JP5753752B2 - Method for producing oil and fat composition - Google Patents
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- JP5753752B2 JP5753752B2 JP2011190755A JP2011190755A JP5753752B2 JP 5753752 B2 JP5753752 B2 JP 5753752B2 JP 2011190755 A JP2011190755 A JP 2011190755A JP 2011190755 A JP2011190755 A JP 2011190755A JP 5753752 B2 JP5753752 B2 JP 5753752B2
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- 238000002955 isolation Methods 0.000 description 3
- VLKZOEOYAKHREP-UHFFFAOYSA-N n-Hexane Chemical compound CCCCCC VLKZOEOYAKHREP-UHFFFAOYSA-N 0.000 description 3
- 235000012424 soybean oil Nutrition 0.000 description 3
- 239000003549 soybean oil Substances 0.000 description 3
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- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 3
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 2
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 description 2
- 108010048733 Lipozyme Proteins 0.000 description 2
- 235000019482 Palm oil Nutrition 0.000 description 2
- 235000002597 Solanum melongena Nutrition 0.000 description 2
- 235000019486 Sunflower oil Nutrition 0.000 description 2
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- 229910052783 alkali metal Inorganic materials 0.000 description 2
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- 238000004458 analytical method Methods 0.000 description 2
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- SWQJXJOGLNCZEY-UHFFFAOYSA-N helium atom Chemical compound [He] SWQJXJOGLNCZEY-UHFFFAOYSA-N 0.000 description 2
- FCCDDURTIIUXBY-UHFFFAOYSA-N lipoamide Chemical compound NC(=O)CCCCC1CCSS1 FCCDDURTIIUXBY-UHFFFAOYSA-N 0.000 description 2
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- 235000011803 sesame oil Nutrition 0.000 description 2
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- 239000002600 sunflower oil Substances 0.000 description 2
- 150000004670 unsaturated fatty acids Chemical class 0.000 description 2
- 235000021122 unsaturated fatty acids Nutrition 0.000 description 2
- QHZLMUACJMDIAE-SFHVURJKSA-N 1-Monopalmitin Natural products CCCCCCCCCCCCCCCC(=O)OC[C@@H](O)CO QHZLMUACJMDIAE-SFHVURJKSA-N 0.000 description 1
- 108090000790 Enzymes Proteins 0.000 description 1
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- 241000287828 Gallus gallus Species 0.000 description 1
- UXDDRFCJKNROTO-UHFFFAOYSA-N Glycerol 1,2-diacetate Chemical compound CC(=O)OCC(CO)OC(C)=O UXDDRFCJKNROTO-UHFFFAOYSA-N 0.000 description 1
- 235000019487 Hazelnut oil Nutrition 0.000 description 1
- 235000018330 Macadamia integrifolia Nutrition 0.000 description 1
- 240000000912 Macadamia tetraphylla Species 0.000 description 1
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- 241001465754 Metazoa Species 0.000 description 1
- 240000007594 Oryza sativa Species 0.000 description 1
- 235000007164 Oryza sativa Nutrition 0.000 description 1
- CBENFWSGALASAD-UHFFFAOYSA-N Ozone Chemical compound [O-][O+]=O CBENFWSGALASAD-UHFFFAOYSA-N 0.000 description 1
- 235000019483 Peanut oil Nutrition 0.000 description 1
- 235000019498 Walnut oil Nutrition 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 239000003570 air Substances 0.000 description 1
- 229910052784 alkaline earth metal Inorganic materials 0.000 description 1
- 150000001342 alkaline earth metals Chemical class 0.000 description 1
- 150000004703 alkoxides Chemical class 0.000 description 1
- 239000000956 alloy Substances 0.000 description 1
- 229910045601 alloy Inorganic materials 0.000 description 1
- 229910052786 argon Inorganic materials 0.000 description 1
- 235000021302 avocado oil Nutrition 0.000 description 1
- 239000008163 avocado oil Substances 0.000 description 1
- 235000015278 beef Nutrition 0.000 description 1
- 230000008901 benefit Effects 0.000 description 1
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- 239000000828 canola oil Substances 0.000 description 1
- 235000019519 canola oil Nutrition 0.000 description 1
- 239000001569 carbon dioxide Substances 0.000 description 1
- 229910002092 carbon dioxide Inorganic materials 0.000 description 1
- UBAZGMLMVVQSCD-UHFFFAOYSA-N carbon dioxide;molecular oxygen Chemical compound O=O.O=C=O UBAZGMLMVVQSCD-UHFFFAOYSA-N 0.000 description 1
- 239000012159 carrier gas Substances 0.000 description 1
- 238000005119 centrifugation Methods 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 239000000306 component Substances 0.000 description 1
- 235000005687 corn oil Nutrition 0.000 description 1
- 239000002285 corn oil Substances 0.000 description 1
- 235000012343 cottonseed oil Nutrition 0.000 description 1
- 239000002385 cottonseed oil Substances 0.000 description 1
- 230000006866 deterioration Effects 0.000 description 1
- 229910001873 dinitrogen Inorganic materials 0.000 description 1
- 238000004090 dissolution Methods 0.000 description 1
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- 238000006911 enzymatic reaction Methods 0.000 description 1
- TVQGDYNRXLTQAP-UHFFFAOYSA-N ethyl heptanoate Chemical compound CCCCCCC(=O)OCC TVQGDYNRXLTQAP-UHFFFAOYSA-N 0.000 description 1
- 238000001914 filtration Methods 0.000 description 1
- 235000021323 fish oil Nutrition 0.000 description 1
- 235000013305 food Nutrition 0.000 description 1
- 239000011521 glass Substances 0.000 description 1
- GFAZGHREJPXDMH-UHFFFAOYSA-N glyceryl dipalmitate Natural products CCCCCCCCCCCCCCCC(=O)OCC(O)COC(=O)CCCCCCCCCCCCCCC GFAZGHREJPXDMH-UHFFFAOYSA-N 0.000 description 1
- 239000010468 hazelnut oil Substances 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 125000004435 hydrogen atom Chemical class [H]* 0.000 description 1
- 238000005984 hydrogenation reaction Methods 0.000 description 1
- 230000003301 hydrolyzing effect Effects 0.000 description 1
- 150000004679 hydroxides Chemical class 0.000 description 1
- 239000011261 inert gas Substances 0.000 description 1
- 238000000691 measurement method Methods 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 238000000199 molecular distillation Methods 0.000 description 1
- 239000010466 nut oil Substances 0.000 description 1
- 235000014593 oils and fats Nutrition 0.000 description 1
- ZQPPMHVWECSIRJ-KTKRTIGZSA-N oleic acid group Chemical group C(CCCCCCC\C=C/CCCCCCCC)(=O)O ZQPPMHVWECSIRJ-KTKRTIGZSA-N 0.000 description 1
- 235000008390 olive oil Nutrition 0.000 description 1
- 239000004006 olive oil Substances 0.000 description 1
- 239000000312 peanut oil Substances 0.000 description 1
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- 238000010008 shearing Methods 0.000 description 1
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- 239000003760 tallow Substances 0.000 description 1
- 238000010998 test method Methods 0.000 description 1
- 238000005809 transesterification reaction Methods 0.000 description 1
- 238000002834 transmittance Methods 0.000 description 1
- 235000015112 vegetable and seed oil Nutrition 0.000 description 1
- 239000008158 vegetable oil Substances 0.000 description 1
- 239000008170 walnut oil Substances 0.000 description 1
Landscapes
- Edible Oils And Fats (AREA)
- Fats And Perfumes (AREA)
Description
本発明は、油脂組成物の製造方法、並びに油脂組成物の固液分別法に関する。 The present invention relates to a method for producing an oil and fat composition and a method for solid-liquid fractionation of the oil and fat composition.
