CN110810524B - Method for preparing milk powder and obtained milk powder - Google Patents
Method for preparing milk powder and obtained milk powder Download PDFInfo
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- CN110810524B CN110810524B CN201911202109.2A CN201911202109A CN110810524B CN 110810524 B CN110810524 B CN 110810524B CN 201911202109 A CN201911202109 A CN 201911202109A CN 110810524 B CN110810524 B CN 110810524B
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- A—HUMAN NECESSITIES
- A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
- A23C—DAIRY PRODUCTS, e.g. MILK, BUTTER OR CHEESE; MILK OR CHEESE SUBSTITUTES; MAKING THEREOF
- A23C9/00—Milk preparations; Milk powder or milk powder preparations
- A23C9/16—Agglomerating or granulating milk powder; Making instant milk powder; Products obtained thereby
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- A—HUMAN NECESSITIES
- A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
- A23C—DAIRY PRODUCTS, e.g. MILK, BUTTER OR CHEESE; MILK OR CHEESE SUBSTITUTES; MAKING THEREOF
- A23C9/00—Milk preparations; Milk powder or milk powder preparations
- A23C9/152—Milk preparations; Milk powder or milk powder preparations containing additives
Abstract
The invention belongs to the field of dairy products, and particularly relates to a method for preparing milk powder, which comprises the following steps: (1) carrying out low-temperature spray granulation on the raw materials to obtain solid particles; the raw materials comprise a raw material for providing milk protein, a raw material for optionally providing fat, a raw material for optionally providing carbohydrate, an optional food additive and optional water, the diameter of a spray nozzle for low-temperature spray granulation is 0.1-1.5 mm, the spray pressure for low-temperature spray granulation is 180-400 bar, and the spray angle for low-temperature spray granulation is 60-100 ℃; (2) and (4) carrying out vacuum freeze drying on the solid particles to obtain the milk powder. The invention also relates to the prepared milk powder. The method has the advantages of high freeze-drying efficiency, good solubility of the prepared milk powder, long shelf life and good taste.
Description
Technical Field
The invention belongs to the field of dairy products, and particularly relates to a method for preparing milk powder and the obtained milk powder.
Background
It is well known that breast milk is the best natural food for infants, containing almost all the nutritional ingredients required by infants. However, women in the modern society face pressure in various aspects of work and life, problems of insufficient lactation, flawless lactation and the like often occur after delivery, and the infant formula milk powder becomes a breast milk substitute in many times.
Infant formulas are of a wide variety and function, and have been subjected to two stages until now: the first stage is nutrition fortification, mainly fortification of vitamins and minerals in infant formula; the second stage is component simulation, which mainly adjusts the types and proportions of fat, protein and the like in the infant formula milk powder to make the infant formula milk powder close to breast milk. But these two phases are limited to nutrients closer to breast milk.
With the progress of modern science, a great deal of epidemiological studies show that breast feeding can effectively reduce the possibility of infection diseases and death caused by the infection diseases within 6 months of newborns, which indicates that breast feeding can protect newborns from infection caused by immune insufficiency, wherein the active substances of immunoglobulin and lactoferrin in breast milk play a role. However, in the conventional process for preparing the infant formula milk powder, the infant formula milk powder needs to be heated and dried, and the active substances such as immunoglobulin, lactoferrin, heat-sensitive vitamins, probiotics, prebiotics and the like are easily inactivated or lost through thermal processing. Therefore, the development of infant formulas faces the problem of how to keep the bioactive substances closer to breast milk.
The vacuum freeze-drying technology (freeze-drying for short) is a technology that a water-containing material is frozen at a low temperature (the temperature is lower than the eutectic point of the material), so that water in the material is changed into solid ice, then the ice is directly sublimated into water vapor under a proper vacuum degree, and the water vapor is collected and condensed by a water vapor condenser (water catcher) in a vacuum system, so that a high-quality dry product is obtained at a low temperature and a low pressure. The technology does not need thermal processing, and can retain the biological activity of the substance. Among them, regarding the low-temperature freezing of water-containing materials, some domestic and foreign documents introduce a technique of obtaining frozen solid particles by spraying water-containing materials into a low-temperature (lower than the eutectic point temperature of the materials) medium, i.e., a low-temperature spray granulation technique; compared with the traditional method of directly freezing the water-containing material in a whole block, the low-temperature spray granulation technology improves the efficiency of vacuum freeze drying to a certain extent. Some researchers try to prepare the milk powder by adopting a low-temperature spray granulation-vacuum freeze drying method, however, raw materials (especially main raw material milk liquid) for preparing the milk powder are different from common materials, the components are complex, the sugar content is high, the fat content is high, moisture contained in solid particles obtained by low-temperature spray granulation of the raw materials cannot be effectively sublimated, the freeze drying efficiency is low, the prepared milk powder is poor in solubility, and the shelf life or quality guarantee period is short, so that the product quality is seriously influenced.
At present, the method for preparing the milk powder by utilizing the vacuum freeze-drying technology has the advantages of high freeze-drying efficiency, good solubility of the prepared milk powder and long shelf life.
Disclosure of Invention
The invention provides a method for preparing milk powder, which adopts a vacuum freeze-drying technology to prepare the milk powder, and has high freeze-drying efficiency, good dissolubility, long shelf life and good taste. The invention also provides milk powder.
The invention relates in a first aspect to a method for preparing milk powder comprising the steps of:
(1) carrying out low-temperature spray granulation on the raw materials to obtain solid particles; the raw materials comprise a raw material for providing milk protein, a raw material for optionally providing fat, a raw material for optionally providing carbohydrate, an optional food additive and optional water, the diameter of a spray nozzle for low-temperature spray granulation is 0.1-1.5 mm, the spray pressure for low-temperature spray granulation is 180-400 bar, and the spray angle for low-temperature spray granulation is 60-100 ℃;
(2) and (4) carrying out vacuum freeze drying on the solid particles to obtain the milk powder.
