CN116063158B - Induction nucleation crystallization method for improving anti-caking performance of xylitol - Google Patents
Induction nucleation crystallization method for improving anti-caking performance of xylitol Download PDFInfo
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- CN116063158B CN116063158B CN202211628448.9A CN202211628448A CN116063158B CN 116063158 B CN116063158 B CN 116063158B CN 202211628448 A CN202211628448 A CN 202211628448A CN 116063158 B CN116063158 B CN 116063158B
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- TVXBFESIOXBWNM-UHFFFAOYSA-N Xylitol Natural products OCCC(O)C(O)C(O)CCO TVXBFESIOXBWNM-UHFFFAOYSA-N 0.000 title claims abstract description 84
- HEBKCHPVOIAQTA-UHFFFAOYSA-N meso ribitol Natural products OCC(O)C(O)C(O)CO HEBKCHPVOIAQTA-UHFFFAOYSA-N 0.000 title claims abstract description 84
- HEBKCHPVOIAQTA-SCDXWVJYSA-N xylitol Chemical compound OC[C@H](O)[C@@H](O)[C@H](O)CO HEBKCHPVOIAQTA-SCDXWVJYSA-N 0.000 title claims abstract description 84
- 229960002675 xylitol Drugs 0.000 title claims abstract description 84
- 235000010447 xylitol Nutrition 0.000 title claims abstract description 84
- 239000000811 xylitol Substances 0.000 title claims abstract description 84
- 238000002425 crystallisation Methods 0.000 title claims abstract description 59
- 238000010899 nucleation Methods 0.000 title claims abstract description 18
- 230000006911 nucleation Effects 0.000 title claims abstract description 18
- 230000006698 induction Effects 0.000 title description 3
- 239000013078 crystal Substances 0.000 claims abstract description 97
- 230000008025 crystallization Effects 0.000 claims abstract description 52
- 238000000034 method Methods 0.000 claims abstract description 30
- 238000001816 cooling Methods 0.000 claims abstract description 28
- 238000001035 drying Methods 0.000 claims abstract description 12
- 238000010438 heat treatment Methods 0.000 claims abstract description 8
- 230000000630 rising effect Effects 0.000 claims abstract description 4
- 230000001939 inductive effect Effects 0.000 claims description 10
- 150000005846 sugar alcohols Chemical class 0.000 abstract description 2
- 239000002245 particle Substances 0.000 description 22
- 238000003921 particle size analysis Methods 0.000 description 8
- 230000008569 process Effects 0.000 description 8
- 230000000052 comparative effect Effects 0.000 description 7
- 238000009826 distribution Methods 0.000 description 7
- 238000005054 agglomeration Methods 0.000 description 3
- 230000002776 aggregation Effects 0.000 description 3
- 238000009835 boiling Methods 0.000 description 2
- 229910003460 diamond Inorganic materials 0.000 description 2
- 239000010432 diamond Substances 0.000 description 2
- 238000001704 evaporation Methods 0.000 description 2
- 230000008020 evaporation Effects 0.000 description 2
- 239000002994 raw material Substances 0.000 description 2
- 239000000654 additive Substances 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000005119 centrifugation Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000005984 hydrogenation reaction Methods 0.000 description 1
- 230000007062 hydrolysis Effects 0.000 description 1
- 238000006460 hydrolysis reaction Methods 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 238000005342 ion exchange Methods 0.000 description 1
- 230000001788 irregular Effects 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 230000001376 precipitating effect Effects 0.000 description 1
- 238000001556 precipitation Methods 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 238000011112 process operation Methods 0.000 description 1
- 230000003746 surface roughness Effects 0.000 description 1
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C29/00—Preparation of compounds having hydroxy or O-metal groups bound to a carbon atom not belonging to a six-membered aromatic ring
- C07C29/74—Separation; Purification; Use of additives, e.g. for stabilisation
- C07C29/76—Separation; Purification; Use of additives, e.g. for stabilisation by physical treatment
- C07C29/78—Separation; Purification; Use of additives, e.g. for stabilisation by physical treatment by condensation or crystallisation
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- Crystallography & Structural Chemistry (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The invention belongs to the technical field of sugar alcohol, and relates to an induced nucleation crystallization method for improving anti-caking performance of xylitol, which comprises the following steps: step one, taking 250ml xylitol concentrated solution with 80-84% of refraction and 80-90 ℃ in a crystallizer, and then slowly cooling at the cooling rate of 0.1-0.4 ℃/min. Step two, when the xylitol concentrated solution is slowly cooled to the point that crystals are just precipitated in the system, different heating rates are set to induce the system to perform first crystallization to prepare crystal nuclei, so that the system is heated to 72-76 ℃, and the step meets the following requirements: the temperature rising rate is 0.2-0.5 ℃/min. And thirdly, maintaining the constant temperature of the system for 30min after the temperature is raised to 72-76 ℃, slowly cooling to 60-65 ℃ and performing secondary crystallization to obtain massecuite, wherein the cooling rate of the step is 0.05-0.1 ℃/min. And fourthly, centrifuging the massecuite, and drying at the temperature of 40-80 ℃ for 8-12 hours to finally obtain xylitol crystals. The method can prepare xylitol crystals with large average grain diameter, smooth crystal surface and stronger anti-caking property.
