JP2622963B2 - Automatic moisture control method in the reaction of fats and oils with enzymes - Google Patents
Automatic moisture control method in the reaction of fats and oils with enzymesInfo
- Publication number
- JP2622963B2 JP2622963B2 JP3564987A JP3564987A JP2622963B2 JP 2622963 B2 JP2622963 B2 JP 2622963B2 JP 3564987 A JP3564987 A JP 3564987A JP 3564987 A JP3564987 A JP 3564987A JP 2622963 B2 JP2622963 B2 JP 2622963B2
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- Japan
- Prior art keywords
- water
- concentration
- fat
- palm oil
- moisture
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- Apparatus Associated With Microorganisms And Enzymes (AREA)
- Measuring Or Testing Involving Enzymes Or Micro-Organisms (AREA)
- Preparation Of Compounds By Using Micro-Organisms (AREA)
Description
【発明の詳細な説明】 〔産業上の利用分野〕 本発明は、油脂類、具体的にはパーム油脂を、酵素、
具体的にはリパーゼを用い、エステル交換反応を行うに
あたって、パーム油脂中の水分濃度を安全かつ正確に所
定濃度に制御させる方法に関する。DETAILED DESCRIPTION OF THE INVENTION [Industrial Application Field] The present invention relates to fats and oils, specifically palm fats and oils,
Specifically, the present invention relates to a method for safely and accurately controlling the water concentration in palm oil and fat to a predetermined concentration when a transesterification reaction is performed using lipase.
従来より油脂類の酵素反応を行う場合、油脂溶液中の
水分濃度によって酵素の働き大きく左右されることが知
られている。すなわち、一般的に水分が皆無の状態では
酵素反応は起こらず、同一酵素において水分が多量の領
域では加水分解反応が主体となり、水分が微量の領域で
はエステル交換反応が主体となる。このことから、油脂
溶液中の水分濃度を制御することが酵素反応を効率よく
進める上で重要なポイントとなる。It has been known that when performing an enzymatic reaction of fats and oils, the action of the enzyme is greatly affected by the water concentration in the fat and oil solution. In other words, in general, no enzymatic reaction occurs in the absence of water, and in the same enzyme, a hydrolysis reaction is mainly performed in a region with a large amount of water, and a transesterification reaction is mainly performed in a region with a small amount of water. For this reason, controlling the water concentration in the fat or oil solution is an important point for efficiently proceeding the enzyme reaction.
油脂溶液中の水分濃度を下げる方法については、従来
より例えば窒素ガスなどの不活性ガスを油脂溶液中に曝
気させ、排出ガス中に水分を同伴させて反応槽外に除去
する方法が知られている。Regarding the method of lowering the water concentration in the fat and oil solution, a method of aerating an inert gas such as nitrogen gas into the fat and oil solution, and entraining water in the exhaust gas to remove the gas from the reaction tank is conventionally known. I have.
また、水分濃度を上げる方法としては油脂溶液中に水
を噴霧させる方法が知られている。Further, as a method for increasing the water concentration, a method of spraying water into a fat or oil solution is known.
ところで、このような従来の方法では、油脂溶液中の
水分濃度を自動制御する方法においては、油脂溶液中
（実際の反応では油脂の溶解度を下げるために、へキサ
ンなどの有機性の溶媒が混合されている）の水分濃度を
溶媒などの妨害および劣化を受けずに、直接、正確、安
全、かつ経済的に測定することのできる水分濃度検出手
段が見当たらず、このため反応溶液中の水分を効率よく
安全かつ正確に自動制御することができなかった。By the way, in such a conventional method, in the method of automatically controlling the water concentration in the fat and oil solution, an organic solvent such as hexane is mixed in the fat and oil solution (in an actual reaction to reduce the solubility of the fat and oil). There is no means for directly, accurately, safely and economically measuring the water concentration without interference and deterioration of the solvent, etc. Automatic control could not be performed efficiently, safely and accurately.
本発明は、このような従来技術を背景になされたもの
で、溶媒などの妨害および劣化を受けずにパーム油脂中
の水分濃度を直接、正確、安全、かつ経済的に測定する
ことで、パーム油脂中の水分濃度を所定濃度に効率よく
安全かつ正確に制御されることができるリパーゼによる
パーム油脂のエステル交換反応における水分自動制御方
法を提供するものである。The present invention has been made on the background of such conventional technology, and directly, accurately, safely, and economically measures the moisture concentration in palm oil and fat without being affected or deteriorated by a solvent or the like. An object of the present invention is to provide a method for automatically controlling water in a transesterification reaction of palm oil with lipase, which can efficiently and safely and accurately control the water concentration in fats and oils to a predetermined concentration.
すなわち、本発明、反応槽内で水分の存在下にパーム
油脂（以下「油脂類」ともいう）のリパーゼ（以下「酵
素」ともいう）によるエステル交換反応（以下「反応」
ともいう）を行うにあたって、少なくともパーム油脂溶
液（以下「油脂溶液」ともいう）中の水分濃度を検出す
る液相中水分濃度センサを含む水分濃度検出手段を用い
て、前記パーム油脂類中の水分濃度を検出させ、前記水
分濃度検出手段で検出された検出信号に基づいて、水分
濃度制御手段により前記油脂類中の水分濃度を所定濃度
に制御させることを特徴とする酵素による油脂類の反応
における水分自動制御方法を提供するものである。That is, in the present invention, a transesterification reaction (hereinafter referred to as "reaction") of palm oil (hereinafter also referred to as "fats") with lipase (hereinafter referred to as "enzyme") in the presence of moisture in a reaction vessel.
At the same time, the water content in the palm oils and fats (hereinafter also referred to as “oil solution”) is measured using a water concentration detecting means including a liquid phase water concentration sensor for detecting the water concentration in the palm oil solution. Detecting the concentration, based on the detection signal detected by the water concentration detecting means, in the reaction of fats and oils by the enzyme characterized by controlling the water concentration in the fats and oils to a predetermined concentration by the water concentration control means An object of the present invention is to provide an automatic moisture control method.
