A method and apparatus for preventing crystallization of diglyceride oil

Abstract

The application discloses a method and device for preventing crystallization of diglyceride oil. The method comprises the following steps: preheating and homogenizing the diglyceride oil to be treated, adding a composite filter aid, and performing adsorption treatment under stirring or ultrasonic action, then filtering to obtain a clear oil phase and a turbid oil phase retained by a filter cake; adding an enzyme preparation to the turbid oil phase to perform enzymatic hydrolysis, then mixing with water, adjusting the pH to 5.5-6.5, inactivating, and centrifuging to obtain an enzymatic hydrolysis clear oil phase; mixing the clear oil phase with the enzymatic hydrolysis clear oil phase, vacuum deodorizing, and aseptically filling to obtain an anti-crystallization diglyceride oil product; wherein the composite filter aid comprises diatomite and silica gel powder; and the enzyme preparation comprises lipase, phospholipase and an enzyme stabilizer. The application selectively removes initial crystallization core substances by adsorption and filtration of the composite filter aid, and then performs directional enzymatic hydrolysis on the turbid oil phase, so that the crystallization inducement is effectively eliminated from the root, and long-term stable storage of the oil is realized.

Description

Technical Field

[0001] This application relates to the field of oil processing technology, specifically to a method and apparatus for preventing the crystallization of diglyceride oil. Background Technology

[0002] Diglyceride oil (DAG), as a functional oil, has physiological effects such as regulating blood lipids and inhibiting fat accumulation, and is widely used in the food, health products and pharmaceutical fields.

[0003] However, when diglyceride oil is stored at low temperatures (4℃~10℃) or stored for a long time, it is prone to crystallization due to residual triglycerides, polymerization of free fatty acids, and crystal transformation (conversion from β' crystal form to β crystal form), resulting in turbidity and decreased fluidity of the oil, which seriously affects product quality and market acceptance.

[0004] In view of this, there is an urgent need for a method and apparatus that can prevent diglyceride oil from crystallizing. Summary of the Invention

[0005] In view of the above problems, this application aims to provide a method and apparatus for preventing the crystallization of diglyceride oil.

[0006] In one aspect, this application provides a method for preventing the crystallization of diglyceride oil.

[0007] The method of this application includes the following steps: Step 1, Preheating and Homogenization: The diglyceride oil to be processed is preheated and homogenized to obtain homogenized diglyceride oil.

[0008] Step 2, Adsorption treatment: A composite filter aid is added to homogenized diglyceride oil, and adsorption treatment is carried out under stirring or ultrasonic treatment to obtain an adsorption-treated mixture; wherein, the composite filter aid includes diatomaceous earth and silica gel powder.

[0009] Step 3, filtration process: The mixture after adsorption treatment is filtered to obtain a clear oil phase and a turbid oil phase retained by the filter cake.

[0010] Step 4, enzymatic hydrolysis: An enzyme preparation was added to the turbid oil phase, and enzymatic hydrolysis was carried out under stirring to obtain the enzymatic hydrolysis product.

[0011] Step 5, inactivation treatment: After adding water to the enzymatic hydrolysis product and mixing, the pH of the system was adjusted to 5.5-6.5, followed by inactivation treatment and centrifugation to obtain the enzymatic hydrolysis clear oil phase.

[0012] Step 6, Post-processing: The clarified oil phase and the enzymatically hydrolyzed clear oil phase are mixed and then deodorized under vacuum, followed by aseptic filling to obtain the anti-crystallization diglyceride oil product.

[0013] In some embodiments of this application, the amount of the composite filter aid added is based on the mass of the diglyceride oil to be treated. a ,and a Satisfying 0.5%≤ a ≤2.0%.

[0014] In some embodiments of this application, the mass ratio of diatomaceous earth to silica gel powder in the composite filter aid is 6~7:2~3.

[0015] In some embodiments of this application, a plate and frame filter is used for filtration, and the filtration pressure is 0.3MPa~0.6MPa, and the filtration temperature is maintained at 38℃~42℃.

[0016] In some embodiments of this application, the preheating and homogenization treatment is carried out at a temperature of 35°C to 45°C for a time of 30 min to 60 min.

[0017] In some embodiments of this application, when adsorption is performed under stirring, the stirring rate is 60 rpm to 100 rpm.

[0018] In some embodiments of this application, when adsorption is performed under ultrasonic action, the ultrasonic power is 500W~800W.

[0019] In some embodiments of this application, the adsorption treatment time is 20 min to 40 min.

[0020] In some embodiments of this application, the mass ratio of the lipase, the phospholipase and the enzyme stabilizer in the enzyme preparation is 50~60:25~35:5~15.

[0021] In some embodiments of this application, the amount of enzyme preparation added is based on the mass of the turbid oil phase. b ,and b Satisfying 0.3%≤ b ≤0.8%.

[0022] In some embodiments of this application, the enzymatic hydrolysis treatment is carried out at a temperature of 45°C to 55°C, for a duration of 2 hours to 4 hours, and with a stirring rate of 60 rpm to 100 rpm.

[0023] In some embodiments of this application, the mass ratio of the enzymatic hydrolysis product to water is 1:0.8~1.2.

[0024] In some embodiments of this application, the inactivation treatment is carried out at a temperature of 80°C to 85°C for 15 min to 20 min.

[0025] In some embodiments of this application, the centrifugation rate is 8000 rpm to 10000 rpm and the centrifugation time is 8 min to 12 min.

[0026] In some embodiments of this application, the volume ratio of the clarified oil phase to the enzymatically hydrolyzed clear oil phase is 85~95:5~15.

[0027] In some embodiments of this application, the vacuum degree during vacuum deodorization is -0.08MPa ~ -0.09MPa, and the processing temperature is 48℃ ~ 52℃.

[0028] In some embodiments of this application, the purity of the diglyceride oil to be treated is 85%~95%, the residual triglyceride content is ≤10%, and the free fatty acid content is ≤3%.

[0029] Secondly, this application provides a device for preventing the crystallization of diglyceride oil.

[0030] It is understood that the apparatus of this application is constructed based on any one of the methods in the first aspect. Therefore, the processing principle of the apparatus of this application during use is consistent with any one of the methods in the first aspect, and has all the beneficial effects brought about by the method itself in the first aspect. Therefore, this application will not repeat the details here, please refer to the content described in the first aspect of this application.

[0031] The apparatus of this application includes a preheating homogenizing device, an adsorption reaction device, a filtration device, an enzymatic hydrolysis device, a centrifugation device, and a vacuum deodorization device connected in sequence.

[0032] In this application, the preheating homogenizing device is used to receive the diglyceride oil to be processed and to preheat and homogenize the diglyceride oil to be processed.

[0033] The input end of the adsorption reaction device is connected to the output end of the preheating homogenizer to receive the homogenized diglyceride oil obtained by the preheating homogenizer and adsorb it.

[0034] The input end of the filtration device is connected to the output end of the adsorption reaction device to receive the mixture obtained by the adsorption reaction device and filter it; the filtration device has a clear oil phase output end and a turbid oil phase output end.