Description
Technical Field
The invention belongs to the technical field of sugar alcohol, and particularly relates to an induced nucleation crystallization method for improving anti-caking performance of xylitol.
Background
The existing xylitol production process takes corncobs as raw materials, and prepares xylitol crystals through the steps of hydrolysis, hydrogenation, decoloration, ion exchange, concentration, crystallization, centrifugation, drying and the like, wherein the crystallization process is a key for determining the quality and yield of xylitol products, and plays a role in determining the morphology, purity, bulk density, particle size distribution and the like of the crystalline products.
The thrust of xylitol crystallization process mainly comes from thermodynamic non-equilibrium characteristic of crystallization system, and the crystallization thermodynamic properties of solubility, metastable zone and induction period have great influence on the selection of crystallization mode and crystallization yield. The existing crystallization modes commonly used in industry comprise evaporation crystallization and cooling crystallization, and the evaporation crystallization and the cooling crystallization are well applied to the crystallization process of xylitol due to the high solubility of xylitol. According to the method, the system is stimulated to nucleate by adding the seed crystal, and then the vacuum degree of the system is maintained between-0.08 and-0.1 MPa while feeding is carried out, so that the system is in a boiling state, and crystals are continuously grown in the boiling concentration process. The patent with publication No. CN1736970A proposes a xylitol cooling crystallization method with crystal seed, which is to slowly cool 85-92% of xylitol raw material liquid, add crystal seed between 55-70 ℃ to control xylitol crystallization nucleation, and finally prepare xylitol crystal with high purity and large granularity.
However, whether it is evaporative crystallization or cooling crystallization, due to unreasonable process operation parameters or the fact that the seed crystal is added empirically, the adding temperature of the seed crystal, the amount of the seed crystal and the granularity of the seed crystal lack theoretical and practical basis, so that the xylitol crystallization process consumes long time, has low yield, occupies higher fine powder, has larger product difference among different batches, and finally leads to easy agglomeration of xylitol products. Although effective in alleviating crystal caking by the addition of anti-caking additives, this approach is generally not allowed in the relevant standards. Therefore, the method is one of important measures for avoiding or relieving the agglomeration of xylitol crystals by optimizing crystallization process parameters and controlling the particle size distribution of the product.
Disclosure of Invention
The invention aims to solve the technical problem of providing the method for inducing nucleation and crystallization for improving the anti-caking performance of xylitol, which can prepare xylitol crystals with large average grain diameter, smooth crystal surface and stronger anti-caking performance.
The invention is realized in this way, and provides an induced nucleation crystallization method for improving the anti-caking property of xylitol, which comprises the following steps:
Step one, taking 250ml xylitol concentrated solution with 80-84% of refraction and 80-90 ℃ in a crystallizer, and then slowly cooling at the cooling rate of 0.1-0.4 ℃/min.
Step two, when the xylitol concentrated solution is slowly cooled to the point that crystals are just precipitated in the system, different heating rates are set to induce the system to perform first crystallization to prepare crystal nuclei, so that the system is heated to 72-76 ℃, and the step meets the following requirements: the temperature rising rate is 0.2-0.5 ℃/min.
And thirdly, maintaining the constant temperature of the system for 30min after the temperature is raised to 72-76 ℃, slowly cooling to 60-65 ℃ and performing secondary crystallization to obtain massecuite, wherein the cooling rate of the step is 0.05-0.1 ℃/min.
And fourthly, centrifuging the massecuite, and drying at the temperature of 40-80 ℃ for 8-12 hours to finally obtain xylitol crystals.