In some embodiments of the first aspect of the present invention, the diameter of the spray opening for low temperature spray granulation is 0.2mm, 0.4mm, 0.5mm, 0.7mm, 0.9mm, 1.0mm, 1.2mm, 1.4 mm.
In some embodiments of the first aspect of the present invention, the spray pressure for cryogenic spray granulation is 200bar, 220bar, 240bar, 250bar, 270bar, 280bar, 300bar, 310bar, 330bar, 350bar, 360bar, 380bar, 390 bar.
In some embodiments of the first aspect of the present invention, the spray angle for cryogenic spray granulation is 65 degrees, 70 degrees, 75 degrees, 80 degrees, 85 degrees, 90 degrees, 95 degrees, 98 degrees.
In some embodiments of the first aspect of the present invention, the spray opening is of a flared configuration, and the spray angle refers to its flare angle.
In certain embodiments of the first aspect of the present invention, in step (1), the cryogenic spray granulation uses liquid nitrogen as the cryogenic medium.
In some embodiments of the first aspect of the present invention, in step (2), the vacuum freeze-drying process comprises the following seven stages in sequence:
the method comprises the following steps: heat-retaining at-60 ℃ to-45 ℃ (e.g., -58 ℃, -55 ℃, -53 ℃, -50 ℃, -48 ℃, -47 ℃, -46 ℃) for 50 to 130 minutes (e.g., 55 minutes, 60 minutes, 65 minutes, 70 minutes, 75 minutes, 80 minutes, 85 minutes, 90 minutes, 95 minutes, 100 minutes, 110 minutes, 120 minutes, 125 minutes);
stage two: heating to-44 deg.C to-36 deg.C (e.g. -42 deg.C, -40 deg.C, -38 deg.C, -37 deg.C) at a rate of 1-10 deg.C/min (e.g. 1.5 deg.C/min, 2 deg.C/min, 2.5 deg.C/min, 2.8 deg.C/min, 3 deg.C/min, 4 deg.C/min, 5 deg.C/min, 6 deg.C/min, 8 deg.C/min, 9 deg.C/min), and holding at the temperature for 1000-1500 minutes (e.g. 1050 minutes, 110015 minutes, 1150 minutes, 1200 minutes, 1250 minutes, 1300 minutes, 1350 minutes, 1400 minutes, 1450 minutes);
stage III: heating to-35 ℃ to-10 ℃ (e.g., -33 ℃, -31 ℃, -30 ℃, -28 ℃, -25 ℃, -22 ℃, -20 ℃, -18 ℃, -16 ℃, -14 ℃, -12) at a rate of 1-11 ℃/min (e.g., 1.2 ℃/min, 2 ℃/min, 3 ℃/min, 4 ℃/min, 5 ℃/min, 6 ℃/min, 7 ℃/min, 8 ℃/min, 9 ℃/min, 10 ℃/min), and holding at that temperature for 1000-1600 minutes (e.g., 1050 minutes, 1100 minutes, 1150 minutes, 1200 minutes, 1250 minutes, 1300 minutes, 1350 minutes, 1400 minutes, 1450 minutes, 1500 minutes, 1550 minutes);
stage IV: heating to-9-5 ℃ (e.g., -7 ℃, -5 ℃, -3 ℃, -1 ℃, 3 ℃, and 4 ℃) at a rate of 1-12 ℃/min (e.g., 2 ℃/min, 2.4 ℃/min, 2.6 ℃/min, 2.8 ℃/min, 3 ℃/min, 4 ℃/min, 5 ℃/min, 6 ℃/min, 7 ℃/min, 8 ℃/min, 9 ℃/min, 10 ℃/min, and 11 ℃/min), holding at that temperature for 900-1600 minutes (e.g., 1000 minutes, 1050 minutes, 1100 minutes, 1150 minutes, 1200 minutes, 1250 minutes, 1300 minutes, 1350 minutes, 1400 minutes, and 1500 minutes);
stage five: heating to 6-15 deg.C (e.g. 8 deg.C, 10 deg.C, 12 deg.C, 13 deg.C, 14 deg.C) at a rate of 1-10 deg.C/min (e.g. 1.5 deg.C/min, 2 deg.C/min 3 deg.C/min, 4 deg.C/min, 5 deg.C/min, 6 deg.C/min, 7 deg.C/min, 8 deg.C/min, 9 deg.C/min), and holding at the temperature for 80-160 minutes (e.g. 90 minutes, 100 minutes, 110 minutes, 120 minutes, 130 minutes, 140 minutes, 150 minutes, 155 minutes);
stage (II): heating to 16-22 deg.C (e.g. 18 deg.C, 19 deg.C, 20 deg.C, 21 deg.C) at a rate of 1-11 deg.C/min (e.g. 1.5 deg.C/min, 2 deg.C/min, 3 deg.C/min, 4 deg.C/min, 5 deg.C/min, 6 deg.C/min, 7 deg.C/min, 8 deg.C/min, 9 deg.C/min, 10 deg.C/min), and holding at the temperature for 100-150 min (e.g. 110 min, 120 min, 130 min, 140 min, 145 min);
stage (c): heating to 23-40 deg.C (e.g., 25 deg.C, 27 deg.C, 29 deg.C, 31 deg.C, 33 deg.C, 35 deg.C, 37 deg.C, 39 deg.C) at a rate of 1-12 deg.C/min (e.g., 1.2 deg.C/min, 2 deg.C/min, 3 deg.C/min, 4 deg.C/min, 5 deg.C/min, 6 deg.C/min, 7 deg.C/min, 8 deg.C/min, 9 deg.C/min, 10 deg.C/min, 11 deg.C/min), and holding at the temperature for 20-100 minutes (e.g., 30 minutes, 40 minutes, 50 minutes, 60 minutes, 70 minutes, 80 minutes, 90 minutes, 95 minutes).