[0035] The input end of the enzymatic hydrolysis device is connected to the output end of the turbid oil phase to receive the turbid oil phase obtained by filtration by the filtration device, and to perform enzymatic hydrolysis and inactivation treatment on the turbid oil phase; the enzymatic hydrolysis device also has an enzyme preparation input end, which is used to add enzyme preparation.

[0036] The input end of the centrifuge device is connected to the output end of the enzymatic hydrolysis device so that the inactivated material enters the centrifuge device for centrifugation.

[0037] The input end of the vacuum deodorization device is connected to the output end of the centrifuge device, and the input end of the vacuum deodorization device is also connected to the output end of the clarified oil phase, so that the clarified oil phase and the enzymatically hydrolyzed clear oil phase obtained by centrifugation are mixed and then vacuum deodorized.

[0038] In some embodiments of this application, the preheating homogenizing device includes a preheating homogenizing tank, which has a diglyceride oil inlet for adding diglyceride oil to be processed.

[0039] In some embodiments of this application, the preheating homogenizing device of this application is further provided with a heating module and a temperature detection module.

[0040] In some embodiments of this application, a heat transfer oil jacket is provided at the bottom of the preheating homogenizing tank.

[0041] In some embodiments of this application, the preheating homogenizing tank is provided with a first stirring module to stir the diglyceride oil to be treated, so as to promote uniform heating of the diglyceride oil to be treated.

[0042] In some embodiments of this application, the adsorption reaction device includes an adsorption reaction vessel, the input end of which is connected to the output end of the preheating homogenizing device via a first conveying pipe, and the adsorption reaction vessel has a composite filter aid inlet for adding composite filter aid so that the homogenized diglyceride oil and composite filter aid are adsorbed in the adsorption reaction device.

[0043] In some embodiments of this application, the adsorption reactor is provided with an adsorption auxiliary device, which includes an ultrasonic generator or a second stirring module.

[0044] In some embodiments of this application, the filtration device further includes a pressure sensor and a first temperature control module, wherein the pressure sensor is used to maintain the filtration pressure of the filtration process at 0.3MPa~0.6MPa, and the first temperature control module is used to maintain the filtration temperature at 38℃~42℃.

[0045] In some embodiments of this application, the filtration device is a plate and frame filter equipped with a pressure sensor and a first temperature control module.

[0046] In some embodiments of this application, the enzymatic hydrolysis reactor further includes a pH monitoring module, a second temperature control module, and a third stirring module. The pH monitoring module monitors the pH value of the materials within the reactor body to control it within the desired pH range. The second temperature control module adjusts the reaction temperature within the reactor body to the temperature for enzymatic hydrolysis or inactivation treatment, depending on the reaction progress. The third stirring module provides the required stirring rate for enzymatic hydrolysis to promote thorough mixing of the turbid oil phase and the enzyme preparation, thereby improving the efficiency of the enzymatic hydrolysis process.

[0047] In some embodiments of this application, the centrifugation apparatus further includes a third temperature control module to control the temperature of the centrifugation process within the desired range.

[0048] In some embodiments of this application, the first conveying pipe is fitted with an insulation layer.

[0049] In some embodiments of this application, a first pump body is provided on the first delivery pipeline, and the first pump body is used to adjust the delivery rate when homogenized diglyceride oil is delivered into the adsorption reaction device.

[0050] In some embodiments of this application, a second pump body is provided on the second conveying pipeline, and the second pump body is used to adjust the conveying rate of the mixture obtained from the adsorption treatment into the filter device.

[0051] In some embodiments of this application, a third pump body is provided on the third conveying pipe, and the third pump body is used to adjust the conveying rate when the turbid oil is conveyed in the enzymatic hydrolysis device.

[0052] In some embodiments of this application, a fourth pump body is provided on the fourth conveying pipeline, and the fourth pump body is used to adjust the conveying rate of the inactivated material when it is conveyed into the centrifuge device.

[0053] In some embodiments of this application, a fifth pump body is provided on the fifth conveying pipeline, and the fifth pump body is used to adjust the conveying rate when the enzymatically hydrolyzed clear oil obtained by centrifugation is conveyed into the vacuum deodorization device.

[0054] In some embodiments of this application, a sixth pump body is provided on the sixth conveying pipe, and the sixth pump body is used to adjust the conveying rate when the clarified grease is conveyed into the vacuum deodorization device.

[0055] The beneficial effects of the technical solutions provided in some embodiments of this application include at least the following: This application selectively removes the initial crystallization core material through sequential preheating and homogenization treatment, adsorption and filtration with composite filter aid, and then performs targeted enzymatic hydrolysis on the turbid oil phase obtained by filtration. This completely destroys the conditions for crystallization formation, effectively eliminates the inducing factors for crystallization from the root, and achieves long-term stable storage of oil.

[0056] The composite filter aid of this application has both adsorption and crystal form regulation functions, and no additional emulsifier is required. After enzymatic hydrolysis, the enzyme preparation is completely removed by centrifugation, and the product purity is ≥99%.

[0057] The device described in this application can directly industrialize the method described in this application, and can be directly connected to existing diglyceride oil production lines. The modification cost is low, which is conducive to industrial promotion. Attached Figure Description

[0058] To more clearly illustrate the technical solutions in the embodiments of this application or the prior art, the drawings used in the description of the embodiments or the prior art will be briefly introduced below. Obviously, the drawings described below are only some embodiments of this application. For those skilled in the art, other drawings can be obtained based on these drawings without creative effort.

[0059] Figure 1 This is a schematic diagram of a device for preventing the crystallization of diglyceride oil according to this application.

[0060] Figure 2 This is a schematic diagram of a preheating homogenizing device according to this application.

[0061] Figure 3 This is a schematic diagram of the architecture and connection of a preheating homogenizing device according to this application.

[0062] Figure 4 This is a schematic diagram of an adsorption reaction device according to this application.

[0063] Figure 5 This is a schematic diagram of the architecture of a filtering device in this application.

[0064] Figure 6 This is a schematic diagram of the architecture of an enzymatic hydrolysis device according to this application.

[0065] Figure 7 This is a schematic diagram of the architecture and connection of a centrifuge device according to this application.

[0066] In the diagram, 100-preheating homogenizer, 101-preheating homogenizer tank, 102-diglyceride oil inlet, 103-heating module, 104-temperature detection module, 105-heat transfer oil jacket, 106-first stirring module; 200-adsorption reaction device, 201-adsorption reaction vessel, 202-composite filter aid inlet, 203-adsorption auxiliary device; 300-filtration device, 301-clarified oil phase output, 302-turbid oil phase output, 303-pressure sensor, 304-first temperature controller. Preparation module; 400-Enzyme hydrolysis device, 401-Enzyme hydrolysis reactor, 402-Enzyme preparation input end, 403-pH monitoring module, 404-Second temperature control module, 405-Third stirring module; 500-Centrifugation device, 501-Third temperature control module; 600-Vacuum deodorization device; 700-Conveying device, 701-First conveying pipe, 702-Second conveying pipe, 703-Third conveying pipe, 704-Fourth conveying pipe, 705-Fifth conveying pipe, 706-Sixth conveying pipe. Detailed Implementation

[0067] To make the objectives, technical solutions, and advantages of this application clearer, the following detailed description is provided in conjunction with the accompanying drawings and embodiments. It should be understood that the specific embodiments described herein are merely illustrative and not intended to limit the scope of this application.

