CN115678674A - Degumming rice bran crude oil and degumming method for refining rice bran oil by using adsorbent and composite phospholipase - Google Patents
Degumming rice bran crude oil and degumming method for refining rice bran oil by using adsorbent and composite phospholipase Download PDFInfo
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- 239000010779 crude oil Substances 0.000 title claims abstract description 109
- ZIIUUSVHCHPIQD-UHFFFAOYSA-N 2,4,6-trimethyl-N-[3-(trifluoromethyl)phenyl]benzenesulfonamide Chemical compound CC1=CC(C)=CC(C)=C1S(=O)(=O)NC1=CC=CC(C(F)(F)F)=C1 ZIIUUSVHCHPIQD-UHFFFAOYSA-N 0.000 title claims abstract description 72
- 102000015439 Phospholipases Human genes 0.000 title claims abstract description 72
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- 239000008165 rice bran oil Substances 0.000 title claims abstract description 70
- 238000000034 method Methods 0.000 title claims abstract description 51
- 241000209094 Oryza Species 0.000 title claims abstract description 49
- 235000007164 Oryza sativa Nutrition 0.000 title claims abstract description 49
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- 238000001816 cooling Methods 0.000 claims abstract description 16
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- PEDCQBHIVMGVHV-UHFFFAOYSA-N Glycerine Chemical compound OCC(O)CO PEDCQBHIVMGVHV-UHFFFAOYSA-N 0.000 description 18
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Abstract
The invention discloses degummed rice bran crude oil and a degummed method for refining rice bran oil by using an adsorbent and composite phospholipase, which comprises the following steps: performing a leaching method on rice bran to obtain crude rice bran oil, and removing impurities in the crude rice bran oil; adding silicon dioxide powder into the rice bran crude oil, keeping the temperature at a first preset temperature, stirring and centrifuging to obtain crude oil, and storing at a second preset temperature; heating the treated crude oil to a third preset temperature, adding a citric acid solution into the crude oil, homogenizing, stirring at 70-75 ℃, cooling, and forming a body system liquid; adjusting the pH of the system liquid to 4.8-5.3, adding compound phospholipase for degumming, reacting completely to obtain an oil sample, demulsifying the oil sample at high temperature, and dehydrating the upper oil phase to obtain degummed crude rice bran oil.
Description
Technical Field
The invention belongs to the technical field of oil processing, and particularly relates to degummed crude rice bran oil and a degummed method for refining rice bran oil by using an adsorbent and composite phospholipase.
Background
Rice bran is one of important oil sources, rice bran is produced in China in about 1200-1600 ten thousand tons every year, and the resources are very rich. Rice bran oil is known as "healthy nutritional oil" abroad. Not only the fatty acid has rich composition types, but also contains various active substances such as vitamin E, sterol, oryzanol and the like. Has the effect of remarkably reducing the content of serum cholesterol and has wide market prospect. At present, the utilization rate of rice bran in China is low, and most of the rice bran is used as livestock and poultry feed or discarded. Not only causes resource waste, but also causes environmental pollution.
The oil refining step is generally "degumming-deacidification-decoloration-deodorization-dewaxing", wherein the gum is generally referred to as phospholipid. The phospholipid compound in the vegetable oil can be combined with protein, mucilage and trace metals to form particles of 1-100nm which are dispersed in the crude oil in a peptization state, and the impurities can greatly influence the quality of the oil, the storage stability, the downstream deep processing catalyst and the product quality, so the degumming is an important link for refining the vegetable oil. There are many methods for removing phospholipids, such as hydration degumming, acid degumming, enzymatic degumming, adsorption degumming, supercritical degumming, etc., of which adsorption degumming is one of the most environmentally friendly methods. The early phospholipid adsorbing materials TrisyI and Sorbsil have certain degumming effect but have higher price. The degumming effect of the active sepiolite is developed and researched subsequently, although the degumming effect is good, the treatment temperature is as high as more than 100 ℃, the energy consumption is high, and the influence of high temperature on the oil quality is obvious.
