CN115125062A - Soybean oil pretreatment process suitable for physical refining and application - Google Patents
Soybean oil pretreatment process suitable for physical refining and application Download PDFInfo
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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
- C11B3/00—Refining fats or fatty oils
- C11B3/001—Refining fats or fatty oils by a combination of two or more of the means hereafter
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- A—HUMAN NECESSITIES
- A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
- A23D—EDIBLE OILS OR FATS, e.g. MARGARINES, SHORTENINGS, COOKING OILS
- A23D9/00—Other edible oils or fats, e.g. shortenings, cooking oils
- A23D9/02—Other edible oils or fats, e.g. shortenings, cooking oils characterised by the production or working-up
- A23D9/04—Working-up
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- 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
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- 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
- C11B3/10—Refining fats or fatty oils by adsorption
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Abstract
The invention relates to a soybean oil pretreatment process suitable for physical refining and application, and belongs to the technical field of edible oil processing. Firstly, preparing phospholipase A1 and phospholipase C into compound enzyme solution, adding the compound enzyme solution into crude oil, then carrying out catalysis degumming on the crude oil by a double-phospholipid enzyme method by adopting an ultrasonic wave auxiliary technology, drying the degummed soybean oil, and removing main color-producing substances and impurities by adopting alkaline clay, wherein part of free fatty acid is also effectively removed in the process. The soybean crude oil is subjected to double-enzyme degumming and alkaline clay decoloring treatment based on the process, and the process parameters are optimized to obtain the grease with higher quality and more suitable for physical refining, so that the physical refining difficulty and the energy consumption in a vacuum distillation stage are reduced, meanwhile, the whole process is short in time consumption and low in water consumption, and the production cost is greatly reduced.
Description
Technical Field
The invention relates to a soybean oil pretreatment process suitable for physical refining and application, and belongs to the technical field of edible oil processing.
Background
The traditional chemical refining process of soybean oil is to carry out degumming, deacidification, decoloration and other processes on leached or squeezed crude soybean oil to obtain the finished product of soybean oil. Generally speaking, crude oil degumming is the first procedure in the oil refining process, incomplete degumming causes large loss of subsequent refined oil, increases the burden of the subsequent refining procedure, and also has adverse effects on processing equipment, such as difficult filtration, equipment coking, increase of clay consumption and the like; meanwhile, the high phosphorus content in the finished oil is accompanied by more metal ions, which can cause the bad phenomena of acid return, color reversion and the like of the finished oil. Deacidification and decolorization are steps after degumming, which mainly remove free fatty acids, pigments, and residual trace phospholipid components from the oil. Because the mechanisms for deacidifying and decoloring fats and oils are different, the operating processes are also significantly different. The conventional deacidification process, also called an alkali refining process, is to add alkali liquor to grease to neutralize free fatty acid in the grease, and remove the formed soapstock by centrifugation. The decolorization is carried out by adding decolorizer into neutralized oil, mixing with grease, staying reacting, and filtering. A large amount of alkali liquor is consumed in the deacidification process, and the loss of neutral oil mainly occurs in the section, so that the traditional chemical refining process of soybean oil is contrary to the call of energy conservation, consumption reduction, quality improvement and loss reduction in the oil and fat industry.
The physical refining of fats and oils generally refers to only a process of removing free fatty acids and odor components from fats and oils by steam distillation in a vacuum state. Compared with chemical refining, the method has the advantages of good physical refining effect, low consumption of acid-base auxiliaries, environmental friendliness, basically no neutral oil loss and very remarkable advantage in producing high-quality salad oil. However, how to adopt a pretreatment process with shorter time consumption and lower water consumption to obtain the grease more suitable for physical refining so as to reduce the refining difficulty and the energy consumption in a vacuum distillation stage is a technical problem to be solved urgently in the grease industry at present.
Disclosure of Invention
The technical problem is as follows:
adopts a pretreatment process with shorter time consumption and lower water consumption to obtain grease more suitable for physical refining so as to reduce the refining difficulty and the energy consumption in a vacuum distillation stage.
