TW201927747A - Method for producing peracetic acid composition to be used as food additive - Google Patents
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- A—HUMAN NECESSITIES
- A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
- A23L—FOODS, 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
- A23L3/00—Preservation of foods or foodstuffs, in general, e.g. pasteurising, sterilising, specially adapted for foods or foodstuffs
- A23L3/34—Preservation of foods or foodstuffs, in general, e.g. pasteurising, sterilising, specially adapted for foods or foodstuffs by treatment with chemicals
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- C07C409/24—Peroxy compounds the —O—O— group being bound between a >C=O group and hydrogen, i.e. peroxy acids
- C07C409/26—Peracetic acid
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Abstract
Description
本發明是關於使用作為食品添加物之過醋酸組成物的製造方法，再者，是關於製造使用作為食品添加物之過醋酸組成物的製造裝置，以及關於使用作為食品添加物之過醋酸組成物。The present invention relates to a method for producing a peracetic acid composition used as a food additive, and more particularly, to a manufacturing apparatus for producing a peracetic acid composition used as a food additive, and to use a peracetic acid composition as a food additive. .
自古已知將醋酸與過氧化氫作為原料即可合成過醋酸水溶液。例如，在日本特公昭61-10465號(專利文獻1)、日本特公昭37-7459號公報、或FRANK P. GREENSPAN的報告(J. Amer. Chem. Soc., 68, 907(1946))中，記載著藉由反應條件或原料投入比的選擇，得以合成過醋酸濃度為1~50重量%的過醋酸水溶液。It has been known since ancient times that an aqueous solution of peracetic acid can be synthesized using acetic acid and hydrogen peroxide as raw materials. For example, in Japanese Patent Publication No. 61-10465 (Patent Document 1), Japanese Patent Publication No. 37-7459, or FRANK P. GREENSPAN (J. Amer. Chem. Soc., 68, 907 (1946)) It is described that the peracetic acid aqueous solution having a peracetic acid concentration of 1 to 50% by weight can be synthesized through the selection of reaction conditions or the input ratio of raw materials.
又，如此所得之過醋酸水溶液，例如，日本特公昭61-10465號、日本特公昭61-14122號公報所記載般，自古以來已知因其氧化力而具有優異的殺菌、消毒、漂白等之能力。另一方面，過醋酸水溶液係與其他有機過酸同樣，是原來不安定的物質，會因加熱、雜質導致的污染等而激烈地分解，所以使用時，貯藏安定性差變成一大缺點。能使過醋酸水溶液的貯藏安定性直接向上提升的安定劑，至今並無所知，但已知藉由封止微量存在的金屬離子可間接地使貯藏安定性向上提升。The peracetic acid aqueous solution thus obtained is, for example, described in Japanese Patent Publication No. 61-10465 and Japanese Patent Publication No. 61-14122. It has been known since ancient times that it has excellent sterilization, disinfection, and bleaching due to its oxidizing power. ability. On the other hand, the peracetic acid aqueous solution is an original unstable substance like other organic peracids, and it will be decomposed violently due to heating, contamination caused by impurities, and the like. Therefore, poor storage stability during use becomes a major disadvantage. Stabilizers that can directly increase the storage stability of a peracetic acid aqueous solution have not been known so far, but it is known that the storage stability can be improved indirectly by blocking metal ions in a trace amount.
如上述，過醋酸水溶液雖具有優異的殺菌、消毒、漂白等之能力，但使用時，貯藏安定性差乃是一大缺點。為了解決此問題，至今有各種提升過醋酸水溶液的貯藏安定性之方法被提出，但仍期待有使貯藏安定性更加提升的方法。
[先前技術文獻]
[專利文獻]As mentioned above, although the peracetic acid aqueous solution has excellent sterilization, disinfection, and bleaching capabilities, poor storage stability during use is a major disadvantage. In order to solve this problem, various methods for improving the storage stability of a peracetic acid aqueous solution have been proposed so far, but methods for improving the storage stability are still expected.
[Prior technical literature]
[Patent Literature]
[專利文獻1]日本特公昭61-10465號[Patent Document 1] Japanese Patent Publication No. 61-10465
[發明所欲解決的課題][Problems to be Solved by the Invention]
本發明係以提供一種貯藏安定性優異的，使用作為食品添加物之過醋酸組成物的製造方法作為課題。再者，本發明係以提供製造上述使用作為食品添加物之過醋酸組成物的製造裝置，及提供上述使用作為食品添加物之過醋酸組成物作為課題。
[用以解決課題之手段]The present invention aims to provide a method for producing a peracetic acid composition which is excellent in storage stability and is used as a food additive. Further, the present invention has as its object to provide a manufacturing apparatus for manufacturing the peracetic acid composition used as a food additive, and to provide the peracetic acid composition used as a food additive.
[Means to solve the problem]
本發明者為了解決該等問題點而專致於研究檢討的結果發現，混合含有既定量鋁之過氧化氫水溶液、醋酸溶液及1-羥基乙叉基-1,1-二膦酸，藉此所得之過醋酸組成物的貯藏安定性會跳躍性地向上提升，終於完成本發明。
即本發明如下。
＜1＞ 一種使用作為食品添加物之過醋酸組成物的製造方法，其係包含混合過氧化氫水溶液、醋酸溶液及含1-羥基乙叉基-1,1-二膦酸之物質的步驟，特徵係
前述過氧化氫水溶液含有鋁10μg/kg以上，且含有過氧化氫30～40質量%。
＜2＞ 如上述＜1＞之製造方法，其中，前述過氧化氫水溶液進一步含有鐵50μg/kg以下，且含有PO4 3-
50mg/kg以下。
＜3＞ 如上述＜1＞或＜2＞之製造方法，其中，前述醋酸溶液含有鋁10μg/kg以上、含有鐵50μg/kg以下、含有PO4 3-
50mg/kg以下，且含有醋酸90~99.99質量%。
＜4＞ 如上述＜1＞~＜3＞中任一項之製造方法，其中，前述含1-羥基乙叉基-1,1-二膦酸之物質含有鋁10μg/kg以上、含有鐵7mg/kg以下、含有PO4 3-
50mg/kg以下，且含有1-羥基乙叉基-1,1-二膦酸55~65質量%。
＜5＞ 如上述＜1＞~＜4＞中任一項之製造方法，其中，前述混合步驟中混合溫度為25~35℃。
＜6＞ 如上述＜1＞~＜5＞中任一項之製造方法，其中，前述混合步驟中混合時間為60分以下。
＜7＞ 如上述＜1＞~＜6＞中任一項之製造方法，其中，前述混合步驟中係於混合之後靜置1日以上。
＜8＞ 如上述＜1＞~＜7＞中任一項之製造方法，其中，進一步包含將所得之過醋酸組成物以水稀釋之步驟。
＜9＞ 一種製造使用作為食品添加物之過醋酸組成物的製造裝置，其係用於上述＜1＞~＜8＞中任一項之使用作為食品添加物之過醋酸組成物的製造方法之製造裝置，其特徵係
具有混合過氧化氫溶液、醋酸溶液及含1-羥基乙叉基-1,1-二膦酸之物質並攪拌而溶解用的混合釜、過氧化氫水溶液投入裝置、溶解之冰醋酸投入裝置及1-羥基乙叉基-1,1-二膦酸投入裝置。
＜10＞ 一種使用作為食品添加物之過醋酸組成物，其係含有鋁50μg/kg以上、含有鐵300μg/kg以下、含有PO4 3-
200mg/kg以下，且以過氧化氫換算，全過氧化物濃度為10～18質量%。
＜11＞ 一種使用作為食品添加物之過醋酸組成物，其係含有鋁25μg/kg以上、含有鐵20μg/kg以下、含有PO4 3-
15mg/kg以下，且以過氧化氫換算，全過氧化物濃度為5～12質量%。
＜12＞ 如上述＜11＞之過醋酸組成物，其係平衡常數為2以上。
＜13＞ 如上述＜11＞或＜12＞之過醋酸組成物，其係不具引火點。
＜14＞ 一種食品的殺菌方法，其係使上述＜10＞~＜13＞中任一項之過醋酸組成物與食品接觸。
[發明之效果]In order to solve these problems, the present inventors devoted themselves to research and review, and found that a hydrogen peroxide aqueous solution containing an amount of aluminum, an acetic acid solution, and 1-hydroxyethylidene-1,1-diphosphonic acid were mixed, thereby The storage stability of the obtained peracetic acid composition will be improved upwards, and the present invention is finally completed.
