CN119143817A - Preparation method of anhydrous lactitol crystal with controllable granularity - Google Patents
Preparation method of anhydrous lactitol crystal with controllable granularity Download PDFInfo
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- CN119143817A CN119143817A CN202411645816.XA CN202411645816A CN119143817A CN 119143817 A CN119143817 A CN 119143817A CN 202411645816 A CN202411645816 A CN 202411645816A CN 119143817 A CN119143817 A CN 119143817A
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- 229960003451 lactitol Drugs 0.000 title claims abstract description 88
- 239000000832 lactitol Substances 0.000 title claims abstract description 88
- VQHSOMBJVWLPSR-JVCRWLNRSA-N lactitol Chemical compound OC[C@H](O)[C@@H](O)[C@@H]([C@H](O)CO)O[C@@H]1O[C@H](CO)[C@H](O)[C@H](O)[C@H]1O VQHSOMBJVWLPSR-JVCRWLNRSA-N 0.000 title claims abstract description 88
- 235000010448 lactitol Nutrition 0.000 title claims abstract description 88
- 239000013078 crystal Substances 0.000 title claims abstract description 82
- 238000002360 preparation method Methods 0.000 title abstract description 18
- 238000001816 cooling Methods 0.000 claims abstract description 63
- 238000001035 drying Methods 0.000 claims abstract description 38
- 239000002245 particle Substances 0.000 claims abstract description 22
- 239000012141 concentrate Substances 0.000 claims description 14
- 238000000034 method Methods 0.000 claims description 8
- 239000000203 mixture Substances 0.000 claims 4
- 239000007788 liquid Substances 0.000 claims 1
- 238000002425 crystallisation Methods 0.000 abstract description 13
- 230000008025 crystallization Effects 0.000 abstract description 13
- 238000010438 heat treatment Methods 0.000 abstract description 11
- 238000004519 manufacturing process Methods 0.000 abstract description 8
- 238000009826 distribution Methods 0.000 abstract description 4
- 150000005846 sugar alcohols Chemical class 0.000 abstract description 4
- 230000000052 comparative effect Effects 0.000 description 12
- ZCWBZRBJSPWUPG-UHFFFAOYSA-N 4-bromo-2-nitroaniline Chemical compound NC1=CC=C(Br)C=C1[N+]([O-])=O ZCWBZRBJSPWUPG-UHFFFAOYSA-N 0.000 description 6
- 229960001159 lactitol monohydrate Drugs 0.000 description 6
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 6
- 230000000694 effects Effects 0.000 description 5
- 239000006041 probiotic Substances 0.000 description 5
- 235000018291 probiotics Nutrition 0.000 description 5
- 238000001704 evaporation Methods 0.000 description 4
- 238000007789 sealing Methods 0.000 description 4
- 230000000529 probiotic effect Effects 0.000 description 3
- 241000894006 Bacteria Species 0.000 description 2
- CZMRCDWAGMRECN-UGDNZRGBSA-N Sucrose Chemical compound O[C@H]1[C@H](O)[C@@H](CO)O[C@@]1(CO)O[C@@H]1[C@H](O)[C@@H](O)[C@H](O)[C@@H](CO)O1 CZMRCDWAGMRECN-UGDNZRGBSA-N 0.000 description 2
- 229930006000 Sucrose Natural products 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 2
- 230000008020 evaporation Effects 0.000 description 2
- 238000002844 melting Methods 0.000 description 2
- 230000008018 melting Effects 0.000 description 2
- 238000004806 packaging method and process Methods 0.000 description 2
- 239000000843 powder Substances 0.000 description 2
- 239000005720 sucrose Substances 0.000 description 2
- 206010010774 Constipation Diseases 0.000 description 1
- 238000007605 air drying Methods 0.000 description 1
- -1 alcohol monohydrate Chemical class 0.000 description 1
- 238000005119 centrifugation Methods 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 239000008187 granular material Substances 0.000 description 1
- 230000000968 intestinal effect Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 235000013406 prebiotics Nutrition 0.000 description 1
- 238000004321 preservation Methods 0.000 description 1
- 229960002920 sorbitol Drugs 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 235000019605 sweet taste sensations Nutrition 0.000 description 1
- 230000007704 transition Effects 0.000 description 1
Classifications
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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
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D9/00—Crystallisation
- B01D9/0004—Crystallisation cooling by heat exchange
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D9/00—Crystallisation
- B01D9/004—Fractional crystallisation; Fractionating or rectifying columns
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D9/00—Crystallisation
- B01D9/0063—Control or regulation
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- 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
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07B—GENERAL METHODS OF ORGANIC CHEMISTRY; APPARATUS THEREFOR
- C07B2200/00—Indexing scheme relating to specific properties of organic compounds
- C07B2200/13—Crystalline forms, e.g. polymorphs
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- Chemical & Material Sciences (AREA)
- Crystallography & Structural Chemistry (AREA)
- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Biotechnology (AREA)
- Health & Medical Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Engineering & Computer Science (AREA)
- Biochemistry (AREA)
- General Health & Medical Sciences (AREA)
- Genetics & Genomics (AREA)
- Molecular Biology (AREA)
- Thermal Sciences (AREA)
- Physics & Mathematics (AREA)
- Saccharide Compounds (AREA)
Abstract
The invention belongs to the technical field of sugar alcohol preparation, and relates to a preparation method of an anhydrous lactitol crystal with controllable granularity, which comprises the steps of taking a lactitol concentrated solution with refraction of 80-82% and temperature of 75-80 ℃ in a crystallizer, then cooling, wherein the cooling rate of the step is 0.5-1 ℃ per minute, stopping cooling when the temperature is reduced to precipitate crystals, maintaining the current temperature for 1-4 hours, then adjusting the cooling rate to 1-1.5 ℃ per minute, continuing cooling, stopping cooling when the temperature is reduced to 20-30 ℃, maintaining the current temperature for 1-3 hours to obtain massecuite, centrifuging the massecuite to obtain wet sugar, sending the wet sugar into a blast drying box, drying the wet sugar at 50-60 ℃ for 1 hour, then slowly heating to 85-90 ℃ at 5-10 ℃ per hour, slowly heating to 105-115 ℃ at 5-10 ℃ per hour after staying for 1 hour, and staying for 1 hour again to obtain the anhydrous lactitol crystal. According to the invention, the anhydrous lactitol is prepared by adopting a gradient cooling crystallization and gradient heating drying mode, so that the anhydrous lactitol crystal with controllable particle size distribution is obtained, and the production difficulty is greatly reduced.
Description
Technical Field
The invention belongs to the technical field of sugar alcohol preparation, and particularly relates to a preparation method of anhydrous lactitol crystals with controllable granularity.
Background
Lactitol (Lactitol, also known as lactitol) is white crystal or crystalline powder, has no odor and sweet taste, has sweetness of 30% -40% of sucrose, and has heat of about half of sucrose (8.4 kJ/g). The chemical nature of lactitol is 4-O-beta-D-galactopyranose-D-sorbitol, its molecular formula is C 12H24O11, molecular weight 344.32. Lactitol is an emerging prebiotic, can proliferate beneficial intestinal bacteria, inhibit harmful bacteria, and has the effects of preventing and treating constipation. The lactitol crystallization products in the current market are mainly lactitol monohydrate, and the application is influenced because of the high moisture content and high water activity of the lactitol monohydrate, and the activity of probiotics can be influenced when the lactitol crystallization products are used for the probiotics. Because of the low water activity, the anhydrous lactitol is suitable for being applied to the probiotic products, and thus, the preparation of the anhydrous lactitol is a key for developing the application of the anhydrous lactitol in the probiotic products.
At present, the preparation of the anhydrous lactitol mainly depends on evaporative crystallization, and the temperature required by the evaporative crystallization is very high due to the higher crystal form transition temperature of the anhydrous lactitol. The publication No. CN112142803A discloses an anhydrous lactitol and a preparation method thereof, and discloses that the anhydrous lactitol crystal needs to be crystallized and centrifugally separated under the condition of more than 70 ℃. The patent publication No. CN112250722A discloses a process for producing lactitol crystals, and discloses that the crystallization temperature and the centrifugation temperature of anhydrous lactitol are more required to be above 78 ℃. Although the anhydrous lactitol crystal can be obtained by crystallization under the condition of high temperature, the control requirement on the evaporation process is very high, the conveying pipeline and the centrifugal equipment are required to be kept at the temperature, the required energy consumption is high, the production risks of blockage, hardening and the like are present, on the other hand, the solubility of the lactitol under the high temperature is greatly increased, and the yield of the anhydrous lactitol crystal is reduced. In addition, the anhydrous lactitol crystal is obtained by high-temperature evaporation, so that the occurrence of hardening in the centrifugal process is often avoided as much as possible, the particle size of the anhydrous lactitol crystal needs to be controlled to be larger, the anhydrous lactitol crystal with overlarge particle size needs to be further crushed in the application of a probiotic product, the equipment cost is increased, the crushed anhydrous lactitol crystal does not have good flowability, and the problems of difficult powder conveying and the like exist in the downstream application.
