WO2021238162A1 - 一种自聚集含水磷脂及其制备方法 - Google Patents

一种自聚集含水磷脂及其制备方法 Download PDF

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WO2021238162A1
WO2021238162A1 PCT/CN2020/135902 CN2020135902W WO2021238162A1 WO 2021238162 A1 WO2021238162 A1 WO 2021238162A1 CN 2020135902 W CN2020135902 W CN 2020135902W WO 2021238162 A1 WO2021238162 A1 WO 2021238162A1
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water
phospholipids
phospholipid
self
aggregating
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PCT/CN2020/135902
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English (en)
French (fr)
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徐子谦
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内蒙古铂贝曼科技有限公司
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Priority claimed from CN202010460588.4A external-priority patent/CN111548365B/zh
Priority claimed from CN202010455248.2A external-priority patent/CN111548862B/zh
Application filed by 内蒙古铂贝曼科技有限公司 filed Critical 内蒙古铂贝曼科技有限公司
Publication of WO2021238162A1 publication Critical patent/WO2021238162A1/zh
Priority to US17/830,423 priority Critical patent/US20220298184A1/en

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    • C—CHEMISTRY; METALLURGY
    • C07—ORGANIC CHEMISTRY
    • C07F—ACYCLIC, CARBOCYCLIC OR HETEROCYCLIC COMPOUNDS CONTAINING ELEMENTS OTHER THAN CARBON, HYDROGEN, HALOGEN, OXYGEN, NITROGEN, SULFUR, SELENIUM OR TELLURIUM
    • C07F9/00—Compounds containing elements of Groups 5 or 15 of the Periodic System
    • C07F9/02—Phosphorus compounds
    • C07F9/06—Phosphorus compounds without P—C bonds
    • C07F9/08—Esters of oxyacids of phosphorus
    • C07F9/09—Esters of phosphoric acids
    • C07F9/10—Phosphatides, e.g. lecithin
    • C07F9/103—Extraction or purification by physical or chemical treatment of natural phosphatides; Preparation of compositions containing phosphatides of unknown structure
    • A—HUMAN NECESSITIES
    • A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
    • A23D—EDIBLE OILS OR FATS, e.g. MARGARINES, SHORTENINGS, COOKING OILS
    • A23D7/00—Edible oil or fat compositions containing an aqueous phase, e.g. margarines
    • A23D7/005—Edible oil or fat compositions containing an aqueous phase, e.g. margarines characterised by ingredients other than fatty acid triglycerides
    • A23D7/0053—Compositions other than spreads
    • A—HUMAN NECESSITIES
    • A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
    • A23D—EDIBLE OILS OR FATS, e.g. MARGARINES, SHORTENINGS, COOKING OILS
    • A23D7/00—Edible oil or fat compositions containing an aqueous phase, e.g. margarines
    • A23D7/01—Other fatty acid esters, e.g. phosphatides
    • A23D7/011—Compositions other than spreads
    • A—HUMAN NECESSITIES
    • A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
    • A23D—EDIBLE OILS OR FATS, e.g. MARGARINES, SHORTENINGS, COOKING OILS
    • A23D7/00—Edible oil or fat compositions containing an aqueous phase, e.g. margarines
    • A23D7/02—Edible oil or fat compositions containing an aqueous phase, e.g. margarines characterised by the production or working-up
    • A23D7/04—Working-up
    • A—HUMAN NECESSITIES
    • A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
    • A23D—EDIBLE OILS OR FATS, e.g. MARGARINES, SHORTENINGS, COOKING OILS
    • A23D9/00—Other edible oils or fats, e.g. shortenings, cooking oils
    • A23D9/007—Other edible oils or fats, e.g. shortenings, cooking oils characterised by ingredients other than fatty acid triglycerides
    • A23D9/013—Other fatty acid esters, e.g. phosphatides
    • A—HUMAN NECESSITIES
    • A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
    • A23D—EDIBLE OILS OR FATS, e.g. MARGARINES, SHORTENINGS, COOKING OILS
    • A23D9/00—Other edible oils or fats, e.g. shortenings, cooking oils
    • A23D9/02—Other edible oils or fats, e.g. shortenings, cooking oils characterised by the production or working-up
    • A23D9/04—Working-up
    • A23D9/05—Forming free-flowing pieces
    • A—HUMAN NECESSITIES
    • A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
    • A23L—FOODS, FOODSTUFFS, OR NON-ALCOHOLIC BEVERAGES, NOT COVERED BY SUBCLASSES A21D OR A23B-A23J; THEIR PREPARATION OR TREATMENT, e.g. COOKING, MODIFICATION OF NUTRITIVE QUALITIES, PHYSICAL TREATMENT; PRESERVATION OF FOODS OR FOODSTUFFS, IN GENERAL
    • A23L29/00—Foods or foodstuffs containing additives; Preparation or treatment thereof
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D11/00—Solvent extraction
    • B01D11/02—Solvent extraction of solids
    • C—CHEMISTRY; METALLURGY
    • C07—ORGANIC CHEMISTRY
    • C07F—ACYCLIC, CARBOCYCLIC OR HETEROCYCLIC COMPOUNDS CONTAINING ELEMENTS OTHER THAN CARBON, HYDROGEN, HALOGEN, OXYGEN, NITROGEN, SULFUR, SELENIUM OR TELLURIUM
    • C07F9/00—Compounds containing elements of Groups 5 or 15 of the Periodic System
    • C07F9/02—Phosphorus compounds
    • C07F9/06—Phosphorus compounds without P—C bonds
    • C07F9/08—Esters of oxyacids of phosphorus
    • C07F9/09—Esters of phosphoric acids
    • C07F9/10—Phosphatides, e.g. lecithin
    • C07F9/106—Adducts, complexes, salts of phosphatides
    • C—CHEMISTRY; METALLURGY
    • C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
    • C11B—PRODUCING, e.g. BY PRESSING RAW MATERIALS OR BY EXTRACTION FROM WASTE MATERIALS, REFINING OR PRESERVING FATS, FATTY SUBSTANCES, e.g. LANOLIN, FATTY OILS OR WAXES; ESSENTIAL OILS; PERFUMES
    • C11B13/00—Recovery of fats, fatty oils or fatty acids from waste materials

Definitions

  • the invention belongs to the technical field of phospholipid processing, and specifically relates to a self-aggregating water-containing phospholipid and a preparation method thereof.
  • the raw material for phospholipid processing is soybean oil feet, abbreviated as oil feet, which is a by-product of the hydration and degumming process in the soybean oil refining process in the field of oil processing. It is also called hydration oil feet.
  • Its main component is phospholipids 30-45g/100g, Soybean oil 20-30g/100g and moisture 30-50g/100g.
  • the trace components are metal ions, such as calcium, magnesium and iron, which exist in the form of phospholipid metal salts.
  • the iron ion content is usually 50 based on acetone insoluble matter. -100mg/kg, up to 150mg/kg or more in individual cases.
  • the dry-based acetone insoluble content is 60-65g/100g; the second is the solvent method to prepare powdered phospholipids, that is, using soybean oil feet or concentrated phospholipids as raw materials, extracting and removing oil with acetone to obtain powdered phospholipids, and their dry-based acetone insolubles
  • the content is 95-98g/100g.
  • the mainstream product on the market is concentrated phospholipids, and powdered phospholipids account for less than 5% of the market.
  • the disadvantage of this process is that the acetone insoluble content of concentrated phospholipids is too low (60-65g/100g) and chemical bleaching is required.
  • the market price is only 40,000 yuan/ton, which is higher than the price of 40,000 yuan/ton for powdered phospholipids. gap.
  • Chinese patent CN103665029A discloses a method for preparing soybean powdered phospholipids.
  • the method uses acetone as a solvent to extract hydrated oil feet, separates the acetone insolubles, and then vacuum-drys the acetone insolubles to remove the solvent to obtain powdered phospholipids.
  • the disadvantages of this method are the use of acetone solvent, high production cost, and there are potential food safety hazards such as environmental pollution and solvent residues, and it is difficult to popularize. Therefore, it cannot promote the upgrading of the product structure of the oil processing field from concentrated phospholipids to powder phospholipids, nor can it be improved. The current situation of high oil refining loss.
  • Chinese Patent CN107325125A discloses a method for preparing hydrated phospholipids from soybean oil feet and the prepared hydrated phospholipids (hereinafter referred to as hydrated phospholipids).
  • the method includes the following steps: Soybean oil feet are added to demineralized water and mixed uniformly, then stand still for chromatography; after chromatography, the temperature is controlled at 85-95°C, and centrifugal separation is performed to obtain hydrated phospholipids, whose acetone insoluble matter can reach 90-92%.
  • the patent has the following defects:
  • the dry-based acetone insoluble content of the hydrated phospholipid is low: this patent is a homogeneous hydration method, that is, the oil feet and water must be mixed uniformly, and emulsification will inevitably occur when the mixing is uniform. If the emulsification is serious, the phospholipid and oil will be very It's hard to separate again. In order to avoid serious emulsification, the patent adopts two measures. First, strictly control the amount of water added, which is 0.25-0.74 times the weight of the oil feet; second, add sodium hydroxide or sulfuric acid as a demulsifier. The problem caused by the above measures is that the main components of soybean oil feet, phospholipids, oils, and phospholipid metal salts have not been effectively separated. The dry-based acetone insoluble content of hydrated phospholipids is only up to 92%, which is 95-98 compared with solvent-method acetone insolubles. Compared with %, there is still a certain gap;
  • the hydrated phospholipid has not been completely dried and lacks industrial use: the hydrated phospholipid has been concentrated and dehydrated, added with preservatives, pasteurized and packaged to obtain a water-containing phospholipid product with a water content of 22.5-41.2%, but this water-containing Phospholipid products do not meet the national standard "GB28401 Food Additive Phospholipids", which stipulates that the moisture content must not exceed 2%, and cannot be sold; if drying is carried out according to the existing method of preparing powdered phospholipids, the time is too long, the production capacity is too low, and there is no industrial production. Feasibility, neither sale nor further processing leads to its lack of industrial use.