In some embodiments of the first aspect of the present invention, in step (2), the vacuum freeze-drying procedure comprises one or more of the following (a) to (T):
(A) in the first stage, heat preservation is carried out at the temperature of minus 55 ℃ to minus 47 ℃;
(B) in the first stage, preserving heat for 60-120 minutes;
(C) in the second step, the temperature is increased at the speed of 1-9 ℃/min;
(D) in the second step, the temperature is raised to-43 ℃ to-38 ℃;
(E) in the second step, the temperature is kept for 1000-1400 minutes;
(F) in the third stage, the temperature is increased at the speed of 1-10 ℃/min;
(G) in the third stage, the temperature is raised to-30 to-15 ℃;
(H) in the third stage, the temperature is kept for 1000-1500 minutes;
(I) in the stage IV, the temperature is increased at the speed of 1-10 ℃/min;
(J) in the stage IV, the temperature is raised to-5-4 ℃;
(K) in the fourth step, the temperature is kept for 1000-1500 minutes;
in the (L) stage, the temperature is raised at the speed of 1-9 ℃/min;
in the (M) stage, the temperature is raised to 7-13 ℃;
in the (N) stage, keeping the temperature for 90-150 minutes;
in the step (O), the temperature is raised at the speed of 1-10 ℃/min;
in the stage (P), the temperature is raised to 18 to 22 ℃;
(Q) in the stage sixthly, keeping the temperature for 100-140 minutes;
(R) in the stage (c), heating at a rate of 1-11 ℃/min;
in the stage (S), the temperature is raised to 23-30 ℃;
and (T) keeping the temperature for 30-90 minutes.
In some embodiments of the first aspect of the present invention, before step (1), further comprising step (1'): mixing the raw material with at least one gas selected from carbon dioxide and air to obtain a mixed material, and using the mixed material in the step (1).
In some embodiments of the first aspect of the present invention, step (1') comprises one or more of the following a to d:
a. the mixing is carried out at 10 ℃ to 30 ℃, for example, 15 ℃, 20 ℃, 25 ℃, 28 ℃;
b. the mixing is carried out at 0.1 to 1MPa, for example, 0.2MPa, 0.4MPa, 0.5MPa, 0.7MPa, 0.8MPa, 0.9 MPa;
c. the volume of the gas is 1 to 10 times, for example, 2, 3, 4, 5, 6, 7, 8, 9 times of the volume of the raw material;
d. mixing through a gas-liquid mixing tank.
In certain embodiments of the first aspect of the present invention, in step (1'), the feedstock is mixed with carbon dioxide gas, or the feedstock is mixed with air to obtain a mixed material, which is used in step (1).
In certain embodiments of the first aspect of the present invention, in step (1'), the gas is pumped into the gas-liquid mixing tank by a high-pressure pump.
In one embodiment of the first aspect of the present invention, in the step (1'), carbon dioxide gas or air is injected into the raw material to obtain a mixed material; preferably, carbon dioxide gas or air is injected through the gas distributor.
In some embodiments of the first aspect of the present invention, the carbon dioxide gas is sterile carbon dioxide gas.
In some embodiments of the first aspect of the present invention, the air is sterile air.
In some embodiments of the first aspect of the present invention, in the step (2), the solid particles are stacked in a low temperature medium to form a layer having a thickness of 0.1 to 2cm (e.g., 0.2cm, 0.4cm, 0.5cm, 0.7cm, 0.8cm, 1cm, 1.2cm, 1.5cm, 1.7cm, 2cm, 2.1cm, 2.3cm), and vacuum freeze-dried.
In certain embodiments of the first aspect of the present invention, in step (2), the cryogenic medium is liquid nitrogen.
In some embodiments of the first aspect of the present invention, in step (2), the solid particles are stacked in a stainless steel container to form a layer with a thickness of 0.1-2 cm, preferably a 304 stainless steel plate.
In some embodiments of the first aspect of the present invention, in the step (2), the vacuum freeze-drying is performed under a vacuum degree of 0.5 to 10Pa (e.g., 0.5Pa, 1Pa, 1.5Pa, 2Pa, 3Pa, 4Pa, 5Pa, 6Pa, 8 Pa).
In some embodiments of the first aspect of the present invention, the raw materials are those conventionally used in the art for the preparation of milk powder.
In some embodiments of the first aspect of the present invention, the raw materials comprise a milk protein providing raw material, a food additive and optionally water, wherein the food additive is a nutritional enhancer.
In some embodiments of the first aspect of the present invention, the raw material providing the milk protein is selected from the group consisting of fresh milk, purified milk, reconstituted milk, milk powder, whey protein powder and whey protein liquid, preferably purified milk.
In some embodiments of the first aspect of the present invention, the nutritional supplement is selected from the group consisting of minerals, vitamins, amino acids, and choline.
In some embodiments of the first aspect of the present invention, the fat-providing material is selected from vegetable fats and oils and animal fats and oils.
In some embodiments of the first aspect of the present invention, the carbohydrate-providing starting material is selected from the group consisting of glucose, fructose, lactose, galactose and starch.
According to the first aspect of the present inventionIn some embodiments, the milk protein is provided as a 3 × 10 starting material6～7×106Parts by weight, e.g. 4X 106Parts by weight, 5X 106Parts by weight, 6X 106And (4) parts by weight.
In some embodiments of the first aspect of the present invention, the nutrient supplement is 4000 to 8000 parts by weight, for example 4000 parts by weight, 5000 parts by weight, 6000 parts by weight, 7000 parts by weight.
In some embodiments of the first aspect of the present invention, the feedstock comprises:
in some embodiments of the first aspect of the present invention, the method further comprises, before all of the steps, step (1-1): and degassing the raw materials to obtain a degassed material.
In some embodiments of the first aspect of the present invention, between step (1-1) and step (1'), or between step (1-1) and step (1), the method further comprises step (1-2): and concentrating the degassed material to obtain a concentrated material.
In some embodiments of the first aspect of the present invention, between step (1-2) and step (1'), or between step (1-2) and step (1), the method further comprises step (1-3): and homogenizing the concentrated material to obtain a homogenized material.
