LOW IRON HYDROUS PHOSPHOLIPID AND METHOD FOR SEPARATING LOW-IRON HYDROUS PHOSPHOLIPIDS FROM SOYBEAN OIL SEDIMENTS

Abstract

The invention belongs to the technical field of phospholipid processing, in particular to a low-iron hydrous phospholipid and a method for separating low-iron hydrous phospholipids from soybean oil sediments. The main components of low-iron water-containing phospholipids are phospholipids, oil and water; its water content is 70-80 g/100 g; on a dry basis, the content of acetone-insoluble matter is 92.5-95.5 g/100 g; in terms of acetone-insoluble matter, the iron content is less than or equal to 18 mg/kg. The low-iron water-containing phospholipid of the present invention is prepared from soybean oil by a hydration method, and is used to solve the defects of low acetone-insoluble content of the water-containing phospholipid, inability to remove iron ions and the industry's long-term dependence on the solvent method to prepare the powdered phospholipid; At the same time, the method solves the technical problem that “the preparation of powder phospholipid by hydration method cannot realize industrial production”.

Claims

1. A low-iron water-containing phospholipid, wherein the main components of the low-iron water-containing phospholipid are phospholipids, oil and water, and the water content is 70-80 g/100 g; on a dry basis, the acetone-insoluble content is 92.5-95.5 g/100 g; in terms of acetone insoluble matter, iron content≤18 mg/kg.

2. The low-iron water-containing phospholipid according to claim 1, wherein the sensory index of the low-iron water-containing phospholipid is a brown translucent fluid.

3. A preparation method of the low-iron hydrous phospholipid of claim 1, comprising the following steps: (1) adding soybean oil sediment into water and soaking it to obtain saturated water-absorbing oil sediment; (2) centrifuging and settling saturated water-absorbing oil sediments to obtain fluid; and (3) standing and layering the fluid for stratification to obtain low-iron hydrous phospholipids and oils.

4. A preparation method of the low-iron hydrous phospholipid of claim 2, comprising the following steps: (1) adding soybean oil sediment into water and soaking it to obtain saturated water-absorbing oil sediment; (2) centrifuging and settling saturated water-absorbing oil sediments to obtain fluid; and (3) standing and layering the fluid for stratification to obtain low-iron hydrous phospholipids and oils.

5. The preparation method according to claim 3, wherein the mass ratio of soybean oil sediments and water described in step (1) is 1:1-3.5; the soaking temperature is 60-95° C.; The soaking time is 1-3 h.

6. The preparation method according to claim 3, wherein before soaking, the soybean oil sediments in step (1) are dispersed into granules by stirring in water, and the particle size is less than or equal to 5 mm.

7. The preparation method according to claim 3, wherein in step (2), the centrifugal sedimentation is intermittent centrifugal sedimentation, the temperature is 60-95° C., the rotational speed is 500-2000 rpm, and the time is 5-15 min.

8. The preparation method according to claim 3, wherein in step (3), the temperature of the static layering is 60-95° C.

9. The preparation method according to claim 3, wherein the preparation method of the low-iron water-containing phospholipid further comprises: adding an electrolyte in the soaking process; the mass fraction of the electrolyte in water is 0.01-0.3%, the electrolyte includes at least one of acid, alkali and salt.

10. The preparation method according to claim 4, wherein the mass ratio of soybean oil sediments and water described in step (1) is 1:1-3.5; the soaking temperature is 60-95° C.; The soaking time is 1-3 h.

11. The preparation method according to claim 4, wherein before soaking, the soybean oil sediments in step (1) are dispersed into granules by stirring in water, and the particle size is less than or equal to 5 mm.

12. The preparation method according to claim 4, wherein in step (2), the centrifugal sedimentation is intermittent centrifugal sedimentation, the temperature is 60-95° C., the rotational speed is 500-2000 rpm, and the time is 5-15 min.

13. The low-iron water-containing phospholipid according to claim 4, wherein in step (3), the temperature of the static layering is 60-95° C.

14. The preparation method according to claim 4, wherein the preparation method of the low-iron water-containing phospholipid further comprises: adding an electrolyte in the soaking process; the mass fraction of the electrolyte in water is 0.01-0.3%, the electrolyte includes at least one of acid, alkali and salt.

15. The preparation method according to claim 9, wherein the electrolyte is at least one of the following components: DL-sodium malic acid, L-malic acid, DL-malic acid, glacial acetic acid, citric acid, potassium citrate, sodium citrate, mono-citric acid Sodium, sodium gluconate, lactic acid, potassium lactate, sodium lactate, potassium carbonate, sodium carbonate, potassium bicarbonate, sodium bicarbonate, sodium sulfate, potassium chloride, potassium hydroxide, sodium hydroxide, hydrochloric acid, phosphoric acid, sodium chloride.