一般に、菜種油や大豆油等の油脂は常温で液状であるが、寒冷地や冷蔵庫等の低温下におかれると結晶が析出して白濁することがある。とりわけ、脂肪酸組成が同じであってもジアシルグリセロールはトリアシルグリセロールに比べて融点が高いため、低温下で結晶化し易いという傾向がある。 In general, fats and oils such as rapeseed oil and soybean oil are liquid at room temperature, but crystals may precipitate and become cloudy when placed under a low temperature such as a cold district or a refrigerator. In particular, even if the fatty acid composition is the same, diacylglycerol has a higher melting point than triacylglycerol, and thus tends to be easily crystallized at a low temperature.
油脂の結晶化を抑制する方法として、ウインタリングによって予め高融点成分を除去する方法が知られている。また、ジアシルグリセロールを高濃度に含む油脂に対しては、ウインタリングの際に分別助剤として乳化剤を添加し、析出した結晶を固液分別する方法が報告されている(特許文献1)。 As a method for suppressing crystallization of fats and oils, a method of previously removing a high melting point component by wintering is known. In addition, for fats and oils containing diacylglycerol at a high concentration, a method has been reported in which an emulsifier is added as a separation aid during wintering and the precipitated crystals are separated into solid and liquid (Patent Document 1).
ウインタリングは、結晶を生成させる晶析工程と結晶を濾別する分別工程とからなるが、油脂の組成によって濾別が困難な場合がある。また、特許文献1のように乳化剤を添加する方法は、高融点成分に乳化剤が濃縮されるため油脂の風味や物性に影響を与える懸念がある。さらに、乳化剤は、諸外国において使用が制限される場合がある。
本発明は、斯かる実情に鑑み、低温での結晶化が抑制された油脂組成物を製造する新たな方法を提供しようとするものである。
Wintering consists of a crystallization step for producing crystals and a fractionation step for separating the crystals, but it may be difficult to separate by the composition of the oil or fat. Moreover, since the emulsifier is concentrated in the high melting point component, the method of adding an emulsifier as in Patent Document 1 may affect the flavor and physical properties of the fats and oils. Furthermore, the use of emulsifiers may be restricted in other countries.
In view of such circumstances, the present invention intends to provide a new method for producing an oil and fat composition in which crystallization at low temperature is suppressed.
本発明者らは、上記課題に鑑み鋭意検討したところ、油脂組成物を冷却した状態において、気泡を接触させると、微細な結晶が当該気泡と共に浮上し、容易に分離できること、斯かる工程を経た油脂は低温下において結晶の析出が抑えられ、低温で結晶が析出しにくくなることを見出した。 The present inventors diligently studied in view of the above problems, and when the oil and fat composition was cooled, when the bubbles were brought into contact with each other, fine crystals floated along with the bubbles and could be easily separated. It has been found that the fats and oils suppress the precipitation of crystals at low temperatures and are difficult to precipitate at low temperatures.
すなわち、本発明は、次の工程(1)、(2)及び(3):
(1)油脂組成物を当該油脂組成物の曇点+0〜+10℃の範囲内に冷却する工程、
(2)冷却した油脂組成物に気泡を接触させる工程、
(3)前記工程により形成した泡沫部を液体部より分離する工程、
を含む、精製油脂組成物の製造方法を提供するものである。
また、本発明は、次の工程(1)、(2)及び(3):
(1)油脂組成物を当該油脂組成物の曇点+0〜+10℃の範囲内に冷却する工程、
(2)冷却した油脂組成物に気泡を接触させる工程、
(3)前記工程により形成した泡沫部と液体部とを分離する工程、
を含む、油脂組成物の固液分別法を提供するものである。
That is, the present invention includes the following steps (1), (2) and (3):
(1) a step of cooling the oil / fat composition within the cloud point +0 to + 10 ° C. of the oil / fat composition;
(2) a step of bringing bubbles into contact with the cooled oil and fat composition;
(3) The process of isolate | separating the foam part formed by the said process from a liquid part,
The manufacturing method of the refined fats and oils composition containing this is provided.
The present invention also includes the following steps (1), (2) and (3):
(1) a step of cooling the oil / fat composition within the cloud point +0 to + 10 ° C. of the oil / fat composition;
(2) a step of bringing bubbles into contact with the cooled oil and fat composition;
(3) The process of isolate | separating the foam part and liquid part which were formed by the said process,
The solid-liquid fractionation method of the oil-fat composition containing this is provided.
本発明によれば、油脂の高融点成分を容易に効率的に分別でき、低温での結晶化が抑制された油脂組成物を製造することができる。また、本発明の方法は、乳化剤の使用を低減、又は回避することができ、さらに分別設備の簡略化や油脂組成物の低コスト化も期待できる。 ADVANTAGE OF THE INVENTION According to this invention, the high melting point component of fats and oils can be fractionated easily and efficiently, and the fat and oil composition by which crystallization at low temperature was suppressed can be manufactured. In addition, the method of the present invention can reduce or avoid the use of an emulsifier, and can be expected to simplify the separation equipment and reduce the cost of the oil and fat composition.
本発明の精製油脂組成物の製造方法、並びに油脂組成物の固液分別法では、(1)油脂組成物を当該油脂組成物の曇点+0〜+10℃の範囲内に冷却する工程、(2)冷却した油脂組成物に気泡を接触させる工程、及び(3)前記工程により形成した泡沫部を液体部より分離する工程を有する。 In the manufacturing method of the refined fat composition of the present invention and the solid-liquid fractionation method of the fat composition, (1) the step of cooling the fat composition within the cloud point +0 to + 10 ° C. of the fat composition, (2 A step of bringing bubbles into contact with the cooled oil and fat composition, and (3) a step of separating the foamed part formed by the above-mentioned process from the liquid part.
