CN111595112A

CN111595112A - Preparation method of powdered phospholipid

Info

Publication number: CN111595112A
Application number: CN202010455170.4A
Authority: CN
Inventors: 徐子谦
Original assignee: Inner Mongolia Boberman Technology Co ltd
Current assignee: Shanghai Beiman Technology Co.,Ltd.
Priority date: 2020-05-26
Filing date: 2020-05-26
Publication date: 2020-08-28
Anticipated expiration: 2040-05-26
Also published as: CN111595112B

Abstract

The invention belongs to the technical field of phospholipid processing, and particularly relates to a preparation method of powdered phospholipid. The preparation method comprises the steps of soaking soybean oil residue in water, naturally settling to obtain self-aggregation water-containing phospholipid, concentrating, stirring and continuously drying the self-aggregation water-containing phospholipid to obtain solid phospholipid, crushing, sieving and drying to obtain powder phospholipid, wherein the content of acetone insoluble substances reaches 92.5-95.5g/100g, the powder phospholipid is natural yellow, and has no solvent and no bleaching. The invention solves the problems of low phospholipid content, deep color, long drying time and lack of industrial feasibility of the existing hydration method powder phospholipid; the preparation method of solvent method powder phospholipid can be replaced to eliminate the pollution of solvent to the environment and the hidden danger of food safety caused by solvent residue and reduce the production cost; and the physical method of stirring is used for changing the color of the object so as to eliminate the hidden danger of food safety brought by chemical bleaching.

Description

Preparation method of powdered phospholipid

Technical Field

The invention belongs to the technical field of phospholipid processing, and particularly relates to a preparation method of powdered phospholipid.

Background

The raw material for processing the phospholipid is soybean oil residue, which is called hydrated oil residue for short, is a byproduct of a hydration degumming process in the soybean oil refining process in the field of oil processing, and is also called hydrated oil residue, wherein the main components comprise 30-45g/100g of phospholipid, 20-30g/100g of soybean oil and 30-50g/100g of water, and the trace components comprise metal ions, such as calcium, magnesium, iron and the like, and exist in the form of phospholipid metal salts, such as iron ion content, usually 50-100mg/kg calculated by acetone insoluble substances, and the content is up to more than 150mg/kg in individual cases.

The method for processing the industrial phospholipid mainly comprises two methods, one is that the concentrated phospholipid is prepared by a hydration method, namely the concentrated phospholipid is obtained by directly drying and dehydrating after soybean oil residue is extracted from crude soybean oil in a hydration manner, and the concentrated phospholipid is also called as fluid phospholipid due to the fluidity, and the content of dry acetone insoluble substances is 60-65g/100 g; and secondly, preparing the powdered phospholipid by a solvent method, namely taking soybean oil residue or concentrated phospholipid as a raw material, and extracting the raw material by using acetone to remove grease to obtain the powdered phospholipid, wherein the content of dry acetone insoluble substances is 95-98g/100 g. The mainstream product in the market is concentrated phospholipid, and the ratio of the powdered phospholipid in the market is less than 5%.

Although the soybean oil residue is mostly processed into concentrated phospholipids, the concentrated phospholipids have a great disadvantage. For example, documents "a process for producing concentrated phospholipids from soybean (Huxing. a process for producing concentrated phospholipids from soybean [ J ]. China fat, 2007,32(9):20-21) and" a process for preparing concentrated phospholipids (Houqing et al. a process for preparing concentrated phospholipids [ J ]. China fat, 2002,27(1):39-40) describe a method for producing concentrated phospholipids by dehydrating and oxidizing and bleaching hydrated oil residues as raw materials. The process has the disadvantages that the content of acetone insoluble substances in the concentrated phospholipid is too low (60-65g/100g), chemical bleaching is needed, the market price is only 0.4 ten thousand yuan/ton, and the price has a large difference with the price of 4 ten thousand yuan/ton of powder phospholipid.

Chinese patent CN103665029A discloses a method for preparing soybean powder phospholipid, which adopts acetone as solvent to extract hydrated oil residue, separates out acetone insoluble substances, and then carries out low-temperature vacuum drying on the acetone insoluble substances to remove the solvent, thus obtaining the powder phospholipid. The method has the disadvantages of high production cost due to the use of acetone solvent, potential food safety hazards of environmental pollution and solvent residue, and difficulty in popularization.

For example, chinese patent CN107325125A discloses a method for preparing a phospholipid hydrate from soybean oil residue and a phospholipid hydrate (hereinafter referred to as phospholipid hydrate) prepared by the method, and the method includes the following steps: adding softened water into soybean oil residue, mixing, standing, and performing chromatography; after the chromatography is finished, controlling the temperature to be 85-95 ℃, and carrying out centrifugal separation to obtain the hydrated phospholipid, wherein the acetone insoluble matter can reach 90-92%. This patent has the following drawbacks:

(1) the dry acetone insoluble content of the hydrated phospholipids is low: the patent is a homogeneous hydration method, namely oil residue and water are mixed uniformly, emulsification inevitably occurs when the mixing is uniform, and phospholipid and oil are difficult to re-separate if the emulsification is serious. In order to avoid serious emulsification, the patent adopts two measures, namely strictly controlling the water adding amount which is 0.25-0.74 times of the weight of oil residue; second, sodium hydroxide or sulfuric acid is added, acting as a demulsifier. The problem brought by the measures is that the main components of phospholipid, grease and phospholipid metal salt in the soybean oil residue are not effectively separated, the content of dry acetone insoluble substances of the hydrated phospholipid reaches only 92 percent at most, and has a certain difference compared with 95-98 percent of acetone insoluble substances in a solvent method;

(2) the drying and dehydration are not completely dried, and the industrial application is lacked: the hydrated phospholipid is subjected to concentration dehydration, preservative addition, pasteurization and packaging to obtain an aqueous phospholipid product with the water content of 22.5-41.2 percent, but the aqueous phospholipid product does not meet the regulation of national standard GB28401 food additive phospholipid on that the water content cannot exceed 2 percent and cannot be sold; if the drying is performed according to the existing method for preparing powdered phospholipids, the time is too long, the productivity is too low, and the industrial production is not feasible, and the powdered phospholipids can not be sold or further processed, so that the powdered phospholipids are not industrially used.

