약간 침전을 확인할 수 있다Some precipitation can be confirmed 22 상당히 많은 양의 침전을 확인할 수 있다A significant amount of precipitation can be found 1One

풍미zest 풍미가 양호하다The flavor is good 44 풍미가 다소 나쁘다(불쾌감 다소 있음)Flavor is a little bad (slightly unpleasant) 33 풍미가 상당히 나쁘다(상당히 불쾌감 강함)Flavor is considerably bad (quite discomfort strong) 22 풍미가 매우 나쁘다(대단히 불쾌감 강함)Flavor is very bad (very strong discomfort) 1One

(실시예 72∼79, 비교예 55∼61, 실시예 88∼96, 비교예 62∼68, 실시예 107∼108, 비교예 73∼76, 78∼81)(Examples 72-79, Comparative Examples 55-61, Examples 88-96, Comparative Examples 62-68, Examples 107-108, Comparative Examples 73-76, 78-81)

실시예 2∼9, 비교예 1∼7 및 실시예 18∼26, 비교예 12∼18, 실시예 69∼70, 비교예 45∼48, 비교예 50∼53으로 조제한 식품첨가물용 칼슘제 및 피로인산제2철분제 슬러리, 또는 식품첨가물용 칼슘제 및 피로인산제2철분제 파우더의 재분산액을 사용한 것을 제외하고는 실시예 71과 동일한 방법으로 칼슘과 철분강화우유를 얻었다. 또, 이들 칼슘 및 철분강화우유의 침전량을 실시예 71에 표시한 것과 동일 방법으로 관찰하였다. 그 결과를 표 8에 나타낸다. 또한, 그 칼슘 및 철분강화우유의 남녀 각 10명에 의한 관능시험을 행하여, 각각 풍미에 관하여 4단계로 판정하여, 그 평균치도 표 8에 나타낸다.Calcium agent and pyrophosphate for food additives prepared in Examples 2 to 9, Comparative Examples 1 to 7 and Examples 18 to 26, Comparative Examples 12 to 18, Examples 69 to 70, Comparative Examples 45 to 48, and Comparative Examples 50 to 53 Calcium and iron powdered milk were obtained in the same manner as in Example 71, except that the redispersion of the ferric slurry or the powder for the food additive and the ferric pyrophosphate powder was used. The amount of precipitated calcium and iron fortified milk was observed in the same manner as shown in Example 71. The results are shown in Table 8. In addition, a sensory test was carried out by ten men and women of calcium and iron fortified milk, and the flavors were determined in four stages, respectively, and the average values thereof are also shown in Table 8.

(실시예 80)(Example 80)

실시예 1에서 조제한 식품첨가물용 칼슘제 슬러리 대신 실시예 10에서 조제한 피로인산제2철분제 슬러리를 사용하는 것, 및 분산액 첨가량을 40g으로 변경한 것을 제외한 기타는 실시예 71과 동일 방법으로 철분강화우유를 얻었다. 또, 이들 철분강화우유 침전량을 실시예 71에 예시한 것과 동일한 방법으로 관찰하였다. 그 결과를 표 9에 나타낸다. 또, 그 철분강화우유의 남녀 각 10명에 의한 관능시험을 행하여, 각각의 풍미에 관하여 4단계로 판정하여, 그 평균치도 표 9에 나타낸다.Instead of the calcium slurry for food additives prepared in Example 1, using the ferric pyrophosphate slurry prepared in Example 10, and other than changing the addition amount of the dispersion to 40g, iron powdered milk in the same manner as in Example 71 Got it. In addition, these iron-enriched milk precipitates were observed in the same manner as in Example 71. The results are shown in Table 9. In addition, a sensory test by ten men and women of the iron fortified milk was carried out, and each flavor was determined in four stages, and the average value thereof is also shown in Table 9.