The most widely applied in the oil degumming industry are phospholipase A (PLA 1) and phospholipase C (PLC), but the defects of the phospholipase A and the phospholipase C exist respectively, most of the PLA1 can carry out enzymolysis on the common phospholipase in oil varieties, the degumming effect is good, but the degumming time is long, and at least 4 hours are needed; most of PLC has high reaction rate, can quickly reduce the content of phospholipid only within 1 hour, but has higher specificity to phosphatidylcholine and phosphatidylethanolamine and lower activity to phosphatidylinositol and the like, so that degumming is incomplete.
Disclosure of Invention
Therefore, the invention aims to provide an enzymatic degumming method which can ensure a better degumming effect and can obviously reduce the cost.
In order to achieve the above object, the present invention also provides a degumming method for refining rice bran oil using an adsorbent and a complex phospholipase, comprising the steps of:
step S100, performing a leaching method on rice bran to obtain crude rice bran oil, and removing impurities in the crude rice bran oil;
step S200, adding silicon dioxide powder into the rice bran crude oil, keeping the temperature at a first preset temperature, stirring and centrifuging to obtain crude oil, and storing the crude oil at a second preset temperature;
step S300, heating the crude oil treated in the step S200 to a third preset temperature, adding a citric acid solution into the crude oil, homogenizing, stirring at 70-75 ℃, cooling, and forming a system liquid;
and S400, adjusting the pH value of the system liquid to 4.8-5.3, adding compound phospholipase for degumming, reacting completely to obtain an oil sample, performing high-temperature demulsification on the oil sample, and dehydrating the upper oil phase to obtain degummed crude rice bran oil.
Preferably, in the degumming method for refining rice bran oil by using the adsorbent and the composite phospholipase, the first preset temperature is 34-36 ℃.
Preferably, in the degumming method for refining rice bran oil by using the adsorbent and the composite phospholipase, the third preset temperature is 70-75 ℃.
Preferably, in the degumming method for refining rice bran oil using an adsorbent and a complex phospholipase, the step S300 comprises:
heating the crude oil treated in the step S200 to 70 ℃, adding a citric acid solution into the crude oil, homogenizing for 1min, stirring for 22-27min at 70 ℃, waiting for cooling to 48-52 ℃, and forming a system liquid.
Preferably, in the degumming method for refining rice bran oil by using the adsorbent and the composite phospholipase, the ratio of the citric acid solution to the crude oil is 0.10ml/100g.
Preferably, in the degumming method for refining rice bran oil using an adsorbent and a complex phospholipase, the step S400 comprises:
adjusting the pH value of the system liquid to 4.8-5.3, adding compound phospholipase for degumming, wherein the degumming ratio of the compound phospholipase is PLA1: PLC =1:2 (v/v), controlling the temperature of an enzymatic degumming reaction system to be 45-55 ℃, stirring intensity to be 500r/min, pH to be 4.5-5.5, reacting for 2-3h, controlling the enzyme addition amount to be 30-60mg/kg, demulsifying at high temperature, controlling the temperature of high-temperature demulsification to be 90-95 ℃ and the demulsification time to be 30-50min, and dehydrating the upper oil phase to obtain the degummed rice bran crude oil.
Preferably, in the degumming method for refining rice bran oil by using the adsorbent and the composite phospholipase, the dehydration mode in the degummed rice bran crude oil obtained after the upper oil phase is dehydrated is vacuum distillation, the temperature is 75 ℃, and the pressure is 0.08Mpa.
Preferably, in the degumming method for refining rice bran oil using the adsorbent and the complex phospholipase, the complex phospholipase comprises phospholipase A 1 And phospholipase C.
Preferably, in the degumming method for refining rice bran oil using an adsorbent and a complex phospholipase, the adjusting the PH of the system liquid to 4.8-5.3 comprises: adding distilled water and a sodium hydroxide solution into the system liquid to adjust the pH of the system liquid to 4.8-5.3, wherein the mass concentration of sodium hydroxide is 4%, the addition amount of distilled water is 3-4ml/100g of crude oil, and the temperature of the distilled water is the same as that of the system liquid.
In order to achieve the purpose, the invention provides degumming rice bran crude oil which is prepared by adopting the degumming method for refining rice bran oil by using an adsorbent and composite phospholipase.