16. The preparation method according to claim 14, wherein the electrolyte is at least one of the following components: DL-sodium malic acid, L-malic acid, DL-malic acid, glacial acetic acid, citric acid, potassium citrate, sodium citrate, mono-citric acid Sodium, sodium gluconate, lactic acid, potassium lactate, sodium lactate, potassium carbonate, sodium carbonate, potassium bicarbonate, sodium bicarbonate, sodium sulfate, potassium chloride, potassium hydroxide, sodium hydroxide, hydrochloric acid, phosphoric acid, sodium chloride.

17. A low-iron powder phospholipid, comprising the low-iron hydrous phospholipid according to claim 1.

18. A low-iron powder phospholipid, comprising the low-iron hydrous phospholipid according to claim 2.

19. A low-iron powder phospholipid, comprising the low-iron hydrous phospholipid prepared by the preparation method according to claim 3.

20. A low-iron powder phospholipid, comprising the low-iron hydrous phospholipid prepared by the preparation method according to claim 4.

21. A low-iron powder phospholipid, comprising the low-iron hydrous phospholipid prepared by the preparation method according to claim 5.

22. A low-iron powder phospholipid, comprising the low-iron hydrous phospholipid prepared by the preparation method according to claim 6.

23. A low-iron powder phospholipid, comprising the low-iron hydrous phospholipid prepared by the preparation method according to claim 7.

24. A low-iron powder phospholipid, comprising the low-iron hydrous phospholipid prepared by the preparation method according to claim 8.

25. A low-iron powder phospholipid, comprising the low-iron hydrous phospholipid prepared by the preparation method according to claim 9.

26. A low-iron powder phospholipid, comprising the low-iron hydrous phospholipid prepared by the preparation method according to claim 10.

27. A low-iron powder phospholipid, comprising the low-iron hydrous phospholipid prepared by the preparation method according to claim 11.

28. A low-iron powder phospholipid, comprising the low-iron hydrous phospholipid prepared by the preparation method according to claim 12.

29. A low-iron powder phospholipid, comprising the low-iron hydrous phospholipid prepared by the preparation method according to claim 13.

30. A low-iron powder phospholipid, comprising the low-iron hydrous phospholipid prepared by the preparation method according to claim 14.

31. A low-iron powder phospholipid, comprising the low-iron hydrous phospholipid prepared by the preparation method according to claim 15.

32. A low-iron powder phospholipid, comprising the low-iron hydrous phospholipid prepared by the preparation method according to claim 16.

Description

BRIEF DESCRIPTION OF THE DRAWINGS

[0126] FIG. 1 is a process flow diagram of soybean oil sediment soaking, centrifugal sedimentation and static stratification to obtain low-iron water-containing phospholipids and oils.

[0127] FIG. 2 is the process schematic diagram that soybean oil sediment obtains low-iron water-containing phospholipid and oil through soaking, centrifugal sedimentation and standing and stratification; wherein:

[0128] (a) Schematic diagram of soybean oil sediments in water.

[0129] (b) Schematic diagram of the soaking system with soybean oil sediment particles as the dispersed phase and water as the continuous phase

[0130] (c) Schematic diagram of saturated water absorbing oil sediment;

[0131] (d) Schematic diagram of batch centrifuge shutdown and charging;

[0132] (e) Schematic diagram of batch centrifuge in operation;

[0133] (f) Schematic diagram of batch centrifuge shutdown and unloading;

[0134] (g) A schematic diagram of the fluid being left and stratified in a static stratification tank to obtain low-iron water-containing phospholipids and oils;

[0135] FIG. 3 is the process flow chart for preparing low-iron solid phospholipids from low-iron hydrous phospholipids.

[0136] FIG. 4 is the process schematic diagram of preparing solid phospholipid by concentrating water-containing phospholipid; wherein:

[0137] (1) is continuous phase water; (2) is soybean oil sediments; (3) is dispersed phase soybean oil sediments particles; (4) is saturated water-absorbing oil sediments; (5) is slag, ie, phospholipid metal salts (6) is a fluid, that is a mixture of oil, low-iron hydrous phospholipid and water; (7) is low-iron hydrous phospholipid; (8) is oil; (9) is concentrated hydrous phospholipid; (10) is hydrous phospholipid elastic body; (11) is a low-iron solid phospholipid. A is a soaking tank; B is a batch centrifuge; C is a static layering tank; D is a speed-regulating gear pump; E is a pipeline agitator; F is a continuous dryer.

DESCRIPTION OF THE EMBODIMENTS

[0138] The content of the present invention will be further described below with reference to the accompanying drawings. The experimental methods described in the following examples are conventional methods unless otherwise specified; the reagents and materials can be obtained from commercial sources unless otherwise specified.

[0139] The vacuum is 0.01-0.004 MPa.