In some embodiments of the first aspect of the present invention, between step (1-3) and step (1'), or between step (1-3) and step (1), the method further comprises step (1-4): and sterilizing the homogenized material to obtain a sterilized material.
In some embodiments of the first aspect of the present invention, the method comprises one or more of the following 1) to 9):
1) in the step (1-1), the temperature of the degassing treatment is 45 ℃ to 90 ℃, for example, 50 ℃, 55 ℃, 60 ℃, 65 ℃, 70 ℃, 75 ℃, 78 ℃, 80 ℃ and 85 ℃;
2) in the step (1-1), the pressure of the degassing treatment is-0.1 to-0.01 MPa, for example, -0.09MPa, -0.08MPa, -0.07MPa, -0.06MPa, -0.05MPa, -0.04MPa, -0.03MPa, or-0.02 MPa;
3) in step (1-2), the dry matter content in the concentrated material is 30-50% by weight, e.g. 34%, 36%, 38%, 40%, 42%, 43%, 45%, 47%, 49%;
4) in the step (1-2), concentration is performed by reduced pressure evaporation;
preferably, the reduced pressure evaporation is carried out at 40 ℃ to 75 ℃ (e.g., 45 ℃, 50 ℃, 55 ℃, 60 ℃, 65 ℃, 70 ℃, 75 ℃);
preferably, the evaporation is carried out under reduced pressure at 1 to 5kPa (e.g., 1.5kPa, 2kPa, 2.5kPa, 3kPa, 3.5kPa, 3.7kPa, 4kPa, 4.5kPa, 5 kPa);
5) in the step (1-3), the temperature of the homogenization treatment is 50 ℃ to 90 ℃, for example, 55 ℃, 60 ℃, 65 ℃, 70 ℃, 75 ℃, 80 ℃ and 85 ℃;
6) in the step (1-3), the primary pressure of the homogenization treatment is 10-25 MPa, such as 15MPa, 18MPa, 20MPa, 23 MPa;
7) in the step (1-3), the secondary pressure of the homogenization treatment is 1-9 MPaa, such as 2MPa, 3MPa, 4MPa, 5MPa, 6MPa, 7MPa, 8 MPa;
8) in the step (1-4), the sterilization temperature is 80 ℃ to 120 ℃, for example, 85 ℃, 90 ℃, 95 ℃, 100 ℃, 105 ℃, 110 ℃ and 115 ℃;
9) in the step (1-4), the sterilization time is 100-600 s, such as 200s, 300s, 400s, and 500 s.
In some embodiments of the first aspect of the present invention, the purified milk is prepared by: cleaning fresh milk at 20-40 deg.C, such as 25 deg.C, 28 deg.C, 30 deg.C, 35 deg.C, 38 deg.C;
preferably, the fresh milk is selected from fresh cow milk, fresh goat milk, fresh deer milk, fresh camel milk and fresh horse milk.
Preferably, the milk is purified by a centrifugal milk purifier;
more preferably, the centrifugal rotation speed is 5000-12000 rpm, such as 6000rpm, 7000rpm, 9000rpm, 11000 rpm;
more preferably, the feed rate is 80% to 95%, e.g. 85%, 90%, 92% of the nominal feed rate of the centrifugal milk cleaner.
In some embodiments of the first aspect of the invention, the milk protein in the feedstock is derived from at least one mammal selected from the group consisting of cattle, sheep, horses, donkeys, camels and deer.
In some embodiments of the first aspect of the present invention, the mineral is selected from the group consisting of calcium, magnesium, potassium, sodium, phosphorus, sulfur, iron, copper, iodine, zinc, manganese, molybdenum, selenium, and food-acceptable compounds thereof.
In some embodiments of the first aspect of the present invention, the vitamin is selected from vitamin A, vitamin B1Vitamin B2Vitamin B4Vitamin B5Vitamin B6Vitamin B9Vitamin B12Vitamin C, vitamin D, vitamin E, vitamin K, vitamin H, vitamin P, vitamin PP, vitamin M, vitamin T and vitamin U.
In some embodiments of the first aspect of the present invention, the amino acid is selected from the group consisting of taurine, leucine, isoleucine, lysine, methionine, phenylalanine, threonine, tryptophan, and histidine.
In some embodiments of the first aspect of the present invention, the food-acceptable calcium compound includes, but is not limited to, calcium carbonate, calcium gluconate, calcium citrate, calcium lactate, calcium L-lactate, calcium hydrogen phosphate, calcium L-threonate, calcium glycinate.
In some embodiments of the first aspect of the present invention, the food-acceptable iron compound includes, but is not limited to, ferrous sulfate, ferrous gluconate, ferric ammonium citrate, ferrous fumarate, ferric citrate, ferrous lactate, hemin, ferric pyrophosphate, ferriporphyrin, ferrous glycinate.
In some embodiments of the first aspect of the present invention, the food acceptable zinc compound includes, but is not limited to, zinc sulfate, zinc gluconate, zinc glycinate, zinc oxide, zinc lactate, zinc citrate, zinc chloride, zinc acetate.
In some embodiments of the first aspect of the present invention, the food-acceptable selenium compound includes, but is not limited to, sodium selenite, sodium selenate, selenoprotein, selenium-enriched edible mushroom powder, L-selenium-methylselenocysteine.
In some embodiments of the first aspect of the present invention, the food acceptable potassium compound includes, but is not limited to, potassium gluconate, potassium citrate, potassium dihydrogen phosphate, dipotassium hydrogen phosphate, potassium chloride.
The second aspect of the invention relates to milk powder prepared by the method of the first aspect of the invention.
The invention has the following beneficial effects:
1. the method has high freeze-drying efficiency.