[0068] In the description of this application, the terms "upper," "lower," "right," etc., refer to the orientation or positional relationship shown in the accompanying drawings, and are used only for ease of description and simplification of operation. They do not indicate or imply that the device or element referred to must have a specific orientation, or be constructed and operated in a specific orientation, and therefore should not be construed as a limitation of this application. In addition, the terms "first" and "second" are used only for descriptive distinction and have no special meaning.

[0069] The endpoints and any values ​​of the ranges disclosed in this application are not limited to the precise ranges or values, and such ranges or values ​​should be understood to include values ​​close to such ranges or values. For numerical ranges, the endpoint values ​​of the various ranges, the endpoint values ​​of the various ranges and individual point values, and individual point values ​​can be combined with each other to obtain one or more new numerical ranges, which should be considered as specifically disclosed herein.

[0070] Unless otherwise specified, all embodiments and optional embodiments of this application can be combined to form new technical solutions. Unless otherwise specified, all technical features and optional technical features of this application may be combined to form new technical solutions. Unless otherwise specified, all steps in this application may be performed sequentially or randomly, preferably sequentially. For example, the method includes steps (a) and (b), indicating that the method may include steps (a) and (b) performed sequentially, or it may include steps (b) and (a) performed sequentially. For example, the method may also include step (c), indicating that step (c) may be added to the method in any order. For example, the method may include steps (a), (b), and (c), or it may include steps (a), (c), and (b), or it may include steps (c), (a), and (b), etc. Unless otherwise specified, the terms "comprising" and "including" as used in this application can be open-ended or closed-ended. For example, "comprising" and "including" can mean that other components not listed may also be included, or that only the listed components may be included. Unless otherwise specified, the term "or" is inclusive in this application. For example, the phrase "A or B" means "A, B, or both A and B". More specifically, the condition "A or B" is satisfied by any of the following conditions: A is true (or exists) and B is false (or does not exist); A is false (or does not exist) and B is true (or exists); or both A and B are true (or exist).

[0071] It should be emphasized that the preparation methods or operation steps not specifically described in this application all refer to the prior art in this field, which should be known by those skilled in the art, and therefore will not be described again in this application.

[0072] As described in the background section, diglyceride oil is prone to crystallization and precipitation due to residual triglycerides, polymerization of free fatty acids, and crystal transformation (conversion from β' crystal form to β crystal form) during low-temperature storage (4-10℃) or long-term storage. This results in turbidity and decreased fluidity of the oil, which seriously affects product quality and market acceptance.

[0073] To prevent oil crystallization, current technologies mainly employ methods such as adding exogenous chemical reagents to regulate crystal form and high-pressure homogenization to optimize the process. Among these, the method of adding exogenous chemical reagents to regulate crystal form, for example, involves a composite emulsifier disclosed in existing technology CN107981319A. While this composite emulsifier can prevent diglyceride oil crystallization to some extent, experimental data shows that the β' crystal content decreases after 30 days, indicating that adding the composite emulsifier cannot fundamentally eliminate the crystallization inducing factor. With prolonged storage, crystallization from the β' crystal form to the β crystal form will still occur. Furthermore, adding the composite emulsifier may introduce foreign matter residues, affecting product quality and market acceptance. High-pressure homogenization can only improve dispersibility in the short term and cannot fundamentally eliminate the crystallization inducing factor.

[0074] In view of this, this application provides a method and apparatus for preventing the crystallization of diglyceride oil.

[0075] In a first aspect, this application provides a method for preventing the crystallization of diglyceride oil, comprising the following steps: Step 1, Preheating and Homogenization: The diglyceride oil to be processed is preheated and homogenized to obtain homogenized diglyceride oil.

[0076] It should be noted that this application takes into account the possibility of small crystals precipitating in diglyceride oil at room temperature. Therefore, this application first preheats the diglyceride oil to be treated to dissolve any small crystals that may precipitate in the oil, thereby promoting the homogenization of the diglyceride oil and improving the processing effect of subsequent processing steps.

[0077] This application does not limit the specific preheating and homogenization treatment temperature, as long as it achieves the intended effect. For example, in some embodiments of this application, the preheating and homogenization treatment temperature is 35℃~45℃. Based on the above scheme, it is possible to promote uniform mixing of diglyceride oil while minimizing nutrient loss.

[0078] For example, the preheating homogenization process temperature is 35°C, 36°C, 37°C, 38°C, 39°C, 40°C, 41°C, 42°C, 43°C, 44°C, 45°C, or any two of the above values.

[0079] This application does not limit the specific processing time for preheating and homogenization, as long as the purpose of this application can be achieved.

[0080] In some embodiments of this application, the preheating and homogenization process takes 30 to 60 minutes. This is to ensure that any small crystals that may precipitate in the diglyceride oil are completely dissolved.

[0081] For example, the preheating homogenization treatment time is 30 min, 35 min, 40 min, 45 min, 50 min, 55 min, 60 min, or any two of the above values.

[0082] In some embodiments of this application, the preheating and homogenization process is carried out under stirring, and the stirring rate is 50 rpm to 100 rpm.

[0083] For example, the stirring rate during the preheating and homogenization process is 50 rpm, 55 rpm, 60 rpm, 65 rpm, 70 rpm, 75 rpm, 80 rpm, 85 rpm, 90 rpm, 95 rpm, 100 rpm, or any two of the above values.

[0084] This application does not limit the specific composition of the diglyceride oil. The appropriate diglyceride oil to be treated can be used according to actual needs. For example, in some embodiments of this application, the purity of the diglyceride oil to be treated is 85%~95%, the residual triglyceride content is ≤10%, and the free fatty acid content is ≤3%.

[0085] Step 2, Adsorption treatment: A composite filter aid is added to homogenized diglyceride oil, and adsorption treatment is carried out under stirring or ultrasonication to obtain an adsorption-treated mixture. The composite filter aid includes diatomaceous earth and silica gel powder.

[0086] It should be noted that this application takes into account that triglyceride polymers and tiny crystal nuclei that may exist in diglyceride oil are likely to act as crystallization nuclei, thereby causing the diglyceride oil to crystallize and precipitate.