Another prior art for extracting phospholipid by hydration method is disclosed in the document "research on liquid crystal separation and purification of soybean phospholipid" (Leziming et al. research on liquid crystal separation and purification of soybean phospholipid [ J ]. Chinese food and oil institute, 2007,22(1):31-32), hereinafter referred to as liquid crystal phospholipid. The method of the document has the following technical defects: (1) the content of insoluble acetone on dry basis of the liquid crystal state phospholipid is low: the homogeneous hydration method is adopted, the water adding amount is 0.67 times of oil residue, and the content of the obtained liquid crystal state phospholipid in dry acetone insoluble matters is only 86.05 percent, which is the same as the defect of the hydrated phospholipid; (2) lack of industrial use: the drying problem of the liquid crystal phospholipid is the same as that of the hydrated phospholipid, although the liquid crystal phospholipid is obtained into powder phospholipid by a batch vacuum drying mode, the drying time is too long, and the color of the phospholipid product is dark (brown), so that the liquid crystal phospholipid cannot be applied to industrial production.

Chinese patent CN102517148A discloses a two-step decolorization method of phospholipid, which adopts two-step decolorization methods of hydrogen peroxide bleaching and silica gel adsorption, and has the following defects: (1) chemical bleaching and decoloring, so that phospholipid generates oxidation byproducts, the naturalness of the phospholipid is damaged, and meanwhile, food safety risks exist and the method does not conform to the large trend of green development; (2) the adsorption and decoloration effects of silica gel are poor, and the invalid silica gel becomes waste residue, which is not beneficial to environmental protection; (3) bleaching destroys the beneficial antioxidant components in the phospholipid, reduces the antioxidant and nutritive values of the phospholipid, and shortens the shelf life of the phospholipid.

In the phospholipid processing field, the substitution of the powdered phospholipid for the concentrated phospholipid is the future direction from the product perspective, the substitution of the hydration method for the solvent method is the future direction from the method perspective, and although some researches on the hydration method exist at present, the purity of the phospholipid prepared by the hydration method is not high enough, the color improvement is not separated from the chemical bleaching method, the dehydration efficiency of the hydration method does not reach the industrial level, and the process technology is not enough in the aspects of integrity and continuity.

Disclosure of Invention

The invention aims to provide a preparation method of powdered phospholipid, which is used for solving the problems of low phospholipid content, deep color, long drying time and lack of industrial feasibility of the existing hydration method of powdered phospholipid; the preparation method of the powdered phospholipid by replacing a solvent method is used for eliminating the pollution of the solvent to the environment and the potential food safety hazard caused by the residual solvent and reducing the production cost; and the current chemical bleaching and decoloring method is replaced by a stirring physical method. The method for preparing the powdered phospholipid belongs to a hydration method, and the obtained powdered phospholipid has the acetone insoluble content of 92.5-95.5g/100g, natural yellow color, no solvent and no bleaching. The preparation method of the powder phospholipid is not reported in the phospholipid processing field and related researches.

In order to achieve the above purpose, the technical scheme provided by the invention is as follows:

a preparation method of powdered phospholipid comprises the following steps:

(1) hydration: soaking soybean oil residue in water, and naturally settling to obtain self-aggregating aqueous phospholipid;

(2) concentration: dehydrating the self-aggregating aqueous phospholipid fraction to obtain a concentrated aqueous phospholipid;

(3) stirring: stirring the concentrated aqueous phospholipid to obtain an aqueous phospholipid elastomer;

(4) and (3) continuous drying: continuously drying and dehydrating the aqueous phospholipid elastomer to obtain solid phospholipid;

(5) crushing, sieving and drying: and (3) crushing, sieving and drying the solid phospholipid to obtain the powder phospholipid.

Preferably, before the soaking in the step (1), the soybean oil foot is broken into particles in water in a stirring manner, the particle size of the oil foot is less than or equal to 5mm, and preferably 0.3-3mm, so that a soaking system with the oil foot particles as a dispersed phase and the water as a continuous phase is formed.

The smaller the particle size of the soybean oil residue is, the larger the contact area of the oil residue and water is, and the mass transfer and heat transfer efficiency of phospholipid and water in the soybean oil residue is improved. However, the particle size of the soybean oil residue is too small, so that the risk of uniform mixing, homogenization and even emulsification of the soybean oil residue and water exists, and the soaking system is damaged.

Preferably, the mass ratio of the soybean oil foot to the water in the step (1) is 1:1-3.5, the soaking temperature is 60-95 ℃, and the soaking time is 1-3 hours.

When the weight of the water is less than 1.0 time of that of the oil residue, the soybean oil residue can not be effectively soaked in the water, and the combination of the phospholipid and the water is further influenced. When the water is more than 3.5 times of the mass of the oil residue, although the soaking of the soybean oil residue is facilitated, the cost of water, the energy consumption and the volume of the equipment are increased.

In water at 0 ℃ to 100 ℃, the combination of phospholipid and water can occur, and the combination efficiency is higher at higher temperature. Therefore, the water temperature is increased, and the soaking time can be shortened. However, in boiling water, stabilization of self-aggregating aqueous phospholipids is not favored, and boiling evaporation of water wastes energy. The temperature of the soaking is therefore preferably 60-95 ℃. When the temperature is above 60 deg.C, the sterilization temperature can prevent oil residue from deteriorating during soaking, and when the temperature is below 95 deg.C, water can be prevented from boiling.