The technical scheme is as follows:
the invention aims to provide a soybean oil pretreatment process suitable for physical refining, which sequentially comprises the following steps of:
(1) preheating the crude soybean oil;
(2) adjusting the pH value of the crude soybean oil obtained in the step (1) to 5-7; shearing at a high speed; stirring at constant speed under heating to condition the crude soybean oil;
(3) fully dissolving and mixing phospholipase A1 (lipase Ultra), phospholipase C and water, shearing at high speed, and hydrating to obtain compound enzyme solution; wherein the enzyme activity of the phospholipase A1 (leucine Ultra) is 10U/mg, the enzyme activity of the phospholipase C is 30U/mg, and the phospholipase A1 (leucine Ultra) and the phospholipase C are added in equal proportion; the water addition amount is 3 to 5 percent of the weight of the crude soybean oil obtained in the step (2); shearing the compound enzyme liquid and the crude soybean oil obtained in the step (2) at a high speed, wherein the mass ratio of the compound enzyme liquid to the crude soybean oil obtained in the step (2) is 4-6 g/kg, and then carrying out ultrasonic-assisted double-enzyme degumming reaction in a water bath environment at 50-60 ℃, wherein the ultrasonic-assisted power is 60-80 kHz, and the ultrasonic-assisted double-enzyme degumming reaction time is 35-60 min;
(4) after degumming, inactivating enzyme, cooling to room temperature, centrifuging to remove phospholipid, taking oil phase, and drying to obtain soybean degumming oil by double-enzyme method;
(5) activating alkaline clay; mixing the activated alkaline clay with the double-enzyme method soybean degumming oil obtained in the step (4) according to the proportion of 2-3% of the mass of the degumming oil, and heating and stirring under negative pressure to carry out a decolorization reaction; cooling and filtering to obtain the soybean oil suitable for subsequent physical refining.
In a preferred embodiment of the present invention, in the step (5), the vacuum degree of the negative pressure of the decolorization reaction is-0.095 to-0.090 MPa, the heating temperature is 95 ℃, the stirring rate is 120 to 150r/min, and the time of the decolorization reaction is 15 to 20 min. The decoloring reaction time is preferably 15 min.
In a preferred embodiment of the invention, in the step (3), the mass ratio of the compound enzyme liquid to the crude soybean oil obtained in the step (2) is 5 g/kg; the shearing rate is 10000 r/min, and the shearing time is 1 min.
In a preferred embodiment of the present invention, in step (3), the water bath temperature of the ultrasonic-assisted two-enzyme degumming reaction is 50 ℃; the ultrasonic-assisted double-enzyme degumming reaction time is 45 min.
As a preferred embodiment of the invention, the crude soybean oil is prepared by squeezing or leaching, and the crude soybean oil is subjected to settling and filtration for impurity removal.
As a preferred embodiment of the present invention, the pH of the crude soybean oil is adjusted by adding citric acid in step (2); the citric acid is of analytical grade and meets the use requirement of food additives.
In the step (2), the concentration of the citric acid solution is 45%, and the pH value of the crude soybean oil obtained in the step (1) is adjusted to 6; the shearing rate of high-speed shearing is 15000 r/min, and the shearing time is 3 min; the tempering temperature is 55 ℃, the stirring speed is 80r/min, and the stirring time is 30 min.
In a preferred embodiment of the present invention, the alkaline clay is a food additive and satisfies the requirements for use in foods.
As a preferred embodiment of the invention, the preheating temperature of the crude soybean oil in the step (1) is 70-80 ℃.
In a preferred embodiment of the present invention, the enzyme deactivation temperature in step (4) is above 90 ℃ and the enzyme deactivation time is 5 min; the centrifugal speed is 6000r/min, and the centrifugal time is 15 min.
As a preferred embodiment of the present invention, in the step (4), the oil phase drying conditions are as follows: the drying temperature is 140 ℃, the vacuum degree of the drying environment is-0.095 to-0.090 MPa, and the drying time is 40 min.
In a preferred embodiment of the present invention, the conditions for activating the alkaline clay in step (5) are: the activation temperature is 105 ℃, the activation time is 1.5-2.5 h, and the dryer is cooled to the room temperature after the activation.
In a preferred embodiment of the present invention, the grease in step (5) is cooled to a vacuum degree of-0.095 to-0.090 MPa, and then vacuum filtered after cooling to 60 ℃.
The second purpose of the invention is to provide the application of the process in the production of high-grade edible soybean salad oil.