[0087] This application considers that diatomaceous earth possesses a porous siliceous mineral framework, whose porous structure facilitates the capture of substances such as triglyceride polymers and microcrystal nuclei, allowing the target product to pass through, thereby separating triglyceride polymers and microcrystal nuclei that may be present in diglyceride oil. Furthermore, this porous siliceous mineral framework is not only highly rigid, ensuring the stability of the porous structure and maintaining its filtration capacity during the filtration process. Silica powder, on the other hand, is amorphous silica with nanoscale three-dimensional network micropores, possessing a large specific surface area and good adsorption capacity. This application, by compounding silica powder with diatomaceous earth, not only achieves the respective functions of each component but also allows the silica powder to fill the gaps in the diatomaceous earth, thereby further enhancing the adsorption and removal of triglyceride polymers and microcrystal nuclei, as well as other possible impurities (such as soluble pigments), in diglyceride oil, further improving the filtration effect. Therefore, this application uses a composite filter aid with diatomaceous earth and silica powder as the main components to adsorb the preheated and homogenized diglyceride oil. This allows the diatomaceous earth and silica powder to form a composite filter aid with rigid spacing, porous structure, and fine adsorption effect, which can better adsorb and remove triglyceride polymers and microcrystal nuclei. Then, through filtration, the composite filter aid formed by diatomaceous earth and silica powder can better form a highly permeable filter layer, thereby preferentially removing triglyceride polymers and microcrystal nuclei from the diglyceride oil, thus effectively preventing the crystallization and precipitation of diglyceride oil.

[0088] In some embodiments of this application, the particle size D50 of diatomaceous earth is 5μm~45μm, preferably 15μm~30μm. Based on the above scheme, diatomaceous earth can better cooperate with silica gel powder, thereby better removing triglyceride polymers and crystal nuclei such as microcrystals from diglyceride oil.

[0089] The silica powder has a particle size of 30-60 mesh and a specific surface area of ​​300 m². 2 / g~600m 2 / g, with a pore volume of 0.6mL / g~1.1mL / g. Based on the above scheme, silica powder can better combine with diatomaceous earth, thereby better removing triglyceride polymers and microcrystal nuclei from diglyceride oil.

[0090] This application does not limit the specific amount of composite filter aid added; the amount of composite filter aid added should be based on the actual mass of the diglyceride oil. For example, in some embodiments of this application, the amount of composite filter aid added is based on the mass of the diglyceride oil to be treated. a ,and a Satisfying 0.5%≤ a ≤2.0%, meaning the amount of composite filter aid added is 0.5%~2.0% of the mass of the diglyceride oil to be treated.

[0091] For example, a The range is 0.5%, 0.6%, 0.8%, 1.0%, 1.2%, 1.4%, 1.6%, 1.8%, 2.0%, or any two of the above values.

[0092] In some embodiments of this application, the mass ratio of diatomaceous earth to silica gel powder in the composite filter aid is 6-7:3-4. Based on the above scheme, it is beneficial for better coordination between diatomaceous earth and silica gel powder, and better removal of triglyceride polymers and crystal nuclei such as microcrystals, thereby further avoiding the crystallization and precipitation of diglyceride oil.

[0093] For example, in the composite filter aid, the mass ratio of diatomaceous earth to silica gel powder is 6-4, 6.5:3.5, 7:3, or any two of the above values.

[0094] In some embodiments of this application, adsorption treatment is performed under stirring, and this application does not limit the specific stirring rate, as long as the function of this application can be achieved. For example, in some embodiments of this application, the stirring rate for adsorption treatment is 60 rpm to 100 rpm.

[0095] For example, the stirring rate of the adsorption treatment is 60 rpm, 65 rpm, 70 rpm, 75 rpm, 80 rpm, 85 rpm, 90 rpm, 95 rpm, 100 rpm or any two of the above values.

[0096] In some embodiments of this application, adsorption treatment is performed under ultrasonic action, and this application does not limit the specific ultrasonic power, as long as the desired effect of this application can be achieved. For example, in some embodiments of this application, the ultrasonic power of the adsorption treatment is 500W~800W.

[0097] For example, the ultrasonic power of the adsorption treatment is 500W, 550W, 600W, 650W, 700W, 750W, 800W or any combination of two of the above values.

[0098] This application does not limit the specific processing time of the adsorption treatment, as long as the function of this application can be achieved. For example, in some embodiments of this application, the processing time of the adsorption treatment is 20 min to 40 min.

[0099] For example, the adsorption treatment time is 20 min, 22 min, 24 min, 26 min, 28 min, 30 min, 32 min, 34 min, 36 min, 38 min, 40 min, or any two of the above values.

[0100] Step 3, filtration process: The mixture after adsorption treatment is filtered to obtain a clear oil phase and a turbid oil phase retained by the filter cake.

[0101] It is understood that the main components of both the clear and turbid oil phases obtained in this application include diglyceride oil. The clear oil phase is composed of components that have removed triglyceride polymers and microcrystal nuclei, and does not contain free fatty acids or high-melting-point diglyceride oil isomers. The turbid oil phase, on the other hand, presents a turbid appearance due to the presence of free fatty acids (FFA) and some high-melting-point diglyceride oil isomers. Therefore, the obtained clear oil phase can be directly processed into the finished product. Although the obtained turbid oil phase contains impurities such as free fatty acids (FFA) and some high-melting-point diglyceride oil isomers, it still contains a large amount of diglyceride oil. Discarding it would result in resource waste and increased processing costs. Therefore, this application further processes the turbid oil phase to remove the free fatty acids (FFA) and some high-melting-point diglyceride oil isomers, and then processes it together with the clear oil phase to produce the finished product. This approach ensures the yield of the finished product while effectively preventing the crystallization of diglyceride oil.

[0102] This application does not limit the specific method of filtration, as long as it achieves the intended function. For example, in some embodiments of this application, a plate and frame filter is used for filtration, with a filtration pressure of 0.3 MPa to 0.6 MPa and a filtration temperature maintained at 38°C to 42°C. Based on the above scheme, when the plate and frame filter is working, the liquid to be filtered enters each filter chamber through the feed port of the plate and frame filter. Through the filter cloth, solids are trapped in the filter chamber and gradually form a filter cake; the liquid is discharged from the machine through the water outlet on the plate and frame. As the filtration process proceeds, filter cake filtration begins, the filter cake thickness gradually increases, and the filtration resistance increases. The longer the filtration time, the higher the separation efficiency, which is beneficial for clarifying the separation of the oil phase and other components.

[0103] In some embodiments of this application, when using a plate and frame filter for filtration, the mesh size of the filter cloth is 500 to 800 mesh. Based on the above scheme, it is beneficial to clarify the oil phase and better separate it from other components.

[0104] Step 4, enzymatic hydrolysis: An enzyme preparation was added to the turbid oil phase, and enzymatic hydrolysis was carried out under stirring to obtain the enzymatic hydrolysis product.

[0105] It should be noted that this application further adds enzyme preparations to enzymatically hydrolyze the free fatty acids and some high-melting-point diglyceride oil isomers in the turbid oil phase, thereby transforming the turbid oil phase into a clear oil phase.

[0106] The enzyme preparation used in this application includes lipase, phospholipase, and enzyme stabilizer; and the mass ratio of lipase, phospholipase, and enzyme stabilizer in the enzyme preparation is 50~60:25~35:5~15. Based on the above scheme, it is possible to ensure enzymatic hydrolysis efficiency while ensuring that other components are not affected.

[0107] This application does not limit the specific type of lipase, as long as it can achieve the function of this application. For example, in some embodiments of this application, the lipase used is a lipase from Candida antarctica.