Disclosure of Invention
The invention aims to solve the technical problems of providing a preparation method of anhydrous lactitol crystals with controllable granularity, which can obtain the anhydrous lactitol crystals under the controllable and mild conditions, and has the advantages of controllable granularity, higher yield and no need of further crushing.
The invention is realized in such a way, and provides a preparation method of anhydrous lactitol crystal with controllable granularity, which comprises the following steps:
Firstly, taking lactitol concentrated solution with refraction of 80-82% and temperature of 75-80 ℃ in a crystallizer, and then slowly cooling at the cooling rate of 0.5-1 ℃ per minute;
Stopping cooling when the lactitol concentrate system slowly cools to start to precipitate crystals, maintaining the current temperature for 1-4 hours, then adjusting the cooling rate to 1-1.5 ℃ per minute, and continuing cooling;
Stopping cooling when the lactitol concentrate is cooled to 20-30 ℃, and maintaining the current temperature for crystal growth for 1-3 hours to obtain massecuite;
step four, centrifuging the massecuite to obtain wet sugar;
and fifthly, sending wet sugar into a blast drying box, drying for 1h at 50-60 ℃ by hot air, slowly heating to 85-90 ℃ at 5-10 ℃ per hour, after staying for 1h, slowly heating to 105-115 ℃ at 5-10 ℃ per hour, and after staying for 1h again, taking out the dried anhydrous lactitol crystal, and sealing and storing.
Compared with the prior art, the preparation method of the anhydrous lactitol crystal with controllable granularity obtains the lactitol crystal with controllable particle size distribution by gradient regulation and control of the cooling rate before and after the crystallization point, removes crystal water at a specific temperature to preserve the crystal morphology structure by gradient heating and drying, realizes the conversion of the lactitol to the anhydrous lactitol, and obtains the anhydrous lactitol crystal with controllable particle size distribution, greatly reduces the production difficulty and has simpler production control.
Detailed Description
In order to make the technical problems, technical schemes and beneficial effects to be solved more clear, the invention is further described in detail below with reference to the embodiments. It should be understood that the specific embodiments described herein are for purposes of illustration only and are not intended to limit the scope of the invention.
The preferred embodiment of the preparation method of the anhydrous lactitol crystal with controllable granularity comprises the following steps:
Firstly, taking lactitol concentrated solution with the refraction of 80-82% and the temperature of 75-80 ℃ in a crystallizer, and then slowly cooling at the cooling rate of 0.5-1 ℃ per minute.
And secondly, stopping cooling when the lactitol concentrate system slowly cools to start to precipitate crystals, maintaining the current temperature for 1-4 hours, then adjusting the cooling rate to be 1-1.5 ℃ per minute, and continuing cooling.
And thirdly, stopping cooling when the lactitol concentrated solution is cooled to 20-30 ℃, and maintaining the current temperature for crystal growth for 1-3 hours to obtain massecuite.
And step four, centrifuging the massecuite to obtain wet sugar.
And fifthly, sending wet sugar into a blast drying box, drying for 1h at 50-60 ℃ by hot air, slowly heating to 85-90 ℃ at 5-10 ℃ per hour, after staying for 1h, slowly heating to 105-115 ℃ at 5-10 ℃ per hour, and after staying for 1h again, taking out the dried anhydrous lactitol crystal, and sealing and storing.
The preparation method adopts a gradient cooling crystallization mode to prepare the lactitol monohydrate crystal. The lactobionic alcohol monohydrate crystal with controllable granularity can be obtained by controlling the cooling process. And then carrying out gradient heating drying on the lactitol monohydrate crystal, removing crystal water at a specific temperature, and preserving the crystal morphology structure of the lactitol monohydrate crystal, thus finally obtaining the anhydrous lactitol crystal with controllable granularity.
