CN104099174A - Multiphase continuous separation method applicable to aqueous-phase oil extraction - Google Patents
Multiphase continuous separation method applicable to aqueous-phase oil extraction Download PDFInfo
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- CN104099174A CN104099174A CN201410329340.9A CN201410329340A CN104099174A CN 104099174 A CN104099174 A CN 104099174A CN 201410329340 A CN201410329340 A CN 201410329340A CN 104099174 A CN104099174 A CN 104099174A
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- water
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- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11B—PRODUCING, e.g. BY PRESSING RAW MATERIALS OR BY EXTRACTION FROM WASTE MATERIALS, REFINING OR PRESERVING FATS, FATTY SUBSTANCES, e.g. LANOLIN, FATTY OILS OR WAXES; ESSENTIAL OILS; PERFUMES
- C11B1/00—Production of fats or fatty oils from raw materials
- C11B1/10—Production of fats or fatty oils from raw materials by extracting
-
- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11B—PRODUCING, e.g. BY PRESSING RAW MATERIALS OR BY EXTRACTION FROM WASTE MATERIALS, REFINING OR PRESERVING FATS, FATTY SUBSTANCES, e.g. LANOLIN, FATTY OILS OR WAXES; ESSENTIAL OILS; PERFUMES
- C11B3/00—Refining fats or fatty oils
- C11B3/003—Refining fats or fatty oils by enzymes or microorganisms, living or dead
Abstract
The invention provides a multiphase continuous separation method applicable to aqueous-phase oil extraction. The method comprises the steps as follows: after crushing, alkaline extraction or enzymolysis is performed on oil materials, grease enters an aqueous phase to form a multiphase mixed system; after settlement is performed on the system, oil, emulsion and residue parts are layered; two-phase separation is performed on residues which settle at the lower layer and contain a few aqueous phase, the residues and the aqueous phase are obtained, and two-phase separation is performed on the obtained aqueous phase again to obtain an emulsion and the aqueous phase; three-phase separation is performed on the oil, the emulsion and part of the aqueous phase which settle at the upper layer to obtain edible vegetable oil, the aqueous phase and a few emulsion; enzymatic demulsification is performed on the emulsions obtained at the upper layer and the lower layer together, and then two-phase centrifugal separation is performed to obtain the edible vegetable oil and the aqueous phase. According to the method, multiphase continuous efficient separation is realized, the edible vegetable oil, the aqueous phase, the emulsion phase and the residues are obtained, enzymatic demulsification and centrifugal separation are performed on the emulsion to further recover the edible vegetable oil, the total oil extraction rate is increased to 90%, and the protein extraction rate is up to 87%.
Description
Technical field
The invention belongs to edible oil separation and extraction technology field, relate in particular to a kind of water that is applicable to and carry oily heterogeneous continuous separation method.
Background technology
Vegetable oil material is the important grease of the mankind and vegetable-protein source.But, the complete processing of the existing squeezing of China's grease, leaching or the two combination, often violent because of processing conditions, destroy protein and other nutritive ingredients, reduce the utilization ratio of oil resource or the economy of complete processing.Meanwhile, taking leaching solvent as main oil extracting process and supporting refinery practice, there is the outstanding problems such as potential Product quality and safety and production environment pollution equivalent risk and utilization of resources comprehensive effectiveness are low.