Has the beneficial effects that:
(1) the invention provides a preparation method of soybean oil suitable for physical refining, which comprises the steps of completely dissolving and mixing phospholipase A1 (lipase Ultra) and phospholipase C in distilled water, completely hydrating to completely develop an enzyme structure, adding the enzyme structure into crude soybean oil, carrying out double-phospholipid enzymatic catalytic degumming by adopting an ultrasonic auxiliary technology, drying the degummed soybean oil, and removing main coloring substances and impurities by adopting alkaline clay, wherein part of free fatty acid is effectively removed in the process. The invention adopts the compound enzyme enzymatic degumming process to avoid twice addition and twice reaction of degumming enzyme, simplifies the degumming process, shortens the degumming time, reduces the single enzyme dosage and the water consumption, and simultaneously reduces the generation of waste water; after the degummed oil is dried, activated alkaline clay is directly adopted for decolorization treatment, trace phospholipid is further removed, the color is improved, the content of free fatty acid is reduced to a certain degree, the processing pressure and the energy consumption of a vacuum water vapor distillation stage in subsequent physical refining can be effectively reduced by the prepared soybean oil, the method is more suitable for distillation physical refining, the process processing chain is short, simple and efficient, and the method is more beneficial to producing high-quality edible soybean oil.
(2) Compared with the traditional processes of enzymatic degumming, alkali refining deacidification, adsorption decoloration and the like of soybean oil, the method has the following outstanding beneficial effects: firstly, twice addition of degumming enzyme and twice reaction are avoided, the degumming process is simplified, the degumming time is shortened, the single enzyme consumption and the water consumption are reduced, and the generation of waste water is reduced; secondly, after the enzyme-method degummed oil is subjected to vacuum drying, the enzyme-method degummed oil is directly added with alkaline clay for treatment without an alkaline refining deacidification process, so that color-producing substances, trace phospholipids and other impurities in the oil are removed, the alkali consumption is effectively reduced in the process, and neutral oil loss and wastewater generation caused by the deacidification process are avoided; and meanwhile, due to the use of the alkaline clay, part of free fatty acid is brought out, and the acid value of the oil can be effectively reduced. In conclusion, the process disclosed by the invention is shorter in time consumption and lower in water consumption, and the grease which is higher in quality and more suitable for physical refining is obtained, so that the physical refining difficulty and the energy consumption in a vacuum distillation stage are reduced.
(3) The process combines distillation physical refining, and is more beneficial to producing high-grade edible soybean salad oil.
Drawings
FIG. 1 is a process flow diagram of a process for making soybean oil suitable for physical refining in accordance with the present invention.
Detailed Description
In order that those skilled in the art will better understand the technical solutions of the present invention, the present invention will be described in further detail with reference to the following embodiments.
Direct sources of materials (including biomaterials) referred to in the examples and comparative examples:
phospholipase a1(Lecitase Ultra): the enzyme activity of a commercial enzyme preparation product purchased by Novexin China company is 10U/mg;
phospholipase C: the enzyme activity of a commercial enzyme preparation product purchased by Shanghai-sourced leaf Biotechnology limited is 30U/mg;
crude soybean oil: leaching with petroleum ether, and removing solvent to obtain crude soybean oil; settling, filtering and impurity removing steps are finished on the crude soybean oil;
alkaline clay: purchased from national star attapulgite Limited of Mingguang city (particle size is more than or equal to 200 meshes, water content is less than 8%);
activated clay: purchased from national star attapulgite limited of Mingguang city (particle size is more than or equal to 200 meshes, water content is less than 8%).