本明細書において油脂とは、モノアシルグリセロール、ジアシルグリセロール、及びトリアシルグリセロールのいずれか1種以上を含むものをいう。油脂としては、植物性油脂、動物性油脂のいずれでもよい。具体的な原料としては、菜種油(キャノーラ油)、ひまわり油、とうもろこし油、大豆油、あまに油、米油、紅花油、綿実油、パーム油、やし油、オリーブ油、ぶどう油、アボカド油、ごま油、落花生油、マカデミアナッツ油、ヘーゼルナッツ油、くるみ油、豚脂、牛脂、鶏油、バター油、魚油等を挙げることができる。またこれらの油脂を分別、混合したもの、水素添加や、エステル交換反応等により脂肪酸組成を調整したものも原料として利用できる。 In this specification, fats and oils refer to those containing any one or more of monoacylglycerol, diacylglycerol, and triacylglycerol. As fats and oils, any of vegetable oils and animal fats may be used. Specific raw materials include rapeseed oil (canola oil), sunflower oil, corn oil, soybean oil, sesame oil, rice oil, safflower oil, cottonseed oil, palm oil, palm oil, olive oil, grape oil, avocado oil, sesame oil Peanut oil, macadamia nut oil, hazelnut oil, walnut oil, lard, beef tallow, chicken oil, butter oil, fish oil and the like. In addition, those obtained by separating and mixing these oils and fats, those obtained by adjusting the fatty acid composition by hydrogenation, transesterification, or the like can be used as raw materials.
脂肪酸組成が同じであってもトリアシルグリセロールに比べ、ジアシルグリセロールは低温下で結晶を析出し易い傾向がある。したがって、本発明の製造方法、並びに固液分別法は、ジアシルグリセロールを高含有する油脂組成物に適用するのが好ましい。
油脂組成物中のジアシルグリセロールの含有量は、体脂肪燃焼作用等の生理作用を効果的に発揮させるという点から20質量%(以下、単に「%」とする)以上が好ましく、40%以上がより好ましく、70%以上が更に好ましい。上限は特に規定されないが、99%以下が好ましく、98%以下がより好ましく、97%以下が更に好ましい。
Even if the fatty acid composition is the same, diacylglycerol tends to precipitate crystals at a lower temperature than triacylglycerol. Therefore, the production method and solid-liquid fractionation method of the present invention are preferably applied to an oil and fat composition containing a high amount of diacylglycerol.
The content of diacylglycerol in the oil and fat composition is preferably 20% by mass (hereinafter simply referred to as “%”) or more, preferably 40% or more from the viewpoint of effectively exerting physiological functions such as body fat burning action. More preferred is 70% or more. The upper limit is not particularly defined, but is preferably 99% or less, more preferably 98% or less, and still more preferably 97% or less.
油脂組成物中、トリアシルグリセロールの含有量は80%以下であるのが好ましく、更に1〜60%、殊更に2〜30%であるのが体脂肪燃焼作用等の生理作用向上の点から好ましい。また、モノアシルグリセロールの含有量は風味を良好とする点から、油脂組成物中に20%以下であるのが好ましく、更に0〜10%、更に0.1〜5%であるのが好ましい。 In the oil and fat composition, the content of triacylglycerol is preferably 80% or less, more preferably 1 to 60%, and particularly preferably 2 to 30% from the viewpoint of improving physiological action such as body fat burning action. . In addition, the content of monoacylglycerol is preferably 20% or less, more preferably 0 to 10%, and further preferably 0.1 to 5% in the oil or fat composition from the viewpoint of improving the flavor.
油脂組成物は、脂肪酸とグリセリンとのエステル化反応、油脂とグリセリンとのグリセロリシス反応等により得ることができる。これらの反応は、アルカリ金属又はその合金、アルカリ金属又はアルカリ土類金属の酸化物、水酸化物もしくは炭素数1〜3のアルコキシド等の化学触媒を用いる化学法とリパーゼ等の酵素を用いる酵素法に大別される。なかでも、触媒としてリパーゼ等を用いて酵素的に温和な条件で反応を行うのが風味等の点で優れており好ましい。 The oil / fat composition can be obtained by an esterification reaction between a fatty acid and glycerin, a glycerolysis reaction between an oil / fat and glycerin, or the like. These reactions include chemical methods using chemical catalysts such as alkali metals or alloys thereof, oxides or hydroxides of alkali metals or alkaline earth metals, or alkoxides having 1 to 3 carbon atoms, and enzymatic methods using enzymes such as lipases. It is divided roughly into. Of these, it is preferable in terms of flavor and the like that the reaction is performed enzymatically using lipase or the like as a catalyst under mild conditions.
本発明において、油脂組成物中の油脂を構成する脂肪酸は特に限定されず、飽和脂肪酸又は不飽和脂肪酸のいずれであってもよいが、本発明の効果が有効に発揮される点から、油脂を構成する脂肪酸中の2〜30%、更に4〜25%、殊更に6〜20%が飽和脂肪酸である油脂組成物に対して適用することが好ましい。飽和脂肪酸としては、炭素数12〜24、更に16〜22のものが好ましい。 In the present invention, the fatty acid constituting the fat in the fat composition is not particularly limited, and may be either a saturated fatty acid or an unsaturated fatty acid. It is preferably applied to an oil or fat composition in which 2 to 30%, further 4 to 25%, particularly 6 to 20% of the constituent fatty acid is a saturated fatty acid. The saturated fatty acid is preferably those having 12 to 24 carbon atoms, and more preferably 16 to 22 carbon atoms.
また、油脂を構成する脂肪酸のうち、不飽和脂肪酸の含有量は70〜98%であることが油脂組成物の外観、工業的生産性の点で好ましく、更に75〜96%、殊更に80〜94%であるのが好ましい。 Of the fatty acids constituting the fats and oils, the unsaturated fatty acid content is preferably 70 to 98% from the viewpoint of the appearance and industrial productivity of the fat and oil composition, more preferably 75 to 96%, and particularly 80 to 80%. 94% is preferred.
本発明においては、冷却工程に先立ち、油脂組成物をあらかじめ当該油脂組成物の曇点よりも10℃以上高い温度にしておくことが好ましい。かかる温度にすることで後に析出させる成分を一旦十分に溶解しておき、後の析出において、高融点成分を選択的に析出させることができる。当該温度は、油脂組成物の曇点に依存するが、例えば、25℃以上が好ましく、30℃以上がより好ましく、40℃以上が更に好ましく、50℃以上が殊更好ましい。 In the present invention, prior to the cooling step, it is preferable that the oil / fat composition is set at a temperature higher by 10 ° C. or more than the cloud point of the oil / fat composition in advance. By setting the temperature to such a temperature, components to be precipitated later can be sufficiently dissolved once, and in the subsequent precipitation, the high melting point component can be selectively precipitated. Although the said temperature depends on the cloud point of an oil-fat composition, for example, 25 degreeC or more is preferable, 30 degreeC or more is more preferable, 40 degreeC or more is further more preferable, 50 degreeC or more is especially preferable.