The water such as water substitution, aqueous enzymatic method method is as a kind of novel oil extracting methods, it is taking machinery and enzymolysis as means destruction plant cell wall, in leaching process without the need for machine solvent, the operations such as the grease extracting does not need to come unstuck, deodorizing, whole production process is carried out under relative low temperature (not higher than 85 DEG C), reduce energy expenditure and investment and production cost, and prevented the formation of the objectionable impurities such as benzopyrene and trans fatty acid.In addition, in extracting grease, protein (or its hydrolysate) and carbohydrate in energy efficient recovery raw material.Therefore the water law technology such as aqueous enzymatic method has obtained paying close attention to widely, especially for the oil plant of high innage albumen if peanut, walnut, sesame and the high oil mass oil plant that is rich in other functional components are as oil tea.Its Patent CN1419837A has reported that one utilizes prozyme (cellulase, polygalacturonase and neutral protease) to extract the method for peanut oil and Semen arachidis hypogaeae protein, and grease yield is 94-96%, and protein yield is 73-75%.2005, Wang Yingyao utilized aqueous enzymatic method to extract peanut grease and protolysate simultaneously, and the milk sap generating in technique has been carried out property analysis and abolished research, and result shows that the highest yield of grease and protolysate reaches respectively 92.2% and 82.5%.2006, Hua Di etc. adopted Alcalase hydrolysis peanut, can extract 79.32% free oil and 71.38% protolysate by a step enzyme digestion reaction.Slag to technique gained and milk sap, select neutral protease As1398 to carry out secondary enzymolysis, and final total free oil yield can reach 91.98%, and total yield of aminosal can reach 88.21%.Except peanut, patent CN101906350A adopts polygalacturonase from camellia seed kernel, to extract grease, and reclaims saponin(e and glucide simultaneously.Patent CN102061217A adopts one or more prozymes in cellulase, amylase, proteolytic enzyme, polygalacturonase to carry out aqueous enzymatic method and carries oil.Although traditional aqueous enzymatic method obtains relatively high grease and protein extracting ratio, due to a large amount of uses of enzyme, production cost is increased, and protein become bitter peptides by enzymolysis, apply limited.Emerging water method because of mainly taking water as extract solvent, enzyme in a small amount makes to obtain not by the peanut protein isolate of enzymic hydrolysis in obtaining high oil fat extraction yield for the breakdown of emulsion of milk sap, and the consumption of enzyme reduces greatly, production cost reduces, and substituting traditional aqueous enzymatic method technique becomes the focus of current research.Wherein Zhu Kai is gorgeous waits people to adopt water substitution to extract grease and the isolated protein in peanut simultaneously, grease extraction rate reached is to 88% left and right, the people such as Liu Miao also adopt water method to extract the grease in walnut, and oil extracting rate reaches 90% left and right, and successfully prepare Walnut Milk with the water of getting after oil.The people such as Li Qiang extract grease and the tea saponin in tea seed with ethanol auxiliary water enzyme process simultaneously, the extraction rate reached 90% of tea-seed oil.
But no matter be water substitution, aqueous enzymatic method or ethanol auxiliary water enzyme process, in oil plant leaching process, the problem of the heterogeneous difficulty or ease high efficiency separation such as oil, water, slag is restricting the further industrialized development of this technique always.In vitro lab scale experiment is also limited in the research of aqueous enzymatic method at present, and multi-phase separation also adopts compact centrifuge to carry out separating for several times mostly, and efficiency is low, and cannot carry out continuously at all.Patent CN101401658A once carried out centrifugal with three-phase centrifuge to the enzymatic hydrolysis system in aqueous enzymatic method pilot process, obtain edible vegetable oil, oil-water mixture and residue three parts, again by oil-water mixture through butterfly centrifugal machine centrifugal two portions, a part is oil and milk sap, another part is hydrolyzed solution.Again by oil and standing edible vegetable oil and the milk sap of obtaining of milk sap.But the residue obtained middle fat residue rate of this centrifuging process is higher, and in hydrolyzed solution, fat content is higher, percent of total oil is only 73.77%, and yield of aminosal is only 55.10%.
Summary of the invention
The object of the present invention is to provide a kind of heterogeneous continuous separation method that is applicable to water and carries oil, be intended to solve the water methods such as water substitution, aqueous enzymatic method and ethanol auxiliary water enzyme process and put forward the problem of extensive high-efficiency and continuous separation and Extraction grease, protein or other functional mass difficulties in oily process.
The present invention be achieved in that a kind of be applicable to water carry oil heterogeneous continuous separation method, comprise the following steps:
(1) after oil plant is pulverized, carry out that alkali is carried or enzymolysis, grease enters water, forms the three-phase mixture system that comprises oil, water, milk sap, residue;
(2) this system is being incubated after sedimentation 0.5-4h at 30-80 DEG C of temperature to oil, milk sap and the layering of slag part;
(3) utilize Horizontal helical type centrifuge to carry out two the residue that contains a small amount of water of sedimentation lower floor and be separated, obtain residue and water, then the water obtaining is carried out to two through disk plate centrifuge again and be separated, obtain milk sap and water in a small amount;
(4) adopt disc centrifuge to carry out three phase separation the oil on sedimentation upper strata, milk sap and part water, obtain edible vegetable oil, water and a small amount of milk sap;
(5) the upper and lower are separated to the milk sap obtaining and carry out in the lump enzyme process breakdown of emulsion, then adopt disc centrifuge to carry out two-phase centrifugation, obtain edible vegetable oil and water.