The invention has the following beneficial effects:
the invention determines the dosage of the added silicon dioxide, optimizes the parameters of the compound enzyme degumming process and determines the optimal degumming process. Compared with the defect of single phospholipase degumming, the compound enzyme not only maintains high-efficiency degumming efficiency, increases oil yield, but also obviously shortens enzymolysis time. The silicon dioxide is added, so that the phospholipid content in the grease is obviously reduced, the active ingredients in the grease are greatly reserved, and the consumption of the phospholipase is reduced. Greatly reduces the production cost of enterprises and obviously increases the economic benefit.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings used in the embodiments or the prior art descriptions will be briefly described below, and it is obvious that the drawings in the following descriptions are some embodiments of the present invention, and other drawings can be obtained by those skilled in the art without creative efforts.
FIG. 1 is a flow chart of an embodiment of the degumming method for rice bran oil refined by using adsorbent and composite phospholipase according to the present invention.
The implementation, functional features and advantages of the objects of the present invention will be further explained with reference to the accompanying drawings.
Detailed Description
In the embodiment of the present invention, the term "and/or" describes an association relationship of an associated object, and indicates that three relationships may exist, for example, a and/or B, and may indicate: a exists alone, A and B exist simultaneously, and B exists alone. The character "/" generally indicates that the former and latter associated objects are in an "or" relationship.
It should be noted that the terms "first," "second," and the like in the description and claims of the present invention and in the drawings described above are used for distinguishing between similar elements and not necessarily for describing a particular sequential or chronological order.
The term "plurality" in the embodiments of the present invention means two or more, and other terms are similar thereto.
In order to make the objects, technical solutions and advantages of the embodiments of the present invention more apparent, the embodiments of the present invention will be described in detail with reference to the accompanying drawings. However, it will be appreciated by those of ordinary skill in the art that in various embodiments of the invention, numerous technical details are set forth in order to provide a better understanding of the present invention. However, the claimed invention may be practiced without these specific details or with various changes and modifications based on the following embodiments. The following embodiments are divided for convenience of description, and should not constitute any limitation to the specific implementation manner of the present invention, and the embodiments may be mutually incorporated and referred to without contradiction.
The invention provides a degumming method for refining rice bran oil by using an adsorbent and composite phospholipase, and the degumming method is shown in figure 1 and comprises the following steps:
step S100, performing a leaching method on rice bran to obtain crude rice bran oil, and removing impurities in the crude rice bran oil;
the impurities in the crude rice bran oil may be removed by centrifugation and filtration, or may be removed by other means, which is not limited herein. In this embodiment, a centrifuge is used for centrifugation, the rotation speed of the centrifuge is 10000r/min, and the centrifugation time is 10min.
Step S200, adding silicon dioxide powder into the rice bran crude oil, keeping the temperature at a first preset temperature, stirring and centrifuging to obtain crude oil, and storing the crude oil at a second preset temperature;
the first preset temperature may be 35 ℃ ± 1 ℃, that is, the first preset temperature is 34 ℃ to 36 ℃, and in this embodiment, the first preset temperature may be 34 ℃, 35 ℃, or 36 ℃.
Preferably, the purity of the silica in the silica powder may be 99.99%.
Preferably, the second preset temperature is 4 ℃.
In this example, the crude oil obtained by stirring and centrifugation was kept at 4 ℃ while stirring with a magnetic stirrer at 200rpm for 20 min.
Step S300, heating the crude oil treated in the step S200 to a third preset temperature, adding a citric acid solution into the crude oil, homogenizing, stirring at 70-75 ℃, cooling, and forming a system liquid;
in this embodiment, the third predetermined temperature may be 70 ℃ to 75 ℃. Wherein the homogenization time may be 1min or longer, which is not limited herein.
Specifically, step S300 includes:
heating the crude oil treated in step S200 to 70 deg.C, adding citric acid solution into the crude oil, homogenizing for 1min, stirring at 70 deg.C for 25min (preferably at 500 r/min), cooling to about 50 deg.C (in this embodiment, cooling to 48-52 deg.C), and making into system liquid.
Wherein, the homogenizer is adopted for homogenization, and the rotating speed of the homogenizer is 10000rpm.
Preferably, the ratio of citric acid solution to crude oil is 0.10ml/100g, i.e. 100g of crude oil is added with 0.10ml of citric acid solution. Wherein the mass concentration of the citric acid solution is 42-47%. Preferably, the citric acid solution has a mass concentration of 45%.