本発明においては、油脂組成物を当該油脂組成物の曇点+0〜+10℃の範囲内に冷却する。なお、「曇点+0〜+10℃」とは、「曇点以上、曇点+10℃以下」の温度範囲を示す表記である(以下同様)。斯かる温度範囲に冷却することにより油脂の高融点成分の中でも初期に析出する部分を微細結晶化して、気泡と共に泡沫部まで浮上させることができ、液体部から容易に分離することができる。
なお、本明細書において油脂組成物の曇点とは、透明な油脂が濁り始める温度であり、後記実施例記載の方法により測定することができる。
油脂組成物の冷却温度が油脂の曇点より低い場合、低温においても結晶析出が抑制された精製油脂組成物が得られるが、比較的融点の低い成分も析出してしまうために、得られる精製油脂組成物の歩留りが低下する。油脂組成物の冷却温度が油脂の曇点より10℃を超えて高い場合、結晶が析出しない、もしくは結晶析出量が不足するため、低温における結晶析出の抑制が不十分となる。
In this invention, an oil-fat composition is cooled in the range of the cloud point + 0 + 10 degreeC of the said oil-fat composition. “Cloud point +0 to + 10 ° C.” is a notation indicating a temperature range of “more than cloud point and less than cloud point + 10 ° C.” (the same applies hereinafter). By cooling to such a temperature range, the part which deposits in the initial stage among the high melting point components of fats and oils can be finely crystallized and floated to the foam part together with the bubbles, and can be easily separated from the liquid part.
In addition, in this specification, the cloud point of an oil-and-fat composition is the temperature at which a transparent oil-and-fat begins to become cloudy, and can be measured by the method described in Examples below.
When the cooling temperature of the oil / fat composition is lower than the cloud point of the oil / fat, a purified oil / fat composition in which crystal precipitation is suppressed even at a low temperature is obtained, but a component having a relatively low melting point is also precipitated, resulting in the purification obtained. The yield of the oil / fat composition is reduced. When the cooling temperature of the oil / fat composition is higher than the cloud point of the oil / fat by more than 10 ° C., crystals do not precipitate or the amount of crystal precipitation is insufficient, so the suppression of crystal precipitation at low temperatures becomes insufficient.
かかる観点より、冷却温度は、油脂組成物の曇点+0〜+9℃が好ましく、更に+0.5〜+9℃、殊更に+1〜+7℃が好ましい。このような温度範囲に設定することにより、高融点成分の結晶をより効率よく気泡で同伴して泡沫部まで浮上させることができ、分離が容易になる。
冷却温度は曇点に依存するが、例えば、0〜24℃が好ましく、2〜22℃がより好ましく、4〜20℃が更に好ましく、6〜18℃が更に好ましく、8〜15℃が更に好ましい。
From this viewpoint, the cooling temperature is preferably a cloud point of the oil or fat composition +0 to + 9 ° C., more preferably +0.5 to + 9 ° C., and particularly preferably +1 to + 7 ° C. By setting to such a temperature range, the high melting point component crystal can be more efficiently accompanied by bubbles and floated to the foam part, and separation becomes easy.
Although cooling temperature depends on a cloud point, for example, 0 to 24 ° C is preferable, 2 to 22 ° C is more preferable, 4 to 20 ° C is further preferable, 6 to 18 ° C is further preferable, and 8 to 15 ° C is further preferable. .
冷却操作は、気泡接触槽のジャケット冷却や熱交換器等により行うことができる。 The cooling operation can be performed by jacket cooling of a bubble contact tank, a heat exchanger, or the like.
本発明では、上記冷却温度範囲に冷却した油脂組成物に気泡を接触させる工程を有する。気泡の接触工程は、油脂組成物を上記温度範囲に調整した後に開始してもよい。この場合は、油脂組成物の冷却速度は特に限定されない。
また、気泡の接触工程を上記温度範囲になる前の冷却工程中に開始してもよい。この場合は、油脂の曇点+0〜+10℃の範囲内までの冷却速度は、結晶を浮上分離し易くする点から、0.5〜30℃/h、更に1〜15℃/h、殊更に2〜10℃/hが好ましい。
In this invention, it has a process which makes a bubble contact the oil-fat composition cooled to the said cooling temperature range. You may start the bubble contact process, after adjusting an oil-fat composition to the said temperature range. In this case, the cooling rate of the oil and fat composition is not particularly limited.
Moreover, you may start the bubble contact process in the cooling process before becoming the said temperature range. In this case, the cooling rate of the fats and oils to the cloud point +0 to + 10 ° C. is 0.5 to 30 ° C./h, more preferably 1 to 15 ° C./h, especially from the viewpoint of facilitating the floating separation of the crystals. 2 to 10 ° C./h is preferable.
油脂組成物と気泡との接触は、気泡発生装置を有する気泡接触槽を用いて行うことができる。気泡発生装置は、気泡接触槽の下部に位置することが好ましい。また、気泡接触槽は、油脂組成物の温度調節のために、ジャケット構造であることが好ましい。また、気泡接触槽は、油脂組成物の液体部と泡沫部を分離するための空間を有することが好ましい。 The contact between the oil and fat composition and the bubbles can be performed using a bubble contact tank having a bubble generator. It is preferable that the bubble generating device is located in the lower part of the bubble contact tank. Moreover, it is preferable that a bubble contact tank is a jacket structure for temperature control of an oil-fat composition. Moreover, it is preferable that a bubble contact tank has the space for isolate | separating the liquid part and foam part of an oil-fat composition.
気泡発生装置としては、気泡をせん断により微細化する装置、油脂組成物中に加圧された気体を溶解させ脱圧により気泡を発生させる装置等を用いることができる。また、多孔質体に気体を流通させることにより気泡を発生することができるエアーストーンを用いることができる。 As the bubble generating device, a device that refines bubbles by shearing, a device that dissolves pressurized gas in the oil and fat composition and generates bubbles by depressurization, and the like can be used. Moreover, the air stone which can generate | occur | produce a bubble by distribute | circulating gas to a porous body can be used.
供給される気体の種類は、特に限定されず、空気、窒素、酸素、二酸化炭素、オゾン、水素、アルゴン、ヘリウム等が挙げられる。特に、油脂組成物の劣化抑制の点から窒素、二酸化炭素、ヘリウム等の不活性気体が好ましい。 The type of gas to be supplied is not particularly limited, and examples include air, nitrogen, oxygen, carbon dioxide, ozone, hydrogen, argon, and helium. In particular, an inert gas such as nitrogen, carbon dioxide, and helium is preferable from the viewpoint of suppressing deterioration of the oil and fat composition.