That is, the present invention is as follows.
<1> A method for producing a peracetic acid composition as a food additive, comprising a step of mixing an aqueous hydrogen peroxide solution, an acetic acid solution, and a substance containing 1-hydroxyethylidene-1,1-diphosphonic acid, The feature is that the aforementioned hydrogen peroxide aqueous solution contains 10 μg / kg or more of aluminum and 30 to 40% by mass of hydrogen peroxide.
<2> The production method according to the above <1>, wherein the aqueous hydrogen peroxide solution further contains 50 μg / kg or less of iron and PO 4 3 to 50 mg / kg or less.
<3> The method according to the above <1> or <2>, wherein the acetic acid solution contains 10 μg / kg or more of aluminum, 50 μg / kg or less of iron, PO 4 3 to 50 mg / kg or less, and 90 to 50% of acetic acid. 99.99% by mass.
<4> The method according to any one of <1> to <3>, wherein the substance containing 1-hydroxyethylidene-1,1-diphosphonic acid contains 10 μg / kg or more of aluminum and 7 mg of iron / kg or less, containing PO 4 3 to 50 mg / kg or less, and containing 55 to 65% by mass of 1-hydroxyethylidene-1,1-diphosphonic acid.
<5> The manufacturing method according to any one of <1> to <4>, wherein the mixing temperature in the mixing step is 25 to 35 ° C.
<6> The manufacturing method according to any one of <1> to <5>, wherein the mixing time in the mixing step is 60 minutes or less.
<7> The manufacturing method according to any one of the above <1> to <6>, wherein in the mixing step, the mixture is left to stand for more than 1 day after mixing.
<8> The manufacturing method according to any one of <1> to <7>, further comprising a step of diluting the obtained peracetic acid composition with water.
<9> A manufacturing apparatus for manufacturing and using a peracetic acid composition as a food additive, which is used in the method for manufacturing a peracetic acid composition as a food additive in any one of the above <1> to <8>. The manufacturing device is characterized by having a mixing kettle for mixing and dissolving a hydrogen peroxide solution, an acetic acid solution, and a substance containing 1-hydroxyethylidene-1,1-diphosphonic acid, a hydrogen peroxide solution input device, and Glacial acetic acid input device and 1-hydroxyethylidene-1,1-diphosphonic acid input device.
<10> A use of peracetic acid as a food additive composition, which comprises an aluminum-based 50μg / kg or more, an iron containing 300μg / kg or less, and PO 4 3- 200mg / kg or less, in terms of hydrogen peroxide and, over the whole The oxide concentration is 10 to 18% by mass.
<11> A peracetic acid composition used as a food additive, which contains 25 μg / kg or more of aluminum, 20 μg / kg or less of iron, and PO 4 3 to 15 mg / kg or less. The oxide concentration is 5 to 12% by mass.
<12> The peracetic acid composition according to the above <11> has a system equilibrium constant of 2 or more.
<13> The peracetic acid composition according to the above <11> or <12> has no ignition point.
<14> A method for sterilizing a food, in which the peracetic acid composition according to any one of the above <10> to <13> is brought into contact with food.
[Effect of the invention]
根據本發明，係可提供貯藏安定性優異的，使用作為食品添加物之過醋酸組成物的製造方法。再者，本發明係可提供製造上述使用作為食品添加物之過醋酸組成物的製造裝置，以及提供上述使用作為食品添加物之過醋酸組成物。
[用以實施發明之形態]According to the present invention, it is possible to provide a method for producing a peracetic acid composition which is excellent in storage stability and is used as a food additive. Furthermore, the present invention can provide a manufacturing apparatus for producing the above-mentioned peracetic acid composition used as a food additive, and to provide the above-mentioned peracetic acid composition used as a food additive.
[Forms for Implementing Invention]
以下，就本發明之使用作為食品添加物之過醋酸組成物的製造方法具體地說明。此外，以下說明之材料及構成等並非是限定本發明者，在本發明之趣旨範圍內可做各種改變。此外，本說明書中使用數值範圍以「~」表示時，乃是包含兩端之數值。Hereinafter, the manufacturing method of the peracetic acid composition used as a food additive of this invention is demonstrated concretely. In addition, the materials and structures described below are not intended to limit the present inventor, and various changes can be made within the scope of the gist of the present invention. In addition, when the numerical range used in this specification is expressed by "~", the numerical values at both ends are included.
本發明之一實施形態，係使用作為食品添加物之過醋酸組成物的製造方法，包含混合過氧化氫水溶液、醋酸溶液及含1-羥基乙叉基-1,1-二膦酸之物質的步驟，其中，前述過氧化氫水溶液係含有鋁10μg/kg以上，且含有過氧化氫30~40質量%。
前述過氧化氫水溶液含有鋁，較佳為10~1000μg/kg、更佳為50~500、特佳為80~400μg/kg。前述過氧化氫水溶液藉由含有鋁10μg/kg以上，因前述過醋酸組成物的貯藏安定性會向上提升而較佳。
又，前述過氧化氫水溶液含有過氧化氫，較佳為32~38質量%、更佳為35~36質量%。前述過氧化氫水溶液藉由含有過氧化氫30~40質量%，因會成為安全、安定、符合食品添加物之成分規格之過氧化氫而較佳。
本發明的過醋酸組成物的製造方法中，已知由醋酸溶液與過氧化氫水溶液而得過醋酸組成物之反應係依下述式之平衡反應。
本反應之反應速度比較慢，為了縮短反應時間，係可使用質子酸觸媒。醋酸溶液雖可以水溶液的形態來添加，但為了反應時間短縮，期望更高濃度者，通常可使用冰醋酸。過氧化氫水溶液之濃度，為了反應時間短縮雖期望更高濃度者，但若從操作時之安全性來考量，則期望更低濃度者，可使用較佳為32~38質量%、更佳為35~36質量%之水溶液。One embodiment of the present invention is a method for producing a peracetic acid composition as a food additive, comprising a mixture of an aqueous hydrogen peroxide solution, an acetic acid solution, and a substance containing 1-hydroxyethylidene-1,1-diphosphonic acid. A step in which the aforementioned hydrogen peroxide aqueous solution contains 10 μg / kg or more of aluminum, and contains 30 to 40% by mass of hydrogen peroxide.