[0140] The definition of the dry acetone insoluble yield of low-iron hydrous phospholipids is: dry base acetone insoluble yield of low-iron hydrous phospholipids=dry base acetone insoluble weight of low iron hydrous phospholipids/soybean oil sediment dry base acetone insoluble weight.

[0141] The definition of iron removal rate in low-iron hydrous phospholipids is: iron removal rate of low-iron hydrous phospholipids=(iron weight in soybean oil sediments−iron weight in low-iron hydrous phospholipids)/iron weight in soybean oil sediments.

[0142] The definition of oil extraction rate is: oil extraction rate=dry basis weight of obtained oil/((1-soybean oil sediment dry basis acetone insoluble content)×soybean oil sediment dry basis weight)

Example 1

[0143] A method for separating low-iron water-containing phospholipids and oils and fats from soybean oil sediments, the preparation process of which is shown in FIG. 1 and FIG. 2, comprises the following steps:

[0144] (1) Soaking: Take soybean oil sediment and add it to water, and disperse the oil sediment in the water into granules by stirring to form a soaking system with oil sediment particles as the dispersed phase and water as the continuous phase.

[0145] The soaking temperature is 60° C., and the soaking time is 3 h to obtain saturated water-absorbing oil sediments.

[0146] The obtained saturated water-absorbing oil sediment is prepared when brown low-iron hydrous phospholipid appeared.

[0147] The oil sediment comes from COFCO Donghai Grain and Oil Industry (Zhangjiagang) Co., Ltd., and its material composition is as follows: water content is 38.12 g/100 g, acetone-insoluble content on a dry basis is 61.47 g/100 g, and iron content in terms of acetone-insoluble matter is 50.13 mg/kg; the water is drinking water; the mass ratio of oil sediments to water is 1:1; the particle size of the oil sediments particles is 0.3-3 mm.

[0148] (2) Centrifugal sedimentation: centrifugal sedimentation of saturated water-absorbing oil sediments, the phospholipid metal salt is separated out in the form of slag, and the obtained fluid is obtained. In this process, the rotation speed of centrifugation is 500 rpm, the time is 15 min, and the temperature of centrifugal sedimentation is the same as that of soaking.

[0149] (3) Standing for stratification: the obtained fluid is stratified by standing to obtain low-iron hydrous phospholipid and oil, and the temperature for standing and stratification is the same as the soaking temperature.

[0150] The water content of the obtained low-iron water-containing phospholipid is 78.12 g/100 g, and the content of acetone-insoluble matter on a dry basis is 94.48 g/100 g. The iron content is 5.51 mg/kg in terms of acetone insoluble matter. The sensory indicators are brown translucent fluid, the dry base acetone insoluble yield of low-iron water-containing phospholipids is 96.48%, the iron removal rate is 89.40%, and the oil extraction rate is 75.92%.

Example 2

[0151] A method for separating low-iron water-containing phospholipids and oils and fats from soybean oil sediments, the preparation process of which is shown in FIG. 1 and FIG. 2, comprises the following steps:

[0152] (1) Soaking: Take soybean oil sediment and add it to water, and disperse the oil sediment in the water into granules by stirring to form a soaking system with oil sediment particles as the dispersed phase and water as the continuous phase.

[0153] The soaking temperature is 70° C., and the soaking time is 3 h to obtain saturated water-absorbing oil sediments.

[0154] The obtained saturated water-absorbing oil sediment is marked by the appearance of brown low-iron hydrous phospholipid.

[0155] The oil sediment comes from COFCO Donghai Grain and Oil Industry (Shandong) Co., Ltd., and its material composition is as follows: water content is 38.57 g/100 g, acetone-insoluble content on a dry basis is 63.61 g/100 g, and iron content in terms of acetone-insoluble matter is 63.45 mg/kg; the water is drinking water containing 0.07% sodium chloride. The mass ratio of oil sediments to water is 1:1.5; the particle size of the oil sediments particles is 0.3-3 mm.

[0156] (2) Centrifugal sedimentation: centrifugal sedimentation of saturated water-absorbing oil sediments, the phospholipid metal salt is separated out in the form of slag, and the obtained fluid is obtained. In this process, the rotation speed of centrifugation is 2000 rpm, the time is 5 min, and the temperature of centrifugal sedimentation is the same as that of soaking.

[0157] (3) Standing for stratification: the obtained fluid is stratified by standing to obtain low-iron hydrous phospholipid and oil, and the temperature for standing and stratification is the same as the soaking temperature.

[0158] The water content of the obtained low-iron water-containing phospholipid is 74.32 g/100 g, and the content of acetone-insoluble matter on a dry basis is 93.98 g/100 g. The iron content is 7.62 mg/kg in terms of acetone insoluble matter. The sensory indicators are brown translucent fluid, the dry base acetone insoluble yield of low-iron water-containing phospholipids is 95.59%, the iron removal rate is 88.52%, and the oil extraction rate is 74.68%.