2. The milk powder prepared by the method has good dissolubility.
3. The milk powder prepared by the method has low surface oil content, long shelf life and long shelf life.
4. The milk powder prepared by the method has good taste.
Detailed Description
Embodiments of the present invention will now be described more fully hereinafter with reference to the accompanying examples, in which some, but not all embodiments of the invention are shown. The following description of at least one exemplary embodiment is merely illustrative in nature and is in no way intended to limit the invention, its application, or uses. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
EXAMPLE 1 preparation of lyophilized milk powder 1
(1) Sterilizing and purifying fresh milk by a centrifugal milk purifier, wherein the purified milk temperature is 30-35 ℃, the feeding amount is reduced by 12 percent compared with the rated amount, and the centrifugal rotating speed is 8000 rpm to obtain milk liquid for storage and standby;
(2) mixing vitamin A15 g and vitamin B32 g129g of vitamin B2Adding 60g of vitamin C, 6000g of calcium lactate, 100g of ferrous sulfate, 40g of zinc gluconate, 12g of sodium selenite, 400g of choline and 75g of taurine into a vacuum mixing tank, mixing for 30-35 minutes under negative pressure of-0.4 bar to-0.75 bar, adding 5000kg of milk obtained in the step (1), and mixing for 30 minutes at 55-60 ℃ to obtain a mixed material;
(3) degassing the mixed material obtained in the step (2) through a degassing tank at the temperature of 60-70 ℃ and the pressure of-0.05 MPa to obtain a degassed material;
(4) cooling the degassed material obtained in the step (3) to 50-60 ℃, and then performing reduced pressure evaporation at 48-65 ℃ under the condition of 1.5-3 kPa to obtain a concentrated material with the dry matter weight percentage content of 40-42%;
(5) homogenizing the concentrated material obtained in the step (4), wherein the temperature of the homogenization treatment is 60-70 ℃, the primary pressure of the homogenization treatment is 17-18 MPa, and the secondary pressure of the homogenization treatment is 3-4 MPa, so as to obtain a homogenized material; preserving the temperature of the homogenized material at 95 +/-5 ℃ for 300s for sterilization to obtain a sterilized material;
(6) injecting the sterilized material obtained in the step (5) into a spray gun of a liquid nitrogen granulation system, wherein the diameter of a spray nozzle is 0.6mm, the spray pressure is 200bar, the spray angle is 90 degrees, the sprayed material is rapidly condensed into solid particles in liquid nitrogen, a freeze-drying tray made of 304 stainless steel is adopted to collect the solid particles, and the freeze-drying tray filled with the solid particles is placed into a front bin of a vacuum freeze-drying machine;
(7) and (3) paving solid particles in the freeze-drying plate into a laminar object with the thickness of 0.5-1 cm, and drying the solid particles in the plate through a vacuum freeze dryer to obtain the freeze-dried milk powder 1. The degree of vacuum was 1.33Pa, and the vacuum freeze-drying procedure was as shown in Table 1.
(8) And (3) carrying out aseptic nitrogen-filled packaging on the freeze-dried milk powder 1.
TABLE 1
EXAMPLE 2 preparation of lyophilized milk powder 2
(1) Sterilizing and purifying fresh milk by a centrifugal milk purifier, wherein the purified milk temperature is 30-35 ℃, the feeding amount is reduced by 12 percent compared with the rated amount, and the centrifugal rotating speed is 8000 rpm to obtain milk liquid for storage and standby;
(2) mixing vitamin A15 g and vitamin B32 g129g of vitamin B2Adding 60g of vitamin C, 6000g of calcium lactate, 100g of ferrous sulfate, 40g of zinc gluconate, 12g of sodium selenite, 400g of choline and 75g of taurine into a vacuum mixing tank, mixing for 30-35 minutes under negative pressure of-0.4 bar to-0.75 bar, adding 5000kg of milk obtained in the step (1), and mixing for 30 minutes at 55-60 ℃ to obtain a mixed material;
(3) degassing the mixed material obtained in the step (2) through a degassing tank at the temperature of 60-70 ℃ and the pressure of-0.05 MPa to obtain a degassed material;
(4) cooling the degassed material obtained in the step (3) to 50-60 ℃, and then performing reduced pressure evaporation at 48-65 ℃ under the condition of 1.5-3 kPa to obtain a concentrated material with the dry matter weight percentage content of 40-42%;
(5) homogenizing the concentrated material obtained in the step (4), wherein the temperature of the homogenization treatment is 60-70 ℃, the primary pressure of the homogenization treatment is 17-18 MPa, and the secondary pressure of the homogenization treatment is 3-4 MPa, so as to obtain a homogenized material; preserving the temperature of the homogenized material at 95 +/-5 ℃ for 300s for sterilization to obtain a sterilized material;
(6) injecting the sterilized material obtained in the step (5) into a spray gun of a liquid nitrogen granulation system, wherein the diameter of a spray nozzle is 0.6mm, the spray pressure is 200bar, the spray angle is 90 degrees, the sprayed material is rapidly condensed into solid particles in liquid nitrogen, a freeze-drying tray made of 304 stainless steel is adopted to collect the solid particles, and the freeze-drying tray filled with the solid particles is placed into a front bin of a vacuum freeze-drying machine;
(7) and (3) paving the solid particles in the freeze-drying plate into a laminar object with the thickness of 0.5-1 cm, and drying the solid particles in the plate by using a vacuum freeze dryer to obtain the freeze-dried milk powder 2. The degree of vacuum was 1.33Pa, and the vacuum freeze-drying procedure was as shown in Table 2.
(8) And (3) carrying out sterile nitrogen-filled packaging on the freeze-dried milk powder 2.