  • the content is only 86.05%, which is the same as the defect of hydrated phospholipids;
  • Lack of industrial use The drying problem of liquid crystal phospholipids is the same as that of hydrated phospholipids. Although liquid crystal phospholipids are obtained by batch vacuum drying to obtain powdered phospholipids, the drying time is If it is too long, the phospholipid product has a darker color (brown) and cannot be used in industrial production.
  • Chinese patent CN102517148A discloses a two-step decolorization method for phospholipids, which adopts a two-step decolorization method of hydrogen peroxide bleaching and silica gel adsorption.
  • the disadvantages of this method are: It is natural and has food safety risks, which is not in line with the general trend of "green" development; (2) The effect of silica gel adsorption and decolorization is very poor, and the invalid silica gel becomes waste residue, which is not conducive to environmental protection; (3) Bleaching destroys the beneficial effects of phospholipids Antioxidant ingredients reduce the antioxidant and nutritional value of phospholipids and shorten the shelf life of phospholipids.
  • the first object of the present invention is to provide a self-aggregating aqueous phospholipid.
  • the self-aggregating aqueous phospholipid of the present invention has the following advantages: its water content reaches saturation, and its dry basis acetone insoluble content is the highest among all known hydration methods , Its dry-based acetone insoluble content has approached or even reached the level of solvent-based powdered phospholipids.
  • the self-aggregating water-containing phospholipid is an intermediate product necessary for the preparation of hydration powder phospholipids. From the perspective of industry development, hydration powder phospholipids will eventually replace solvent powder phospholipids and become the mainstream product to eliminate environmental pollution caused by organic solvents. , Food safety hazards caused by solvent residues and lower production costs.
  • the invention solves the technical problem that the prior art cannot prepare high-purity water-containing phospholipids and powdered phospholipids from soybean oil feet by a hydration method.
  • the self-aggregating aqueous phospholipids have not been reported in the field of phospholipid processing and related research.
  • the second object of the present invention is to provide a method for separating self-aggregated aqueous phospholipids from soybean oil feet.
  • the invention is used to solve the defects of low acetone insoluble content of the water-containing phospholipids prepared by the prior method and the industry's long-term dependence on the solvent method for preparing powdered phospholipids, and is used to solve the technical problem that the powdered phospholipids cannot be industrialized by the hydration method.
  • the purpose of the self-aggregating water-containing phospholipid prepared by the present invention is to prepare powdered phospholipids by hydration method.
  • the content of acetone insoluble matter is as high as 92.5-95.5g/100g.
  • the color is natural yellow, without bleaching and solvent.
  • the third object of the present invention is to provide the application of the self-aggregating aqueous phospholipid in the preparation of powdered phospholipids.
  • a self-aggregating water-containing phospholipid the main components of the self-aggregating water-containing phospholipid are phospholipids, oil and water, the water content is 70-80g/100g, and the acetone-insoluble content is 92.5-95.5g/100g on a dry basis.
  • the self-aggregating aqueous phospholipid is a brown translucent fluid.
  • the self-aggregating water-containing phospholipids refer to aggregates formed by spontaneous combination and spontaneous aggregation of phospholipids in soybean oil feet and water.
  • the present invention also relates to a preparation method of the self-aggregating water-containing phospholipid, which includes the following steps: soaking soybean oil feet in water to obtain saturated water-absorbing oil feet, which are obtained by natural sedimentation.
  • the mass ratio of the soybean oil feet to water is 1:1 to 3.5.
  • the soybean oily feet cannot be effectively soaked in the water, which affects the combination of phospholipids and water.
  • the water is more than 3.5 times the mass of the oil feet, although it is beneficial to the soaking of the soybean oil feet, it increases the cost of water, energy consumption and the volume of the equipment.
  • the soaking temperature is 60-95°C.
  • the soaking temperature is preferably 60-95°C.
  • the temperature is above 60°C, it belongs to the sterilization temperature, which can prevent the oil feet from deteriorating during soaking, and when the temperature is less than 95°C, it can prevent the water from boiling.
  • the soaking time is 1-3h.
  • the soaking time refers to the time required to obtain saturated water-absorbing oil feet.
  • the soaking time starts from the soaking of the soybean oil feet in granular form in water until brown self-aggregating water-containing phospholipids begin to appear in the soybean oil feet. Soybean oil feet during soaking are yellow, and the self-aggregating water-containing phospholipids appearing are brown, so it can be visually judged whether the soaking has reached the end time.
  • the soaking is static soaking.
  • the soybean oil feet are dispersed in water in a stirring manner to become granular.
  • the particle size of the soybean oil feet particles is ⁇ 5mm.
  • the particle size of the soybean oil feet particles is 0.3-3 mm.
  • soybean oil feet The smaller the particle size of the soybean oil feet, the larger the contact area between the oil feet and water, which is more conducive to improving the mass transfer and heat transfer efficiency of the phospholipids and water in the soybean oil feet.
  • the particle size of soybean oil feet is too small, and there is a risk that the soybean oil feet and water will be uniformly mixed and homogenized, which destroys the soaking system.
  • the preparation method further includes adding an electrolyte to the soaking system.
  • the mass fraction of the electrolyte in the water is 0.01-0.3%.
  • a proper amount of electrolyte is conducive to the combination of phospholipids and water in soybean oil feet. Too much electrolyte will inhibit the combination of phospholipids and water. Too little or no electrolytes will increase the water content of self-aggregated hydrated phospholipids, resulting in energy waste during dehydration. .
  • the electrolyte includes at least one of acid, alkali and salt.
  • the electrolyte is DL-sodium malate, L-malic acid, DL-malic acid, glacial acetic acid, citric acid, potassium citrate, sodium citrate, monosodium citrate, sodium gluconate, lactic acid, lactic acid At least one of potassium, sodium lactate, potassium carbonate, sodium carbonate, potassium bicarbonate, sodium bicarbonate, sodium sulfate, potassium chloride, potassium hydroxide, sodium hydroxide, hydrochloric acid, phosphoric acid, and sodium chloride.
  • the natural settlement time is 3-8h.
  • the present invention also relates to the application of the self-aggregating water-containing phospholipids or the self-aggregating water-containing phospholipids prepared by the preparation method in the preparation of powdered phospholipids.
  • using the self-aggregating aqueous phospholipids to prepare powdered phospholipids includes the following steps:
  • the water-containing phospholipid elastomer means that the water-containing phospholipid is an elastomer in the category of colloidal chemistry, and its rheological properties are that the storage modulus G′ is 5-10 times larger than the loss modulus G′′, showing stronger The solid characteristic (elasticity) of the liquid, while the liquid characteristic (viscosity) becomes weaker, it belongs to the elastomer.
  • the continuously output water-containing phospholipid elastomer is fed into a continuous pressure or vacuum dryer through a feed port with a pore size of 2-6 mm, and dried at 120-160°C for 6-20 minutes to obtain
  • the continuous output strip solid phospholipid has a water content of 3-10g/100g, a dry basis acetone insoluble content of 92.5-95.5g/100g, and a sensory index of a yellow strip-like solid.
  • the water content of the powdered phospholipids in step (4) is equivalent to the drying loss described in the national standard "GB28401 Food Additive Phospholipids".
  • the vacuum is 0.01-0.004 MPa.
  • the water content of the self-aggregating water-containing phospholipids of the present invention has reached 70-80g/100g, and the water absorption of the phospholipids has reached saturation: when the water absorption of the phospholipids is saturated, the lipophilicity of the phospholipids is reduced to a minimum, that is, the oil content of the self-aggregating water-containing phospholipids is the smallest , And the purity of phospholipids is the highest, and its dry-based acetone insoluble content reaches 92.5-95.5g/100g.
  • the dry basis acetone insoluble content of the self-aggregating water-containing phospholipid of the present invention is the highest among all current hydration methods: the dry basis acetone insoluble content of the self-aggregating water-containing phospholipid of the present invention is 92.5-95.5g/100g, patent The published hydrated phospholipid is 90-92g/100g, and the liquid crystalline phospholipid reported in the literature is 86.05g/100g.
  • the dry-based acetone insoluble content of the self-aggregating water-containing phospholipid of the present invention is the closest to the solvent method: the dry-based acetone insoluble content of the self-aggregating water-containing phospholipid of the present invention is 92.5-95.5g/100g, which is close to or even reaching the solvent method.
  • the level of powdered phospholipids 95-98g/100g. From the perspective of industry development, the hydration method will eventually replace the solvent method and become the mainstream product to eliminate environmental pollution caused by organic solvents, food safety hazards caused by solvent residues, and reduce production costs.
  • the self-aggregating aqueous phospholipids of the present invention are currently the most suitable The phospholipid product that replaces the solvent method does not contain organic solvents.
  • the self-aggregating water-containing phospholipids and the powdered phospholipids prepared by the present invention have complete technology from soybean oil feet to powdered phospholipids, and have great advantages in terms of quality, shelf life, production cost, environmental protection and food safety, and are suitable for industrialization Production.
  • the present invention optimizes the process parameters such as the amount of water, the particle size of the dispersed phase oil feet of the immersion system, temperature and time, so that the water content of the self-aggregating water-containing phospholipid reaches saturation, and the dry-based acetone insoluble content reaches the level of the hydration method. The highest value.
