A preparation method of sodium phytate for oil-soluble food

By mixing sodium phytate with vegetable oil in a spray condensation storage device, the problem of insufficient solubility of sodium phytate in oily foods is solved, and the preparation of oil-soluble sodium phytate is achieved, with good antioxidant effect and stability, and the process is simple and suitable for large-scale production.

CN119111721BActive Publication Date: 2025-05-13JINGJIANG SHENJIN SCI&TECH CO LTD
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Patent Information

Application Number
CN202411377142.X
Authority / Receiving Office
CN · China
Patent Type
Patents(China)
Current Assignee / Owner
Filing Date
2024-09-30
Publication Date
2025-05-13
Estimated Expiration
2044-09-30

AI Technical Summary

Technical Problem

In the prior art, the solubility of sodium phytate in oils is too small, making it difficult to widely use in oily foods, and the existing process costs are high and the process is complex.

Method used

The microemulsion method is improved by using a spray condensation storage device, and sodium phytate is mixed with vegetable oil through spray condensation technology to form sodium phytate for oil-soluble foods. The process includes configuring the ratio of sodium phytate solution to vegetable oil, adding an emulsifier, and atomizing, mixing and liquefaction through high-pressure gas to finally obtain oil-soluble sodium phytate.

Benefits of technology

It has achieved good solubility, excellent antioxidant activity and stability of sodium phytate in oily foods, and has a simple process and common raw materials, which are suitable for large-scale production.

✦ Generated by Eureka AI based on patent content.

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Abstract

The invention discloses a method for preparing sodium phytate for oil-soluble food, comprising the following steps: step (1): preparing a sodium phytate solution with a concentration of 0.1-0.5% to obtain an aqueous phase; step (2): taking a vegetable oil with a volume of 2-5 times the aqueous phase obtained in step (1), adding an emulsifier with a volume of 0.01-0.05 of the aqueous phase as the oil phase, atomizing, mixing and liquefying the oil phase and the aqueous phase in a spray condensation storage device to obtain sodium phytate for oil-soluble food. The invention belongs to the technical field of food additives, has the characteristics of high dispersibility and good stability, can be effectively applied to oily foods, and prevents oxidation of oily foods.
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Description

Technical Field

[0001] The invention relates to the technical field of food additives, and in particular to a method for preparing sodium phytate for oil-soluble food. Background Art

[0002] The water solubility of sodium phytate determines its great potential for use in water-soluble foods, but it is not conducive to its widespread use in fat or oil-soluble foods. Although sodium phytate has a good antioxidant effect on oils such as rapeseed oil, soybean oil, lard, and peanut oil, the main problem in actual industrial production and use is that the solubility of water-soluble sodium phytate in oils is too low, and it needs to be further modified into a fat-soluble product through structure modification, or dispersed in oils through emulsification, microemulsion preparations, etc.

[0003] CN101390641A discloses the preparation and application of a class of edible oil antioxidants. The antioxidant is phytic acid amino acid ester salt. The present invention is characterized in that 1) alcohol and amino acid are first mixed, then thionyl chloride is added dropwise, and the amino acid ester is obtained by heating reaction; 2) phytic acid is dissolved in water, the phytic acid solution is adjusted to neutrality with amino acid ester, and dehydrated under reduced pressure to obtain phytic acid amino acid ester salt. The phytic acid amino acid ester salt prepared by the present invention is directly added to edible oil or first dissolved in a small amount of ethanol and then added to edible oil. The prepared phytic acid amino acid ester salt has good oil solubility, excellent antioxidant activity and stability in edible oil. Although this method can obtain a good oil solubility effect, it has the problems of high cost and complex process.

[0004] The microemulsion method is a low-cost and efficient process route. The current microemulsion method has problems such as poor emulsion dispersion and large water phase particle size. It is necessary to further reduce the particle size of the water phase droplets and improve the dispersion. Summary of the invention

[0005] To this end, the present invention provides a method for preparing sodium phytate for oil-soluble food to solve the above problems in the prior art.