Example 1
Carrying out double-enzyme degumming and alkaline clay decoloring treatment on the crude soybean oil sequentially according to the following steps:
(1) preheating 500g of crude soybean oil at 70-80 ℃;
(2) slowly adding a 45% citric acid solution into the soybean crude oil obtained in the step (1), and stirring while adding to adjust the pH of the system to 6.0; shearing at high speed of 15000 r/min for 3 min; stirring at 55 deg.C and 80r/min for 30min to condition crude soybean oil;
(3) fully mixing and dissolving 0.1g of phospholipase A1(Lecitase Ultra), 0.1g of phospholipase C powder and 20g of deionized water, shearing for 1min at 10000 r/min, and hydrating to obtain a compound enzyme solution;
(4) shearing the crude soybean oil obtained in the step (2) and 2.5g of the compound enzyme liquid obtained in the step (3) at a high speed for 1min at a rotating speed of 10000 r/min; then carrying out ultrasonic-assisted double-enzyme degumming for 45min at the temperature of 50 ℃ and the ultrasonic-assisted power of 60 kHz;
(5) after the degumming, adjusting the temperature of the system to 90 ℃, and incubating for 5 min; then standing and cooling to room temperature, and centrifuging at the rotating speed of 6000r/min for 15min to remove phospholipid; drying the obtained grease for 40min at the temperature of 140 ℃ and the vacuum degree of-0.095 to-0.090 MPa to obtain the soybean degummed oil by the double-enzyme method;
(6) baking the alkaline clay for 1.5-2.5 hours at 105 ℃ to activate the alkaline clay; then taking out and cooling to room temperature in a dryer; adding the activated alkaline clay into the double-enzyme method soybean degummed oil obtained in the step (5) according to the proportion of 2% of the mass of the degummed oil, heating to 95 ℃ under the vacuum degree of-0.095 to-0.090 MPa, and stirring for decolorization reaction for 15min at 120-150 r/min;
(7) after the decolorization reaction is finished, the soybean oil is continuously cooled to 60 ℃ under the vacuum degree of-0.095 to-0.090 MPa, and then is subjected to vacuum filtration to obtain the soybean oil suitable for physical refining.
Example 2
Referring to example 1, the only difference is that the dosage of the enzyme complex enzyme solution in step (4) is reduced, but the ultrasonic-assisted two-enzyme degumming time is slightly prolonged, specifically:
in the step (4), the dosage of the enzyme complex enzyme solution is adjusted to be 2.0g, and the degumming time of the ultrasonic-assisted double-enzyme method is adjusted to be 60 min.
Example 3
Referring to example 1, the difference is only that the dosage of the enzyme complex enzyme solution in the step (4) is increased, but the ultrasonic-assisted two-enzyme degumming time is slightly shortened, specifically:
in the step (4), the dosage of the enzyme complex enzyme solution is adjusted to be 3.0g, and the degumming time of the ultrasonic-assisted double-enzyme method is adjusted to be 35 min.
Example 4
Referring to example 1, the differences are only that the pH value of the system in step (2) is slightly increased (the amount of citric acid is reduced), the enzymolysis temperature in step (4) is slightly increased, and the ultrasonic-assisted two-enzyme degumming time is prolonged, specifically:
adjusting the pH value of the system to 7.0 in the step (2);
the enzymolysis temperature in the step (4) is adjusted to 60 ℃, and the ultrasonic-assisted double-enzyme degumming time is adjusted to 60 min.
Example 5
Referring to example 1, the only difference is that the amount of alkaline clay used in step (6) is increased to slightly decrease the decolorization reaction time, specifically:
in the step (6), the dosage of the alkaline clay is adjusted to be 3% of the mass of the degummed oil, and the decoloring reaction time is adjusted to be 10 min.
Experimental example 1
The soybean oil suitable for physical refining prepared in the examples 1-5 is respectively subjected to a heating test, measurement of phospholipid, peroxide value, acid value and color and luster by the methods in GB/T5531-2018 test plant oil heating test, measurement of phospholipid content in GB/T5537-2008 test food and oil, measurement of peroxide value in GB 5009.227-2016 food safety national standard food, measurement of acid value in GB 5009.229-2016 food safety national standard food and measurement of color and luster of GB/T22460 2008 animal plant oil and oil lovibond, and the measurement and calculation results are shown in Table 1:
TABLE 1
Injecting:
(1) the luvibond colorimetric method is adopted to measure the color of the grease, and a 133.4mm standard glass colorimetric groove is adopted;
(2) in the same example, "sample 1" and "sample 2" in the table represent the two-enzyme method soybean degummed oil obtained in step (5) and the alkaline clay-decolorized oil obtained in step (7) in this example (i.e., soybean oil and fat suitable for physical refining), respectively;
(3) in the table, "Y" and "R" represent a yellow value and a red value, respectively.
As can be seen from table 1, the soybean oil phospholipid content after the soybean oil crude oil is treated by the process of the present invention (sample 2 in table 1) is lower than 5mg/kg, indexes such as acid value, peroxide value, color and luster of the oil are significantly improved, the removal effect of phospholipid, free fatty acid and color and luster is proved to be improved, the problems of incomplete degumming, unstable key indexes such as acid value, peroxide value and the like of the oil in the current common process are solved, and the quality assurance of the raw material is provided for the subsequent production of high-grade edible salad oil by further adopting a physical refining means.