[0108] This application does not limit the specific type of phospholipase, as long as it can achieve the functions of this application. For example, in some embodiments of this application, the phospholipase used includes Novozymes phospholipase and / or Novozymes lipase 435. It should be noted that Novozymes phospholipase, also known as Lecitase® Ultra, is a carboxylate hydrolase (EC 3.1.1.3) obtained from Thermomyces lanuginosus / Fusarium oxysporum through protein engineering; it is produced by deep fermentation of a genetically modified Aspergillus oryzae microorganism. Lecitase Ultra has the inherent activity of hydrolyzing both phospholipid and triglyceride structures. Novozymes lipase 435, also known as Novozym435, is a lipase obtained from (B-lipase) Candidaantarctica; it is prepared by deep fermentation of a genetically modified Aspergillus oryzae microorganism and absorption onto a macroporous resin.

[0109] This application does not limit the specific type of enzyme stabilizer, as long as it can achieve the functions of this application. For example, in some embodiments of this application, the enzyme stabilizers used include the complex enzyme stabilizer AES and enzyme stabilizer M. It should be noted that the complex enzyme stabilizer AES is also called Enzyme Stabilizer AES.

[0110] This application does not limit the specific amount of enzyme preparation added; the appropriate amount of enzyme preparation should be added based on the actual mass of the turbid oil phase. For example, in some embodiments of this application, the amount of enzyme preparation added is based on the mass of the turbid oil phase. b ,and b Satisfying 0.3%≤ b ≤0.8%, meaning the amount of enzyme preparation added is 0.3%~0.8% of the mass of the turbid oil phase. Based on the above scheme, it is beneficial that the added enzyme preparation can fully enzymatically hydrolyze the free fatty acids and some high-melting-point diglyceride oil isomers in the turbid oil phase.

[0111] For example, b The range is 0.3%, 0.35%, 0.4%, 0.45%, 0.5%, 0.55%, 0.6%, 0.65%, 0.7%, 0.75%, 0.8%, or any two of the above values.

[0112] In some embodiments of this application, the enzymatic hydrolysis treatment temperature is 45℃~55℃. Based on the above, not only can enzymatic hydrolysis of free fatty acids and some high-melting-point diglyceride oil isomers be achieved, but the treatment temperature is also lower than that of traditional oil processing, which helps to reduce energy consumption.

[0113] For example, the enzymatic hydrolysis treatment temperature is 45℃, 46℃, 47℃, 48℃, 49℃, 50℃, 51℃, 52℃, 53℃, 54℃, 55℃ or any two of the above values.

[0114] In some embodiments of this application, the enzymatic hydrolysis treatment time is 2 to 4 hours. Based on the above, it is possible to further shorten the treatment time while achieving enzymatic hydrolysis of free fatty acids and some high-melting-point diglyceride oil isomers, which is beneficial for further reducing energy consumption.

[0115] For example, the enzymatic hydrolysis treatment time is 2h, 2.2h, 2.4h, 2.6h, 2.8h, 3.0h, 3.2h, 3.4h, 3.6h, 3.8h, 4h or any two of the above values.

[0116] In some embodiments of this application, the stirring rate of the enzymatic hydrolysis process is 60 rpm to 100 rpm. Based on the above, it is possible to ensure sufficient contact between the turbid oil phase and the enzyme preparation, thereby improving the enzymatic hydrolysis efficiency and effect on free fatty acids and some high-melting-point diglyceride oil isomers.

[0117] For example, the stirring rate of the enzymatic hydrolysis is 60 rpm, 65 rpm, 70 rpm, 75 rpm, 80 rpm, 85 rpm, 90 rpm, 95 rpm, 100 rpm or any two of the above values.

[0118] Step 5, inactivation treatment: After adding water to the enzymatic hydrolysis product and mixing, the pH of the system was adjusted to 5.5-6.5, followed by inactivation treatment and centrifugation to obtain the enzymatic hydrolysis clear oil phase.

[0119] It should be noted that this application adjusts the pH to 5.5-6.5 so that the enzyme can be better inactivated under this pH environment.

[0120] In some embodiments of this application, the mass ratio of the enzymatic hydrolysis product to water is 1:0.8~1.2. Based on the above scheme, the viscosity of the enzymatic hydrolysis product can be reduced without increasing the difficulty of subsequent processing, so as to better and more accurately adjust the pH of the enzymatic hydrolysis product to 5.5~6.5, thereby better inactivating the enzyme and terminating the enzymatic hydrolysis reaction.

[0121] For example, the mass ratio of the enzymatic hydrolysis product to water is 1:0.8, 1:0.9, 1:1, 1:1.1, 1:1.2 or any two of the above values.

[0122] In some embodiments of this application, the inactivation treatment temperature is 80°C to 85°C. Based on the above scheme, it is beneficial to improve the inactivation efficiency.

[0123] For example, the inactivation treatment temperature is 80°C, 81°C, 82°C, 83°C, 84°C, 85°C, or any two of the above values.

[0124] In some embodiments of this application, the inactivation treatment time is 15-20 minutes. Based on the above scheme, it is beneficial to further improve the inactivation efficiency.

[0125] For example, the inactivation treatment time is 15 min, 16 min, 17 min, 18 min, 19 min, 20 min, or any two of the above values.

[0126] In some embodiments of this application, the centrifugation rate is 8000 rpm to 10000 rpm and the centrifugation time is 8 min to 12 min.

[0127] For example, the centrifugation rate of the centrifugation process is 8000 rpm, 8200 rpm, 8400 rpm, 8600 rpm, 8800 rpm, 9000 rpm, 9200 rpm, 9400 rpm, 9600 rpm, 9800 rpm, 10000 rpm or a range of any two of the above values.

[0128] For example, the centrifugation time for centrifugation is 8 min, 9 min, 10 min, 11 min, 12 min, or any range of two of the above values.

[0129] Step 6, Post-processing: The clarified oil phase and the enzymatically hydrolyzed clear oil phase are mixed and then deodorized under vacuum, followed by aseptic filling to obtain the anti-crystallization diglyceride oil product.

[0130] It should be noted that in some embodiments of this application, the volume ratio of the clarified oil phase to the enzymatically hydrolyzed clear oil phase is 85~95:5~15.

[0131] In some embodiments of this application, the vacuum degree during vacuum deodorization is -0.08MPa ~ -0.09MPa, and the processing temperature is 48℃ ~ 65℃.

[0132] For example, the processing temperature during vacuum deodorization is 48°C, 50°C, 52°C, 54°C, 56°C, 58°C, 60°C, 62°C, 64°C, 65°C, or any combination of two of the above values.

[0133] Secondly, this application provides a device for preventing the crystallization of diglyceride oil.

[0134] It is understood that the apparatus of this application is constructed based on any one of the methods in the first aspect. Therefore, the processing principle of the apparatus of this application during use is consistent with any one of the methods in the first aspect, and has all the beneficial effects brought about by the method itself in the first aspect. Therefore, this application will not repeat the details here, please refer to the content described in the first aspect of this application.

[0135] Figure 1 This is a schematic diagram of a device for preventing the crystallization of diglyceride oil according to this application.