The preparation method of the particle size-controllable anhydrous lactitol crystal according to the present invention is further described below by way of specific examples.
Example 1
A first example of the process for preparing particle size-controllable anhydrous lactitol crystals according to the invention comprises the steps of feeding 400mL of a lactitol concentrate having a refractive index of 80% and a temperature of 75 ℃ into a crystallizer and then slowly cooling at a rate of 0.5 ℃ per minute. When the temperature is reduced to 58 ℃, the system stops cooling when the system is observed to start to precipitate crystals, and the system temperature is maintained at 58 ℃ at this time, and the temperature is kept for 4 hours. Then cooling to 30 ℃ at the speed of 1 ℃ per minute, stopping cooling, and preserving heat and growing crystals for 3 hours at the temperature of 30 ℃ to obtain massecuite. Taking out the massecuite, centrifuging at 1000rpm for 3min, feeding the obtained wet sugar into a blast drying oven, drying at 60deg.C for 1 hr, gradually increasing the temperature of the blast drying oven to 85deg.C at 10 deg.C/hr, and standing at 85deg.C for 1 hr. Finally, the temperature is continuously increased to 105 ℃ at 10 ℃ per hour, and after the temperature is kept at 105 ℃ and dried for 1 hour, 237g of anhydrous lactitol crystal is obtained and stored in a sealed way.
Example 2
A second example of the process for preparing particle size-controllable anhydrous lactitol crystals according to the invention comprises the steps of feeding 400mL of a lactitol concentrate having a refractive index of 80.5% and a temperature of 75 ℃ into a crystallizer and then slowly cooling at a rate of 0.8 ℃ per minute. When the system is cooled to 55 ℃, the system stops cooling when the system is observed to start to precipitate crystals, and the temperature of the system is maintained at 55 ℃ at this time, and the temperature is kept for 1h. And then continuously cooling to 25 ℃ at the speed of 1.2 ℃ per minute, stopping cooling, and preserving the temperature at 25 ℃ for 2 hours to obtain massecuite. Taking out the massecuite, centrifuging at 1000rpm for 3min, feeding the obtained wet sugar into a blast drying oven, drying at 50 ℃ for 1h, gradually increasing the temperature of the blast drying oven to 85 ℃ at 5 ℃ per h, and staying at 85 ℃ for 1h for drying. Finally, the temperature is continuously increased to 115 ℃ at 5 ℃ per hour, and after the temperature is kept at 115 ℃ and dried for 1 hour, 242.5g of anhydrous lactitol crystal is obtained and packaged in a sealed way.
Example 3
A third example of the process for preparing anhydrous lactitol crystals of controlled particle size according to the present invention comprises the steps of feeding 400mL of a lactitol concentrate having a refractive index of 82% and a temperature of 80 ℃ into a crystallizer, and then slowly cooling at a rate of 1 ℃ per minute. When the system is cooled to 54 ℃, the system stops cooling when the system is observed to start to precipitate crystals, and the system temperature is maintained at 54 ℃ at this time, and the temperature is kept for 1h. And then continuously cooling to 20 ℃ at the speed of 1.5 ℃ per minute, stopping cooling, and preserving the temperature at 20 ℃ for 1h to obtain massecuite. Taking out the massecuite, centrifuging at 1000rpm for 3min, delivering the obtained wet sugar into a blast drying oven, drying at 60 ℃ for 1h, gradually increasing the temperature of the blast drying oven to 90 ℃ at 7.5 ℃ per h, and staying at 90 ℃ for 1h for drying. Finally, the temperature is continuously increased to 110 ℃ at 7.5 ℃ per hour, and after the temperature is kept at 110 ℃ and dried for 1 hour, 256g of anhydrous lactitol crystal is obtained for sealing packaging.
In order to further illustrate the improving effect of the production method of the present invention, a further description will be given below in conjunction with comparative examples.