Preferably, in step (1), described alkali is carried or enzymolysis is specially: the oil plant after pulverizing is fed intake by certain material-water ratio, mixed system is stirred, stirring velocity is turn/min of 50-300, temperature of reaction is adjusted to 30-80 DEG C, in the time that temperature of reaction reaches requirement simultaneously, the pH value of system is adjusted to 7.5-10 and carries out alkali and carry or add proteolytic enzyme or/and combinative enzyme hydrolysis cell wallss such as amylase or/and cellulases, discharge grease.
Preferably, in step (3), described horizontal helical type is centrifugal to be specially: the residue of sedimentation lower floor and water are undertaken to two by Horizontal helical type centrifuge and be separated, obtain residue and water; Wherein, the sleeping centrifugal rotating speed of spiral shell is turn/min of 2000-5000.
Preferably, in step (4), described disc-type is centrifugal to be specially: the oil on sedimentation upper strata, milk sap and part water are carried out to three phase separation by disc centrifuge, obtain edible vegetable oil, water and a small amount of milk sap; Wherein, the rotating speed of disc centrifuge is turn/min of 4000-8000.
Preferably, in step (5), described enzyme process breakdown of emulsion is specially: the upper and lower are separated to the milk sap obtaining and mix with water according to a certain percentage, stirring velocity is turn/min of 30-300, temperature of reaction is adjusted to 30-80 DEG C, pH value is adjusted to 3-10, then adds 0.01-2.5% proteolytic enzyme to carry out enzyme process breakdown of emulsion, and 0.5-4h is carried out in reaction; Described disc centrifuge two-phase centrifugation is reclaimed in the process of edible vegetable oil, and the rotating speed of disc centrifuge is turn/min of 4000-8000.
The present invention is directed to water substitution, the water methods such as aqueous enzymatic method and ethanol auxiliary water enzyme process are extracted grease in oil plant simultaneously, in protein or other functional mass processes, oil, water, the heterogeneous key issue that is difficult to high efficiency separation such as slag, conversion conventional thought, provide a kind of water that is applicable to carry oily heterogeneous continuous separation method, system after first extraction being finished is incubated after the sedimentation regular hour at a certain temperature, residue in lower floor after sedimentation is carried out to sufficient separate by slag with water by Horizontal helical type centrifuge with part water, the water obtaining is carried out to video disc separation, obtain a small amount of milk sap and water.Oil, milk sap and water after selecting disc centrifuge to sedimentation in upper strata carry out three phase separation again, obtain edible vegetable oil, water and a small amount of milk sap; The milk sap obtaining is carried out to enzyme process breakdown of emulsion, then adopt disc centrifuge to carry out two-phase centrifugation, obtain edible vegetable oil and water.The present invention realizes heterogeneous continuous high-efficient and separates, and obtains edible vegetable oil, water, and emulsus liquid phase and residue, milk sap, through enzyme process breakdown of emulsion, centrifugation, further reclaims edible vegetable oil.In this experiment, percent of total oil brings up to 90%, and protein extracting ratio, also up to 87%, has further advanced water method to carry oily industrialization development.
Embodiment
In order to make object of the present invention, technical scheme and advantage clearer, below in conjunction with embodiment, the present invention is further elaborated.Should be appreciated that specific embodiment described herein, only in order to explain the present invention, is not intended to limit the present invention.
Embodiment 1
(1) 100kg is peeled peanut raw material, purchased from From Shandong Rizhao, after pulverizing, feed intake by 1:6 material-water ratio, mixed system is stirred, stirring velocity is 200 turn/min, temperature of reaction is adjusted to 50 DEG C simultaneously, in the time that temperature of reaction reaches requirement, the pH value of system is adjusted to 10 and carries out alkali and carry 4h, obtain the system of oil, water, milk sap, the heterogeneous mixing of residue;
(2) this system is incubated after sedimentation 1.5h at 70 DEG C of temperature to oil, milk sap and the layering of slag part;
(3) utilize Horizontal helical type centrifuge to carry out two with 3500 turn/min the residue that contains a small amount of water of sedimentation lower floor and be separated, obtain residue and water; And it is centrifugal that the water obtaining is carried out to disc-type with 7000 turn/min, obtains milk sap and water; The milk sap oleaginousness wherein obtaining accounts for 14.80% of total oil content amount, and in the water of acquisition, oil-contg and protein content account for respectively in raw material separately 1.80% of total amount and 57.53%.The oleaginousness of slag phase and protein content account for respectively in raw material separately 2.86% of total amount and 12.87%.