  • Figure 1 is a process flow diagram of soaking soybean oil feet and naturally sedimenting to obtain self-aggregating water-containing phospholipids.
  • Figure 2 is a schematic diagram of the process of soaking soybean oil feet and naturally settling to obtain self-aggregating water-containing phospholipids. in:
  • (a) is a schematic diagram of soybean oil feet in water
  • (c) is a schematic diagram of the self-aggregating water-containing phospholipid that begins to settle naturally in the saturated water-absorbing oil foot;
  • (d) is a schematic diagram of the self-aggregated water-containing phospholipids and residues of the oily feet obtained by natural sedimentation of saturated water-absorbing oily feet.
  • Figure 3 is a process flow diagram for preparing solid phospholipids from self-aggregating aqueous phospholipids.
  • Figure 4 is a schematic diagram of the process for preparing solid phospholipids by concentrating aqueous phospholipids.
  • Fig. 5 is a rheological characteristic diagram of the storage modulus G'and loss modulus G" of the water-containing phospholipid elastomer prepared by self-aggregating water-containing phospholipids in Application Example 1.
  • Figure 6 is a rheological characteristic diagram of the storage modulus G'and loss modulus G" of the water-containing phospholipid elastomer prepared from the self-aggregating water-containing phospholipid in Application Example 2.
  • (1) is continuous phase water; (2) is soybean oil feet; (3) is dispersed phase soybean oil feet particles; (4) is saturated water-absorbing oil feet; (5) is self-aggregating water-containing phospholipids; (6) It is oily residue; (7) is concentrated aqueous phospholipid; (8) is aqueous phospholipid elastomer; (9) is solid phospholipid.
  • A is a soaking tank; B is a speed-regulating gear pump; C is a pipeline agitator; D is a continuous dryer.
  • the yield of self-aggregated water-containing phospholipids on dry basis acetone insoluble matter the weight of self-aggregated water-containing phospholipids on dry basis acetone insoluble matter/the weight of soybean oil feet dry basis acetone insoluble matter.
  • a self-aggregating water-containing phospholipid refers to Figure 1 and Figure 2 (a)- Figure 2 (d), the preparation method includes the following steps:
  • Soaking Take soybean oil feet into water, stir the oil feet in the water and disperse them into granules, forming a soaking system with soybean oil feet particles as the dispersed phase and water as the continuous phase.
  • the soaking temperature is 60°C.
  • the soaking time is 3h to get saturated water-absorbent feet.
  • the saturated water-absorbing oily foot is marked by the appearance of brown self-aggregating water-containing phospholipids.
  • the soybean oily foot comes from COFCO Jiayue (Tianjin) Co., Ltd., and its material composition: the water content is 41.03g/100g, and the dry-based acetone insoluble content is 61.13g/100g; the water is drinking water; oily feet The mass ratio to water is 1:1; the particle size of the oily feet particles is 0.3-3mm.
  • the water content of the obtained self-aggregating water-containing phospholipids was 77.78g/100g, the dry-based acetone insolubles content was 93.81g/100g, the sensory index was brown translucent fluid, and the self-aggregating water-containing phospholipids had a dry-based acetone-insoluble yield of 75.63. %.
  • a self-aggregating water-containing phospholipid refers to Figure 1 and Figure 2 (a)- Figure 2 (d), the preparation method includes the following steps:
  • Soaking Take the soybean oil feet and add them to the water, and stir the oil feet in the water to disperse them into granules to form a soaking system with soybean oil feet particles as the dispersed phase and water as the continuous phase.
  • the soaking temperature is 70°C.
  • the soaking time is 3h to get saturated water-absorbent feet.
  • the saturated water-absorbing oily foot is marked by the appearance of brown self-aggregating water-containing phospholipids.
  • the oil feet come from COFCO Grain and Oils Industry (Jiujiang) Co., Ltd., and its material composition: the water content is 37.56g/100g, and the dry basis acetone insoluble content is 60.87g/100g; the water is purified drinking water, which is added to the water Table salt and sodium chloride are added in an amount of 0.07% of the weight of purified drinking water; the mass ratio of oil feet to water is 1:1.5; and the particle size of the oil feet particles is 0.3-3 mm.
  • the water content of the obtained self-aggregating water-containing phospholipids was 74.00g/100g, the dry-based acetone insolubles content was 93.75g/100g, the sensory index was brown translucent fluid, and the self-aggregating water-containing phospholipids had a dry-based acetone-insoluble yield of 78.09 %.
  • a self-aggregating aqueous phospholipid referring to Figure 1 and Figure 2(a)- Figure 2(d), the preparation method includes the following steps:
  • Soaking Take soybean oil feet into water, stir the oil feet in the water and disperse them into granules to form a soaking system with soybean oil feet particles as the dispersed phase and water as the continuous phase.
  • the soaking temperature is 80°C.
  • the soaking time is 2h to get saturated water-absorbent feet.
  • the saturated water-absorbing oily foot is marked by the appearance of brown self-aggregating water-containing phospholipids.
  • the oil feet come from COFCO Grain and Oils Industry (Huanggang) Co., Ltd., and its material composition: the water content is 38.42g/100g, and the dry basis acetone insoluble content is 61.02g/100g; the water is purified drinking water, which is added to the water
  • the food additive lactic acid with a concentration of 80% is added in an amount of 0.05% of the weight of purified drinking water; the mass ratio of oil feet to water is 1:2; and the particle size of the oil feet particles is 0.3-3 mm.
  • the water content of the obtained self-aggregating water-containing phospholipid was 73.12g/100g, the dry-based acetone insoluble content was 92.53g/100g, the sensory index was brown translucent fluid, and the dry-based acetone-insoluble yield of self-aggregating water-containing phospholipids was 80.72 %.
  • a self-aggregating aqueous phospholipid referring to Figure 1 and Figure 2(a)- Figure 2(d), the preparation method includes the following steps:
  • the oil feet come from Bangji (Nanjing) Grain and Oil Co., Ltd., and its material composition: the water content is 39.78g/100g, the dry basis acetone insoluble content is 62.05g/100g; the water is purified drinking water, which is added to the water
  • the food additive sodium hydroxide is added in an amount of 0.03% of the weight of purified drinking water; the mass ratio of oil feet to water is 1:2.5; the particle size of the oil feet particles is 0.3-3 mm.
  • the water content of the obtained self-aggregating water-containing phospholipid was 77.56g/100g, the dry-based acetone insoluble content was 95.42g/100g, the sensory index was brown translucent fluid, and the dry-based acetone-insoluble yield of self-aggregating water-containing phospholipids was 82.71 %.
  • a self-aggregating aqueous phospholipid referring to Figure 1 and Figure 2(a)- Figure 2(d), the preparation method includes the following steps:
  • the oil feet are from China National Grain Storage Zhenjiang Grain and Oil Co., Ltd., and its material composition is as follows: the water content is 37.69g/100g, and the dry basis acetone insoluble content is 63.45g/100g; the water is purified drinking water, and the food additive lemon is added to the water. Acid and table salt, sodium chloride, citric acid, the added amount is 0.028% of the weight of purified drinking water, the added amount of salt is 0.052% of the weight of purified drinking water; the mass ratio of oil feet to water is 1:3; the oil feet particles, Its particle size is 0.3-3mm.
  • the water content of the obtained self-aggregating water-containing phospholipid was 72.33g/100g, the dry-based acetone insoluble content was 93.65g/100g, the sensory index was brown translucent fluid, and the dry-based acetone-insoluble yield of self-aggregating water-containing phospholipids was 83.35. %.
  • a self-aggregating aqueous phospholipid referring to Figure 1 and Figure 2(a)- Figure 2(d), the preparation method includes the following steps:
  • the oil feet come from China Textile Grain and Oils (Dongguan) Co., Ltd., and its material composition: the water content is 40.23g/100g, and the dry basis acetone insoluble content is 62.39g/100g; the water is purified drinking water, which is added to the water
  • the food additive citric acid the added amount of citric acid is 0.038% of the weight of purified drinking water
  • the mass ratio of oily feet to water is 1:3.5
  • the particle size of the oily feet particles is 0.3-3mm.
  • the water content of the obtained self-aggregating water-containing phospholipids was 73.01g/100g, the dry-based acetone insolubles content was 94.18g/100g, the sensory index was brown translucent fluid, and the self-aggregating water-containing phospholipids had a dry-based acetone-insoluble yield of 83.98. %.
  • a method for preparing hydrated phospholipids from soybean oil feet which is derived from a method for preparing hydrated phospholipids from soybean oil feet disclosed in patent CN107325125A, and includes the following steps:
  • soybean oil feet Take soybean oil feet, add 0.53 times the weight of soybean oil feet to drinking purified water, add soybean oil feet weight of 0.03% sulfuric acid and mix well, heat the mixture to 85°C, keep it for 6 hours, then keep it at 85°C, 4500r/min Centrifugal separation under conditions for 5 minutes to obtain hydrated phospholipids.
  • the soybean oil feet used are produced by COFCO Grain and Oils Industry (Huanggang) Co., Ltd., with a water content of 38.42g/100g and a dry basis acetone insoluble content of 61.02g/100g.
  • the obtained hydrated phospholipid has a water content of 64.03g/100g, a dry basis acetone insoluble content of 90.01g/100g, and a sensory index of brown translucent fluid.
  • the hydration method and the water content of the phospholipids are different: the hydrated phospholipids are prepared by a homogeneous hydration method. Soybean oil feet and water need to be mixed uniformly. The water added for hydration operations is 0.25-0.74 times the weight of the oil feet. Emulsification occurs when there is more water, so the water absorption of hydrated phospholipids is far from reaching the level of saturation, and the water content of phospholipids is only 64.03g/100g; the self-aggregating phospholipids of the present invention are prepared by immersion hydration method, and soybean oil feet are used as granular form. The dispersed phase, with water as the continuous phase, constitutes the soaking system.
