CN101838181B - Preparation method of xylitol micro powders - Google Patents
Preparation method of xylitol micro powders Download PDFInfo
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- CN101838181B CN101838181B CN 200910019943 CN200910019943A CN101838181B CN 101838181 B CN101838181 B CN 101838181B CN 200910019943 CN200910019943 CN 200910019943 CN 200910019943 A CN200910019943 A CN 200910019943A CN 101838181 B CN101838181 B CN 101838181B
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- xylitol
- preparation
- temperature
- micro powders
- stirring
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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 57
- HEBKCHPVOIAQTA-UHFFFAOYSA-N meso ribitol Natural products OCC(O)C(O)C(O)CO HEBKCHPVOIAQTA-UHFFFAOYSA-N 0.000 title claims abstract description 57
- 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 57
- 229960002675 xylitol Drugs 0.000 title claims abstract description 57
- 235000010447 xylitol Nutrition 0.000 title claims abstract description 57
- 239000000811 xylitol Substances 0.000 title claims abstract description 57
- 239000000843 powder Substances 0.000 title claims abstract description 28
- 238000002360 preparation method Methods 0.000 title claims abstract description 13
- 238000003756 stirring Methods 0.000 claims abstract description 26
- 239000013078 crystal Substances 0.000 claims abstract description 21
- 238000002425 crystallisation Methods 0.000 claims abstract description 7
- 238000013467 fragmentation Methods 0.000 claims abstract description 7
- 238000006062 fragmentation reaction Methods 0.000 claims abstract description 7
- 238000002156 mixing Methods 0.000 claims abstract description 6
- 230000008025 crystallization Effects 0.000 claims abstract description 4
- 239000007788 liquid Substances 0.000 claims description 15
- 238000002844 melting Methods 0.000 claims description 10
- 230000008018 melting Effects 0.000 claims description 10
- 238000000034 method Methods 0.000 claims description 8
- 239000002245 particle Substances 0.000 claims description 7
- 238000005516 engineering process Methods 0.000 claims description 4
- 230000000694 effects Effects 0.000 claims description 3
- 230000004927 fusion Effects 0.000 claims description 2
- 238000010008 shearing Methods 0.000 claims description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 2
- 239000000155 melt Substances 0.000 claims 1
- 238000010583 slow cooling Methods 0.000 claims 1
- 238000001816 cooling Methods 0.000 abstract description 7
- 238000012216 screening Methods 0.000 abstract description 7
- 238000004519 manufacturing process Methods 0.000 abstract description 6
- 238000009826 distribution Methods 0.000 abstract description 5
- 239000008187 granular material Substances 0.000 abstract 1
- 230000008719 thickening Effects 0.000 abstract 1
- 238000010438 heat treatment Methods 0.000 description 7
- 239000000047 product Substances 0.000 description 4
- 238000009792 diffusion process Methods 0.000 description 3
- 238000005303 weighing Methods 0.000 description 3
- 239000007795 chemical reaction product Substances 0.000 description 2
- 230000007812 deficiency Effects 0.000 description 2
- 235000013305 food Nutrition 0.000 description 2
- 238000010298 pulverizing process Methods 0.000 description 2
- 229940112822 chewing gum Drugs 0.000 description 1
- 235000015218 chewing gum Nutrition 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 230000009977 dual effect Effects 0.000 description 1
- 238000001704 evaporation Methods 0.000 description 1
- 230000008020 evaporation Effects 0.000 description 1
- 239000007937 lozenge Substances 0.000 description 1
- 239000003595 mist Substances 0.000 description 1
- 230000002000 scavenging effect Effects 0.000 description 1
- 238000004513 sizing Methods 0.000 description 1
- 238000001694 spray drying Methods 0.000 description 1
- 238000005507 spraying Methods 0.000 description 1
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- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The invention discloses a preparation method of xylitol micro powders, belonging to the technical field of functional sugar production. The preparation process comprises the three processing steps: (1) preparation of molten xylitol, (2) mixing and cooling crystallization and (3) fragmentation of thermal soft crystalline block. and the concrete steps are as follows: cooling and stirring the prepared molten xylitol to gradually form seed crystals to crystallize and thicken to form soft blocks, and then forming white xylitol powders along with the further reduction of temperature and the shear force of stirring, wherein the sizes of the powder granules depend on the stirring shear force after thickening; and screening to obtain xylitol micro powders with different specifications and good flowability. The obtained xylitol micro powders of the invention has good flowability, narrow granular distribution range and more than 99% of purity, and are food-grade xylitol micro powder products meeting requirements.
Description
Technical field
The invention belongs to technical field of functional sugar production, particularly by Xylitol melting, cooling, stirred crystallization, stirring pulverizing, sizing screening being prepared the production technique of xylitol micro powders.
Technical background
Xylitol micro powders is widely used in the food service industrys such as Xylitol lozenge, chewing gum, the mouthfeel of the end product that its particle size distribution range and mobile directly impact are corresponding and end product manufacturer's ease of use.Explore that particle size distribution range is narrow, good product mobility, xylitol micro powders production technique that purity is high, be that each large Xylitol manufacturing enterprise is always at problems of concern.