発生させる気泡の量は、気体の流量や溶解タンクの圧力、循環流量により調整することができ、泡沫部への液体部巻き込み抑制の点から油脂組成物1kgあたり1〜1000ml/min、更に2〜500ml/min、殊更4〜200ml/minが好ましい。 The amount of bubbles to be generated can be adjusted by the flow rate of gas, the pressure of the dissolution tank, and the circulation flow rate. From the viewpoint of suppressing the entrainment of the liquid part into the foam part, 1-1000 ml / min per 1 kg of the oil and fat composition, and 2 500 ml / min, especially 4 to 200 ml / min is preferred.
また、平均気泡径は、結晶を浮上分離し易くする点から1〜1000μm、更に10〜600μm、殊更20〜400μmが好ましい。平均気泡径は、実施例記載の測定方法にて求められるものである。 The average bubble diameter is preferably 1 to 1000 μm, more preferably 10 to 600 μm, and particularly preferably 20 to 400 μm from the viewpoint of facilitating the floating separation of crystals. The average cell diameter is determined by the measurement method described in the examples.
冷却した油脂組成物と気泡を接触させる工程の時間は、飽和脂肪酸を構成脂肪酸とする油脂を十分に分離除去する観点から、0.1〜48時間、更に0.3〜24時間、殊更に0.5〜12時間が好ましい。なお、ここでの時間は、油脂組成物が当該油脂組成物の曇点+0〜+10℃の温度範囲内にある時間の合計を意味する。 The time for the step of bringing the cooled oil and fat composition into contact with the bubbles is 0.1 to 48 hours, 0.3 to 24 hours, particularly 0 to 0, from the viewpoint of sufficiently separating and removing the fat and oil containing the saturated fatty acid as a constituent fatty acid. .5-12 hours are preferred. In addition, time here means the sum total of the time when an oil-fat composition exists in the temperature range of the cloud point + 0 + 10 degreeC of the said fat-and-oil composition.
気泡は、油脂組成物と接触した後、浮上し、液体部(液体油脂組成物)の上部に泡沫部を形成する。この泡沫部を液体部より分離することにより、精製油脂組成物を得ることができる。泡沫部の分離は、気泡接触槽より溢流、吸引等の方法で行うことができる。
油脂組成物に対する泡沫部の割合は、油脂組成物中の飽和脂肪酸濃度により決定されるが、析出した高融点成分を十分に除去する観点より、3〜45%、更に5〜40%、更に8〜30%、更に10〜25%が好ましい。
Bubbles float after contact with the oil / fat composition, and form a foam part on top of the liquid part (liquid oil / fat composition). By separating this foam part from the liquid part, a purified fat composition can be obtained. Separation of the foam portion can be performed by a method such as overflow or suction from the bubble contact tank.
Although the ratio of the foam part with respect to fats and oils composition is determined by the saturated fatty acid density | concentration in fats and oils composition, from a viewpoint of fully removing the high melting-point component which precipitated, 3-45%, Furthermore, 5-40%, Furthermore 8 -30%, more preferably 10-25%.
泡沫部は、例えば、静置分離、濾過、遠心分離等により、泡沫部分離固体部油脂組成物と泡沫部分離液体部油脂組成物に分別することができる。静置分離する場合は、固体部と液体部を十分に分離させる観点より、気泡分離塔内の温度に対し+0〜10℃、更に+0.5〜9℃、更に+1〜7℃の温度範囲内で、1〜72時間、更に2〜48時間、殊更3〜24時間行うのが好ましい。油脂組成物に対する泡沫部分離固体部油脂組成物の割合は、油脂組成物中の飽和脂肪酸濃度により決定されるが、析出した高融点成分を十分に分離する観点より、1.5〜35%、更に3〜25%、更に4〜20%、更に5〜15%が好ましい。回収した泡沫部分離液体部油脂組成物は、油脂組成物の一部として再利用してもよい。 A foam part can be fractionated into a foam part isolation | separation oil part fat composition and a foam part isolation | separation liquid part fat composition by stationary separation, filtration, centrifugation, etc., for example. In the case of stationary separation, from the viewpoint of sufficiently separating the solid part and the liquid part, the temperature is within the temperature range of +0 to 10 ° C., further +0.5 to 9 ° C., and further +1 to 7 ° C. with respect to the temperature in the bubble separation tower. And preferably 2 to 48 hours, more preferably 3 to 24 hours. The ratio of the foam part separation solid part fat composition to the fat composition is determined by the saturated fatty acid concentration in the fat composition, but from the viewpoint of sufficiently separating the precipitated high melting point component, 1.5 to 35%, Further, 3 to 25%, further 4 to 20%, and further 5 to 15% are preferable. You may reuse the collect | recovered foam part isolation | separation liquid part oil-fat composition as a part of oil-fat composition.
本発明の方法により、油脂組成物から高融点成分が分別除去され、低温における結晶化が抑制された精製油脂組成物が得られる。 By the method of the present invention, a high melting point component is separated and removed from the oil and fat composition, and a purified oil and fat composition in which crystallization at low temperature is suppressed is obtained.
油脂組成物からの精製油脂組成物の回収率(歩留まり)は、油脂組成物の高融点成分濃度に依存するが、50〜99%が好ましく、60〜98%がより好ましく、70〜97%が更に好ましく、75〜96%が更に好ましい。 The recovery rate (yield) of the purified fat composition from the fat composition depends on the high melting point component concentration of the fat composition, but is preferably 50 to 99%, more preferably 60 to 98%, and more preferably 70 to 97%. More preferred is 75 to 96%.
本発明の方法では、高融点成分として、飽和脂肪酸を構成脂肪酸とする油脂を好適に分別除去することができ、炭素数12〜24の飽和脂肪酸を構成脂肪酸とする油脂をより好適に分別除去することができる。
油脂組成物が、菜種油に由来するジアシルグリセロールを高含有する油脂組成物である場合、高融点成分としては、1,3−ジ飽和ジアシルグリセロールが好適に分別除去される。高融点成分としては、1,3−ジ飽和ジアシルグリセロールを指標として用いることができ、例えば1,3−ジパルミチンジアシルグリセロールを指標として好適に用いることができる。
In the method of the present invention, as a high melting point component, fats and oils having saturated fatty acids as constituent fatty acids can be suitably separated and removed, and fats and oils having saturated fatty acids having 12 to 24 carbon atoms as constituent fatty acids are more preferably separated and removed. be able to.
When the oil / fat composition is an oil / fat composition containing a high content of diacylglycerol derived from rapeseed oil, 1,3-disaturated diacylglycerol is suitably fractionated and removed as the high melting point component. As the high melting point component, 1,3-disaturated diacylglycerol can be used as an index, and for example, 1,3-dipalmitine diacylglycerol can be preferably used as an index.
