JPH0413990B2 - - Google Patents
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- Publication number
- JPH0413990B2 JPH0413990B2 JP61116346A JP11634686A JPH0413990B2 JP H0413990 B2 JPH0413990 B2 JP H0413990B2 JP 61116346 A JP61116346 A JP 61116346A JP 11634686 A JP11634686 A JP 11634686A JP H0413990 B2 JPH0413990 B2 JP H0413990B2
- Authority
- JP
- Japan
- Prior art keywords
- membrane
- fruit juice
- permeation rate
- minutes
- recovery
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Expired - Lifetime
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- Non-Alcoholic Beverages (AREA)
- Separation Using Semi-Permeable Membranes (AREA)
Description
(産業上の利用分野)
果汁は、飲料用としてそのまゝの状態で多く消
費されているが、飲料の成分として、混合調製し
た状態で混濁を生じず、清澄状態を維持する果汁
の需要が、最近高まつている。本発明は上記特性
の清澄果汁を原料果汁から製造する方法を提供す
るものである。対象果汁は、柑橘類(温州,八朔
等)、ベリー類(いちご類)、プラム類(梅、桃
等)、林檎、葡萄、パイナツプル、等殆んどすべ
ての果汁を含む。
(従来技術)
懸濁しているパルプ分を遠心分離または超遠心
分離で除去したのち、溶解しているペクチン質
を、ペクチナーゼ等の酵素で分解する方法が実用
化されている。しかし、酵素反応を40〜60℃の高
温で数時間以上かけて行う結果、芳香を失うと同
時に特有の悪臭が加わつて果汁の品質劣化を避け
ることができず、更に使用する酵素が高価なた
め、清澄化のコストが嵩む欠点を有している。
これらの欠点を克服する方法として限外過膜
を用いて、ペクチン質を常温で別除去する方法
が試験されている。
(解決しようとする問題点)
果汁を限外過膜で処理する方法の問題点とし
て膜透過速度の急激な経時低下がある。このた
め、所定量の果汁を所定時間で処理するためには
大規模の膜装置が必要となり、この欠点のため
に、酵素法に取つて替る程の有利性をもちえなく
なる恐れがある。
本発明は、果汁をクロスフローにより膜処理す
る工程で簡単、安価な膜透過速度回復法を考案
し、これを周期的に施すことにより平均膜透過速
度を高く維持して、膜装置大規模化の欠点を克服
しようとするものである。
低下した膜透過速度の回復法として、界面活性
剤、酸、アルカリ、酸化剤、酵素、温湯等による
洗條が良く知られており、適切な選定をすると非
常に有効である。しかし、この方法は運転を終了
し、液を回収した後でないと実施することができ
ない。運転中に行いうる膜透過速度回復法として
は原液の流れ方向を反転したり、高速でフラツシ
ユしてフアウリング層を除去する方法、原液に気
泡を吹き込んでつくる気液界面や、原液に加えた
スポンジボール等の固体で擦り取る方法、透過液
を逆透過させて膜表面のフアウリング層を離脱さ
せる方法等がある。しかし、気泡や固体を加える
方法は管状膜モジユールでのみ可能であつて、空
間効率、エネルギー効率の良い中空糸膜モジユー
ルやスパイラルまたはプリーツモジユールには適
用することができない。透過液の一部を逆透過さ
せる方法は有効であるが、折角膜透過した液を原
液に戻す不利と、逆透過させるために透過液を加
圧するポンプを必要とする欠点がある。原液の流
れ方向を逆転したり、印加圧力を開放して高速で
フラツシユする方法は最も簡単であるが、効果の
点で劣る。
(問題点を解決するための手段)
本発明者等は鋭意研究の結果、簡単でしかも有
効な膜透過速度回復法を考察した。すなわち、透
過液取出口を一定時間閉鎖して、膜透過を停止さ
せた後、該閉鎖状態のままで背圧調整弁を開放し
て原液をフラツシユさせ、更に好ましくは上記一
連の操作に対し原液の流れ方向を反転させる操作
であり、かつ、この操作を30分を超えない間隔で
20秒以上、好ましくは1分以上続けることを特徴
とする膜透過速度回復法である。
(本発明の効果)
本発明の方法によれば、果汁処理で汚れた膜面
を簡単な操作によつて洗條することが出来、膜透
過速度が回復される。これを周期的に実施するこ
とにより、平均膜透過速度を長期間高く維持出来
るので膜面の汚れを予め見込んだ膜装置大規模化
の設備投資が軽減される。
(実施例)
以下実施例に則つて説明する。
比較例 1
温州みかんストレート果汁(糖度 ブリツクス
10.7°)50を空隙0.2mm×0.2mmの布で過した
のち、第1図の装置を用いてポンプ吐出量1.2
m3/h、モジユール出口圧1Kg/cm2の条件で中空
糸UF膜モジユールに供給して清澄果汁を製造し
た。モジユールはダイセル化学製の内圧型で、有
効膜面積0.44m2、中空糸内径0.8mm、中空糸有効
長270mm、膜素材ポリエーテルサルホン、純水透
過速度5/m2、min・Kg/cm2以上、トリプシンイ
ンヒビター(分子量2.8万)排除率65〜85%、オ
バルブミン(分子量4.5万)排除率99%以上であ
る。
膜透過速度(=清澄果汁製造速度)は第2図に
示す様に急激に経時低下した。
そこで、モジユール内の原液流動方向を逆転す
る操作を20分毎に行つたが、透過速度の経時低下
を防止または軽減する効果は全くみられなかつ
た。
参考例 1
比較例1と同じ果汁、同じモジユール、同じ条
件で清澄果汁を製造した。たゞし20分毎に原液流
動方向を逆転する操作の代りに30分毎に透過液取
出口を2分間閉鎖した。
また、透過液取出口閉鎖操作時の原液の流動方
向は、そのまゝと逆転するのとを交互に行つた。
結果を第3図に示す。透過液取出口を閉鎖して、
原液を流す操作が低下した膜透過速度を回復させ
る効果が大きく、また、その時に原液の流動方向
を逆転させた方が更に大きい。この操作の透過速
度回復効果を次式で定義する回復率で表わして表
1に示す。
Rn=Pn−P′n-1/Pn-1−P′n-1×100
Rn:透過速度回復率(%)
Pn:操作直後の透過速度
P′n-1:〃直前の〃
Pn-1:前回操作直後の〃