As can be seen from the results of performance tests comparing the two-enzyme method degummed soybean oil obtained in step (5) and the alkaline clay decolorized oil obtained in step (7) in each example, after the alkaline clay decolorization steps of steps (6) to (7) are omitted, the phospholipid content of the prepared two-enzyme method degummed soybean oil (sample 1 in table 1) is greater than 5mg/kg, the color is darker, the acid value and peroxide number are higher than those of the prepared two-enzyme method degummed soybean oil (sample 2 in table 1), which indicates that the quality is inferior to that of sample 2, which indicates that the alkaline clay decolorization steps of steps (6) to (7) are omitted, the phospholipid cannot be removed well, the acid value is reduced, the oil quality is improved, the difficulty in the subsequent steam distillation process is increased, and the alkaline clay decolorization steps of steps (6) to (7) are proved to be very important.
To further highlight the improved effect of the present invention compared to the prior art, the time and water consumption required for the conventional degumming, deacidification and decolorization processes were counted and compared with the present invention process, and the comparison results are shown in table 2:
TABLE 2
Injecting:
(1) in the table, the conventional process is counted by the common time of conventional continuous hydration degumming, high-temperature light alkali deacidification and continuous decolorization processes;
(2) the water consumption of the degumming process is 2-3 times of the phospholipid content according to the medium-temperature hydration process, and the soybean crude oil phospholipid accounts for about 1%; the water consumption of the deacidification process is calculated according to the water consumption of the commonly adopted long mixed alkali refining process;
(3) the data in the table are estimated data and may be slightly different from actual production.
The results in table 2 show that, compared with the conventional process technology, the process of the invention has the advantages that the water consumption (0.65-1.35 h) is far lower than that of the conventional process (4.9-7.5 h), the water consumption (0.5-1.0%) is also far lower than that of the conventional process (12-23%), and the quality of the treated oil product is better, so that great convenience is provided for removing free fatty acid and other odor components by further vacuum steam distillation in the follow-up process, and the process is more beneficial to producing high-grade edible soybean salad oil.
To further illustrate the importance of the steps and parameters involved in the present invention, the following comparative examples are included to illustrate the comparative operation of the process not providing parameters in accordance with the present invention.
Comparative example 1
Referring to example 1, the only difference is that the amount of the enzyme complex solution used in step (4) is too low, specifically:
the dosage of the enzyme complex enzyme solution in the step (4) is adjusted to 1.5 g.
In the process, the dosage of the complex enzyme (phospholipase A1 and phospholipase C) is too low, and the enzyme addition amount is only 3g/kg of soybean crude oil. Analyzing the phospholipid content of the double-enzyme method soybean degummed oil obtained in the step (5) of the comparative example 1, and carrying out thermal test detection, wherein the result shows that the phospholipid content is higher, and after the oil is heated and cooled, obvious black precipitates appear in the oil, and the color of the oil is obviously deepened compared with that before the oil is heated; and (3) analyzing the final oil, namely the alkaline clay decolored oil obtained in the step (7) (namely the soybean oil suitable for physical refining), and various indexes of the oil are not ideal.
Comparative example 2
Referring to example 1, the only difference is that the ultrasonic assisted two-enzyme degumming time in step (4) is too short, specifically:
and (4) adjusting the degumming time of the ultrasonic-assisted double-enzyme method in the step (4) to be 20 min.
In the process, the ultrasonic-assisted double-enzyme method degumming time is only 20min, the phospholipid content of the double-enzyme method soybean degummed oil obtained in the step (5) of the comparative example 2 is analyzed, and a thermal test is carried out to detect, wherein the result shows that the phospholipid content is higher, the heating test result of the oil shows that obvious black precipitates appear in the oil, and the color of the oil is obviously deepened compared with that before heating; and (3) analyzing the final oil, namely the alkaline clay decolored oil obtained in the step (7) (namely the soybean oil suitable for physical refining), and various indexes of the oil are not ideal.
Comparative example 3
With reference to example 1, the only difference is that the enzymatic hydrolysis temperature in step (4) is too low, in particular:
the enzymolysis temperature in the step (4) is adjusted to 35 ℃.