[0006] In order to achieve the above object, the present invention provides the following technical solutions:

[0007] A method for preparing sodium phytate for oil-soluble food comprises the following steps:

[0008] Step (1): preparing a sodium phytate solution with a concentration of 0.1-0.5% to obtain an aqueous phase;

[0009] Step (2): Take 2-5 times the volume of the aqueous phase obtained in step (1), add 0.01-0.05 of the volume of the aqueous phase of the vegetable oil, as the oil phase, and atomize, mix and liquefy the oil phase and the aqueous phase in a spray condensation storage device to obtain sodium phytate for oil-soluble food.

[0010] The spray condensation storage device comprises a tower body and a condensation storage device, wherein a feed port is provided at the upper end of the tower body, and an oil inlet pipe and a water inlet pipe entering the tower body are connected to the feed port, the oil inlet pipe is coaxial with the water inlet pipe and is arranged inside the water inlet pipe, and an oil nozzle and a water nozzle are respectively provided at the lower ends of the oil inlet pipe and the water inlet pipe; the tower body is provided with an air inlet, and the air inlet is connected to the air inlet pipe entering the tower body, and the air inlet pipe is respectively connected to the oil nozzle and the water nozzle; a discharge port is provided at the bottom of the tower body, and a mist suction pile is provided at the discharge port, and one end of the mist suction pile extends into the tower body, and the other end thereof is connected to the condensation storage device.

[0011] Sodium phytate has poor oil solubility. As can be seen from the background technology, the microemulsion method is a low-cost and efficient process path. This scheme improves the microemulsion method through a spray condensation storage device. The basic working process of atomization of the spray condensation storage device is: the oil phase and the water phase are respectively introduced into the oil inlet pipe and the water inlet pipe, and the high-pressure gas is introduced into the air inlet pipe and respectively introduced into the oil nozzle and the water nozzle. Under the action of the gas pressure, the oil phase and the water phase are sprayed out and atomized. During the operation, the gas drives the oil phase and the water phase to spray out from the oil nozzle and the water nozzle. The stability and uniformity of the atomization are achieved by designing the formula ratio of the water phase and the oil phase, regulating the temperature of the oil inlet pipe and the water inlet pipe, and regulating the air pressure of the air inlet pipe. Since the particle size of the atomized droplets is micron-level, under the joint action of the nozzle gas and gravity during the spraying process, irregular movement occurs, achieving a uniform dispersion effect, and finally the atomized droplets are sucked into the condensation storage device through the mist suction pile and condensed and liquefied to obtain oil-soluble sodium phytate for food. The vegetable oil in the oil phase can be any edible vegetable oil, such as peanut oil, corn oil, olive oil or commercially available blended oil.

[0012] Preferably, the atomization, mixing and liquefaction in the spray condensation storage device include the following processes:

[0013] Step (a) Feeding: introducing the oil phase and the water phase into the oil inlet pipe and the water inlet pipe respectively;

[0014] Step (b) ventilation atomization: passing high-pressure gas through the air inlet pipe (2-1) into the oil nozzle and the water nozzle respectively to form atomized droplets in the tower body;

[0015] Step (c) atomization liquefaction: the atomized liquid droplets are sucked in and mixed by a mist suction pile and then collected in a condensation storage device to obtain sodium phytate for oil-soluble food.

[0016] Preferably, the HLB value of the emulsifier is 4-8.

[0017] Preferably, the emulsifier is one or more of Span 40, Span 60 and Span 80.

[0018] ‌HLB of emulsifier refers to the Hydrophilic Lipophilic Balance‌, which is an indicator used to indicate the hydrophilicity of the emulsifier. The size of the HLB value reflects the size and balance of the hydrophilic and lipophilic groups in the surfactant molecule, thus determining the hydrophilicity or lipophilicity of the surfactant. The larger the HLB value, the stronger the hydrophilicity of the surfactant; the smaller the HLB value, the stronger the lipophilicity of the surfactant.

[0019] Preferably, the amount of the emulsifier added is 0.01-0.03 of the volume of the sodium phytate solution; the amount of the emulsifier added satisfies the formula: 3dV / r.