The result of the soaking was a saturated water absorption heel, marked by the onset of brown self-aggregating aqueous phospholipids in the soybean heel. The soaking time refers to the time required for obtaining saturated water absorption oil foot. The soaking time is from the beginning of standing and soaking the soybean oil residue in water in a granular form until brown self-aggregation water-containing phospholipid begins to appear in the soybean oil residue. The soybean oil foot in the soaking is yellow, and the self-aggregating aqueous phospholipid appeared is brown, so that it can be judged visually whether the saturated water-absorbing oil foot is obtained by the soaking.

Preferably, the soaking is standing soaking.

During the soaking period, stirring operation is not suitable to prevent emulsification.

Preferably, the soaking in the step (1) further comprises adding electrolyte into the oil residue or the water, wherein the electrolyte is added in an amount of 0.01-0.3% of the mass fraction of the water.

More preferably, the electrolyte comprises at least one of acid, alkali and salt, and preferably, the electrolyte is at least one of DL-sodium malate, L-malic acid, DL-malic acid, glacial acetic acid, citric acid, potassium citrate, sodium citrate, monosodium citrate, sodium gluconate, lactic acid, potassium lactate, sodium lactate, potassium carbonate, sodium carbonate, potassium bicarbonate, sodium sulfate, potassium chloride, potassium hydroxide, sodium hydroxide, hydrochloric acid, phosphoric acid and sodium chloride.

The proper amount of electrolyte is beneficial to the combination of the phospholipid and water in the soybean oil residue, the combination of the phospholipid and the water can be inhibited when the electrolyte is too much, and the water content of the self-aggregation water-containing phospholipid is higher when the electrolyte is too little or not added, so that the energy waste during dehydration is caused.

Preferably, the natural settling temperature in the step (1) is 60-95 ℃ and the time is 3-8 h.

The result of said natural sedimentation is a self-aggregating aqueous phospholipid. At the end of natural sedimentation, two components, namely the self-aggregating aqueous phospholipid and the residue of the oil residue, are obtained from the saturated water-absorbing oil residue.

Preferably, during the natural settling, stirring is not preferred to prevent emulsification.

Preferably, the main components of the self-aggregation water-containing phospholipid are phospholipid, grease and water, and the water content is 70-80g/100 g; the acetone insoluble content is 92.5-95.5g/100g on a dry basis, and the sensory index is a brown translucent fluid.

Preferably, the concentration in step (2) means evaporating and dehydrating the self-aggregated aqueous phospholipid to obtain a concentrated aqueous phospholipid, the water content of the concentrated aqueous phospholipid is 25-65g/100g, and the acetone insoluble content and sensory index of the concentrated aqueous phospholipid are the same as those of the self-aggregated aqueous phospholipid.

Preferably, the stirring in the step (3) is a continuous mode, the concentrated aqueous phospholipid is continuously pushed into the stirrer, the pushing speed is 10-100cm/min, the stirring speed is 800-.

Preferably, the aqueous phospholipid elastomer has the same water content and acetone insoluble content as the concentrated aqueous phospholipid, but the sensory index changes to a yellow opaque semi-solid.

The aqueous phospholipid elastomer is an elastomer in the colloid chemistry category, the rheological property of the aqueous phospholipid elastomer is that the storage modulus G 'is 5-10 times larger than the loss modulus G' and the aqueous phospholipid elastomer shows stronger solid characteristics (elasticity) and weaker liquid characteristics (viscosity) and belongs to the elastomer.

Preferably, the continuous drying in the step (4) includes two modes of normal pressure continuous drying and vacuum continuous drying, the drying temperature is 120-160 ℃, and the drying time is 6-20 min.

The result of said continuous drying is a solid phospholipid.

Preferably, the solid phospholipid has a water content of 3-10g/100g, a dry acetone insoluble content of 92.5-95.5g/100g and a yellow solid sensory index.

Preferably, the powdered phospholipid obtained in the step (5) has the water content of less than or equal to 2g/100g, the content of acetone insoluble substances in terms of dry basis of 92.5-95.5g/100g, the sensory index of the powdered phospholipid is yellow powder, and the product meets the national standard GB28401 food additive phospholipid.

The moisture content of the powder phospholipid is equal to the drying decrement of the national standard GB28401 food additive phospholipid.

Preferably, the drying in the step (5) refers to vacuum drying at 60 ℃ for 30-60min, and the vacuum is 0.01-0.004 MPa.

The invention has the beneficial effects that:

firstly, the preparation method of the hydration-method powder phospholipid has industrial feasibility: at present, the hydration method powder phospholipid is only researched in the literature of research on liquid crystal state separation and purification of soybean phospholipid, but the obtained powder phospholipid has low content, deep color and long drying time, and is lack of industrial feasibility. The dry acetone insoluble content of the hydration-method powder phospholipid prepared by the invention reaches 92.5-95.5g/100g, the color is natural yellow, the drying time for preparing the solid phospholipid is shortened to be within 20min, and the industrial technical problem of the hydration-method powder phospholipid preparation method is systematically solved.

Secondly, the preparation method of the hydration method powder phospholipid replaces the solvent method, and the technical conditions are mature: at present, powdered phospholipid is mainly produced by a solvent method, and the solvent method has the problems of environmental pollution, potential food safety hazards of solvent residues, high production cost and the like. From the viewpoint of industrial development, the hydration method is finally the mainstream preparation method of the powdered phospholipid instead of the solvent method. The content of the dry acetone insoluble substances of the hydration-method powdered phospholipid prepared by the invention is 92.5-95.5g/100g, is very close to the content of the dry acetone insoluble substances of the solvent-method powdered phospholipid (95-98g/100g), can completely replace the solvent-method powdered phospholipid, is beneficial to environmental protection and food safety, and the production cost of the hydration method is far lower than that of the solvent method.