(실시예 81∼86, 비교예 83∼86, 실시예 97∼104, 비교예 87∼90, 비교예 77, 82)(Examples 81-86, Comparative Examples 83-86, Examples 97-104, Comparative Examples 87-90, Comparative Examples 77, 82)

실시예 11∼16, 비교예 8∼11, 실시예 27∼34, 비교예 19∼22, 비교예 49, 54로 조제한 식품첨가물용 피로인산제2철분제 슬러리, 또는 식품첨가물용 피로인산제2철분제 파우더의 재분산액을 사용한 것을 제외하고는 실시예 80과 동일한 방법으로 철분강화우유를 얻었다. 또, 이들 철분강화우유 침전량을 실시예 71에 예시한 것과 동일한 방법으로 관찰하였다. 그 결과를 표 9에 나타낸다. 또, 그 철분강화우유의 남녀 각 10명에 의한 관능시험을 행하여 각각 풍미에 관하여 4단계로 판정하여 그 평균치도 표 9에 나타낸다.Ferrophosphoric acid ferric phosphate slurry prepared in Examples 11 to 16, Comparative Examples 8 to 11, Examples 27 to 34, Comparative Examples 19 to 22, Comparative Examples 49 and 54, or ferric pyrophosphate for food additives Iron-reinforced milk was obtained in the same manner as in Example 80, except that the powder redispersion was used. In addition, these iron-enriched milk precipitates were observed in the same manner as in Example 71. The results are shown in Table 9. In addition, sensory tests were performed by ten men and women of the iron fortified milk, and the flavors were determined in four stages, respectively, and the average values thereof are also shown in Table 9.

(실시예 87)(Example 87)

실시예 17에서 조제한 식품첨가물용 피로인산제2철분제 슬러리를 사용하는 것, 및 분산액 첨가량을 134g으로 변경하는 것을 제외한 기타는 실시예 71과 동일 방법으로 철분강화우유를 얻었다. 또, 이들 철분강화우유 침전량을 실시예 71에 예시한 것과 동일한 방법으로 관찰하였다. 그 결과를 표 9에 나타낸다. 또, 그 철분강화우유의 남녀 각 10명에 의한 관능시험을 행하고, 각각에 풍미에 관하여 4단계 로 판정하여, 그 평균치도 표 9에 나타낸다.Iron-reinforced milk was obtained in the same manner as in Example 71 except for using the ferric pyrophosphate slurry for food additives prepared in Example 17 and changing the amount of dispersion added to 134 g. In addition, these iron-enriched milk precipitates were observed in the same manner as in Example 71. The results are shown in Table 9. In addition, a sensory test was carried out by ten men and women of the iron fortified milk, and the flavors were determined in four stages, respectively, and the average values thereof are also shown in Table 9.

