CN116926147A - Method and device for preparing lactose and galacto-oligosaccharide - Google Patents
Method and device for preparing lactose and galacto-oligosaccharide Download PDFInfo
- Publication number
- CN116926147A CN116926147A CN202310893092.XA CN202310893092A CN116926147A CN 116926147 A CN116926147 A CN 116926147A CN 202310893092 A CN202310893092 A CN 202310893092A CN 116926147 A CN116926147 A CN 116926147A
- Authority
- CN
- China
- Prior art keywords
- lactose
- treatment
- residual
- outlet
- enzyme
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
- 239000008101 lactose Substances 0.000 title claims abstract description 282
- 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 title claims abstract description 276
- 235000021255 galacto-oligosaccharides Nutrition 0.000 title claims abstract description 71
- 150000003271 galactooligosaccharides Chemical class 0.000 title claims abstract description 71
- 238000000034 method Methods 0.000 title claims abstract description 61
- GUBGYTABKSRVRQ-XLOQQCSPSA-N Alpha-Lactose Chemical compound O[C@@H]1[C@@H](O)[C@@H](O)[C@@H](CO)O[C@H]1O[C@@H]1[C@@H](CO)O[C@H](O)[C@H](O)[C@H]1O GUBGYTABKSRVRQ-XLOQQCSPSA-N 0.000 title claims abstract description 19
- 238000001914 filtration Methods 0.000 claims abstract description 90
- 108090000790 Enzymes Proteins 0.000 claims abstract description 75
- 102000004190 Enzymes Human genes 0.000 claims abstract description 75
- 239000000047 product Substances 0.000 claims abstract description 66
- 238000002425 crystallisation Methods 0.000 claims abstract description 63
- 230000008025 crystallization Effects 0.000 claims abstract description 63
- 238000000354 decomposition reaction Methods 0.000 claims abstract description 63
- 239000012452 mother liquor Substances 0.000 claims abstract description 63
- 238000010791 quenching Methods 0.000 claims abstract description 49
- 238000000926 separation method Methods 0.000 claims abstract description 47
- 239000007788 liquid Substances 0.000 claims abstract description 45
- 239000012141 concentrate Substances 0.000 claims abstract description 37
- 230000000171 quenching effect Effects 0.000 claims abstract description 30
- 239000002994 raw material Substances 0.000 claims abstract description 22
- 238000004519 manufacturing process Methods 0.000 claims abstract description 20
- 239000000413 hydrolysate Substances 0.000 claims abstract description 18
- 238000005374 membrane filtration Methods 0.000 claims description 47
- 239000000706 filtrate Substances 0.000 claims description 45
- 239000012528 membrane Substances 0.000 claims description 40
- 238000006243 chemical reaction Methods 0.000 claims description 36
- 239000000463 material Substances 0.000 claims description 32
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 30
- 150000002772 monosaccharides Chemical class 0.000 claims description 27
- 230000008569 process Effects 0.000 claims description 23
- 238000000746 purification Methods 0.000 claims description 19
- 238000001816 cooling Methods 0.000 claims description 16
- 239000012465 retentate Substances 0.000 claims description 15
- 238000006460 hydrolysis reaction Methods 0.000 claims description 13
- 238000010438 heat treatment Methods 0.000 claims description 12
- 230000007062 hydrolysis Effects 0.000 claims description 12
- 238000001179 sorption measurement Methods 0.000 claims description 10
- 229930182830 galactose Natural products 0.000 claims description 9
- 238000001728 nano-filtration Methods 0.000 claims description 9
- 229910052799 carbon Inorganic materials 0.000 claims description 6
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 6
- 238000002156 mixing Methods 0.000 claims description 5
- 108010009736 Protein Hydrolysates Proteins 0.000 claims description 4
- 238000003860 storage Methods 0.000 claims description 4
- 238000001035 drying Methods 0.000 claims description 3
- 239000012530 fluid Substances 0.000 claims description 3
- 150000004676 glycans Chemical class 0.000 claims description 3
- 239000000178 monomer Substances 0.000 claims description 3
- 229920001282 polysaccharide Polymers 0.000 claims description 3
- 239000005017 polysaccharide Substances 0.000 claims description 3
- 238000002360 preparation method Methods 0.000 claims description 3
- 230000000630 rising effect Effects 0.000 claims description 2
- 239000006227 byproduct Substances 0.000 abstract description 8
- 230000008901 benefit Effects 0.000 abstract description 7
- 230000035484 reaction time Effects 0.000 abstract description 6
- 239000002699 waste material Substances 0.000 abstract description 6
- 238000009776 industrial production Methods 0.000 abstract description 4
- 230000009286 beneficial effect Effects 0.000 abstract 1
- 229940088598 enzyme Drugs 0.000 description 56
- 239000000243 solution Substances 0.000 description 12
- 239000000376 reactant Substances 0.000 description 9
- 239000013078 crystal Substances 0.000 description 7
- 239000011550 stock solution Substances 0.000 description 6
- 230000000694 effects Effects 0.000 description 5
- 235000013305 food Nutrition 0.000 description 5
- 108010093031 Galactosidases Proteins 0.000 description 4
- 102000002464 Galactosidases Human genes 0.000 description 4
- 230000005764 inhibitory process Effects 0.000 description 3
- 238000004064 recycling Methods 0.000 description 3
- 238000007086 side reaction Methods 0.000 description 3
- 239000000126 substance Substances 0.000 description 3
- 239000000758 substrate Substances 0.000 description 3
- 108090000604 Hydrolases Proteins 0.000 description 2
- 102000004157 Hydrolases Human genes 0.000 description 2
- WQZGKKKJIJFFOK-PHYPRBDBSA-N alpha-D-galactose Chemical compound OC[C@H]1O[C@H](O)[C@H](O)[C@@H](O)[C@H]1O WQZGKKKJIJFFOK-PHYPRBDBSA-N 0.000 description 2
- 150000001413 amino acids Chemical class 0.000 description 2
- 230000000903 blocking effect Effects 0.000 description 2
- 239000007795 chemical reaction product Substances 0.000 description 2
- 239000007805 chemical reaction reactant Substances 0.000 description 2
- 239000003814 drug Substances 0.000 description 2
- 239000012535 impurity Substances 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- 239000010413 mother solution Substances 0.000 description 2
- 229920001542 oligosaccharide Polymers 0.000 description 2
- 238000001556 precipitation Methods 0.000 description 2
- 102000004169 proteins and genes Human genes 0.000 description 2
- 108090000623 proteins and genes Proteins 0.000 description 2
- 150000003839 salts Chemical class 0.000 description 2
- 238000010583 slow cooling Methods 0.000 description 2
- 102100026189 Beta-galactosidase Human genes 0.000 description 1
- 241000186000 Bifidobacterium Species 0.000 description 1
- WQZGKKKJIJFFOK-GASJEMHNSA-N Glucose Natural products OC[C@H]1OC(O)[C@H](O)[C@@H](O)[C@@H]1O WQZGKKKJIJFFOK-GASJEMHNSA-N 0.000 description 1
- 108010059881 Lactase Proteins 0.000 description 1
- 241000124008 Mammalia Species 0.000 description 1
- 239000005862 Whey Substances 0.000 description 1
- 102000007544 Whey Proteins Human genes 0.000 description 1
- 108010046377 Whey Proteins Proteins 0.000 description 1
- 230000009471 action Effects 0.000 description 1
- 235000020244 animal milk Nutrition 0.000 description 1
- 230000000712 assembly Effects 0.000 description 1
- 238000000429 assembly Methods 0.000 description 1
- WQZGKKKJIJFFOK-VFUOTHLCSA-N beta-D-glucose Chemical compound OC[C@H]1O[C@@H](O)[C@H](O)[C@@H](O)[C@@H]1O WQZGKKKJIJFFOK-VFUOTHLCSA-N 0.000 description 1