Thirdly, the preparation method of the hydration-method powder phospholipid does not rely on chemical bleaching and decoloring: the phospholipids prepared by the prior art can be used for obtaining a yellow product only by chemical bleaching, and the chemically bleached phospholipids have oxidation byproducts, so that potential food safety hazards exist, and the quality guarantee period is greatly shortened; the invention adopts a physical stirring method to convert brown water-containing phospholipid into yellow water-containing phospholipid elastomer, obtains natural yellow powder phospholipid, does not need chemical bleaching, and maintains the naturalness and food safety of soybean phospholipid.

Fourthly, the powder phospholipid of the invention has complete preparation process and is suitable for industrial production.

Drawings

FIG. 1 is a flow chart of a process for preparing powdered phospholipids from soybean oil residues by hydration;

FIG. 2 is a schematic diagram of a process for preparing solid phospholipids from concentrated aqueous phospholipids by stirring and continuous drying;

FIG. 3 is a graph of the rheological profile of storage modulus G 'versus loss modulus G' for the aqueous phospholipid elastomer of example 2;

FIG. 4 rheological profile of storage modulus G 'versus loss modulus G' for example 4 aqueous phospholipid elastomer.

Wherein: the method comprises the steps of concentrating water-containing phospholipid; the preparation method comprises the following steps of (1) preparing a water-containing phospholipid elastomer; and the third is solid phospholipid. A is a speed-regulating gear pump; b is a pipeline stirrer; and C, a continuous dryer.

Detailed Description

The invention will be further described with reference to specific embodiments, and the advantages and features of the invention will become apparent as the description proceeds. These examples are illustrative only and do not limit the scope of the present invention in any way. It will be understood by those skilled in the art that various changes in form and details may be made therein without departing from the spirit and scope of the invention, and that such changes and modifications may be made without departing from the spirit and scope of the invention. The experimental methods described in the following examples are all conventional methods unless otherwise specified; the reagents and materials, unless otherwise indicated, are commercially available; the vacuum is 0.01-0.004 MPa.

Example 1

A method for preparing powdered phospholipid with reference to figures 1 and 2 comprises the following steps:

(1) hydration: adding soybean oil residue into water, and stirring to break the oil residue into granules in water to form a soaking system with soybean oil residue granules as disperse phase and water as continuous phase, wherein the soaking temperature is 60 ℃, and the soaking time is 3h to obtain saturated water-absorbing oil residue. The saturated water-absorbing oil foot is marked by the initial appearance of brown self-aggregating aqueous phospholipids.

The soybean oil residue is from Zhongliangyouyue (Tianjin) Co., Ltd, and the material composition is as follows: the water content was 41.03g/100g, the content of acetone insolubles on a dry basis was 61.13g/100 g; the water is drinking water; the mass ratio of oil residue to water is 1: 1; the grain diameter of the oil residue particles is 0.3-3 mm.

And (3) saturating the water-absorbing oil residue, and keeping the soaking temperature for natural settling for 3h to obtain the self-aggregation water-containing phospholipid and the oil residue.

The resulting self-aggregating aqueous phospholipid had a water content of 77.78g/100g, a dry acetone insoluble content of 93.81g/100g, and a sensory index of brown translucent fluid.

(2) Concentration: reducing the water content of the water-containing phospholipid obtained in the step (1) to 65g/100g in a vacuum thin film evaporator at 90 ℃ to obtain concentrated water-containing phospholipid, wherein the dry acetone insoluble content and sensory index of the concentrated water-containing phospholipid are the same as those of self-aggregation water-containing phospholipid;

(3) stirring: pushing the concentrated aqueous phospholipid obtained in the step (2) into a stirrer at a speed of 100cm/min, wherein the rotation speed is 800rpm, and the time is 5s, so as to obtain a continuously output aqueous phospholipid elastomer, wherein the water content and the acetone insoluble content of the aqueous phospholipid elastomer are the same as those of the concentrated aqueous phospholipid, but the sensory index of the aqueous phospholipid elastomer is changed into yellow opaque semisolid;

(4) and (3) continuous drying: feeding the continuously output water-containing phospholipid elastomer obtained in the step (3) into a normal-pressure continuous dryer through a feed inlet with the aperture of 2mm, and drying at 160 ℃ for 6min to obtain continuously output solid phospholipid, wherein the water content of the solid phospholipid is 9.95g/100g, the content of dry acetone insoluble substances is 93.81g/100g, and the sensory index of the solid phospholipid is yellow strip-shaped solid;

(5) crushing, sieving and drying: and (3) crushing the strip-shaped solid phospholipid obtained in the step (4), sieving the powder with a 18-mesh sieve, and drying the powder in a double-cone rotary vacuum dryer at 60 ℃ for 40min in vacuum to obtain powder phospholipid, wherein the water content of the powder phospholipid is 1.85g/100g, the content of the dry acetone insoluble substances is 93.81g/100g, the sensory index of the powder phospholipid is yellow powder, and the product meets the national standard GB28401 food additive phospholipid.

Example 2

(1) hydration: adding soybean oil residue into water, and stirring to break the oil residue into granules in water to form a soaking system with soybean oil residue granules as disperse phase and water as continuous phase, wherein the soaking temperature is 70 deg.C, and the soaking time is 3 hr to obtain saturated water-absorbing oil residue. The saturated water-absorbing oil foot is marked by the initial appearance of brown self-aggregating aqueous phospholipids.

