CN112142803A - Anhydrous lactitol and preparation method thereof - Google Patents
Anhydrous lactitol and preparation method thereof Download PDFInfo
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- CN112142803A CN112142803A CN202011215758.9A CN202011215758A CN112142803A CN 112142803 A CN112142803 A CN 112142803A CN 202011215758 A CN202011215758 A CN 202011215758A CN 112142803 A CN112142803 A CN 112142803A
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- C07H1/00—Processes for the preparation of sugar derivatives
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07H—SUGARS; DERIVATIVES THEREOF; NUCLEOSIDES; NUCLEOTIDES; NUCLEIC ACIDS
- C07H1/00—Processes for the preparation of sugar derivatives
- C07H1/06—Separation; Purification
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- C—CHEMISTRY; METALLURGY
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- C07H—SUGARS; DERIVATIVES THEREOF; NUCLEOSIDES; NUCLEOTIDES; NUCLEIC ACIDS
- C07H15/00—Compounds containing hydrocarbon or substituted hydrocarbon radicals directly attached to hetero atoms of saccharide radicals
- C07H15/02—Acyclic radicals, not substituted by cyclic structures
- C07H15/04—Acyclic radicals, not substituted by cyclic structures attached to an oxygen atom of the saccharide radical
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Abstract
The invention provides a preparation method of anhydrous lactitol, and belongs to the technical field of lactitol preparation. The preparation method of anhydrous lactitol provided by the invention comprises the following steps: lactose reduction hydrogenation, decolorization, ion exchange, evaporation, vacuum crystallization, feed supplement crystallization, a crystallization-assisting tank and centrifugation. The anhydrous lactitol prepared by the preparation method disclosed by the invention is low in moisture content, high in melting point, low in hygroscopicity and good in product quality, and can meet more market demands.
Description
Technical Field
The invention relates to the technical field of lactitol preparation, and particularly relates to anhydrous lactitol and a preparation method thereof.
Background
Lactitol (Lactotol, also called as Lactitol) white crystal or crystalline powder, has no odor and sweet taste, the sweetness is 30-40 percent of that of cane sugar, and the calorie is about half of that of cane sugar (8.4 kJ/g). The chemical nature of lactitol is 4-O-beta-D-galactopyranose-D-sorbitol, the molecular formula of which is C12H24O11, molecular weight 344.32.
Lactitol is a new prebiotic, can proliferate intestinal beneficial bacteria, inhibit harmful bacteria, and has the effects of preventing and treating constipation. At present, the lactitol crystal product in the market is mainly monohydrate lactitol, and due to the fact that the monohydrate lactitol is high in water content and water activity, the activity of probiotics is influenced when the crystalline product is used for probiotic products, and the application is influenced. Anhydrous lactitol is suitable for application in probiotic products due to its low water activity, so the preparation of anhydrous lactitol is a key to the development of its application in probiotic products. At present, there is no method for the preparation of anhydrous lactitol.
Disclosure of Invention
The invention aims to provide a preparation method of anhydrous lactitol.
In order to achieve the above object, the present invention provides the following preparation method:
the invention provides a preparation method of anhydrous lactitol, which comprises the following steps:
(1) hydrogenation reduction of lactose: dissolving lactose in water to prepare a lactose solution, adjusting the pH value to 6.0-8.5, adding a catalyst to perform catalytic hydrogenation reaction to obtain a hydrogenated liquid;
(2) and (3) decoloring: adding activated carbon into the hydrogenated liquid for decolorization, and filtering after decolorization to obtain a lactitol filtrate;
(3) ion exchange: subjecting the lactitol filtrate to ion exchange to remove ions to obtain a lactitol purification solution;
(4) and (3) evaporation: concentrating the lactitol purified liquid through an evaporator until the concentration of solid matters in the obtained lactitol liquid is 50-65%;
(5) vacuum crystallization: adding the lactitol liquid with the solid concentration of 50-65% into a crystallization kettle, vacuum-concentrating until the solid concentration in the lactitol liquid is 78-92%, slowly heating and stirring for crystallization to obtain lactitol paste A;
(6) feeding and crystallizing: after 4-8 h of crystallization, supplementing 0.05-0.2 times of 50-65% lactitol liquid according to the addition amount of the lactitol liquid in the step (5), slowly heating and stirring for crystallization, supplementing again after 2-5h, and repeatedly supplementing for 1-4 times to obtain lactitol paste B;
(7) crystallization in a crystallization-promoting groove: mixing the lactitol syrup A and the lactitol syrup B obtained in the steps (5) and (6), putting the mixture into a preheating crystallization-assisting tank, and crystallizing at constant temperature to obtain an anhydrous lactitol mixture;
(8) centrifuging: preheating a centrifuge, putting the anhydrous lactitol mixture into the preheated centrifuge for centrifugation, and drying to obtain anhydrous lactitol.