(Industrial Application Field) Fruit juice is largely consumed in its raw state for beverages, but there is a demand for fruit juice that does not become cloudy and remains clear when mixed and prepared as a component of beverages. , has been increasing recently. The present invention provides a method for producing clarified fruit juice having the above characteristics from raw fruit juice. Target fruit juices include almost all fruit juices such as citrus fruits (Wenzhou, Hassaku, etc.), berries (strawberries), plums (plums, peaches, etc.), apples, grapes, pineapple, etc. (Prior Art) A method has been put into practical use in which suspended pulp is removed by centrifugation or ultracentrifugation, and then dissolved pectin is decomposed using an enzyme such as pectinase. However, as the enzymatic reaction is carried out at a high temperature of 40 to 60 degrees Celsius over several hours, it loses its aroma and adds a unique odor, making it impossible to avoid quality deterioration of the fruit juice.Furthermore, the enzymes used are expensive. However, it has the disadvantage that the cost of clarification increases. As a method to overcome these drawbacks, a method is being tested in which pectin is separately removed at room temperature using an ultrafiltration membrane. (Problems to be Solved) A problem with the method of treating fruit juice with an ultrafiltration membrane is that the membrane permeation rate rapidly decreases over time. For this reason, a large-scale membrane device is required to process a predetermined amount of fruit juice in a predetermined time, and this drawback may not provide enough advantages to replace the enzymatic method. The present invention devises a simple and inexpensive membrane permeation rate recovery method in the process of membrane processing of fruit juice by cross-flow, and by periodically applying this method, the average membrane permeation rate can be maintained high and the membrane device can be scaled up. It attempts to overcome the shortcomings of Washing with surfactants, acids, alkalis, oxidizing agents, enzymes, hot water, etc. is well known as a method for restoring the reduced membrane permeation rate, and is very effective if properly selected. However, this method can only be carried out after the operation has been completed and the liquid has been recovered. Membrane permeation rate recovery methods that can be performed during operation include reversing the flow direction of the stock solution, flashing at high speed to remove the fouling layer, creating an air-liquid interface by blowing air bubbles into the stock solution, and using a sponge added to the stock solution. There are methods such as scraping with a solid object such as a ball, and reverse permeation of the permeated liquid to remove the fouling layer on the surface of the membrane. However, the method of adding air bubbles or solids is only possible with tubular membrane modules, and cannot be applied to hollow fiber membrane modules or spiral or pleated membrane modules, which have good space and energy efficiency. Although the method of allowing a portion of the permeate to pass back through is