In the process, the enzymolysis temperature is too low and is only 35 ℃, the phospholipid content of the double-enzyme method soybean degummed oil obtained in the step (5) of the comparative example 3 is analyzed, and a thermal test is carried out to detect, wherein the result shows that the phospholipid content is higher, the heating test result of the oil shows that obvious black precipitates appear in the oil, and the color of the oil is obviously deepened compared with that before heating; and (3) analyzing the final oil, namely the alkaline clay decolored oil obtained in the step (7) (namely the soybean oil suitable for physical refining), and various indexes of the oil are not ideal.
Comparative example 4
Referring to example 1, the only difference is that no ultrasonic assistance is employed.
In the process, a double-enzyme method soybean degumming test is carried out without ultrasonic assistance, the phospholipid content of the double-enzyme method soybean degumming oil obtained in the step (5) of the comparative example 4 is analyzed, and a thermal test is carried out to detect, wherein the result shows that the phospholipid content is higher, the heating test result of the oil shows that obvious black precipitates appear in the oil, and the color of the oil is obviously deepened compared with that before heating; and (4) analyzing the final grease, namely the alkaline clay decolored oil obtained in the step (7) (namely the soybean grease suitable for physical refining), wherein each index of the oil is not ideal.
Comparative example 5
With reference to example 1, the only difference is that in step (6) the amount of alkaline clay used is too low, in particular:
in the step (6), the dosage of the alkaline clay is adjusted to be 1 percent of the mass of the degummed oil.
In the process, the dosage of the alkaline clay is too low and is only 1% of the mass of the degummed oil, and tests show that the indexes of acid value, color and the like of the alkaline clay decolored oil (namely, the soybean oil and fat suitable for physical refining) obtained in the step (7), which is the final oil of the comparative example 5, are not ideal, and the phosphorus content is slightly higher.
Comparative example 6
With reference to example 1, the only difference is that the bleaching time of the alkaline clay in step (6) is too short, in particular:
and (4) adjusting the alkaline clay decoloring time to 10min in the step (6).
In the process, the alkaline clay decolorization time is too short and is only 10min, and tests show that the indexes of acid value, color and the like of the final oil of the comparative example 5, namely the alkaline clay decolorized oil obtained in the step (7) (namely, the soybean oil suitable for physical refining) are not ideal, and the phosphorus content is higher.
Comparative example 7
Referring to example 1, the only difference is that the alkaline clay was replaced with a common activated clay.
In the process, as alkaline clay is not adopted and common active clay is used instead, tests show that the final grease of the comparative example 5, namely the active clay decolorized oil obtained in the step (7), has the indexes of acid value, peroxide value, color and luster and the like which are not obviously improved compared with the grease obtained in the step (5) although the content of phospholipid is reduced, particularly the acid value of the grease is seriously returned to acid after being treated by the common clay, and the indexes are obviously increased, so that the inconvenience and difficulty are increased for subsequent distillation deacidification.
Experimental example 2
Similarly, the soybean oil prepared in the proportion 1-7 is respectively subjected to a heating test, phospholipid, peroxide value, acid value and color and luster measurement by the methods described in GB/T5531 & 2018 test of vegetable oil and grain heating test, GB/T5537 & 2008 test of phospholipid content, GB 5009.227-2016 safety national standard food peroxide value measurement, GB 5009.229-2016 food safety national standard food acid value measurement and GB/T22460 & 2008 test of ludwippon color and luster of animal and vegetable oil and fat, and the measurement and calculation results are shown in Table 3:
TABLE 3
Injecting:
(1) the color of the grease is measured by adopting a Lovibond colorimetric method, and a 133.4mm standard glass colorimetric groove is adopted;
(2) in the table, "sample 1" and "sample 2" in the same comparative example represent the two-enzyme method soybean degummed oil obtained in step (5) and the alkaline clay decolorized oil obtained in step (7) in this example (i.e., soybean oil and fat suitable for physical refining), respectively;
(3) in the table, "Y" and "R" represent a yellow value and a red value, respectively.