In the cooling process, when the crystallization system just separates out crystals, heating operation is set to induce the system to crystallize for the first time to prepare crystal nuclei, so that a large number of fine crystals are prevented from being generated; compared with the existing method for keeping the system at constant temperature after crystal precipitation, the method can ensure that the crystal system consumes supersaturation in a crystal growth mode, thereby achieving the aim of preparing xylitol crystals with stronger anti-caking performance.
Compared with the prior art, the method for inducing nucleation and crystallization for improving the anti-caking performance of xylitol provided by the invention has the advantages that after crystals are precipitated in a crystallization system, the system is induced to prepare crystal nuclei for the first crystallization by setting a heating operation, so that on one hand, the system is prevented from spontaneously precipitating more crystals, and on the other hand, part of fine crystals can be dissolved to control the quantity of the crystal nuclei, and the principle is mainly that the supersaturation degree of the system is consumed through crystal growth instead of nucleation. The xylitol crystal prepared by the method has larger average particle size, the surface of the crystal is smooth and regular, and the fluidity and the anti-caking performance are obviously improved.
Drawings
FIG. 1 is a schematic view showing a microscopic image of the grain habit of xylitol crystals obtained by the preparation of example 1.
FIG. 2 is a schematic view of microscopic images of the grain habit of xylitol crystals prepared in example 2.
FIG. 3 is a schematic view of microscopic images of the grain habit of xylitol crystals prepared in example 3.
FIG. 4 is a schematic diagram of microscopic images of the grain habit of xylitol crystals prepared in comparative example.
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 method for inducing nucleation and crystallization for improving the anti-caking property of xylitol comprises the following steps:
Step one, taking 250ml xylitol concentrated solution with 80-84% of refraction and 80-90 ℃ in a crystallizer, and then slowly cooling at the cooling rate of 0.1-0.4 ℃/min.
Step two, when the xylitol concentrated solution is slowly cooled to the point that crystals are just precipitated in the system, different heating rates are set to induce the system to prepare crystal nuclei by first crystallization, so that the system is heated to 72-76 ℃ in a short time, and the following requirements are met: the temperature rising rate is 0.2-0.5 ℃/min.
And thirdly, maintaining the constant temperature of the system for 30min after the temperature is raised to 72-76 ℃, slowly cooling to 60-65 ℃ and performing secondary crystallization to obtain massecuite, wherein the cooling rate of the step is 0.05-0.1 ℃/min.
And step four, centrifuging the massecuite obtained in the step three, and drying for 8-12 hours at the temperature of 40-80 ℃ to finally obtain xylitol crystals.
The method for inducing nucleation and crystallization to improve the anti-blocking property of xylitol according to the present invention is further illustrated by the following specific examples.
Example 1
The first embodiment of the method for inducing nucleation and crystallization for improving the anti-caking property of xylitol of the present invention comprises the following steps: 250ml of xylitol concentrated solution with 82% of refraction and 85 ℃ of temperature is fed into a crystallizer, and then the temperature is slowly reduced at the speed of 0.3 ℃/min; when the system is cooled to 66.5 ℃, the system is observed to start to precipitate crystals, at the moment, the system is set to heat to 75 ℃ at the speed of 0.45 ℃/min for the first time to crystallize to prepare crystal nuclei, and the constant temperature is maintained for 30min at 75 ℃; then cooling to 65 ℃ at the speed of 0.067 ℃/min for the second crystallization to obtain massecuite; and finally taking out the massecuite obtained by crystallization, centrifugally separating for 3min at 1000rpm by using a centrifugal machine, and drying at 60 ℃ for 12h to obtain xylitol crystals.
According to the particle size analysis method, the xylitol crystals prepared in this example were subjected to particle size analysis, and the crystal habit of the xylitol crystals was observed under a polarizing microscope, the particle size distribution results are shown in table 1, and the particle habit is shown in fig. 1. The prepared xylitol crystals have regular and smooth surfaces, no phenomenon that fine crystals are attached to the surfaces of large particles, and larger average particle size. The anti-blocking strength of the xylitol crystals prepared in this example was measured to be 23g.