油脂組成物が、菜種油に由来するジアシルグリセロールを高含有する油脂組成物である場合、精製油脂組成物中の1,3−ジパルミチンジアシルグリセロールの含有量は、油脂組成物中の1,3−ジパルミチンジアシルグリセロールの含有量よりも5%以上、更に10〜60%減少したものであるのが、低温状態での結晶化抑制の点から好ましい。 When the oil / fat composition is an oil / fat composition containing a high content of diacylglycerol derived from rapeseed oil, the content of 1,3-dipalmitine diacylglycerol in the purified oil / fat composition is 1,3-dipalglycerol in the oil / fat composition. It is preferable that the content of dipalmitin diacylglycerol is reduced by 5% or more and further by 10 to 60% from the viewpoint of suppressing crystallization in a low temperature state.
また、油脂組成物が、菜種油に由来するジアシルグリセロールを高含有する油脂組成物である場合、精製油脂組成物中の1,3−ジパルミチンジアシルグリセロールの含有量は、低温状態で結晶化抑制の点から0.09%以下、更に0.08%以下、殊更0.07%以下が好ましい。下限は特に規定されないが、工業的生産性の点から0.01%以上、更に0.02%以上、殊更0.03%以上が好ましい。 In addition, when the oil and fat composition is an oil and fat composition containing a high content of diacylglycerol derived from rapeseed oil, the content of 1,3-dipalmitin diacylglycerol in the refined oil and fat composition is low in crystallization at low temperatures. From this point, 0.09% or less, further 0.08% or less, and particularly 0.07% or less are preferable. The lower limit is not particularly defined, but is preferably 0.01% or more, more preferably 0.02% or more, and particularly preferably 0.03% or more from the viewpoint of industrial productivity.
精製油脂組成物中のジアシルグリセロールの含有量は、生理効果、油脂の工業的生産性の点から、20%以上が好ましく、40%以上がより好ましく、70%以上が更に好ましい。上限は特に規定されないが、99%以下が好ましく、98%以下がより好ましく、97%以下が更に好ましい。 The content of diacylglycerol in the refined fat composition is preferably 20% or more, more preferably 40% or more, and still more preferably 70% or more from the viewpoint of physiological effects and industrial productivity of the fat. The upper limit is not particularly defined, but is preferably 99% or less, more preferably 98% or less, and still more preferably 97% or less.
本発明の製造方法、並びに固液分別法により得られた精製油脂組成物は、一般の食用油脂と同様に使用でき、油脂を用いた各種飲食物に広範に適用することができる。 The refined fat composition obtained by the production method of the present invention and the solid-liquid fractionation method can be used in the same manner as general edible fats and oils, and can be widely applied to various foods and drinks using fats and oils.
〔分析方法〕
(i)油脂の構成脂肪酸組成
日本油化学会編「基準油脂分析試験法」中の「脂肪酸メチルエステルの調製法(2.4.1.−1996)」に従って脂肪酸メチルエステルを調製し、得られたサンプルを、American Oil Chemists' Society Official Method Ce 1f−96(GLC法)により測定した。
[Analysis method]
(I) Fatty Acid Composition of Fats and Oils Fatty acid methyl esters were prepared and obtained according to “Preparation Method of Fatty Acid Methyl Esters (2.4.1.-1996)” in “Standard Fat and Fat Analysis Test Method” edited by Japan Oil Chemists' Society. The samples were measured by American Oil Chemist's Society Official Method Ce 1-96 (GLC method).
(ii)油脂のグリセリド組成
油脂のグリセリド組成とともに、1,3−ジアシルグリセロール(1,3−DAG)、1,2−ジアシルグリセロール(1,2−DAG)及び高融点成分の1,3−ジパルミチンジアシルグリセロール(1,3−PP−DAG)、1−モノパルミチンモノアシルグリセロール(1−P−MAG)はガスクロマトグラフィー(GLC)に供して分析した。ガラス製サンプル瓶に、油脂サンプル約10mgとトリメチルシリル化剤(「シリル化剤TH」、関東化学製)0.5mLを加え、密栓し、70℃で15分間加熱した。これに水1.0mLとヘキサン1.5mLを加え、振とうした。静置後、上層をガスクロマトグラフィー(GLC)に供して分析した。
<GLC条件>
(条件)
装置:アジレント6890シリーズ(アジレントテクノジー社製)
インテグレーター:ケミステーションB 02.01 SR2(アジレントテクノジー社製)
カラム:DB−1ht、10m(アジレントテクノジー社製)
キャリアガス:1.0mL He/min
インジェクター:Split(1:50)、T=320℃
ディテクター:FID、T=350℃
オーブン温度:80℃から340℃まで1℃/分で昇温、340℃で15分間保持
(Ii) Glycerol composition of fat and oil Along with the glyceride composition of fat and oil, 1,3-diacylglycerol (1,3-DAG), 1,2-diacylglycerol (1,2-DAG) and 1,3-di of high melting point component Palmitic diacylglycerol (1,3-PP-DAG) and 1-monopalmitin monoacylglycerol (1-P-MAG) were subjected to gas chromatography (GLC) and analyzed. To a glass sample bottle, about 10 mg of an oil and fat sample and 0.5 mL of a trimethylsilylating agent (“silylating agent TH”, manufactured by Kanto Chemical) were added, sealed, and heated at 70 ° C. for 15 minutes. To this, 1.0 mL of water and 1.5 mL of hexane were added and shaken. After standing, the upper layer was analyzed by gas chromatography (GLC).
<GLC conditions>
(conditions)
Equipment: Agilent 6890 series (manufactured by Agilent Technologies)
Integrator: ChemStation B 02.01 SR2 (manufactured by Agilent Technologies)
Column: DB-1ht, 10 m (manufactured by Agilent Technologies)
Carrier gas: 1.0 mL He / min
Injector: Split (1:50), T = 320 ° C.
Detector: FID, T = 350 ° C
Oven temperature: raised from 80 ° C to 340 ° C at a rate of 1 ° C / min and held at 340 ° C for 15 minutes
(iii)油脂組成物の曇点の測定
試料をキャピラリー管に入れ、光の透過度を検出する方式のMETTLER FR900サーモシステム81HT(メトラー・トレド製)を用いて、0.5℃/分で冷却したときの結晶析出温度を測定した。
(Iii) Measurement of cloud point of oil / fat composition Cooling at 0.5 ° C./min using a METLER FR900 thermosystem 81HT (manufactured by METTLER TOLEDO), which is a method of detecting the light transmittance by putting a sample in a capillary tube. The crystal precipitation temperature was measured.
(iv)平均気泡径の測定
平均気泡径は、油脂組成物を充填した2mm幅のスリットに気泡を導入して、カメラにより直接撮影した画像から測定して求めた。
(Iv) Measurement of average bubble diameter The average bubble diameter was determined by measuring bubbles from a 2 mm wide slit filled with an oil and fat composition and measuring the image directly from a camera.
(v)泡沫部分離固体部油脂組成物の歩留まりの算出法
次式により、油脂組成物の歩留まりを算出した。
泡沫部分離固体部油脂組成物の重量/油脂組成物の重量×100 (%)
(V) Method for calculating yield of foam part-separated solid part fat composition The yield of the fat composition was calculated according to the following equation.