[0136] like Figure 1 The apparatus shown includes a preheating homogenizing device 100, an adsorption reaction device 200, a filtration device 300, an enzymatic hydrolysis device 400, a centrifugation device 500, a vacuum deodorization device 600, and a conveying device 700 for connecting the various devices, all connected in sequence.

[0137] In this application, the conveying device 700 includes a plurality of conveying pipes, such as at least a first conveying pipe 701, a second conveying pipe 702, a third conveying pipe 703, a fourth conveying pipe 704, a fifth conveying pipe 705, and a sixth conveying pipe 706.

[0138] In this application, the preheating homogenizing device 100 is used to preheat and homogenize the diglyceride oil to be processed.

[0139] In this application, the input end of the adsorption reaction device 200 is connected to the output end of the preheating homogenizing device 100 through a first conveying pipe 701 to receive the homogenized diglyceride oil obtained by the preheating homogenizing device 100, and to perform adsorption treatment in the adsorption reaction device 200.

[0140] In this application, the input end of the filtration device 300 is connected to the output end of the adsorption reaction device 200 via a second conveying pipe 702 to receive the mixture obtained by adsorption treatment in the adsorption reaction device 200 and to filter it to remove triglyceride polymers and microcrystal nuclei adsorbed in the composite filter aid, thereby obtaining a clear oil phase and a turbid oil phase retained by the filter cake. The filtration device 300 has a clear oil phase output end 301 and a turbid oil phase output end 302.

[0141] In this application, the enzymatic hydrolysis device 400 includes an enzymatic hydrolysis reactor 401. The input end of the enzymatic hydrolysis reactor 401 is connected to the output end of the turbid oil phase through a third conveying pipe 703 to receive the turbid oil phase obtained after filtration by the filtration device 300, and to perform enzymatic hydrolysis and inactivation treatment on the turbid oil phase. The enzymatic hydrolysis reactor 401 also has an enzyme preparation input end 402 for adding enzyme preparations.

[0142] In this application, the input end of the centrifuge device 500 is connected to the output end of the enzymatic hydrolysis reactor 401 through a fourth conveying pipe 704, so that the inactivated material enters the centrifuge device 500 for centrifugation.

[0143] In this application, the input end of the vacuum deodorization device 600 is connected to the output end of the centrifugation device 500 through a fifth conveying pipe 705, and the input end of the vacuum deodorization device 600 is also connected to the clarified oil phase output end 301 through a sixth conveying pipe 706, so as to facilitate the mixing of the clarified oil phase and the enzymatically hydrolyzed clear oil phase obtained by centrifugation.

[0144] Figure 2 This is a schematic diagram of a preheating homogenizing device according to this application.

[0145] In some embodiments of this application, the structure of the preheating homogenizing device 100 is as follows: Figure 2 As shown, the preheating homogenizing device 100 includes a preheating homogenizing tank 101, which has a diglyceride oil inlet 102 for adding diglyceride oil to be processed.

[0146] Figure 3 This is a schematic diagram of the architecture and connection of a preheating homogenizing device according to this application.

[0147] In some embodiments of this application, the preheating homogenizing device 100 of this application is... Figure 2 Based on the above, a heating module 103 and a temperature detection module 104 are also provided, and their connection structure is as follows: Figure 3 As shown, the heating module 103 is used to heat the preheating homogenizing tank 101 to provide suitable temperature conditions for the preheating homogenization process; the temperature detection module 104 is used to detect the temperature in the preheating homogenizing tank 101 in real time so that the temperature provided by the heating module 103 is stabilized within the temperature range required for the preheating homogenization process.

[0148] Please refer to some embodiments of this application. Figure 2 The bottom of the preheating homogenizing tank 101 is provided with a heat transfer oil jacket 105, and the heating module 103 is disposed in the heat transfer oil jacket 105 so as to heat the heat transfer oil jacket 105 through the heating module 103, thereby realizing the heating of the preheating homogenizing tank 101.

[0149] Please refer to some embodiments of this application. Figure 2The preheating homogenizing tank 101 is equipped with a first stirring module 106 to stir the diglyceride oil to be treated, thereby promoting uniform heating of the oil. This application does not limit the specific structure or type of the first stirring module 106, as long as it achieves the function of this application. For example, in some embodiments of this application, the first stirring module 106 includes a spiral stirring paddle.

[0150] Figure 4 This is a schematic diagram of an adsorption reaction device according to this application.

[0151] In some embodiments of this application, the structure of the adsorption reaction device 200 is as follows: Figure 4 As shown, the adsorption reaction device 200 includes an adsorption reaction vessel 201. The input end of the adsorption reaction vessel 201 is connected to the output end of the preheating homogenization device 100 via a first conveying pipe 701. The adsorption reaction vessel 201 has a composite filter aid inlet 202, which is used to add composite filter aid so that the homogenized diglyceride oil and composite filter aid are adsorbed within the adsorption reaction device 200. An adsorption auxiliary device 203 is provided inside the adsorption reaction vessel 201. The adsorption auxiliary device 203 includes an ultrasonic generator or a second stirring module, which provides ultrasonic action for the adsorption process via the ultrasonic generator or stirring action via the second stirring module.

[0152] Figure 5 This is a schematic diagram of the architecture of a filtering device in this application.

[0153] In some embodiments of this application, the filtering device 300 of this application is... Figure 1 Based on the above, the filtration device 300 also includes a pressure sensor 303 and a first temperature control module 304. The pressure sensor 303 is used to maintain the filtration pressure of the filtration process at 0.3MPa~0.6MPa, and the first temperature control module 304 is used to maintain the filtration temperature at 38℃~42℃.

[0154] For example, the filtration device 300 of this application is a plate and frame filter equipped with a pressure sensor 303 and a first temperature control module 304.

[0155] Figure 6 This is a schematic diagram of the architecture of an enzymatic hydrolysis device according to this application.

[0156] In some embodiments of this application, the enzymatic hydrolysis device 400 of this application is... Figure 1Based on the above, the enzymatic hydrolysis reactor 401 further includes a pH monitoring module 403, a second temperature control module 404, and a third stirring module 405. The pH monitoring module monitors the pH value of the materials within the reactor body to control it within the desired pH range. The second temperature control module adjusts the reaction temperature within the reactor body to the temperature for enzymatic hydrolysis or inactivation treatment according to the reaction progress. The third stirring module provides the required stirring rate for enzymatic hydrolysis to promote thorough mixing of the turbid oil phase and the enzyme preparation, thereby improving the efficiency of the enzymatic hydrolysis process.

[0157] Figure 7 This is a schematic diagram of the architecture and connection of a centrifuge device according to this application.

[0158] In some embodiments of this application, the centrifuge device 500 of this application is... Figure 1 Based on the above, the centrifugation device 500 further includes a third temperature control module 501 to control the temperature of the centrifugation process within the required range.

[0159] In some embodiments of this application, a thermal insulation layer is provided on the first conveying pipe 701 to ensure that the diglyceride oil remains homogeneous during the conveying process. This application does not limit the specific material of the thermal insulation layer, as long as it can achieve the function of this application.