  • the amount of water added for the hydration operation is 1.0-3.5 times the weight of the oil foot to ensure that there is excess free water around the phospholipid, and ensure that the water absorption of the phospholipid reaches the saturation value. It is 70-80g/100g. Only when the water content of the phospholipid reaches saturation can the acetone insoluble content of the phospholipid reach the maximum value, which is 92.5-95.5g/100g.
  • the purity of the phospholipids is different: the dry-based acetone insoluble content of the hydrated phospholipid is 90-92g/100g; the dry-based acetone insoluble content of the self-aggregated water-containing phospholipid of the present invention is 92.5-95.5g/100g, which is the current hydration phospholipid The highest content in the medium is close to or even reaching the level of 95-98g/100g in the solvent method.
  • a method for preparing liquid crystal phospholipids from soybean oil feet is derived from the document "Research on Separation and Purification of Soybean Phospholipids in Liquid Crystal State", and includes the following steps:
  • soybean oil feet Take the soybean oil feet, add 0.67 times the weight of the soybean oil feet to the purified drinking water and mix well, heat the mixture to 70°C and keep it for 4 hours, then centrifuge at 70°C and 4500r/min for 5 minutes to obtain liquid crystal phospholipids .
  • the soybean oil feet used are produced by China Textile Grain & Oils (Dongguan) Co., Ltd., with a water content of 40.23g/100g and a dry basis acetone insoluble content of 62.39g/100g.
  • the obtained liquid crystal phospholipid has a water content of 63.89g/100g, a dry basis acetone insoluble content of 86.23g/100g, and a sensory index of brown translucent fluid.
  • the degree of hydration is different: the water content of the liquid crystal phospholipid is only 63.89g/100g.
  • the liquid crystal phospholipid is prepared by a homogeneous hydration method.
  • the soybean oil feet and water need to be mixed uniformly, and the amount of water needs to be strictly controlled, otherwise Emulsification will occur, and the amount of water added for the hydration operation is 0.67 times the weight of the oil feet, so the water absorption of the liquid crystal phospholipid is far from saturated, and the defect is exactly the same as the patent hydrated phospholipid;
  • the water content of the self-aggregating hydrated phospholipid of the present invention is 70-80g/100g, self-aggregating water-containing phospholipids are prepared by immersion hydration method.
  • Soybean oil feet use granular as the dispersed phase and water as the continuous phase to form the soaking system.
  • the amount of water added for the hydration operation is 1.0 of the weight of the oil feet. -3.5 times to ensure that the phospholipid absorption capacity reaches saturation.
  • the acetone insoluble content of the phospholipid can reach its maximum value only when the water absorption of the phospholipid reaches saturation.
  • the purity of the phospholipids is different: the dry-based acetone insoluble content of the liquid crystal phospholipids is only 86.23g/100g, the solid phospholipids obtained by drying are brown, and the powdered phospholipids are brown; the self-aggregating water-containing phospholipids of the present invention are insoluble in acetone on a dry basis The content of acetone is 92.5-95.5g/100g, and there is a big difference in the content of insoluble matter in acetone on a dry basis between the two.
  • the solid phospholipids and powder phospholipids prepared from the aggregation of water-containing phospholipids of the present invention are both yellow.
  • a method for preparing powdered soybean phospholipids is derived from patent CN103665029A.
  • a method for preparing powdered soybean phospholipids includes the following steps:
  • the soybean oil base comes from Bangji (Nanjing) Grain and Oil Co., Ltd., and its material composition: water content is 39.78g/100g, dry basis acetone insoluble matter content is 62.05g/100g.
  • step (2) For the solid part obtained in step (1), mix the solid part and anhydrous acetone in a weight ratio of 1:10, stir and extract for 20 min under normal pressure and room temperature, and then centrifuge for solid-liquid separation. Centrifugation time is 1 min. The speed is 5000 rpm, and the solid part is collected. The solid part was crushed and dried under vacuum at 60° C. for 5 hours to obtain soybean powder phospholipid.
  • the dry base acetone insoluble content was 95.30 g/100 g, and the drying loss was 0.65 g/100 g, which was a brown powder.
  • Comparative Example 3 is a powdered phospholipid prepared by the solvent method.
  • the solvent method has environmental pollution caused by solvent volatilization.
  • the product loss on drying is 0.65g/100g, and the component of the loss on drying is a solvent.
  • Food safety hazards caused by solvent residues; the powdered phospholipids prepared by the application of the present invention belong to a hydration method and have no environmental pollution.
  • the powdered phospholipid prepared in Comparative Example 3 is brown.
  • the drying time is long and the phospholipid has a darker color; the self-aggregating water-containing phospholipid of the present invention has a short drying time when preparing the powdered phospholipid.
  • the color is natural yellow.
  • the application of preparing solid phospholipids and powder phospholipids from self-aggregating water-containing phospholipids in Example 2, referring to Figures 3 and 4, includes the following steps:
  • Example 2 Take the self-aggregating water-containing phospholipid prepared in Example 2 and concentrate to obtain a concentrated water-containing phospholipid; (2) Stir the concentrated water-containing phospholipid to obtain a water-containing phospholipid elastomer; (3) Dry the water-containing phospholipid elastomer to obtain a bar (4) pulverizing, sieving, and drying the bar-shaped solid phospholipid to obtain a powdered phospholipid.
  • Step (1) Preparation of concentrated water-containing phospholipids: the self-aggregating water-containing phospholipids of Example 2 were concentrated to 55g/100g in a vacuum thin film evaporator at 95°C to obtain concentrated water-containing phospholipids with a dry-based acetone-insoluble content of 93.75 g/100g, the sensory index is brown translucent fluid.
  • Step (2) Preparation of water-containing phospholipid elastomer: Push the concentrated water-containing phospholipid of step (1) into the agitator at a speed of 80 cm/min, the stirring speed is 900 rpm, and the stirring time is 10 s to obtain a continuous output of the water-containing phospholipid elastomer. Its water content and acetone insoluble content are the same as concentrated water-containing phospholipids, but the sensory index changes to yellow opaque semi-solid.
  • Step (3) Preparation of solid phospholipids: Pass the water-containing phospholipid elastomer continuously output in step (2) through a set of feed ports with a pore size of 3 mm, and send it to a continuous pressure dryer, and dry at 150°C for 8 minutes to obtain a continuous output
  • the strip-shaped solid phospholipid has a water content of 7.23g/100g, a dry-based acetone insoluble content of 93.75g/100g, and a sensory index of a yellow strip-shaped solid.
  • Step (4) Preparation of powdered phospholipids: pulverize the solid phospholipids of step (3), pass through an 18-mesh sieve, and dry in a double cone vacuum dryer at 60°C for 40 minutes to obtain powdered phospholipids with a water content of 1.43g/ 100g, the dry-based acetone insoluble content is 93.75g/100g, the sensory index is yellow powder, and the product implements the national standard "GB28401 Food Additive Phospholipid".
  • the application of preparing solid phospholipids and powder phospholipids from self-aggregating water-containing phospholipids in Example 4, referring to Figures 3 and 4, includes the following steps:
  • Example 4 Take the self-aggregating water-containing phospholipid prepared in Example 4 and concentrate to obtain concentrated water-containing phospholipid; (2) Stir the concentrated water-containing phospholipid to obtain a water-containing phospholipid elastomer; (3) Dry the water-containing phospholipid elastomer to obtain a bar (4) pulverizing, sieving, and drying the bar-shaped solid phospholipid to obtain a powdered phospholipid.
  • Step (1) Preparation of concentrated water-containing phospholipids: the self-aggregating water-containing phospholipids of Example 4 were concentrated to 45g/100g in a vacuum thin film evaporator at 105°C to obtain concentrated water-containing phospholipids with a dry-based acetone-insoluble content of 95.42 g/100g, the sensory index is brown translucent fluid.
  • Step (2) Preparation of water-containing phospholipid elastomer: Push the concentrated water-containing phospholipid of step (1) into the agitator at a speed of 40 cm/min.
  • the stirring speed is 1100 rpm and the stirring time is 20 s to obtain a continuous output of the water-containing phospholipid elastomer.
  • Its water content and acetone insoluble content are the same as concentrated water-containing phospholipids, but the sensory index changes to yellow opaque semi-solid.
  • Step (3) Preparation of solid phospholipids:
  • the aqueous phospholipid elastomer continuously output in step (2) is fed into a continuous vacuum dryer through a set of feed ports with a pore size of 4 mm, and dried at 130°C for 15 minutes to obtain continuous output strips.
  • Step (4) Preparation of powdered phospholipids: pulverize the solid phospholipids of step (3), pass through an 18-mesh sieve, and vacuum dry at 60°C for 30 minutes in a double cone vacuum dryer to obtain powdered phospholipids with a water content of 1.18g/ 100g, the dry acetone insoluble content is 95.42g/100g, the sensory index is yellow powder, and the product implements the national standard "GB28401 Food Additive Phospholipid".
  • the rheological characterization of the water-containing phospholipid elastomer prepared in Application Example 1 and Application Example 2 is performed, and the test results are shown in Figure 5 and Figure 6, respectively.
  • the instrument and parameters used in the test are: RS6000 Rotational Rheometer (Haake Company, Germany), the Z41Ti coaxial drum sensor system is used to measure the rotor (the diameter of the drum and the rotor are 43.40mm and 41.42mm respectively), and the sample is being transmitted. The thickness at the center of the sensor system is 3mm.
  • the storage modulus G′ of the water-containing phospholipid elastomer provided by the application example 1 and the application example 2 is more than 5 times larger than the loss modulus G′′ in the measured frequency range, and they are almost It has nothing to do with frequency, indicating that elasticity is far greater than viscosity, showing strong solid characteristics (elasticity), while liquid characteristics (viscosity) become weaker, which is an elastomer.

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Abstract

本发明属于磷脂加工技术领域，具体涉及一种自聚集含水磷脂及其制备方法。所述自聚集含水磷脂，其主要成分是磷脂、油脂和水，含水量为70-80g/100g，以干基计丙酮不溶物含量为92.5-95.5g/100g，感官指标为棕色半透明流体。本发明解决了现有的含水磷脂的丙酮不溶物含量不高、以及行业长期依赖溶剂法制备粉末磷脂的缺陷，还解决了水化法粉末磷脂无法实现工业化生产的技术难题。本发明自聚集含水磷脂的用途是制备水化法粉末磷脂，丙酮不溶物含量高达92.5-95.5g/100g，色泽为自然黄色，不漂白、无溶剂，可以取代溶剂法粉末磷脂，避免溶剂法粉末磷脂带来的环境污染和食品安全隐患，并且水化法粉末磷脂的生产成本远低于溶剂法。

Description

一种自聚集含水磷脂及其制备方法 技术领域
本发明属于磷脂加工技术领域，具体涉及一种自聚集含水磷脂及其制备方法。
背景技术
磷脂加工的原料是大豆油脚，简称油脚，是油脂加工领域的大豆油脂精炼过程中水化脱胶工艺的副产物，也称为水化油脚，其主要成分是磷脂30-45g/100g、大豆油20-30g/100g和水分30-50g/100g，微量成分是金属离子，如钙、镁和铁等，以磷脂金属盐的形式存在，如铁离子含量，以丙酮不溶物计通常为50-100mg/kg，个别情况高达150mg/kg以上。
工业化的磷脂加工方法主要有两种，一是水化法制备浓缩磷脂，即从大豆毛油中水化提取大豆油脚后，直接干燥脱水得到浓缩磷脂，因其具有流动性也称为流体磷脂，其干基丙酮不溶物含量为60-65g/100g；二是溶剂法制备粉末磷脂，即以大豆油脚或者浓缩磷脂为原料，用丙酮萃取除去油脂，得到粉末磷脂，其干基丙酮不溶物含量为95-98g/100g。目前市场上主流产品是浓缩磷脂，粉末磷脂在市场中占比不足5％。
虽然大豆油脚绝大多数被加工成浓缩磷脂，但浓缩磷脂有很大缺陷。例如文献《大豆浓缩磷脂生产工艺》(胡兴中.大豆浓缩磷脂生产工艺[J].中国油脂，2007,32(9):20-21)和《浓缩磷脂制取工艺与实践》(胡庆涛等.浓缩磷脂制取工艺与实践[J].中国油脂，2002,27(1):39-40)介绍了以水化油脚为原料进行脱水、氧化漂白生产浓缩磷脂的方法。该工艺的缺点是浓缩磷脂的丙酮不溶物含量太低(60-65g/100g)、需要化学漂白，市场价格仅为0.4万元/吨，与粉末磷脂4万元/吨的售价有较大差距。
中国专利CN103665029A公开了一种制备大豆粉末磷脂的方法，该方法采用丙酮作为溶剂萃取水化油脚，分离出丙酮不溶物，再低温真空干燥丙酮不溶物脱除溶剂，得到粉末磷脂。该方法的缺点是使用丙酮溶剂，生产成本高，并且存在环境污染和溶剂残留的食品安全隐患，难以普遍推广，因此不能促进油脂加工领域从浓缩磷脂向粉末磷脂转化的产品结构升级，也不能改善油脂精炼损耗高的现状。
目前水化法制备磷脂的研究存在诸多缺陷，比如中国专利CN107325125A 公开了一种大豆油脚制备水合磷脂的方法及其制得的水合磷脂(以下简称水合磷脂)，该方法包括如下操作步骤：取大豆油脚加入软化水混合均匀后，静置进行层析；层析结束后控制温度为85-95℃，进行离心分离得到水合磷脂，其丙酮不溶物能够达到90-92％。该专利存在如下缺陷：
(1)水合磷脂的干基丙酮不溶物含量低：该专利是均质水化方法，即油脚与水要混合均匀，混合均匀时不可避免地发生乳化，如果乳化严重，磷脂与油脂就很难再分离。为了避免严重乳化，该专利采取了两个措施，第一、严格控制加水量，加水量是油脚重量的0.25-0.74倍；第二，加入氢氧化钠或者硫酸，用作破乳剂。上述措施带来的问题是大豆油脚中的主要成分磷脂、油脂和磷脂金属盐没有得到有效分离，水合磷脂的干基丙酮不溶物含量最高仅达到92％，与溶剂法丙酮不溶物95-98％相比，尚有一定的差距；
(2)水合磷脂未能彻底干燥，缺乏工业用途：该水合磷脂通过浓缩脱水、添加防腐剂、巴氏杀菌和包装得到了一种含水量为22.5-41.2％的含水磷脂产品，但是这种含水磷脂产品不符合国家标准《GB28401食品添加剂磷脂》关于水分不得超过2％的规定，不能销售；如果按照现有的制备粉末磷脂的方法进行干燥，则时间太长、产能太低，没有工业化生产的可行性，既不能销售也不能进一步加工导致其缺乏工业用途。
另一种水化法提取磷脂的现有技术，如文献《液晶态分离提纯大豆磷脂的研究》(李子明等.液晶态分离提纯大豆磷脂的研究[J].中国粮油学报，2007,22(1):31-32)，以下简称液晶态磷脂。该文献方法存在以下技术缺陷：(1)液晶态磷脂的干基丙酮不溶物含量较低：采用均质水化方法，加水量是0.67倍油脚，得到的液晶态磷脂的干基丙酮不溶物含量仅为86.05％，这与水合磷脂的缺陷相同；(2)缺乏工业用途：液晶态磷脂的干燥问题与水合磷脂相同，虽然液晶态磷脂用间歇式真空干燥方式得到了粉末磷脂，但是干燥时间太长，磷脂产品的色泽较深(棕色)，无法应用于工业化生产。
中国专利CN102517148A公开了一种磷脂两步脱色方法，采用过氧化氢漂白和硅胶吸附的两步脱色方法，该方法的缺点是：(1)化学漂白脱色，使磷脂产生氧化副产物、破坏磷脂的天然性，同时存在食品安全风险，不符合“绿色”发展的大趋势；(2)硅胶吸附脱色的效果很差，失效的硅胶成为废渣，不利于环保；(3)漂白破坏了磷脂中有益的抗氧化成分，使磷脂的抗氧化性、营养价值降低， 缩短了磷脂的保质期。
在磷脂加工领域，从产品的角度看粉末磷脂替代浓缩磷脂是未来的方向，从方法的角度看水化法替代溶剂法是未来的方向，虽然目前已有一些水化法的研究，但是水化法制备得到的磷脂的纯度仍不够高、色泽改善仍未脱离化学漂白的方法、水化法的脱水效率仍未达到工业化的水平、工艺技术在完整性和连续化方面尚有不足。
因此，开发一种能解决上述技术问题的自聚集含水磷脂及从大豆油脚中分离自聚集含水磷脂的方法是非常必要的。
发明内容
本发明的第一个目的在于提供一种自聚集含水磷脂，本发明自聚集含水磷脂具有以下优势：其含水量达到饱和、其干基丙酮不溶物含量在已知的所有水化法中是最高的、其干基丙酮不溶物含量已经接近甚至达到溶剂法粉末磷脂的水平。所述自聚集含水磷脂是制备水化法粉末磷脂所必需的中间产品，从行业发展的角度看，水化法粉末磷脂最终要替代溶剂法粉末磷脂成为主流产品，以消除有机溶剂造成的环境污染、溶剂残留造成的食品安全隐患和降低生产成本。本发明解决了现有技术不能用水化法从大豆油脚中制备高纯度含水磷脂和粉末磷脂的技术难题。所述自聚集含水磷脂，在磷脂加工领域和相关研究中均未见报道。
本发明的第二个目的在于提供了一种从大豆油脚中分离自聚集含水磷脂的方法。本发明用以解决现有方法制备的含水磷脂的丙酮不溶物含量不高、以及行业长期依赖溶剂法制备粉末磷脂的缺陷，用以解决水化法粉末磷脂无法实现工业化生产的技术难题。本发明制备的自聚集含水磷脂的用途是制备水化法粉末磷脂，丙酮不溶物含量高达92.5-95.5g/100g，色泽为自然黄色，不漂白、无溶剂，可以取代溶剂法粉末磷脂，避免溶剂法粉末磷脂带来的环境污染和食品安全隐患，并且水化法粉末磷脂的生产成本远低于溶剂法。所述从大豆油脚中分离自聚集含水磷脂的方法，在磷脂加工领域和相关研究中均未见报道。
本发明的第三个目的在于提供了所述自聚集含水磷脂在制备粉末磷脂中的应用。
为实现以上目的，本发明提供的技术方案如下：
一种自聚集含水磷脂，所述自聚集含水磷脂的主要成分是磷脂、油脂和水，含水量为70-80g/100g，以干基计丙酮不溶物含量为92.5-95.5g/100g。
优选地，所述自聚集含水磷脂为棕色半透明流体。
所述自聚集含水磷脂是指大豆油脚中的磷脂与水自发结合、自发聚集形成的聚集体。
本发明还涉及上述自聚集含水磷脂的制备方法，包括如下步骤：将大豆油脚在水中浸泡，得到饱和吸水油脚，自然沉降，即得。
所述的浸泡，是指大豆油脚在水中是分散相，而水是连续相，构成了一种浸泡体系。
所述浸泡的结果，是得到饱和吸水油脚。在浸泡结束时，饱和吸水油脚中的磷脂吸水量达到饱和，即磷脂含水量达到70-80g/100g。
优选地，所述大豆油脚与水的质量比为1:1-3.5。
当水少于油脚重量的1.0倍时，大豆油脚无法在水中实现有效浸泡，进而影响磷脂与水的结合。当水多于油脚质量的3.5倍时，虽然有利于大豆油脚的浸泡，但增加了水的成本、能源消耗和增加了设备的体积。
优选地，所述浸泡的温度为60-95℃。
在0℃到100℃的水中，磷脂与水都可以发生结合，温度越高结合的效率越高。因此，提高水温，可以缩短浸泡时间。但是在沸水中，不利于自聚集含水磷脂的稳定，并且水的沸腾蒸发也浪费能源。因此所述浸泡的温度优选为60-95℃。当温度在60℃以上时属于杀菌温度，可以防止浸泡期间油脚发生变质，而小于95℃可防止水发生沸腾。
优选地，所述浸泡的时间为1-3h。
所述浸泡时间，是指得到饱和吸水油脚所需的时间，浸泡时间，从大豆油脚呈颗粒状在水中静置浸泡开始，到大豆油脚中开始出现棕色自聚集含水磷脂为止。浸泡中的大豆油脚为黄色，而出现的自聚集含水磷脂是棕色，因此可以目测判断浸泡是否达到结束时间。
优选地，所述浸泡为静置浸泡。
浸泡期间，不宜有搅拌操作，以防止出现乳化现象。
优选地，在浸泡之前，所述大豆油脚以搅拌的方式在水中打散成为颗粒状。
更优选地，所述大豆油脚颗粒的粒径≤5mm。
更优选地，所述大豆油脚颗粒的粒径为0.3-3mm。
大豆油脚粒径越小，油脚与水的接触面积越大，越有利于提高大豆油脚中磷脂与水的传质与传热效率。但是，大豆油脚粒径太小，存在大豆油脚与水被混合均匀、出现均质化的风险，破坏了浸泡体系。
优选地，所述制备方法还包括在所述浸泡体系中添加电解质。
更优选地，所述电解质在水中的质量分数为0.01-0.3％。
适量的电解质有利于大豆油脚中磷脂与水的结合，电解质过多时会抑制磷脂与水的结合，太少或者不添加电解质，则自聚集含水磷脂的含水量偏高，造成脱水时的能源浪费。
更优选地，所述电解质包括酸、碱和盐中的至少一种。
更优选地，所述电解质为DL-苹果酸钠、L-苹果酸、DL-苹果酸、冰乙酸、柠檬酸、柠檬酸钾、柠檬酸钠、柠檬酸一钠、葡萄糖酸钠、乳酸、乳酸钾、乳酸钠、碳酸钾、碳酸钠、碳酸氢钾、碳酸氢钠、硫酸钠、氯化钾、氢氧化钾、氢氧化钠、盐酸、磷酸和氯化钠中的至少一种。
优选地，所述自然沉降的时间为3-8h。
所述自然沉降的结果，是得到自聚集含水磷脂。在自然沉降结束时，从饱和吸水油脚得到自聚集含水磷脂和油脚剩余物两种组份。自然沉降期间，不宜有搅拌操作，以防止出现乳化现象。
本发明还涉及上述自聚集含水磷脂或者上述制备方法制备得到的自聚集含水磷脂在制备粉末磷脂中的应用。
优选地，采用所述自聚集含水磷脂制备粉末磷脂，包括如下步骤：
(1)制备浓缩含水磷脂：将所述自聚集含水磷脂在真空条件下在90-110℃使含水量浓缩到25-65g/100g，得到浓缩含水磷脂，其干基丙酮不溶物含量为92.5-95.5g/100g，感官指标为棕色半透明流体。
(2)制备含水磷脂弹性体：将所述浓缩含水磷脂以10-100cm/min的速度推送到搅拌器中，搅拌转数为800-1200rpm，搅拌时间为5-30s，得到连续输出的含水磷脂弹性体，其含水量、丙酮不溶物含量与浓缩含水磷脂相同，但感官指标变化为黄色不透明半固体。
所述含水磷脂弹性体，是指该含水磷脂是一种胶体化学范畴的弹性体，其流变学性质为储能模量G′比损耗模量G″大5-10倍，表现出较强的固体特征(弹性)，而液体特征(粘性)变得较弱，属于弹性体。
(3)制备固体磷脂：将所述连续输出的含水磷脂弹性体通过孔径为2-6mm的进料口，送入常压或者真空连续干燥机中，在120-160℃干燥6-20min，得到连续输出的条状固体磷脂，其含水量为3-10g/100g，干基丙酮不溶物含量为92.5-95.5g/100g，感官指标为黄色条状固体。
(4)制备粉末磷脂：将所述条状固体磷脂粉碎、过筛，在60℃真空干燥30-60min，得到粉末磷脂，其含水量为≤2g/100g，干基丙酮不溶物含量为92.5-95.5g/100g，感官指标为黄色粉末，产品执行国家标准《GB28401食品添加剂磷脂》。
步骤(4)所述粉末磷脂的含水量，等同于国家标准《GB28401食品添加剂磷脂》所述的干燥减量。
所述真空为0.01-0.004MPa。
本发明的有益效果是：
第一、本发明自聚集含水磷脂的含水量达到了70-80g/100g，磷脂吸水量达到了饱和：磷脂吸水量达到饱和时，磷脂亲油性降低到最小，即自聚集含水磷脂的油脂含量最小，且磷脂的纯度最高，其干基丙酮不溶物含量达到92.5-95.5g/100g。
第二、本发明自聚集含水磷脂的干基丙酮不溶物含量，在目前所有水化法中是最高的：本发明自聚集含水磷脂的干基丙酮不溶物含量为92.5-95.5g/100g，专利公开的水合磷脂为90-92g/100g，文献报道的液晶态磷脂为86.05g/100g。
第三、本发明自聚集含水磷脂的干基丙酮不溶物含量与溶剂法最相近：本发明自聚集含水磷脂的干基丙酮不溶物含量为92.5-95.5g/100g，已经接近甚至达到了溶剂法粉末磷脂95-98g/100g的水平。从行业发展的角度看，水化法最终要替代溶剂法成为主流产品，以消除有机溶剂造成的环境污染、溶剂残留造成的食品安全隐患和降低生产成本，本发明自聚集含水磷脂是目前最适合替代溶剂法的磷脂产品，产品中不含有机溶剂。
第四、本发明自聚集含水磷脂及其制备的粉末磷脂，从大豆油脚到粉末磷脂具有完整的工艺技术，在品质、保质期、生产成本、环保和食品安全方面都具有很大优势，适合工业化生产。
本发明优化了水的用量、浸泡体系的分散相油脚颗粒粒径、温度和时间等工 艺参数，使自聚集含水磷脂的含水量达到饱和，使其干基丙酮不溶物含量达到水化法的最高值。
附图说明
图1为大豆油脚浸泡并自然沉降得到自聚集含水磷脂的工艺流程图。
图2为大豆油脚浸泡并自然沉降得到自聚集含水磷脂的工艺示意图。其中：
(a)为大豆油脚在水中的示意图；
(b)为大豆油脚颗粒是分散相、水是连续相的浸泡体系示意图；
(c)为饱和吸水油脚开始出现自然沉降的自聚集含水磷脂的示意图；
(d)为饱和吸水油脚经自然沉降得到自聚集含水磷脂和油脚剩余物的示意图。
图3为自聚集含水磷脂制备固体磷脂的工艺流程图。
图4为浓缩含水磷脂制备固体磷脂的工艺示意图。
图5为应用例1自聚集含水磷脂制备得到的含水磷脂弹性体的储能模量G′与损耗模量G″的流变学特征图。
图6为应用例2自聚集含水磷脂制备得到的含水磷脂弹性体的储能模量G′与损耗模量G″的流变学特征图。
其中：(1)是连续相水；(2)是大豆油脚；(3)是分散相大豆油脚颗粒；(4)是饱和吸水油脚；(5)是自聚集含水磷脂；(6)是油脚剩余物；(7)是浓缩含水磷脂；(8)是含水磷脂弹性体；(9)是固体磷脂。A是浸泡罐；B是调速齿轮泵；C是管道搅拌器；D是连续式干燥机。
具体实施方式
以下结合附图对本发明的内容作进一步说明。下述实施例中所述实验方法，如无特殊说明，均为常规方法；所述试剂和材料，如无特殊说明，均可从商业途径获得；所述真空为0.01-0.004MPa。
自聚集含水磷脂的干基丙酮不溶物得率的定义：
自聚集含水磷脂的干基丙酮不溶物得率＝自聚集含水磷脂的干基丙酮不溶物重量/大豆油脚干基丙酮不溶物重量。
实施例1
一种自聚集含水磷脂，制备方法参照图1和图2(a)-图2(d)，其制备方 法包括如下步骤：
(1)浸泡：取大豆油脚加入水中，以搅拌方式把油脚在水中打散成为颗粒状，形成以大豆油脚颗粒为分散相、水为连续相的浸泡体系，浸泡温度为60℃，浸泡时间为3h，得到饱和吸水油脚。所述饱和吸水油脚，以开始出现棕色自聚集含水磷脂为标志。
所述大豆油脚来自中粮佳悦(天津)有限公司，其物质组成：含水量是41.03g/100g，干基丙酮不溶物含量是61.13g/100g；所述水，是生活饮用水；油脚与水的质量比为1:1；所述油脚颗粒，其粒径为0.3-3mm。
(2)自然沉降：饱和吸水油脚，保持浸泡的温度自然沉降3h，得到自聚集含水磷脂和油脚剩余物。
所得到的自聚集含水磷脂的含水量为77.78g/100g，干基丙酮不溶物含量为93.81g/100g，感官指标为棕色半透明流体，自聚集含水磷脂的干基丙酮不溶物得率为75.63％。
实施例2
一种自聚集含水磷脂，制备方法参照图1和图2(a)-图2(d)，其制备方法包括如下步骤：
(1)浸泡：取大豆油脚加入水中，以搅拌方式把油脚在水中打散成为颗粒状，形成以大豆油脚颗粒为分散相、水为连续相的浸泡体系，浸泡温度为70℃，浸泡时间为3h，得到饱和吸水油脚。所述饱和吸水油脚，以开始出现棕色自聚集含水磷脂为标志。
所述油脚来自中粮粮油工业(九江)有限公司，其物质组成：含水量是37.56g/100g，干基丙酮不溶物含量是60.87g/100g；所述水，是饮用净化水，在水中加入食盐氯化钠，添加量是饮用净化水重量的0.07％；油脚与水的质量比为1:1.5；所述油脚颗粒，其粒径为0.3-3mm。
(2)自然沉降：饱和吸水油脚，保持浸泡的温度自然沉降8h，得到自聚集含水磷脂和油脚剩余物。
所得到的自聚集含水磷脂的含水量为74.00g/100g，干基丙酮不溶物含量为93.75g/100g，感官指标为棕色半透明流体，自聚集含水磷脂的干基丙酮不溶物得率为78.09％。
实施例3
一种自聚集含水磷脂，参照图1和图2(a)-图2(d)，其制备方法包括如下步骤：
(1)浸泡：取大豆油脚加入水中，以搅拌方式把油脚在水中打散成为颗粒状，形成以大豆油脚颗粒为分散相、水为连续相的浸泡体系，浸泡温度为80℃，浸泡时间为2h，得到饱和吸水油脚。所述饱和吸水油脚，以开始出现棕色自聚集含水磷脂为标志。
所述油脚来自中粮粮油工业(黄冈)有限公司，其物质组成：含水量是38.42g/100g，干基丙酮不溶物含量是61.02g/100g；所述水，是饮用净化水，在水中加入浓度为80％的食品添加剂乳酸，添加量是饮用净化水重量的0.05％；油脚与水的质量比为1:2；所述油脚颗粒，其粒径为0.3-3mm。
(2)自然沉降：饱和吸水油脚，保持浸泡的温度自然沉降4h，得到自聚集含水磷脂和油脚剩余物。
所得到的自聚集含水磷脂的含水量为73.12g/100g，干基丙酮不溶物含量为92.53g/100g，感官指标为棕色半透明流体，自聚集含水磷脂的干基丙酮不溶物得率为80.72％。
实施例4
一种自聚集含水磷脂，参照图1和图2(a)-图2(d)，其制备方法包括如下步骤：
(1)浸泡：取大豆油脚加入水中，以搅拌方式把油脚在水中打散成为颗粒状，形成以大豆油脚颗粒为分散相、水为连续相的浸泡体系，浸泡温度为90℃，浸泡时间为2h，得到饱和吸水油脚。所述饱和吸水油脚，以开始出现棕色自聚集含水磷脂为标志。
所述油脚来自邦基(南京)粮油有限公司，其物质组成：含水量是39.78g/100g，干基丙酮不溶物含量是62.05g/100g；所述水，是饮用净化水，在水中加入食品添加剂氢氧化钠，添加量是饮用净化水重量的0.03％；油脚与水的质量比为1:2.5；所述油脚颗粒，其粒径为0.3-3mm。
(2)自然沉降：饱和吸水油脚，保持浸泡的温度自然沉降5h，得到自聚集含水磷脂和油脚剩余物。
所得到的自聚集含水磷脂的含水量为77.56g/100g，干基丙酮不溶物含量为95.42g/100g，感官指标为棕色半透明流体，自聚集含水磷脂的干基丙酮不溶物得 率为82.71％。
实施例5
一种自聚集含水磷脂，参照图1和图2(a)-图2(d)，其制备方法包括如下步骤：
(1)浸泡：取大豆油脚加入水中，以搅拌方式把油脚在水中打散成为颗粒状，形成以大豆油脚颗粒为分散相、水为连续相的浸泡体系，浸泡温度为95℃，浸泡时间为1h时，得到饱和吸水油脚。所述饱和吸水油脚，以开始出现棕色自聚集含水磷脂为标志。
所述油脚来自中储粮镇江粮油有限公司，其物质组成：含水量是37.69g/100g，干基丙酮不溶物含量是63.45g/100g；所述水，是饮用净化水，在水中加入食品添加剂柠檬酸和食盐氯化钠，柠檬酸添加量是饮用净化水重量的0.028％，食盐添加量是饮用净化水重量的0.052％；油脚与水的质量比为1:3；所述油脚颗粒，其粒径为0.3-3mm。
(2)自然沉降：饱和吸水油脚，保持浸泡的温度自然沉降6h，得到自聚集含水磷脂和油脚剩余物。
所得到的自聚集含水磷脂的含水量为72.33g/100g，干基丙酮不溶物含量为93.65g/100g，感官指标为棕色半透明流体，自聚集含水磷脂的干基丙酮不溶物得率为83.35％。
实施例6
一种自聚集含水磷脂，参照图1和图2(a)-图2(d)，其制备方法包括如下步骤：
(1)浸泡：取大豆油脚加入水中，以搅拌方式把油脚在水中打散成为颗粒状，形成以大豆油油脚颗粒为分散相、水为连续相的浸泡体系，浸泡温度为95℃，浸泡时间为1h时，得到饱和吸水油脚。所述饱和吸水油脚，以开始出现棕色自聚集含水磷脂为标志。
所述油脚来自中纺粮油(东莞)有限公司，其物质组成：含水量是40.23g/100g，干基丙酮不溶物含量是62.39g/100g；所述水，是饮用净化水，在水中加入食品添加剂柠檬酸，柠檬酸添加量是饮用净化水重量的0.038％；油脚与水的质量比为1:3.5；所述油脚颗粒，其粒径为0.3-3mm。
(2)自然沉降：饱和吸水油脚，保持浸泡的温度自然沉降7h，得到自聚集 含水磷脂和油脚剩余物。
所得到的自聚集含水磷脂的含水量为73.01g/100g，干基丙酮不溶物含量为94.18g/100g，感官指标为棕色半透明流体，自聚集含水磷脂的干基丙酮不溶物得率为83.98％。
对比例1
一种由大豆油脚制备水合磷脂的方法，方法来源于专利CN107325125A公开的一种大豆油脚制备水合磷脂的方法，包括如下步骤：
取大豆油脚，加入0.53倍大豆油脚重量的饮用净化水、加入大豆油脚重量的0.03％硫酸混合均匀，将混合物加热到85℃后保温静置6小时，然后在85℃、4500r/min条件下离心分离5min，得到水合磷脂。所用大豆油脚由中粮粮油工业(黄冈)有限公司生产，其含水量为38.42g/100g，干基丙酮不溶物含量为61.02g/100g。
所得的水合磷脂，含水量为64.03g/100g，干基丙酮不溶物含量为90.01g/100g，感官指标为棕色半透明流体。
本发明与对比例1制备的水合磷脂进行比较，主要区别包括如下几个方面：
第一、水化方法和磷脂含水量不同：水合磷脂是一种均质水化法制备的，大豆油脚与水需要混合均匀，水化操作的加水量为油脚重量的0.25-0.74倍，水多则发生乳化，所以水合磷脂的吸水量远未达到饱和的程度，磷脂含水量仅为64.03g/100g；本发明自聚集含水磷脂是浸泡水化法制备的，大豆油脚以颗粒状作为分散相，以水为连续相，构成浸泡体系，水化操作的加水量为油脚重量的1.0-3.5倍，确保在磷脂的周围存在多余的游离水，确保磷脂吸水量达到饱和，该饱和值为70-80g/100g。只有磷脂的含水量达到饱和，磷脂的丙酮不溶物含量才能达到最大值，该最大值为92.5-95.5g/100g。
第二、磷脂纯度不同：水合磷脂的干基丙酮不溶物含量为90-92g/100g；本发明自聚集含水磷脂的干基丙酮不溶物含量为92.5-95.5g/100g，是目前水化法磷脂中含量最高的，已经接近甚至达到溶剂法95-98g/100g的水平。
对比例2
一种由大豆油脚制备液晶态磷脂的方法，方法来源于文献《液晶态分离提纯大豆磷脂的研究》，包括如下步骤：
取大豆油脚，加入0.67倍大豆油脚重量的饮用净化水混合均匀，将混合物加热到70℃后保温静置4小时，然后在70℃、4500r/min条件下离心分离5min，得到液晶态磷脂。所用大豆油脚由中纺粮油(东莞)有限公司生产，其含水量为40.23g/100g，干基丙酮不溶物含量为62.39g/100g。
所得的液晶态磷脂，含水量为63.89g/100g，干基丙酮不溶物含量为86.23g/100g，感官指标为棕色半透明流体。
把液晶态磷脂通过一组孔径为2mm的圆形进料口，在干燥托盘上布料，在间歇式真空干燥箱中65℃干燥240min，得到棕色块状固体磷脂，其含水量为6.38g/100g，干基丙酮不溶物含量为86.23g/100g；取所述棕色固体磷脂粉碎、过18目筛，在真空干燥箱中60℃干燥30min，得到粉末磷脂，含水量为1.24g/100g，干基丙酮不溶物含量为86.23g/100g，感官指标为褐色粉末。