TABLE 2
EXAMPLE 3 preparation of lyophilized milk powder 3
(1) Sterilizing and purifying fresh milk by a centrifugal milk purifier, wherein the purified milk temperature is 30-35 ℃, the feeding amount is reduced by 12 percent compared with the rated amount, and the centrifugal rotating speed is 8000 rpm to obtain milk liquid for storage and standby;
(2) mixing vitamin A15 g and vitamin B32 g129g of vitamin B2Adding 60g of vitamin C, 6000g of calcium lactate, 100g of ferrous sulfate, 40g of zinc gluconate, 12g of sodium selenite, 400g of choline and 75g of taurine into a vacuum mixing tank, mixing for 30-35 minutes under negative pressure of-0.4 bar to-0.75 bar, adding 5000kg of milk obtained in the step (1), and mixing for 30 minutes at 55-60 ℃ to obtain a mixed material;
(3) degassing the mixed material obtained in the step (2) through a degassing tank at the temperature of 60-70 ℃ and the pressure of-0.05 MPa to obtain a degassed material;
(4) cooling the degassed material obtained in the step (3) to 50-60 ℃, and then performing reduced pressure evaporation at 48-65 ℃ under the condition of 1.5-3 kPa to obtain a concentrated material with the dry matter weight percentage content of 40-42%;
(5) homogenizing the concentrated material obtained in the step (4), wherein the temperature of the homogenization treatment is 60-70 ℃, the primary pressure of the homogenization treatment is 17-18 MPa, and the secondary pressure of the homogenization treatment is 3-4 MPa, so as to obtain a homogenized material; preserving the temperature of the homogenized material at 95 +/-5 ℃ for 300s for sterilization to obtain a sterilized material;
(6) cooling the sterilized material obtained in the step (5) to 15-19 ℃, injecting the sterilized material into an inflation liquid mixing tank, pumping compressed carbon dioxide into a gas-liquid mixing tank through a gas high-pressure pump, keeping the pressure in the gas-liquid mixing tank at 0.2MPa, and performing gas-liquid mixing at 20 ℃ by using a gas distributor in the tank, wherein the inflation volume of the carbon dioxide gas is 3 times that of the sterilized material, so as to obtain a material containing carbon dioxide gas;
(7) injecting a material containing carbon dioxide gas into a spray gun of a liquid nitrogen granulation system, wherein the diameter of a spray nozzle is 0.6mm, the spray pressure is 200bar, the spray angle is 90 degrees, the sprayed material is rapidly condensed into solid particles in liquid nitrogen, a freeze-drying tray made of 304 stainless steel is adopted to collect the solid particles, and the freeze-drying tray containing the solid particles is placed into a front bin of a vacuum freeze-drying machine;
(8) and (3) paving the solid particles in the freeze-drying plate into a laminar object with the thickness of 0.5-1 cm, and drying the solid particles in the plate by using a vacuum freeze dryer to obtain the freeze-dried milk powder 3. The vacuum degree was 1.33Pa, and the procedure of vacuum freeze-drying was as shown in Table 2.
(9) And (3) carrying out aseptic nitrogen-filled packaging on the freeze-dried milk powder 3.
EXAMPLE 4 preparation of lyophilized milk powder 4
(1) Sterilizing and purifying fresh milk by a centrifugal milk purifier, wherein the purified milk temperature is 30-35 ℃, the feeding amount is reduced by 12 percent compared with the rated amount, and the centrifugal rotating speed is 8000 rpm to obtain milk liquid for storage and standby;
(2) mixing vitamin A15 g and vitamin B32 g129g of vitamin B2Adding 60g of vitamin C, 6000g of calcium lactate, 100g of ferrous sulfate, 40g of zinc gluconate, 12g of sodium selenite, 400g of choline and 75g of taurine into a vacuum mixing tank, mixing for 30-35 minutes under negative pressure of-0.4 bar to-0.75 bar, adding 5000kg of milk obtained in the step (1), and mixing for 30 minutes at 55-60 ℃ to obtain a mixed material;
(3) degassing the mixed material obtained in the step (2) through a degassing tank at the temperature of 60-70 ℃ and the pressure of-0.05 MPa to obtain a degassed material;
(4) cooling the degassed material obtained in the step (3) to 50-60 ℃, and then performing reduced pressure evaporation at 48-65 ℃ under the condition of 1.5-3 kPa to obtain a concentrated material with the dry matter weight percentage content of 40-42%;
(5) homogenizing the concentrated material obtained in the step (4), wherein the temperature of the homogenization treatment is 60-70 ℃, the primary pressure of the homogenization treatment is 17-18 MPa, and the secondary pressure of the homogenization treatment is 3-4 MPa, so as to obtain a homogenized material; preserving the temperature of the homogenized material at 95 +/-5 ℃ for 300s for sterilization to obtain a sterilized material;
(6) cooling the sterilized material obtained in the step (5) to 15-19 ℃, injecting the sterilized material into an inflation liquid mixing tank, pumping compressed air into a gas-liquid mixing tank through a gas high-pressure pump, keeping the pressure in the gas-liquid mixing tank at 0.2MPa, and performing gas-liquid mixing at 20 ℃ by using a gas distributor in the tank, wherein the inflation volume is 3 times of that of the sterilized material, so as to obtain a material containing air;
(7) injecting the air-containing material obtained in the step (6) into a spray gun of a liquid nitrogen granulation system, wherein the diameter of a spray nozzle is 0.6mm, the spray pressure is 200bar, the spray angle is 90 degrees, the sprayed material is rapidly condensed into solid particles in liquid nitrogen, a freeze-drying tray made of 304 stainless steel is adopted to collect the solid particles, and the freeze-drying tray containing the solid particles is placed into a front bin of a vacuum freeze-drying machine;
(8) and (3) paving the solid particles in the freeze-drying plate into a laminar object with the thickness of 0.5-1 cm, and drying the solid particles in the plate by using a vacuum freeze dryer to obtain freeze-dried milk powder 4. The vacuum degree was 1.33Pa, and the procedure of vacuum freeze-drying was as shown in Table 2.
(9) And (4) carrying out aseptic nitrogen-filled packaging on the freeze-dried milk powder 4.
Comparative example 1
In the step (6), the diameter of the spray nozzle is 2mm, the spray pressure is 150bar, the spray angle is 20 degrees, and the rest is the same as that in the example 1, so that the freeze-dried milk powder A is obtained.
Comparative example 2
Replacing steps (6) to (7) with: directly injecting the sterilized material into a mold with a depth (thickness) of not more than 1.5cm, drying the material by a vacuum freeze dryer with a vacuum degree of 1.33Pa, wherein the vacuum freeze drying procedure is as shown in Table 2, and the rest is the same as that of example 2 to obtain lyophilized milk powder B.