The oil residue is from the food and grain industry (Jiujiang) limited company, and the material composition of the oil residue is as follows: the water content was 37.56g/100g, the dry acetone insoluble content was 60.87g/100 g; the water is purified drinking water, salt and sodium chloride are added into the water, and the adding amount of the salt and the sodium chloride is 0.07 percent of the weight of the purified drinking water; the mass ratio of oil residue to water is 1: 1.5; the grain diameter of the oil residue particles is 0.3-3 mm.

And (3) saturating the water-absorbing oil residue, and keeping the soaking temperature for natural sedimentation for 8h to obtain the self-aggregation water-containing phospholipid and the oil residue.

The resulting self-aggregating aqueous phospholipid had a water content of 74.00g/100g, a dry acetone insoluble content of 93.75g/100g, and a sensory index of brown translucent fluid.

(2) Concentration: reducing the water content of the water-containing phospholipid obtained in the step (1) to 55g/100g in a vacuum thin film evaporator at 95 ℃ to obtain concentrated water-containing phospholipid, wherein the dry acetone insoluble content and sensory index of the concentrated water-containing phospholipid are the same as those of self-aggregation water-containing phospholipid;

(3) stirring: pushing the concentrated aqueous phospholipid obtained in the step (2) into a stirrer at a speed of 80cm/min, wherein the rotation speed is 900rpm, and the time is 10s, so as to obtain a continuously output aqueous phospholipid elastomer, wherein the water content and the acetone insoluble content of the aqueous phospholipid elastomer are the same as those of the concentrated aqueous phospholipid, but the sensory index of the aqueous phospholipid elastomer is changed into yellow opaque semisolid;

(4) and (3) continuous drying: feeding the water-containing phospholipid elastomer continuously output in the step (3) into a normal-pressure continuous dryer through a feed inlet with the aperture of 3mm, and drying at 150 ℃ for 8min to obtain continuously output solid phospholipid, wherein the water content of the solid phospholipid is 7.23g/100g, the content of dry acetone insoluble substances is 93.75g/100g, and sensory indexes of the solid phospholipid are yellow strip-shaped solids;

(5) crushing, sieving and drying: and (3) crushing the strip-shaped solid phospholipid obtained in the step (4), sieving the powder with a 18-mesh sieve, and performing vacuum drying in a double-cone rotary vacuum dryer at 60 ℃ for 40min to obtain powder phospholipid, wherein the water content of the powder phospholipid is 1.43g/100g, the content of the dry acetone insoluble substances is 93.75g/100g, the sensory index of the powder phospholipid is yellow powder, and the product meets the national standard GB28401 food additive phospholipid.

Example 3

(1) hydration: adding soybean oil residue into water, and stirring to break the oil residue into granules in water to form a soaking system with soybean oil residue granules as disperse phase and water as continuous phase, wherein the soaking temperature is 80 deg.C, and the soaking time is 2 hr to obtain saturated water-absorbing oil residue. The saturated water-absorbing oil foot is marked by the initial appearance of brown self-aggregating aqueous phospholipids.

The oil residue is from the food, grain and oil industry (Huanggang) Co., Ltd, and the material composition is as follows: the water content is 38.42g/100g, and the content of acetone insoluble matter is 61.02g/100 g; the water is purified drinking water, food additive lactic acid with the concentration of 80% is added into the water, and the adding amount is 0.05% of the weight of the purified drinking water; the mass ratio of oil residue to water is 1: 2; the grain diameter of the oil residue particles is 0.3-3 mm.

And (3) saturating the water-absorbing oil residue, and keeping the soaking temperature for natural settling for 4 hours to obtain the self-aggregation water-containing phospholipid and the oil residue.

The resulting self-aggregating aqueous phospholipid had a water content of 73.12g/100g, a dry acetone insoluble content of 92.53g/100g, and a sensory index of brown translucent fluid.

(2) Concentration: reducing the water content of the water-containing phospholipid obtained in the step (1) to 50g/100g in a vacuum thin film evaporator at 100 ℃ to obtain a concentrated water-containing phospholipid, wherein the dry acetone insoluble content and sensory index of the concentrated water-containing phospholipid are the same as those of the self-aggregation water-containing phospholipid;

(3) stirring: pushing the concentrated aqueous phospholipid obtained in the step (2) into a stirrer at the speed of 60cm/min, wherein the rotation speed is 1000rpm, and the time is 15s, so as to obtain a continuously output aqueous phospholipid elastomer, wherein the water content and the acetone insoluble content of the aqueous phospholipid elastomer are the same as those of the concentrated aqueous phospholipid, but the sensory index of the aqueous phospholipid elastomer is changed into yellow opaque semisolid;

(4) and (3) continuous drying: feeding the water-containing phospholipid elastomer continuously output in the step (3) into a vacuum continuous dryer through a feed inlet with the aperture of 3.5mm, and drying at 140 ℃ for 10min to obtain continuously output strip-shaped solid phospholipid, wherein the water content of the strip-shaped solid phospholipid is 5.67g/100g, the content of dry acetone insoluble substances is 92.53g/100g, and sensory indexes of the strip-shaped solid are yellow;

(5) crushing, sieving and drying: and (3) crushing the strip-shaped solid phospholipid obtained in the step (4), sieving the powder with a 18-mesh sieve, and performing vacuum drying in a double-cone rotary vacuum dryer at 60 ℃ for 60min to obtain powder phospholipid, wherein the water content of the powder phospholipid is 0.35g/100g, the content of the dry acetone insoluble substances is 92.53g/100g, the sensory index of the powder phospholipid is yellow powder, and the product meets the national standard GB28401 food additive phospholipid.

Example 4

(1) hydration: adding soybean oil residue into water, and stirring to break the oil residue into granules in water to form a soaking system with soybean oil residue granules as disperse phase and water as continuous phase, wherein the soaking temperature is 90 deg.C, and the soaking time is 2 hr to obtain saturated water-absorbing oil residue. The saturated water-absorbing oil foot is marked by the initial appearance of brown self-aggregating aqueous phospholipids.