The aqueous hydrogen peroxide solution contains aluminum, preferably 10 to 1000 μg / kg, more preferably 50 to 500, and particularly preferably 80 to 400 μg / kg. It is preferable that the hydrogen peroxide aqueous solution contains aluminum in an amount of 10 μg / kg or more, because the storage stability of the peracetic acid composition is improved upward.
The hydrogen peroxide solution contains hydrogen peroxide, preferably 32 to 38% by mass, and more preferably 35 to 36% by mass. The above-mentioned hydrogen peroxide aqueous solution contains 30 to 40% by mass of hydrogen peroxide, which is preferable because it is safe, stable, and conforms to the ingredient specifications of food additives.
In the method for producing a peracetic acid composition of the present invention, it is known that the reaction of obtaining a peracetic acid composition from an acetic acid solution and an aqueous hydrogen peroxide solution is an equilibrium reaction according to the following formula.
The reaction speed of this reaction is relatively slow. In order to shorten the reaction time, a protonic acid catalyst can be used. Although the acetic acid solution can be added in the form of an aqueous solution, in order to shorten the reaction time, if a higher concentration is desired, glacial acetic acid is usually used. Although the concentration of the hydrogen peroxide solution is expected to be shorter in order to shorten the reaction time, if it is considered from the viewpoint of safety during operation, it is preferable to use a lower concentration, preferably 32 to 38% by mass, more preferably 35 ~ 36 mass% aqueous solution.
本發明中使用的1-羥基乙叉基-1,1-二膦酸(以下稱為「HEDP」)乃是具有金屬封止作用之質子酸，賦予所得過醋酸組成物之貯藏安定性向上提升。為了獲得本發明的過醋酸組成物，雖可考量各種方法，但一般而言，係於上述1-羥基乙叉基-1,1-二膦酸之存在下使過氧化氫水溶液及醋酸溶液以較佳為1：1~5莫耳、更佳為1：2~4莫耳之比例反應的方法來實施。必要時，係可將該反應粗液以水、過氧化氫水溶液或醋酸溶液中之1種以上予以稀釋。
本發明中使用的1-羥基乙叉基-1,1-二膦酸的使用量，過醋酸組成物中較佳為0.1~1.0質量%、更佳為0.2~0.9質量%。1-羥基乙叉基-1,1-二膦酸的使用量若大於1.0質量%，前述過醋酸組成物會有不符食品添加物之成分規格的情況，另一方面，若較0.1質量%更少，前述過醋酸組成物的貯藏安定性會有降低的情況。The 1-hydroxyethylidene-1,1-diphosphonic acid (hereinafter referred to as "HEDP") used in the present invention is a protonic acid with a metal-sealing effect, which improves the storage stability of the obtained peracetic acid composition. . In order to obtain the peracetic acid composition of the present invention, although various methods can be considered, in general, an aqueous hydrogen peroxide solution and an acetic acid solution are prepared in the presence of the above-mentioned 1-hydroxyethylidene-1,1-diphosphonic acid. The reaction method is preferably performed in a ratio of 1: 1 to 5 moles, more preferably 1: 2 to 4 moles. If necessary, the crude reaction liquid can be diluted with one or more kinds of water, aqueous hydrogen peroxide solution or acetic acid solution.
The amount of 1-hydroxyethylidene-1,1-diphosphonic acid used in the present invention is preferably 0.1 to 1.0% by mass, and more preferably 0.2 to 0.9% by mass in the peracetic acid composition. If the amount of 1-hydroxyethylidene-1,1-diphosphonic acid is more than 1.0% by mass, the aforementioned peracetic acid composition may not meet the ingredient specifications of food additives. On the other hand, if it is more than 0.1% by mass If it is small, the storage stability of the peracetic acid composition may be reduced.
前述過氧化氫水溶液係以含有鐵50μg/kg以下，且含有PO4 3-
50mg/kg以下為佳。前述過氧化氫水溶液含有鐵，更佳為30μg/kg以下、特佳為1μg/kg以上30μg/kg以下，且含有PO4 3-
，更佳為40mg/kg以下、特佳為1mg/kg以上40mg/kg以下。
前述過氧化氫水溶液若含有鐵50μg/kg以下，則前述過醋酸組成物的貯藏安定性會向上提升而較佳。又，前述過氧化氫水溶液若含有PO4 3-
50mg/kg以下，則因成為符合食品添加物的成分規格之過氧化氫而較佳。The hydrogen peroxide aqueous solution containing an iron-based 50μg / kg or less, and containing PO 4 3- 50mg / kg or less is preferable. The aqueous hydrogen peroxide solution contains iron, more preferably 30 μg / kg or less, particularly preferably 1 μg / kg or more and 30 μg / kg or less, and PO 4 3- , more preferably 40 mg / kg or less, and particularly preferably 1 mg / kg or more. Below 40mg / kg.
If the aqueous hydrogen peroxide solution contains 50 μg / kg or less of iron, the storage stability of the peracetic acid composition will be improved upward, which is preferable. In addition, if the aqueous hydrogen peroxide solution contains PO 4 3 to 50 mg / kg or less, it is preferred to be hydrogen peroxide that meets the component specifications of food additives.
前述醋酸溶液係以含有鋁10μg/kg以上、含有鐵50μg/kg以下、含有PO4 3- 50mg/kg以下，且含有醋酸90~99.99質量%為佳。前述醋酸溶液含有鋁，更佳為10~1000μg/kg、特佳為50~150μg/kg，含有鐵更佳為30μg/kg以下、特佳為1μg/kg以上30μg/kg以下，含有PO4 3- 更佳為30mg/kg以下、特佳為0~15mg/kg，含有醋酸，更佳為95~99.99質量%、特佳為99~99.99質量%。The acetic acid solution preferably contains 10 μg / kg or more of aluminum, 50 μg / kg or less of iron, 3 to 50 mg / kg of PO 4 or less, and 90 to 99.99% by mass of acetic acid. The aforementioned acetic acid solution contains aluminum, more preferably 10 to 1000 μg / kg, particularly preferably 50 to 150 μg / kg, more preferably iron, 30 μg / kg or less, particularly preferably 1 μg / kg to 30 μg / kg, and contains PO 4 3 - more preferably 30mg / kg or less, and particularly preferably 0 ~ 15mg / kg, containing acetic acid, more preferably 95 to 99.99 mass%, particularly preferably 99 to 99.99 mass%.