사용한 칼슘제 및 철분제슬러리 또는 파우더의재분산액Redispersion of used calcium and iron slurry or powder 침전물의 양Amount of sediment 풍미zest 10일후10 days later 20일후20 days later 60일후60 days later 실시예 71실시예 72실시예 73실시예 74실시예 75실시예 76실시예 77실시예 78실시예 79실시예 88실시예 89실시예 90실시예 91실시예 92실시예 93실시예 94실시예 95실시예 96실시예 107실시예 108비교예 55비교예 56비교예 57비교예 58비교예 59비교예 60비교예 61비교예 62비교예 63비교예 64비교예 65비교예 66비교예 67비교예 68비교예 73비교예 74비교예 75비교예 76비교예 78비교예 79비교예 80비교예 81Example 71 Example 72 Example 73 Example 74 Example 75 Example 76 Example 77 Example 78 Example 79 Example 88 Example 89 Example 90 Example 91 Example 92 Example 93 Example 94 Example 95 Example 96 Example 107 Example 108 Comparative Example 55 Comparative Example 56 Comparative Example 57 Comparative Example 58 Comparative Example 59 Comparative Example 60 Comparative Example 61 Comparative Example 62 Comparative Example 63 Comparative Example 64 Comparative Example 65 Comparative Example 66 Comparative Example 67 Example 68 Comparative Example 73 Comparative 74 Comparative 75 Comparative 76 76 Comparative 78 Comparative 79 Comparative 80 실시예 1에 의한 조제품실시예 2에 의한 조제품실시예 3에 의한 조제품실시예 4에 의한 조제품실시예 5에 의한 조제품실시예 6에 의한 조제품실시예 7에 의한 조제품실시예 8에 의한 조제품실시예 9에 의한 조제품실시예 18에 의한 조제품실시예 19에 의한 조제품실시예 20에 의한 조제품실시예 21에 의한 조제품실시예 22에 의한 조제품실시예 23에 의한 조제품실시예 24에 의한 조제품실시예 25에 의한 조제품실시예 26에 의한 조제품실시예 69에 의한 조제품실시예 70에 의한 조제품비교예 1에 의한 조제품비교예 2에 의한 조제품비교예 3에 의한 조제품비교예 4에 의한 조제품비교예 5에 의한 조제품비교예 6에 의한 조제품비교예 7에 의한 조제품비교예 12에 의한 조제품비교예 13에 의한 조제품비교예 14에 의한 조제품비교예 15에 의한 조제품비교예 16에 의한 조제품비교예 17에 의한 조제품비교예 18에 의한 조제품비교예 45에 의한 조제품비교예 46에 의한 조제품비교예 47에 의한 조제품비교예 48에 의한 조제품비교예 50에 의한 조제품비교예 51에 의한 조제품비교예 52에 의한 조제품비교예 53에 의한 조제품Preparation according to Example 1 Preparation according to Example 2 Preparation according to Example 3 Preparation according to Example 5 Preparation according to Example 5 Preparation according to Example 7 Preparation according to Example 8 Preparation according to Example 9 Preparation according to Example 18 Preparation according to Example 19 Preparation according to Example 20 Preparation according to Example 21 Preparation according to Example 22 Preparation According to Example 23 According to Preparation Example 24 to Example 25 Preparation according to Example 26 Preparation according to Example 69 Preparation according to Example 70 Preparation according to Example 1 Preparation according to Example 2 Preparation according to Example 2 Preparation according to Comparative Example 4 Preparation Comparative Example 6 Comparative Preparation Example 7 Preparation Example 12 Preparation Example 13 Preparation Comparative Example 13 Preparation Example Comparative Preparation Example 15 Preparation Comparative Example 16 Preparation of Comparative Example 17 Preparation of Comparative Example 18 Preparation of Comparative Example 45 Preparation of Comparative