- 108010005774 beta-Galactosidase Proteins 0.000 description 1
- 235000013365 dairy product Nutrition 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 150000002016 disaccharides Chemical class 0.000 description 1
- 235000013350 formula milk Nutrition 0.000 description 1
- 239000008103 glucose Substances 0.000 description 1
- 230000036541 health Effects 0.000 description 1
- 230000003301 hydrolyzing effect Effects 0.000 description 1
- 230000036039 immunity Effects 0.000 description 1
- 229940116108 lactase Drugs 0.000 description 1
- -1 lactose oligosaccharides Chemical class 0.000 description 1
- 230000037356 lipid metabolism Effects 0.000 description 1
- 229920002521 macromolecule Polymers 0.000 description 1
- 235000013336 milk Nutrition 0.000 description 1
- 239000008267 milk Substances 0.000 description 1
- 210000004080 milk Anatomy 0.000 description 1
- 238000012544 monitoring process Methods 0.000 description 1
- 235000015097 nutrients Nutrition 0.000 description 1
- 150000002482 oligosaccharides Chemical class 0.000 description 1
- 238000004886 process control Methods 0.000 description 1
- 230000035755 proliferation Effects 0.000 description 1
- 230000001737 promoting effect Effects 0.000 description 1
- 235000020185 raw untreated milk Nutrition 0.000 description 1
- 235000020122 reconstituted milk Nutrition 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 230000006098 transglycosylation Effects 0.000 description 1
- 238000005918 transglycosylation reaction Methods 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C12—BIOCHEMISTRY; BEER; SPIRITS; WINE; VINEGAR; MICROBIOLOGY; ENZYMOLOGY; MUTATION OR GENETIC ENGINEERING
- C12P—FERMENTATION OR ENZYME-USING PROCESSES TO SYNTHESISE A DESIRED CHEMICAL COMPOUND OR COMPOSITION OR TO SEPARATE OPTICAL ISOMERS FROM A RACEMIC MIXTURE
- C12P19/00—Preparation of compounds containing saccharide radicals
- C12P19/12—Disaccharides
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08B—POLYSACCHARIDES; DERIVATIVES THEREOF
- C08B37/00—Preparation of polysaccharides not provided for in groups C08B1/00 - C08B35/00; Derivatives thereof
- C08B37/0006—Homoglycans, i.e. polysaccharides having a main chain consisting of one single sugar, e.g. colominic acid
- C08B37/0036—Galactans; Derivatives thereof
-
- C—CHEMISTRY; METALLURGY
- C12—BIOCHEMISTRY; BEER; SPIRITS; WINE; VINEGAR; MICROBIOLOGY; ENZYMOLOGY; MUTATION OR GENETIC ENGINEERING
- C12M—APPARATUS FOR ENZYMOLOGY OR MICROBIOLOGY; APPARATUS FOR CULTURING MICROORGANISMS FOR PRODUCING BIOMASS, FOR GROWING CELLS OR FOR OBTAINING FERMENTATION OR METABOLIC PRODUCTS, i.e. BIOREACTORS OR FERMENTERS
- C12M21/00—Bioreactors or fermenters specially adapted for specific uses
- C12M21/18—Apparatus specially designed for the use of free, immobilized or carrier-bound enzymes
-
- C—CHEMISTRY; METALLURGY
- C12—BIOCHEMISTRY; BEER; SPIRITS; WINE; VINEGAR; MICROBIOLOGY; ENZYMOLOGY; MUTATION OR GENETIC ENGINEERING
- C12M—APPARATUS FOR ENZYMOLOGY OR MICROBIOLOGY; APPARATUS FOR CULTURING MICROORGANISMS FOR PRODUCING BIOMASS, FOR GROWING CELLS OR FOR OBTAINING FERMENTATION OR METABOLIC PRODUCTS, i.e. BIOREACTORS OR FERMENTERS
- C12M33/00—Means for introduction, transport, positioning, extraction, harvesting, peeling or sampling of biological material in or from the apparatus
- C12M33/14—Means for introduction, transport, positioning, extraction, harvesting, peeling or sampling of biological material in or from the apparatus with filters, sieves or membranes
-
- C—CHEMISTRY; METALLURGY
- C12—BIOCHEMISTRY; BEER; SPIRITS; WINE; VINEGAR; MICROBIOLOGY; ENZYMOLOGY; MUTATION OR GENETIC ENGINEERING
- C12M—APPARATUS FOR ENZYMOLOGY OR MICROBIOLOGY; APPARATUS FOR CULTURING MICROORGANISMS FOR PRODUCING BIOMASS, FOR GROWING CELLS OR FOR OBTAINING FERMENTATION OR METABOLIC PRODUCTS, i.e. BIOREACTORS OR FERMENTERS
- C12M47/00—Means for after-treatment of the produced biomass or of the fermentation or metabolic products, e.g. storage of biomass
- C12M47/10—Separation or concentration of fermentation products
-
- C—CHEMISTRY; METALLURGY
- C12—BIOCHEMISTRY; BEER; SPIRITS; WINE; VINEGAR; MICROBIOLOGY; ENZYMOLOGY; MUTATION OR GENETIC ENGINEERING
- C12P—FERMENTATION OR ENZYME-USING PROCESSES TO SYNTHESISE A DESIRED CHEMICAL COMPOUND OR COMPOSITION OR TO SEPARATE OPTICAL ISOMERS FROM A RACEMIC MIXTURE
- C12P19/00—Preparation of compounds containing saccharide radicals
-
- C—CHEMISTRY; METALLURGY
- C12—BIOCHEMISTRY; BEER; SPIRITS; WINE; VINEGAR; MICROBIOLOGY; ENZYMOLOGY; MUTATION OR GENETIC ENGINEERING
- C12P—FERMENTATION OR ENZYME-USING PROCESSES TO SYNTHESISE A DESIRED CHEMICAL COMPOUND OR COMPOSITION OR TO SEPARATE OPTICAL ISOMERS FROM A RACEMIC MIXTURE
- C12P19/00—Preparation of compounds containing saccharide radicals
- C12P19/04—Polysaccharides, i.e. compounds containing more than five saccharide radicals attached to each other by glycosidic bonds
-
- C—CHEMISTRY; METALLURGY
- C12—BIOCHEMISTRY; BEER; SPIRITS; WINE; VINEGAR; MICROBIOLOGY; ENZYMOLOGY; MUTATION OR GENETIC ENGINEERING
- C12P—FERMENTATION OR ENZYME-USING PROCESSES TO SYNTHESISE A DESIRED CHEMICAL COMPOUND OR COMPOSITION OR TO SEPARATE OPTICAL ISOMERS FROM A RACEMIC MIXTURE
- C12P19/00—Preparation of compounds containing saccharide radicals
- C12P19/14—Preparation of compounds containing saccharide radicals produced by the action of a carbohydrase (EC 3.2.x), e.g. by alpha-amylase, e.g. by cellulase, hemicellulase
Landscapes
- Chemical & Material Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Organic Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Zoology (AREA)
- Health & Medical Sciences (AREA)
- Wood Science & Technology (AREA)
- Bioinformatics & Cheminformatics (AREA)
- Biotechnology (AREA)
- Genetics & Genomics (AREA)
- Biochemistry (AREA)
- General Health & Medical Sciences (AREA)
- Microbiology (AREA)
- General Engineering & Computer Science (AREA)
- Chemical Kinetics & Catalysis (AREA)
- General Chemical & Material Sciences (AREA)
- Molecular Biology (AREA)
- Biomedical Technology (AREA)
- Sustainable Development (AREA)
- Materials Engineering (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Preparation Of Compounds By Using Micro-Organisms (AREA)
Abstract
The application provides a method and a device for preparing lactose and galacto-oligosaccharide. The method comprises the steps of carrying out lactose concentration treatment on a liquid lactose-containing raw material, and separating to obtain lactose concentrated solution; purifying the lactose concentrate to obtain lactose and lactose crystallization mother liquor; carrying out complete decomposition treatment on lactose crystallization mother liquor until the galactooligosaccharide production rate of the lactose crystallization mother liquor is 15-30%, and carrying out quenching treatment; filtering and separating the quenched lactose crystallization mother liquor hydrolysate to separate residual enzyme and galactooligosaccharide flow components; the lactose and enzyme contents in the residual lactose crystallization mother liquor hydrolysate were adjusted, and the total decomposition treatment, the quenching treatment and the filtration separation treatment were repeated. Compared with the prior art, the application has at least one of the following beneficial effects: can obtain food-grade and medical-grade lactose, has the advantages of reduced content of byproducts, improved product yield, reduced production cost, reduced reaction time, no three wastes and suitability for industrial production.