Comparative example 3
Steps (1) to (5) are the same as in example 1;
cooling the sterilization material obtained in the step (5) to 60-70 ℃, carrying out high-pressure spraying through a spray head, fully contacting with clean hot air at 150-180 ℃, exchanging heat, and rapidly evaporating water in the emulsion to rapidly turn the emulsion into spherical powder, and continuously discharging the hot air and water vapor to enable the drying tower to be in a negative pressure environment; and carrying out secondary drying and cooling on the obtained powder by a fluidized bed, and screening by a vibrating screen to obtain the milk powder C with uniform granularity.
Test example 1 solubility test
And testing the water solubility of the freeze-dried milk powder 1-4, the freeze-dried milk powder A-B and the milk powder C.
The test method comprises the following steps: the daily consumer usage habits were simulated, using 10% concentration as the test concentration. Adding 10g of milk powder sample into a glass beaker filled with 90g of purified water, keeping the recommended milk powder dissolution temperature at 55 ℃ for dissolution, and beginning to dissolve by only simulating human hand shaking frequency with a shaker at 120 revolutions per minute.
Adding a milk powder sample into purified water, timing until all the blocks are dissipated, and recording as the time consumed for dissolving completely;
pouring all the dissolved liquid on a glass flat plate, and observing the number of visible particles with the particle size of more than 1 mm;
and thirdly, observing the wall hanging condition of the liquid after the dissolution is finished.
The results are shown in Table 3.
TABLE 3
As can be seen from Table 3, the solubility of the milk powder prepared by the method of the present invention is better than that of the freeze-dried milk powders A to B. The milk powder prepared by the method of the invention retains more bioactive substances than milk powder C. Moreover, the liquid nitrogen granulation treatment, the vacuum freeze-drying procedure and the gas-liquid mixing treatment adopted in the method of the present invention all contribute to the improvement of the solubility of the milk powder.
Test example 2 examination of Freeze drying efficiency
The water content of the freeze-dried milk powder 1-4 and the water content of the freeze-dried milk powder A-B are detected according to the method of the national standard GB5009.3-2016 'determination of water content in food safety national standard food', and the result is shown in Table 4. Wherein, the lower the water content of the sample, the higher the freeze-drying efficiency; conversely, the lower the lyophilization efficiency.
TABLE 4
| Sample (I) | Water content |
| Freeze-dried milk powder 1 | 2.3 |
| Freeze-dried milk powder 2 | 2.2 |
| Freeze-dried milk powder 3 | 1.9 |
| Freeze-dried milk powder 4 | 2.0 |
| Freeze-dried milk powder A | 4.5 |
| Freeze-dried milk powder B | 5.5 |
As can be seen from Table 4, the method of the present invention has higher lyophilization efficiency than the methods of comparative examples 1 to 2. In addition, the liquid nitrogen granulation treatment and the gas-liquid mixing treatment adopted by the method of the invention are beneficial to improving the freeze-drying efficiency.
Test example 3 surface oil content and shelf life investigation
GB5009.6 ' determination of fat in national food safety Standard ' Soxhlet extraction method ' is adopted to determine the surface oil content of freeze-dried milk powder 1-4 and freeze-dried milk powder A-B which are placed for 24 months at normal temperature, and the results are shown in Table 5. Wherein, the higher the surface oil content is, the more easily the product is oxidized and generates unpleasant odor in the shelf life, and the shorter the shelf life of the product is.
TABLE 5
| Sample (I) | Surface oil content |
| Freeze-dried milk powder 1 | 7.6 |
| Freeze-dried milk powder 2 | 7.9 |
| Freeze-dried milk powder 3 | 7.3 |
| Freeze-dried milk powder 4 | 7.5 |
| Freeze-dried milk powder A | 9.8 |
| Freeze-dried milk powder B | 10.2 |
As can be seen from Table 5, compared with the freeze-dried milk powders A to B, the freeze-dried milk powder prepared by the method has lower surface oil content and longer shelf life. This shows that the liquid nitrogen granulation, the vacuum freeze-drying procedure and the gas-liquid mixing treatment adopted in the method of the present invention contribute to the prolongation of the shelf life of the product.
Test example 4 taste evaluation
The taste of the freeze-dried milk powder 1-4, the taste of the freeze-dried milk powder A-B and the taste of the milk powder C are evaluated by 25 professionals, the full score of each index is 10, and the higher the score is, the higher the index evaluation is. The average score and the average total score of each index are shown in Table 6.
TABLE 6
As can be seen from Table 6, compared with the freeze-dried milk powders A to B and the milk powder C, the average total score of the taste evaluation of the freeze-dried milk powder prepared by the method is higher, and the taste fineness score of the freeze-dried milk powder is obviously higher than that of the freeze-dried milk powders A to B and the milk powder C.
It should be understood that the above examples are only for clarity of illustration and are not intended to limit the embodiments. Other variations and modifications will be apparent to persons skilled in the art in light of the above description. And are neither required nor exhaustive of all embodiments. And obvious variations or modifications therefrom are within the scope of the invention.
Claims (22)
1. A method of preparing milk powder comprising the steps of:
(1) carrying out low-temperature spray granulation on the raw materials to obtain solid particles; the raw materials comprise a raw material for providing milk protein, a raw material for providing fat, a raw material for providing carbohydrate, an optional food additive and optional water, the diameter of a spray nozzle for low-temperature spray granulation is 0.2-1.0 mm, the spray pressure for low-temperature spray granulation is 180-250 bar, and the spray angle for low-temperature spray granulation is 80-100 ℃;
(2) and (4) carrying out vacuum freeze drying on the solid particles to obtain the milk powder.
2. The method according to claim 1, wherein in step (1), the cryogenic spray granulation uses liquid nitrogen as a cryogenic medium.