Comparative example 1
The first comparative example of the preparation of anhydrous lactitol crystals in the conventional manner according to the present invention comprises the steps of feeding 400mL of a lactitol concentrate having a refractive index of 80.5% and a temperature of 75℃into a crystallizer, and slowly evaporating under vacuum conditions of 75℃to-0.08 MPa for 1h to a refractive index of 85%. Then adding 1%o and 200 meshes of anhydrous lactitol seed crystal, continuously evaporating for 4 hours, taking out massecuite, preheating a centrifuge by 90 ℃ hot water, centrifugally separating for 3 minutes by the preheated centrifuge at 2000rpm, and drying the obtained wet sugar in a 60 ℃ forced air drying box for 6 hours to obtain 196.5g of anhydrous lactitol crystal, and sealing and packaging.
Comparative example 2
A second comparative example of the preparation of anhydrous lactitol crystals according to the present invention comprises the steps of feeding 400mL of a lactitol concentrate having a refractive index of 80% and a temperature of 75℃into a crystallizer, and then cooling at a rate of 1℃per minute. When the system is cooled to 55 ℃, the system is observed to start to precipitate crystals, the cooling is stopped, and the temperature of the system is maintained at 55 ℃ and the temperature is kept for 1h. And then continuously cooling to 25 ℃ at the speed of 1 ℃ per minute, stopping cooling, and preserving the temperature at 25 ℃ for 2 hours to obtain massecuite. Taking out the massecuite, centrifuging at 1000rpm for 3min, and drying at 60deg.C for 6 hr to obtain 248g anhydrous lactitol crystal.
Comparative example 3
A third comparative example of the preparation of anhydrous lactitol crystals according to the present invention comprises the steps of feeding 400mL of lactitol concentrate having a refractive index of 81% and a temperature of 75 ℃ into a crystallizer, and then cooling at a rate of 0.8 ℃ per minute. When the system is cooled to 56 ℃, the system is observed to start to precipitate crystals, the cooling is stopped, the system temperature is maintained at 56 ℃, and the temperature is kept for 1h. And then continuously cooling to 20 ℃ at the speed of 1 ℃ per minute, stopping cooling, and preserving heat and growing crystals for 2 hours at 20 ℃ to obtain massecuite. Taking out the massecuite, centrifuging at 1000rpm for 3min, and drying at 105deg.C in a blast drying oven for 6 hr to obtain lactitol crystal which is obviously melted and hardened without granule.
Table 1 comparison of experimental results of examples and comparative examples
From the particle size data of the anhydrous lactitol crystal particles prepared in three examples in table 1, it is illustrated that the crystal products with particle sizes intensively distributed in different mesh number intervals can be obtained by controlling different cooling rates in the gradient cooling interval, when the cooling rate is lower (example 1:0.5 ℃ per minute &1 ℃ per minute), the particle sizes are intensively distributed over 40 meshes, when the cooling rate is moderate (example 2:0.8 ℃ per minute &1.2 ℃ per minute), the particle sizes are intensively distributed between 40-80 meshes, and when the cooling rate is further accelerated (example 3:1 ℃ per minute &1.5 ℃ per minute), the particle sizes are intensively distributed under 80 meshes, so that the control of the target particle sizes can be realized according to the cooling rate, and the purpose of controllable particle sizes of the prepared anhydrous lactitol crystal is realized.
From the three examples in Table 1 and the yield and moisture data of comparative example 1, it is demonstrated that the single yield of the conventional evaporative crystallization is relatively low, and that the evaporative crystallization product tends to be doped with a small amount of lactitol monohydrate due to the technical difficulties of the evaporative crystallization and the post-treatment heat preservation, and cannot be removed under the conventional drying condition, thus resulting in higher moisture content of the evaporative crystallization product than the examples using the gradient heating drying treatment of the present invention.
From the moisture data of examples 1 to 3 and comparative examples 2 to 3 in Table 1, the conventional sugar alcohol drying mode (comparative example 2:60 ℃ C., 6 h) failed to convert lactitol to anhydrous lactitol, and the moisture was very high, whereas the temperature was increased based on the conventional sugar alcohol drying mode (comparative example 3:105 ℃ C., 6 h), the melting point of lactitol was lower, crystal melting hardening occurred, and the original morphology of crystals was lost. In the embodiments 1-3, the gradient heating drying method is adopted, and on the basis of removing the water, the complete crystal structure is maintained, and the original particle size distribution is not changed.
The foregoing description of the preferred embodiments of the invention is not intended to be limiting, but rather is intended to cover all modifications, equivalents, and alternatives falling within the spirit and principles of the invention.
Claims (4)
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