本发明与对比例2制备的液晶态磷脂进行比较，主要区别包括如下几个方面：
第一、水化程度不同：液晶态磷脂的含水量只有63.89g/100g，液晶态磷脂是一种均质水化法制备的，大豆油脚与水需要混合均匀，需要严格控制加水量，否则会发生乳化，水化操作的加水量为油脚重量的0.67倍，所以液晶态磷脂的吸水量远未达到饱和的程度，缺陷与专利水合磷脂完全相同；本发明自聚集含水磷脂的含水量为70-80g/100g，自聚集含水磷脂是浸泡水化法制备的，大豆油脚以颗粒状作为分散相，以水为连续相，构成浸泡体系，水化操作的加水量为油脚重量的1.0-3.5倍，确保磷脂吸水量达到饱和。只有磷脂吸水量达到饱和，磷脂的丙酮不溶物含量才能达到最大值。
第二、磷脂纯度不同：液晶态磷脂的干基丙酮不溶物含量仅为86.23g/100g，干燥制取的固体磷脂为棕色、粉末磷脂为褐色；本发明的自聚集含水磷脂的干基丙酮不溶物含量为92.5-95.5g/100g，两者干基丙酮不溶物含量相差较大。本发明自聚集含水磷脂制取的固体磷脂和粉末磷脂均为黄色。
对比例3
一种粉末大豆磷脂的制备方法，方法来源于专利CN103665029A一种粉末大豆磷脂的制备方法，包括如下步骤：
⑴按大豆油脚与无水丙酮以1:10的重量比混合，在常压、室温条件下搅拌萃取20min，离心分离进行固液分离，离心时间1min，离心速度为4000rpm，收 集固体部分。
所述大豆油脚来自邦基(南京)粮油有限公司，其物质组成：含水量为39.78g/100g，干基丙酮不溶物含量62.05g/100g。
⑵对步骤⑴所得到的固体部分，按照固体部分与无水丙酮以1:10的重量比例混合，在常压、室温条件下搅拌萃取20min，然后离心分离进行固液分离，离心时间1min，离心速度为5000rpm，收集固体部分。将固体部分进行破碎，在真空60℃条件下干燥5h，得到大豆粉末磷脂，干基丙酮不溶物含量为95.30g/100g，干燥减量为0.65g/100g，为褐色粉末。
本发明与对比例3制备的粉末磷脂进行比较，主要区别包括如下几个方面：
第一、环保与食品安全性的区别：对比例3是溶剂法制备的粉末磷脂，溶剂法存在溶剂挥发的环境污染，产品干燥减量为0.65g/100g，干燥减量的成分是溶剂，存在溶剂残留的食品安全隐患；本发明的应用制备的粉末磷脂，属于水化法，没有环境污染，产品干燥减量为≤2g/100g，干燥减量的成分是水，没有食品安全隐患。
第二、色泽上的区别：对比例3制备的粉末磷脂是褐色，为了降低溶剂残留干燥时间长，磷脂的色泽较深；本发明的自聚集含水磷脂在制备粉末磷脂时的干燥时间短，磷脂色泽为自然黄色。
应用例1
由实施例2自聚集含水磷脂制备固体磷脂、粉末磷脂的应用，参照图3和图4，包括如下步骤：
(1)取实施例2制备的自聚集含水磷脂进行浓缩，得到浓缩含水磷脂；(2)对浓缩含水磷脂进行搅拌，得到含水磷脂弹性体；(3)对含水磷脂弹性体进行干燥，得到条形固体磷脂；(4)对条形固体磷脂进行粉碎、过筛、干燥，得到粉末磷脂。
步骤(1)制备浓缩含水磷脂：将实施例2的自聚集含水磷脂在真空薄膜蒸发器中在95℃使含水量浓缩到55g/100g，得到浓缩含水磷脂，其干基丙酮不溶物含量为93.75g/100g，感官指标为棕色半透明流体。
步骤(2)制备含水磷脂弹性体：将步骤(1)浓缩含水磷脂以80cm/min的速度推送到搅拌器中，搅拌转数为900rpm，搅拌时间为10s，得到连续输出的含 水磷脂弹性体，其含水量、丙酮不溶物含量与浓缩含水磷脂相同，但感官指标变化为黄色不透明半固体。
步骤(3)制备固体磷脂：将步骤(2)连续输出的含水磷脂弹性体通过一组孔径为3mm的进料口，送入常压连续干燥机中，在150℃干燥8min，得到连续输出的条状固体磷脂，其含水量为7.23g/100g，干基丙酮不溶物含量为93.75g/100g，感官指标为黄色条状固体。
步骤(4)制备粉末磷脂：将步骤(3)条状固体磷脂粉碎、过18目筛，在双锥回旋真空干燥机中在60℃真空干燥40min，得到粉末磷脂，其含水量为1.43g/100g，干基丙酮不溶物含量为93.75g/100g，感官指标为黄色粉末，产品执行国家标准《GB28401食品添加剂磷脂》。
应用例2
由实施例4自聚集含水磷脂制备固体磷脂、粉末磷脂的应用，参照图3和图4，包括如下步骤：
(1)取实施例4制备的自聚集含水磷脂进行浓缩，得到浓缩含水磷脂；(2)对浓缩含水磷脂进行搅拌，得到含水磷脂弹性体；(3)对含水磷脂弹性体进行干燥，得到条形固体磷脂；(4)对条形固体磷脂进行粉碎、过筛、干燥，得到粉末磷脂。
步骤(1)制备浓缩含水磷脂：将实施例4的自聚集含水磷脂在真空薄膜蒸发器中在105℃使含水量浓缩到45g/100g，得到浓缩含水磷脂，其干基丙酮不溶物含量为95.42g/100g，感官指标为棕色半透明流体。
步骤(2)制备含水磷脂弹性体：将步骤(1)浓缩含水磷脂以40cm/min的速度推送到搅拌器中，搅拌转数为1100rpm，搅拌时间为20s，得到连续输出的含水磷脂弹性体，其含水量、丙酮不溶物含量与浓缩含水磷脂相同，但感官指标变化为黄色不透明半固体。
步骤(3)制备固体磷脂：将步骤(2)连续输出的含水磷脂弹性体通过一组孔径为4mm的进料口，送入真空连续干燥机中，在130℃干燥15min，得到连续输出的条状固体磷脂，其含水量为5.32g/100g，干基丙酮不溶物含量为95.42g/100g，感官指标为黄色条状固体。
步骤(4)制备粉末磷脂：将步骤(3)条状固体磷脂粉碎、过18目筛，在双锥回旋真空干燥机中在60℃真空干燥30min，得到粉末磷脂，其含水量为 1.18g/100g，干基丙酮不溶物含量为95.42g/100g，感官指标为黄色粉末，产品执行国家标准《GB28401食品添加剂磷脂》。
测试例1
对应用例1、应用例2制得的含水磷脂弹性体进行流变学表征，测试结果分别如图5、图6所示。检测所采用的仪器及参数为：RS6000旋转流变仪(德国HAAKE公司)，测量转子使用Z41Ti同轴转筒传感系统(转筒和转子的直径分别为43.40mm和41.42mm)，样品在传感系统中央的厚度为3mm。
由图5、图6可以看出，应用例1、应用例2提供的含水磷脂弹性体在测量的频率范围内，储能模量G′比损耗模量G″大5倍以上，而且它们几乎与频率无关，说明弹性远远大于粘性，表现出较强的固体特征(弹性)，而液体特征(粘性)变得较弱，属于弹性体。
上述详细说明是针对本发明其中之一可行实施例的具体说明，该实施例并非用以限制本发明的专利范围，凡未脱离本发明所为的等效实施或变更，均应包含于本发明技术方案的范围内。

Claims (10)

  1. 一种自聚集含水磷脂，其特征在于，所述自聚集含水磷脂的主要成分是磷脂、油脂和水，含水量为70-80g/100g，以干基计丙酮不溶物含量为92.5-95.5g/100g。
  2. 根据权利要求1所述的自聚集含水磷脂，其特征在于，所述自聚集含水磷脂为棕色半透明流体。
  3. 一种权利要求1或2所述的自聚集含水磷脂的制备方法，其特征在于，包括如下步骤：将大豆油脚在水中浸泡，得到饱和吸水油脚，自然沉降，即得。
  4. 根据权利要求3所述的制备方法，其特征在于，所述大豆油脚与水的质量比为1:1-3.5。
  5. 根据权利要求3所述的制备方法，其特征在于，所述浸泡的温度为60-95℃，所述浸泡的时间为1-3h，所述自然沉降的时间为3-8h。
  6. 根据权利要求3所述的制备方法，其特征在于，在所述浸泡之前，所述大豆油脚以搅拌的方式在水中打散成为颗粒状，颗粒粒径≤5mm。
  7. 根据权利要求3所述的制备方法，其特征在于，所述制备方法还包括在所述浸泡体系中添加电解质。
  8. 根据权利要求7所述的制备方法，其特征在于，所述电解质在水中的质量分数为0.01-0.3％；所述电解质包括酸、碱和盐中的至少一种。
  9. 根据权利要求7所述的制备方法，其特征在于，所述电解质为DL-苹果酸钠、L-苹果酸、DL-苹果酸、冰乙酸、柠檬酸、柠檬酸钾、柠檬酸钠、柠檬酸一钠、葡萄糖酸钠、乳酸、乳酸钾、乳酸钠、碳酸钾、碳酸钠、碳酸氢钾、碳酸氢钠、硫酸钠、氯化钾、氢氧化钾、氢氧化钠、盐酸、磷酸和氯化钠中的至少一种。
  10. 权利要求1-2任一项所述自聚集含水磷脂或权利要求3-9任一项所述的制备方法制备得到的自聚集含水磷脂在制备粉末磷脂中的应用。
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