CN110663773A - Method for separating natural whey protein from fresh milk and application - Google Patents
Method for separating natural whey protein from fresh milk and application Download PDFInfo
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- CN110663773A CN110663773A CN201910015705.3A CN201910015705A CN110663773A CN 110663773 A CN110663773 A CN 110663773A CN 201910015705 A CN201910015705 A CN 201910015705A CN 110663773 A CN110663773 A CN 110663773A
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- 108010046377 Whey Proteins Proteins 0.000 title claims abstract description 91
- 102000007544 Whey Proteins Human genes 0.000 title claims abstract description 91
- 235000021119 whey protein Nutrition 0.000 title claims abstract description 68
- 235000013336 milk Nutrition 0.000 title claims abstract description 34
- 239000008267 milk Substances 0.000 title claims abstract description 34
- 210000004080 milk Anatomy 0.000 title claims abstract description 34
- 238000000034 method Methods 0.000 title claims abstract description 33
- 239000012528 membrane Substances 0.000 claims abstract description 52
- 238000000108 ultra-filtration Methods 0.000 claims abstract description 39
- 238000001471 micro-filtration Methods 0.000 claims abstract description 32
- 235000020251 goat milk Nutrition 0.000 claims abstract description 27
- 239000005862 Whey Substances 0.000 claims abstract description 23
- 239000012466 permeate Substances 0.000 claims abstract description 13
- 238000011033 desalting Methods 0.000 claims abstract description 12
- 238000005238 degreasing Methods 0.000 claims abstract description 10
- 239000000843 powder Substances 0.000 claims abstract description 9
- 235000013350 formula milk Nutrition 0.000 claims abstract description 7
- 239000005018 casein Substances 0.000 claims abstract description 4
- BECPQYXYKAMYBN-UHFFFAOYSA-N casein, tech. Chemical group NCCCCC(C(O)=O)N=C(O)C(CC(O)=O)N=C(O)C(CCC(O)=N)N=C(O)C(CC(C)C)N=C(O)C(CCC(O)=O)N=C(O)C(CC(O)=O)N=C(O)C(CCC(O)=O)N=C(O)C(C(C)O)N=C(O)C(CCC(O)=N)N=C(O)C(CCC(O)=N)N=C(O)C(CCC(O)=N)N=C(O)C(CCC(O)=O)N=C(O)C(CCC(O)=O)N=C(O)C(COP(O)(O)=O)N=C(O)C(CCC(O)=N)N=C(O)C(N)CC1=CC=CC=C1 BECPQYXYKAMYBN-UHFFFAOYSA-N 0.000 claims abstract description 4
- 235000021240 caseins Nutrition 0.000 claims abstract description 4
- 239000012465 retentate Substances 0.000 claims abstract description 4
- 235000020247 cow milk Nutrition 0.000 claims abstract description 3
- 230000014759 maintenance of location Effects 0.000 claims abstract description 3
- 239000007788 liquid Substances 0.000 claims description 21
- 239000000463 material Substances 0.000 claims description 14
- 239000006071 cream Substances 0.000 claims description 7
- 238000000909 electrodialysis Methods 0.000 claims description 7
- 239000008367 deionised water Substances 0.000 claims description 6
- 229910021641 deionized water Inorganic materials 0.000 claims description 6
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 6
- 230000015572 biosynthetic process Effects 0.000 claims description 5
- 239000000919 ceramic Substances 0.000 claims description 5
- 239000012141 concentrate Substances 0.000 claims description 5
- 239000012065 filter cake Substances 0.000 claims description 5
- 150000003839 salts Chemical class 0.000 claims description 5
- 239000002033 PVDF binder Substances 0.000 claims description 3
- 229920002981 polyvinylidene fluoride Polymers 0.000 claims description 3
- 239000004743 Polypropylene Substances 0.000 claims description 2
- 229920002492 poly(sulfone) Polymers 0.000 claims description 2
- -1 polypropylene Polymers 0.000 claims description 2
- 229920001155 polypropylene Polymers 0.000 claims description 2
- 239000011148 porous material Substances 0.000 claims description 2
- 238000002360 preparation method Methods 0.000 claims 1
- 238000000926 separation method Methods 0.000 abstract description 10
- 238000004519 manufacturing process Methods 0.000 abstract description 4
- 235000013365 dairy product Nutrition 0.000 abstract description 2
- 235000013351 cheese Nutrition 0.000 description 10
- 238000005516 engineering process Methods 0.000 description 7
- 239000000243 solution Substances 0.000 description 7
- 235000020183 skimmed milk Nutrition 0.000 description 5
- 239000000126 substance Substances 0.000 description 5