effective, it has the disadvantage of returning the liquid that has permeated the cornea back to the original solution, and the disadvantage that it requires a pump to pressurize the permeate for reverse permeation. The simplest method is to reverse the flow direction of the stock solution or release the applied pressure to flash at high speed, but it is less effective. (Means for Solving the Problems) As a result of intensive research, the present inventors have considered a simple and effective method for restoring membrane permeation rate. That is, after closing the permeate outlet for a certain period of time to stop membrane permeation, the back pressure regulating valve is opened while the permeate outlet is kept closed to flush the stock solution. This is an operation that reverses the flow direction of the
This membrane permeation rate recovery method is characterized by continuing for 20 seconds or more, preferably 1 minute or more. (Effects of the Present Invention) According to the method of the present invention, the membrane surface contaminated by fruit juice treatment can be cleaned by a simple operation, and the membrane permeation rate is restored. By carrying out this process periodically, the average membrane permeation rate can be maintained high for a long period of time, thereby reducing the capital investment required to increase the scale of the membrane device in advance of anticipating fouling of the membrane surface. (Example) The following will explain based on an example. Comparative example 1 Satsuma mandarin straight fruit juice (sugar content Brix
10.7°) 50 through a cloth with a gap of 0.2mm x 0.2mm, and then use the device shown in Fig.
Clear fruit juice was produced by supplying the juice to a hollow fiber UF membrane module under conditions of m 3 /h and module outlet pressure of 1 Kg/cm 2 . The module is an internal pressure type manufactured by Daicel Chemical, effective membrane area 0.44 m 2 , hollow fiber inner diameter 0.8 mm, hollow fiber effective length 270 mm, membrane material polyether sulfone, pure water permeation rate 5/m 2 , min・Kg/cm 2 or more, trypsin inhibitor (molecular weight 28,000) elimination rate is 65-85%, ovalbumin (molecular weight 45,000) elimination rate is 99% or more. As shown in FIG. 2, the membrane permeation rate (=clarified juice production rate) decreased rapidly over time. Therefore, an operation was performed to reverse the flow direction of the stock solution in the module every 20 minutes, but no effect was observed in preventing or reducing the decrease in permeation rate over time. Reference Example 1 A clarified fruit juice was produced using the same juice, the same module, and the same conditions as in Comparative Example 1. However, instead of reversing the flow direction of the stock solution every 20 minutes, the permeate outlet was closed for 2 minutes every 30 minutes. In addition, the flow direction of the stock solution during the operation of closing the permeate outlet was alternately maintained as it was and reversed.
The results are shown in Figure 3. Close the permeate outlet and
The operation of flowing the stock solution has a great effect in restoring the reduced membrane permeation rate, and it is even more effective to reverse the flow direction of the stock solution at that time. The permeation rate recovery effect of this operation is shown in Table 1 as a recovery rate defined by the following equation. Rn=Pn−P′n -1 /Pn -1 −P′n -1 ×100 Rn: Permeation speed recovery rate (%) Pn: Permeation speed immediately after operation P′n -1 : Immediately before Pn -1 : Immediately after the previous operation
【表】
参考例 2
温州みかん濃縮還元果汁(糖度 ブリツクス
11.1°)30を空隙0.2mm×0.2mmの布で粗過し
たのち、比較例1の装置を用いて同条件で膜透過
実験を行つた。たゞし、透過液も少量のサンプリ
ング以外はタンクに還流して、原液濃度が一定に
保たれる様にした。
透過液取出口を閉鎖して同時に原液の流動方向
を逆転する操作を行う間隔と閉鎖している時間を
種々変えて、これらが回復効果に及ぼす影響を第
4図に示す。各操作の効果を透過速度回復率で表
わし、表2に示す。10分間隔で操作した場合、操
作時間20秒以上で顕著な回復効果がみられ、操作
時間1分以上で略100%の回復がみられた。また、
表1の操作ロ,ニ,ヘと比較することにより、操
作間隔が40分以上になると効果が減少することが
示される。[Table] Reference example 2 Satsuma mandarin orange concentrate juice (sugar content Brix
11.1°) 30 was roughly filtered through a cloth with a gap of 0.2 mm x 0.2 mm, and then a membrane permeation experiment was conducted under the same conditions using the apparatus of Comparative Example 1. However, the permeate was also returned to the tank except for a small amount of sampling, so that the concentration of the stock solution was kept constant. FIG. 4 shows the influence of these changes on the recovery effect by varying the interval at which the permeate outlet is closed and at the same time reversing the flow direction of the stock solution and the time during which it is closed. The effects of each operation are expressed in terms of permeation rate recovery rate and are shown in Table 2. When the operation was performed at 10-minute intervals, a remarkable recovery effect was observed when the operation time was 20 seconds or more, and approximately 100% recovery was observed when the operation time was 1 minute or more. Also,
By comparing operations B, D, and F in Table 1, it is shown that the effect decreases when the operation interval becomes 40 minutes or more.
【表】
*前回の回復操作で回復すべきだつたが操作時間
が短くて回復できなかつた分も一緒に回復してい
るため大きくなつた。そこで前々回の操作に対し
て計算すると100%となる。
参考例 3
レモン濃縮還元果汁(糖度ブリツクス6.0°)15
を比較例1に用いたと同じフローラインの小型
装置を用いてポンプ吐出量0.6m3/h、モジユー
ル出口圧1.6Kg/cm2の条件で中空糸UF膜モジユー
ルに供給して清澄果汁を製造した。モジユールは
比較例1に用いたものと中空糸の本数が半分で、
有効膜面積が1/2である以外は等しいものを使用
した。運転は15分毎に透過液(=清澄果汁)の取
出口を1分間閉止すると共に原液の流動方向を逆
転させる操作を行いながら連続して2時間行つ
た。操作毎の透過速度回復率は第5図にみられる
様に57%,80%,86%,100%,75%,80%,63
%,50%で平均74%であつた。
参考例 4
パイナツプル濃縮還元果汁(糖度 ブリツクス
11.3°)20を空隙0.2mm×0.2mmの布で過した
のち、参考例3に用いた装置を用いて清澄果汁を
製造した。運転は15分毎に透過液の取出口を1分
間閉止する操作を行いながら連続して2時間半行
つた。操作毎の透過速度回復率は第6図にみられ
る様に、85%,92%,108%,93%,100%,80
%,77%,100%,83%,92%で、平均回復率は
91%であつた。
参考例 5
チエリー濃縮還元果汁(糖度ブリツクス6.7°)
20参考例3の装置を用いて同じ条件で清澄化処
理を1時間半行つた。たゞし、膜透過速度回復操
作は15分毎と20分毎を交互に行つた。
第7図と表3にみられる様に15分毎の回復率は
55%,72%,71%,また、20分毎の回復率は54
%,77%で、両者共、同程度の効果を示した。
次に、同じ果汁20を用いて、膜透過速度回復
操作の間隔を45分毎にした以外は全く同じ条件で
清澄化処理を行つた。回復率は第8図にみられる
様に38%と49%、平均44%で、15分毎と20分毎の
平均回復率66%の2/3であつた。[Table] *The amount that should have been recovered by the previous recovery operation, but could not be recovered due to the short operation time, was also recovered, so it became larger. So, if you calculate it for the operation before the previous one, it will be 100%. Reference example 3 Lemon concentrated and reduced juice (sugar content Brix 6.0°) 15
was supplied to a hollow fiber UF membrane module using the same small flow line device used in Comparative Example 1 under conditions of a pump discharge rate of 0.6 m 3 /h and a module outlet pressure of 1.6 Kg/cm 2 to produce clarified fruit juice. . The module has half the number of hollow fibers as that used in Comparative Example 1,
The same membrane was used except that the effective membrane area was 1/2. The operation continued for 2 hours while closing the outlet for the permeate (=clarified fruit juice) for 1 minute every 15 minutes and reversing the flow direction of the stock solution. As shown in Figure 5, the permeation rate recovery rate for each operation was 57%, 80%, 86%, 100%, 75%, 80%, 63
%, 50%, with an average of 74%. Reference example 4 Pineapple concentrated reduced fruit juice (sugar content Brix
11.3°) 20 was passed through a cloth with a gap of 0.2 mm x 0.2 mm, and then clarified fruit juice was produced using the apparatus used in Reference Example 3. The operation continued for 2 and a half hours while closing the permeate outlet for 1 minute every 15 minutes. As shown in Figure 6, the permeation rate recovery rate for each operation is 85%, 92%, 108%, 93%, 100%, 80%.
%, 77%, 100%, 83%, 92%, and the average recovery rate is
It was 91%. Reference example 5 Thierry concentrated fruit juice (sugar content Brix 6.7°)
20 Clarification treatment was carried out for 1.5 hours using the apparatus of Reference Example 3 under the same conditions. However, the membrane permeation rate recovery operation was performed alternately every 15 minutes and every 20 minutes. As seen in Figure 7 and Table 3, the recovery rate every 15 minutes is
55%, 72%, 71%, and recovery rate every 20 minutes is 54
%, 77%, and both showed similar effectiveness. Next, using the same fruit juice 20, clarification treatment was performed under exactly the same conditions except that the membrane permeation rate recovery operation was performed every 45 minutes. As shown in Figure 8, the recovery rates were 38% and 49%, with an average of 44%, which was two-thirds of the average recovery rate of 66% for every 15 minutes and every 20 minutes.
【表】
実施例 1
夏みかんストレート果汁(糖度 ブリツクス
10.1°)50を比較例1と同じ装置を用いて、ポ
ンプ吐出量1.2m3/h、モジユール出口圧力1.6
Kg/cm2の条件で清澄化処理した。膜透過速度回復
操作として20分毎に透過液取出口を1分間閉止す
る操作を運転開始後1時間40分まで5回(第9図
でイからホまで)行い、2時間目からは、透過液
取出口を閉止したのち、モジユール出口配管の調
圧弁を開放する操作を4回(第9図でヘからリま
で)行つた。
表4に示す様に透過液取出口を閉止するだけの
操作の場合の平均回復率が48%に対し、供給果汁
の印加圧力の解放を加えた操作の平均回復率は75
%で回復効果に56%の増加がみられた。[Table] Example 1 Summer mandarin orange straight fruit juice (Sugar content Brix
10.1°) 50 using the same equipment as Comparative Example 1, pump discharge amount 1.2 m 3 /h, module outlet pressure 1.6
Clarification treatment was carried out under the condition of Kg/cm 2 . As a membrane permeation rate recovery operation, the operation of closing the permeate outlet for 1 minute every 20 minutes was performed five times (from A to E in Figure 9) until 1 hour and 40 minutes after the start of operation. After closing the liquid outlet, the operation of opening the pressure regulating valve of the module outlet piping was performed four times (from F to R in FIG. 9). As shown in Table 4, the average recovery rate is 48% when the permeate outlet is simply closed, whereas the average recovery rate is 75% when the pressure applied to the supplied juice is released.
%, a 56% increase in recovery effect was seen.