Preferably, in the step (1), the content of solids in the lactose solution is 30-55%; the addition amount of the catalyst is 5-15% of the dry basis of the material.
Preferably, in the step (1), the temperature of the hydrogenation reaction is 100-130 ℃, and the pressure of the hydrogenation reaction is 5-13 Mpa.
Preferably, in the step (5), the vacuum degree of the vacuum concentration is-0.1 to-0.03 Mpa.
Preferably, in the step (5), the heating temperature is 70-95 ℃.
Preferably, in the step (6), the heating temperature is 70-95 ℃.
Preferably, in the step (7), the temperature of the preheating crystallization-assisting groove is 70-80 ℃, and the constant-temperature crystallization time is 2-8 h.
Preferably, in the step (8), the preheating temperature of the centrifuge is 70-80 ℃.
In addition, the present invention provides an anhydrous lactitol characterized in that the anhydrous lactitol is produced by the production method.
Preferably, the anhydrous lactitol has a moisture content of less than 1% and has a melting point of 144-150 ℃.
The invention has the beneficial effects that:
the invention provides a preparation method of anhydrous lactitol, which supplements materials in the crystallization process, thereby ensuring more sufficient crystallization. The anhydrous lactitol prepared by the method has low water content, high melting point, low hygroscopicity and good product quality, and can meet more new market requirements.
Detailed Description
In order to clearly illustrate the technical features of the present solution, the present solution is explained below by way of specific embodiments.
Example 1
(1) Preparing lactose into a solution with the solid content of 45%, adding the solution into a reaction kettle, adjusting the pH of the solution to 7.5, adjusting the temperature of the reaction kettle to 110 ℃, adding a catalyst with the material dry basis content of 10%, introducing hydrogen to the pressure of 10Mpa for hydrogenation reaction, and continuing introducing hydrogen during the reaction until the pressure of the reaction kettle is not reduced, and stopping the reaction to obtain a hydrogenated liquid;
(2) adding activated carbon into the hydrogenated liquid for decolorization, and filtering to obtain a lactitol filtrate;
(3) carrying out ion exchange on the lactitol filtrate to obtain a lactitol purified solution;
(4) primarily concentrating the purified solution by an evaporator to obtain a lactitol solution with the solid concentration of 60%;
(5) putting the obtained lactitol into a crystallization kettle for vacuum crystallization, continuously concentrating the material under the vacuum degree of-0.08 to-0.1 Mpa until the solid concentration is 83%, adding seed crystals, controlling the temperature to be 80 to 88 ℃, slowly stirring under normal pressure, controlling the vacuum degree to be-0.03 to-0.05 Mpa when the material is turbid, continuously concentrating, and keeping the sugar paste in a supersaturated state to obtain a lactitol paste A;
(6) supplementing a lactitol liquid with the temperature of 70-75 ℃ and the solid concentration of 60% after 4-8 h, wherein the supplement amount is 0.1 time of the initial lactitol liquid amount in the crystallization kettle, then continuously concentrating and crystallizing under the vacuum degree of-0.03-0.05 Mpa, keeping the temperature at 80-88 ℃, supplementing materials again after 2-5h, and supplementing materials for 4 times in total to obtain a lactitol paste B;
(7) putting the lactitol paste A and the lactitol paste B obtained in the steps (5) and (6) into a crystallization assisting groove preheated to 75 ℃ in advance, starting stirring, and continuing to grow the crystal grains for 5 hours;
(8) placing the mixture into a centrifugal machine preheated to 75 ℃ for centrifugation, and drying to obtain anhydrous lactitol crystals 1.