- GUBGYTABKSRVRQ-QKKXKWKRSA-N Lactose Natural products OC[C@H]1O[C@@H](O[C@H]2[C@H](O)[C@@H](O)C(O)O[C@@H]2CO)[C@H](O)[C@@H](O)[C@H]1O GUBGYTABKSRVRQ-QKKXKWKRSA-N 0.000 description 4
- 238000002474 experimental method Methods 0.000 description 4
- 239000012530 fluid Substances 0.000 description 4
- 238000010438 heat treatment Methods 0.000 description 4
- 238000002955 isolation Methods 0.000 description 4
- 210000003734 kidney Anatomy 0.000 description 4
- 239000008101 lactose Substances 0.000 description 4
- 239000007858 starting material Substances 0.000 description 4
- 235000013343 vitamin Nutrition 0.000 description 4
- 229940088594 vitamin Drugs 0.000 description 4
- 229930003231 vitamin Natural products 0.000 description 4
- 239000011782 vitamin Substances 0.000 description 4
- 241000283707 Capra Species 0.000 description 3
- 238000001914 filtration Methods 0.000 description 3
- 229910052500 inorganic mineral Inorganic materials 0.000 description 3
- 235000021243 milk fat Nutrition 0.000 description 3
- 239000011707 mineral Substances 0.000 description 3
- 239000012460 protein solution Substances 0.000 description 3
- 239000002994 raw material Substances 0.000 description 3
- 239000000654 additive Substances 0.000 description 2
- 239000006227 byproduct Substances 0.000 description 2
- 238000010612 desalination reaction Methods 0.000 description 2
- 239000002699 waste material Substances 0.000 description 2
- 230000000996 additive effect Effects 0.000 description 1
- 238000010790 dilution Methods 0.000 description 1
- 239000012895 dilution Substances 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000005187 foaming Methods 0.000 description 1
- 235000013305 food Nutrition 0.000 description 1
- 229920002521 macromolecule Polymers 0.000 description 1
- 238000001728 nano-filtration Methods 0.000 description 1
- 235000015097 nutrients Nutrition 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 235000018102 proteins Nutrition 0.000 description 1
- 108090000623 proteins and genes Proteins 0.000 description 1
- 102000004169 proteins and genes Human genes 0.000 description 1
- 238000000746 purification Methods 0.000 description 1
- 238000007670 refining Methods 0.000 description 1
- 238000001223 reverse osmosis Methods 0.000 description 1
Classifications
-
- 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
-
- 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
- A23C7/00—Other dairy technology
- A23C7/04—Removing unwanted substances other than lactose or milk proteins from milk
-
- A—HUMAN NECESSITIES
- A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
- A23J—PROTEIN COMPOSITIONS FOR FOODSTUFFS; WORKING-UP PROTEINS FOR FOODSTUFFS; PHOSPHATIDE COMPOSITIONS FOR FOODSTUFFS
- A23J1/00—Obtaining protein compositions for foodstuffs; Bulk opening of eggs and separation of yolks from whites
- A23J1/20—Obtaining protein compositions for foodstuffs; Bulk opening of eggs and separation of yolks from whites from milk, e.g. casein; from whey
- A23J1/205—Obtaining protein compositions for foodstuffs; Bulk opening of eggs and separation of yolks from whites from milk, e.g. casein; from whey from whey, e.g. lactalbumine
Abstract
A method for separating natural whey protein from fresh milk and an application thereof belong to the technical field of dairy product production. Aiming at the problem that the prior separation method destroys the functional properties of whey in fresh milk, the invention provides a method for separating natural whey protein from fresh milk, which comprises the following steps: 1) degreasing: centrifugally degreasing fresh milk to obtain degreased fresh milk, wherein the fresh milk is cow milk or goat milk; 2) and (3) microfiltration: microfiltering the defatted fresh milk by using a microfiltration membrane, wherein the retentate is casein solution after microfiltration, and the permeate is whey; 3) and (3) ultrafiltration: performing ultrafiltration on whey by using an ultrafiltration membrane, wherein the retention solution after ultrafiltration is whey protein concentrated solution; 4) desalting: desalting the concentrated whey protein to obtain natural whey protein. The whey protein has no phase change in the separation process, retains the natural functional properties of whey protein, and can be used for the production of infant milk powder.