[0020] The required amount of emulsifier satisfies the formula: 3dV / r, where d is the thickness of the emulsifier monolayer and r is the radius of the water phase droplet in the oil phase. The formula is derived as follows: Assuming that the volume of the sodium phytate solution is V, it is dispersed in the system as small droplets with a particle size of 2r, that is, the volume V1 is 4πr 3 / 3, the surface area S is 4πr 2 , it can be dispersed into n=V / V1 particles. Assuming that the thickness of the emulsifier film on the surface of the droplet is d, the volume of the emulsifier film required for each small droplet is Sd, that is, the total volume required is nSd, and 3dV / r is converted into 3d / r, which is 0.01-0.03.

[0021] Preferably, in step (b), the particle size of the atomized droplets is 5-10 μm.

[0022] Preferably, the oil spray head and water spray head are provided with oil spray micropores and water spray micropores on their surfaces, respectively. The oil spray micropores are provided with an oil inlet and an oil outlet, the oil inlet diameter is larger than the oil outlet, and the line connecting the oil inlet and the oil outlet does not pass through the axis of the oil inlet pipe; the water spray micropores are provided with a water inlet and a water outlet, the water inlet diameter is larger than the water outlet, and the line connecting the water inlet and the water outlet does not pass through the axis of the water inlet pipe. The reason why the lines connecting the oil inlet and the oil outlet and the water inlet and the water outlet do not pass through the axis of the oil inlet pipe is to provide a cyclone for the atomized droplets in the tower body, and to give the spray a tangential force, so that the atomized droplets are absorbed by the mist suction pile in a spiral descending motion process, thereby improving the dispersion of the atomized droplets in the tower body.

[0023] Preferably, in step (b), the pressure of the high-pressure gas is 0.1-2 MPa.

[0024] Preferably, in step (b), the temperature of the water phase in the water inlet pipe is 60-100°C.

[0025] The temperature of the water phase in the water inlet pipe is 60-100°C. The main purposes of controlling the water phase temperature are three: 1. Since the oil inlet pipe is arranged in the water inlet pipe, the water phase in the water inlet pipe heats the oil phase in the oil inlet pipe, which improves the fluidity of the oil phase and can better achieve the atomization effect of the oil phase; 2. Ensure the atomization environment temperature, prevent premature liquefaction, ensure the kinetic energy of the droplets, and improve dispersibility; 3. Prevent the precipitation of sodium phytate.

[0026] Preferably, a mist absorption hole is provided on the surface of the mist absorption pile, and the center line of the mist absorption hole does not pass through the axis of the mist absorption pile.

[0027] The design of the mist suction pile is to provide a low air pressure for the atomized liquid in the tower, so that the atomized droplets will eventually move toward the mist suction pile, reducing condensation and aggregation inside the tower body; the center line of the mist suction hole does not pass through the axis of the mist suction pile in order to allow the inhaled atomized droplets to continue to mix and gradually cool and liquefy. Sodium phytate microcrystals may precipitate from the water phase during the liquefaction process, but because the water phase has good dispersibility and small droplets, the microcrystals can also be evenly distributed and will not affect the final use. During the atomization and condensation process, when the oil phase contacts the water phase droplets, the dispersant in the oil phase will capture the water phase droplets and coat their surface, ultimately making the water phase droplets stable.

[0028] Compared with the existing technology, the advantages of this solution are:

[0029] 1. The preparation process of this scheme is simple, the raw materials are conventional, and it is suitable for large-scale production;

[0030] 2. The sodium phytate aqueous phase droplets for oil-soluble food prepared in this scheme have a small average particle size of about 5-10 microns, high dispersibility, and high stability, and can be effectively applied to oily foods to prevent their oxidation. BRIEF DESCRIPTION OF THE DRAWINGS

[0031] Figure 1 A cross-sectional view of a spray condensation storage device provided in Example 1 of the present invention;

[0032] Figure 2 A horizontal cross-sectional view of an oil spray nozzle of a spray condensation storage device provided in Example 1 of the present invention;

[0033] Figure 3 A vertical cross-sectional view of a water nozzle of a spray condensation storage device provided in Example 1 of the present invention;

[0034] Figure 4 A vertical cross-sectional view of a mist absorbing pile of a spray condensation storage device provided in Example 1 of the present invention;