本發明中所使用的含1-羥基乙叉基-1,1-二膦酸之物質，係以含有鋁10μg/kg以上、含有鐵7mg/kg以下、含有PO4 3-
50mg/kg以下，且含有1-羥基乙叉基-1,1-二膦酸55~65質量%為佳。
前述含1-羥基乙叉基-1,1-二膦酸之物質含有鋁更佳為10~1000μg/kg，含有鐵更佳為5mg/kg以下、特佳為0.1~5mg/kg，含有PO4 3-
更佳為30mg/kg以下、特佳為0~15mg/kg，含有1-羥基乙叉基-1,1-二膦酸更佳為58~62質量%。The 1-hydroxyethylidene-1,1-diphosphonic acid-containing substance used in the present invention is one containing 10 μg / kg or more of aluminum, 7 mg / kg or less of iron, and 3 to 50 mg / kg of PO 4 or less. The content of 1-hydroxyethylidene-1,1-diphosphonic acid is preferably 55 to 65% by mass.
The aforementioned 1-hydroxyethylidene-1,1-diphosphonic acid-containing substance preferably contains 10 to 1000 μg / kg of aluminum, more preferably 5 mg / kg or less of iron, and particularly preferably 0.1 to 5 mg / kg of PO, and contains PO. 4 3- is more preferably 30 mg / kg or less, particularly preferably 0 to 15 mg / kg, and 1-hydroxyethylidene-1,1-diphosphonic acid is more preferably 58 to 62% by mass.
前述混合步驟中混合溫度係以25~35℃為佳、25~30℃更佳。混合溫度若為25~35℃，則反應速度不會過慢，且在可抑制醋酸的揮發及過氧化氫、過醋酸之分解的點上較佳。
前述混合步驟中混合時間係以60分以下為佳、10~60分更佳。混合時間若超過60分，則混合所需的電力消費量會變大，成本會增加。
前述混合步驟中於混合之後靜置1日以上，在反應終了之點上較佳，靜置1~10日更佳。
本發明中，再以包含將所得之過醋酸組成物以水稀釋之步驟，在不會引火之點上較佳。The mixing temperature in the foregoing mixing step is preferably 25 to 35 ° C, and more preferably 25 to 30 ° C. If the mixing temperature is 25 to 35 ° C, the reaction rate will not be too slow, and it is preferable that the volatilization of acetic acid and the decomposition of hydrogen peroxide and peracetic acid can be suppressed.
The mixing time in the aforementioned mixing step is preferably 60 minutes or less, and more preferably 10 to 60 minutes. If the mixing time exceeds 60 minutes, the power consumption required for mixing will increase, and the cost will increase.
In the aforementioned mixing step, it is allowed to stand for more than 1 day after mixing. It is better at the end of the reaction, and it is more preferable to let it stand for 1 to 10 days.
In the present invention, it is preferable to further include a step of diluting the obtained peracetic acid composition with water, since it does not cause ignition.
本發明的其他一實施形態，乃是一種製造使用作為食品添加物之過醋酸組成物的製造裝置，其係用於上述使用作為食品添加物之過醋酸組成物的製造方法之製造裝置，具有混合過氧化氫溶液、醋酸溶液及含1-羥基乙叉基-1,1-二膦酸之物質並攪拌而溶解用的混合釜、過氧化氫水溶液投入裝置、溶解之冰醋酸投入裝置、及1-羥基乙叉基-1,1-二膦酸投入裝置。Another embodiment of the present invention is a manufacturing apparatus for manufacturing a peracetic acid composition used as a food additive, which is a manufacturing apparatus used for the above-mentioned manufacturing method of a peracetic acid composition used as a food additive, and has mixing Mixing kettle for hydrogen peroxide solution, acetic acid solution and 1-hydroxyethylidene-1,1-diphosphonic acid and stirring and dissolving, hydrogen peroxide solution input device, dissolved glacial acetic acid input device, and 1 -Hydroxyethylidene-1,1-diphosphonic acid is charged into the device.
藉由本發明的製造方法所得之過醋酸組成物含有過醋酸較佳為5~20質量%、更佳為5~15質量%，含有過氧化氫較佳為4~15質量%、更佳為4~10質量%，含有醋酸較佳為10~50質量%、更佳為30~50質量%。過醋酸之濃度未達5質量%的話，因過醋酸的安定性會降低而不佳，又若超過20質量%，則操作時的危險性會變大而不佳。又，過氧化氫之濃度，若超過15質量%時同樣不佳，醋酸之濃度若超過50質量%時，在對人體的刺激性或臭氣的面上較不佳。The peracetic acid composition obtained by the production method of the present invention preferably contains 5 to 20% by mass, more preferably 5 to 15% by mass, and preferably contains 4 to 15% by mass, and more preferably 4 to 4%. ~ 10% by mass. The content of acetic acid is preferably 10 ~ 50% by mass, and more preferably 30 ~ 50% by mass. If the concentration of peracetic acid is less than 5% by mass, the stability of peracetic acid will be lowered, and if it exceeds 20% by mass, the danger during operation will be increased. Also, if the concentration of hydrogen peroxide exceeds 15% by mass, the same is not good, and if the concentration of acetic acid exceeds 50% by mass, it is not good on the irritating or odorous surface of the human body.
藉由本發明的製造方法所得之過醋酸組成物，係以下述二個實施形態所示者。
即，本發明之一實施形態係含鋁50μg/kg以上(較佳為50~300μg/kg)、含鐵300μg/kg以下(較佳為250μg/kg以下)、含PO4 3-
200mg/kg以下(較佳為0.1~100mg/kg)，且在過氧化氫換算下，係為全過氧化物濃度為10~18質量%(較佳為11~15質量%)之使用作為食品添加物之過醋酸組成物。The peracetic acid composition obtained by the production method of the present invention is shown in the following two embodiments.
That is, one embodiment of the present invention contains aluminum 50 μg / kg or more (preferably 50 to 300 μg / kg), iron 300 μg / kg or less (preferably 250 μg / kg or less), and PO 4 3 to 200 mg / kg. The following (preferably 0.1 to 100 mg / kg) and the total peroxide concentration in terms of hydrogen peroxide are 10 to 18% by mass (preferably 11 to 15% by mass) for use as a food additive Peracetic acid composition.
再者、本發明之另外的一實施形態係使用作為食品添加物之過醋酸組成物，其特徵係含鋁25μg/kg以上(較佳為25~200μg/kg)、含鐵20μg/kg以下(較佳為15μg/kg以下)、含PO4 3-
15mg/kg以下(較佳為0.1~10mg/kg)，且以過氧化氫換算，全過氧化物濃度為5~12質量%(較佳為6~11質量%)。
上述過醋酸組成物中的平衡常數係2以上為佳、2~3更佳。平衡常數未達2的話，前述過醋酸組成物的貯藏安定性會有降低的情況。
上述過醋酸組成物不具引火點，在操作時的安全性之點上較佳。In addition, another embodiment of the present invention uses a peracetic acid composition as a food additive, which is characterized by containing 25 μg / kg or more of aluminum (preferably 25 to 200 μg / kg) or less than 20 μg / kg of iron ( It is preferably 15 μg / kg or less), containing PO 4 3 to 15 mg / kg or less (preferably 0.1 to 10 mg / kg), and in terms of hydrogen peroxide, the total peroxide concentration is 5 to 12 mass% (preferably (6 to 11% by mass).