And S400, adjusting the pH of the system liquid to 4.8-5.3, adding compound phospholipase for degumming, reacting completely to obtain an oil sample, performing high-temperature demulsification on the oil sample, and dehydrating the upper oil phase to obtain degummed crude rice bran oil.
Specifically, the pH of the system liquid is adjusted to 4.8 to 5.3 in step S400 by adding distilled water and a sodium hydroxide solution to the system liquid to adjust the system pH. Wherein the mass concentration of the sodium hydroxide is 4 percent. In this example, the amount of distilled water added was 3 to 4ml per 100g of crude oil, and the temperature of distilled water was the same as that of the system liquid.
And B, degumming by adding the composite phospholipase in the step S400, wherein the proportion of the composite phospholipase in the step of completely reacting to obtain the oil sample is PLA1: PLC =1:5-5:1 (v/v), preferably PLA1: PLC =1:2 (v/v).
More specifically, step S400 includes: adjusting the pH of the system liquid to 4.8-5.3, and adding compound phospholipase for degumming, wherein the degumming ratio of the compound phospholipase is PLA1: PLC =1:2 (v/v), wherein the temperature of an enzymatic degumming reaction system is 45-55 ℃, the stirring intensity is 500r/min, the pH is 4.5-5.5, the reaction time is 2-3h, the enzyme addition amount is 30-60mg/kg, the high-temperature demulsification is carried out at the temperature of 90-95 ℃ for 30-50min, and the upper oil phase is dehydrated to obtain the degummed crude rice bran oil, wherein the dehydration mode is vacuum distillation, such as rotary evaporation dehydration, the temperature is 75 ℃, and the pressure is 0.08Mpa.
Preferably, the complex phospholipase comprises phospholipase A 1 And phospholipase C. Phosphorus (P)Lipase A 1 And phospholipase C are both Lecite Ultra.
The invention also provides degummed rice bran crude oil which is prepared by the degummed rice bran oil refining method by using the adsorbent and the composite phospholipase. The degumming example of the crude rice bran oil comprises all the above degumming examples of the rice bran oil refining method by using the adsorbent and the composite phospholipase, and the beneficial effects of the degumming method of the rice bran oil refining method by using the adsorbent and the composite phospholipase can also be applied to degumming the crude rice bran oil.
Degumming method for refining rice bran oil by using adsorbent and composite phospholipase
The degumming method for refining rice bran oil by using the adsorbent and the composite phospholipase comprises the following steps:
s1, performing a leaching method on rice bran to obtain crude rice bran oil, and removing impurities in the crude rice bran oil;
s2, adding silicon dioxide powder into the rice bran crude oil, keeping the temperature at 34-36 ℃, stirring and centrifuging to obtain crude oil, and storing at 4 +/-1 ℃;
s3, heating the centrifuged crude oil to 70-75 ℃, adding a citric acid solution with the same temperature as the crude oil into the crude oil, wherein the ratio of the citric acid solution to the crude oil is 0.10ml/100g, homogenizing, stirring at 70-75 ℃, cooling to 48-52 ℃, and forming a system liquid;
s4, adjusting the pH value of the system liquid to 4.8-5.3, and adding compound phospholipase for degumming, wherein the degumming ratio of the compound phospholipase is PLA1: PLC =1:2 (v/v), the temperature of an enzymatic degumming reaction system is 45-55 ℃, the stirring strength is 500r/min, the pH is 4.5-5.5, the reaction time is 2-3h, PLA1: 5-5:1 (v/v), the enzyme addition amount is 30-60mg/kg, the high-temperature demulsification is carried out at the temperature of 90-95 ℃ for 30-50min, and the degummed crude rice bran oil is obtained after the upper oil phase is dehydrated, wherein the dehydration mode is vacuum distillation, the temperature is 75 ℃, and the pressure is 0.08Mpa.