[0035] Figure 5 A horizontal cross-sectional view of a mist absorbing pile of a spray condensation storage device provided in Example 1 of the present invention;

[0036] Figure 6A general spray device nozzle provided for Comparative Example 5;

[0037] In the figure: 1. tower body; 2. air inlet; 2-1. air inlet pipe; 3. feed inlet; 3-1. oil inlet pipe; 3-2. water inlet pipe; 3-3. oil nozzle; 3-3-1. oil spray micropores; 3-3-2. oil inlet; 3-3-3. oil outlet; 3-4. water nozzle; 3-4-1. water spray micropores; 3-4-2. water inlet; 3-4-3. water outlet; 4. feed outlet; 4-1. mist suction pile; 4-1-1. mist suction hole; 5. condensation storage device; 6-1. equal-diameter micropores. DETAILED DESCRIPTION

[0038] The following is a description of the implementation of the present invention by specific embodiments. People familiar with the art can easily understand other advantages and effects of the present invention from the contents disclosed in this specification. Obviously, the described embodiments are part of the embodiments of the present invention, not all of the embodiments. Based on the embodiments of the present invention, all other embodiments obtained by ordinary technicians in this field without creative work are within the scope of protection of the present invention.

[0039] Embodiment 1: A method for preparing sodium phytate for oil-soluble food, comprising the following steps:

[0040] Step (1): preparing a sodium phytate solution with a concentration of 0.2% to obtain an aqueous phase;

[0041] Step (2): taking 3 times the volume of the vegetable oil obtained in step (1) with the volume of the aqueous phase, adding 0.03 of the volume of the aqueous phase of Span 40 with an HLB of 4.6 as the oil phase, atomizing the oil phase and the aqueous phase in a spray condensation storage device, mixing and liquefying, and obtaining oil-soluble sodium phytate for food;

[0042] like Figure 1 As shown, the spray condensation storage device includes a tower body 1 and a condensation storage device 5. The upper end of the tower body is provided with a feed port 3, and the feed port 3 is connected to an oil inlet pipe 3-1 and a water inlet pipe 3-2 entering the tower body. The oil inlet pipe 3-1 is coaxial with the water inlet pipe 3-2 and is placed in the water inlet pipe 3-2. The lower ends of the oil inlet pipe 3-1 and the water inlet pipe 3-2 are respectively provided with an oil nozzle 3-3 and a water nozzle 3-4; the tower body is provided with an air inlet 2, and the air inlet 2 is connected to an air inlet pipe 2-1 entering the tower body. -1, the air inlet pipe 2-1 is connected to the oil nozzle 3-3 and the water nozzle 3-4 respectively; during the atomization process, the oil phase and the water phase are introduced from the oil inlet pipe 3-1 and the water inlet pipe 3-2 respectively, and are sprayed out from the oil nozzle 3-3 and the water nozzle 3-4 to be atomized along with the gas pressure introduced into the air inlet pipe 2-1; a discharge port 4 is provided at the bottom of the tower body, and a mist suction pile 4-1 is provided at the discharge port, one end of the mist suction pile 4-1 extends into the tower body, and the other end is introduced into the condensation storage device 5;

[0043] The atomization, mixing and liquefaction in the spray condensation storage device include the following processes:

[0044] Step (a) Feeding: The oil phase and the water phase are introduced into the oil inlet pipe 3-1 and the water inlet pipe 3-2 respectively, and the temperature of the water phase is 80°C;

[0045] Step (b) ventilation atomization: high-pressure gas with a pressure of 0.5 MPa is introduced into the oil nozzle 3-3 and the water nozzle 3-4 respectively, and the particle size of the atomized droplets is 8 μm;

[0046] Step (c) atomization liquefaction: the atomized liquid droplets are sucked and mixed by the atomization pile 4-1 and then collected in the condensation storage device 5 to obtain sodium phytate for oil-soluble food;