Example 3

[0159] A method for separating low-iron water-containing phospholipids and oils and fats from soybean oil sediments, the preparation process of which is shown in FIG. 1 and FIG. 2, comprises the following steps:

[0160] (1) Soaking: Take soybean oil sediment and add it to water, and disperse the oil sediment in the water into granules by stirring to form a soaking system with oil sediment particles as the dispersed phase and water as the continuous phase.

[0161] The soaking temperature is 80° C., and the soaking time is 2 h to obtain saturated water-absorbing oil sediments.

[0162] The obtained saturated water-absorbing oil sediment is marked by the appearance of brown low-iron hydrous phospholipid.

[0163] The oil sediment comes from COFCO Donghai Grain and Oil Industry (Jiangsu) Co., Ltd., and its material composition is as follows: water content is 39.85 g/100 g, acetone-insoluble content on a dry basis is 62.23 g/100 g, and iron content in terms of acetone-insoluble matter is 75.07 mg/kg; the water is drinking water;

[0164] Lactic acid with a concentration of 80% is added to the water, and the addition amount is 0.05% of the weight of drinking purified water;

[0165] The mass ratio of oil sediments to water is 1:2; the particle size of the oil sediments particles is 0.3-3 mm.

[0166] (2) Centrifugal sedimentation: centrifugal sedimentation of saturated water-absorbing oil sediments, the phospholipid metal salt is separated out in the form of slag, and the obtained fluid is obtained. In this process, the rotation speed of centrifugation is 500 rpm, the time is 15 min, and the temperature of centrifugal sedimentation is the same as that of soaking.

[0167] (3) Standing for stratification: the obtained fluid is stratified by standing to obtain low-iron hydrous phospholipid and oil, and the temperature for standing and stratification is the same as the soaking temperature.

[0168] The water content of the obtained low-iron water-containing phospholipid is 73.88 g/100 g, and the content of acetone-insoluble matter on a dry basis is 93.69 g/100 g. The iron content is 9.78 mg/kg in terms of acetone insoluble matter. The sensory indicators are brown translucent fluid, the dry base acetone insoluble yield of low-iron water-containing phospholipids is 94.48%, the iron removal rate is 87.69%, and the oil extraction rate is 73.89%.

Example 4

[0169] A method for separating low-iron water-containing phospholipids and oils and fats from soybean oil sediments, the preparation process of which is shown in FIG. 1 and FIG. 2, comprises the following steps:

[0170] (1) Soaking: Take soybean oil sediment and add it to water, and disperse the oil sediment in the water into granules by stirring to form a soaking system with oil sediment particles as the dispersed phase and water as the continuous phase.

[0171] The soaking temperature is 90° C., and the soaking time is 2 h to obtain saturated water-absorbing oil sediments.

[0172] The obtained saturated water-absorbing oil sediment is marked by the appearance of brown low-iron hydrous phospholipid.

[0173] The oil sediment comes from COFCO Donghai Grain and Oil Industry (Chaohu) Co., Ltd., and its material composition is as follows: water content is 37.68 g/100 g, acetone-insoluble content on a dry basis is 62.58 g/100 g, and iron content in terms of acetone-insoluble matter is 78.08 mg/kg; the water is drinking water;

[0174] Sodium hydroxide is added to the water, and the addition amount is 0.05% of the weight of drinking purified water;

[0175] The mass ratio of oil sediments to water is 1:2.5; the particle size of the oil sediments particles is 0.3-3 mm.

[0176] (2) Centrifugal sedimentation: centrifugal sedimentation of saturated water-absorbing oil sediments, the phospholipid metal salt is separated out in the form of slag, and the obtained fluid is obtained. In this process, the rotation speed of centrifugation is 2000 rpm, the time is 5 min, and the temperature of centrifugal sedimentation is the same as that of soaking.

[0177] (3) Standing for stratification: the obtained fluid is stratified by standing to obtain low-iron hydrous phospholipid and oil, and the temperature for standing and stratification is the same as the soaking temperature.

[0178] The water content of the obtained low-iron water-containing phospholipid is 78.33 g/100 g and the content of acetone-insoluble matter on a dry basis is 95.41 g/100 g. The iron content is 10.98 mg/kg in terms of acetone insoluble matter. The sensory indicators are brown translucent fluid, the dry base acetone insoluble yield of low-iron water-containing phospholipids is 93.15%, the iron removal rate is 86.90%, and the oil extraction rate is 73.05%.

Example 5

[0179] A method for separating low-iron water-containing phospholipids and oils and fats from soybean oil sediments, the preparation process of which is shown in FIG. 1 and FIG. 2, comprises the following steps:

[0180] (1) Soaking. Take soybean oil sediment and add it to water, and disperse the oil sediment in the water into granules by stirring to form a soaking system with oil sediment particles as the dispersed phase and water as the continuous phase.