Example 2
The second embodiment of the method for inducing nucleation and crystallization for improving the anti-caking property of xylitol of the present invention comprises the steps of: 250ml of xylitol concentrated solution with 82% of refraction and 85 ℃ of temperature is fed into a crystallizer, and then the temperature is slowly reduced at the speed of 0.3 ℃/min; when the system is cooled to 66.5 ℃, the system is observed to start to precipitate crystals, at the moment, the system is set to heat to 75 ℃ at the speed of 0.34 ℃/min for the first time to crystallize to prepare crystal nuclei, and the constant temperature is maintained for 30min at 75 ℃; then cooling to 65 ℃ at the speed of 0.067 ℃/min for the second crystallization to obtain massecuite; and finally taking out the massecuite obtained by crystallization, centrifugally separating for 2min at 1200rpm by using a centrifugal machine, and drying at 60 ℃ for 12h to obtain xylitol crystals.
According to the particle size analysis method, the xylitol crystals prepared in this example were subjected to particle size analysis, and the crystal habit of the xylitol crystals was observed under a polarizing microscope, the particle size distribution results are shown in table 1, and the particle habit is shown in fig. 2. The prepared xylitol crystal has smooth surface and regular diamond shape. The anti-blocking strength of the xylitol crystals prepared in this example was measured to be 24g.
Example 3
The third embodiment of the method for inducing nucleation and crystallization for improving the anti-caking property of xylitol of the present invention comprises the following steps: 250ml of xylitol concentrated solution with 82% of refraction and 85 ℃ of temperature is fed into a crystallizer, and then the temperature is slowly reduced at the speed of 0.3 ℃/min; when the system is cooled to 66.5 ℃, the system is observed to start to precipitate crystals, at the moment, the system is set to heat to 75 ℃ at the speed of 0.28 ℃/min for the first time to crystallize to prepare crystal nuclei, and the constant temperature is maintained at 75 ℃ for 30min; then cooling to 65 ℃ at the speed of 0.067 ℃/min for the second crystallization to obtain massecuite; and finally taking out the massecuite obtained by crystallization, centrifugally separating for 5min at 800rpm by using a centrifugal machine, and drying at 60 ℃ for 12h to obtain xylitol crystals.
According to the particle size analysis method, the xylitol crystals prepared in this example were subjected to particle size analysis, and the crystal habit of the xylitol crystals was observed under a polarizing microscope, the particle size distribution results are shown in table 1, and the particle habit is shown in fig. 3. The xylitol crystals prepared have a small amount of fine crystals attached to the periphery of large particles, but the surface is still relatively regular. The anti-blocking strength of the xylitol crystals prepared in this example was measured to be 25g.
To further illustrate the improvement effect of the method of the present invention, a further description will be given below in connection with comparative examples.
Comparative example
A comparative example of the present invention comprises the steps of: 250ml of xylitol concentrated solution with 82% of refraction and 85 ℃ of temperature is fed into a crystallizer, and then the temperature is slowly reduced at the speed of 0.3 ℃/min; when the system is cooled to 66.5 ℃, the system is observed to start to precipitate crystals, and the system does not perform heating-up induced crystallization operation at the moment, and is maintained at the constant temperature of 66.5 ℃ for 30min; then cooling to 65 ℃ at the speed of 0.01 ℃/min, and ending the crystallization process; and finally taking out the massecuite obtained by crystallization, centrifugally separating for 5min at 800rpm by using a centrifugal machine, and drying at 60 ℃ for 12h to obtain xylitol crystals.
According to the particle size analysis method, the xylitol crystals prepared in this example were subjected to particle size analysis, and the crystal habit of the xylitol crystals was observed under a polarizing microscope, the particle size distribution results are shown in table 1, and the particle habit is shown in fig. 4. The prepared xylitol crystals have rough and irregular surfaces, and basically belong to small-particle agglomerates although the particles are large. The anti-blocking strength of the xylitol crystals prepared in this example was measured to be 30g.
Table 1 comparison of the results of the particle size distribution of xylitol crystals prepared in each example and comparative example
The comparison results of the examples and the comparative examples shown in the table 1 show that when the crystallization system just separates out crystals, the heating-induced crystallization is arranged to prepare crystal nuclei, the prepared xylitol crystals have smooth and regular surfaces and take on regular diamond shapes, and the phenomenon that fine crystals are attached to the periphery of large particles hardly occurs; in the comparative example, however, the xylitol crystals prepared were basically agglomerates of small particles although the particles were large, the particle agglomeration phenomenon was serious, and the surface roughness of the particles was high. As can be seen from the analysis of the anti-caking performance of the prepared xylitol crystals, the xylitol crystals prepared by the method have stronger anti-caking performance and are less prone to caking. (the higher the anti-blocking strength value, the worse the corresponding anti-blocking property, and conversely, the lower the value, the better the anti-blocking property.)