[0047] like Figure 2 and Figure 3 As shown, the surfaces of the oil spray head 3-3 and the water spray head 3-4 are respectively provided with oil spray micropores 3-3-1 and water spray micropores 3-4-1, the oil spray micropore 3-3-1 is provided with an oil inlet 3-3-2 and an oil outlet 3-3-3, the diameter of the oil inlet 3-3-2 is larger than the oil outlet 3-3-3, and the line connecting the oil inlet 3-3-2 and the oil outlet 3-3-3 does not pass through the axis of the oil inlet pipe 3-1; the water spray micropore 3-4-1 is provided with a water inlet 3-4-2 and a water outlet 3-4-3, the diameter of the water inlet 3-4-2 is larger than the water outlet 3-4-3, and the line connecting the water inlet 3-4-2 and the water outlet 3-4-3 does not pass through the axis of the water inlet pipe 3-2;

[0048] like Figure 4 As shown in Figure 5, a fog suction hole 4-1-1 is provided on the surface of the fog suction pile 4-1, and the center line of the fog suction hole 4-1-1 does not pass through the axis of the fog suction pile. The atomized liquid droplets are sucked in and collected through the suction hole.

[0049] Embodiment 2: A method for preparing sodium phytate for oil-soluble food, comprising the following steps:

[0050] Step (1): preparing a sodium phytate solution with a concentration of 0.5% to obtain an aqueous phase;

[0051] Step (2): taking 5 times the volume of the vegetable oil obtained in step (1) with the volume of the aqueous phase, adding 0.03 of the volume of the aqueous phase of Span 40 with an HLB of 4.6 as the oil phase, atomizing the oil phase and the aqueous phase in a spray condensation storage device, mixing and liquefying, and obtaining sodium phytate for oil-soluble food;

[0052] The atomization, mixing and liquefaction in the spray condensation storage device include the following processes:

[0053] Step (a) Feeding: The oil phase and the water phase are introduced into the oil inlet pipe and the water inlet pipe respectively, and the temperature of the water phase is 100°C;

[0054] Step (b) ventilation atomization: a high-pressure gas with a pressure of 0.5 MPa is introduced into the oil nozzle and the water nozzle respectively, and the particle size of the atomized droplets is 5 μm;

[0055] Step (c) atomization liquefaction: the atomized liquid droplets are sucked in and mixed by a mist suction pile and then collected in a condensation storage device to obtain sodium phytate for oil-soluble food.

[0056] Embodiment 3: A method for preparing sodium phytate for oil-soluble food, comprising the following steps:

[0057] Step (1): preparing a sodium phytate solution with a concentration of 0.1% to obtain an aqueous phase;

[0058] Step (2): taking 2 times the volume of the vegetable oil obtained in step (1) and adding 0.03 of the volume of the water phase of Span 40, HLB of 4.6, as the oil phase, atomizing the oil phase and the water phase in a spray condensation storage device, mixing and liquefying, and obtaining oil-soluble sodium phytate for food;

[0059] The atomization, mixing and liquefaction in the spray condensation storage device include the following processes:

[0060] Step (a) Feeding: The oil phase and the water phase are introduced into the oil inlet pipe and the water inlet pipe respectively, and the temperature of the water phase is 100°C;

[0061] Step (b) ventilation atomization: a high-pressure gas with a pressure of 1 MPa is introduced into the oil nozzle and the water nozzle respectively, and the particle size of the atomized droplets is 5 μm;

[0062] Step (c) atomization liquefaction: the atomized liquid droplets are sucked in and mixed by a mist suction pile and then collected in a condensation storage device to obtain sodium phytate for oil-soluble food.

[0063] Comparative Example 1: Commercially available oil-soluble sodium phytate.

[0064] Comparative Example 2: A method for preparing sodium phytate for oil-soluble food, comprising the following steps:

[0065] Step (1): preparing a sodium phytate solution with a concentration of 0.2% to obtain an aqueous phase;

[0066] Step (2): Take 3 times the volume of the vegetable oil obtained in step (1) and add 0.03 of the volume of the water phase of Span 40, HLB of 4.6, as the oil phase. After mixing the oil phase and the water phase, disperse them mechanically at 5000 r / min for 30 minutes to obtain sodium phytate for oil-soluble food.