Example 46 Preparation of Comparative Example 46 Preparation of Comparative Example 47 Preparation of Comparative Example 48 Preparation of Comparative Example 50 Preparation of Comparative Example 51 Preparation according to Example 52 Preparation according to Example 53 333333333333333333333231331323133131113111333333333333333333333231331323133131113111 332333333333333333333121321312132131113111332333333333333333333121321312132131113111 322323333332323333333121321312132131113111322323333332323333333121321312132131113111 444433234444433234441313443131344344314431444433234444433234441313443131344344314431

사용한 칼슘제 및 철분제슬러리 또는 파우더의재분산액Redispersion of used calcium and iron slurry or powder 침전물의 양Amount of sediment 풍미zest 10일후10 days later 20일후20 days later 60일후60 days later 실시예 80실시예 81실시예 82실시예 83실시예 84실시예 85실시예 86실시예 87실시예 97실시예 98실시예 99실시예 100실시예 101실시예 102실시예 103실시예 104비교예 83비교예 84비교예 85비교예 86비교예 87비교예 88비교예 89비교예 90비교예 77비교예 82Example 80 Example 81 Example 82 Example 83 Example 84 Example 85 Example 86 Example 87 Example 97 Example 98 Example 99 Example 100 Example 101 Example 102 Example 103 Example 104 Comparative Example 83 Comparative Example 84 Comparative Example 85 Comparative Example 86 Comparative Example 87 Comparative Example 88 Comparative Example 89 Comparative Example 90 Comparative Example 77 Comparative Example 82 실시예 10에 의한 조제품실시예 11에 의한 조제품실시예 12에 의한 조제품실시예 13에 의한 조제품실시예 14에 의한 조제품실시예 15에 의한 조제품실시예 16에 의한 조제품실시예 17에 의한 조제품실시예 27에 의한 조제품실시예 28에 의한 조제품실시예 29에 의한 조제품실시예 30에 의한 조제품실시예 31에 의한 조제품실시예 32에 의한 조제품실시예 33에 의한 조제품실시예 34에 의한 조제품비교예 8에 의한 조제품비교예 9에 의한 조제품비교예 10에 의한 조제품비교예 11에 의한 조제품비교예 19에 의한 조제품비교예 20에 의한 조제품비교예 21에 의한 조제품비교예 22에 의한 조제품비교예 49에 의한 조제품비교예 54에 의한 조제품Preparation according to Example 10 Preparation according to Example 11 Preparation according to Example 12 Preparation according to Example 13 Preparation according to Example 14 Preparation according to Example 16 Preparation Example according to Example 16 Preparation according to Example 27 Preparation according to Example 28 Preparation according to Example 29 Preparation according to Example 30 Preparation according to Example 31 Preparation according to Example 32 According to Preparation Example 8 according to Preparation Example 34 according to Example 33 Preparation Example by Example 9 Preparation Example by Example 10 Preparation Example by Example 11 Preparation Example by Example 19 Preparation Example by Example 20 Preparation Example by Example 21 Preparation Example by Example 22 Preparation Example by Example 49 Preparation according to Comparative Example 54 3333323333333233231313131133333233333332332313131311 3332322332323223131313131133323223323232231313131311 3232322332323223131313131132323223323232231313131311 4333243443332434312431241143332434433324343124312411

이상과 같이 본 발명의 식품첨가용 칼슘제 및/또는 피로인산제2철분제 슬러리 또는 파우더는 액 중에서의 재분산성, 액 중에서의 장기안정성, 및 풍미가 매우 우수하고, 이 식품첨가용 칼슘제 및/또는 피로인산제2철분제 슬러리, 또는 파우더를 이용하여 조제되는 식품조성물은 중성·산성의 어느 영역에 있어서도 장기간의 보존안정성이 매우 우수하다.As described above, the slurry or powder for food additive calcium and / or ferric pyrophosphate powder of the present invention is very excellent in redispersibility in liquid, long-term stability in liquid, and flavor, and the food additive calcium agent and / or fatigue The food composition prepared by using a ferric phosphate slurry or powder has excellent long-term storage stability in both neutral and acidic regions.

Claims (10)

탄산칼슘, 인산칼슘(이하, 칼슘제라 함) 및 피로인산제2철로 이루어지는 군에서 선택된 적어도 1종 100중량부에 대하여 알긴산프로필렌글리콜에스테르(이하, PGA라 함)를 1.5∼40중량부 첨가하고 또한 식품첨가제 중의 칼슘제 및/또는 철분제의 입도분포에 있어서의 중량(체적)평균경 G(㎛)가 0.04㎛
Figure pct00017
G
Figure pct00018
0.8㎛인 것을 특징으로 하는 고분산성을 갖는 식품첨가제.
1.5-40 parts by weight of an alginate propylene glycol ester (hereinafter referred to as PGA) is added to 100 parts by weight of at least one selected from the group consisting of calcium carbonate, calcium phosphate (hereinafter referred to as calcium) and ferric pyrophosphate. The weight (volume) average diameter G (μm) in the particle size distribution of the calcium agent and / or the iron agent in the food additive is 0.04 μm.
Figure pct00017
G
Figure pct00018
A food additive having high dispersibility, characterized in that 0.8㎛.
제 1 항에 있어서, PGA의 첨가량이 1.5∼30중량부인 것을 특징으로 하는 식품첨가제.The food additive according to claim 1, wherein the amount of PGA added is 1.5 to 30 parts by weight. 제 1 항에 있어서, PGA의 첨가량이 5∼15중량부인 것을 특징으로 하는 식품첨가제.The food additive of Claim 1 whose addition amount of PGA is 5-15 weight part. 제 1 항에 있어서, 칼슘제의 질소흡착법(BET법)에 의한 비표면적이 6∼60m2/g의 범위인 것을 특징으로 하는 식품첨가제.The food additive according to claim 1, wherein the specific surface area of the calcium agent by nitrogen adsorption (BET method) is in the range of 6 to 60 m 2 / g. 제 1 항 내지 3 항중 어느 한항에 있어서, 인산칼슘이 피로인산이수소칼슘, 인산일수소칼슘 및 인산삼칼슘으로 이루어지는 군에서 선택되는 적어도 1종인 것을 특징으로 하는 식품첨가제.The food additive according to any one of claims 1 to 3, wherein the calcium phosphate is at least one member selected from the group consisting of calcium dihydrogen phosphate, calcium dihydrogen phosphate and tricalcium phosphate. 피로인산제2철 100중량부에 대하여, PGA를 1.5∼40중량부 첨가하고, 하기 ①, ②를 함께 구비하는 조건하에서 분산, 분쇄하는 것을 특징으로 하는 식품첨가물용 피로인산제2철분제의 제조방법.1.5 to 40 parts by weight of PGA is added to 100 parts by weight of ferric pyrophosphate, and dispersed and pulverized under the conditions including (1) and (2) below to produce ferric pyrophosphate for food additives. .
Figure pct00019
Figure pct00019
W
Figure pct00020
1.26 ②
W
Figure pct00020
1.26 ②
X = 피로인산제2철분제 슬러리의 분쇄 또는 분산전의 pH값X = pH value before grinding or dispersing the ferric pyrophosphate slurry Y = 피로인산제2철분제 슬러리의 분쇄 또는 분산후의 pH값Y = pH value after grinding or dispersing the ferric pyrophosphate slurry Z = 피로인산제2철분제 슬러리의 철분제 고형분 농도(%)Z = iron solid concentration of ferric pyrophosphate slurry (%)
제 6 항에 있어서, PGA의 첨가량이 피로인산제2철 100중량부에 대하여 1.5∼30중량부인 것을 특징으로 하는 식품첨가물용 피로인산제2철분제의 제조방법.The method for producing ferric pyrophosphate for food additives according to claim 6, wherein the amount of PGA added is 1.5 to 30 parts by weight based on 100 parts by weight of ferric pyrophosphate. 제 6 항에 있어서, PGA의 첨가량이 피로인산제2철 100중량부에 대하여 5∼15중량부인 것을 특징으로 하는 식품첨가물용 피로인산제2철분제의 제조방법.The method for producing ferric pyrophosphate for food additives according to claim 6, wherein the amount of PGA added is 5 to 15 parts by weight based on 100 parts by weight of ferric pyrophosphate. 제 1 항 기재의 식품첨가제를 함유하여 이루어지는 것을 특징으로 하는 식품조성물.A food composition comprising the food additive according to claim 1. 제 6 항 기재의 방법으로 얻어진 식품첨가제를 함유하여 이루어지는 것을 특징으로 하는 식품조성물.A food composition comprising a food additive obtained by the method of claim 6.
KR1019970702896A 1994-11-01 1995-10-27 Highly dispersible food additive and food composition containing the same KR100262379B1 (en)

Applications Claiming Priority (3)

Application Number Priority Date Filing Date Title
JP29372094 1994-11-01
JP94-293720 1994-11-01
PCT/JP1995/002208 WO1996013176A1 (en) 1994-11-01 1995-10-27 Highly dispersible food additive and food composition containing the same

Publications (2)

Publication Number Publication Date
KR970706739A KR970706739A (en) 1997-12-01
KR100262379B1 true KR100262379B1 (en) 2000-08-01

Family

ID=17798376

Family Applications (1)

Application Number Title Priority Date Filing Date
KR1019970702896A KR100262379B1 (en) 1994-11-01 1995-10-27 Highly dispersible food additive and food composition containing the same

Country Status (5)

Country Link
JP (1) JP3189901B2 (en)
KR (1) KR100262379B1 (en)
CN (1) CN1075358C (en)
TW (1) TW334344B (en)
WO (1) WO1996013176A1 (en)

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
KR102588519B1 (en) 2023-07-13 2023-10-13 주식회사 에이비파트너스 Food additive composition with improved dispersibility and palatability