[0181] The soaking temperature is 95° C., and the soaking time is 1 h to obtain saturated water-absorbing oil sediments.

[0182] The obtained saturated water-absorbing oil sediment is marked by the appearance of brown low-iron hydrous phospholipid.

[0183] The oil sediment comes from Louis Dreyfus (Bazhou) Feed Protein Co., Ltd., and its material composition is as follows: water content is 37.99 g/100 g, acetone-insoluble content on a dry basis is 63.08 g/100 g, and iron content in terms of acetone-insoluble matter is 96.23 mg/kg; the water is drinking water;

[0184] Citric acid and sodium chloride are added to the water, and the amount of citric acid added is 0.028% of the water, and the amount of salt added is 0.052% of the water;

[0185] The mass ratio of oil sediments to water is 1:3; the particle size of the oil sediments particles is 0.3-3 mm.

[0186] (2) Centrifugal sedimentation: centrifugal sedimentation of saturated water-absorbing oil sediments, the phospholipid metal salt is separated out in the form of slag, and the obtained fluid is obtained. In this process, the rotation speed of centrifugation is 1000 rpm, the time is 10 min, and the temperature of centrifugal sedimentation is the same as that of soaking.

[0187] (3) Standing for stratification: the obtained fluid is stratified by standing to obtain low-iron hydrous phospholipid and oil, and the temperature for standing and stratification is the same as the soaking temperature.

[0188] The water content of the obtained low-iron water-containing phospholipid is 73.02 g/100 g and the content of acetone-insoluble matter on a dry basis is 92.50 g/100 g. The iron content is 13.48 mg/kg in terms of acetone insoluble matter. The sensory indicators are brown translucent fluid, the dry base acetone insoluble yield of low-iron water-containing phospholipids is 92.65%, the iron removal rate is 87.02%, and the oil extraction rate is 70.23%.

Example 6

[0189] A method for separating low-iron water-containing phospholipids and oils and fats from soybean oil sediments, the preparation process of which is shown in FIG. 1 and FIG. 2, comprises the following steps:

[0190] (1) Soaking: Take soybean oil sediment and add it to water, and disperse the oil sediment in the water into granules by stirring to form a soaking system with oil sediment particles as the dispersed phase and water as the continuous phase.

[0191] The soaking temperature is 95° C., and the soaking time is 1 h to obtain saturated water-absorbing oil sediments.

[0192] The obtained saturated water-absorbing oil sediment is marked by the appearance of brown low-iron hydrous phospholipid.

[0193] The oil sediment comes from Qinhuangdao Jinhai Grain and Oil Industry Co., Ltd., and its material composition is as follows: water content is 40.43 g/100 g, acetone-insoluble content on a dry basis is 60.89 g/100 g, and iron content in terms of acetone-insoluble matter is 98.59 mg/kg; the water is drinking water:

[0194] Citric acid is added to the water, and the amount of citric acid added is 0.038% of the water;

[0195] The mass ratio of oil sediments to water is 1:3.5; the particle size of the oil sediments particles is 0.3-3 mm.

[0196] (2) Centrifugal sedimentation: centrifugal sedimentation of saturated water-absorbing oil sediments, the phospholipid metal salt is separated out in the form of slag, and the obtained fluid is obtained. In this process, the rotation speed of centrifugation is 1500 rpm, the time is 5 min, and the temperature of centrifugal sedimentation is the same as that of soaking.

[0197] (3) Standing for stratification: the obtained fluid is stratified by standing to obtain low-iron hydrous phospholipid and oil, and the temperature for standing and stratification is the same as the soaking temperature.

[0198] The water content of the obtained low-iron water-containing phospholipid is 73.38 g/100 g and the content of acetone-insoluble matter on a dry basis is 93.56 g/100 g. The iron content is 13.52 mg/kg in terms of acetone insoluble matter. The sensory indicators are brown translucent fluid, the dry base acetone insoluble yield of low-iron water-containing phospholipids is 92.03%, the iron removal rate is 87.38%, and the oil extraction rate is 70.01%.

Comparative Example 1

[0199] A method for preparing hydrated phospholipids from soybean oil sediments, which is derived from a method for preparing hydrated phospholipids from soybean oil sediments disclosed in patent CN107325125A, comprising the following steps:

[0200] 0.53 times of drinking purified water and 0.03% of sulfuric acid are added to soybean oil sediments, mixed well, and the mixture is heated to 85° C. and kept for 6 hours. Then, centrifuge at 85° C. and 4500 r/min for 5 min to obtain hydrated phospholipids.