Example 2
(1) Preparing lactose into a solution with the solid content of 30%, adding the solution into a reaction kettle, adjusting the pH of the solution to 6.0, controlling the temperature of the reaction kettle to be 100 ℃, adding a catalyst with the material dry basis of 5%, introducing hydrogen to the pressure of 5Mpa for hydrogenation reaction, and continuing introducing hydrogen during the reaction until the pressure of the reaction kettle is not reduced, and stopping the reaction to obtain a hydrogenated liquid;
(2) adding activated carbon into the hydrogenated liquid for decolorization, and filtering to obtain a lactitol filtrate;
(3) carrying out ion exchange on the filtrate to obtain a lactitol purified solution;
(4) primarily concentrating the lactitol purified solution through an evaporator to obtain a lactitol solution with the solid concentration of 50%;
(5) putting the obtained lactitol into a crystallization kettle for vacuum crystallization, continuously concentrating the material at a vacuum degree of-0.08 to-0.1 until the solid concentration is 78%, controlling the temperature at 70 to 80 ℃ without adding seed crystals, slowly stirring at normal pressure, controlling the vacuum degree at-0.03 to-0.05 when the material is turbid, continuously concentrating, and keeping the sugar mass in a supersaturated state to obtain the lactitol paste;
(6) after 4-8 h, putting the lactitol paste obtained in the step (5) into a crystallization assisting tank preheated to 70 ℃ in advance, and starting stirring to enable the crystal grains to continue to grow for 2 h;
(8) and putting the mixture into a centrifugal machine preheated to 70 ℃ for centrifugation, and drying to obtain anhydrous lactitol crystals 2.
Example 3 (1) preparing lactose into a solution with a solid content of 55%, adding the solution into a reaction kettle, adjusting the pH of the solution to 8.0, controlling the temperature of the reaction kettle to 130 ℃, adding a catalyst with a material dry basis of 15%, introducing hydrogen to the pressure of 13Mpa to perform hydrogenation reaction, and continuing introducing hydrogen during the reaction until the pressure of the reaction kettle is not reduced, and stopping the reaction to obtain a hydrogenated liquid;
(2) adding activated carbon into the hydrogenated liquid for decolorization, and filtering to obtain a lactitol filtrate;
(3) carrying out ion exchange on the filtrate to obtain a lactitol purified solution;
(4) primarily concentrating the purified solution by an evaporator to obtain a lactitol solution with the solid concentration of 65%;
(5) putting the obtained lactitol into a crystallization kettle for vacuum crystallization, continuously concentrating the material under the vacuum degree of-0.08 to-0.1 Mpa until the solid concentration is 92%, adding seed crystals, controlling the temperature to be 88 to 95 ℃, slowly stirring under normal pressure, controlling the vacuum degree to be-0.03 to-0.05 Mpa when the material is turbid, continuously concentrating, and keeping the sugar paste in a supersaturated state to obtain a lactitol paste A;
(6) supplementing a lactitol liquid with the temperature of 70-75 ℃ and the solid concentration of 65% after 4-8 h, wherein the supplement amount is 0.2 times of the initial lactitol liquid amount in the crystallization kettle, then continuously concentrating and crystallizing under the vacuum degree of-0.03-0.05 Mpa, keeping the temperature at 80-95 ℃, supplementing materials again after 2-5h, and supplementing materials for 2 times in total to obtain a lactitol paste B;
(7) putting the lactitol paste A and the lactitol paste B obtained in the steps (5) and (6) into a crystallization assisting groove preheated to 80 ℃ in advance, starting stirring, and continuing to grow the crystal grains for 8 hours;
(8) placing the mixture into a centrifuge preheated to 80 ℃ for centrifugation, and drying to obtain anhydrous lactitol crystals 3.
Example 4
In order to examine the advantages of the anhydrous lactitol prepared by the present invention over ordinary crystalline lactitol, the present invention compared the moisture content, water activity (%), melting point and hygroscopicity of anhydrous lactitol and ordinary crystalline lactitol, and the results are shown in table 1.
TABLE 1 Difference between Anhydrous lactitol and ordinary crystalline lactitol
It can be seen from the table that the anhydrous lactitol has a lower water content, a lower water activity and a lower hygroscopicity than ordinary crystalline lactitol, and the anhydrous lactitol has a higher melting point than ordinary crystalline lactitol, so that the anhydrous lactitol prepared by the method has better quality and can meet more new market requirements.
The technical features of the present invention which are not described in the above embodiments may be implemented by or using the prior art, and are not described herein again, of course, the above description is not intended to limit the present invention, and the present invention is not limited to the above examples, and variations, modifications, additions or substitutions which may be made by those skilled in the art within the spirit and scope of the present invention should also fall within the protection scope of the present invention.