[0160] In some embodiments of this application, a first pump body is provided on the first delivery pipe 701, and the first pump body is used to adjust the delivery rate when homogenized diglyceride oil is delivered into the adsorption reaction device 200.

[0161] In some embodiments of this application, a second pump body is provided on the second conveying pipe 702, and the second pump body is used to adjust the conveying rate of the mixture obtained by adsorption treatment into the filter device 300.

[0162] In some embodiments of this application, a third pump body is provided on the third conveying pipe 703, and the third pump body is used to adjust the conveying rate when the turbid oil is conveyed in the phase-to-phase enzymatic hydrolysis device 400.

[0163] In some embodiments of this application, a fourth pump body is provided on the fourth conveying pipe 704, and the fourth pump body is used to adjust the conveying rate of the inactivated material when it is conveyed into the centrifuge device 500.

[0164] In some embodiments of this application, a fifth pump body is provided on the fifth conveying pipe 705, and the fifth pump body is used to adjust the conveying rate when the enzymatically hydrolyzed clear oil obtained by centrifugation is conveyed in the vacuum deodorization device 600.

[0165] In some embodiments of this application, a sixth pump body is provided on the sixth conveying pipe 706, and the sixth pump body is used to adjust the conveying rate when the clarified grease is conveyed into the vacuum deodorization device 600.

[0166] The physical properties mentioned in this application can be measured using the following methods, and the physical properties in the following embodiments and comparative examples are measured using the following methods.

[0167] Storage performance stability test: This application evaluates the storage stability of diglyceride oil products by considering both their transparency and crystallization. Higher transparency and absence of crystallization after a certain storage period indicate better storage stability.

[0168] 1. Transparency test: The transparency was obtained according to the transparency test method in GB / T 5525-2025 "Identification of Transparency, Odor and Taste of Vegetable Oils".

[0169] 2. Crystallization test: You can directly observe with the naked eye whether there is any solid precipitation and whether the product becomes cloudy.

[0170] The following examples and comparative examples illustrate the implementation of this application in more detail. It should be noted that in the following examples and comparative examples, the lipase used is a lipase from *Candida antarctica*, purchased from Qingdao Weilan Biotechnology Co., Ltd. The Novozymes phospholipase used is Lecitase® Ultra manufactured by Novozymes Denmark; the Novozymes lipase 435 used is Novozym 435 manufactured by Novozymes Denmark; the complex enzyme stabilizer AES used is a complex enzyme stabilizer purchased from BASF SE (BASF); and the enzyme stabilizer M used is enzyme stabilizer M manufactured by Novozymes Denmark.

[0171] Example 1 This embodiment provides a method for preventing diglyceride oil from crystallizing, including the following steps: Step 1, Preheating and Homogenization: Using 90% pure diglyceride oil as the diglyceride oil to be treated, 100 kg was preheated to 40°C and then stirred at 60 rpm for 45 min at 40°C to obtain homogenized diglyceride oil.

[0172] Step 2, Adsorption treatment: Add 1.2 kg of composite filter aid (65% diatomaceous earth and 35% silica gel powder) to the homogenized diglyceride oil, and stir at 70 rpm for 30 min to obtain the adsorption-treated mixture.

[0173] Step 3, filtration process: The adsorption-treated mixture was filtered using a plate and frame filter at a temperature of 40°C and a pressure of 0.4 MPa. 92 kg of clear oil phase and 8 kg of turbid oil phase were collected.

[0174] Step 4, enzymatic hydrolysis: Add 0.05 kg of enzyme preparation (55% lipase, 30% phospholipase, and 15% enzyme stabilizer) to the turbid oil phase obtained in step 3, and perform enzymatic hydrolysis at 50°C and 80 rpm for 3 hours to obtain the enzymatic hydrolysis product.

[0175] Step 5, inactivation treatment: Add 8 kg of deionized water to the enzymatic hydrolysis product obtained in step 4, mix, adjust the pH of the system to 6.0, then inactivate at 82℃ for 20 min, and then centrifuge at 9000 rpm for 10 min to obtain 7.5 kg of enzymatic hydrolysis clear oil phase.

[0176] Step 6, Post-processing: After mixing the clarified oil phase obtained in step 6 with the enzymatically hydrolyzed clear oil phase obtained in step 3, the mixture was vacuum deodorized at -0.085 MPa and 50°C, and then aseptically filled to obtain the anti-crystallization diglyceride oil product.

[0177] Examples 2 to 5, and Comparative Examples 1 and 2, differ from Example 1 only in that: Adjust the amount of composite filter aid added according to Table 1.

[0178] Comparative Example 1 did not add any composite filter aid.

[0179] Comparative Example 2 uses the existing technology CN107981319 A's composite emulsifier addition method, adding 1.0% composite emulsifier (65% mono- and diglyceride fatty acid esters, 25% polyglycerol esters, and 10% sorbitan tristearate) to the same raw material diglyceride oil.

[0180] Examples 6 to 9 and Comparative Example 3 differ from Example 1 only in that: Adjust the mass ratio of diatomaceous earth to silica gel powder in the composite filter aid according to Table 1. For ease of description, this application uses M1 to represent the mass ratio of diatomaceous earth to silica gel powder in the composite filter aid.

[0181] In Comparative Example 3, the filter aid used was diatomaceous earth (without silica gel powder).

[0182] The diglyceride oil products obtained in each example and Comparative Example 1 were stored at a temperature of 4°C, and the crystallization and transparency were monitored after 1 month, 2 months, 3 months, 6 months, 15 months, 20 months and 24 months of storage. The results of the storage stability test are summarized in Table 1.

[0183] Table 1

[0184] According to the test results in Table 1, it is clear that, compared with the prior art of Comparative Example 2, Examples 1 to 9 of this application can all be stored at 4°C for more than 15 months without crystallization and with a transparency of ≥95%. This indicates that this application, through sequential preheating and homogenization treatment, adsorption filtration with composite filter aid, selectively removes the initial crystallization core material, and then performs targeted enzymatic hydrolysis on the turbid oil phase obtained by filtration, can completely destroy the conditions for crystallization formation, effectively eliminate the crystallization inducing factors from the root, and achieve long-term stable storage of oil.

[0185] By comparing the test results of Examples 1 to 5 in Table 1 with those of Comparative Example 1, it is clear that when a composite filter aid is used, it can promote the removal of initial crystallization nuclei, thereby facilitating the long-term stable storage of oils and fats. In particular, when the amount of composite filter aid added... a Satisfying 0.5%≤ a At ≤2.0%, it is possible to better remove the initial crystallization core material and better improve the long-term stable storage performance of oils and fats.

[0186] By comparing the test results of Examples 6 to 9 in Table 1 with those of Comparative Example 3, it is clear that when the composite filter aid includes diatomaceous earth and silica gel powder, the synergistic effect of diatomaceous earth and silica gel powder can remove the initial crystallization core material, thereby facilitating the long-term stable storage of oils. In particular, when the mass ratio of diatomaceous earth to silica gel powder in the composite filter aid is 6~7:3~4, the long-term stable storage performance of oils can be further improved.