[0067] Comparative Example 3: A method for preparing sodium phytate for oil-soluble food, comprising the following steps:

[0068] Step (1): preparing a sodium phytate solution with a concentration of 0.2% to obtain an aqueous phase;

[0069] Step (2): taking 3 times the volume of the vegetable oil obtained in step (1) with the volume of the aqueous phase, adding 0.03 of the volume of the aqueous phase of Span 40 with an HLB of 4.6 as the oil phase, atomizing the oil phase and the aqueous phase in a spray condensation storage device, mixing and liquefying, and obtaining oil-soluble sodium phytate for food;

[0070] The atomization, mixing and liquefaction in the spray condensation storage device include the following processes:

[0071] Step (a) Feeding: The oil phase and the water phase are introduced into the oil inlet pipe and the water inlet pipe respectively, and the temperature of the water phase is 20°C;

[0072] Step (b) ventilation atomization: a high-pressure gas with a pressure of 0.8 MPa is introduced into the oil nozzle and the water nozzle respectively, and the particle size of the atomized droplets is 13 μm;

[0073] Step (c) atomization liquefaction: the atomized liquid droplets are sucked in and mixed by a mist suction pile and then collected in a condensation storage device to obtain sodium phytate for oil-soluble food.

[0074] Comparative Example 4: A method for preparing sodium phytate for oil-soluble food, comprising the following steps:

[0075] Step (1): preparing a sodium phytate solution with a concentration of 0.2% to obtain an aqueous phase;

[0076] Step (2): taking 3 times the volume of the vegetable oil obtained in step (1) with the volume of the aqueous phase, adding 0.1 volume of Span 40 with an HLB of 4.6 as the oil phase, atomizing the oil phase and the aqueous phase in a spray condensation storage device, mixing and liquefying, and obtaining sodium phytate for oil-soluble food;

[0077] The atomization, mixing and liquefaction in the spray condensation storage device include the following processes:

[0078] Step (a) Feeding: The oil phase and the water phase are introduced into the oil inlet pipe and the water inlet pipe respectively, and the temperature of the water phase is 100°C;

[0079] Step (b) ventilation atomization: a high-pressure gas with a pressure of 0.5 MPa is introduced into the oil nozzle and the water nozzle respectively, and the particle size of the atomized droplets is 15 μm;

[0080] Step (c) atomization liquefaction: the atomized liquid droplets are sucked in and mixed by a mist suction pile and then collected in a condensation storage device to obtain sodium phytate for oil-soluble food.

[0081] Comparative Example 5: A method for preparing sodium phytate for oil-soluble food, comprising the following steps:

[0082] Step (1): preparing a sodium phytate solution with a concentration of 0.2% to obtain an aqueous phase;

[0083] Step (2): taking 3 times the volume of the vegetable oil obtained in step (1) with the volume of the aqueous phase, adding 0.03 of the volume of the aqueous phase of Span 40 with an HLB of 4.6 as the oil phase, atomizing the oil phase and the aqueous phase by ordinary spraying, liquefying, and obtaining oil-soluble sodium phytate for food;

[0084] The atomization, mixing and liquefaction in the spray condensation storage device include the following processes:

[0085] Step (a) Feeding: The oil phase and the water phase are introduced into the oil inlet pipe and the water inlet pipe respectively, and the temperature of the water phase is 80°C;

[0086] Step (b) ventilation atomization: a high-pressure gas with a pressure of 0.8 MPa is introduced into the oil nozzle and the water nozzle respectively, and the particle size of the atomized droplets is 6 μm; Figure 6 As shown, the oil nozzle or the water nozzle is provided with an equal-diameter micro-hole 6-1 structure, and the hole axis passes through the axis of the oil inlet pipe or the water inlet pipe;

[0087] Step (c) liquefaction: The liquid is gathered and liquefied naturally at the bottom of the tower.