Description
Technical Field
The application relates to the field of food and medicine, in particular to a method and a device for preparing lactose and galactooligosaccharide.
Background
Lactose is common disaccharide in mammal milk, is one of main nutrients for children to develop, is important for teenager's intelligence development, and may be used widely in food and medicine. In the prior art, the method for producing the food-grade lactose or the medical-grade lactose mainly comprises multiple times of crystallization and precipitation, wherein the purification and impurity removal effects are not ideal or the activated carbon adsorption treatment is carried out, and the produced residual liquid also contains residual lactose, so that waste is caused.
Galactooligosaccharides (GOS) are produced from lactose by transglycosylation by a galactosidase enzyme. In nature, galactooligosaccharides exist in animal milk in trace amounts, and are functional oligosaccharides with natural properties. Galacto-oligosaccharide has various functional characteristics of promoting the proliferation of bifidobacteria, improving lipid metabolism, improving immunity and the like, and is widely applied to various fields of dairy products, infant formulas, health care foods and the like. The current method for preparing galactooligosaccharides mainly uses lactose as a substrate and is hydrolyzed into galactooligosaccharides by galactosidase. But the monosaccharides and galactose byproducts produced during the production process inhibit the progress of the reaction, and the galactooligosaccharide products produced are also decomposed into galactose. Therefore, the method for preparing galacto-oligosaccharide in the prior art can lead to overlong reaction time, untimely product separation, increased byproducts, incomplete reaction and low product yield.
Thus, there is a need for improved methods and apparatus for preparing lactose and galactooligosaccharides.
Disclosure of Invention
In view of the deficiencies of the prior art, it is an object of the present application to provide a method and apparatus for preparing lactose and galactooligosaccharides that at least to some extent alleviates or even solves at least one of the problems set forth in the background art above.
In one aspect of the application, the application provides a process for preparing lactose and galactooligosaccharides, the process comprising: carrying out lactose concentration treatment on the liquid lactose-containing raw material, and separating to obtain lactose concentrated solution; purifying the lactose concentrated solution to prepare lactose, and separating to obtain lactose crystallization mother liquor; carrying out complete decomposition treatment on lactose crystallization mother liquor until the galactooligosaccharide production rate of the lactose crystallization mother liquor is 15-30%, and carrying out quenching treatment on lactose crystallization mother liquor hydrolysate subjected to the complete decomposition treatment; filtering and separating the lactose crystallization mother liquor hydrolysate subjected to the quenching treatment to separate residual enzyme and galactooligosaccharide flow components; and adjusting the lactose and enzyme contents in the residual lactose mother liquid hydrolysate, and repeating the total decomposition treatment, the quenching treatment and the filtration separation treatment.
Further, the lactose concentration treatment comprises the steps of filtering the liquid lactose-containing raw material by using a nanofiltration membrane with the molecular weight cutoff of 400D-600D, and filtering the obtained filtrate by using a nanofiltration membrane with the molecular weight cutoff of 150D-300D, wherein the trapped liquid is the lactose concentrate.
Further, subjecting the lactose concentrate to a purification treatment to produce lactose comprises: adding 0.2-2% active carbon into the lactose concentrated solution, heating to 50-70 ℃ and keeping for 3-10min, and filtering out the active carbon to obtain the lactose concentrated solution without active carbon; heating the activated carbon lactose-removed concentrated solution to 70-100deg.C to evaporate water until sugar degree is 50-68 ℃, cooling to 38-42deg.C at 88-100deg.C, and drying to obtain pharmaceutical lactose; optionally, the cooling comprises cooling at a rate of 0.1-1 ℃ per minute.
Further, subjecting the lactose concentrate to a purification treatment to produce lactose comprises: heating the lactose concentrate to 70-100deg.C to evaporate water to sugar degree of 50-68 deg.C, and cooling to 38-42deg.C at 80-90deg.C to form food-grade lactose crystal; optionally, the cooling comprises cooling at a rate of 0.1-1 ℃ per minute.
Further, the total decomposition treatment comprises reacting at 45-60 ℃ for 1-5min in the presence of an enzyme.
Further, the mass ratio of the enzyme to lactose in the total decomposition treated material is (0.3-1): (80-120).
Further, the quenching treatment is to reduce the temperature of the material to below 40 ℃ in 5min.
Further, in the filtration separation treatment, the filtration separation treatment is performed under the condition of maintaining the temperature of the quenched material.
Further, in the filtering separation treatment, the time of the filtering separation treatment is not more than 10min.
Further, in the filtration separation process, the filtration separation process includes a first membrane filtration process and a second membrane filtration process.
Further, the first membrane filtration treatment is carried out by adopting a filter membrane with the molecular weight cutoff of 5KD-50KD, the filtrate of the first membrane filtration treatment is a galactooligosaccharide flow component, and the trapped liquid generated by the first membrane filtration treatment contains the residual enzyme.
Further, the filtering area of the filter membrane of the first membrane filtering treatment can concentrate the volume of the trapped liquid to 10-30% of the original liquid within 10min.
Still further, the galacto-oligosaccharide flow component comprises lactose, a monosaccharide product, and galacto-oligosaccharide.
Further, the second membrane filtration treatment is performed on the galactooligosaccharide flow component using a filter membrane having a molecular weight cut-off of from 250KD to 500KD, the filtrate of the second membrane filtration treatment comprising the residual lactose and monosaccharide products, and optionally continuing with a third membrane filtration treatment.
Further, the retentate produced by the second membrane filtration process contains galactooligosaccharides.
Further, the filtration area of the filter membrane of the second membrane filtration treatment can concentrate the volume of the trapped liquid to 10-30% of the original liquid within 10min.
Further, the molecular weight cut-off of the filter membrane of the third membrane filtration treatment is 200-300D, the filtrate of the third membrane filtration treatment comprises monosaccharide product, and the cut-off liquid comprises the residual lactose.
Further, the third membrane filtration treatment is performed when monosaccharide products in the material to be subjected to the total decomposition treatment account for 15% or more of the total sugar of the material, and is stopped when monosaccharide products account for 15% or less of the total sugar of the material.
Further, the filtration area of the filter membrane for the third membrane filtration can concentrate the volume of the trapped liquid to 10-30% of the stock liquid within 10min.
Further, the method further comprises mixing the residual lactose and enzyme produced by the membrane filtration treatment with untreated lactose crystallization mother liquor and enzyme, and continuing the total decomposition treatment.
Further, the residual lactose and enzyme are subjected to temperature rising treatment in advance and then mixed with the untreated lactose crystallization mother liquor and enzyme.
Further, the enzyme includes an enzyme that hydrolyzes lactose to galactose monomers and polymerizes to polysaccharide composed of 2 to 9 galactose.
Further, the total decomposition treatment, the quenching treatment and the filtration separation treatment are repeated a plurality of times so that the hydrolysis rate of lactose is not lower than 80%.
Still further, the hydrolysis rate of lactose to 80% or more is achieved within 120min or less.