Example 1
S1, performing a leaching method on rice bran to obtain crude rice bran oil, and removing impurities in the crude rice bran oil;
s2, placing 100g of rice bran crude oil into a 250mL conical flask with a plug, adding 1.5g of silicon dioxide powder into 100g of rice bran crude oil, keeping the temperature at 35 ℃, stirring the mixture at a speed of 200rpm by using a magnetic stirrer for 20min, centrifuging the mixture to obtain crude oil, and storing the crude oil at 4 +/-1 ℃;
s3, heating the centrifuged crude oil to 70 ℃ in a glycerol bath constant-temperature magnetic stirrer, adding 100 mu L of 45% citric acid solution with the same temperature as the crude oil into the crude oil according to the proportion of 0.10ml/100g of the crude oil, homogenizing for 1min at the rotation speed of 10000rpm by using a high-speed homogenizer, stirring and reacting for 25min at the rotation speed of 500r/min, and cooling to 50 ℃ to form a system liquid;
s4, adding 3mL of distilled water and 600 muL of 4% NaoH to adjust the pH of the system liquid to 4.8-5.3, and adding 1.0mL of compound phospholipase for degumming, wherein the compound phospholipase is PLA1: PLC =1:2 (v/v), the temperature of an enzymatic degumming reaction system is 50 ℃, the stirring intensity is 500r/min, the reaction time is 3h, after the reaction is finished, the conical flask filled with the reaction mixture is placed in an oil bath at 95 ℃ for 30min for demulsification, the reaction mixture is quickly centrifuged on a centrifuge at 10,000rpm for 5min to collect an upper oil layer, and the upper oil layer is rotated and evaporated to remove water under the conditions of 0.08Mpa and 75 ℃ to obtain the degummed crude rice bran oil.
Example 2
S1, performing a leaching method on rice bran to obtain crude rice bran oil, and removing impurities in the crude rice bran oil;
s2, placing 100g of rice bran crude oil into a 250mL conical flask with a plug, adding 1.5g of silicon dioxide powder into 100g of rice bran crude oil, keeping the temperature at 35 ℃, stirring for 20min at the speed of 200rpm by using a magnetic stirrer, centrifuging to obtain crude oil, and storing at 4 +/-1 ℃;
s3, heating the centrifuged crude oil to 70 ℃ in a glycerol bath constant-temperature magnetic stirrer, adding 100 mu L of 45% citric acid solution with the same temperature as the crude oil into the crude oil according to the proportion of 0.10ml/100g of the crude oil, homogenizing for 1min at the rotation speed of 10000rpm by using a high-speed homogenizer, stirring and reacting for 25min at the rotation speed of 500r/min, and cooling to 55 ℃ to form a system liquid;
s4, adding 4mL of distilled water and 600 muL of 4% of NaoH to adjust the pH of the system liquid to 4.8-5.3, and adding 1.5mL of compound phospholipase for degumming, wherein the compound phospholipase is PLA1: PLC =1:2 (v/v), keeping the temperature of an enzymatic degumming reaction system at 50 ℃, stirring intensity at 500r/min, reacting for 3h, after the reaction is finished, placing a conical flask filled with the reaction mixture in an oil bath at 95 ℃ for 30min for demulsification, quickly centrifuging the reaction mixture on a centrifuge at 10,000rpm for 5min, collecting an upper oil layer, and rotationally evaporating at 0.08Mpa and 75 ℃ for removing water to obtain the degummed rice bran crude oil.
Example 3
S1, performing a leaching method on rice bran to obtain crude rice bran oil, and removing impurities in the crude rice bran oil;
s2, placing 100g of rice bran crude oil into a 250mL conical flask with a plug, adding 1.5g of silicon dioxide powder into 100g of rice bran crude oil, keeping the temperature at 35 ℃, stirring the mixture at a speed of 200rpm by using a magnetic stirrer for 20min, centrifuging the mixture to obtain crude oil, and storing the crude oil at 4 +/-1 ℃;
s3, heating the centrifuged crude oil to 70 ℃ in a glycerin bath constant-temperature magnetic stirrer, adding 100 mu L of 45% citric acid solution with the same temperature as the crude oil into the crude oil according to the proportion of 0.10ml/100g of the crude oil, homogenizing for 1min at the rotation speed of 10000rpm by using a high-speed homogenizer, stirring and reacting for 25min at the rotation speed of 500r/min, and cooling to 55 ℃ to form a body system liquid;
s4, adding 4mL of distilled water and 600 muL of 4% of NaoH to adjust the pH of the system liquid to 4.8-5.3, and adding 1.5mL of compound phospholipase for degumming, wherein the compound phospholipase is PLA1: PLC =2:1 (v/v), keeping the temperature of an enzymatic degumming reaction system at 55 ℃, stirring intensity at 500r/min, reacting for 3h, after the reaction is finished, placing a conical flask filled with the reaction mixture in an oil bath at 95 ℃ for 30min for demulsification, quickly centrifuging the reaction mixture on a centrifuge at 10,000rpm for 5min, collecting an upper oil layer, and rotationally evaporating at 0.08Mpa and 75 ℃ for removing water to obtain the degummed rice bran crude oil.