Description
Technical Field
The invention belongs to the technical field of dairy product production, and particularly relates to a method for separating natural whey protein from fresh milk and application thereof.
Background
Whey is a byproduct after cheese processing, nine tons of whey are discharged when one ton of cheese is produced, the residual whey after cheese processing is discharged to cause waste and pollute the environment, and in order to solve the problem, whey protein is separated from whey to prepare whey protein powder, so that the problems of waste and pollution caused by the traditional production of whey are solved, and high economic value is created. However, the whey protein nutrient in the whey protein powder prepared in the way is damaged to a certain extent, and the functional characteristics of the whey protein are changed due to the action of the whey protein and cheese starter, rennin or additive. Therefore, the goat milk whey protein is produced in an efficient and high-quality mode, and the method has great significance for producing the pure natural one hundred percent goat milk infant formula milk powder in the true sense.
The membrane technology is an emerging processing technology and is widely applied in the food industry. The membrane separation technology has the functions of separation, concentration, purification and refining. The membrane technology is a high-efficiency separation technology, and a filtering membrane with very fine micropores is used for treating liquid, and small particles and even dissolved substances in the liquid are intercepted and separated. According to the diameter of the pores of the filter membrane, there are generally 4 categories, namely microfiltration, ultrafiltration, nanofiltration and reverse osmosis. The filter uses pressure difference as driving force to filter, and the device is simple, easy to operate, and easy to control and maintain.
At present, whey protein in the domestic and foreign markets is mainly prepared by processing cheese by-product whey, and the whey protein prepared by the method reacts with cheese starter, rennin or additives, so that the functional characteristics of the whey, such as the gelling property, the foaming property, the film forming property and the like, are changed.
Disclosure of Invention
Aiming at the problem that the prior separation method destroys the functional properties of whey in fresh milk, the invention provides a method for separating natural whey protein from fresh milk, which comprises the following steps:
1) degreasing: centrifugally degreasing fresh milk to obtain degreased fresh milk, wherein the fresh milk is cow milk or goat milk;
2) and (3) microfiltration: microfiltering the defatted fresh milk by using a microfiltration membrane, wherein the retentate is casein solution after microfiltration, and the permeate is whey;
3) and (3) ultrafiltration: performing ultrafiltration on whey by using an ultrafiltration membrane, wherein the retention solution after ultrafiltration is whey protein concentrated solution;
4) desalting: desalting the whey protein concentrate to obtain natural whey protein.
Further defined, the degreasing in the step 1) is to heat fresh milk to 45-55 ℃, and centrifugally degrease to obtain degreased fresh milk and cream.
Further limiting, in the step 2), the aperture of the microfiltration membrane is 0.1-0.2 μm, and the microfiltration membrane is one of a ceramic membrane, a polyvinylidene fluoride membrane, a polysulfone membrane and a polypropylene membrane.
Further defined, the microfiltration conditions of step 2) are: the material film inlet pressure is 0.08-0.12MPa, the film outlet pressure is 0.06-0.10MPa, the flow is 50-55L/min, and the material liquid circulation temperature is 40-50 ℃.
Further limited, deionized water at 40-50 ℃ is added into the trapped fluid in real time during the microfiltration process in the step 2) for dilution, so as to reduce the formation of filter cakes.
Further limiting, the ultrafiltration membrane in the step 3) is an 8000-10000Da roll-type ultrafiltration membrane.
Further defined, the ultrafiltration conditions of step 3) are: the material film inlet pressure is 0.10-0.14MPa, the film outlet pressure is 0.08-0.10MPa, the flow is 20-30L/min, and the material liquid circulation temperature is 40-50 ℃.
Further limiting, the desalting in the step 4) is to carry out desalting by electrodialysis under the conditions of 220V constant voltage, 3-5A current and 26 +/-2 ℃ and stop when the salt content in the solution reaches 70000 mg/L.
The natural whey protein obtained by the method can be used for preparing infant milk powder.
Advantageous effects
1) The invention adopts the membrane technology to separate the whey protein in the skim milk, the whey protein prepared by the membrane technology does not react with rennin and cheese starter, the natural functional property of the whey protein is kept, and the whey protein prepared by the goat milk can be used as the main raw material of one hundred percent of pure goat milk infant milk powder.
2) The microfiltration and ultrafiltration separation processes of the prepared whey protein are all separation at 40-50 ℃, the separation conditions are mild, no phase change occurs in the separation process, and the protein is not denatured at high temperature; the prepared whey protein is subjected to electrodialysis desalination treatment to obtain desalted whey protein, and the desalted whey protein is used for producing infant formula milk powder and can reduce the pressure of the kidney of an infant.
Detailed Description
The method for separating the natural whey protein from the fresh milk comprises the following steps:
heating fresh milk to 45-55 deg.C, and separating cream with a cream separator; performing a microfiltration experiment on the skim milk, controlling the temperature of the skim milk in the raw material tank to be maintained at 40-50 ℃ by using a heat exchanger, and performing the microfiltration experiment on the skim milk to fully filter the whey protein in the trapped fluid, improve the filtration rate, dilute the skim milk by adding deionized water while filtering, wherein the microfiltration permeated fluid is whey and the casein is trapped in the trapped fluid; whey passes through the ultrafiltration membrane, whey protein is a macromolecular substance and is intercepted by the ultrafiltration membrane, and small molecular substances such as lactose, vitamins and the like permeate through the ultrafiltration membrane, so that the concentration of the whey protein can be realized by ultrafiltration; and performing electrodialysis desalination on the ultrafiltered whey protein to obtain the desalted whey protein, wherein the prepared desalted whey protein can be used for producing infant formula milk powder.
The following examples, which are intended to further illustrate the invention and are not intended to limit the invention, describe the process for the isolation of native whey protein from fresh milk using goat milk as the starting material.
The raw materials, instruments, equipment and the like described in the present invention can be obtained commercially without specific description.
Example 1. method for isolating native whey protein from goat milk.
1) Degreasing: heating goat milk to 45 deg.C, and centrifuging with a milk fat separator to obtain defatted goat milk and cream.
2) And (3) microfiltration: microfiltering defatted goat milk, wherein the microfiltration membrane is a 0.14 μm ceramic membrane, the material inlet pressure is 0.10MPa, the membrane outlet pressure is 0.08MPa, the flow rate is controlled at 53L/min, the feed liquid circulation temperature is controlled at 45 ℃ by a heat exchanger, the formation of a filter cake layer is reduced in the microfiltering process, the flow rate of the feed liquid is improved, deionized water with the temperature of 45 ℃ is added in real time, the microfiltered permeate liquid is goat milk whey, and the trapped liquid is goat cheese protein solution.
3) And (3) ultrafiltration: the microfiltration permeate passes through a 9000Da roll type ultrafiltration membrane, the flow rate of ultrafiltration equipment is controlled to be 25L/min, the material inlet pressure is 0.12MPa, the membrane outlet pressure is 0.09MPa, the feed liquid circulation temperature is 45 ℃, and the molecular mass of whey protein in whey is more than 10000Da, so that the whey protein in goat milk can be intercepted by ultrafiltration to obtain whey protein concentrate, and small molecular substances such as lactose, minerals, vitamins and the like exist in the permeate through the membrane.
4) Desalting: the infant kidney cannot bear high salinity, and desalted whey protein is obtained after the whey protein prepared by ultrafiltration is desalted by electrodialysis under the conditions that: the operation is carried out under the constant pressure operation condition of 220V, the current is 3A, the temperature in the whole experiment process is 26 ℃, and the salt content in the solution reaches 70000 mg/L. Thus obtaining the natural whey protein.
Example 2. method for isolation of native whey protein from goat milk.
1) Degreasing: heating goat milk to 50 deg.C, and centrifuging with a milk fat separator to obtain defatted goat milk and cream.
2) And (3) microfiltration: microfiltering defatted goat milk, wherein the microfiltration membrane is a 0.2 μm ceramic membrane, the material inlet pressure is 0.08MPa, the membrane outlet pressure is 0.06MPa, the flow rate is controlled at 50L/min, the feed liquid circulation temperature is controlled at 40 ℃ by a heat exchanger, the formation of a filter cake layer is reduced in the microfiltering process, the flow rate of the feed liquid is improved, deionized water with the temperature of 40 ℃ is added in real time, the microfiltered permeate liquid is goat milk whey, and the trapped liquid is goat cheese protein solution.
3) And (3) ultrafiltration: the microfiltration permeate passes through a 10000Da roll type ultrafiltration membrane, the flow of ultrafiltration equipment is controlled by 20L/min, the material inlet pressure is 0.10MPa, the membrane outlet pressure is 0.08MPa, the feed liquid circulation temperature is 40 ℃, and the molecular mass of whey protein in whey is more than 10000Da, so that the whey protein in goat milk can be intercepted by ultrafiltration to obtain whey protein concentrate, and small molecular substances such as lactose, minerals, vitamins and the like exist in the permeate through the membrane.
4) Desalting: the infant kidney cannot bear high salinity, and desalted whey protein is obtained after the whey protein prepared by ultrafiltration is desalted by electrodialysis under the conditions that: the operation is carried out under the constant pressure operation condition of 220V, the current is 4A, the temperature in the whole experimental process is 27 ℃, and the salt content in the solution reaches 70000 mg/L. Thus obtaining the natural whey protein. .
Example 3. method for isolation of native whey protein from goat milk.
1) Degreasing: heating goat milk to 55 deg.C, and centrifuging with a milk fat separator to obtain defatted goat milk and cream.
2) And (3) microfiltration: microfiltering defatted goat milk, wherein the microfiltration membrane is a 0.1 μm ceramic membrane, the material inlet pressure is 0.12MPa, the membrane outlet pressure is 0.10MPa, the flow rate is controlled at 55L/min, the feed liquid circulation temperature is controlled at 50 ℃ by a heat exchanger, the formation of a filter cake layer is reduced in the microfiltering process, the flow rate of the feed liquid is improved, deionized water with the temperature of 50 ℃ is added in real time, the microfiltered permeate liquid is goat milk whey, and the trapped liquid is goat cheese protein solution.
3) And (3) ultrafiltration: the microfiltration permeate passes through an 8000Da roll type ultrafiltration membrane, the flow of ultrafiltration equipment is controlled by 30L/min, the material inlet pressure is 0.14MPa, the membrane outlet pressure is 0.10MPa, the feed liquid circulation temperature is 50 ℃, and the molecular mass of whey protein in whey is more than 10000Da, so that the whey protein in goat milk can be intercepted by ultrafiltration to obtain whey protein concentrate, and small molecular substances such as lactose, minerals, vitamins and the like exist in the permeate through the membrane.
4) Desalting: the infant kidney cannot bear high salinity, and desalted whey protein is obtained after the whey protein prepared by ultrafiltration is desalted by electrodialysis under the conditions that: the operation is carried out under the constant pressure operation condition of 220V, the current is 5A, the temperature in the whole experiment process is 28 ℃, and the salt content in the solution reaches 70000 mg/L. Thus obtaining the natural whey protein.
Example 4. method for isolating native whey protein from milk.
Example 1 was repeated, differing from example 1 in that the fresh milk in this example was milk.
Example 5. method for isolation of native whey protein from goat milk.
Example 1 was repeated, which is different from example 1 in that the microfiltration membrane in step 2) in this example was a polyvinylidene fluoride membrane.
Claims (9)
1. A method for separating natural whey protein from fresh milk is characterized by comprising the following steps:
1) degreasing: centrifugally degreasing fresh milk to obtain degreased fresh milk, wherein the fresh milk is cow milk or goat milk;
2) and (3) microfiltration: microfiltering the defatted fresh milk by using a microfiltration membrane, wherein the retentate is casein solution after microfiltration, and the permeate is whey;
3) and (3) ultrafiltration: performing ultrafiltration on whey by using an ultrafiltration membrane, wherein the retention solution after ultrafiltration is whey protein concentrated solution;
4) desalting: desalting the whey protein concentrate to obtain natural whey protein.
2. The method as claimed in claim 1, wherein the step 1) of defatting is to heat fresh milk to 45-55 ℃, and centrifugally defatting is carried out to obtain defatted fresh milk and cream.
3. The method as claimed in claim 1, wherein the pore size of the microfiltration membrane in step 2) is 0.1-0.2 μm, and the microfiltration membrane is one of a ceramic membrane, a polyvinylidene fluoride membrane, a polysulfone membrane and a polypropylene membrane.
4. The method of claim 1, wherein the microfiltration conditions of step 2) are: the material film inlet pressure is 0.08-0.12MPa, the film outlet pressure is 0.06-0.10MPa, the flow is 50-55L/min, and the material liquid circulation temperature is 40-50 ℃.
5. The method of claim 1, wherein the microfiltration process of step 2) is diluted with deionized water at 40-50 ℃ added to the retentate in real time to reduce filter cake formation.
6. The method as claimed in claim 1, wherein the ultrafiltration membrane of step 3) is a 8000-10000Da roll-to-roll type ultrafiltration membrane.
7. The method according to claim 1, wherein the ultrafiltration conditions of step 3) are: the material film inlet pressure is 0.10-0.14MPa, the film outlet pressure is 0.08-0.10MPa, the flow is 20-30L/min, and the material liquid circulation temperature is 40-50 ℃.
8. The method as claimed in claim 1, wherein the desalting in step 4) is carried out by electrodialysis under the conditions of constant pressure of 220V, current of 3-5A and temperature of 26 +/-2 ℃, and the salt content in the solution is stopped reaching 70000 mg/L.
9. Use of native whey protein obtained by the process of any of claims 1-8 for the preparation of infant milk powder.
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| CN201910015705.3A CN110663773A (en) | 2019-01-08 | 2019-01-08 | Method for separating natural whey protein from fresh milk and application |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112825917A (en) * | 2020-12-30 | 2021-05-25 | 宜宾惠美纤维新材料股份有限公司 | Goat milk degreasing method suitable for goat milk protein fibers |
| CN115191486A (en) * | 2021-04-14 | 2022-10-18 | 内蒙古伊利实业集团股份有限公司 | Method for improving stability of liquid goat milk and prepared liquid goat milk |
| CN117481198A (en) * | 2024-01-02 | 2024-02-02 | 内蒙古蒙牛乳业（集团）股份有限公司 | Membrane separation recombination method for core nutritional ingredients of infant milk product and application of membrane separation recombination method |
| CN117481251A (en) * | 2024-01-02 | 2024-02-02 | 内蒙古蒙牛乳业（集团）股份有限公司 | Whey protein preparation method and whey protein beverage |
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