In another aspect of the present application, there is provided an apparatus for preparing lactose and galacto-oligosaccharides, characterized in that the apparatus comprises a lactose concentration unit, a purification unit, a total decomposition unit, a quenching unit and a filtration separation unit, which are sequentially connected, wherein the filtration separation unit has a residual lactose loop and a residual enzyme loop, and the residual lactose loop and the residual enzyme loop are both connected with the total decomposition unit.
Further, the lactose concentration unit comprises a nanofiltration membrane with a molecular weight cut-off of 400D-600D and 150D-300D, and is provided with a liquid lactose-containing raw material inlet and a lactose concentrate outlet; wherein the lactose concentrate outlet is connected to the purification unit.
Further, the purification unit includes an adsorption assembly and a crystallization assembly, and has a lactose concentrate inlet, a crystallized lactose outlet, and a lactose crystallization mother liquor outlet; the adsorption component is connected with the crystallization component.
Further, the crystalline lactose outlet is connected to a lactose storage tank; the lactose crystallization mother liquor outlet is connected with the full decomposition unit; the adsorption assembly includes activated carbon.
Further, the total decomposition unit comprises a lactose crystallization mother liquor inlet, a material inlet, a decomposition product outlet, a residual enzyme inlet and a residual lactose inlet; the decomposition product outlet is connected to the quench unit.
Further, the quench unit includes a decomposition product inlet, a heat exchange assembly, and a quench product outlet; the quench product outlet is connected to the filtration separation unit.
Further, the filtering separation unit comprises a first filtering component and a second filtering component; and has a residual lactose circuit and a residual enzyme circuit.
Still further, the first filter assembly has a quench product inlet, a residual enzyme outlet, and a first filtrate outlet, and is coupled to the quench unit.
Still further, the second filter assembly has a first filtrate inlet, a galactooligosaccharide outlet, and a second filtrate outlet, and is connected to the first filtrate outlet.
Still further, the residual enzyme outlet is connected to the residual enzyme circuit and the second filtrate outlet is connected to the residual lactose circuit.
Further, the filtration separation unit further comprises a third filtration assembly; the third filter assembly comprises a second filtrate inlet, a trapped fluid outlet and a third filtrate outlet; wherein the retentate outlet is connected to the residual lactose loop.
In general, the present application has at least one of the following benefits:
1. the application prepares lactose by using liquid lactose-containing raw materials, can obtain food-grade and medical-grade lactose, has high purity of the obtained food-grade lactose and medical-grade lactose, prepares galactooligosaccharides by using reaction residual liquid, and reduces production cost;
2. the application adopts the intermittent reaction process flow to prepare the galactooligosaccharide, processes the materials according to the circulation of full reaction-slow reaction and separation-full reaction, separates the reaction products and reactants in time, reduces the occurrence of side reaction, reduces the content of byproducts and improves the product generation rate;
3. the method provided by the application separates and recycles reactants in the process of preparing the galactooligosaccharide, so that the reactants are fully reacted, the production cost is reduced, the galactooligosaccharide can be prepared by taking the high ash lactose mother liquor as a raw material, the energy is saved, the environment is protected, and no three wastes are generated.
4. The device reduces the reaction time, lowers the production cost, and is suitable for industrial production.
The foregoing summary is for the purpose of the specification only and is not intended to be limiting in any way. In addition to the illustrative aspects, embodiments, and features described above, further aspects, embodiments, and features of the present application will become apparent by reference to the drawings and the following detailed description.
Drawings
In the drawings, the same reference numerals refer to the same or similar parts or elements throughout the several views unless otherwise specified. The figures are not necessarily drawn to scale. It is appreciated that these drawings depict only some embodiments according to the disclosure and are not therefore to be considered limiting of its scope.
FIG. 1 is a flow chart of a method according to an embodiment of the application;
FIG. 2 is a schematic diagram of a structure according to an embodiment of the present application;
fig. 3 is a schematic view of a part of a structure according to an embodiment of the present application.
Reference numerals illustrate: 100-total decomposition unit, 110-lactose crystallization mother liquor inlet, 120-material inlet, 130-decomposition product outlet, 140-residual enzyme inlet, 150-residual lactose inlet, 200-quenching unit, 210-decomposition product inlet, 220-quenching product outlet, 300-filtration separation unit, 310-residual enzyme circuit, 320-residual lactose circuit, 330-first filtration module, 331-quenching product inlet, 332-residual enzyme outlet, 333-first filtrate outlet, 340-second filtration module, 341-first filtrate inlet, 342-galacto-oligosaccharide outlet, 343-second filtrate outlet, 350-third filtration module, 351-second filtrate inlet, 352-retentate outlet, 353-third filtrate outlet, 400-purification unit, 410-lactose mother liquor inlet, 420-crystallized lactose outlet, 430-lactose crystallization mother liquor outlet, 500-lactose concentration unit, 510-liquid lactose-containing raw material inlet, 520-lactose concentration liquid outlet, 10-lactose storage tank.
Detailed Description
In order to more clearly understand the technical features, objects and advantages of the present application, a further detailed description will now be made of the technical scheme of the present application. Hereinafter, only certain exemplary embodiments are briefly described. As will be recognized by those of skill in the pertinent art, the described embodiments may be modified in various different ways without departing from the spirit or scope of the present application. Accordingly, the drawings and description are to be regarded as illustrative in nature and not as restrictive.
In one aspect of the application, a method of preparing lactose and galactooligosaccharides is provided. Referring to fig. 1, the method comprises lactose concentrating liquid lactose-containing raw material, and separating to obtain lactose concentrate; purifying the lactose concentrated solution to prepare lactose, and separating to obtain lactose crystallization mother liquor; carrying out full decomposition treatment on lactose crystallization mother liquor; quenching the lactose crystallization mother liquor hydrolysate subjected to the complete decomposition treatment; filtering and separating the lactose crystallization mother liquor hydrolysate subjected to quenching treatment; the lactose and enzyme contents in the residual lactose mother liquor hydrolysate were adjusted, and the total decomposition treatment, the quenching treatment and the filtration separation treatment were repeated. Detecting the production rate of the galacto-oligosaccharide in the process of carrying out the full decomposition treatment, and carrying out quenching treatment on the obtained lactose crystallization mother liquor hydrolysate when the production rate of the galacto-oligosaccharide is 15-30%; and in the filtering and separating treatment process, lactose and enzyme remained in the lactose mother liquor hydrolysate, monosaccharide products generated by side reaction and galactooligosaccharide flow are timely separated. The method has at least one of the following advantages: can obtain food-grade and medical-grade lactose, has the advantages of reduced content of byproducts, improved product yield, reduced production cost, reduced reaction time, no three wastes and suitability for industrial production.
For easy understanding, the principle by which the above advantageous effects can be achieved by the method is first briefly described below: the application prepares lactose concentrate by liquid lactose-containing raw material, prepares lactose by using lactose concentrate, prepares galactooligosaccharide by using the produced residual lactose crystallization mother liquor, and fully utilizes the reaction materials; wherein the lactose produced includes, but is not limited to, food grade lactose and pharmaceutical grade lactose. In addition, in the process of preparing the galacto-oligosaccharide, the application adopts a batch reaction process flow, and timely separates reactants from products in the reaction process to prevent byproducts from being generated and products from being decomposed; and the separated reactants are injected into the circulation to carry out full decomposition reaction again, thus greatly reducing the time required by the reaction and improving the product yield. For example, the hydrolysis rate of lactose can be made to be 80% or more within 120min by repeating the steps of the present application 4 to 5 times. In addition, the method can prepare the galactooligosaccharide by taking the high ash lactose mother solution as a raw material, is energy-saving and environment-friendly, and has no three wastes.