[0201] The soybean oil sediment is produced by COFCO Huanghai Cereals and Oils Industry (Shandong) Co., Ltd., and its water content is 38.57 g/100 g, the dry acetone-insoluble content is 63.61 g/100 g, and the iron content in terms of acetone-insoluble matter is 63.45 mg/kg.

[0202] The water content of the obtained hydrated phospholipid is 64.19 g/100 g, the content of acetone-insoluble matter on a dry basis is 90.12 g/100 g, the iron content is 63.45 mg/kg in terms of acetone-insoluble matter, and the sensory index is a brown translucent fluid.

[0203] The main difference between the present invention and the hydrated phospholipid prepared in Comparative Example 1 includes the following aspects:

[0204] The main difference between the hydrated phospholipid prepared by the present invention and the hydrated phospholipid prepared by Comparative Example 1 includes the following aspects:

[0205] First, the hydration method and the water content of the phospholipids are different. Hydrated phospholipids are prepared by a homogeneous hydration method, in which soybean oil sediments and water need to be mixed evenly, and the amount of water added in the hydration operation is 0.25-0.74 times the weight of the oil sediments. Too much water will cause emulsification. Therefore, the water absorption of hydrated phospholipids is far from saturated, and the water content of phospholipids is only 64.19 g/100 g.

[0206] The low-iron water-containing phospholipid prepared by the present invention is prepared by soaking and hydration method. In the method, soybean oil sediments are in a granular state as a dispersed phase and water is a continuous phase to form a soaking system. In this process, the amount of water added is 1.0-3.5 times the weight of the oil sediment. The phospholipids are saturated with excess free water in the surrounding, with a phospholipid saturation value of 70-80 g/100 g.

[0207] Only when the water content of phospholipids reaches saturation, the acetone-insoluble content of phospholipids can reach the maximum value of 92.5-95.5 g/100 g.

[0208] The water absorption of phospholipids to achieve saturation has the following effects, one is that the acetone-insoluble content of the phospholipids is the highest; the other is that the metal salts of the phospholipids are separated; The third is to facilitate the separation of phospholipids, phospholipid metal salts and oils in oil sediments.

[0209] Second, the phospholipid purity is different. The acetone-insoluble content of the hydrated phospholipids is 90-92 g/100 g on a dry basis, and the phospholipid metal salts cannot be removed.

[0210] In the patent for hydrated phospholipids, by bleaching and decolorizing with hydrogen peroxide, the natural nature of phospholipids is destroyed, and the shelf life and food safety cannot be guaranteed.

[0211] The dry acetone-insoluble content of the low-iron water-containing phospholipid of the invention is 92.5-95.5 g/100 g, the low-iron water-containing phospholipid can remove the phospholipid metal salt which is a dark red substance, and the removal of the phospholipid metal salt is conducive to the preparation of yellow powdered phospholipids.

[0212] The powder phospholipid prepared by the low-iron water-containing phospholipid of the present invention is naturally yellow, and does not need chemical bleaching.

Comparative Example 2

[0213] A method for preparing liquid crystal phospholipid from soybean oil sediment, which is derived from the document “Separation and Purification of Soybean Phosphatides in Liquid Crystal Phase”, comprising the following steps:

[0214] 0.67 times of purified drinking water and soybean oil are mixed evenly, the mixture is heated to 70° C., kept for 4 hours, and then centrifuged at 70° C. and 4500 r/min for 5 minutes to obtain liquid crystal phospholipids.

[0215] The soybean oil sediment is produced by Qinhuangdao Jinhai Grain and Oil Industry Co., Ltd., and its water content is 40.43 g/100 g, the dry acetone-insoluble content is 60.89 g/100 g, and the iron content in terms of acetone-insoluble matter is 98.59 mg/kg.

[0216] The water content of the obtained hydrated phospholipid is 64.08 g/100 g, the content of acetone-insoluble matter on a dry basis is 86.06 g/100 g, the iron content is 98.59 mg/kg in terms of acetone-insoluble matter, and the sensory index is a brown translucent fluid.

[0217] The liquid crystalline phospholipid is passed through a circular feed port with a pore diameter of 2 mm, and is placed on a drying tray according to the same strip shape and density as in Example 1, and dried in an intermittent vacuum drying oven at 65° C. for 240 min to obtain a brown block solid phospholipid. The water content of solid phospholipid is 6.79 g/100 g, and the content of acetone-insoluble matter on a dry basis is 86.06 g/100 g. The brown solid phospholipid is pulverized, passed through an 18-mesh sieve, and dried in a vacuum drying oven at 60° C. for 30 min to obtain powdered phospholipid. The water content of powder phospholipids is 1.38 g/100 g, the content of acetone-insoluble matter on a dry basis is 86.06%, and the iron content in terms of acetone-insoluble matter is 98.59 mg/kg, and the sensory index is brown powder.