第1図は本発明の果汁を清澄化する方法を実施
する装置を示す概略図で、1は原液果汁タンク、
2は供給ポンプ、3は調整バルブ、4は流量計、
5は四方弁、6は中空糸UF膜モジユール、7は
調整バルブ、8は流量計、9は圧力計、10は圧
力計、11は透過液取出口を示す。
第2図は比較例1、第3図は参考例1、第4図
は参考例2、第5図は参考例3、第6図は参考例
4、第7図は参考例5の前半、第8図は参考例5
の後半、第9図は実施例1の実験結果を示す図で
ある。
FIG. 1 is a schematic diagram showing an apparatus for carrying out the method of clarifying fruit juice of the present invention, in which 1 is a stock juice tank;
2 is a supply pump, 3 is a regulating valve, 4 is a flow meter,
5 is a four-way valve, 6 is a hollow fiber UF membrane module, 7 is a regulating valve, 8 is a flow meter, 9 is a pressure gauge, 10 is a pressure gauge, and 11 is a permeate outlet. Figure 2 is Comparative Example 1, Figure 3 is Reference Example 1, Figure 4 is Reference Example 2, Figure 5 is Reference Example 3, Figure 6 is Reference Example 4, Figure 7 is the first half of Reference Example 5, Figure 8 is reference example 5
The latter half of FIG. 9 is a diagram showing the experimental results of Example 1.
Claims (1)
方法において、膜透過液取出口を一定時間閉鎖し
た後、該閉鎖状態のままで印加圧力を解放して膜
面のフアウリングを供給果汁の流動で除去して低
下した膜透過速度を回復させる操作を30分を超え
ない間隔で、20秒間以上、好ましくは1分間以上
の条件で行うことによつて、平均膜透過速度を高
く維持することを特徴とする果汁を清澄化する方
法。 2 供給果汁の流動が方向を反転させるものであ
る特許請求の範囲第1項記載の果汁を清澄化する
方法。[Claims] 1. In a method for clarifying fruit juice using a cross-flow membrane method, after a membrane permeate outlet is closed for a certain period of time, the applied pressure is released while the membrane is in the closed state to prevent fouling on the membrane surface. The average membrane permeation rate can be increased by performing an operation for recovering the membrane permeation rate that has been reduced by removing the supplied fruit juice by flowing it at intervals of no more than 30 minutes for at least 20 seconds, preferably for at least 1 minute. A method for clarifying fruit juice, characterized in that: 2. The method for clarifying fruit juice according to claim 1, wherein the direction of flow of the supplied fruit juice is reversed.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP61116346A JPS62272957A (en) | 1986-05-21 | 1986-05-21 | Clarification of fruit juice |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP61116346A JPS62272957A (en) | 1986-05-21 | 1986-05-21 | Clarification of fruit juice |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPS62272957A JPS62272957A (en) | 1987-11-27 |
| JPH0413990B2 true JPH0413990B2 (en) | 1992-03-11 |
Family
ID=14684673
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP61116346A Granted JPS62272957A (en) | 1986-05-21 | 1986-05-21 | Clarification of fruit juice |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPS62272957A (en) |
Families Citing this family (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH0339084A (en) * | 1989-07-04 | 1991-02-20 | Daicel Chem Ind Ltd | Concentration of culture solution of unicellular algae |
| DE4401456A1 (en) * | 1994-01-19 | 1995-07-20 | Wissenschaftsfoerderung Der De | Process for clarifying beer using crossflow microfiltration |
Family Cites Families (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS5811090A (en) * | 1981-07-13 | 1983-01-21 | Arubatsuku Service Kk | Reverse osmosis device or ultrafiltration device for production of pure water |
| JPS58163406A (en) * | 1982-03-23 | 1983-09-28 | Nitto Electric Ind Co Ltd | Filtration of liquid |
| JPS59203609A (en) * | 1983-05-02 | 1984-11-17 | Daicel Chem Ind Ltd | Method for restoring separation capacity of separation membrane |
| JPS60804A (en) * | 1983-06-20 | 1985-01-05 | Poritetsukusu:Kk | Ultrafiltration apparatus |
-
1986
- 1986-05-21 JP JP61116346A patent/JPS62272957A/en active Granted
Also Published As
| Publication number | Publication date |
|---|---|
| JPS62272957A (en) | 1987-11-27 |
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Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| LAPS | Cancellation because of no payment of annual fees |