The equilibrium constant in the peracetic acid composition is preferably 2 or more, and more preferably 2 to 3. If the equilibrium constant is less than 2, the storage stability of the peracetic acid composition may decrease.
The above peracetic acid composition has no ignition point, and is preferable in terms of safety during operation.
本發明中所謂的過氧化物(以下稱為全過氧化物)，係指本發明的過醋酸組成物中的過醋酸與過氧化氫，各自濃度(mol/L)的和稱為過氧化物濃度(以下稱為全過氧化物濃度)。本發明的過醋酸組成物中的過氧化物濃度較佳為1~7mol/L、更佳為2~5mol/L。低於此範圍時，過醋酸濃度即殺菌力會降低，而超過此範圍時，則安定性會有降低的情況。The so-called peroxide (hereinafter referred to as total peroxide) in the present invention refers to the sum of the respective concentrations (mol / L) of peracetic acid and hydrogen peroxide in the peracetic acid composition of the present invention. Concentration (hereinafter referred to as the total peroxide concentration). The peroxide concentration in the peracetic acid composition of the present invention is preferably 1 to 7 mol / L, and more preferably 2 to 5 mol / L. Below this range, the concentration of peracetic acid, that is, the bactericidal power will decrease, and if it exceeds this range, the stability may decrease.
本發明之另外的一實施形態，係使本發明的過醋酸組成物與食品接觸之食品的殺菌方法。使過醋酸組成物與食品接觸之方法，可舉例如，於過醋酸組成物中使食品浸漬之方法，或是對食品噴霧過醋酸組成物之方法等，但並不受限於此等。
本發明的過醋酸組成物，因貯藏安定性優，在使用於食品的殺菌方法時優點也多。Another embodiment of the present invention is a method for sterilizing a food in which the peracetic acid composition of the present invention is brought into contact with food. The method for bringing the peracetic acid composition into contact with food includes, for example, a method of impregnating food in a peracetic acid composition, or a method of spraying a peracetic acid composition on food, but is not limited thereto.
The peracetic acid composition of the present invention has excellent storage stability, and has many advantages when used in a food sterilization method.
[實施例][Example]
以下，藉由實施例進一步詳細地說明本實施形態，但本實施形態並不受限於此等實施例。各物性值的測定係以下述所示之方法來進行。Hereinafter, this embodiment will be described in more detail by way of examples, but this embodiment is not limited to these examples. The measurement of each physical property value was performed by the method shown below.
＜過醋酸組成物的過氧化氫濃度＞
過醋酸組成物的過氧化氫濃度藉由氧化還原滴定來進行。具體而言，精密地秤量試料約0.1g，置入250mL的三角燒瓶，加入75mL的0.5mol/L硫酸當作檢液。於此檢液中滴加數滴試亞鐵靈試液，再以0.1mol/L硫酸鈰(IV)溶液滴定，算出過氧化氫濃度。＜ Hydrogen peroxide concentration of peracetic acid composition ＞
The hydrogen peroxide concentration of the peracetic acid composition was performed by redox titration. Specifically, approximately 0.1 g of the sample is accurately weighed, placed in a 250 mL Erlenmeyer flask, and 75 mL of 0.5 mol / L sulfuric acid is used as a test solution. Several drops of the test ferrous solution were added to this test solution, and then titrated with a 0.1 mol / L cerium (IV) sulfate solution to calculate the hydrogen peroxide concentration.
＜過醋酸組成物的醋酸及過醋酸濃度＞
過醋酸組成物的醋酸及過醋酸濃度係藉由中和滴定來進行。具體而言，精密地秤量試料約0.1g，置入100mL的燒杯，加入純水約50mL作為檢液。將此檢液以0.1mol/L氫氧化鈉溶液滴定，由第一拐點下的添加量算出醋酸濃度、由第一拐點至第二拐點的添加量算出過醋酸濃度。＜ Acetic acid and peracetic acid concentration of peracetic acid composition ＞
The acetic acid and peracetic acid concentrations of the peracetic acid composition were performed by neutralization titration. Specifically, approximately 0.1 g of the sample is accurately weighed, placed in a 100 mL beaker, and approximately 50 mL of pure water is added as a test solution. This test solution was titrated with a 0.1 mol / L sodium hydroxide solution, and the acetic acid concentration was calculated from the addition amount at the first inflection point, and the peracetic acid concentration was calculated from the addition amount at the first inflection point to the second inflection point.
＜過醋酸組成物的全過氧化物濃度＞
過醋酸組成物的全過氧化物濃度係藉由碘還原滴定法來進行。具體而言，精密地秤量試料約0.1g，置入250mL的三角燒瓶，加入純水100mL、1.8mol/L硫酸10mL之後，加入10質量%之碘化鉀溶液10mL且滴入1質量%鉬酸銨溶液數滴作為檢液。於此檢液中滴入0.1mol/L硫代硫酸鈉溶液，對指示劑使用澱粉直到液體的青紫色消失變成無色為止作為終點，來定量游離的碘。從該碘量以過氧化氫換算計算出全過氧化物濃度。<Total peroxide concentration of peracetic acid composition>
The total peroxide concentration of the peracetic acid composition was measured by an iodine reduction titration method. Specifically, approximately 0.1 g of the sample is accurately weighed, placed in a 250 mL Erlenmeyer flask, 100 mL of pure water and 10 mL of 1.8 mol / L sulfuric acid are added, 10 mL of 10% by mass potassium iodide solution is added, and 1% by mass of ammonium molybdate solution A few drops are used as the test solution. A 0.1 mol / L sodium thiosulfate solution was added dropwise to this test solution, and starch was used as an indicator until the blue-violet color of the liquid disappeared and became colorless as an end point to quantify free iodine. From this amount of iodine, the total peroxide concentration was calculated in terms of hydrogen peroxide.
＜過醋酸組成物的安定度＞
過醋酸組成物的安定度，乃是將置入時的全過氧化物濃度作為100，藉由測定時的全過氧化物濃度之比率來算出。＜ Stability of peracetic acid composition ＞
The stability of the peracetic acid composition was calculated by taking the total peroxide concentration at the time of insertion as 100 and the ratio of the total peroxide concentration at the time of measurement.
＜過醋酸組成物的平衡常數＞
過醋酸組成物的平衡常數係由下述式算出。
平衡常數=過醋酸濃度(mol/L)×水之濃度(mol/L)
÷過氧化氫濃度(mol/L)÷醋酸濃度(mol/L)<Equilibrium constant of peracetic acid composition>
The equilibrium constant of the peracetic acid composition is calculated by the following formula.
Equilibrium constant = concentration of peracetic acid (mol / L) × concentration of water (mol / L)
÷ hydrogen peroxide concentration (mol / L) ÷ acetic acid concentration (mol / L)
＜過醋酸組成物的引火點＞
過醋酸組成物的引火點係藉由Cleveland開放式引火點試驗所測定。依照JIS-K2265之方法，使用Cleveland開放式引火點試驗器。<Ignition point of peracetic acid composition>
The ignition point of a peracetic acid composition was measured by a Cleveland open ignition point test. In accordance with the method of JIS-K2265, a Cleveland open ignition point tester was used.