Example 4
S1, performing a leaching method on rice bran to obtain crude rice bran oil, and removing impurities in the crude rice bran oil;
s2, placing 100g of rice bran crude oil into a 250mL conical flask with a plug, adding 1.5g of silicon dioxide powder into 100g of rice bran crude oil, keeping the temperature at 35 ℃, stirring the mixture at a speed of 200rpm by using a magnetic stirrer for 20min, centrifuging the mixture to obtain crude oil, and storing the crude oil at 4 +/-1 ℃;
s3, heating the centrifuged crude oil to 70 ℃ in a glycerin bath constant-temperature magnetic stirrer, adding 100 mu L of 45% citric acid solution with the same temperature as the crude oil into the crude oil according to the proportion of 0.10ml/100g of the crude oil, homogenizing for 1min at the rotation speed of 10000rpm by using a high-speed homogenizer, stirring and reacting for 25min at the rotation speed of 500r/min, and cooling to 55 ℃ to form a body system liquid;
s4, adding 4mL of distilled water and 600 muL of 4% of NaoH to adjust the pH of the system liquid to 4.8-5.3, and adding 1.5mL of compound phospholipase for degumming, wherein the compound phospholipase is PLA1: PLC =1:2 (v/v), keeping the temperature of an enzymatic degumming reaction system at 45 ℃, stirring intensity at 500r/min, reacting for 2h, after the reaction is finished, placing a conical flask filled with the reaction mixture in an oil bath at 95 ℃ for 30min for demulsification, quickly centrifuging the reaction mixture on a centrifuge at 10,000rpm for 5min, collecting an upper oil layer, and rotationally evaporating at 0.08Mpa and 75 ℃ for removing water to obtain the degummed rice bran crude oil.
Example 5
S1, performing a leaching method on rice bran to obtain crude rice bran oil, and removing impurities in the crude rice bran oil;
s2, placing 100g of rice bran crude oil into a 250mL conical flask with a plug, adding 1.5g of silicon dioxide powder into 100g of rice bran crude oil, keeping the temperature at 35 ℃, stirring the mixture at a speed of 200rpm by using a magnetic stirrer for 20min, centrifuging the mixture to obtain crude oil, and storing the crude oil at 4 +/-1 ℃;
s3, heating the centrifuged crude oil to 70 ℃ in a glycerol bath constant-temperature magnetic stirrer, adding 100 mu L of 45% citric acid solution with the same temperature as the crude oil into the crude oil according to the proportion of 0.10ml/100g of the crude oil, homogenizing for 1min at the rotation speed of 10000rpm by using a high-speed homogenizer, stirring and reacting for 25min at the rotation speed of 500r/min, and cooling to 55 ℃ to form a system liquid;
s4, adding 4mL of distilled water, 600 μ L of 4% of NaoH to adjust the pH of the system liquid to 4.8-5.3, adding 2mL of composite phospholipase for degumming, wherein the composite phospholipase is PLA1: PLC =1:2 (v/v), keeping the temperature of an enzymatic degumming reaction system at 50 ℃, stirring intensity at 500r/min, reacting for 3h, after the reaction is finished, placing a conical flask filled with the reaction mixture in an oil bath at 95 ℃ for 30min for demulsification, quickly centrifuging the reaction mixture on a centrifuge at 10,000rpm for 5min, collecting an upper oil layer, and rotationally evaporating at 0.08Mpa and 75 ℃ for removing water to obtain the degummed rice bran crude oil.
Comparative example 1
S1, performing a leaching method on rice bran to obtain crude rice bran oil, and removing impurities in the crude rice bran oil;
s2, placing 100g of rice bran crude oil into a 250mL conical flask with a plug, adding 0g of silicon dioxide powder into 100g of rice bran crude oil, keeping the temperature at 35 ℃, stirring the mixture for 20min at the speed of 200rpm by using a magnetic stirrer, centrifuging the mixture to obtain crude oil, and storing the crude oil at the temperature of 4 +/-1 ℃;
s3, heating the centrifuged crude oil to 70 ℃ in a glycerol bath constant-temperature magnetic stirrer, adding 100 mu L of 45% citric acid solution with the same temperature as the crude oil into the crude oil according to the proportion of 0.10ml/100g of the crude oil, homogenizing for 1min at the rotation speed of 10000rpm by using a high-speed homogenizer, stirring and reacting for 25min at the rotation speed of 500r/min, and cooling to 55 ℃ to form a system liquid;
s4, adding 4mL of distilled water and 600 muL of 4% of NaoH to adjust the pH of the system liquid to 4.8-5.3, and adding 1mL of compound phospholipase for degumming, wherein the compound phospholipase is PLA1: PLC =1:2 (v/v), keeping the temperature of an enzymatic degumming reaction system at 60 ℃, stirring intensity at 500r/min, reacting for 3h, after the reaction is finished, placing a conical flask filled with the reaction mixture in an oil bath at 95 ℃ for 30min for demulsification, quickly centrifuging the reaction mixture on a centrifuge at 10,000rpm for 5min, collecting an upper oil layer, and rotationally evaporating at 0.08Mpa and 75 ℃ for removing water to obtain the degummed rice bran crude oil.
Comparative example 2
S1, performing a leaching method on rice bran to obtain crude rice bran oil, and removing impurities in the crude rice bran oil;
s2, placing 100g of rice bran crude oil into a 250mL conical flask with a plug, adding 0g of silicon dioxide powder into 100g of rice bran crude oil, keeping the temperature at 35 ℃, stirring the mixture for 20min at the speed of 200rpm by using a magnetic stirrer, centrifuging the mixture to obtain crude oil, and storing the crude oil at the temperature of 4 +/-1 ℃;
s3, heating the centrifuged crude oil to 70 ℃ in a glycerin bath constant-temperature magnetic stirrer, adding 100 mu L of 45% citric acid solution with the same temperature as the crude oil into the crude oil according to the proportion of 0.10ml/100g of the crude oil, homogenizing for 1min at the rotation speed of 10000rpm by using a high-speed homogenizer, stirring and reacting for 25min at the rotation speed of 500r/min, and cooling to 55 ℃ to form a body system liquid;
s4, adding 4mL of distilled water, 600 μ L of 4% of NaoH to adjust the pH of the system liquid to 4.8-5.3, adding 1.5mL of composite phospholipase for degumming, wherein the composite phospholipase is PLA1: PLC =1:5 (v/v), keeping the temperature of an enzymatic degumming reaction system at 55 ℃, stirring intensity at 500r/min, reacting for 2h, after the reaction is finished, placing a conical flask filled with the reaction mixture in an oil bath at 95 ℃ for 30min for demulsification, quickly centrifuging the reaction mixture on a centrifuge at 10,000rpm for 5min, collecting an upper oil layer, and rotationally evaporating at 0.08Mpa and 75 ℃ for removing water to obtain the degummed rice bran crude oil.
TABLE 1 examples and comparative examples
As can be seen from Table 1, the degumming method for refining rice bran oil by using the adsorbent and the composite phospholipase provided by the invention not only maintains high-efficiency degumming time, increases oil yield, but also obviously shortens enzymolysis time.
Furthermore, by adding silicon dioxide, the content of phospholipid in the grease is obviously reduced, active ingredients in the grease are greatly reserved, and the consumption of phospholipase is reduced.
It is to be understood that the above-described embodiments are only a few, but not all, embodiments of the present invention. Based on the embodiments of the present invention, those skilled in the art may make other variations or modifications without creative efforts, and shall fall within the protection scope of the present invention.
Claims (10)
1. A degumming method for refining rice bran oil by using an adsorbent and composite phospholipase is characterized by comprising the following steps:
step S100, performing a leaching method on rice bran to obtain crude rice bran oil, and removing impurities in the crude rice bran oil;
step S200, adding silicon dioxide powder into the rice bran crude oil, keeping the temperature at a first preset temperature, stirring and centrifuging to obtain crude oil, and storing the crude oil at a second preset temperature;
step S300, heating the crude oil treated in the step S200 to a third preset temperature, adding a citric acid solution into the crude oil, homogenizing, stirring at 70-75 ℃, cooling, and forming a system liquid;
and S400, adjusting the pH value of the system liquid to 4.8-5.3, adding compound phospholipase for degumming, reacting completely to obtain an oil sample, performing high-temperature demulsification on the oil sample, and dehydrating the upper oil phase to obtain degummed crude rice bran oil.
2. The degumming process for refining rice bran oil with an adsorbent and a complex phospholipase according to claim 1, wherein the first predetermined temperature is 34 ℃ to 36 ℃.
3. The degumming process for refining rice bran oil with an adsorbent and a complex phospholipase according to claim 1, wherein the third predetermined temperature is 70 ℃ to 75 ℃.
4. The degumming process for refining rice bran oil with an adsorbent and a complex phospholipase according to claim 3, wherein the step S300 comprises:
heating the crude oil treated in the step S200 to 70 ℃, adding a citric acid solution into the crude oil, homogenizing for 1min, stirring for 22min-27min at 70 ℃, waiting for cooling to 48-52 ℃, and forming a system liquid.
5. The degumming process for refining rice bran oil with an adsorbent and a complex phospholipase according to claim 4, wherein the ratio of the citric acid solution to the crude oil is 0.10ml/100g.
6. The degumming process for refining rice bran oil with an adsorbent and a complex phospholipase according to claim 4, wherein the step S400 comprises:
adjusting the pH value of the system liquid to 4.8-5.3, adding compound phospholipase for degumming, wherein the degumming ratio of the compound phospholipase is PLA1: PLC =1:2 (v/v), controlling the temperature of an enzymatic degumming reaction system to be 45-55 ℃, stirring intensity to be 500r/min, pH to be 4.5-5.5, reacting for 2-3h, controlling the enzyme addition amount to be 30-60mg/kg, demulsifying at high temperature, controlling the temperature of high-temperature demulsification to be 90-95 ℃ and the demulsification time to be 30-50min, and dehydrating the upper oil phase to obtain the degummed rice bran crude oil.
7. The degumming method for refining rice bran oil with the adsorbent and the composite phospholipase according to claim 6, wherein the dehydration in the degummed crude rice bran oil obtained by dehydrating the upper oil phase is vacuum distillation at 75 ℃ and 0.08Mpa.
8. The degumming process for refining rice bran oil with an adsorbent and a complex phospholipase according to claim 6, wherein the complex phospholipase comprises phospholipase A 1 And phospholipase C.
9. The degumming process for refining rice bran oil with an adsorbent and a complex phospholipase according to claim 6, wherein the adjusting the pH of the system liquid to 4.8-5.3 comprises: adding distilled water and a sodium hydroxide solution into the system liquid to adjust the pH of the system liquid to 4.8-5.3, wherein the mass concentration of sodium hydroxide is 4%, the addition amount of distilled water is 3-4ml/100g of crude oil, and the temperature of the distilled water is the same as that of the system liquid.
10. The degummed crude rice bran oil, which is prepared by the degummed method for refining the rice bran oil by using the adsorbent and the composite phospholipase according to any one of claims 1 to 9.
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| CN105038978A (en) * | 2007-01-30 | 2015-11-11 | 邦奇油类公司 | Enzymatic degumming utilizing a mixture of pla and plc phospholipases |
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| CN111349512A (en) * | 2020-03-11 | 2020-06-30 | 陕西科技大学 | Method for degumming rice bran oil with high acid value by enzyme method |
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| CN105038978A (en) * | 2007-01-30 | 2015-11-11 | 邦奇油类公司 | Enzymatic degumming utilizing a mixture of pla and plc phospholipases |
| CN110016387A (en) * | 2019-05-09 | 2019-07-16 | 四川省农业科学院农产品加工研究所 | Edible vegetable oil degumming agent and preparation method thereof and refined oil method |
| CN111349512A (en) * | 2020-03-11 | 2020-06-30 | 陕西科技大学 | Method for degumming rice bran oil with high acid value by enzyme method |
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