CN115160384A - Method for producing galactose and glucose by taking milk as raw material - Google Patents

Method for producing galactose and glucose by taking milk as raw material Download PDF

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Publication number
CN115160384A
CN115160384A CN202210791307.2A CN202210791307A CN115160384A CN 115160384 A CN115160384 A CN 115160384A CN 202210791307 A CN202210791307 A CN 202210791307A CN 115160384 A CN115160384 A CN 115160384A
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China
Prior art keywords
glucose
galactose
milk
solution
producing
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CN202210791307.2A
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Chinese (zh)
Inventor
徐以泓
张宝园
董岩岩
卢丽丽
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Anhui Hegeng Bio Tech Co ltd
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Anhui Hegeng Bio Tech Co ltd
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    • CCHEMISTRY; METALLURGY
    • C07ORGANIC CHEMISTRY
    • C07HSUGARS; DERIVATIVES THEREOF; NUCLEOSIDES; NUCLEOTIDES; NUCLEIC ACIDS
    • C07H1/00Processes for the preparation of sugar derivatives
    • C07H1/06Separation; Purification
    • C07H1/08Separation; Purification from natural products
    • CCHEMISTRY; METALLURGY
    • C07ORGANIC CHEMISTRY
    • C07HSUGARS; DERIVATIVES THEREOF; NUCLEOSIDES; NUCLEOTIDES; NUCLEIC ACIDS
    • C07H3/00Compounds containing only hydrogen atoms and saccharide radicals having only carbon, hydrogen, and oxygen atoms
    • C07H3/02Monosaccharides
    • CCHEMISTRY; METALLURGY
    • C12BIOCHEMISTRY; BEER; SPIRITS; WINE; VINEGAR; MICROBIOLOGY; ENZYMOLOGY; MUTATION OR GENETIC ENGINEERING
    • C12PFERMENTATION OR ENZYME-USING PROCESSES TO SYNTHESISE A DESIRED CHEMICAL COMPOUND OR COMPOSITION OR TO SEPARATE OPTICAL ISOMERS FROM A RACEMIC MIXTURE
    • C12P19/00Preparation of compounds containing saccharide radicals
    • C12P19/02Monosaccharides
    • CCHEMISTRY; METALLURGY
    • C07ORGANIC CHEMISTRY
    • C07BGENERAL METHODS OF ORGANIC CHEMISTRY; APPARATUS THEREFOR
    • C07B2200/00Indexing scheme relating to specific properties of organic compounds
    • C07B2200/13Crystalline forms, e.g. polymorphs

Abstract

The invention discloses a method for producing galactose and glucose by taking milk as a raw material, which comprises the following steps: (1) Using protease to degrease and filter milk to prepare crude lactose liquid; (2) Hydrolyzing the crude lactose liquid under acidic and high-temperature conditions, heating and preserving heat, adding alkali for neutralization, and then filtering; (3) Carrying out decoloration, filtration and desalination treatment on the neutralized solution; (4) Concentrating and carrying out chromatographic separation on the desalted solution to obtain a galactose enrichment solution and a glucose enrichment solution; (5) Concentrating and crystallizing the galactose enrichment solution and the glucose enrichment solution respectively; (6) And respectively centrifuging, drying, crushing and packaging the crystallized galactose and glucose crude products to finally obtain high-quality galactose and glucose with the purity of more than 99%. The method provided by the invention is simple to operate, does not use an organic solvent, and does not have the food safety problem of organic solvent residue.

Description

Method for producing galactose and glucose by taking milk as raw material
Technical Field
The invention relates to the technical field of galactose production, in particular to a method for producing galactose and glucose by taking milk as a raw material.
Background
Milk is one of the oldest natural beverages, is known as 'white blood', and has imaginable importance to human bodies. Milk is expressed from female cows as the name implies. Milk is also graded differently in different countries. The milk has complex types, at least more than 100 types, and the main components of the milk comprise water, lactose, fat, phospholipid, protein, inorganic salt and the like. Lactose has low sweetness, is not easy to be absorbed and utilized by adults, is easy to crystallize and causes lactose intolerance if being directly applied to liquid dairy products to replace cane sugar or syrup, and simultaneously, lactose mineral salts, particularly sodium and potassium, have great influence on the taste and the addition of the product. If the lactose liquid is directly discharged, the lactose discharge treatment cost is high and the environmental pollution is serious because the biological oxygen demand is high.
The prior art still stays in the production of a mixture of galactose and glucose by taking milk as a raw material, and no related process for producing single products of galactose and glucose by taking milk as a raw material is found at present.
Disclosure of Invention
Aiming at the problems, the invention aims to provide a method for producing galactose and glucose by taking milk as a raw material, the production method of galactose and the product purification process relate to chromatographic separation and crystallization technologies, the method is advanced, the purity of the produced single galactose and glucose reaches over 99 percent, in addition, the solvent used by the production method is purified water, other organic solvents are not added in the whole process, and the problem of food safety risk caused by organic solvent residue is effectively avoided.
In order to realize the purpose of the invention, the invention is realized by the following technical scheme: a method for producing galactose and glucose from milk comprises the following steps:
(1) Using protease to degrease and filter milk to prepare crude lactose liquid;
(2) Hydrolyzing the crude lactose liquid under acidic and high-temperature conditions, heating and preserving heat, adding alkali for neutralization, and then filtering;
(3) Carrying out decoloration, filtration and desalination treatment on the neutralized solution;
(4) Concentrating and carrying out chromatographic separation on the desalted solution to obtain a galactose enrichment solution and a glucose enrichment solution;
(5) Concentrating and crystallizing the galactose enrichment solution and the glucose enrichment solution respectively;
(6) And respectively centrifuging, drying, crushing and packaging the crystallized galactose and glucose crude products to finally obtain high-quality galactose and glucose with the purity of more than 99%.
The further improvement lies in that: the step (1) comprises the following steps:
a. and (3) heating: adding milk into a reaction kettle, starting stirring, and heating the milk;
b. adding an enzyme: after the temperature of the milk is raised to 60 ℃, adding protease, wherein the adding amount of the protease is 1-5% of the mass of the milk;
c. degreasing: continuously stirring, keeping the temperature of the milk at 50-70 ℃, and degreasing for 1-3 hours;
d. and (3) filtering: and (3) carrying out filter pressing on the degreased milk, wherein the filter pressing equipment is a plate-and-frame filter press.
The further improvement lies in that: the acid in the step (2) is diluted phosphoric acid, the concentration of the diluted phosphoric acid is 5% -40%, and the pH value of the solution after the acid is added is 1-4.
The further improvement lies in that: in the step (2), the high temperature is 90-130 ℃, and the heat preservation time is 2-6 hours.
The further improvement is that: the alkali in the step (2) is calcium hydroxide suspension, the mass fraction of the calcium hydroxide suspension is 10-40%, and the pH value of a solution neutralized by the calcium hydroxide suspension is 3-6.
The further improvement lies in that: the wood activated carbon is adopted for decolorization in the step (3), the addition amount of the wood activated carbon is 0.5 percent of the mass of the reaction solution, the addition temperature is 50-70 ℃, and the heat preservation time is 0.5-2 hours.
The further improvement is that: and (5) concentrating the solution in the step (4), wherein the concentration of the concentrated solution is controlled to be 35-50%.
The further improvement lies in that: six serially connected chromatographic separation columns are adopted in the chromatographic separation in the step (4), the adsorption medium filled in the chromatographic separation columns is sodium type cation adsorption resin, and the used eluent is purified water.
The further improvement lies in that: in the step (5), the galactose enrichment solution is concentrated, and the concentration of the concentrated galactose enrichment solution is 60% -75%, and in the step (5), the glucose enrichment solution is concentrated, and the concentration of the concentrated glucose enrichment solution is 75% -85%.
The further improvement lies in that: the drying temperature in the step (6) is 85-95 ℃, the drying time is 2-5 hours, and the moisture of the semi-lactose and the glucose after drying is controlled below 1.0 percent.
The invention has the beneficial effects that: according to the invention, the protease is adopted to degrease the milk, so that the prepared lactose has high purity and stable crystal form, and is beneficial to subsequent hydrolysis; the invention does not use organic solvent, thus avoiding the pollution of the organic solvent to the product; the invention adopts chromatographic separation and crystallization technology to effectively separate and purify lactose hydrolysate galactose and glucose, and galactose and glucose products with high purity and good quality are obtained.
Drawings
FIG. 1 is a flow chart of the production method of the present invention.
FIG. 2 is a HPLC chart of a mixed solution after milk hydrolysis according to the present invention.
FIG. 3 is an HPLC chart of galactose as a finished product of the present invention.
FIG. 4 is an HPLC chart of the final product glucose of the present invention.
Detailed Description
In order to further understand the present invention, the following detailed description will be made with reference to the following examples, which are only used for explaining the present invention and are not to be construed as limiting the scope of the present invention.
According to fig. 1, 2 and 3, the present embodiment provides a method for producing galactose and glucose from milk, which comprises the following steps:
(1) Using protease to degrease and filter milk to prepare crude lactose liquid;
(2) Hydrolyzing the crude lactose liquid under acidic and high-temperature conditions, heating and preserving heat, adding alkali for neutralization, and then filtering;
(3) Carrying out decoloration, filtration and desalination treatment on the neutralized solution;
(4) Concentrating and carrying out chromatographic separation on the desalted solution to obtain a galactose enrichment solution and a glucose enrichment solution;
(5) Concentrating and crystallizing the galactose enrichment solution and the glucose enrichment solution respectively;
(6) And respectively centrifuging, drying, crushing and packaging the crystallized galactose and glucose crude products to finally obtain high-quality galactose and glucose with the purity of more than 99%.
Examples
Pouring milk into a reaction kettle, starting stirring of the reaction kettle at the rotation speed of 30 revolutions per minute, starting a heating device of the reaction kettle, slowly adding protease into the reaction kettle after the temperature of the milk is raised to 60 ℃, wherein the adding amount of the protease is 3% of the mass of the milk, starting timing after the protease is added, finishing milk degreasing after 2 hours, introducing the milk into a plate-and-frame filter press, collecting filtrate, and carrying out the next operation;
introducing the collected filtrate into a hydrolysis kettle, adding 30 mass percent of diluted phosphoric acid, adjusting the pH value of the solution to 2.1, hydrolyzing at the temperature of 115 ℃ for 4 hours, cooling to 80 ℃, adding 20 mass percent of calcium hydroxide suspension, adjusting the pH value to 4.5, wherein the content of galactose in the hydrolyzed milk is 47.772 percent, the content of glucose is 51.971 percent, filtering, collecting the filtrate, and carrying out the next operation;
wood activated carbon is adopted for decoloring the filtrate in the previous step, the addition amount of the wood activated carbon is 0.5 percent of the mass of the reaction solution, the addition temperature is 62 ℃, the heat preservation time is 1.5 hours, the decoloring effect is determined by testing the light transmittance of the decolored solution, and the light transmittance requirement is more than 92 percent;
enabling the decolored solution to enter an ion exchange column for desalting, enabling two ion exchange columns to be provided, enabling one ion exchange column to be an anode column, filling cation exchange resin in the anode column, enabling one ion exchange column to be an anion exchange column, filling anion exchange resin in the anion exchange column, and testing the conductivity of the desalted solution, wherein the conductivity is required to be 30 mu s/cm smaller;
evaporating and concentrating the desalted solution, wherein the concentration of the concentrated solution is 40%, then separating and removing impurities by using a program type simulated moving bed chromatographic separation device to obtain a galactose enrichment solution and a glucose enrichment solution respectively, wherein the chromatographic separation adopts six chromatographic separation columns and a program control system which are connected in series, an adsorption medium filled in the chromatographic separation columns is sodium type cation adsorption resin, and the used eluent is purified water;
carrying out evaporation concentration on the galactose enrichment solution and the glucose enrichment solution obtained after chromatographic separation respectively, wherein the concentration of the galactose enrichment solution is 65% after concentration, the concentration of the glucose enrichment solution is 82%, and the concentrated galactose enrichment solution and the concentrated glucose enrichment solution are crystallized by adopting crystallization tanks respectively;
and (3) respectively carrying out centrifugal drying on the galactose crude product and the glucose crude product by adopting a centrifugal machine, respectively collecting the dried galactose crude product and the dried glucose crude product, and then drying at the drying temperature of 94 ℃ for 3 hours, wherein the moisture content of the galactose after drying is 0.05 percent, and the moisture content of the glucose is 0.04 percent. The dried product has particles and a small amount of powder, the material is crushed by a crusher and then packaged;
the purity of the packaged galactose product is 99.877%, and the purity of the glucose product is 99717%.
The foregoing illustrates and describes the principles, general features, and advantages of the present invention. It will be understood by those skilled in the art that the present invention is not limited to the embodiments described above, which are given by way of illustration of the principles of the present invention, but that various changes and modifications may be made without departing from the spirit and scope of the invention, and such changes and modifications are within the scope of the invention as claimed. The scope of the invention is defined by the appended claims and equivalents thereof.

Claims (10)

1. A method for producing galactose and glucose by taking milk as a raw material is characterized by comprising the following steps:
(1) Using protease to degrease and filter milk to prepare crude lactose liquid;
(2) Hydrolyzing the crude lactose liquid under acidic and high-temperature conditions, heating and preserving heat, adding alkali for neutralization, and then filtering;
(3) Carrying out decoloration, filtration and desalting treatment on the neutralized solution;
(4) Concentrating and carrying out chromatographic separation on the desalted solution to obtain a galactose enrichment solution and a glucose enrichment solution;
(5) Concentrating and crystallizing the galactose enrichment solution and the glucose enrichment solution respectively;
(6) And (3) respectively centrifuging, drying, crushing and packaging the crystallized galactose and glucose crude products to finally obtain high-quality galactose and glucose with the purity of more than 99%.
2. The method for producing galactose and glucose by using milk as raw material according to claim 1, wherein the step (1) comprises the following steps:
a. and (3) heating: adding milk into a reaction kettle, starting stirring, and heating the milk;
b. adding an enzyme: after the temperature of the milk is raised to 60 ℃, adding protease, wherein the adding amount of the protease is 1-5% of the mass of the milk;
c. degreasing: continuously stirring, keeping the temperature of the milk at 50-70 ℃, and degreasing for 1-3 hours;
d. and (3) filtering: and (3) carrying out filter pressing on the degreased milk, wherein the filter pressing equipment is a plate-and-frame filter press.
3. The method for producing galactose and glucose from milk according to claim 1, wherein the acid in step (2) is diluted phosphoric acid, the concentration of diluted phosphoric acid is 5% -40%, and the pH of the solution after adding acid is 1-4.
4. The method for producing galactose and glucose from milk according to claim 1, wherein the high temperature in step (2) is 90-130 ℃ and the holding time is 2-6 hours.
5. The method for producing galactose and glucose from milk according to claim 1, wherein the base in step (2) is calcium hydroxide suspension, the mass fraction of the calcium hydroxide suspension is 10% -40%, and the pH value of the solution neutralized by calcium hydroxide suspension is 3-6.
6. The method for producing galactose and glucose by using milk as a raw material according to claim 1, wherein the wood activated carbon is used for decolorization in the step (3), the addition amount of the wood activated carbon is 0.5% of the mass of the reaction solution, the addition temperature is 50-70 ℃, and the heat preservation time is 0.5-2 hours.
7. The method for producing galactose and glucose from milk according to claim 1, wherein the concentration of the solution in step (4) is controlled to be 35% -50%.
8. The method for producing galactose and glucose from milk according to claim 1, wherein the chromatographic separation in step (4) uses six chromatographic separation columns connected in series, the adsorption medium filled in the chromatographic separation columns is sodium type cation adsorption resin, and the eluent used is purified water.
9. The method for producing galactose and glucose by using milk as a raw material according to claim 1, wherein the galactose-enriched liquid is concentrated in step (5) to a concentration of 60% -75% and the glucose-enriched liquid is concentrated in step (5) to a concentration of 75% -85%.
10. The method for producing galactose and glucose from milk according to claim 1, wherein the drying temperature in step (6) is 85-95 ℃, the drying time is 2-5 hours, and the moisture content of galactose and glucose after drying is controlled below 1.0%.
CN202210791307.2A 2022-07-07 2022-07-07 Method for producing galactose and glucose by taking milk as raw material Pending CN115160384A (en)

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN116926147A (en) * 2023-07-19 2023-10-24 安徽天凯生物科技有限公司 Method and device for preparing lactose and galacto-oligosaccharide

Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN112646847A (en) * 2019-10-12 2021-04-13 内蒙古伊利实业集团股份有限公司 Preparation method of galactose glucose mixture
CN112876520A (en) * 2021-02-07 2021-06-01 安徽禾庚生物技术有限公司 Preparation method of high-quality arabinose, galactose, rhamnose and glucuronic acid

Patent Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN112646847A (en) * 2019-10-12 2021-04-13 内蒙古伊利实业集团股份有限公司 Preparation method of galactose glucose mixture
CN112876520A (en) * 2021-02-07 2021-06-01 安徽禾庚生物技术有限公司 Preparation method of high-quality arabinose, galactose, rhamnose and glucuronic acid

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN116926147A (en) * 2023-07-19 2023-10-24 安徽天凯生物科技有限公司 Method and device for preparing lactose and galacto-oligosaccharide

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