According to the embodiment of the application, in the process of preparing lactose concentrate, the method comprises the steps of filtering liquid lactose-containing raw materials by using a nanofiltration membrane with the molecular weight cutoff of 400D-600D, collecting the obtained filtrate, and filtering the obtained filtrate by using a nanofiltration membrane with the molecular weight cutoff of 150D-300D, wherein the cutoff is the lactose concentrate, so that lactose in the liquid lactose-containing raw materials is fully extracted, and small molecular substances such as inorganic salts, monosaccharides, amino acids and the like and macromolecular substances such as proteins and the like are fully removed to a great extent.
According to the examples of the present application, the kind of the liquid lactose-containing raw material is not particularly limited as long as lactose is contained, and for example, in a specific embodiment, the liquid lactose-containing raw material includes, but is not limited to, raw milk, reconstituted milk, liquid whey, or a combination thereof.
According to an embodiment of the application, the purification treatment comprises extracting lactose from the lactose concentrate to produce pharmaceutical grade lactose. Specifically, activated carbon is first added to the lactose concentrate, and after the activated carbon is added to the lactose concentrate, heat treatment may be performed until the temperature is 50 to 70 ℃, which is maintained for 3 to 10 minutes, to sufficiently adsorb impurities, wherein the addition amount of the activated carbon is not particularly limited, and for example, 0.2 to 2% of the activated carbon may be added in specific embodiments. And filtering the activated carbon to obtain a lactose concentrated solution without any particular limitation, as long as the activated carbon can be filtered out, for example, using filter paper, a filter membrane, a filter screen, etc. Heating the obtained lactose concentrated solution at 70-100deg.C to evaporate water until sugar degree is 50-68 deg.C, slowly cooling at 88-100deg.C until the temperature is 38-42 deg.C to form pharmaceutical lactose crystal, centrifuging the cooled mixture in a centrifuge to separate the pharmaceutical lactose crystal, and collecting the obtained liquid for subsequent treatment, wherein the obtained liquid is lactose crystal mother liquor. Wherein slow cooling comprises cooling at a rate of 0.1-1deg.C per minute.
According to an embodiment of the application, the purification treatment comprises extracting lactose from the lactose concentrate to produce food grade lactose. The preparation of the food-grade lactose comprises heating the obtained lactose concentrated solution at 70-100deg.C to evaporate water until the sugar degree is 50-68 ℃, slowly cooling at 80-90deg.C until the temperature is 38-42 ℃ to form food-grade lactose crystal, centrifuging the cooled mixture in a centrifuge to separate the obtained food-grade lactose crystal, and collecting the obtained liquid for subsequent treatment, wherein the obtained liquid is lactose crystal mother liquor. Wherein slow cooling comprises cooling at a rate of 0.1-1deg.C per minute.
Lactose crystallization mother liquor is the residual liquid produced after crystallization treatment, which contains very high ash content, ash content is more than 10%, even 19% or more, and ash content in common lactose-containing raw materials is usually less than 0.5%. However, a high ash content reduces the activity of lactose hydrolase (e.g., galactosidase, etc.), and reduces the hydrolysis rate of lactose, so that it is difficult to prepare lactose oligosaccharides using high ash lactose solution as a raw material in the related art. The method of the application continuously separates reactants and products, and ensures the optimal ratio of the reactants and the products by complete reaction, slow reaction and separation and complete reaction circulation and adding enzyme and lactose in the circulation process, and simultaneously continuously separates substrates and products. The method can effectively control the content of reactants, avoid the reduction of lactose hydrolase activity, and further realize the preparation of galactooligosaccharides by taking high ash lactose mother liquor as a raw material.
According to an embodiment of the present application, the total decomposition treatment comprises mixing lactose crystallization mother liquor with an enzyme and carrying out the reaction in the presence of the enzyme, wherein the temperature and time of the reaction are not particularly limited as long as the reaction is stopped when the galactooligosaccharide production rate is 15 to 30%, for example, in a specific embodiment, the reaction may be carried out at a temperature of 45 to 60℃for 1 to 5 minutes, preferably at a temperature of 50 to 55℃for 2 to 4 minutes, to obtain lactose crystallization mother liquor hydrolysate. Wherein the lactose crystallization mother liquor hydrolysate comprises galactooligosaccharides generated by the reaction, unreacted lactose, residual enzyme and generated byproducts. The process controls the reaction temperature and time, so that the effect of full reaction is achieved in a short time, and the proper time is selected to timely perform separation treatment by monitoring the galactooligosaccharide production rate. Therefore, the problem of low hydrolysis rate in the current process of preparing galactooligosaccharide by hydrolyzing lactase can be relieved and even solved, the time consumption of hydrolysis reaction and the problem of precipitation and membrane blocking during filtration of sugar membranes can be relieved. The timely separation treatment can also solve the problems that the hydrolysis of the substrate lactose into the galactooligosaccharide product causes the product inhibition, the galactooligosaccharide is simultaneously decomposed into monosaccharide, and the reaction is further caused to be carried out to the product inhibition.
In the present application, the mixing ratio of lactose crystallization mother liquor and enzyme is not particularly limited, but in order to avoid the reaction proceeding too fast or too slow, in the specific embodiment, the mass ratio of enzyme and lactose in the total decomposition treated material is (0.3-1): (80-120), preferably (0.5-0.8): (90-110). In addition, enzymes used in the present application include enzymes that hydrolyze lactose to galactose monomers and polymerize to polysaccharides consisting of 2-9 galactose, including but not limited to galactosidase.
According to the embodiment of the application, the quenching treatment comprises the steps of reducing the temperature of lactose crystallization mother liquor hydrolysate obtained by the full-treatment reaction to below 40 ℃ within 5min, and reducing the reaction rate to enable the reaction to be carried out slowly so as to prevent the inhibition of products and the decomposition of the products and reduce the occurrence of side reactions. That is, the application can control multiple problems caused by excessive lactose decomposition reaction to a great extent by quenching the material reaching the production rate of the lactose oligomer, and further control each component in the material which is filtered and separated subsequently in a reasonable proportion, thereby solving the problem of filtering and blocking the film, improving the production efficiency of the method and reducing the production time.
According to an embodiment of the present application, the filtration separation treatment comprises treating the lactose crystallization mother liquor hydrolyzed solution subjected to the quenching treatment to separate its components, specifically, the filtration separation treatment is performed at a temperature of not higher than 40 ℃ to maintain the temperature of the material after the quenching treatment. Preferably, the temperature of the filtration separation treatment is the same as or similar to the temperature of the quenching treatment, wherein the time of the filtration separation treatment is not more than 15min, preferably not more than 10min. Since a certain time is required for the filtration and separation treatment, the temperature during the filtration and separation treatment is maintained at the temperature of the quenched material, and the excessive progress of the reaction can be prevented.
According to an embodiment of the present application, the filtration separation process includes a first membrane filtration process and a second membrane filtration process. Wherein the first membrane filtration treatment comprises treating the quenched lactose crystallization mother liquor hydrolysate with a filter membrane to separate galacto-oligosaccharide stream components, wherein the galacto-oligosaccharide stream components comprise lactose, monosaccharide products, and galacto-oligosaccharides, wherein the monosaccharide products include, but are not limited to, glucose and galactose. In a specific embodiment, the treatment may be performed with a filter having a molecular weight cut-off of 5KD to 50KD, wherein the filtrate from the first membrane filtration treatment is a galactooligosaccharide stream component, and the resulting retentate contains residual enzyme. In addition, the filtration area of the filter membrane of the first membrane filtration treatment is not particularly limited, and specifically may be determined according to the volume of the produced lactose crystallization mother liquor hydrolysate as long as the volume of the retentate can be concentrated to 10 to 30% of the stock solution, and preferably the filtration area of the filter membrane of the first membrane filtration can concentrate the volume of the retentate to 10 to 30% of the stock solution within 10 minutes.