[0088] Comparative Example 6: A method for preparing sodium phytate for oil-soluble food, comprising the following steps:

[0089] Step (1): preparing a sodium phytate solution with a concentration of 0.2% to obtain an aqueous phase;

[0090] Step (2): taking 3 times the volume of the vegetable oil obtained in step (1) with the volume of the aqueous phase, adding 0.03 of the volume of the aqueous phase of Span 40 with an HLB of 4.6 as the oil phase, atomizing the oil phase and the aqueous phase in a spray condensation storage device, mixing and liquefying, and obtaining oil-soluble sodium phytate for food;

[0091] The atomization, mixing and liquefaction in the spray condensation storage device include the following processes:

[0092] Step (a) Feeding: The oil phase and the water phase are introduced into the oil inlet pipe and the water inlet pipe respectively, and the temperature of the water phase is 80°C;

[0093] Step (b) ventilation atomization: a high-pressure gas with a pressure of 3 MPa is introduced into the oil nozzle and the water nozzle respectively, and the particle size of the atomized droplets is 14 μm;

[0094] Step (c) atomization liquefaction: the atomized liquid droplets are sucked in and mixed by a mist suction pile and then collected in a condensation storage device to obtain sodium phytate for oil-soluble food.

[0095] Detection method:

[0096] Static light scattering method: Static light scattering method is a commonly used method for measuring the particle size of oil-in-water emulsions. Its principle is to use the scattering and transmission of different relative light in the sample to determine the size of the water phase droplets. The specific operation is to inject the sample to be tested into the sample box, irradiate the sample with a laser beam, detect the scattering and transmission of light, and calculate the particle size distribution of the water phase droplets in the sample based on the scattering angle and light intensity information, and calculate the particle size distribution index (PDI) and the average particle size;

[0097] Centrifugation method: The centrifugation method is to observe the stratification by centrifugation at 500r / min for 3min;

[0098] Oily food preservation test: Fresh beef was soaked in the sodium phytate for oil-soluble food of Examples 1-3 and Comparative Examples 1-5 for 1 min, then transferred to a sterile beaker and refrigerated at 4°C. The semi-micro nitrogen determination method in GB / T 5009.44-2003 was used to determine the volatile basic nitrogen value (TVB-N) of the beef at 0, 2, 4, and 6 days.

[0099] The test results are shown in Table 1.

[0100] Table 1

[0101]

[0102] Comparative Example 1 is a reference example. The results of the oily food preservation test of sodium phytate in Examples 1-3 of this scheme are better than those in Comparative Example 1, indicating that this scheme has a better preservation effect than the commercially available products, and is also more advantageous in dispersibility (distribution of the water phase in Table 1) and stability (stratification in Table 1).

[0103] Comparative Example 2 is compared with Example 1 in that the conventional mechanical force dispersion method is adopted. After mechanical dispersion, the water phase dispersibility of Comparative Example 2 is not good, and the particle size of the water phase droplets is large, which leads to low stability of the oil-soluble sodium oleate obtained in Comparative Example 2 and poor subsequent preservation effect. During mechanical force dispersion, the two phases are repeatedly cut and stirred by mechanical segmentation, Bernoulli principle, etc. to obtain an oil-in-water structure, and a large amount of oil phase and water phase are always in contact, so it is difficult to achieve uniformity and low particle size. In Example 1, a gas phase is introduced into the two phases during the atomization process by a spray method, so that the oil phase is separated from the water phase, and thus better dispersibility can be obtained.

[0104] The difference between Comparative Example 3 and Example 1 is that the water phase temperature is lower. The water phase temperature is heated by the oil inlet pipe during the feeding process. The higher the oil temperature, the better the fluidity and the better the atomization effect under the action of high-pressure gas. However, the lower temperature of Comparative Example 3 leads to a higher viscosity of the vegetable oil, which is not easy to disperse, and then leads to poor dispersibility, large water phase particle size, centrifugal stratification, and ultimately poor preservation effect.

[0105] Comparative Example 4 is compared with Example 1 in that there is an excess of Span 40. Excessive Span 40 will lead to a decrease in the strength of the interface layer, affecting the stability of the system, and at the same time there is a steric hindrance effect, which reduces the stability and ultimately leads to a poor preservation effect.

[0106] The difference between Comparative Example 5 and Example 1 is that the oil spray head and water spray head have different structures and different liquefaction processes. The oil spray head and water spray head structures of Comparative Example 5 make the movement of oil phase droplets and water phase droplets simple "flat throwing", which makes the mixing uniformity of the two phase droplets worse, and finally liquefies naturally at the bottom of the tower body, cools slowly, and makes the stability of the water phase droplets decrease, and finally makes the preservation effect poor. The structural design of Example 1 can effectively overcome this problem.

[0107] The difference between Comparative Example 6 and Example 1 is that the high-pressure gas pressure is different. Too high a gas pressure leads to inefficient spraying. The stable existence of atomization requires certain conditions, including temperature, airflow, droplet state, etc. Too high a gas pressure leads to the destruction of the atomization equilibrium conditions in the tower body, which easily leads to premature liquefaction; at the same time, too high a gas pressure will also lead to excessive gas flow rate at the nozzle, resulting in too low a nozzle temperature, causing liquefaction at the water phase or oil phase nozzle, ultimately leading to poor dispersibility, large water phase particle size, and centrifugal stratification, which ultimately leads to poor preservation effect. It was found through experiments that the high-pressure gas pressure cannot exceed 2MPa, preferably less than 1MPa.

Claims

1. A method for preparing sodium phytate for oil-soluble food, characterized in that: The following steps are involved: Step (1): preparing a sodium phytate solution with a concentration of 0.1-0.5% to obtain an aqueous phase; Step (2): taking 2-5 times the volume of the aqueous phase obtained in step (1), adding 0.01-0.05 times the volume of the aqueous phase of the vegetable oil as the oil phase, atomizing, mixing and liquefying the oil phase and the aqueous phase in a spray condensation storage device to obtain oil-soluble sodium phytate for food; In step (2), the atomization, mixing and liquefaction in the spray condensation storage device include the following processes: Step (a) Feeding: The oil phase and the water phase are respectively introduced into the oil inlet pipe (3-1) and the water inlet pipe (3-2), wherein the temperature of the water phase in the water inlet pipe is 60-100°C; Step (b) ventilation atomization: passing high-pressure gas through the air inlet pipe (2-1) into the oil nozzle (3-3) and the water nozzle (3-4) respectively, forming atomized droplets in the tower body (1), wherein the particle size of the atomized droplets is 5-10 μm, and the pressure of the high-pressure gas is 0.1-2 MPa; Step (c) mist absorption liquefaction: the mist droplets are sucked in and mixed by a mist absorption pile (4-1) and then collected in a condensation storage device (5) to obtain oil-soluble sodium phytate for food, wherein the surface of the mist absorption pile (4-1) is provided with a mist absorption hole (4-1-1), and the center line of the mist absorption hole (4-1-1) does not pass through the axis of the mist absorption pile; The spray condensation storage device comprises a tower body (1) and a condensation storage device (5); a feed port (3) is provided at the upper end of the tower body (1); an oil inlet pipe (3-1) and a water inlet pipe (3-2) are connected to the feed port (3) and enter the tower body; the oil inlet pipe (3-1) and the water inlet pipe (3-2) are coaxial and arranged inside the water inlet pipe (3-2); an oil spray head (3-3) and a water spray head (3-2) are provided at the lower ends of the oil inlet pipe (3-1) and the water inlet pipe (3-2), respectively. -4); the tower body (1) is provided with an air inlet (2), the air inlet (2) is connected to an air inlet pipe (2-1) entering the tower body (1), the air inlet pipe (2-1) is respectively connected to an oil spray head (3-3) and a water spray head (3-4); a discharge port (4) is provided at the bottom of the tower body (1), the discharge port (4) is provided with a mist suction pile (4-1), one end of the mist suction pile (4-1) extends into the tower body (1), and the other end is connected to a condensation storage device (5).

2. A method for preparing sodium phytate for oil-soluble food according to claim 1, characterized in that: In step (2), the HLB value of the emulsifier is 4-8; the emulsifier is one or more of Span 40, Span 60 and Span 80.

3. A method for preparing sodium phytate for oil-soluble food according to claim 1, characterized in that: In step (2), the amount of the emulsifier added is 0.01-0.03 times the volume of the sodium phytate solution.

Citation Information

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