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)
1. An induced nucleation crystallization method for improving the anti-caking property of xylitol is characterized by comprising the following steps:
Step one, taking 250ml of xylitol concentrated solution with 80-84% of refraction and 80-90 ℃ in a crystallizer, and slowly cooling at a cooling rate of 0.1-0.4 ℃/min;
step two, when the xylitol concentrated solution is slowly cooled to 66.5 ℃, observing that crystals are precipitated in the system, setting different heating rates to induce the system to crystallize for the first time to prepare crystal nuclei, and heating the system to 72-76 ℃, wherein the steps meet the following requirements: the temperature rising rate is 0.2-0.5 ℃/min;
Maintaining the constant temperature of the system for 30min after the temperature is raised to 72-76 ℃, slowly cooling to 60-65 ℃ and performing secondary crystallization to obtain massecuite, wherein the cooling rate of the step is 0.05-0.1 ℃/min;
and fourthly, centrifuging the massecuite, and drying at 40-80 ℃ for 8-12 hours to finally obtain xylitol crystals.
2. The method for inducing nucleation and crystallization for improving the anti-blocking performance of xylitol according to claim 1, comprising the steps of: 250ml of xylitol concentrated solution with 82% of refraction and 85 ℃ of temperature is fed into a crystallizer, and then the temperature is slowly reduced at the speed of 0.3 ℃/min; when the system is cooled to 66.5 ℃, the system is observed to start to precipitate crystals, at the moment, the system is set to heat to 75 ℃ at the speed of 0.45 ℃/min for the first time to crystallize to prepare crystal nuclei, and the constant temperature is maintained for 30min at 75 ℃; then cooling to 65 ℃ at the speed of 0.067 ℃/min for the second crystallization to obtain massecuite; and finally taking out the massecuite, centrifugally separating for 3min at 1000rpm by using a centrifugal machine, and drying at 60 ℃ for 12h to obtain xylitol crystals.
3. The method for inducing nucleation and crystallization for improving the anti-blocking performance of xylitol according to claim 1, comprising the steps of: 250ml of xylitol concentrated solution with 82% of refraction and 85 ℃ of temperature is fed into a crystallizer, and then the temperature is slowly reduced at the speed of 0.3 ℃/min; when the system is cooled to 66.5 ℃, the system is observed to start to precipitate crystals, at the moment, the system is set to heat to 75 ℃ at the speed of 0.34 ℃/min for the first time to crystallize to prepare crystal nuclei, and the constant temperature is maintained for 30min at 75 ℃; then cooling to 65 ℃ at the speed of 0.067 ℃/min for the second crystallization to obtain massecuite; and finally taking out the massecuite, centrifugally separating for 2min under the condition of 1200rpm by using a centrifugal machine, and drying for 12h at 60 ℃ to obtain xylitol crystals.
4. The method for inducing nucleation and crystallization for improving the anti-blocking performance of xylitol according to claim 1, comprising the steps of: 250ml of xylitol concentrated solution with 82% of refraction and 85 ℃ of temperature is fed into a crystallizer, and then the temperature is slowly reduced at the speed of 0.3 ℃/min; when the system is cooled to 66.5 ℃, the system is observed to start to precipitate crystals, at the moment, the system is set to heat to 75 ℃ at the speed of 0.28 ℃/min for the first time to crystallize to prepare crystal nuclei, and the constant temperature is maintained at 75 ℃ for 30min; then cooling to 65 ℃ at the speed of 0.067 ℃/min for the second crystallization to obtain massecuite; and finally taking out the massecuite, centrifugally separating for 5min at 800rpm by using a centrifugal machine, and drying at 60 ℃ for 12h to obtain xylitol crystals.
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| 木糖醇工业结晶过程控制***设计与开发;侯宝红;信息与控制;20060831;第35卷(第4期);541-544 * |
| 木糖醇溶解度和结晶介稳区的研究;朱路甲;中国食品添加剂;20051231(第2期);35-37 * |
| 木糖醇的结晶动力学;朱路甲;河北大学学报(自然科学版);20080731;第28卷(第4期);390-394 * |
| 木糖醇结晶的热力学特性;侯宝红;天津大学学报;20060430;第39卷(第4期);404-407 * |
| 由木糖醇发酵液制备木糖醇结晶体的研究;梅余霞;中国优秀博硕士学位论文全文数据库 (硕士)工程科技Ⅰ辑;20021215(第2期);B024-65 * |
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