(4) adopt disc centrifuge to carry out three phase separation with 7000 turn/min the oil on sedimentation upper strata, milk sap and part water, obtain edible vegetable oil, water and a small amount of milk sap.Wherein edible vegetable oil yield is 77.33% of raw material total oil content, and in water, oil and protein content account for respectively in raw material separately 3.38% of total amount and 29.73%, and milk sap oil-containing is 0.80% of raw material oleaginousness.
(5) the upper and lower are separated to the milk sap obtaining and carry out in the lump enzyme process breakdown of emulsion, milk sap mixes with water according to a certain percentage, stirring velocity is 100 turn/min, temperature of reaction is adjusted to 50 DEG C, pH value is adjusted to 7.5, and adds 0.8% proteolytic enzyme to carry out enzymolysis 2h, then utilizes disc centrifuge to separate taking rotating speed as 7000 turn/min, obtain edible vegetable oil and water, edible vegetable oil yield is 12.87% of raw material total oil content.Finally after breakdown of emulsion, obtaining total edible vegetable oil yield is 90.20% of raw material oil-containing, and extraction rate of protein is 87.26% of material protein content.Wherein, edible vegetable oil yield (%) and extraction rate of protein (%) can calculate by following formula:
Than the shortcoming and defect of prior art, the present invention has following beneficial effect: the present invention is in auxiliary water method is extracted oil plant simultaneously in grease, protein or other functional mass processes, solve the key issue of the heterogeneous difficulty or ease high efficiency separation such as oil, water, slag, realize heterogeneous high efficiency separation, obtain edible vegetable oil, water, emulsus liquid phase and residue, in examination experiment, percent of total oil brings up to 90%, and protein extracting ratio, also up to 87%, has further advanced water method to carry oily industrialization development.
The foregoing is only preferred embodiment of the present invention, not in order to limit the present invention, all any amendments of doing within the spirit and principles in the present invention, be equal to and replace and improvement etc., within all should being included in protection scope of the present invention.
Claims (5)
1. be applicable to water and carry a heterogeneous continuous separation method for oil, it is characterized in that, comprise the following steps:
(1) after oil plant is pulverized, carry out that alkali is carried or enzymolysis, grease enters water, forms the three-phase mixture system that comprises oil, water, milk sap, residue;
(2) this system is being incubated after sedimentation 0.5～4h at 30～80 DEG C of temperature to oil, milk sap and the layering of slag part;
(3) utilize Horizontal helical type centrifuge to carry out two the residue that contains a small amount of water of sedimentation lower floor and be separated, obtain residue and water, then the water obtaining is carried out to two through disk plate centrifuge again and be separated, obtain milk sap and water in a small amount;
(4) adopt disc centrifuge to carry out three phase separation the oil on sedimentation upper strata, milk sap and part water, obtain edible vegetable oil, water and a small amount of milk sap;
(5) the upper and lower are separated to the milk sap obtaining and carry out in the lump enzyme process breakdown of emulsion, then adopt disc centrifuge to carry out two-phase centrifugation, obtain edible vegetable oil and water.
2. the water that is applicable to as claimed in claim 1 is carried oily heterogeneous continuous separation method, it is characterized in that, in step (1), described alkali is carried or enzymolysis is specially: the oil plant after pulverizing is fed intake by certain material-water ratio, mixed system is stirred, stirring velocity is 50～300 turn/min, temperature of reaction is adjusted to 30～80 DEG C simultaneously, in the time that temperature of reaction reaches requirement, the pH value of system is adjusted to 7.5～10 and carries out alkali and carry or add proteolytic enzyme or/and combinative enzyme hydrolysis cell wallss such as amylase or/and cellulases, discharge grease.
3. the water that is applicable to as claimed in claim 2 is carried oily heterogeneous continuous separation method, it is characterized in that, in step (3), described horizontal helical type is centrifugal to be specially: the residue of sedimentation lower floor and water are undertaken to two by Horizontal helical type centrifuge and be separated, obtain residue and water; Wherein, the sleeping centrifugal rotating speed of spiral shell is 2000～5000 turn/min.
4. the water that is applicable to as claimed in claim 3 is carried oily heterogeneous continuous separation method, it is characterized in that, in step (4), described disc-type is centrifugal to be specially: the oil on sedimentation upper strata, milk sap and part water are carried out to three phase separation by disc centrifuge, obtain edible vegetable oil, water and a small amount of milk sap; Wherein, the rotating speed of disc centrifuge is 4000～8000 turn/min.
5. the water that is applicable to as claimed in claim 4 is put forward the oil recovery method in the milk sap obtaining in oil, it is characterized in that, in step (5), described enzyme process breakdown of emulsion is specially: the upper and lower are separated to the milk sap obtaining and mix with water according to a certain percentage, stirring velocity is 30～300 turn/min, and temperature of reaction is adjusted to 30～80 DEG C, and pH value is adjusted to 3～10, then add 0.01～2.5% proteolytic enzyme to carry out enzyme process breakdown of emulsion, 0.5～4h is carried out in reaction; Described disc centrifuge two-phase centrifugation is reclaimed in the process of edible vegetable oil, and the rotating speed of disc centrifuge is 4000～8000 turn/min.
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| CN201410329340.9A CN104099174A (en) | 2014-07-10 | 2014-07-10 | Multiphase continuous separation method applicable to aqueous-phase oil extraction |
| CN201710145527.7A CN106833882A (en) | 2014-07-10 | 2014-07-10 | A kind of multiphase continuous separation method that oil is mutually carried suitable for water |
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104431358A (en) * | 2014-11-28 | 2015-03-25 | 国家粮食局科学研究院 | System and method for treating liquid phase obtained in process course of extracting camellia oleosa seed oil by adopting aqueous enzymatic method |
| CN104479854A (en) * | 2014-11-27 | 2015-04-01 | 江南大学 | Method for extracting peanut oil and peanut protein simultaneously |
| CN104745287A (en) * | 2015-03-17 | 2015-07-01 | 吉林农业大学 | Extracting method for ginseng seed oil |
| CN105623833A (en) * | 2015-09-16 | 2016-06-01 | 华侨大学 | Demulsification treatment method for aqueous enzymatic method extracted tea seed oil |
| CN105925368A (en) * | 2016-06-13 | 2016-09-07 | 江南大学 | Method for preparing walnut oil by performing emulsion breaking on walnut oil body by water method |
| CN115812841A (en) * | 2022-12-14 | 2023-03-21 | 中国农业科学院农产品加工研究所 | Method for efficiently and synchronously separating oil and protein in peanut oil aqueous enzymatic preparation |
Families Citing this family (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109233993A (en) * | 2018-11-09 | 2019-01-18 | 黛君本草生命科技（深圳）有限公司 | A kind of preparation process of rice bran oil |
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104479854A (en) * | 2014-11-27 | 2015-04-01 | 江南大学 | Method for extracting peanut oil and peanut protein simultaneously |
| CN104431358A (en) * | 2014-11-28 | 2015-03-25 | 国家粮食局科学研究院 | System and method for treating liquid phase obtained in process course of extracting camellia oleosa seed oil by adopting aqueous enzymatic method |
| CN104745287A (en) * | 2015-03-17 | 2015-07-01 | 吉林农业大学 | Extracting method for ginseng seed oil |
| CN105623833A (en) * | 2015-09-16 | 2016-06-01 | 华侨大学 | Demulsification treatment method for aqueous enzymatic method extracted tea seed oil |
| CN105925368A (en) * | 2016-06-13 | 2016-09-07 | 江南大学 | Method for preparing walnut oil by performing emulsion breaking on walnut oil body by water method |
| CN105925368B (en) * | 2016-06-13 | 2019-08-30 | 油谷生物科技南京有限公司 | A method of walnut oil is prepared by water law demulsification walnut oil body |
| CN115812841A (en) * | 2022-12-14 | 2023-03-21 | 中国农业科学院农产品加工研究所 | Method for efficiently and synchronously separating oil and protein in peanut oil aqueous enzymatic preparation |
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| CN106833882A (en) | 2017-06-13 |
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Application publication date: 20141015 |