The oil foot is from the Pongji (Nanjing) grain and oil Co., Ltd, and the material composition of the oil foot is as follows: the water content is 39.78g/100g, and the content of acetone insoluble matter is 62.05g/100 g; the water is purified drinking water, and a food additive sodium hydroxide is added into the water, wherein the addition amount of the sodium hydroxide is 0.03 percent of the weight of the purified drinking water; the mass ratio of oil residue to water is 1: 2.5; the grain diameter of the oil residue particles is 0.3-3 mm.

And (3) saturating the water-absorbing oil residue, and keeping the soaking temperature for natural settling for 5h to obtain the self-aggregation water-containing phospholipid and the oil residue.

The resulting self-aggregating aqueous phospholipid had a water content of 77.56g/100g, a dry acetone insoluble content of 95.42g/100g, and a sensory index of brown translucent fluid.

(2) Concentration: reducing the water content of the water-containing phospholipid obtained in the step (1) to 45g/100g in a vacuum thin film evaporator at 105 ℃ to obtain a concentrated water-containing phospholipid, wherein the dry acetone insoluble content and sensory index of the concentrated water-containing phospholipid are the same as those of the self-aggregation water-containing phospholipid;

(3) stirring: pushing the concentrated aqueous phospholipid obtained in the step (2) into a stirrer at a speed of 40cm/min, wherein the rotation speed is 1100rpm, and the time is 20s, so as to obtain a continuously output aqueous phospholipid elastomer, wherein the water content and the acetone insoluble content of the aqueous phospholipid elastomer are the same as those of the concentrated aqueous phospholipid, but the sensory index of the aqueous phospholipid elastomer is changed into yellow opaque semisolid;

(4) and (3) continuous drying: feeding the continuously output water-containing phospholipid elastomer obtained in the step (3) into a vacuum continuous dryer through a feed inlet with the aperture of 4mm, and drying at 130 ℃ for 15min to obtain continuously output solid phospholipid, wherein the water content of the solid phospholipid is 5.32g/100g, the content of dry acetone insoluble substances is 95.42g/100g, and the sensory index of the solid phospholipid is yellow strip-shaped solid;

(5) crushing, sieving and drying: and (3) crushing the strip-shaped solid phospholipid obtained in the step (4), sieving the powder with a 18-mesh sieve, and performing vacuum drying in a double-cone rotary vacuum dryer at 60 ℃ for 30min to obtain powder phospholipid, wherein the water content of the powder phospholipid is 1.18g/100g, the content of the dry acetone insoluble substances is 95.42g/100g, the sensory index of the powder phospholipid is yellow powder, and the product meets the national standard GB28401 food additive phospholipid.

Example 5

(1) hydration: adding soybean oil residue into water, and stirring to break the oil residue into granules in water to form a soaking system with soybean oil residue granules as disperse phase and water as continuous phase, wherein the soaking temperature is 95 deg.C, and the soaking time is 1 hr to obtain saturated water-absorbing oil residue. The saturated water-absorbing oil foot is marked by the initial appearance of brown self-aggregating aqueous phospholipids.

The oil residue is from the grain and oil limited company of Zhongbao Zhenjiang, and the material composition is as follows: the water content was 37.69g/100g, the content of acetone insolubles on a dry basis was 63.45g/100 g; the water is purified drinking water, food additives of citric acid and common salt and sodium chloride are added into the water, the addition amount of the citric acid is 0.028 percent of the weight of the purified drinking water, and the addition amount of the common salt is 0.052 percent of the weight of the purified drinking water; the mass ratio of oil residue to water is 1: 3; the grain diameter of the oil residue particles is 0.3-3 mm.

And (3) saturating the water-absorbing oil residue, and keeping the soaking temperature for natural settling for 6 hours to obtain the self-aggregation water-containing phospholipid and the oil residue.

The resulting self-aggregating aqueous phospholipid had a water content of 72.33g/100g, a dry acetone insoluble content of 93.65g/100g, and a sensory index of brown translucent fluid.

(2) Concentration: reducing the water content of the water-containing phospholipid obtained in the step (1) to 35g/100g in a vacuum thin film evaporator at 110 ℃ to obtain a concentrated water-containing phospholipid, wherein the dry acetone insoluble content and sensory index of the concentrated water-containing phospholipid are the same as those of the self-aggregation water-containing phospholipid;

(3) stirring: pushing the concentrated aqueous phospholipid obtained in the step (2) into a stirrer at a speed of 25cm/min, wherein the rotation speed is 1200rpm, and the time is 25s, so as to obtain a continuously output aqueous phospholipid elastomer, wherein the water content and the acetone insoluble content of the aqueous phospholipid elastomer are the same as those of the concentrated aqueous phospholipid, but the sensory index of the aqueous phospholipid elastomer is changed into yellow opaque semisolid;

(4) and (3) continuous drying: feeding the water-containing phospholipid elastomer continuously output in the step (3) into a vacuum continuous dryer through a feed inlet with the aperture of 5mm, and drying at 120 ℃ for 20min to obtain continuously output solid phospholipid, wherein the water content of the solid phospholipid is 3.03g/100g, the content of dry acetone insoluble substances is 93.65g/100g, and sensory indexes of the solid phospholipid are yellow strip-shaped solids;

(5) crushing, sieving and drying: and (3) crushing the strip-shaped solid phospholipid obtained in the step (4), sieving the powder with a 18-mesh sieve, and performing vacuum drying in a double-cone rotary vacuum dryer at 60 ℃ for 30min to obtain powder phospholipid, wherein the water content of the powder phospholipid is 0.58g/100g, the content of the dry acetone insoluble substances is 93.65g/100g, the sensory index of the powder phospholipid is yellow powder, and the product meets the national standard GB28401 food additive phospholipid.