Claims (10)
1. A method for the preparation of anhydrous lactitol, comprising the steps of:
(1) hydrogenation reduction of lactose: dissolving lactose in water to prepare a lactose solution, adjusting the pH value to 6.0-8.5, adding a catalyst to perform catalytic hydrogenation reaction to obtain a hydrogenated liquid;
(2) and (3) decoloring: adding activated carbon into the hydrogenated liquid for decolorization, and filtering after decolorization to obtain a lactitol filtrate;
(3) ion exchange: subjecting the lactitol filtrate to ion exchange to remove ions to obtain a lactitol purification solution;
(4) and (3) evaporation: concentrating the lactitol liquid purified solution through an evaporator until the concentration of solid matters in the obtained lactitol liquid is 50-65%;
(5) vacuum crystallization: adding the lactitol liquid with the solid concentration of 50-65% into a crystallization kettle, vacuum-concentrating until the solid concentration in the lactitol liquid is 78-92%, slowly heating and stirring for crystallization to obtain lactitol paste A;
(6) feeding and crystallizing: after 4-8 h of crystallization, supplementing 0.05-0.2 times of 50-65% lactitol liquid according to the addition amount of the lactitol liquid in the step (5), slowly heating and stirring for crystallization, supplementing again after 2-5h, and repeatedly supplementing for 1-4 times to obtain lactitol paste B;
(7) crystallization in a crystallization-promoting groove: mixing the lactitol syrup A and the lactitol syrup B obtained in the steps (5) and (6), putting the mixture into a preheating crystallization-assisting tank, and crystallizing at constant temperature to obtain an anhydrous lactitol mixture;
(8) centrifuging: preheating a centrifuge, putting the anhydrous lactitol mixture into the preheated centrifuge for centrifugation, and drying to obtain anhydrous lactitol.
2. The process according to claim 1, wherein in the step (1), the content of solids in the lactose solution is 30 to 55%; the addition amount of the catalyst is 5-15% of the dry basis of the material.
3. The method according to claim 1, wherein in the step (1), the temperature of the hydrogenation reaction is 100 to 130 ℃, and the pressure of the hydrogenation reaction is 5 to 13 MPa.
4. The method according to claim 1, wherein in the step (5), the vacuum degree of the vacuum concentration is-0.1 to-0.03 Mpa.
5. The method according to claim 1, wherein the heating temperature in the step (5) is 70 to 95 ℃.
6. The method according to claim 1, wherein the heating temperature in the step (6) is 70 to 95 ℃.
7. The preparation method according to claim 1, wherein in the step (7), the temperature of the preheating crystallization-promoting tank is 70-80 ℃, and the constant-temperature crystallization time is 2-8 h.
8. The method according to claim 1, wherein the preheating temperature of the centrifuge in the step (8) is 70 to 80 ℃.
9. An anhydrous lactitol prepared by the method according to any one of claims 1 to 8.
10. Anhydrous lactitol according to claim 9, having a moisture content of less than 1% and a melting point of 144-150 ℃.
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| CN202011215758.9A CN112142803A (en) | 2020-11-04 | 2020-11-04 | Anhydrous lactitol and preparation method thereof |
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| CN202011215758.9A CN112142803A (en) | 2020-11-04 | 2020-11-04 | Anhydrous lactitol and preparation method thereof |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113856308A (en) * | 2021-10-28 | 2021-12-31 | 江苏先卓食品科技股份有限公司 | Purifier of lactitol production usefulness |
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| CN103980329A (en) * | 2014-05-29 | 2014-08-13 | 山东绿健生物技术有限公司 | Method for preparing crystalline lactitol |
| CN106260387A (en) * | 2016-08-26 | 2017-01-04 | 山东绿健生物技术有限公司 | A kind of low-yield functional hard candy |
| CN110818752A (en) * | 2019-12-03 | 2020-02-21 | 山东福田药业有限公司 | Process for producing lactitol |
| CN112250722A (en) * | 2020-10-28 | 2021-01-22 | 何定兵 | Production process of lactitol crystal |
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- 2020-11-04 CN CN202011215758.9A patent/CN112142803A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN103980329A (en) * | 2014-05-29 | 2014-08-13 | 山东绿健生物技术有限公司 | Method for preparing crystalline lactitol |
| CN106260387A (en) * | 2016-08-26 | 2017-01-04 | 山东绿健生物技术有限公司 | A kind of low-yield functional hard candy |
| CN110818752A (en) * | 2019-12-03 | 2020-02-21 | 山东福田药业有限公司 | Process for producing lactitol |
| CN112250722A (en) * | 2020-10-28 | 2021-01-22 | 何定兵 | Production process of lactitol crystal |
Non-Patent Citations (1)
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| 黄亚东等: "《生物工程设备及操作技术》", 30 September 2014 * |
Cited By (1)
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| CN113856308A (en) * | 2021-10-28 | 2021-12-31 | 江苏先卓食品科技股份有限公司 | Purifier of lactitol production usefulness |
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