According to an embodiment of the application, the second membrane filtration treatment comprises separating the galacto-oligosaccharide stream components, and in a specific embodiment, the galacto-oligosaccharide stream components may be treated with a filter having a molecular weight cut-off of from 250KD to 500KD, wherein the filtrate of the second membrane filtration treatment comprises residual lactose and monosaccharide products and the retentate comprises galacto-oligosaccharides. In addition, the filtration area of the filter membrane of the second membrane filtration treatment is not particularly limited, and specifically may be determined according to the volume of the produced galactooligosaccharide flow component as long as the volume of the retentate can be concentrated to 10 to 30% of the stock solution, and preferably the filtration area of the filter membrane of the second membrane filtration can concentrate the volume of the retentate to 10 to 30% of the stock solution within 10 minutes.
According to the embodiment of the application, a small amount of monosaccharide product can be contained in lactose added in the material subjected to the total decomposition treatment, however, when the monosaccharide product in the material subjected to the total decomposition treatment accounts for more than 15% of the total sugar in the material, the filtrate subjected to the second membrane filtration treatment can be further subjected to the third membrane filtration treatment and stopped when the monosaccharide product accounts for 15% or less of the total sugar in the material. Wherein the molecular weight cut-off of the filter membrane of the third membrane filtration treatment is 200-300D, the filtrate of the third membrane filtration treatment comprises monosaccharide product, and the cut-off liquid comprises residual lactose. In addition, the filtration area of the filtration membrane of the third membrane filtration treatment is not particularly limited, and specifically may be determined according to the volume of the filtrate of the second membrane filtration treatment to be produced, as long as the volume of the retentate can be concentrated to 10 to 30% of the stock solution, and preferably the filtration area of the filtration membrane of the third membrane filtration can concentrate the volume of the retentate to 10 to 30% of the stock solution within 10 minutes.
According to an embodiment of the present application, the method of the present application further comprises heating the residual lactose and enzyme obtained by the filtration and separation treatment, mixing the residual lactose and enzyme with untreated lactose crystallization mother liquor and enzyme, and continuing the total decomposition reaction. Wherein the mass ratio of enzyme to lactose is (0.3-1): (80-120), preferably (0.5-0.8): (90-110). Further, the temperature of the temperature-raising treatment is 45 to 60 ℃, preferably 50 to 55 ℃.
According to an embodiment of the present application, the method of the present application comprises repeating the steps of the above-mentioned total decomposition treatment, quenching treatment, and filtration separation treatment a plurality of times so that the hydrolysis rate of lactose is not less than 80%. Wherein, the hydrolysis rate of lactose is not lower than 80% within 120 min. In a specific embodiment, the hydrolysis rate of lactose can be more than 80% within 120min by repeating the steps of full decomposition treatment, quenching treatment and filtering separation treatment for 4-5 times, and the hydrolysis rate of lactose is continuously increased along with the increase of the times of repeating the steps of the method.
According to embodiments of the present application, the batch reaction process may be used to prepare galactooligosaccharides, but is not limited to, and may also be used to prepare other materials that may be by-produced and readily decomposed during the reaction.
In another aspect of the present application, the present application provides an apparatus for preparing lactose and galactooligosaccharides, referring to fig. 2, comprising a total decomposition unit 100, a quenching unit 200, a filtration separation unit 300, a purification unit 400, and a lactose concentration unit 500. The lactose concentration unit 500, the purification unit 400, the total decomposition unit 100, the quenching unit 200 and the filtration and separation unit 300 are connected in sequence, the filtration and separation unit 300 is provided with a residual lactose circuit 320 and a residual enzyme circuit 310, and the residual lactose circuit 320 and the residual enzyme circuit 310 are connected with the total decomposition unit 100. The device has at least one of the following advantages: reduces the reaction time, reduces the production cost, is suitable for industrial production, can prepare galactooligosaccharide by taking high ash lactose mother liquor as a raw material, is energy-saving and environment-friendly, and has no three wastes.
In accordance with an embodiment of the present application, the lactose concentration unit includes a liquid lactose-containing feed inlet 510 and a lactose concentrate outlet 520, and the lactose concentrate outlet 520 is connected to the purification unit to deliver lactose concentrate to purification but to conduct purification treatment as described herein. Specifically, the lactose concentration unit comprises nanofiltration membranes with the molecular weight cut-off of 400D-600D and 150D-300D so as to remove inorganic salts, small molecular weight substances such as monosaccharides and amino acids, and large molecular weight substances such as proteins in the liquid lactose-containing raw material respectively.
In accordance with an embodiment of the present application, purification unit 400 comprises lactose concentrate inlet 410, crystallized lactose outlet 420, and lactose crystallized mother liquor outlet 430, wherein crystallized lactose outlet 420 is connected to lactose storage tank 10; the lactose crystallization mother liquor outlet 430 is connected to the total decomposition unit 100. In particular embodiments, purification unit 400 includes an adsorption module and a crystallization module, and the adsorption module is coupled to the crystallization module, and the adsorption module used may include activated carbon; in addition, the crystallization assembly includes a temperature adjusting element to adjust the temperature of the reaction mass.
According to an embodiment of the present application, the total decomposition unit 100 comprises a lactose crystallization mother liquor inlet 110, a material inlet 120, a decomposition product outlet 130, a residual enzyme inlet 140, and a residual lactose inlet 150, wherein lactose crystallization mother liquor enters from the lactose crystallization mother liquor inlet 110, enzyme enters from the material inlet 120, and the lactose crystallization mother liquor and the enzyme react to generate lactose crystallization mother liquor hydrolysate, and the lactose crystallization mother liquor hydrolysate flows out from the decomposition product outlet 130; the recycled residual enzyme and residual lactose enter from the residual enzyme inlet 140 and residual lactose inlet 150, respectively, to repeat the reaction; in addition, to adjust the mass ratio of lactose to enzyme in the reactants, untreated lactose crystallization mother liquor and enzyme may be fed from the feed inlet 120 to carry out a total decomposition reaction together with residual enzyme and residual lactose obtained by recycling.
In accordance with an embodiment of the present application, quench unit 200 is connected to decomposition product outlet 130 of total decomposition unit 100, which includes decomposition product inlet 210 and quench product outlet 220, and has a heat exchange assembly for quenching; in the specific embodiment, the lactose crystallization mother liquor hydrolysate enters the quenching unit 200 from the decomposition product inlet 210, is cooled under the action of a heat exchange component, and then flows out from the quenching product outlet 220.
According to an embodiment of the present application, the filtering separation unit 300 has a residual enzyme circuit 310 and a residual lactose circuit 320, and both the residual enzyme circuit 310 and the residual lactose circuit 320 are connected to the total decomposition unit 100 to re-inject the separated residual enzyme and residual lactose into the total decomposition unit 100 for reaction. Referring to fig. 2 and 3, in a specific embodiment, the filtering separation unit 300 includes a first filtering assembly 330 and a second filtering assembly 340, and the first filtering assembly 330 is connected with the second filtering assembly 340. The first filter assembly 330 has a quench product inlet 331, a residual enzyme outlet 332, and a first filtrate outlet 333, and is connected to the quench unit 200; wherein the residual enzyme outlet 332 is connected to the residual enzyme circuit 310 and the first filtrate outlet 333 is connected to the second filter assembly 340. The second filter assembly 340 has a first filtrate inlet 341, a galacto-oligosaccharide outlet 342 and a second filtrate outlet 343, wherein the second filtrate outlet 343 is connected to the residual lactose circuit 320. In addition, the filtering separation unit 300 may further include a third filtering component 350 to further perform a third filtering process on the solution flowing out of the second filtrate outlet 343 to remove the monosaccharide product to reduce the content of the monosaccharide product when the monosaccharide product in the material to be subjected to the total decomposition treatment is 15% or more of the total sugar of the material, and stop the process when the monosaccharide product is 15% or less of the total sugar of the material; wherein the third filter assembly 350 comprises a second filtrate inlet 351, a retentate outlet 352 and a third filtrate outlet 353, wherein the retentate outlet 352 is connected to the residual lactose circuit 320. Specifically, the quenched lactose crystallization mother liquor hydrolysate is injected into the first filter assembly 330 from the quenched product inlet 331, and residual enzyme is separated, and a galactooligosaccharide stream component is obtained; the galactooligosaccharide flow component is injected into the second filter assembly 340 from the first filtrate inlet 341, the produced galactooligosaccharide is filtered out, the obtained filtrate is injected into the residual lactose circuit 320 for recycling reaction, or the obtained filtrate is injected into the third filter assembly 350 to filter out monosaccharide products, the obtained trapped liquid is injected into the residual lactose circuit 320 for recycling reaction, wherein the residual enzyme circuit 310 and the residual lactose circuit 320 can further comprise heating elements for heating residual enzyme and residual lactose and then delivering the heated residual enzyme and residual lactose to the full reaction unit 100. In addition, the first, second and third filter assemblies 350 each comprise a filter membrane, wherein the filter membrane used in the first filter assembly 330 has a molecular weight cut-off of 5KD to 50KD, the filter membrane used in the second filter assembly 340 has a molecular weight cut-off of 250KD to 500KD, and the filter membrane used in the third filter assembly 350 has a molecular weight cut-off of 200D to 300D; also, in particular embodiments, it is preferred that the molecular weight cut-off of the filter membrane used in the second filter assembly 340 is greater than the molecular weight cut-off of the filter membrane used in the third filter assembly 350.