Example 6

(1) hydration: adding soybean oil foot into water, and stirring to break the oil foot into granules in water to form a soaking system with soybean oil foot granules as disperse phase and water as continuous phase, wherein the soaking temperature is 95 ℃, and the soaking time is 1h to obtain saturated water absorption oil foot. The saturated water-absorbing oil foot is marked by the initial appearance of brown self-aggregating aqueous phospholipids.

The oil foot is from China spinning grain oil (Dongguan) Co., Ltd, and the material composition of the oil foot is as follows: the water content was 40.23g/100g, the content of acetone insolubles on a dry basis was 62.39g/100 g; the water is purified drinking water, and a food additive citric acid is added into the water, wherein the addition amount of the citric acid is 0.038 percent of the weight of the purified drinking water; the mass ratio of oil residue to water is 1: 3.5; the grain diameter of the oil residue particles is 0.3-3 mm.

And (3) saturating the water-absorbing oil residue, and keeping the soaking temperature for natural sedimentation for 7 hours to obtain the self-aggregation water-containing phospholipid and the oil residue.

The resulting self-aggregating aqueous phospholipid had a water content of 73.01g/100g, a dry acetone insoluble content of 94.18g/100g, and a sensory index of brown translucent fluid.

(2) Concentration: reducing the water content of the water-containing phospholipid obtained in the step (1) to 25g/100g in a vacuum thin film evaporator at 110 ℃ to obtain a concentrated water-containing phospholipid, wherein the dry acetone insoluble content and sensory index of the concentrated water-containing phospholipid are the same as those of the self-aggregation water-containing phospholipid;

(3) stirring: pushing the concentrated aqueous phospholipid obtained in the step (2) into a stirrer at a speed of 10cm/min, wherein the rotation speed is 1200rpm, and the time is 30s, so as to obtain a continuously output aqueous phospholipid elastomer, wherein the water content and the acetone insoluble content of the aqueous phospholipid elastomer are the same as those of the concentrated aqueous phospholipid, but the sensory index of the aqueous phospholipid elastomer is changed into yellow opaque semisolid;

(4) and (3) continuous drying: feeding the continuously output water-containing phospholipid elastomer obtained in the step (3) into a vacuum continuous dryer through a feed inlet with the aperture of 6mm, and drying at 120 ℃ for 6min to obtain continuously output solid phospholipid, wherein the water content of the solid phospholipid is 4.61g/100g, the content of dry acetone insoluble substances is 94.18g/100g, and the sensory index of the solid phospholipid is yellow strip-shaped solid;

(5) crushing, sieving and drying: and (3) crushing the strip-shaped solid phospholipid obtained in the step (4), sieving the powder with a 18-mesh sieve, and performing vacuum drying in a double-cone rotary vacuum dryer at 60 ℃ for 30min to obtain powder phospholipid, wherein the water content of the powder phospholipid is 0.98g/100g, the content of the dry acetone insoluble substances is 94.18g/100g, the sensory index of the powder phospholipid is yellow powder, and the product meets the national standard GB28401 food additive phospholipid.

Comparative example 1

A method for preparing liquid crystal state phospholipid from soybean oil foot is derived from the research on liquid crystal state separation and purification of soybean phospholipid in the literature, and comprises the following steps:

adding 0.67 times of drinking purified water to soybean oil residue, mixing, heating to 70 deg.C, standing for 4 hr, and centrifuging at 70 deg.C and 4500r/min for 5min to obtain liquid crystal phospholipid. The soybean oil foot was produced by Zhongwan grain oil (Dongguan) Co., Ltd., and had a water content of 40.23g/100g and a dry acetone insoluble content of 62.39g/100 g.

The obtained liquid crystalline phospholipid had a water content of 63.89g/100g, a dry acetone insoluble content of 86.23g/100g, and a sensory index of brown translucent fluid.

Liquid crystal state phospholipid is distributed on a drying tray through a group of circular feed inlets with the aperture of 2mm, and is dried for 240min at 65 ℃ in an intermittent vacuum drying oven to obtain brown massive solid phospholipid, the water content of which is 6.38g/100g, and the content of dry acetone insoluble substances is 86.23g/100 g; and (3) crushing the brown solid phospholipid, sieving the crushed brown solid phospholipid by a 18-mesh sieve, and drying the powder phospholipid in a vacuum drying oven at 60 ℃ for 30min to obtain powder phospholipid, wherein the water content of the powder phospholipid is 1.24g/100g, the content of dry acetone insoluble substances is 86.23%, and the sensory index of the powder phospholipid is brown powder.

Compared with the liquid crystal phospholipid prepared in the comparative example 1, the liquid crystal phospholipid mainly has the following differences:

first, difference in solid phospholipids: the solid phospholipid prepared from liquid crystal state phospholipid is brown, the dry acetone insoluble substance is 86.23%, and the drying time is 240 min; the solid phospholipid prepared by the invention is yellow, the content of the dry acetone insoluble substance is 92.5-95.5g/100g, and the drying time is 6-20 min. Therefore, the drying efficiency of the liquid crystal phospholipid is very low, the color is also deep, and the industrialization feasibility is not realized.

Second, differences in the composition of the powdered phospholipid material: the powder phospholipid prepared from the liquid crystal state phospholipid is brown, and the content of the dry acetone insoluble substance is 86.23g/100 g; the powder phospholipid prepared by the invention is yellow, and the content of dry acetone insoluble substances is 92.5-95.5g/100 g. It can be seen that the liquid crystalline phospholipids have a low acetone insoluble content and are not industrially feasible from the viewpoint of phospholipid content.