[0218] Comparing the product of the present invention and the liquid crystal phospholipid of Comparative Example 2, it is found that the differences mainly include the following aspects:

[0219] First, Liquid crystal phospholipids are prepared by homogeneous hydration method. Soybean oil sediments and water need to be mixed evenly, and the amount of water added is 0.67 times the weight of the oil sediments. Therefore, the water absorption of liquid crystal phospholipids is far from saturated, and the water content is only 64.08 g/100 g. The defects are exactly the same as the patented hydrated phospholipids.

[0220] The low-iron water-containing phospholipid prepared by the present invention is prepared by soaking and hydration method. In the method, soybean oil sediments are in a granular state as a dispersed phase and water is a continuous phase to form a soaking system. In this process, the amount of water added is 1.0-3.5 times the weight of the oil sediment. The phospholipids are saturated with excess free water in the surrounding, with a phospholipid saturation value of 70-80 g/100 g.

[0221] Second, the phospholipid purity is different. The dry acetone-insoluble content of the liquid crystal phospholipids is 86.06 g/100 g, and the phospholipid metal salts could not be removed. The solid phospholipids prepared by drying are light brown, and the powder phospholipids are dark brown.

[0222] The acetone-insoluble content on a dry basis of the low-iron water-containing phospholipid of the present invention is 92.5-95.5 g/100 g, and the phospholipid metal salt can be removed, and the content of the acetone-insoluble matter on a dry basis is quite different. Both the solid phospholipid and the powder phospholipid prepared from the low-iron water-containing phospholipid of the present invention are yellow.

Comparative Example 3

[0223] A preparation method of powdered soybean lecithin, which is derived from patent CN103665029A preparation method of powdered soybean lecithin, comprising the following steps:

[0224] (1) Soybean oil sediments and anhydrous acetone are mixed at a weight ratio of 1:10, stirred and extracted under normal pressure and room temperature for 20 minutes, then centrifuged 1 minute with 4000 rpm centrifugal speed for solid-liquid separation, and the solid part is collected.

[0225] The soybean oil sediment comes from Qinhuangdao Jinhai Grain and Oil Industry Co., Ltd., and its material composition is as follows: water content is 40.43 g/100 g, acetone-insoluble content on a dry basis is 60.89 g/100 g, and iron content in terms of acetone-insoluble matter is 98.59 mg/kg.

[0226] (2) The solid part obtained in step (1) is mixed with anhydrous acetone at a weight ratio of 1:10, stirred and extracted under normal pressure and room temperature for 20 min, and then centrifuged 1 minute with 5000 rpm centrifugal speed for solid-liquid separation.

[0227] The solid part is crushed and dried under vacuum at 60° C. for 5 hours to obtain soybean powder phospholipid.

[0228] The dry acetone-insoluble content of the powdered phospholipid is 95.58 g/100 g, the iron content is 98.59 mg/kg in terms of acetone-insoluble matter, the drying reduction is 0.54 g/100 g, and the color is brown.

[0229] Comparing the product of the present invention and the powder phospholipid of Comparative Example 3, it is found that the differences mainly include the following aspects:

[0230] First, the difference between environmental protection and food safety:

[0231] In Comparative Example 3, a method for preparing powdered phospholipid by a solvent method is provided, in which solvent volatilization will cause pollution to the environment. At the same time, the residual solvent has a potential food safety hazard.

[0232] The method for preparing the powdered phospholipid by the product of the present invention belongs to the hydration method, and there is no environmental pollution. The drying reduction of the product is less than or equal to 2 g/100 g, and the drying reduction component is water, and there is no food safety hazard.

[0233] Second, the color is different. The powdered phospholipids prepared in Comparative Example 3 could not be freed from phospholipid metal salts. In order to reduce the residual amount of solvent, the drying time of powdered phospholipids during the preparation process is longer, and the color of the product is darker.

[0234] However, when the powder phospholipid is prepared by using the low-iron hydrous phospholipid of the present invention, the drying time is short, the metal salt of the phospholipid can be removed, and the color of the phospholipid is natural yellow.

Application 1

[0235] The low-iron hydrous phospholipids prepared in Example 4 are used in the preparation of solid phospholipids and powdered phospholipids.

[0236] The preparation process for preparing solid phospholipids and low-iron powder phospholipids with low-iron hydrous phospholipids is shown in FIG. 3 and FIG. 4, including the following steps:

[0237] (1) Concentrating the low-iron hydrous phospholipid prepared in Example 2 to obtain a concentrated hydrous phospholipid;

[0238] (2) Stirring the concentrated hydrous phospholipid to obtain a hydrous phospholipid elastomer;

[0239] (3) Drying the water-containing phospholipid elastomer to obtain a bar-shaped solid phospholipid;

[0240] (4) Pulverizing, sieving and drying the strip-shaped solid phospholipids to obtain powdered phospholipids.