In general, the method and the device for preparing lactose and galacto-oligosaccharide provided by the application separate reaction products and reactants in time by adopting the intermittent reaction process flow, and separate and recycle the reactants, so that the content of byproducts is reduced, the product generation rate is improved, the reaction time is reduced, the production cost is reduced, and in addition, the galacto-oligosaccharide is prepared by taking the high ash lactose mother solution as the raw material.
While the fundamental and principal features of the application and advantages of the application have been shown and described, it will be apparent to those skilled in the art that the application is not limited to the details of the foregoing exemplary embodiments, but may be embodied in other specific forms without departing from the spirit or essential characteristics thereof. Accordingly, the embodiments are to be considered in all respects as illustrative and not restrictive.
Furthermore, it should be understood that although the present disclosure describes embodiments, not every embodiment is provided with a separate embodiment, and that this description is provided for clarity only, and that the disclosure is not limited to the embodiments described in detail below, and that the embodiments described in the examples may be combined as appropriate to form other embodiments that will be apparent to those skilled in the art.
Claims (20)
1. A process for the preparation of lactose and galactooligosaccharides, said process comprising:
carrying out lactose concentration treatment on the liquid lactose-containing raw material, and separating to obtain lactose concentrated solution;
purifying the lactose concentrated solution to prepare lactose, and separating to obtain lactose crystallization mother liquor;
carrying out complete decomposition treatment on lactose crystallization mother liquor until the galactooligosaccharide production rate of the lactose crystallization mother liquor is 15-30%, and carrying out quenching treatment on lactose crystallization mother liquor hydrolysate subjected to the complete decomposition treatment;
filtering and separating the lactose crystallization mother liquor hydrolysate subjected to the quenching treatment to separate residual enzyme and galactooligosaccharide flow components;
and adjusting the lactose and enzyme contents in the residual lactose crystallization mother liquor hydrolysate, and repeating the total decomposition treatment, the quenching treatment and the filtration separation treatment.
2. The method according to claim 1, wherein the lactose concentration treatment comprises filtering the liquid lactose-containing raw material with a nanofiltration membrane with a molecular weight cut-off of 400D-600D, and filtering the obtained filtrate with a nanofiltration membrane with a molecular weight cut-off of 150D-300D, wherein the cut-off is the lactose concentrate.
3. The method of claim 1, wherein purifying the lactose concentrate to produce lactose comprises:
adding 0.2-2% active carbon into the lactose concentrated solution, heating to 50-70 ℃ and keeping for 3-10min, and filtering out the active carbon to obtain the lactose concentrated solution without active carbon;
heating the concentrated solution of lactose without activated carbon to 70-100deg.C to evaporate water to sugar degree of 50-68 deg.C, cooling to 38-42deg.C at 88-100deg.C, drying to obtain pharmaceutical lactose,
optionally, the cooling comprises cooling at a rate of 0.1-1 ℃ per minute.
4. The method of claim 1, wherein purifying the lactose concentrate to produce lactose comprises:
heating the lactose concentrate to 70-100deg.C to evaporate water to sugar degree of 50-68 deg.C, cooling to 38-42deg.C at 80-90deg.C, drying to obtain food-grade lactose,
optionally, the cooling comprises cooling at a rate of 0.1-1 ℃ per minute.
5. The method according to claim 1, wherein the total decomposition treatment comprises a reaction at 45-60 ℃ for 1-5min in the presence of an enzyme.
6. The method according to claim 5, wherein the mass ratio of the enzyme to lactose in the total decomposed material is (0.3-1): (80-120).
7. The method of claim 1, wherein the quenching is to reduce the temperature of the material to below 40 ℃ within 5 minutes.
8. The method of claim 1, wherein the filtering separation process satisfies at least one of the following conditions:
the filtering separation treatment is carried out under the condition of maintaining the temperature of the quenched material;
the time of the filtering separation treatment is not more than 10min;
the filtration separation treatment includes a first membrane filtration treatment and a second membrane filtration treatment.
9. The method of claim 8, wherein the first membrane filtration process is performed using a filter membrane having a molecular weight cut-off of 5KD to 50KD, the filtrate of the first membrane filtration process is a galacto-oligosaccharide stream component, and the retentate produced by the first membrane filtration process contains the residual enzyme;
optionally, the filtering area of the filter membrane of the first membrane filtering treatment can concentrate the volume of the trapped liquid to 10-30% of the stock liquid within 10min;
wherein the galacto-oligosaccharide flow component comprises lactose, a monosaccharide product, and galacto-oligosaccharide.
10. The method according to claim 8, wherein the second membrane filtration treatment is performed on the galactooligosaccharide flow component using a filter membrane having a molecular weight cut-off of 250KD to 500KD, the filtrate of the second membrane filtration treatment comprising the residual lactose and monosaccharide products, and optionally continuing with a third membrane filtration treatment;
the trapped fluid generated by the second membrane filtration treatment contains galactooligosaccharides;
optionally, the filtration area of the filter membrane of the second membrane filtration treatment can concentrate the volume of the trapped liquid to 10-30% of the stock liquid within 10min;
the molecular weight cut-off of the filter membrane of the third membrane filtration treatment is 200-300D, the filtrate of the third membrane filtration treatment comprises monosaccharide products, and the cut-off liquid comprises the residual lactose;
optionally, when monosaccharide products in the material to be subjected to the total decomposition treatment account for more than 15% of the total sugar of the material, performing the third membrane filtration treatment, and stopping when monosaccharide products account for 15% or less of the total sugar of the material;
optionally, the filtration area of the filter membrane of the third membrane filtration can concentrate the volume of the trapped liquid to 10-30% of the original liquid within 10min.
11. The method according to claim 9 or 10, further comprising mixing the residual lactose and enzyme produced by the membrane filtration process with untreated lactose crystallization mother liquor and enzyme, continuing the total decomposition process;
optionally, the residual lactose and enzyme are subjected to temperature rising treatment in advance and then mixed with the untreated lactose crystallization mother liquor and enzyme.
12. The method of claim 1, wherein the enzyme comprises an enzyme that hydrolyzes lactose to galactose monomers and polymerizes to a polysaccharide consisting of 2-9 galactose.
13. The method according to claim 1, wherein the total decomposition treatment, the quenching treatment and the filtration separation treatment are repeated a plurality of times so that the hydrolysis rate of lactose is not less than 80%;
the hydrolysis rate of lactose is not lower than 80% and is not higher than 120 min.