(實施例1)
將純水2.8g與60質量%的1-羥基乙叉基-1,1-二膦酸(Italmatch Japan股份公司製、製品名：Dequest 2010) 0.6g、冰醋酸29.8g(昭和電工股份公司製、製品名：99%純良醋酸)、35質量%的過氧化氫水溶液(三菱瓦斯化學股份公司製、製品名：Diapower HP、含微量鋁)16.8g、SUS304(別名：18Cr-8Ni、18鉻不鏽鋼)之試驗片置入聚乙烯容器內予以混合。調合時的全過氧化物濃度為11.9%。混合後，於25℃靜置10日，獲得含有過氧化氫5.5質量%、醋酸48.7質量%、過醋酸13.4質量%及1-羥基乙叉基-1,1-二膦酸0.8質量%之使用作為食品添加物之過醋酸組成物。放入SUS304之試驗片的目的，是假設以SUS容器製造過醋酸組成物之故。所得的過醋酸組成物，自調合起21日後測定全過氧化物濃度，且計算安定度。(Example 1)
2.8 g of pure water and 60% by mass of 1-hydroxyethylidene-1,1-diphosphonic acid (manufactured by Italmatch Japan Co., Ltd., product name: Dequest 2010) 0.6 g and 29.8 g of glacial acetic acid (manufactured by Showa Denko Corporation) Product name: 99% pure acetic acid), 35 mass% hydrogen peroxide solution (manufactured by Mitsubishi Gas Chemical Co., Ltd., product name: Diapower HP, containing trace aluminum) 16.8g, SUS304 (alias: 18Cr-8Ni, 18 chromium stainless steel The test pieces of) were mixed in a polyethylene container. The total peroxide concentration during blending was 11.9%. After mixing, it was left to stand at 25 ° C for 10 days to obtain a use containing 5.5% by mass of hydrogen peroxide, 48.7% by mass of acetic acid, 13.4% by mass of peracetic acid, and 0.8% by mass of 1-hydroxyethylidene-1,1-diphosphonic acid. Peracetic acid composition as a food additive. The purpose of putting the test piece of SUS304 is to assume that the peracetic acid composition is manufactured in a SUS container. The obtained peracetic acid composition was measured for the total peroxide concentration 21 days after the blending, and the stability was calculated.
(實施例2)
於35質量%的過氧化氫水溶液(三菱瓦斯化學股份公司製、製品名：UELM35)中添加硫酸鉀鋁・12水(和光純藥工業股份公司製、試藥特級)，除了使添加後之35質量%過氧化氫水溶液中的鋁含量成為10μg/kg之外，其餘係與實施例1同樣地操作，得到含有過氧化氫5.5質量%、醋酸48.9質量%、過醋酸13.1質量%、及1-羥基乙叉基-1,1-二膦酸0.8質量%之使用作為食品添加物之過醋酸組成物。所得的過醋酸組成物，自調合起21日後測定全過氧化物濃度，且計算安定度。(Example 2)
Potassium aluminum sulfate and 12 water (made by Wako Pure Chemical Industries, Ltd.) are added to a 35 mass% aqueous hydrogen peroxide solution (manufactured by Mitsubishi Gas Chemical Co., Ltd., product name: UELM35). Except that the aluminum content in the mass% hydrogen peroxide aqueous solution was 10 μg / kg, the rest was operated in the same manner as in Example 1 to obtain 5.5 mass% of hydrogen peroxide, 48.9 mass% of acetic acid, 13.1 mass% of peracetic acid, and 1- A peracetic acid composition used as a food additive in which 0.8% by mass of hydroxyethylidene-1,1-diphosphonic acid is used. The obtained peracetic acid composition was measured for the total peroxide concentration 21 days after the blending, and the stability was calculated.
(實施例3)
於35質量%的過氧化氫水溶液(三菱瓦斯化學股份公司製、製品名：UELM35)中添加硫酸鉀鋁・12水(和光純藥工業股份公司製、試藥特級)，除了使添加後之35質量%過氧化氫水溶液中的鋁含量成為100μg/kg之外，其餘係與實施例1同樣地操作，得到含有過氧化氫5.5質量%、醋酸48.8質量%、過醋酸13.5質量%、及1-羥基乙叉基-1,1-二膦酸0.8質量%之使用作為食品添加物之過醋酸組成物。所得的過醋酸組成物，自調合起21日後測定全過氧化物濃度，且計算安定度。(Example 3)
Potassium aluminum sulfate and 12 water (made by Wako Pure Chemical Industries, Ltd.) are added to a 35 mass% aqueous hydrogen peroxide solution (manufactured by Mitsubishi Gas Chemical Co., Ltd., product name: UELM35). Except that the aluminum content in the mass% hydrogen peroxide aqueous solution was 100 μg / kg, the rest of the system was operated in the same manner as in Example 1, and 5.5 mass% of hydrogen peroxide, 48.8 mass% of acetic acid, 13.5% by mass of peracetic acid, and A peracetic acid composition used as a food additive in which 0.8% by mass of hydroxyethylidene-1,1-diphosphonic acid is used. The obtained peracetic acid composition was measured for the total peroxide concentration 21 days after the blending, and the stability was calculated.
(實施例4)
除了未置入SUS304之試驗片，以及使用三菱瓦斯化學股份公司製之35質量%的過氧化氫水溶液(製品名：35%過氧化氫)來取代三菱瓦斯化學股份公司製之35質量%的過氧化氫水溶液(製品名：Diapower HP、含微量鋁)之外，其餘係與實施例1同樣地操作，得到含有過氧化氫5.5質量%、醋酸47.8質量%、過醋酸14.2質量%、及1-羥基乙叉基-1,1-二膦酸0.8質量%之使用作為食品添加物之過醋酸組成物。所得的過醋酸組成物，自調合起63日後測定全過氧化物濃度，且計算安定度。(Example 4)
In addition to the test piece without SUS304, and a 35 mass% hydrogen peroxide aqueous solution (product name: 35% hydrogen peroxide) manufactured by Mitsubishi Gas Chemical Co., Ltd. was used instead of the 35 mass% manufactured by Mitsubishi Gas Chemical Co., Ltd. Except for an aqueous hydrogen oxide solution (product name: Diapower HP, containing a trace amount of aluminum), the rest of the system was operated in the same manner as in Example 1 to obtain 5.5% by mass of hydrogen peroxide, 47.8% by mass of acetic acid, 14.2% by mass of peracetic acid, and 1- A peracetic acid composition used as a food additive in which 0.8% by mass of hydroxyethylidene-1,1-diphosphonic acid is used. The obtained peracetic acid composition was measured for the total peroxide concentration 63 days after the blending, and the stability was calculated.