Comparative example 2

A method for preparing powdered soybean phospholipid is disclosed in patent CN103665029A, and comprises the following steps:

mixing soybean oil residue and anhydrous acetone in a weight ratio of 1:10, stirring and extracting for 20min under the conditions of normal pressure and room temperature, performing centrifugal separation for solid-liquid separation, wherein the centrifugal time is 1min, the centrifugal speed is 4000rpm, and collecting solid parts.

The soybean oil foot is from the Pongji (Nanjing) grain and oil Co., Ltd, and the material composition of the soybean oil foot is as follows: the water content was 39.78g/100g, and the dry acetone insoluble content was 62.05g/100 g.

Mixing the solid part obtained in the step with anhydrous acetone in a weight ratio of 1:10, stirring and extracting for 20min under the conditions of normal pressure and room temperature, then performing centrifugal separation for solid-liquid separation, wherein the centrifugal speed is 5000rpm, and collecting the solid part, wherein the centrifugal time is 1 min. Crushing the solid part, and drying at 60 deg.C under vacuum for 5 hr to obtain soybean powder phospholipid, wherein the content of insoluble acetone is 95.30g/100g, and the weight loss is 0.65g/100g, and the soybean powder phospholipid is brown powder.

Compared with the powder phospholipid prepared in the comparative example 2, the main differences comprise the following aspects:

first, difference in drying time: comparative example 2 is solvent process powdered phospholipid, drying time 300 min; the drying time for preparing the solid phospholipid is 6-20min, because the drying time from the solid phospholipid to the powder phospholipid is not a control factor of the process time, and therefore the drying time is not calculated in the process time. It can be seen that the drying efficiency of solvent method powder phospholipid is very low, and there is no feasibility of large-scale production, which is the main reason that solvent method powder phospholipid is produced in small batch and small scale at present.

Second, differences in the composition of the powdered phospholipid material: comparative example 2 the content of acetone insoluble matter in the dried base of powdered phospholipid obtained by the solvent method was 95.30g/100g, the powdered phospholipid was brown powder, the amount of acetone loss by drying was 0.65g/100g, the component reduced by drying was acetone, which is an organic solvent, and the powdered phospholipid had potential safety hazards in food; the powder phospholipid prepared by the invention belongs to hydration method powder phospholipid, the content of dry acetone insoluble substances is 92.5-95.5%, the powder is yellow powder, the drying decrement is less than or equal to 2g/100g, the component reduced by drying is water, and the food safety hidden trouble is avoided.

Test example 1

The aqueous phospholipid elastomers prepared in example 2 and example 4 were subjected to rheological characterization, and the results are shown in fig. 3 and fig. 4. The instruments and parameters used for detection are as follows: RS6000 rotational rheometer (HAAKE, Germany), the measuring rotor used a Z41Ti coaxial drum sensing system (drum and rotor diameters 43.40mm and 41.42mm, respectively) with a sample thickness of 3mm in the center of the sensing system.

As can be seen from FIGS. 3 and 4, the aqueous phospholipid elastomers provided in examples 2 and 4 have storage modulus G 'more than 5 times greater than loss modulus G' in the measured frequency range, and they are almost independent of frequency, indicating that elasticity is much greater than viscosity, showing stronger solid characteristics (elasticity), while liquid characteristics (viscosity) become weaker and belong to elastomers.

The above detailed description is specific to one possible embodiment of the present invention, and the embodiment is not intended to limit the scope of the present invention, and all equivalent implementations or modifications without departing from the scope of the present invention should be included in the technical scope of the present invention.

Claims

1. A method for preparing powdered phospholipid, which is characterized by comprising the following steps:

2. The method of claim 1, wherein the soybean oil foot is broken up into particles with a particle size of 5mm or less, preferably 0.3 to 3mm, in water by stirring before the soaking in step (1).

3. The method according to claim 1, wherein the mass ratio of the soybean oil foot to the water in the step (1) is 1:1-3.5, the soaking temperature is 60-95 ℃, and the soaking time is 1-3 hours.

4. The method according to claim 1, wherein the step (1) further comprises adding an electrolyte to the soybean oil residue or the water, wherein the electrolyte is added in an amount of 0.01 to 0.3% by mass based on the water.

5. The method of claim 4, wherein the electrolyte comprises at least one of an acid, a base, and a salt, and preferably wherein the electrolyte is at least one of DL-sodium malate, L-malic acid, DL-malic acid, glacial acetic acid, citric acid, potassium citrate, sodium citrate, monosodium citrate, sodium gluconate, lactic acid, potassium lactate, sodium lactate, potassium carbonate, sodium carbonate, potassium bicarbonate, sodium sulfate, potassium chloride, potassium hydroxide, sodium hydroxide, hydrochloric acid, phosphoric acid, and sodium chloride.

6. The method of claim 1, wherein the natural settling temperature of step (1) is 60-95 ℃ for 3-8 hours.

7. The method according to claim 1, wherein in step (1), the self-aggregating aqueous phospholipid has a water content of 70 to 80g/100 g; the content of acetone insoluble matter is 92.5-95.5g/100g on a dry basis.

8. The method of claim 1, wherein in step (2), the concentrated aqueous phospholipid has a water content of 25 to 65g/100 g.

9. The method as set forth in claim 1, wherein the stirring in step (3) is a continuous manner, and the concentrated aqueous phospholipid is continuously fed into the stirrer at a feeding speed of 10-100cm/min, a stirring speed of 800-1200rpm, and a stirring time of 5-30s, to obtain the aqueous phospholipid elastomer which is continuously output.

10. The method as claimed in claim 1, wherein the continuous drying in step (4) includes two modes of continuous drying under normal pressure and continuous drying under vacuum, the drying temperature is 120-.