14. An apparatus for preparing lactose and galacto-oligosaccharides by the method of any one of claims 1-13, characterized in that the apparatus comprises a lactose concentration unit, a purification unit, a total decomposition unit, a quenching unit and a filtration separation unit, which are connected in sequence, the filtration separation unit having a residual lactose loop and a residual enzyme loop, both of which are connected to the total decomposition unit.
15. The apparatus of claim 14, wherein the lactose concentration unit comprises nanofiltration membranes having molecular weight cut-offs of 400D-600D and 150D-300D and has a liquid lactose-containing feed inlet and a lactose concentrate outlet;
wherein the lactose concentrate outlet is connected to the purification unit.
16. The apparatus of claim 14, wherein the purification unit comprises an adsorption module and a crystallization module and has a lactose concentrate inlet, a crystallized lactose outlet, and a lactose crystallization mother liquor outlet;
the adsorption component is connected with the crystallization component;
wherein the crystalline lactose outlet is connected with a lactose storage tank;
the lactose crystallization mother liquor outlet is connected with the full decomposition unit;
the adsorption assembly includes activated carbon.
17. The apparatus of claim 14, wherein the total decomposition unit comprises a lactose crystallization mother liquor inlet, a material inlet, a decomposition product outlet, a residual enzyme inlet, and a residual lactose inlet;
the decomposition product outlet is connected to the quench unit.
18. The apparatus of claim 14, wherein the quench unit comprises a decomposition product inlet, a heat exchange assembly, and a quench product outlet;
the quench product outlet is connected to the filtration separation unit.
19. The apparatus of claim 14, wherein the filtration separation unit comprises a first filtration assembly and a second filtration assembly; and has a residual lactose circuit and a residual enzyme circuit;
the first filter assembly has a quench product inlet, a residual enzyme outlet, and a first filtrate outlet, and is connected to the quench unit;
the second filter assembly is provided with a first filtrate inlet, a galacto-oligosaccharide outlet and a second filtrate outlet and is connected with the first filtrate outlet;
wherein the residual enzyme outlet is connected with the residual enzyme loop, and the second filtrate outlet is connected with the residual lactose loop.
20. The apparatus of claim 19, wherein the filtration separation unit further comprises a third filtration assembly;
the third filter assembly comprises a second filtrate inlet, a trapped fluid outlet and a third filtrate outlet;
wherein the retentate outlet is connected to the residual lactose loop.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202310893092.XA CN116926147A (en) | 2023-07-19 | 2023-07-19 | Method and device for preparing lactose and galacto-oligosaccharide |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202310893092.XA CN116926147A (en) | 2023-07-19 | 2023-07-19 | Method and device for preparing lactose and galacto-oligosaccharide |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN116926147A true CN116926147A (en) | 2023-10-24 |
Family
ID=88387392
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202310893092.XA Pending CN116926147A (en) | 2023-07-19 | 2023-07-19 | Method and device for preparing lactose and galacto-oligosaccharide |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN116926147A (en) |
Citations (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2012047122A1 (en) * | 2010-10-07 | 2012-04-12 | Anthony James Styles | Lactose production |
| CN103484574A (en) * | 2013-09-22 | 2014-01-01 | 江苏道宁药业有限公司 | Officinal lactose production technology |
| CN105612258A (en) * | 2013-09-05 | 2016-05-25 | 菲仕兰康必奶荷兰有限公司 | Production of galacto-oligosaccharides |
| CN109293715A (en) * | 2018-10-25 | 2019-02-01 | 广州市乐提食品科技发展有限公司 | A kind of continuous producing method of high purity lactose |
| CN109548872A (en) * | 2018-12-07 | 2019-04-02 | 新疆旺源生物科技集团有限公司 | A kind of preparation method of Low lactose milk camel cream |
| CN113444129A (en) * | 2021-07-21 | 2021-09-28 | 曲阜贝斯迪生物医药有限公司 | Method for extracting crystallized lactose for processing edible lactose |
| CN115141865A (en) * | 2022-09-06 | 2022-10-04 | 山东百龙创园生物科技股份有限公司 | Method for preparing lactulose and co-producing galacto-oligosaccharide |
| CN115160384A (en) * | 2022-07-07 | 2022-10-11 | 安徽禾庚生物技术有限公司 | Method for producing galactose and glucose by taking milk as raw material |
-
2023
- 2023-07-19 CN CN202310893092.XA patent/CN116926147A/en active Pending
Patent Citations (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2012047122A1 (en) * | 2010-10-07 | 2012-04-12 | Anthony James Styles | Lactose production |
| CN105612258A (en) * | 2013-09-05 | 2016-05-25 | 菲仕兰康必奶荷兰有限公司 | Production of galacto-oligosaccharides |
| CN103484574A (en) * | 2013-09-22 | 2014-01-01 | 江苏道宁药业有限公司 | Officinal lactose production technology |
| CN109293715A (en) * | 2018-10-25 | 2019-02-01 | 广州市乐提食品科技发展有限公司 | A kind of continuous producing method of high purity lactose |
| CN109548872A (en) * | 2018-12-07 | 2019-04-02 | 新疆旺源生物科技集团有限公司 | A kind of preparation method of Low lactose milk camel cream |
| CN113444129A (en) * | 2021-07-21 | 2021-09-28 | 曲阜贝斯迪生物医药有限公司 | Method for extracting crystallized lactose for processing edible lactose |
| CN115160384A (en) * | 2022-07-07 | 2022-10-11 | 安徽禾庚生物技术有限公司 | Method for producing galactose and glucose by taking milk as raw material |
| CN115141865A (en) * | 2022-09-06 | 2022-10-04 | 山东百龙创园生物科技股份有限公司 | Method for preparing lactulose and co-producing galacto-oligosaccharide |
Non-Patent Citations (1)
| Title |
|---|
| 江正强等: "食品酶学与酶工程原理", 30 September 2018, 国轻工业出版社, pages: 150 * |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| Vera et al. | Synthesis and purification of galacto-oligosaccharides: state of the art | |
| CN1303091C (en) | Preparation of oligo-wood sugar | |
| CN107058416B (en) | Fermentation process for refining glutamic acid | |
| CN105612258B (en) | Production of galacto-oligosaccharides | |
| CN108822163B (en) | Comprehensive cyclic production method of D-glucosamine hydrochloride | |
| CN108285912B (en) | Method for preparing and extracting pharmaceutical grade valine by fermentation | |
| CN101508740A (en) | Process for preparing poly-glucose | |
| CN102976923A (en) | New process for extracting lactic acid from lactic acid fermentation liquid | |
| CN113215210B (en) | Method for preparing sialic acid by adopting polysialic acid fermentation liquor | |
| CN113214076A (en) | Method for recovering lactic acid from lactic acid distillation kettle bottom liquid | |
| CN102603548B (en) | Method for extracting L-alanine from mother solution | |
| CN111172145A (en) | Immobilized enzyme and method for producing functional oligosaccharide by using same | |
| CN113005161B (en) | Preparation method of polysialic acid and polysialic acid product | |
| CN114539333A (en) | Cyclic production process of sialic acid | |
| KR20130057540A (en) | Methods for purifying lactic acid | |
| CN116926147A (en) | Method and device for preparing lactose and galacto-oligosaccharide | |
| WO2004078989A1 (en) | Process for purifying difructose-dianhydride iii | |
| CN110627848B (en) | Method for removing impurities in sialic acid and application thereof | |
| CN109369731B (en) | Method for removing glucose in xylose production process | |
| CN112662714B (en) | Production process for preparing ornithine | |
| CN215209405U (en) | Production system for preparing ornithine | |
| CN113045610B (en) | Method for extracting glucosamine from N-acetylglucosamine fermentation liquor | |
| CN109234336A (en) | A kind of method of dextrase enzymolysis inulin production oligofructose | |
| CN106589006A (en) | Boracic acid recovery and reutilization method in lactulose preparation | |
| CN114573644A (en) | Preparation method of sialic acid |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination |