CN114349802A - Production method of plant source D-tagatose - Google Patents
Production method of plant source D-tagatose Download PDFInfo
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- CN114349802A CN114349802A CN202111493409.8A CN202111493409A CN114349802A CN 114349802 A CN114349802 A CN 114349802A CN 202111493409 A CN202111493409 A CN 202111493409A CN 114349802 A CN114349802 A CN 114349802A
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Abstract
The invention discloses a production method of plant source D-tagatose, which comprises the steps of taking plant secretion Arabic gum as a raw material, and preparing the D-tagatose through the processes of sol, filtration, hydrolysis, isomerization, neutralization, decolorization, secondary filtration, concentration, chromatographic separation, secondary decolorization, tertiary filtration, desalting, secondary concentration, crystallization, centrifugation and drying, and specifically comprises the steps of sol filtration, hydrolysis processing, isomerization processing, secondary filtration after neutralization reaction and decolorization processing, step four, chromatographic separation, step five, secondary decolorization and filtration desalting, step six, concentration and crystallization, and step seven, centrifugal drying; the method has simple steps, greatly improves the utilization rate of equipment, saves the working time, reduces the loss of materials, collects the byproducts D-galactose, L-arabinose, L-rhamnose and D-glucuronic acid with high value, can realize industrial production and has higher economic value.
Description
Technical Field
The invention relates to the technical field of D-tagatose production, in particular to a production method of plant source D-tagatose.
Background
Acacia gum is also called arabic gum, mainly produced from natural plant gum in African semi-desert zone, and is made by drying gum exudate of trunk or branch of Acacia tree of African Leguminosae or similar tree species, acacia gum is a carbohydrate polymer, can be partially degraded in large intestine, can supplement cellulose for human body, has energy value less than half compared with starch and maltodextrin, and can obtain L-arabinose, D-galactose, L-rhamnose, D-glucuronic acid and other heterosugar mixture after hydrolysis of polysaccharide in acacia gum;
at present, most of raw materials for producing the D-tagatose by the traditional process are from animal sources, lactose or whey is used as the raw material for producing the animal source D-tagatose, the steps of the existing D-tagatose production process are fuzzy, product separation of some chemical reactions is not described in detail, and the purity of the produced D-tagatose is low, so that the invention provides the production method of the plant source D-tagatose to solve the problems in the prior art.
Disclosure of Invention
In view of the above problems, the present invention is directed to a method for producing plant-derived D-tagatose, which has simple steps, greatly improves the utilization rate of equipment, simultaneously saves working time and reduces material loss, and collects highly valuable byproducts D-galactose, L-arabinose, L-rhamnose and D-glucuronic acid, thereby realizing industrial production and having high economic value.
In order to realize the purpose of the invention, the invention is realized by the following technical scheme: a production method of plant source D-tagatose comprises the steps of taking plant secretion Arabic gum as a raw material, and preparing the D-tagatose through the processes of sol, filtration, hydrolysis, isomerization, neutralization, decoloration, secondary filtration, concentration, chromatographic separation, secondary decoloration, tertiary filtration, desalination, secondary concentration, crystallization, centrifugation and drying.
A production method of plant source D-tagatose comprises the following steps:
step one, dissolving arabic gum in purified water, and then filtering to obtain a arabic gum solution, wherein the mass percentage concentration of the arabic gum is controlled to be 30-40%;
step two, introducing the Arabic gum solution into a hydrolysis tank, adding dilute sulfuric acid for hydrolysis, and obtaining a hydrolysis solution with the concentration of 30-40% after the hydrolysis reaction is finished;
adding the hydrolysate into calcium hydroxide slurry for isomerization reaction, adding dilute sulfuric acid for neutralization reaction, adding active carbon for decolorization, performing secondary filtration on the decolorized material by using a plate-and-frame filter press, and concentrating to obtain an isomerization solution with the concentration of 40-50%;
step four, performing chromatographic separation and impurity removal on the concentrated heterogeneous liquid by using a chromatographic separation device to obtain a liquid rich in D-tagatose, D-galactose liquid, L-arabinose liquid, L-rhamnose liquid and D-glucuronic acid liquid;
step five, adding activated carbon into the D-tagatose-rich liquid obtained by separation and collection in the step four for secondary decolorization, performing tertiary filtration by adopting a rod filter, and then desalting;
step six, carrying out secondary concentration on the D-tagatose-rich liquid after desalting, and introducing the D-tagatose-rich liquid into a crystallizing tank for gradient cooling crystallization;
step seven, centrifuging and drying the crystallization liquid obtained in the step six to obtain a high-content D-tagatose finished product;
and step eight, respectively carrying out decoloring, filtering, desalting, concentrating, crystallizing, centrifuging and drying on the D-galactose liquid, the L-arabinose liquid, the L-rhamnose liquid and the D-glucuronic acid liquid collected in the step four to obtain high-quality byproducts D-galactose, L-arabinose, L-rhamnose and D-glucuronic acid for producing the D-tagatose.
The further improvement lies in that: in the second step, the pH value of the dilute sulfuric acid for the hydrolysis reaction is adjusted to be 0.5-3.0, and the temperature is raised to 100 ℃ and 150 ℃ for reaction for 2-6 hours.
The further improvement lies in that: the mass ratio of the isomerization reaction hydrolysate to the calcium hydroxide in the third step is 5-20: 1; the isomerization reaction is controlled at 10-30 deg.C for 2-4 hr, and the neutralization reaction is controlled at pH 3.0-7.0.
The further improvement lies in that: the chromatographic separation device in the fourth step is a program type simulated moving bed chromatographic separation device, and comprises 6 chromatographic separation columns, wherein the separation temperature is 40-60 ℃, the chromatographic separation columns are filled with calcium type cation adsorption resin, and the eluent is purified water.
The further improvement lies in that: and when the secondary decolorization is carried out in the fifth step, the decolorization temperature is controlled to be 60-80 ℃, and the decolorization time is 15-30 minutes.
The further improvement lies in that: the hydrolysis process of the second step and the isomerization, neutralization and decoloration processes of the third step are all completed in the same reaction kettle.
The invention has the beneficial effects that: the method has simple steps, greatly improves the utilization rate of equipment, saves the working time, reduces the loss of materials, collects the byproducts D-galactose, L-arabinose, L-rhamnose and D-glucuronic acid with high value, can realize industrial production and has higher economic value.
Drawings
FIG. 1 is a flow chart of the production method of the present invention.
FIG. 2 is an HPLC chart of a hydrolysate after the gum arabic is hydrolyzed.
FIG. 3 is a HPLC chart of the mixture liquid after the isomerization of the hydrolysate.
FIG. 4 is an HPLC chart of the finished D-tagatose 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.
Example one
According to fig. 1, the present embodiment provides a method for producing plant-derived D-tagatose, which comprises preparing D-tagatose from acacia, which is a plant secretion, by sol-gel, filtration, hydrolysis, isomerization, neutralization, decolorization, secondary filtration, concentration, chromatographic separation, secondary decolorization, tertiary filtration, desalination, secondary concentration, crystallization, centrifugation and drying.
A production method of plant source D-tagatose comprises the following steps:
step one, dissolving arabic gum in purified water, and then filtering to obtain a arabic gum solution, wherein the mass percentage concentration of the arabic gum is controlled to be 30-40%;
step two, introducing the Arabic gum solution into a hydrolysis tank, adding dilute sulfuric acid for hydrolysis, adjusting the pH value to 0.5-3.0 by dilute sulfuric acid in the hydrolysis reaction, heating to 100-150 ℃, reacting for 2-6 hours, and obtaining hydrolysate with the concentration of 30-40% after the hydrolysis reaction is finished;
adding the hydrolysate into the calcium hydroxide slurry for isomerization reaction, wherein the mass ratio of the hydrolysate to the calcium hydroxide is (5-20): 1, controlling the reaction temperature of isomerization reaction to be 10-30 ℃, reacting for 2-4 hours, adding dilute sulfuric acid for neutralization reaction, controlling the pH value to be 3.0-7.0, adding activated carbon for decolorization, performing secondary filtration on the decolorized material by using a plate-and-frame filter press, and concentrating to obtain an isomerization solution with the concentration of 40-50%;
performing chromatographic separation and impurity removal on the concentrated heterogeneous liquid by using a chromatographic separation device to obtain a liquid rich in D-tagatose, D-galactose liquid, L-arabinose liquid, L-rhamnose liquid and D-glucuronic acid liquid, wherein the chromatographic separation device is a program simulated moving bed chromatographic separation device and comprises 6 chromatographic separation columns, the separation temperature is 40-60 ℃, the chromatographic separation columns are filled with calcium type cation adsorption resin, and the eluent is purified water;
step five, adding activated carbon into the D-tagatose-rich liquid obtained by separation and collection in the step four for secondary decolorization, controlling the decolorization temperature at 60-80 ℃, carrying out the decolorization for 15-30 minutes, carrying out tertiary filtration by adopting a rod filter, and then carrying out desalination;
step six, carrying out secondary concentration on the D-tagatose-rich liquid after desalting, and introducing the D-tagatose-rich liquid into a crystallizing tank for gradient cooling crystallization;
step seven, centrifuging and drying the crystallization liquid obtained in the step six to obtain a high-content D-tagatose finished product;
and step eight, respectively carrying out decoloring, filtering, desalting, concentrating, crystallizing, centrifuging and drying on the D-galactose liquid, the L-arabinose liquid, the L-rhamnose liquid and the D-glucuronic acid liquid collected in the step four to obtain high-quality byproducts D-galactose, L-arabinose, L-rhamnose and D-glucuronic acid for producing the D-tagatose.
The hydrolysis process of the second step and the isomerization, neutralization and decoloration processes of the third step are all completed in the same reaction kettle.
Example two
According to the drawings shown in fig. 1, 2, 3 and 4, the embodiment provides a production method of plant source D-tagatose, which specifically comprises the following steps:
1. preparing hydrolysate, adding 750KG purified water into 500KG Arabic gum for dissolving, filtering to obtain the concentration of Arabic gum solution of 35%, adding 10% dilute sulfuric acid, adjusting the pH value to 1.2, hydrolyzing at 105 ℃ for 5 hours to obtain a mixed sugar solution containing L-arabinose, D-galactose, L-rhamnose and D-glucuronic acid, and detecting the mixed sugar solution by a High Performance Liquid Chromatography (HPLC), wherein the content of D-galactose is 42.435%, and the detection result of HPLC is shown in the attached figure 2 of the specification.
2. Preparing D-tagatose isomerous liquid, after hydrolysis reaction, adding 170KG calcium hydroxide, mixing and stirring in a reaction kettle, controlling the temperature to be 22 ℃, after reaction time is 2 hours, adding dilute sulfuric acid, adjusting the pH value to be 5.4 to obtain a mixed liquid containing D-tagatose, L-arabinose, D-galactose, L-rhamnose and D-glucuronic acid, and detecting the mixed liquid by a High Performance Liquid Chromatograph (HPLC), wherein the content of D-tagatose is 29.354%, and the detection result of HPLC is shown in figure 3 of the specification.
3. Separating and purifying the D-tagatose, and S1, concentrating the mixed solution obtained in the step 2, wherein the concentration of the concentrated material is 45%; s2, separating the concentrated mixed solution by using a sequential simulated moving bed chromatographic separation device, wherein 6 chromatographic columns are provided, calcium type cation adsorption resin is filled in the chromatographic columns, purified water is used as an eluent, the mixed solution and the purified water are heated to 50 ℃, and are separated in the chromatographic separation device to obtain a solution rich in D-tagatose, the content of the D-tagatose in the solution is 85%, and simultaneously, a D-galactose solution with the content of 65%, an L-rhamnose solution with the content of 60%, an L-arabinose solution with the content of 75%, a D-glucuronic acid solution with the content of 60% and a small amount of ionic liquid are obtained; s3, concentrating the solution rich in D-tagatose, cooling and crystallizing the concentrated solution rich in D-tagatose in a crystallizing tank, centrifuging the crystallized material in a centrifuge, collecting the centrifuged semi-finished product of D-tagatose, drying the semi-finished product of D-tagatose, and packaging the finished product of D-tagatose after drying, wherein the content of the finished product of D-tagatose is 99.832%, and the HPLC detection result is shown in the attached figure 4 of the specification; s4, carrying out operations of decoloring, filtering, desalting, concentrating, crystallizing, centrifuging and drying on the D-galactose liquid, the L-arabinose liquid, the L-rhamnose liquid and the D-glucuronic acid liquid collected in the S2 respectively to obtain high-quality byproducts D-galactose, L-arabinose, L-rhamnose and D-glucuronic acid for producing the D-tagatose.
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 described in the specification and illustrated only to illustrate the principle of the present invention, but that various changes and modifications may be made therein without departing from the spirit and scope of the present invention, which fall within the scope of the invention as claimed. The scope of the invention is defined by the appended claims and equivalents thereof.
Claims (7)
1. A production method of plant source D-tagatose is characterized in that: the preparation method comprises the steps of taking plant secretion Arabic gum as a raw material, and preparing the D-tagatose through the processes of sol, filtration, hydrolysis, isomerization, neutralization, decoloration, secondary filtration, concentration, chromatographic separation, secondary decoloration, tertiary filtration, desalination, secondary concentration, crystallization, centrifugation and drying.
2. The method for producing D-tagatose of plant origin according to claim 1, comprising the steps of:
step one, dissolving arabic gum in purified water, and then filtering to obtain a arabic gum solution, wherein the mass percentage concentration of the arabic gum is controlled to be 30-40%;
step two, introducing the Arabic gum solution into a hydrolysis tank, adding dilute sulfuric acid for hydrolysis, and obtaining a hydrolysis solution with the concentration of 30-40% after the hydrolysis reaction is finished;
adding the hydrolysate into calcium hydroxide slurry for isomerization reaction, adding dilute sulfuric acid for neutralization reaction, adding active carbon for decolorization, performing secondary filtration on the decolorized material by using a plate-and-frame filter press, and concentrating to obtain an isomerization solution with the concentration of 40-50%;
step four, performing chromatographic separation and impurity removal on the concentrated heterogeneous liquid by using a chromatographic separation device to obtain a liquid rich in D-tagatose, D-galactose liquid, L-arabinose liquid, L-rhamnose liquid and D-glucuronic acid liquid;
step five, adding activated carbon into the D-tagatose-rich liquid obtained by separation and collection in the step four for secondary decolorization, performing tertiary filtration by adopting a rod filter, and then desalting;
step six, carrying out secondary concentration on the D-tagatose-rich liquid after desalting, and introducing the D-tagatose-rich liquid into a crystallizing tank for gradient cooling crystallization;
step seven, centrifuging and drying the crystallization liquid obtained in the step six to obtain a high-content D-tagatose finished product;
and step eight, respectively carrying out decoloring, filtering, desalting, concentrating, crystallizing, centrifuging and drying on the D-galactose liquid, the L-arabinose liquid, the L-rhamnose liquid and the D-glucuronic acid liquid collected in the step four to obtain high-quality byproducts D-galactose, L-arabinose, L-rhamnose and D-glucuronic acid for producing the D-tagatose.
3. The method for producing D-tagatose from a plant source according to claim 1, wherein: in the second step, the pH value of the dilute sulfuric acid for the hydrolysis reaction is adjusted to be 0.5-3.0, and the temperature is raised to 100 ℃ and 150 ℃ for reaction for 2-6 hours.
4. The method for producing D-tagatose from a plant source according to claim 1, wherein: the mass ratio of the isomerization reaction hydrolysate to the calcium hydroxide in the third step is 5-20: 1; the isomerization reaction is controlled at 10-30 deg.C for 2-4 hr, and the neutralization reaction is controlled at pH 3.0-7.0.
5. The method for producing D-tagatose from a plant source according to claim 1, wherein: the chromatographic separation device in the fourth step is a program type simulated moving bed chromatographic separation device, and comprises 6 chromatographic separation columns, wherein the separation temperature is 40-60 ℃, the chromatographic separation columns are filled with calcium type cation adsorption resin, and the eluent is purified water.
6. The method for producing D-tagatose from a plant source according to claim 1, wherein: and when the secondary decolorization is carried out in the fifth step, the decolorization temperature is controlled to be 60-80 ℃, and the decolorization time is 15-30 minutes.
7. The method for producing D-tagatose from a plant source according to claim 1, wherein: the hydrolysis process of the second step and the isomerization, neutralization and decoloration processes of the third step are all completed in the same reaction kettle.
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Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN102876752A (en) * | 2012-09-07 | 2013-01-16 | 山东绿健生物技术有限公司 | Production method for crystalline tagatose |
| CN103025894A (en) * | 2010-06-02 | 2013-04-03 | 无锡甘泉医药科技有限公司 | Process for manufacturing tagatose and glucose |
| CN109384820A (en) * | 2017-08-10 | 2019-02-26 | 南京凯通粮食生化研究设计有限公司 | The method for preparing arabinose, galactolipin, rhamnose and glucuronic acid |
| CN112708702A (en) * | 2021-02-07 | 2021-04-27 | 安徽禾庚生物技术有限公司 | Method for producing plant source D-tagatose |
| 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 |
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- 2021-12-08 CN CN202111493409.8A patent/CN114349802A/en active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103025894A (en) * | 2010-06-02 | 2013-04-03 | 无锡甘泉医药科技有限公司 | Process for manufacturing tagatose and glucose |
| CN102876752A (en) * | 2012-09-07 | 2013-01-16 | 山东绿健生物技术有限公司 | Production method for crystalline tagatose |
| CN109384820A (en) * | 2017-08-10 | 2019-02-26 | 南京凯通粮食生化研究设计有限公司 | The method for preparing arabinose, galactolipin, rhamnose and glucuronic acid |
| CN112708702A (en) * | 2021-02-07 | 2021-04-27 | 安徽禾庚生物技术有限公司 | Method for producing plant source D-tagatose |
| 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 |
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