(實施例5)
除了未置入SUS304之試驗片，以及使用三菱瓦斯化學股份公司製之35質量%的過氧化氫水溶液(製品名：35%過氧化氫)來取代三菱瓦斯化學股份公司製之35質量%的過氧化氫水溶液(製品名：Diapower HP、含微量鋁)、使用CHELEST股份公司製之1-羥基乙叉基-1,1-二膦酸(製品名：PH-210)來取代Italmatch Japan股份公司製之1-羥基乙叉基-1,1-二膦酸(製品名：Dequest 2010)之外，其餘係與實施例1同樣地操作，獲得含有過氧化氫5.5質量%、醋酸48.0質量%、過醋酸14.0質量%、及1-羥基乙叉基-1,1-二膦酸0.8質量%之使用作為食品添加物之過醋酸組成物。所得的過醋酸組成物，自調合起63日後測定全過氧化物濃度，且計算安定度。(Example 5)
In addition to the test piece without SUS304, and a 35 mass% hydrogen peroxide aqueous solution (product name: 35% hydrogen peroxide) manufactured by Mitsubishi Gas Chemical Co., Ltd. was used instead of the 35 mass% manufactured by Mitsubishi Gas Chemical Co., Ltd. Aqueous hydrogen oxide solution (product name: Diapower HP, containing trace aluminum), 1-hydroxyethylidene-1,1-diphosphonic acid (product name: PH-210) manufactured by CHELEST AG was used instead of Italmatch Japan Corporation Except for 1-hydroxyethylidene-1,1-diphosphonic acid (product name: Dequest 2010), the rest were operated in the same manner as in Example 1 to obtain 5.5 mass% of hydrogen peroxide, 48.0 mass% of acetic acid, and 14.0 mass% of acetic acid and 0.8 mass% of 1-hydroxyethylidene-1,1-diphosphonic acid are used as a peracetic acid composition as a food additive. The obtained peracetic acid composition was measured for the total peroxide concentration 63 days after the blending, and the stability was calculated.
(實施例6)
將純水3.4g與60質量%的1-羥基乙叉基-1,1-二膦酸(Italmatch Japan股份公司製、製品名：Dequest 2010)0.6g、冰醋酸26.6g(昭和電工股份公司製、製品名：99%純良醋酸)、35質量%的過氧化氫水溶液(三菱瓦斯化學股份公司製、製品名：35%過氧化氫)19.4g於聚乙烯容器內混合。調合時的全過氧化物濃度為13.7%。混合後，於25℃靜置10日，獲得含有過氧化氫7.4質量%、醋酸42.3質量%、過醋酸13.7質量%、及1-羥基乙叉基-1,1-二膦酸0.8質量%之使用作為食品添加物之過醋酸組成物。所得的過醋酸組成物，自調合起35日後測定全過氧化物濃度，且計算安定度。(Example 6)
3.4 g of pure water and 60% by mass of 1-hydroxyethylidene-1,1-diphosphonic acid (Italmatch Japan Co., Ltd., product name: Dequest 2010) 0.6 g and 26.6 g of glacial acetic acid (manufactured by Showa Denko Corporation) Product name: 99% pure acetic acid), 19.5% of a 35 mass% hydrogen peroxide solution (manufactured by Mitsubishi Gas Chemical Co., Ltd., product name: 35% hydrogen peroxide) are mixed in a polyethylene container. The total peroxide concentration during blending was 13.7%. After mixing, it was left to stand at 25 ° C for 10 days to obtain 7.4% by mass of hydrogen peroxide, 42.3% by mass of acetic acid, 13.7% by mass of peracetic acid, and 0.8% by mass of 1-hydroxyethylidene-1,1-diphosphonic acid. Peracetic acid composition used as a food additive. The obtained peracetic acid composition was measured for a total peroxide concentration 35 days after the blending, and the stability was calculated.
(實施例7)
除了使用35質量%的過氧化氫水溶液(三菱瓦斯化學股份公司製、製品名：Diapower HP、含微量鋁)來取代35質量%的過氧化氫水溶液(三菱瓦斯化學股份公司製、製品名：35%過氧化氫)之外，其餘係與實施例6同樣地操作，獲得含有過氧化氫7.5質量%、醋酸42.1質量%、過醋酸14.1質量%、及1-羥基乙叉基-1,1-二膦酸0.8質量%之使用作為食品添加物之過醋酸組成物。所得的過醋酸組成物，自調合起35日後測定全過氧化物濃度，且計算安定度。(Example 7)
Instead of using a 35 mass% aqueous hydrogen peroxide solution (manufactured by Mitsubishi Gas Chemical Co., Ltd., product name: Diapower HP, containing trace aluminum), instead of a 35 mass% aqueous hydrogen peroxide solution (manufactured by Mitsubishi Gas Chemical Co., Ltd., product name: 35) Except for hydrogen peroxide), the rest of the system was operated in the same manner as in Example 6 to obtain 7.5% by mass of hydrogen peroxide, 42.1% by mass of acetic acid, 14.1% by mass of peracetic acid, and 1-hydroxyethylidene-1,1- 0.8 mass% of bisphosphonic acid is used as a peracetic acid composition as a food additive. The obtained peracetic acid composition was measured for a total peroxide concentration 35 days after the blending, and the stability was calculated.
(實施例8)
除了於35質量%的過氧化氫水溶液(三菱瓦斯化學股份公司製、製品名：35%過氧化氫)中添加鐵標準液(和光純藥工業股份公司製、Fe1000)、磷酸二氫鈉二水合物(和光純藥工業股份公司製、試藥特級)，並使添加後之35質量%的過氧化氫水溶液中的鐵含量成為100μg/kg、使PO4 3-
含量成為52.9mg/kg之外，其餘係與實施例6同樣地操作，獲得含有過氧化氫7.3質量%、醋酸42.2質量%、過醋酸13.9質量%、及1-羥基乙叉基-1,1-二膦酸0.8質量%之使用作為食品添加物之過醋酸組成物。所得的過醋酸組成物，自調合起35日後測定全過氧化物濃度，且計算安定度。(Example 8)
In addition to a 35% by mass aqueous hydrogen peroxide solution (manufactured by Mitsubishi Gas Chemical Co., Ltd., product name: 35% hydrogen peroxide), an iron standard solution (manufactured by Wako Pure Chemical Industries, Ltd., Fe1000), and sodium dihydrogen phosphate dihydrate were added. Material (manufactured by Wako Pure Chemical Industries, Ltd., special reagent), and the iron content in the 35% by mass hydrogen peroxide aqueous solution after addition should be 100 μg / kg, and the PO 4 3- content should be in addition to 52.9 mg / kg The rest of the system was operated in the same manner as in Example 6, and 7.3% by mass of hydrogen peroxide, 42.2% by mass of acetic acid, 13.9% by mass of peracetic acid, and 0.8% by mass of 1-hydroxyethylidene-1,1-diphosphonic acid were obtained. Peracetic acid composition used as a food additive. The obtained peracetic acid composition was measured for a total peroxide concentration 35 days after the blending, and the stability was calculated.
(實施例9)
除了於35質量%的過氧化氫水溶液(三菱瓦斯化學股份公司製、製品名：35%過氧化氫)中添加鐵標準液(和光純藥工業股份公司製、Fe1000)、磷酸二氫鈉二水合物(和光純藥工業股份公司製、試藥特級)，並使添加後之35質量%的過氧化氫水溶液中的鐵含量成為510μg/kg、使PO4 3-
含量成為52.9mg/kg之外，其餘係與實施例6同樣地操作，獲得含有過氧化氫7.3質量%、醋酸42.4質量%、過醋酸13.7質量%、及1-羥基乙叉基-1,1-二膦酸0.8質量%之使用作為食品添加物之過醋酸組成物。所得的過醋酸組成物，自調合起35日後測定全過氧化物濃度，且計算安定度。(Example 9)
In addition to a 35% by mass aqueous hydrogen peroxide solution (manufactured by Mitsubishi Gas Chemical Co., Ltd., product name: 35% hydrogen peroxide), an iron standard solution (manufactured by Wako Pure Chemical Industries, Ltd., Fe1000), and sodium dihydrogen phosphate dihydrate were added. Material (manufactured by Wako Pure Chemical Industries, Ltd., special reagent), and the iron content in the 35% by mass hydrogen peroxide aqueous solution after addition was 510 μg / kg, and the PO 4 3- content was 52.9 mg / kg. The rest of the system was operated in the same manner as in Example 6 to obtain 7.3% by mass of hydrogen peroxide, 42.4% by mass of acetic acid, 13.7% by mass of peracetic acid, and 0.8% by mass of 1-hydroxyethylidene-1,1-diphosphonic acid. Peracetic acid composition used as a food additive. The obtained peracetic acid composition was measured for a total peroxide concentration 35 days after the blending, and the stability was calculated.
(實施例10)
將純水55.0g與60質量%的1-羥基乙叉基-1,1-二膦酸(Italmatch Japan股份公司製、製品名：Dequest 2010) 12.8g、冰醋酸651.0g(昭和電工股份公司製、製品名：99%純良醋酸)、35質量%的過氧化氫水溶液(三菱瓦斯化學股份公司製、製品名：35%過氧化氫)381.1g在聚乙烯容器內混合之後，於25℃靜置10日，獲得含有過氧化氫5.8質量%、醋酸47.7質量%、過醋酸14.5質量%、及1-羥基乙叉基-1,1-二膦酸0.7質量%之使用作為食品添加物之過醋酸組成物。平衡常數為2.4。將所得的過醋酸組成物以純水稀釋1.2倍，於25℃靜置10日，獲得含有過氧化氫6.0質量%、醋酸42.4質量%、過醋酸9.4質量%、及1-羥基乙叉基-1,1-二膦酸0.6質量%之使用作為食品添加物之過醋酸組成物。就所得的過醋酸組成物算出平衡常數，並測定引火點。(Example 10)
55.0 g of pure water and 60% by mass of 1-hydroxyethylidene-1,1-diphosphonic acid (Italmatch Japan Co., Ltd., product name: Dequest 2010) 12.8 g, 651.0 g of glacial acetic acid (manufactured by Showa Denko Corporation) Product name: 99% pure acetic acid), 35 mass% hydrogen peroxide solution (manufactured by Mitsubishi Gas Chemical Co., Ltd., product name: 35% hydrogen peroxide) 381.1 g are mixed in a polyethylene container, and then left to stand at 25 ° C On the 10th, peracetic acid containing 5.8% by mass of hydrogen peroxide, 47.7% by mass of acetic acid, 14.5% by mass of peracetic acid, and 0.7% by mass of 1-hydroxyethylidene-1,1-diphosphonic acid was obtained.组合 物。 Composition. The equilibrium constant is 2.4. The obtained peracetic acid composition was diluted 1.2 times with pure water, and left to stand at 25 ° C for 10 days to obtain 6.0 mass% of hydrogen peroxide, 42.4 mass% of acetic acid, 9.4 mass% of peracetic acid, and 1-hydroxyethylidene- 0.6 mass% of 1,1-bisphosphonic acid is used as a peracetic acid composition as a food additive. An equilibrium constant was calculated for the obtained peracetic acid composition, and the ignition point was measured.
(實施例11)
除了將所得的過醋酸組成物以純水稀釋1.3倍之外，其餘係與實施例10同樣地操作，獲得含有過氧化氫6.0質量%、醋酸39.9質量%、過醋酸7.9質量%、及1-羥基乙叉基-1,1-二膦酸0.5質量%之使用作為食品添加物之過醋酸組成物。就所得的過醋酸組成物算出平衡常數，並測定引火點。(Example 11)
Except that the obtained peracetic acid composition was diluted 1.3 times with pure water, the rest of the system was operated in the same manner as in Example 10 to obtain 6.0% by mass of hydrogen peroxide, 39.9% by mass of acetic acid, 7.9% by mass of peracetic acid, and 1- 0.5% by mass of hydroxyethylidene-1,1-diphosphonic acid is used as a peracetic acid composition as a food additive. An equilibrium constant was calculated for the obtained peracetic acid composition, and the ignition point was measured.
(實施例12)
除了將所得的過醋酸組成物以純水稀釋1.4倍之外，其餘係與實施例10同樣地操作，獲得含有過氧化氫5.9質量%、醋酸37.7質量%、過醋酸6.2質量%、及1-羥基乙叉基-1,1-二膦酸0.5質量%之使用作為食品添加物之過醋酸組成物。就所得的過醋酸組成物算出平衡常數，並測定引火點。(Example 12)
Except that the obtained peracetic acid composition was diluted 1.4 times with pure water, the rest of the system was operated in the same manner as in Example 10 to obtain 5.9% by mass of hydrogen peroxide, 37.7% by mass of acetic acid, 6.2% by mass of peracetic acid, and 1- 0.5% by mass of hydroxyethylidene-1,1-diphosphonic acid is used as a peracetic acid composition as a food additive. An equilibrium constant was calculated for the obtained peracetic acid composition, and the ignition point was measured.
(比較例1)
除了使用35質量%的過氧化氫水溶液(三菱瓦斯化學股份公司製、製品名：UELM35)來取代35質量%的過氧化氫水溶液(三菱瓦斯化學股份公司製、製品名：Diapower HP、含微量鋁)之外，其餘係與實施例1同樣地操作，獲得含有過氧化氫5.5質量%、醋酸48.7質量%、過醋酸13.5質量%、及1-羥基乙叉基-1,1-二膦酸0.8質量%之使用作為食品添加物之過醋酸組成物。所得的過醋酸組成物，自調合起21日後測定全過氧化物濃度，且計算安定度。(Comparative example 1)
In addition to using a 35 mass% hydrogen peroxide solution (manufactured by Mitsubishi Gas Chemical Co., Ltd., product name: UELM35) instead of a 35 mass% hydrogen peroxide solution (manufactured by Mitsubishi Gas Chemical Co., Ltd., product name: Diapower HP, containing trace aluminum The rest of the system was operated in the same manner as in Example 1 to obtain 5.5% by mass of hydrogen peroxide, 48.7% by mass of acetic acid, 13.5% by mass of peracetic acid, and 0.8% of 1-hydroxyethylidene-1,1-diphosphonic acid. Percent by mass is used as a peracetic acid composition as a food additive. The obtained peracetic acid composition was measured for the total peroxide concentration 21 days after the blending, and the stability was calculated.
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