Foam part separated solid part oil / fat composition weight / fat composition / weight x 100 (%)
〔油脂組成物aの調製〕
菜種油を加水分解して得た脂肪酸870質量部と触媒として1,3位選択性固定化リパーゼ(Lipozyme RM IM:ノボルディスクインダストリー社製)50質量部とを混合し、グリセリン130質量部を添加してエステル化反応を行った。リパーゼ製剤を濾別した後、反応終了品を分子蒸留し、更に脱色、酸処理、水洗した後、245℃にて34分脱臭して油脂組成物aを得た。
[Preparation of oil and fat composition a]
870 parts by weight of fatty acid obtained by hydrolyzing rapeseed oil and 50 parts by weight of 1,3-position-selective immobilized lipase (Lipozyme RM IM: manufactured by Novoldisk Industries) as a catalyst were mixed, and 130 parts by weight of glycerin was added. The esterification reaction was performed. After the lipase preparation was filtered off, the reaction-finished product was subjected to molecular distillation, further decolorized, acid-treated and washed with water, and then deodorized at 245 ° C. for 34 minutes to obtain an oil and fat composition a.
〔油脂組成物bの調製〕
菜種油を大豆油に換えた他は油脂組成物aの調製と同じ操作を行い、油脂組成物bを得た。
[Preparation of oil and fat composition b]
The oil and fat composition b was obtained in the same manner as in the preparation of the oil and fat composition a except that the rapeseed oil was changed to soybean oil.
〔油脂組成物cの調製〕
高オレイン酸ヒマワリ油を828質量部と触媒として1,3位選択性固定化リパーゼ(Lipozyme RM IM:ノボルディスクインダストリー社製)100質量部と蒸留水20質量部を混合し、グリセリン172質量部を添加してグリセロリシス反応を行った。リパーゼ製剤を濾別した後、反応終了品を脱グリセリンして油脂組成物cを得た。
[Preparation of Oil and Fat Composition c]
828 parts by mass of high oleic sunflower oil and 1,3-position selective immobilized lipase (Lipozyme RM IM: NOVOLDIS INDUSTRY Co., Ltd.) 100 parts by mass and distilled water 20 parts by mass were mixed with 172 parts by mass of glycerin. The glycerolysis reaction was performed by addition. After the lipase preparation was filtered off, the reaction finished product was deglycerinized to obtain an oil and fat composition c.
表1に、油脂組成物a〜cの組成、及び曇点、並びに高融点成分名、油脂組成物a〜c中の高融点成分濃度、及びグリセリドの構成脂肪酸中の炭素数12〜24の飽和脂肪酸量を示した。 Table 1 shows composition of oil and fat compositions a to c, cloud point, and high melting point component name, high melting point component concentration in fat and oil compositions a to c, and saturation of 12 to 24 carbon atoms in constituent fatty acids of glycerides. The amount of fatty acid is shown.
試験例1
図1に示すジャケット冷却式の円筒状気泡接触槽(内径100mm×高さ1000mm、以下同じ)に油脂組成物aを6.0kg仕込み、50℃で完全溶解した。気泡発生放置(OM4−MDG−045、オーラテック製)と円筒状気泡接触槽の間を約120ml/minで循環させた。気泡発生放置の圧力を0.26MPaに調整し、円筒状気泡接触槽の直前で脱圧することで連続的に気泡を発生させながら、油脂組成物aを4℃/hで冷却し、13℃で10時間保持した。このときの平均気泡径は79μmであった。また、油脂組成物aの曇点+0〜+10℃の範囲内での油脂組成物と気泡の接触時間は11時間であった(表では「冷却温度範囲での気泡接触時間」と表記した。以下同じ。)。円筒状気泡接触槽の下部から100mm高い位置に取り付けたサンプリング口から精製油脂組成物を抜き出した。また、泡沫部はナスフラスコに抜き出し、15℃で12時間静置させて、分離した泡沫部分離液体部油脂組成物を分離して泡沫部分離固体部油脂組成物を得た。
Test example 1
6.0 kg of the oil and fat composition a was charged in a jacket-cooled cylindrical bubble contact tank (inner diameter 100 mm × height 1000 mm, the same applies hereinafter) shown in FIG. 1 and completely dissolved at 50 ° C. It was circulated at a rate of about 120 ml / min between the bubble generation standing (OM4-MDG-045, Auratec) and the cylindrical bubble contact tank. The oil and fat composition a was cooled at 4 ° C./h at 13 ° C. while adjusting the pressure for generating bubbles to 0.26 MPa and continuously generating bubbles by depressurizing immediately before the cylindrical bubble contact tank. Hold for 10 hours. The average bubble diameter at this time was 79 μm. In addition, the contact time between the oil and fat composition and the bubbles within the range of the cloud point +0 to + 10 ° C. of the oil and fat composition a was 11 hours (in the table, expressed as “bubble contact time in the cooling temperature range”. the same.). The refined fat composition was extracted from a sampling port attached at a position 100 mm higher from the lower part of the cylindrical bubble contact tank. Moreover, the foam part was extracted into an eggplant flask and allowed to stand at 15 ° C. for 12 hours to separate the separated foam part separated liquid part fat composition, thereby obtaining a foam part separated solid part fat composition.
試験例2
ジャケット冷却式の円筒状気泡接触槽に油脂組成物bを6.0kg仕込み、50℃で完全溶解した。気泡発生放置(OM4−MDG−045、オーラテック製)と円筒状気泡接触槽の間を約120ml/minで循環させた。気泡発生放置の圧力を0.26MPaに調整し、円筒状気泡接触槽の直前で脱圧することで連続的に気泡を発生させながら、油脂組成物bを4℃/hで冷却し、17℃で4時間保持した。油脂組成物bの曇点+0〜+10℃の範囲内での油脂組成物と気泡の接触時間は5.15時間であった。円筒状気泡接触槽の下部から100mm高い位置に取り付けたサンプリング口から精製油脂組成物を抜き出した。
Test example 2
In a jacket-cooled cylindrical bubble contact tank, 6.0 kg of the oil / fat composition b was charged and completely dissolved at 50 ° C. It was circulated at a rate of about 120 ml / min between the bubble generation standing (OM4-MDG-045, Auratec) and the cylindrical bubble contact tank. The oil and fat composition b was cooled at 4 ° C./h at 17 ° C. while adjusting the pressure for bubble generation to 0.26 MPa and continuously generating bubbles by releasing the pressure immediately before the cylindrical bubble contact tank. Hold for 4 hours. The contact time between the oil and fat composition and the bubbles in the range of cloud point +0 to + 10 ° C. of the oil and fat composition b was 5.15 hours. The refined fat composition was extracted from a sampling port attached at a position 100 mm higher from the lower part of the cylindrical bubble contact tank.