次に、本発明の酵素による油脂類の反応における水分
自動制御方法の構成を図面に基づいて説明する。Next, the configuration of the method for automatically controlling water in the reaction of fats and oils with the enzyme of the present invention will be described based on the drawings.
本発明の酵素による油脂類の反応における水分自動制
御方法を使用した水分自動制御反応装置は、第１図に示
すように、反応槽10、曝気部20、撹拌部（撹拌位置）3
0、給水部40、水分濃度検出部（水分濃度検出手段）5
0、水分濃度制御部（水分濃度制御手段）60、および気
化溶媒冷却回収部70を備えている。As shown in FIG. 1, an automatic moisture control reaction apparatus using the automatic moisture control method in the reaction of fats and oils with the enzyme of the present invention comprises a reaction tank 10, an aeration unit 20, a stirring unit (stirring position) 3
0, water supply section 40, moisture concentration detection section (moisture concentration detection means) 5
0, a water concentration control unit (water concentration control means) 60, and a vaporized solvent cooling and recovery unit 70.
前記反応槽10は、酵素による油脂類の酵素反応を行う
ための槽で、この反応槽10の下部にはジャケット11が形
成されており、またこの反応槽10には、ジャケット11内
の水および反応槽10内の油脂溶液Ｕを所定温度に制御す
るためのヒータ121を有する水温温度指示調節計12が取
り付けられている。The reaction tank 10 is a tank for performing an enzymatic reaction of fats and oils with an enzyme.A jacket 11 is formed at a lower portion of the reaction tank 10, and the reaction tank 10 includes water and water in the jacket 11. A water temperature indicator controller 12 having a heater 121 for controlling the temperature of the oil solution U in the reaction tank 10 to a predetermined temperature is attached.
前記曝気部20は、反応槽10内の油脂溶液Ｕ中の水分濃
度を下げるための油脂溶液Ｕ（油脂のほかに水Ｗおよび
有機性の溶媒Ｙをも含有する溶液）を、例えば窒素ガス
などの不活性ガスＦで曝気させるための曝気部で、不活
性ガスボンベ21、不活性ガス循環ポンプ22、およびガス
吹き出しノズル23を有している。The aeration unit 20 includes a fat / oil solution U (a solution containing water W and an organic solvent Y in addition to the fat / oil) for lowering the water concentration in the fat / oil solution U in the reaction tank 10, for example, nitrogen gas or the like. An aeration unit for aerating with the inert gas F, which has an inert gas cylinder 21, an inert gas circulation pump 22, and a gas blowing nozzle 23.
この不活性ガスボンベ21は、不活性ガスＦが圧縮収納
されているボンベであり、また不活性ガス循環ポンプ22
は、不活性ガスボンベ21内の不活性ガスＦを反応槽10内
へ送るための輸送ポンプで、この不活性ガス循環ポンプ
22に前記ガス吹き出しノズル23が、先端部の不活性ガス
Ｆの吹き出し口231を反応槽10の底部内に位置させて接
続されている。なお、前記不活性ガスボンベ21はレギュ
レータ24を有しており、また不活性ガス循環ポンプ22と
不活性ガスボンベ21とは不活性ガス用連通パイプ25を介
して接続されている。さらに、不活性ガスボンベ21近く
の不活性ガス連通用パイプ25には不活性ガスボンベ用弁
26が設けられている。The inert gas cylinder 21 is a cylinder in which the inert gas F is compressed and stored.
Is a transport pump for sending the inert gas F in the inert gas cylinder 21 into the reaction tank 10.
The gas blow-out nozzle 23 is connected to 22 with the blow-out port 231 of the inert gas F at the tip located inside the bottom of the reaction tank 10. The inert gas cylinder 21 has a regulator 24, and the inert gas circulation pump 22 and the inert gas cylinder 21 are connected via an inert gas communication pipe 25. Further, the inert gas communication pipe 25 near the inert gas cylinder 21 has an inert gas cylinder valve.
26 are provided.
前記撹拌部30は、油脂溶液Ｕを混合するとともに曝気
部20による曝気に加えて、油脂溶液Ｕ中の水分濃度低下
をさらに促進させるための油脂溶液Ｕの撹拌部で、反応
槽10の上部に取り付けられた撹拌用モータ31と、前記ガ
ス吹き出しノズル23より上方の反応槽10の底部内に配置
された撹拌羽根32とを有している。The stirrer 30 is a stirrer for the fat and oil solution U for further mixing and mixing the fat and oil solution U and aeration by the aeration unit 20, and further promoting a decrease in the water concentration in the fat and oil solution U. It has a stirring motor 31 attached thereto, and a stirring blade 32 arranged in the bottom of the reaction tank 10 above the gas blowing nozzle 23.
前記給水部40は、反応槽10内の水量を補給するための
給水部で、水Ｗを貯水する給水槽41、この給水槽41と反
応槽10とを連通し、かつ反応槽側の先端に給水用スプレ
ーノズル421が接続された給水用連通パイプ42、および
この給水用連通パイプ42の途中に設けられた給水用ポン
プ43を有している。The water supply unit 40 is a water supply unit for replenishing the amount of water in the reaction tank 10, a water supply tank 41 for storing water W, communicates the water supply tank 41 with the reaction tank 10, and is provided at the tip of the reaction tank side. It has a water supply communication pipe 42 to which a water supply spray nozzle 421 is connected, and a water supply pump 43 provided in the middle of the water supply communication pipe 42.
前記水分濃度検出部50は、油脂中の水分濃度を検出す
るための検出部であり、溶液中水分指示計（液相中水分
濃度センサ）51、溶液温度指示計（液相中水分濃度セン
サ）52、ガス体水分指示計（気相中水分濃度センサ）5
3、ガス体温度指示計（気相中水分濃度センサ）54を有
している。The water concentration detecting section 50 is a detecting section for detecting the water concentration in fats and oils, and includes a water indicator in solution (moisture concentration sensor in liquid phase) 51 and a liquid temperature indicator (moisture concentration sensor in liquid phase). 52, Gas moisture indicator (moisture concentration sensor in gas phase) 5
3. A gas temperature indicator (moisture concentration sensor in gas phase) 54 is provided.
なお、溶液中水分指示計51としては、石油化学分野で
広く使用されている露点温度計を使用することが好まし
く、またこの水分計の検出部にはAl2O3薄膜を使用する
ことが好ましく、さらに防曝型の水分計とした方が溶媒
中でも使用できるために好ましい。かくて、溶液中の水
分は、溶液中水分指示計51と溶液中温度指示計52とから
溶液中の当該温度での露点を計算し、溶液中の水分濃度
を決定することができる。As the moisture indicator in solution 51, it is preferable to use a dew point thermometer widely used in the petrochemical field, and it is preferable to use an Al 2 O 3 thin film for the detection unit of the moisture meter. Further, it is preferable to use an anti-exposure type moisture meter because it can be used in a solvent. Thus, for the water content in the solution, the dew point in the solution at the temperature can be calculated from the water content indicator 51 in the solution and the temperature indicator 52 in the solution to determine the water concentration in the solution.
一方、気相中の水分濃度は、ガス体水分指示計53とガ
ス体温度指示計54とから、気相中の相対湿度を決定する
ことができる。On the other hand, as for the moisture concentration in the gas phase, the relative humidity in the gas phase can be determined from the gas body moisture indicator 53 and the gas body temperature indicator 54.
これらの水分指示計、あるいは温度指示計は、前記溶
液中水分指示計51や溶液温度指示計52と同様な計器が好
ましいが特に限定されるものではなく、従来公知のもの
が使用できる。The moisture indicator or the temperature indicator is preferably the same instrument as the solution-in-solution moisture indicator 51 or the solution temperature indicator 52, but is not particularly limited, and conventionally known instruments can be used.
次に、前記水分濃度制御部60は、前記水分濃度検出部
50で検出された検出信号に基づいて油脂中の水分濃度を
所定濃度に制御させるための制御部で、マイクロコンピ
ュータ61、不活性ガス流量指示調節計62、回転数指示調
整計63、および水流量指示調節計64を有している。Next, the water concentration control unit 60 includes the water concentration detection unit.
A control unit for controlling the water concentration in the fat or oil to a predetermined concentration based on the detection signal detected at 50, a microcomputer 61, an inert gas flow rate controller 62, a rotation speed controller 63, and a water flow rate. It has an indicating controller 64.
このマイクロコンピュータ61は、水分濃度制御部60の
制御回路部である。なお、水分濃度を制御するコンピュ
ータには、必ずしもマイクロコンピュータを使用しなく
ても、水分濃度が制御できれば他のコンピュータでもよ
い。The microcomputer 61 is a control circuit of the moisture concentration controller 60. The computer for controlling the moisture concentration does not necessarily need to use a microcomputer, but may be another computer as long as the computer can control the moisture concentration.
不活性ガス流量指示調節計62は、マイクロコンピュー
タ61の指令により不活性ガス循環ポンプ22による不活性
ガスＦの吹き出し流量を調節する調節計で、ガス吹き出
しノズル23の途中に連接されている。なお、不活性ガス
流量指示調節計62には、前記不活性ガス吹き出しノズル
23の吹き出し口231から吹き出される不活性ガスＦの流
量を検出する図示しない流量検出部が内蔵されている。
ただし、外設すれば必ずしも流量検出部を内蔵する必要
はない。The inert gas flow rate controller 62 is a controller for adjusting the flow rate of the inert gas F blown by the inert gas circulation pump 22 in accordance with a command from the microcomputer 61, and is connected to the middle of the gas blowing nozzle 23. The inert gas flow rate indicator controller 62 includes the inert gas blowing nozzle.
A flow rate detector (not shown) for detecting the flow rate of the inert gas F blown out from the blow-out ports 231 of the 23 is built in.
However, if it is provided outside, it is not always necessary to incorporate the flow detection unit.
回転数指示調節計63は、マイクロコンピュータ61の指
令により撹拌モータ31の回転数を調節する調節計で、撹
拌用モータ31に取り付けられている。なお、回転数指示
調節計63にはモータ回転数を検出する図示しない回転数
検出部が内蔵されている。ただし、外設すれば必ずしも
回転数検出部を内蔵する必要はない。The rotation speed indicating controller 63 is a controller for adjusting the rotation speed of the stirring motor 31 according to a command from the microcomputer 61, and is attached to the stirring motor 31. The rotation speed indicating controller 63 has a built-in rotation speed detection unit (not shown) for detecting the motor rotation speed. However, if it is provided outside, it is not always necessary to incorporate the rotation speed detecting unit.
水流量指示調節計64は、マイクロコンピュータ61の指
令により給水用ポンプ43による送水量を調節する調節計
で、給水用ポンプ43と反応槽10との間の給水用連通パイ
プ42に連接されている。なお、水流量指示調節計64に
は、給水槽41からの水量を検出する図示しない水量検出
部が内蔵されている。ただし、外設すれば必ずしも水量
検出部を内蔵する必要はない。The water flow rate instruction controller 64 is a controller that adjusts the amount of water supplied by the water supply pump 43 according to a command from the microcomputer 61, and is connected to the water supply communication pipe 42 between the water supply pump 43 and the reaction tank 10. . It should be noted that the water flow rate indicating controller 64 has a built-in water amount detection unit (not shown) for detecting the amount of water from the water supply tank 41. However, if it is provided outside, it is not always necessary to incorporate the water amount detection unit.
なお、これらの調節計62〜64のほかにも、水分濃度を
制御可能な他の調節計を設けてもかまわない。In addition to these controllers 62 to 64, other controllers capable of controlling the water concentration may be provided.
前記気化溶媒冷却回収部70は、反応槽10内の気化溶媒
ｙを冷却して再利用できるように液体に変換させる回収
部で、冷却塔71、水冷循環器72、気化溶媒流入パイプ7
3、液化溶媒流出パイプ74、および不活性ガス回収パイ
プ75を有している。The vaporized solvent cooling and recovery unit 70 is a recovery unit that cools and converts the vaporized solvent y in the reaction tank 10 into a liquid so that it can be reused.The cooling tower 71, the water-cooled circulator 72, and the vaporized solvent inflow pipe 7
3. It has a liquefied solvent outflow pipe 74 and an inert gas recovery pipe 75.
水冷循環器72は、前記冷却塔71に設けられて気化溶媒
ｙと水蒸気ｗとを冷却させる水冷装置である。The water cooling circulator 72 is a water cooling device provided in the cooling tower 71 for cooling the vaporized solvent y and the steam w.
また、気化溶媒流入パイプ73は、主に反応槽10内の不
活性ガスＦを冷却塔71内に導くためのパイプで、反応槽
10の上部と冷却塔71のほぼ中央部とを連通させている。The vaporized solvent inflow pipe 73 is a pipe for mainly guiding the inert gas F in the reaction tank 10 into the cooling tower 71.
The upper part of 10 and the substantially central part of the cooling tower 71 communicate with each other.
さらに、液化溶媒流出パイプ74は、前記水冷循環器72
で冷却されて液化した溶媒Ｙの反応槽10への返却用パイ
プであり、冷却塔71の下部と反応槽10の上部とを連通さ
せている。Further, the liquefied solvent outflow pipe 74 is connected to the water-cooled circulator 72.
A pipe for returning the solvent Y cooled and liquefied in the reaction tank 10 to the reaction tank 10, and communicates a lower part of the cooling tower 71 with an upper part of the reaction tank 10.
さらにまた、不活性ガス回収パイプ75は、冷却塔71に
流入された不活性ガスＦのリサイクル用パイプであっ
て、冷却塔71と上部と前記不活性ガス連通用パイプ25と
を連通させている。Furthermore, the inert gas recovery pipe 75 is a pipe for recycling the inert gas F that has flowed into the cooling tower 71, and connects the cooling tower 71 with the upper part and the inert gas communication pipe 25. .
なお、この不活性ガス回収パイプ75には、外部排気用
の不活性ガス排気用弁751が設けられている。Note that the inert gas recovery pipe 75 is provided with an inert gas exhaust valve 751 for external exhaust.
なお、この気化溶媒冷却回収部70は、必ずしも必要で
はないが、設置した方が溶媒Ｙを再使用できて好まし
い。The vaporized solvent cooling / recovering section 70 is not always necessary, but is preferably installed because the solvent Y can be reused.
次に、本発明の酵素による油脂類の反応における水分
自動制御方法を使用した水分自動制御反応装置の作用を
説明する。Next, the operation of the automatic moisture control reaction apparatus using the automatic moisture control method in the reaction of fats and oils with the enzyme of the present invention will be described.
まず、油脂溶液Ｕ中の水分濃度を低下させる場合につ
いて説明すると、予め不活性ガスボンベ用弁26の弁を開
き、かつ不活性ガス循環ポンプ22を駆動させて不活性ガ
スボンベ21内の不活性ガスＦを不活性ガス連通用パイプ
25内へ流入させる。これにより、不活性ガスＦは、不活
性ガス循環ポンプ22の駆動によりガス吹き出しノズル23
へ流れて行き、吹き出し口231から反応槽10の油脂溶液
Ｕ中に吹き出され、油脂溶液Ｕを不活性ガスＦで曝気さ
せる。このため、油脂溶液Ｕ中の水Ｗは、不活性ガスＦ
に伴って水蒸気ｗとなり油脂溶液Ｕ中から除去され、油
脂溶液Ｕ中の水分濃度が低下される。First, the case where the water concentration in the oil solution U is reduced will be described. First, the valve of the inert gas cylinder valve 26 is opened, and the inert gas circulation pump 22 is driven to activate the inert gas F in the inert gas cylinder 21. The inert gas communication pipe
Allow to flow into 25. As a result, the inert gas F is supplied to the gas blowing nozzle 23 by the driving of the inert gas circulation pump 22.
The oil and fat solution U is blown out from the outlet 231 into the oil and fat solution U in the reaction tank 10 and is aerated with the inert gas F. For this reason, the water W in the oil and fat solution U is
As a result, water vapor w is removed from the fat and oil solution U, and the water concentration in the fat and oil solution U is reduced.
また、このとき反応槽10の油脂溶液Ｕは、撹拌羽根32
で撹拌されているため、完全混合されるとともに油脂溶
液Ｕ中の水Ｗの気化がさらに促進されてより多くの水Ｗ
が油脂溶液Ｕ中から除去され、油脂溶液Ｕ中の水分濃度
の低下がさらに進む。At this time, the oil solution U in the reaction tank 10 is
, The mixture is completely mixed and the vaporization of the water W in the fat and oil solution U is further promoted, so that more water W
Is removed from the fat / oil solution U, and the water concentration in the fat / oil solution U further decreases.
反応槽10内のガス体となった水蒸気ｗ、不活性ガスＦ
および気化溶媒ｙは、気化溶媒流入パイプ73を介して冷
却塔71へ流入され、ここで冷却循環器72により冷却され
る。これにより、水蒸気ｗと気化溶媒ｙとが液化して元
の水Ｗと溶媒Ｙとになり、これらは比重差で分離されて
水Ｗは外部排出され、また溶液Ｙは液化溶媒流出パイプ
74を介して反応槽10内へ返却される。Steam w, inert gas F which has become a gas in the reaction tank 10
The vaporized solvent y flows into the cooling tower 71 via the vaporized solvent inflow pipe 73, where it is cooled by the cooling circulator 72. Thereby, the water vapor w and the vaporized solvent y are liquefied to become the original water W and the solvent Y, which are separated by a specific gravity difference and the water W is discharged to the outside, and the solution Y is a liquefied solvent outflow pipe.
It is returned into the reaction tank 10 via 74.
一方、不活性ガスＦは、不活性ガス回収パイプ75を介
して曝気部20の前記不活性ガス用連通パイプ25に送られ
て再利用される。なお、不活性ガス排気用弁751を開け
ることで使用後の不活性ガスＦを外部排気させることも
できる。On the other hand, the inert gas F is sent to the inert gas communication pipe 25 of the aeration unit 20 via the inert gas recovery pipe 75 and is reused. In addition, by opening the inert gas exhaust valve 751, the used inert gas F can be exhausted to the outside.
また、油脂溶液Ｕ中の水分濃度が所定濃度より低くな
ったときには、給水槽40内の所定量の水Ｗを給水用ポン
プ43により給水用スプレーノズル421から噴出させる。When the water concentration in the fat / oil solution U becomes lower than the predetermined concentration, a predetermined amount of water W in the water supply tank 40 is ejected from the water supply spray nozzle 421 by the water supply pump 43.
次に、油脂溶液Ｕ中の水分濃度を上昇させる場合に
は、前述した油脂溶液Ｕ中の水分濃度が所定濃度より低
くなったときと同様に、給水用ポンプ43を駆動させて給
水槽41内の水Ｗを給水用スプレーノズル421から噴出さ
せる。これにより、油脂溶液Ｕ中の水量が増加して油脂
溶液Ｕ中の水分濃度を上昇させることができる。Next, when increasing the water concentration in the oil and fat solution U, the water supply pump 43 is driven to drive the water in the water supply tank 41 in the same manner as when the water concentration in the oil and fat solution U becomes lower than the predetermined concentration. Of water W is ejected from the water supply spray nozzle 421. Thereby, the amount of water in the fat and oil solution U increases, and the water concentration in the fat and oil solution U can be increased.
次にまた、この水分自動制御反応装置における水分自
動制御方法を説明すると、まず装置運転開始時に、
（１）油脂溶液Ｕ中の水分濃度の最大値および最小値、
（２）不活性ガス流量の最大値および最小値（最小値は
通常ゼロ）、および（３）撹拌羽根回転数の最大値およ
び最小値を設定する。なお、測定時間の間隔をも設定し
た方が良好である。Next, the automatic moisture control method in this automatic moisture control reaction apparatus will be described.
(1) the maximum value and the minimum value of the water concentration in the oil solution U,
(2) The maximum value and the minimum value of the inert gas flow rate (the minimum value is usually zero), and (3) The maximum value and the minimum value of the rotation speed of the stirring blade are set. It is better to set the measurement time interval.
反応槽10内の油脂溶液Ｕ中の水分濃度は、溶液中水分
指示計51および溶液温度指示計52で検出され、また反応
槽10内のガス体中の水分濃度は、ガス体水分指示計53お
よびガス体温度指示計54で検出されてマイクロコンピュ
ータ61へのその検出信号が送られる。The moisture concentration in the oil solution U in the reaction vessel 10 is detected by a moisture indicator 51 in the solution and a solution temperature indicator 52, and the moisture concentration in the gas in the reaction vessel 10 is measured by a moisture indicator 53 in the gas body. The detection signal is sent to the microcomputer 61 after being detected by the gas body temperature indicator 54.
このマイクロコンピュータ61では、それぞれの指示計
51〜54で検出された検出信号を、前記（１）の油脂溶液
Ｕ中の水分濃度の最大値および最小値と比較して水分濃
度の制御が行われる。In this microcomputer 61, each indicator
The detection signal detected in 51 to 54 is compared with the maximum value and the minimum value of the water concentration in the fat / oil solution U of (1) to control the water concentration.
すなわち、反応槽10内の水分濃度が高い場合には、不
活性ガス流量指示調節計62で不活性ガス循環ポンプ22の
出力を上げて不活性ガスＦの流量を増加させたり、回転
数指示調節計63で撹拌モータ31の出力を上げて撹拌羽根
32の回転数を増加させる。また、反応槽10内の水分濃度
が低い場合には、水流量指示調節計64で給水用ポンプ43
を作動させて給水槽41内の水Ｗを反応槽10内に噴出させ
る。That is, when the water concentration in the reaction tank 10 is high, the output of the inert gas circulation pump 22 is increased by the inert gas flow rate indicator controller 62 to increase the flow rate of the inert gas F, The output of the stirring motor 31 is increased by a total of 63 and the stirring blade
Increase 32 rpm. When the water concentration in the reaction tank 10 is low, the water supply pump 43
Is operated to cause the water W in the water supply tank 41 to squirt into the reaction tank 10.
なお、このマイクロコンピュータ61による水分制御
を、第２図の水分制御フローチャートを参照してさらに
詳細に説明すると、まずステップ611で各指示計51〜54
で検出された検出信号が油脂溶液Ｕ中の水分濃度の最大
値より低いかどうかをチェックし、低ければステップ61
2で油脂溶液Ｕ中の水分濃度の最小値より高いかどうか
をチェックする。ここで、この最小値より高ければ、予
め設定していた水分濃度の範囲内であるために制御終了
となる。The moisture control by the microcomputer 61 will be described in more detail with reference to the moisture control flowchart of FIG.
It is checked whether or not the detection signal detected in the step is lower than the maximum value of the water concentration in the fat and oil solution U.
In step 2, it is checked whether the water concentration in the oil solution U is higher than the minimum value. Here, if it is higher than the minimum value, the control is terminated because it is within the range of the moisture concentration set in advance.
また、ステップ611で各指示計51〜54で検出された検
出信号が油脂溶液Ｕ中の水分濃度の最大値より高けれ
ば、ステップ613で反応槽10内のガス体中の水分濃度の
最大値より高いかどうかをチェックし、高ければステッ
プ614で不活性ガス流量の許容範囲内かどうかをチェッ
クし、範囲内であれば、不活性ガスＦの増加量を演算し
て不活性ガス流量指示調節計62へ所定量になるまで不活
性ガスＦの増加指令を発信し、また範囲外であれば、ス
テップ613での最大値より低い場合と同様にステップ615
へ行く。このステップ615では、撹拌モータ31の回転数
が許容範囲内かどうかをチェックし、範囲内であれば回
転数増加量の演算をして回転数指示調節計63へ撹拌モー
タ31の回転数の増加指令を所定量になるまで発信し、ま
た範囲外であれば外部へ警報する。If the detection signal detected by each of the indicators 51 to 54 in Step 611 is higher than the maximum value of the water concentration in the fat and oil solution U, then in Step 613, the detection signal is higher than the maximum value of the water concentration in the gas in the reaction tank 10. It is checked whether it is high, and if it is high, it is checked in step 614 whether it is within the allowable range of the inert gas flow rate. An increase command of the inert gas F is transmitted to the predetermined amount to 62, and if it is out of the range, the flow proceeds to step 615 similarly to the case where the maximum value is lower than the maximum value in step 613.
Go to In this step 615, it is checked whether or not the rotation speed of the stirring motor 31 is within the allowable range. If the rotation speed is within the range, a calculation of the rotation speed increase amount is performed, and the rotation speed indication controller 63 increases the rotation speed of the stirring motor 31. The command is issued until a predetermined amount is reached, and if it is out of the range, an alarm is issued to the outside.
さらに、前記ステップ612で油脂溶液Ｕ中の水分濃度
の最小値により低い場合には、ステップ616で反応槽10
内のガス体中の水分濃度の最大値より高いかどうかをチ
ェックし、高ければステップ617で撹拌モータ31の回転
数が許容範囲内かどうかをチェックし、範囲内であれば
回転数減少量の演算をして回転数指示調節計63へ撹拌モ
ータ31の回転数の減少指令を所定量になるまで発信し、
また範囲外であれば、ステップ616での最大値より低い
場合と同様にステップ618へ行く。このステップ618で
は、不活性ガス流量の許容範囲内かどうかをチェック
し、範囲内であれば、不活性ガスＦの減少量を演算して
不活性ガス流量指示調節計62へ所定量になるまで不活性
ガスＦの減少指令を発信し、また範囲外であれば、給水
槽41内の水Ｗの添加量を演算して水流量指示調節計64へ
所定量になるまで水Ｗの添加指令を発信する。Further, if the water concentration in the oil solution U is lower than the minimum value in step 612, the reaction tank 10
It is checked whether it is higher than the maximum value of the water concentration in the gas body in the inside.If it is higher, it is checked in step 617 whether the rotation speed of the stirring motor 31 is within the allowable range. The calculation is performed, and a reduction command of the rotation speed of the stirring motor 31 is transmitted to the rotation speed instruction controller 63 until the predetermined amount is reached,
If the value is out of the range, the process proceeds to step 618 as in the case where the value is lower than the maximum value in step 616. In this step 618, it is checked whether or not the flow rate is within the allowable range of the inert gas flow rate. A command to decrease the inert gas F is transmitted, and if it is out of the range, the addition amount of the water W in the water supply tank 41 is calculated and the addition command of the water W is sent to the water flow rate indicating controller 64 until the predetermined amount is reached. send.
このようにすることで、溶媒Ｙなどの妨害および劣化
を受けずに油脂類中の水分濃度を直接、正確、安全、か
つ経済的に測定できて、油脂類中の水分濃度を所定濃度
に効率よく安全かつ正確に制御させることができる。By doing so, the water concentration in fats and oils can be directly, accurately, safely and economically measured without being affected or deteriorated by the solvent Y and the like, and the water concentration in fats and oils can be efficiently reduced to a predetermined concentration. It can be controlled well and safely and accurately.
また、本発明では、油脂中の水分濃度の制御効果を向
上させるために、反応槽10内の油脂溶液Ｕ中の水分濃度
を検出するだけでなく、反応槽10内のガス体中の水分濃
度をも検出して制御するための、水分濃度の制御がより
効率よく正確にできる。Further, in the present invention, in order to improve the control effect of the moisture concentration in the fat and oil, not only the moisture concentration in the fat and oil solution U in the reaction vessel 10 is detected, but also the moisture concentration in the gas body in the reaction vessel 10 is improved. The water concentration can be controlled more efficiently and accurately for detecting and controlling the water concentration.
本発明の酵素による油脂類の反応における水分自動制
御方法は、少なくとも油脂溶液中の水分濃度を検出する
液相中水分濃度センサを含む水分濃度検出手段を用い
て、前記油脂類中の水分濃度を検出させ、前記水分濃度
検出手段で検出された検出信号に基づいて、水分濃度制
御手段により前記油脂類中の水分濃度を所定濃度に制御
させることで、溶媒などの妨害および劣化を受けずに油
脂類中の水分濃度を直接、正確、安全、かつ経済的に測
定できて、油脂類中の水分濃度を所定濃度に効率よく安
全かつ正確に制御させることができる。The automatic moisture control method in the reaction of fats and oils with the enzyme of the present invention uses a moisture concentration detecting means including a liquid-phase moisture concentration sensor that detects at least the moisture concentration in the fat and oil solution to determine the moisture concentration in the fats and oils. By controlling the water concentration in the fats and oils to a predetermined concentration by the water concentration control means based on the detection signal detected by the water concentration detection means, the It is possible to directly, accurately, safely and economically measure the water concentration in the oils and fats, and to efficiently and safely and accurately control the water concentration in the fats and oils to a predetermined concentration.
以下、実施例を挙げ、本発明をさらに具体的に説明す
るが、本発明は以下の実施例に限定されるものではな
い。Hereinafter, the present invention will be described more specifically with reference to Examples, but the present invention is not limited to the following Examples.
実施例１ 第１図の装置を用い、パーム油脂とステアリン酸とか
ら、リパーゼを作用させてカカオ脂の代用脂となる対称
形トリグリセリドを製造した。Example 1 Using the apparatus shown in FIG. 1, lipase was allowed to act from palm oil and fat and stearic acid to produce a symmetric triglyceride serving as a fat substitute for cocoa butter.
すなわち、反応槽10に、パーム油100重量部に対し、
ステアリン酸75重量部、ヘキサン320重量部、固定化酵
素3.5重量部、および水1.5重量部を使用し（全量２）
を仕込んだ。That is, in the reaction tank 10, for 100 parts by weight of palm oil,
Using 75 parts by weight of stearic acid, 320 parts by weight of hexane, 3.5 parts by weight of immobilized enzyme, and 1.5 parts by weight of water (total amount 2)
Was charged.
なお、水は予め固定化酵素に添加し、均一に湿潤させ
て使用し、またこのときの反応温度は42〜43℃であっ
た。In addition, water was added to the immobilized enzyme in advance and used after being uniformly wetted, and the reaction temperature at this time was 42 to 43 ° C.
反応溶液中の水分制御値は、第１段階の加水分解反応
では、無調整で飽和水分濃度の800〜1,000mg/kgを維持
でき、その反応時間は２時間であった。第２段階のエス
テル交換反応では、窒素ガスを系内に吹き込むことによ
り急激に水分を除去して水分値を100mg/kg程度に下げ、
そののち、系内の水分値を100〜150mg/kgに制御した。
このときの反応時間は、6.5時間であった。その結果、
パーム油脂の1,3−位置がステアリン酸に置き代わった
対称型トリグリセリドが80％の収率で得られた。本実施
例における反応時間と反応系内の水分濃度あるいは窒素
ガス流量の相関関係を、第３図に示す。The control value of the water content in the reaction solution could be maintained at a saturated water concentration of 800 to 1,000 mg / kg without adjustment in the first stage hydrolysis reaction, and the reaction time was 2 hours. In the second-stage transesterification reaction, water is rapidly removed by blowing nitrogen gas into the system to reduce the water value to about 100 mg / kg.
After that, the water value in the system was controlled at 100 to 150 mg / kg.
At this time, the reaction time was 6.5 hours. as a result,
A symmetric triglyceride in which 1,3-position of palm oil was replaced by stearic acid was obtained in a yield of 80%. FIG. 3 shows the correlation between the reaction time and the water concentration or the nitrogen gas flow rate in the reaction system in this embodiment.
なお、本実施例では、水分の除去の規模が小さいた
め、撹拌羽根の回転数は200rpmの一定値とし、不活性ガ
スの制御のみで充分制御が可能であった。また、油脂溶
液中の水分の定量は、一定量サンプルを採取し、カール
フィッシャー法によって測定した。連続的に測定した水
分計（露点温度計）による露点温度とカールフィッシャ
ー法による水分値との関係を第４図に示す。In this example, since the scale of water removal was small, the rotation speed of the stirring blade was set to a constant value of 200 rpm, and sufficient control was possible only by controlling the inert gas. In addition, the quantitative determination of the water content in the fat and oil solution was measured by a Karl Fischer method by collecting a fixed amount of a sample. FIG. 4 shows the relationship between the dew point temperature measured continuously by a moisture meter (dew point thermometer) and the moisture value measured by the Karl Fischer method.
両値との間には、相関関係が成立することが分かる。
このように、連続的に水分濃度を測定できる水分計（露
点温度計）を使用することにより油脂溶液中の水分濃度
の測定と制御が正確、迅速、安全に行うことができるこ
とが判明した。It can be seen that a correlation is established between the two values.
As described above, it has been found that the measurement and control of the moisture concentration in the fat and oil solution can be performed accurately, quickly and safely by using a moisture meter (dew point thermometer) capable of continuously measuring the moisture concentration.
本発明によれば、溶媒などの妨害および劣化を受けず
に油脂類中の水分濃度を直接、正確、安全、かつ経済的
に測定できて、油脂類中の水分濃度を所定濃度に効率よ
く安全かつ正確に制御させることができるという効果が
得られる。According to the present invention, the water concentration in fats and oils can be measured directly, accurately, safely, and economically without being affected or deteriorated by a solvent or the like, and the water concentration in fats and oils can be efficiently and safely maintained at a predetermined concentration. In addition, the effect of being able to control accurately is obtained.
また、水分濃度検出手段として、前記液相中水分濃度
センサのほかに、前記反応槽内の気相部の水分濃度を検
出する気相中水分濃度センサをも共用させることで、よ
り正確に油脂類中の水分濃度を制御させることができる
という効果が得られる。In addition, in addition to the water concentration sensor in the liquid phase, a water concentration sensor in the gas phase for detecting the water concentration in the gas phase in the reaction tank is also used as the water concentration detection means, so that the oil and fat can be more accurately detected. The effect that the water concentration in a kind can be controlled can be obtained.
さらに、水分濃度制御手段によって前記油脂溶液中に
不活性ガス曝気流量を制御することで、油脂溶液中の水
分濃度をより効率よく正確に低下させることができると
いう効果が得られる。Further, by controlling the aeration flow rate of the inert gas in the fat and oil solution by the moisture concentration control means, it is possible to obtain the effect that the moisture concentration in the fat and oil solution can be more efficiently and accurately reduced.
さらにまた、水分濃度制御手段によって前記油脂溶液
中の不活性ガス曝気流量と前記撹拌装置の回転数とを制
御することで、単独で前記油脂溶液中の不活性ガス曝気
流量を制御する場合よりさらに効率よく正確に低下させ
ることできるという効果が得られる。Further, by controlling the inert gas aeration flow rate in the fat and oil solution and the rotation speed of the stirrer by the water concentration control means, the inert gas aeration flow rate in the fat and oil solution alone is further controlled. The effect is obtained that the temperature can be efficiently and accurately reduced.
第１図は本発明の酵素による油脂類の反応における水分
自動制御方法を使用した水分自動制御反応装置の概略
図、第２図は第１図の装置における水分制御を示すフロ
ーチャート図、第３図は本発明の第１図の装置を使用し
た実施例における反応時間と反応系内の水分濃度あるい
は窒素ガス流量の相関関係を示す図、第４図は本発明の
第１図の装置を使用した実施例における水分濃度と露点
温度との関係を示す図である。 W;水、U;油脂溶液、F;不活性ガス 10;反応槽、30;撹拌部（撹拌装置） 50;水分濃度検出部（水分濃度検出手段） 51;溶液中水分指示計（液相中水分濃度センサ） 52;溶液温度指示計（液相中水分濃度センサ） 53;ガス体水分指示計（気相中水分濃度センサ） 54;ガス体温度指示計（気相中水分濃度センサ） 60;水分濃度制御部（水分濃度制御手段）FIG. 1 is a schematic diagram of an automatic moisture control reaction apparatus using an automatic moisture control method in the reaction of fats and oils with the enzyme of the present invention, FIG. 2 is a flowchart showing moisture control in the apparatus of FIG. 1, and FIG. FIG. 4 is a diagram showing the correlation between the reaction time and the water concentration in the reaction system or the flow rate of nitrogen gas in the embodiment using the apparatus of FIG. 1 of the present invention, and FIG. 4 uses the apparatus of FIG. 1 of the present invention. It is a figure which shows the relationship between the water concentration and dew point temperature in an Example. W; water, U; oil and fat solution, F; inert gas 10; reaction tank, 30; stirring section (stirring device) 50; moisture concentration detecting section (moisture concentration detecting means) 51; moisture indicator in solution (in liquid phase) 52; solution temperature indicator (moisture concentration sensor in liquid phase) 53; gas moisture indicator (moisture concentration sensor in vapor phase) 54; gas temperature indicator (moisture concentration sensor in vapor phase) 60; Moisture concentration control unit (moisture concentration control means)
Claims (5)
パーム油脂をエステル交換反応を行うにあたって、少な
くともパーム油脂溶液中の水分濃度を検出する液相中水
分濃度センサを含む水分濃度検出手段を用いて、前記パ
ーム油脂中の水分濃度を検出させ、前記水分濃度検出手
段で検出された検出信号に基づいて、水分濃度制御手段
により前記パーム油脂中の水分濃度を所定濃度に制御さ
せることを特徴とするリパーゼによるパーム油脂のエス
テル交換反応における水分自動制御方法。1. A method for transesterifying a palm oil or fat with a lipase in the presence of water in a reaction vessel, wherein at least a water concentration detecting means including a liquid phase water concentration sensor for detecting a water concentration in the palm oil solution is provided. The water concentration in the palm fat is detected by the water concentration detecting means, and the water concentration in the palm fat is controlled to a predetermined concentration by the water concentration controlling means based on the detection signal detected by the water concentration detecting means. Method for automatic control of water in transesterification of palm oil with lipase.
水分濃度センサのほかに、前記反応槽内の気相部の水分
濃度を検出する気相中水分濃度センサをも共用した特許
請求の範囲第１項記載のリパーゼによるパーム油脂のエ
ステル交換反応における水分自動制御方法。2. A water vapor concentration sensor for detecting a water concentration in a gas phase portion in the reaction tank in addition to the liquid water concentration sensor as the water concentration detecting means. 2. A method for automatically controlling moisture in a transesterification reaction of palm oil or fat with a lipase according to claim 1.
ために、前記パーム油脂溶液に水を供給する場合におい
て、前記水分濃度制御手段によって前記パーム油脂溶液
中の水分供給量を制御することで、前記パーム油脂中の
水分濃度を所定濃度に制御させた特許請求の範囲第１項
または第２項記載のリパーゼによるパーム油脂のエステ
ル交換反応における水分自動制御方法。3. The method according to claim 1, wherein when the water is supplied to the palm oil / fat solution in order to increase the water concentration in the palm oil / fat solution, the water supply amount in the palm oil / fat solution is controlled by the water concentration control means. 3. The method for automatically controlling moisture in a transesterification reaction of palm oil with lipase according to claim 1, wherein the moisture concentration in said palm oil is controlled to a predetermined concentration.
ために、前記パーム油脂溶液を不活性ガスで曝気させた
場合において、前記水分濃度制御手段によって前記パー
ム油脂溶液中の不活性ガス曝気流量を制御することで、
前記パーム油脂中の水分濃度を所定濃度に制御させた特
許請求の範囲第１項または第２項記載のリパーゼによる
パーム油脂のエステル交換反応における水分自動制御方
法。4. The method according to claim 1, wherein said palm oil / fat solution is aerated with an inert gas in order to reduce the water concentration in said palm oil / fat solution. By controlling
3. The method for automatically controlling moisture in a transesterification reaction of palm oil or fat with a lipase according to claim 1 or 2, wherein the concentration of moisture in the palm fat is controlled to a predetermined concentration.
ために、前記パーム油脂溶液を前記不活性ガスで曝気さ
せるとともに、撹拌装置で撹拌させた場合において、前
記水分濃度制御手段によって前記パーム油脂溶液中の不
活性ガス曝気流量と前記撹拌装置の回転数とを制御する
ことで、前記パーム油脂中の水分濃度を所定濃度に制御
させた特許請求の範囲第１項または第２項記載のリパー
ゼによるパーム油脂のエステル交換反応における水分自
動制御方法。5. When the palm oil / fat solution is aerated with the inert gas and agitated by a stirrer to reduce the moisture concentration in the palm oil / fat solution, the palm oil / fat is controlled by the water concentration control means. The lipase according to claim 1 or 2, wherein the concentration of water in the palm fat is controlled to a predetermined concentration by controlling the flow rate of aeration of the inert gas in the solution and the rotation speed of the stirring device. Method for automatic control of moisture in transesterification of palm oils and fats by HPLC.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP3564987A JP2622963B2 (en) | 1987-02-20 | 1987-02-20 | Automatic moisture control method in the reaction of fats and oils with enzymes |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP3564987A JP2622963B2 (en) | 1987-02-20 | 1987-02-20 | Automatic moisture control method in the reaction of fats and oils with enzymes |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPS63207393A JPS63207393A (en) | 1988-08-26 |
| JP2622963B2 true JP2622963B2 (en) | 1997-06-25 |
Family
ID=12447722
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP3564987A Expired - Fee Related JP2622963B2 (en) | 1987-02-20 | 1987-02-20 | Automatic moisture control method in the reaction of fats and oils with enzymes |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JP2622963B2 (en) |
Families Citing this family (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5204251A (en) * | 1987-05-11 | 1993-04-20 | Kanegafuchi Kagaku Kogyo & Kabushiki Kaisha | Process of enzymatic interesterification maintaining a water content of 30-300 ppm using Rhizopus |
| JPH02238886A (en) * | 1989-03-10 | 1990-09-21 | Kanegafuchi Chem Ind Co Ltd | Enzymatic reaction model of fats and oils in microorganism base and control of enzymatic reaction by same model |
| CN100347284C (en) * | 2005-05-20 | 2007-11-07 | 清华大学 | Airlift circulating reactor needing no foreign gas |
| EP2483614B1 (en) * | 2009-09-30 | 2020-06-24 | Global Life Sciences Solutions USA LLC | Disposable bioreactor condenser bag and filter heater |
-
1987
- 1987-02-20 JP JP3564987A patent/JP2622963B2/en not_active Expired - Fee Related
Also Published As
| Publication number | Publication date |
|---|---|
| JPS63207393A (en) | 1988-08-26 |
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