[0187] Examples 10 to 14 differ from Example 1 only in that: Adjust the amount of enzyme preparation added according to Table 2. b .

[0188] Examples 15 to 17 differ from Example 1 only in that: According to Table 2, the mass ratio of lipase, phospholipase, and enzyme stabilizer in the enzyme preparation is adjusted. For ease of description, this application uses M2 to represent the mass ratio of lipase, phospholipase, and enzyme stabilizer in the enzyme preparation.

[0189] Table 2

[0190] Based on the test results in Table 2, it is clear that this application, through sequential preheating and homogenization treatment, adsorption filtration with a composite filter aid, selectively removes the initial crystallization core substances. Then, by performing targeted enzymatic hydrolysis on the turbid oil obtained after filtration relative to the free fatty acids and some high-melting-point diglyceride oil isomers in the turbid oil phase, the conditions for crystallization formation are completely destroyed, effectively eliminating the inducing factors for crystallization from the root, and achieving long-term stable storage of the oil. In particular, when the amount of enzyme preparation added... b Satisfying 0.3%≤ b At a concentration of ≤0.8%, it is possible to better achieve targeted enzymatic hydrolysis of free fatty acids and some high-melting-point diglyceride oil isomers in the turbid oil phase, thereby better improving the long-term stable storage performance of the oil.

[0191] The test results in Table 2 further clarify that when the enzyme preparation includes lipase, phospholipase, and enzyme stabilizer, the synergistic effect of these enzymes effectively enables targeted enzymatic hydrolysis of free fatty acids and some high-melting-point diglyceride oil isomers in the turbid oil phase, thus facilitating long-term stable storage of the oil. In particular, when the mass ratio of lipase, phospholipase, and enzyme stabilizer in the enzyme preparation is 50–60:25–35:5–15, the long-term stable storage performance of the oil is further improved.

[0192] Obviously, the above embodiments of this application are merely examples for clear illustration and are not intended to limit the implementation of this application. Those skilled in the art can make other variations or modifications based on the above description. It is neither necessary nor possible to exhaustively list all possible implementations here. Any modifications, equivalent substitutions, and improvements made within the spirit and principles of this application should be included within the scope of protection claimed by this application.

Claims

1. A method for preventing the crystallization of diglyceride oil, characterized in that, Includes the following steps: The diglyceride oil to be processed is preheated and homogenized to obtain homogenized diglyceride oil; A composite filter aid is added to homogenized diglyceride oil, and adsorption treatment is carried out under stirring or ultrasonic treatment to obtain an adsorption-treated mixture; wherein, the composite filter aid includes diatomaceous earth and silica gel powder. The mixture after adsorption treatment is filtered to obtain a clear oil phase and a turbid oil phase retained by the filter cake. An enzyme preparation is added to the turbid oil phase, and enzymatic hydrolysis is performed under stirring to obtain the enzymatic hydrolysis product; the enzyme preparation includes lipase, phospholipase and enzyme stabilizer; Water was added to the enzymatic hydrolysis product and mixed. The pH of the system was adjusted to 5.5-6.5, followed by inactivation treatment and centrifugation to obtain the enzymatic hydrolysis clear oil phase. The clarified oil phase and the enzymatically hydrolyzed clarified oil phase are mixed and then vacuum deodorized, followed by aseptic filling to obtain the anti-crystallization diglyceride oil product.

2. The method according to claim 1, characterized in that, Based on the mass of the diglyceride oil to be treated, the amount of the composite filter aid added is: a ,and a Satisfying 0.5%≤ a ≤2.0%; In the composite filter aid, the mass ratio of diatomaceous earth to silica gel powder is 6~7:3~4.

3. The method according to claim 1, characterized in that, The filtration process is carried out using a plate and frame filter with a filtration pressure of 0.3MPa~0.6MPa and a filtration temperature of 38℃~42℃.

4. The method according to claim 1, characterized in that, The preheating and homogenization treatment is carried out at a temperature of 35℃~45℃ for a time of 30min~60min.

5. The method according to claim 1, characterized in that, When performing adsorption treatment under stirring, the stirring rate is 60 rpm to 100 rpm; When performing adsorption treatment under ultrasonic action, the ultrasonic power is 500W~800W and the ultrasonic frequency is 10kHz~40kHz. The adsorption treatment time is 20 min to 40 min.

6. The method according to claim 1, characterized in that, In the enzyme preparation, the mass ratio of the lipase, the phospholipase and the enzyme stabilizer is 50~60:25~35:5~15; Based on the mass of the turbid oil phase, the amount of enzyme preparation added is: b ,and b Satisfying 0.3%≤ b ≤0.8%; The enzymatic hydrolysis treatment is carried out at a temperature of 45℃~55℃, for a time of 2h~4h, and with a stirring rate of 60rpm~100rpm.

7. The method according to claim 1, characterized in that, The mass ratio of the enzymatic hydrolysis product to water is 1:0.8~1.2; The inactivation treatment is performed at a temperature of 80℃~85℃ for 15min~20min. The centrifugation process is carried out at a centrifugation rate of 8000 rpm to 10000 rpm and a centrifugation time of 8 min to 12 min.

8. The method according to claim 1, characterized in that, The volume ratio of the clarified oil phase to the enzymatically hydrolyzed clear oil phase is 85~95:5~15; The vacuum degree during vacuum deodorization is -0.08MPa ~ -0.09MPa, and the processing temperature is 48℃~52℃.

9. The method according to claim 1, characterized in that, The purity of the diglyceride oil to be treated is 85%~95%, the residual triglyceride content is ≤10%, and the free fatty acid content is ≤3%.

10. An apparatus based on the method of any one of claims 1 to 9, characterized in that, The device includes: A preheating homogenizing device (100) is used to receive the diglyceride oil to be processed and to preheat and homogenize the diglyceride oil to be processed. An adsorption reaction device (200) is connected at its input end to the output end of the preheating homogenizing device (100) to receive the homogenized diglyceride oil obtained by the preheating homogenizing device (100) and adsorb it. A filtration device (300) has its input end connected to the output end of the adsorption reaction device (200) to receive the mixture obtained by adsorption treatment by the adsorption reaction device (200) and to filter it; the filtration device (300) has a clear oil phase output end (301) and a turbid oil phase output end (302). An enzymatic hydrolysis device (400) has its input end connected to the output end (302) of the turbid oil phase to receive the turbid oil phase obtained by filtration by the filtration device (300) and to perform enzymatic hydrolysis and inactivation treatment on the turbid oil phase; the enzymatic hydrolysis device (400) also has an enzyme preparation input end (402) for adding enzyme preparations; A centrifuge device (500) is provided, the input end of which is connected to the output end of the enzymatic hydrolysis device (400) so that the inactivated material enters the centrifuge device (500) for centrifugation. The vacuum deodorization device (600) has its input end connected to the output end of the centrifuge device (500), and the input end of the vacuum deodorization device (600) is also connected to the output end (301) of the clarified oil phase, so that the clarified oil phase and the enzymatically hydrolyzed clear oil phase obtained by centrifugation are mixed and then vacuum deodorized.

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