Families Citing this family (10)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP3159931B2 (en) * 1997-02-14 2001-04-23 株式会社ヤクルト本社 Fermented milk with enhanced iron content and method for producing the same
KR100491425B1 (en) * 1997-03-24 2005-05-24 마루오 칼슘 가부시키가이샤 Food additive slurry composition and powder composition and food compositions containing these, and method for producing food additive slurry composition
CN1090006C (en) * 1997-03-24 2002-09-04 丸尾钙株式会社 Food additive slurry composition and powder composition and food compositions contg. same
US5820903A (en) * 1997-06-30 1998-10-13 General Mills, Inc. Calcium fortified yogurt and methods of preparation
WO2004039178A1 (en) * 2002-10-16 2004-05-13 Maruo Calcium Company Limited Food additive composition and food composition containing the same
KR101142916B1 (en) * 2011-07-11 2012-05-10 주식회사 일신웰스 Liquid slurry composition with improved storage stability and preparation method thereof
KR102008043B1 (en) * 2012-03-21 2019-08-06 가부시키가이샤 야쿠르트 혼샤 Iron pyrophosphate composition
CN104082754A (en) * 2014-06-11 2014-10-08 南通昊友食品添加剂有限公司 Production method for ferric pyrophosphate
JP6459129B2 (en) * 2015-04-13 2019-01-30 富田製薬株式会社 Ferric pyrophosphate-containing powder and method for producing the same
JPWO2021215530A1 (en) 2020-04-23 2021-10-28

Citations (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPS5484068A (en) * 1977-12-13 1979-07-04 Kikkoman Shoyu Co Ltd Production of lactic acid fermented beverage

Family Cites Families (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPS5813358A (en) * 1981-07-15 1983-01-25 Kibun Kk Preparation of acidic soybean milk drink
JPH02142457A (en) * 1988-11-22 1990-05-31 Ichimaru Pharcos Co Ltd Stabilization of acidic solution or drink containing hem-iron

Patent Citations (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPS5484068A (en) * 1977-12-13 1979-07-04 Kikkoman Shoyu Co Ltd Production of lactic acid fermented beverage

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
KR102588519B1 (en) 2023-07-13 2023-10-13 주식회사 에이비파트너스 Food additive composition with improved dispersibility and palatability

Also Published As

Publication number Publication date
JP3189901B2 (en) 2001-07-16
CN1171035A (en) 1998-01-21
TW334344B (en) 1998-06-21
CN1075358C (en) 2001-11-28
KR970706739A (en) 1997-12-01
WO1996013176A1 (en) 1996-05-09

Similar Documents

Publication Publication Date Title
JP3512113B2 (en) Food additive slurry composition and powder composition, and food composition containing these
KR100492656B1 (en) Food additive slurry compositions and powder compositions and food compositions containing the same
KR100262379B1 (en) Highly dispersible food additive and food composition containing the same
US7264834B2 (en) Food-additive slurry composition and powder composition, and food composition containing these
JP4107380B2 (en) Food additive composition and food composition containing the same
JP4042977B2 (en) Method for producing food additive composition
KR100491425B1 (en) Food additive slurry composition and powder composition and food compositions containing these, and method for producing food additive slurry composition
JP3504217B2 (en) Food additive slurry composition and powder composition, and food composition containing these
KR100974852B1 (en) Inorganic­particle­containing additive composition, process for producing the same, and food composition containing the additive composition
JP3247173B2 (en) Method for producing calcium agent powder for food additives having high dispersibility, and food composition containing the powder
KR20050050138A (en) Food additive composition and food composition containing the same
JPH06127909A (en) Production of calcium phosphate dispersed body and food composition
JP2003235511A (en) Method for producing calcium preparation composition for food addition and the calcium preparation composition for food addition
KR0123539B1 (en) Production of highly dispersible calcium preparation powder for food additive, and food composition incorporated with
JPH06125741A (en) Calcium agent slurry for adding to food
JP4951052B2 (en) Food additive slurry composition and powder composition, and food composition containing them
JP2001186863A (en) Food additive slurry composition, powder composition and food composition containing these compositions
JPH09308460A (en) High-disperion calcium agent as food additive and food composition containing the same
JPH11146770A (en) Calcium agent for adding to food and having high dispersing capacity, and food composition containing the same
JPH06127939A (en) Production of calcium carbonate dispersion and food composition

Legal Events

Date Code Title Description
A201 Request for examination
AMND Amendment
E902 Notification of reason for refusal
AMND Amendment
E601 Decision to refuse application
J201 Request for trial against refusal decision
B701 Decision to grant
GRNT Written decision to grant
FPAY Annual fee payment

Payment date: 20130307

Year of fee payment: 14

FPAY Annual fee payment

Payment date: 20140327

Year of fee payment: 15

LAPS Lapse due to unpaid annual fee