試験例3
ジャケット冷却式の円筒状気泡接触槽に油脂組成物cを6.0kg仕込み、50℃で完全溶解後、25℃に冷却した。気泡発生放置(OM4−MDG−045、オーラテック製)と円筒状気泡接触槽の間を約120ml/minで循環させた。気泡発生放置の圧力を0.26MPaに調整し、円筒状気泡接触槽の直前で脱圧することで連続的に気泡を発生させながら、油脂組成物cを1℃/hで15℃まで冷却した。油脂組成物cの曇点+0〜+10℃の範囲内での油脂組成物と気泡の接触時間は5.2時間であった。円筒状気泡接触槽の下部から100mm高い位置に取り付けたサンプリング口から精製油脂組成物を抜き出した。また、泡沫部はナスフラスコに抜き出し20℃で48時間静置させて、巻き込んだ泡沫部分離液体部油脂組成物を分離して泡沫部分離固体部油脂組成物を得た。
Test example 3
In a jacket-cooled cylindrical bubble contact tank, 6.0 kg of the oil / fat composition c was charged, completely dissolved at 50 ° C, and then cooled to 25 ° C. It was circulated at a rate of about 120 ml / min between the bubble generation standing (OM4-MDG-045, Auratec) and the cylindrical bubble contact tank. The oil-and-fat composition c was cooled to 15 ° C. at 1 ° C./h while continuously generating bubbles by adjusting the pressure for leaving the bubbles to 0.26 MPa and releasing the pressure immediately before the cylindrical bubble contact tank. The contact time between the oil and fat composition and the bubbles in the range of cloud point +0 to + 10 ° C. of the oil and fat composition c was 5.2 hours. The refined fat composition was extracted from a sampling port attached at a position 100 mm higher from the lower part of the cylindrical bubble contact tank. Moreover, the foam part was extracted into an eggplant flask and allowed to stand at 20 ° C. for 48 hours to separate the entrained foam part separated liquid part oil and fat composition to obtain a foam part separated solid part oil and fat composition.
試験例4
ジャケット冷却式の円筒状気泡接触槽に油脂組成物aを6.0kg仕込み、50℃で完全溶解した。円筒状気泡接触槽の底面にエアーストーン(25φ丸#180、いぶきエアストーン製)を3個取り付けた。エアーストーン1個あたり、窒素ガス約50ml/minを供給し、連続的に気泡を発生させながら、油脂組成物aを12℃/hで冷却し、10℃で10時間保持した。油脂組成物aの曇点+0〜+10℃の範囲内での油脂組成物と気泡の接触時間は10.58時間であった。このときの平均気泡径は725μmであった。円筒状気泡接触槽の下部から100mm高い位置に取り付けたサンプリング口から精製油脂組成物を抜き出した。
Test example 4
In a jacket-cooled cylindrical bubble contact tank, 6.0 kg of the oil composition a was charged and completely dissolved at 50 ° C. Three air stones (25φ round # 180, manufactured by Ibuki Air Stone) were attached to the bottom surface of the cylindrical bubble contact tank. Nitrogen gas was supplied at about 50 ml / min per air stone, and the oil and fat composition a was cooled at 12 ° C./h while continuously generating bubbles, and held at 10 ° C. for 10 hours. The contact time between the oil and fat composition and the bubbles in the range of cloud point +0 to + 10 ° C. of the oil and fat composition a was 10.58 hours. At this time, the average bubble diameter was 725 μm. The refined fat composition was extracted from a sampling port attached at a position 100 mm higher from the lower part of the cylindrical bubble contact tank.
表1に、各試験例の、泡沫部分離液体部油脂組成物の収率、泡沫部分離固体部油脂組成物の組成、高融点成分名、泡沫部分離固体部油脂組成物中の高融点成分の含有量、グリセリドの構成脂肪酸中の炭素数12〜24の飽和脂肪酸量、及び収率を示した。
また、精製油脂組成物の組成、曇点、高融点成分名、精製油脂組成物中の高融点成分の含有量、グリセリドの構成脂肪酸中の炭素数12〜24の飽和脂肪酸量、及び収率を示した。
Table 1 shows the yield of the foam-part separated liquid oil composition, the composition of the foam-separated solid oil composition, the high-melting-point component name, and the high-melting-point component in the foam-separated solid oil composition. Content, the amount of saturated fatty acid having 12 to 24 carbon atoms in the constituent fatty acid of glyceride, and the yield.
In addition, the composition of the refined fat and oil composition, cloud point, high melting point component name, content of the high melting point component in the refined fat and oil composition, the amount of saturated fatty acid having 12 to 24 carbon atoms in the constituent fatty acid of the glyceride, and the yield Indicated.
表1から明らかなように、本発明の方法によれば、油脂中のグリセリド組成、1,2−DAGと1,3−DAGの比率、飽和脂肪酸量はほとんど変化なく、高融点成分、特に1,3−PP、1−P等の結晶核となる成分を効率的に分別除去することができ、低温で結晶化が抑制された優れた精製油脂組成物を製造できることが確認された。 As is apparent from Table 1, according to the method of the present invention, the glyceride composition in fats and oils, the ratio of 1,2-DAG and 1,3-DAG, and the amount of saturated fatty acid hardly change, and the high melting point component, particularly 1 , 3-PP, 1-P, and other components that become crystal nuclei can be efficiently separated and removed, and it has been confirmed that an excellent refined oil and fat composition in which crystallization is suppressed at low temperatures can be produced.
Claims (5)
(1)油脂組成物を当該油脂組成物の曇点+0〜+10℃の範囲内に冷却する工程、
(2)冷却した油脂組成物に気泡を接触させる工程、
(3)前記工程により形成した泡沫部を液体部より分離する工程、
を含む、精製油脂組成物の製造方法。 Next steps (1), (2) and (3):
(1) a step of cooling the oil / fat composition within the cloud point +0 to + 10 ° C. of the oil / fat composition;
(2) a step of bringing bubbles into contact with the cooled oil and fat composition;
(3) The process of isolate | separating the foam part formed by the said process from a liquid part,
The manufacturing method of the refined fats and oils composition containing this.
(1)油脂組成物を当該油脂組成物の曇点+0〜+10℃の範囲内に冷却する工程、
(2)冷却した油脂組成物に気泡を接触させる工程、
(3)前記工程により形成した泡沫部と液体部とを分離する工程、
を含む、油脂組成物の固液分別法。 Next steps (1), (2) and (3):
(1) a step of cooling the oil / fat composition within the cloud point +0 to + 10 ° C. of the oil / fat composition;
(2) a step of bringing bubbles into contact with the cooled oil and fat composition;
(3) The process of isolate | separating the foam part and liquid part which were formed by the said process,
The solid-liquid fractionation method of fats and oils composition containing this.
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