[0241] In step (1), the low-iron water-containing phospholipid of Example 2 is concentrated to 55 g/100 g in a vacuum thin-film evaporator at 95° C. to obtain a concentrated water-containing phospholipid with a dry-base acetone-insoluble content of 93.98 g/100 g, 7.62 mg/kg iron content in terms of acetone insoluble matter, and brown translucent fluid.

[0242] In step (2), the concentrated hydrous phospholipid of step (1) is pushed into the mixer at a speed of 80 cm/min, the stirring revolution is 900 rpm, and the stirring time is 10 s to obtain a continuous output hydrous phospholipid elastomer.

[0243] The water content and acetone insoluble content of the water-containing phospholipid elastomer are the same as those of the concentrated water-containing phospholipid, but the sensory indicators changed to yellow opaque semi-solid.

[0244] In step (3), the water-containing phospholipid elastomer continuously output in step (2) is fed into a continuous atmospheric pressure dryer through a set of feed ports with a pore diameter of 3 mm, and dried at 150° C. for 8 minutes to obtain continuous output strip solids phospholipids. The water content of the strip-shaped solid phospholipid is 7.33 g/100 g, the content of acetone-insoluble matter on a dry basis is 93.98 g/100 g, and the sensory index is a yellow strip-shaped solid.

[0245] In step (4), the solid phospholipids in strips of step (3) are pulverized, passed through an 18-mesh sieve, and dried in a double-cone cyclotron vacuum dryer at 60° C. for 40 min to obtain low-iron powder phospholipids.

[0246] The low-iron powder phospholipid has a water content of 1.38 g/100 g, a dry acetone-insoluble content of 93.98 g/100 g, and an iron content of 7.62 mg/kg in terms of acetone-insoluble matter. The sensory index is a yellow powder.

[0247] The product implements the national standard “GB28401 Food Additive Phospholipids”.

Application 2

[0248] The low-iron hydrous phospholipids prepared in Example 4 are used in the preparation of solid phospholipids and powdered phospholipids.

[0249] The preparation process for preparing solid phospholipids and low-iron powder phospholipids with low-iron hydrous phospholipids is shown in FIG. 3 and FIG. 4, including the following steps:

[0250] (1) Concentrating the low-iron hydrous phospholipid prepared in Example 4 to obtain a concentrated hydrous phospholipid;

[0251] (2) Stirring the concentrated hydrous phospholipid to obtain a hydrous phospholipid elastomer;

[0252] (3) Drying the water-containing phospholipid elastomer to obtain a bar-shaped solid phospholipid;

[0253] (4) Pulverizing, sieving and drying the strip-shaped solid phospholipids to obtain powdered phospholipids.

[0254] In step (1), the low-iron water-containing phospholipid of Example 4 is concentrated to 45 g/100 g in a vacuum thin-film evaporator at 105° C. to obtain a concentrated water-containing phospholipid with a dry-base acetone-insoluble content of 95.41 g/100 g, 10.98 mg/kg iron content in terms of acetone insoluble matter, and brown translucent fluid.

[0255] In step (2), the concentrated hydrous phospholipid of step (1) is pushed into the mixer at a speed of 40 cm/min, the stirring revolution is 1100 rpm, and the stirring time is 20 s to obtain a continuous output hydrous phospholipid elastomer.

[0256] The water content and acetone insoluble content of the water-containing phospholipid elastomer are the same as those of the concentrated water-containing phospholipid, but the sensory indicators changed to yellow opaque semi-solid.

[0257] In step (3), the water-containing phospholipid elastomer continuously output in step (2) is fed into a continuous atmospheric pressure dryer through a set of feed ports with a pore diameter of 4 mm, and dried at 130° C. for 15 minutes to obtain continuous output strip solids phospholipids. The water content of the strip-shaped solid phospholipid is 5.47 g/100 g, the content of acetone-insoluble matter on a dry basis is 95.41 g/100 g, and the sensory index is a yellow strip-shaped solid.

[0258] In step (4), the solid phospholipids in strips of step (3) are pulverized, passed through an 18-mesh sieve, and dried in a double-cone cyclotron vacuum dryer at 60° C. for 30 min to obtain low-iron powder phospholipids.

[0259] The low-iron powder phospholipid has a water content of 1.23 g/100 g, a dry acetone-insoluble content of 95.41 g/100 g, and an iron content of 10.98 mg/kg in terms of acetone-insoluble matter. The sensory index is a yellow powder.

[0260] The product implements the national standard “GB28401 Food Additive Phospholipids”.

[0261] The above detailed description is a specific description of one of the feasible embodiments of the present invention, which is not intended to limit the scope of the present invention. Any equivalent implementation or modification that does not depart from the present invention shall be included in the present invention.