3. The method as claimed in claim 1, wherein in step (2), the vacuum freeze-drying procedure comprises the following seven stages in sequence:
the method comprises the following steps: preserving the heat for 50-130 minutes at-60 ℃ to-45 ℃;
stage two: heating to-44-36 ℃ at the speed of 1-10 ℃/min, and keeping the temperature at-44-36 ℃ for 1000-1500 minutes;
stage III: heating to-35 to-10 ℃ at the speed of 1-11 ℃/min, and preserving the heat for 1000-1600 minutes at-35 to-10 ℃;
stage IV: heating to-9-5 ℃ at the speed of 1-12 ℃/min, and preserving the heat for 900-1600 minutes at-9-5 ℃;
stage five: heating to 6-15 ℃ at the speed of 1-10 ℃/min, and preserving the heat at 6-15 ℃ for 80-160 minutes;
stage (II): heating to 16-22 ℃ at the speed of 1-11 ℃/min, and preserving the heat at 16-22 ℃ for 100-150 minutes;
stage (c): heating to 23-40 ℃ at the speed of 1-12 ℃/min, and preserving the heat at 23-40 ℃ for 20-100 minutes.
4. The method of claim 3, wherein, in step (2), the vacuum freeze-drying procedure is characterized by one or more of the following (A) to (T):
(A) in the first stage, heat preservation is carried out at the temperature of minus 55 ℃ to minus 47 ℃;
(B) in the first stage, preserving heat for 60-120 minutes;
(C) in the second step, the temperature is increased at the speed of 1-9 ℃/min;
(D) in the second step, the temperature is raised to-43 ℃ to-38 ℃;
(E) in the second step, the temperature is kept for 1000-1400 minutes;
(F) in the third stage, the temperature is increased at the speed of 1-10 ℃/min;
(G) in the third stage, the temperature is raised to-30 to-15 ℃;
(H) in the third stage, the temperature is kept for 1000-1500 minutes;
(I) in the stage IV, the temperature is increased at the speed of 1-10 ℃/min;
(J) in the stage IV, the temperature is raised to-5-4 ℃;
(K) in the fourth step, the temperature is kept for 1000-1500 minutes;
in the (L) stage, the temperature is raised at the speed of 1-9 ℃/min;
in the (M) stage, the temperature is raised to 7-13 ℃;
in the (N) stage, keeping the temperature for 90-150 minutes;
in the step (O), the temperature is raised at the speed of 1-10 ℃/min;
in the stage (P), the temperature is raised to 18 to 22 ℃;
(Q) in the stage sixthly, keeping the temperature for 100-140 minutes;
(R) in the stage (c), heating at a rate of 1-11 ℃/min;
in the stage (S), the temperature is raised to 23-30 ℃;
and (T) keeping the temperature for 30-90 minutes.
5. The method of claim 3, wherein, prior to step (1), further comprising the step (1'): mixing the raw material with at least one gas selected from carbon dioxide and air to obtain a mixed material, and using the mixed material in the step (1).
6. The method according to claim 5, wherein step (1') is characterized by one or more of the following a to d:
a. the mixing is carried out at 10-30 ℃;
b. the mixing is carried out under 0.1-1 MPa;
c. the volume of the gas is 1-10 times of the volume of the raw material;
d. mixing through a gas-liquid mixing tank.
7. The method according to claim 1, wherein in the step (2), the solid particles are stacked in a low-temperature medium to form a layer with a thickness of 0.1-2 cm, and vacuum freeze-drying is carried out.
8. The method according to claim 7, wherein in step (2), the cryogenic medium is liquid nitrogen.
9. The method according to claim 7, wherein in the step (2), the solid particles are stacked in a stainless steel container to form a layer with a thickness of 0.1-2 cm.
10. The method according to claim 7, wherein in the step (2), the vacuum freeze-drying is performed under a vacuum degree of 0.5 to 10 Pa.
11. The method according to any one of claims 1 to 10, wherein the raw material providing the milk protein is selected from the group consisting of fresh milk, purified milk, reconstituted milk, milk powder, whey protein powder and whey protein liquid.
12. The method according to any one of claims 1 to 10, wherein the raw material providing the milk protein is purified milk.
13. The method according to any one of claims 1 to 10, wherein the raw material providing the milk protein is 3 x 106～7×106And (4) parts by weight.
14. The process of any one of claims 1 to 10, wherein the feedstock comprises:
15. the method of claim 5, wherein, prior to all steps, the method further comprises the step (1-1): and degassing the raw materials to obtain a degassed material.
16. The method of claim 15, wherein, between step (1-1) and step (1'), the method further comprises step (1-2): and concentrating the degassed material to obtain a concentrated material.
17. The method of claim 16, wherein, between step (1-2) and step (1'), the method further comprises step (1-3): and homogenizing the concentrated material to obtain a homogenized material.
18. The method of claim 17, wherein, between step (1-3) and step (1'), the method further comprises step (1-4): and sterilizing the homogenized material to obtain a sterilized material.
19. The method according to any one of claims 15 to 18, characterized by one or more of the following 1) to 9):
1) in the step (1-1), the temperature of the degassing treatment is 45-90 ℃;
2) in the step (1-1), the pressure of the degassing treatment is-0.1 to-0.01 MPa;
3) in the step (1-2), the weight content of dry matters in the concentrated material is 30-50%;
4) in the step (1-2), concentration is performed by reduced pressure evaporation;
5) in the step (1-3), the temperature of homogenization treatment is 50-90 ℃;
6) in the step (1-3), the primary pressure of the homogenization treatment is 10-25 MPa;
7) in the step (1-3), the secondary pressure of the homogenization treatment is 1-9 MPa;
8) in the step (1-4), the sterilization temperature is 80-120 ℃;
9) in the step (1-4), the sterilization time is 100-600 s.
20. The process according to claim 19, wherein in item 4), in step (1-2), the evaporation under reduced pressure is carried out at 40 ℃ to 75 ℃.
21. The method according to claim 19, wherein in item 4), the evaporation under reduced pressure is carried out at 1 to 5kPa in step (1-2).
22. A milk powder made by the method of any one of claims 1 to 21.
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