The results in table 3 show that, after deviating from the recommended parameters of the two-enzyme degumming in the invention process (comparative examples 1 to 4), although the final oil has no obvious precipitate, the phospholipid content in the oil is still too high and exceeds 10mg/kg, the color of the oil is also deep, and new processing difficulty is brought to the subsequent steam distiller distillation; if the method deviates from the recommended steps or parameters of the subsequent alkaline decoloring and impurity removing process in the process (comparative example 5-comparative example 7), although the peroxide value and the color of the oil are improved to a certain extent, the improvement range is small, the phospholipid content does not reach the empirical recommended value suitable for the physical refining process below 5mg/kg, particularly after the alkaline clay is replaced by the activated clay, the oil has an obvious acid returning phenomenon, and the acid value is obviously higher than that before treatment.
Although the present invention has been described with reference to the preferred embodiments, it should be understood that various changes and modifications can be made therein by one skilled in the art without departing from the spirit and scope of the invention as defined by the appended claims.
Claims (10)
1. The pretreatment process of the soybean oil suitable for physical refining is characterized by sequentially comprising the following steps of:
(1) preheating the crude soybean oil;
(2) adjusting the pH value of the crude soybean oil obtained in the step (1) to 5-7; shearing at a high speed; stirring at constant speed under heating to condition the crude soybean oil;
(3) fully dissolving and mixing phospholipase A1 (lipase Ultra), phospholipase C and water, shearing at high speed, and hydrating to obtain compound enzyme solution; wherein the enzyme activity of the phospholipase A1 (leucine Ultra) is 10U/mg, the enzyme activity of the phospholipase C is 30U/mg, and the phospholipase A1 (leucine Ultra) and the phospholipase C are added in equal proportion; the water addition amount is 3 to 5 percent of the weight of the crude soybean oil obtained in the step (2); shearing the compound enzyme liquid and the crude soybean oil obtained in the step (2) at a high speed, wherein the mass ratio of the compound enzyme liquid to the crude soybean oil obtained in the step (2) is 4-6 g/kg, and then carrying out ultrasonic-assisted double-enzyme degumming reaction in a water bath environment at 50-60 ℃, wherein the ultrasonic-assisted power is 60-80 kHz, and the ultrasonic-assisted double-enzyme degumming reaction time is 35-60 min;
(4) after degumming, inactivating enzyme, cooling to room temperature, centrifuging to remove phospholipid, taking oil phase and drying to obtain double-enzyme soybean degummed oil;
(5) activating alkaline clay; mixing the activated alkaline clay with the double-enzyme method soybean degumming oil obtained in the step (4) according to the proportion of 2-3% of the mass of the degumming oil, and heating and stirring under negative pressure to carry out a decolorization reaction; cooling and filtering to obtain the soybean oil suitable for subsequent physical refining.
2. The process according to claim 1, wherein in the step (5), the vacuum degree of the negative pressure of the decolorization reaction is-0.095 to-0.090 MPa, the heating temperature is 95 ℃, the stirring speed is 120 to 150r/min, and the time of the decolorization reaction is 15 to 20 min.
3. The process according to claim 1, wherein in the step (3), the mass ratio of the complex enzyme solution to the crude soybean oil obtained in the step (2) is 5 g/kg; the shearing rate is 10000 r/min, and the shearing time is 1 min.
4. The process according to claim 1, wherein in the step (3), the temperature of the water bath for the ultrasonic-assisted double-enzyme degumming reaction is 50 ℃; the ultrasonic-assisted double-enzyme degumming reaction time is 45 min.
5. The process of claim 1, wherein the crude soybean oil is obtained by pressing or leaching, and the crude soybean oil is subjected to settling and filtration to remove impurities.
6. The process according to claim 1, wherein the pH of the crude soybean oil is adjusted by adding citric acid in the step (2); the citric acid is of analytical grade and meets the use requirement of food additives.
7. The process as claimed in claim 6, wherein in the step (2), the concentration of the citric acid solution is 45%, and the pH of the crude soybean oil obtained in the step (1) is adjusted to 6; the shearing rate of high-speed shearing is 15000 r/min, and the shearing time is 3 min; the tempering temperature is 55 ℃, the stirring speed is 80r/min, and the stirring time is 30 min.
8. The process of claim 1 wherein the alkaline clay is a food aid and meets food use requirements.
9. The process of claim 1, wherein the conditions for activating the alkaline clay in step (5) are: the activation temperature is 105 ℃, the activation time is 1.5-2.5 h, and the dryer is cooled to the room temperature after the activation.
10. Use of the process of any one of claims 1 to 9 in the production of high grade edible soybean salad oil.
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