At present, the production technique known of xylitol micro powders is mechanical disintegration (comprising Universalpulverizer, turbine pulverizing mill, Icing Sugar machine, shredder) method.But because Xylitol fusing point low (92-96 ℃) therefore adopts comminuting method can produce because of mechanical energy and gives birth to the phenomenon that heat bonds, bring great difficulty for the classification techniques such as screening, selection by winnowing.Because the friability of xylitol crystal is very strong, thus the micro powder product of pulverizer acquisition, granularity is generally partially thin, and particle size range distributes wide, does not meet the specification of quality of product.
In addition, European patent EP 1424319B1 has introduced and has adopted spraying drying to prepare the technique of xylitol micro powders.But because the vitreum invert point of Xylitol is too low, even transfer air intake and air outlet temperature very lowly, the yield of micro mist also only has about 10%, and major part is all pasted on wall.Application is restricted.
Summary of the invention
For the deficiencies in the prior art, the invention provides a kind of preparation method of xylitol micro powders, to solve the above deficiency of mechanical disintegration and spray drying technology.
The step that the technical solution adopted for the present invention to solve the technical problems comprises is: preparation melting Xylitol, the fragmentation of stirring decrease temperature crystalline, hot soft junction crystal block body, sieve the xylitol micro powders that obtains good fluidity, even particle distribution by specification again.The concrete technology step is as follows:
1, the preparation of melting Xylitol: the melting Xylitol refers to xylitol purity more than 99%, and water content is lower than 5% melt liquid shape Xylitol.This can directly be obtained through multiple-effect evaporation or vacuum concentration by the Xylitol scavenging solution, and when concentrated, temperature is controlled at 75-200 ℃ and is advisable, and temperature is crossed low slowly concentrated, and it is yellow that excess Temperature then can gradually become; Also can be obtained through high-temperature fusion by xylitol crystal, temperature is controlled at 93-250 ℃ and is advisable, and temperature is unsuitable too high, avoids repeatedly heating, and prevents the variable color of Xylitol liquid; All can obtain to melt to the xylitol liquid of vitreous state by above-mentioned dual mode.
2, stir decrease temperature crystalline: will melt to the xylitol liquid of vitreous state in the step 1, stir cooling, mixing speed is 5-20 rev/min.Along with the reduction wall of temperature will slowly produce small crystal grain, because the effect of stirring is so that crystal grain spreads in whole container, so that the liquid molten Xylitol in the whole container produces crystalline particle, naked eyes can be seen.Continue to stir until fully crystallization, retrogradation to soft dough shape, this moment, temperature was about 75-95 ℃.
3, the fragmentation of hot soft junction crystal block body: only there are 5 minutes in the state that the melting Xylitol is in hot soft junction crystal block body, stirs with 50-200 rev/min faster rotational speed, and is broken rapidly to hot magma body to stir the shearing force that produces.Along with the progressively reduction of temperature, obtain gradually the white xylitol powder of good fluidity.
Positively effect of the present invention be adopt xylitol powder that this preparation technology obtains through screening can obtain good fluidity, particle size distribution range is narrow, purity is more than 99%, satisfactory food grade xylitol micro powders product.
Embodiment
The invention will be further described below in conjunction with embodiment.
Embodiment 1
Take by weighing 1500g crystal Xylitol, add in the electromagnetic oven pan, 210 ℃ of heating and meltings stir simultaneously, make to be heated evenly, and melt to fully transparently, and pure liquid is aobvious weak yellow, and stopped heating slowly stirs cooling, and mixing speed is 10 rev/mins.Along with the reduction of temperature, produce white crystals in the bottom of pot, along with stirring rapidly diffusion, subsequently, pure liquid generation fusion-crystallization also produces crystal grain.Continue to keep 10 rev/mins speed to stir, until form gradually soft dough shape.Strengthen rotating speed to 60 rev/min, the software agglomerate is stirred rapidly fragmentation, can obtain the xylitol powder of dark white.Can obtain 70-200 purpose xylitol micro powders through screening, amount to 526g.
Embodiment 2
Take by weighing 1500g crystal Xylitol, add in the electromagnetic oven pan, 160 ℃ of heating and meltings stir simultaneously, make to be heated evenly, melt to fully transparent, pure liquid color duskiness, stopped heating slowly stirs cooling, mixing speed is 8 rev/mins.Along with the reduction of temperature, produce white crystals in the bottom of pot, along with stirring rapidly diffusion, subsequently, pure liquid generation fusion-crystallization also produces crystal grain.Continue to keep 8 rev/mins speed to stir, until form gradually soft dough shape.Strengthen rotating speed to 60 rev/min, the software agglomerate is stirred rapidly fragmentation, can obtain the xylitol powder of white.Can obtain 70-200 purpose xylitol micro powders through screening, amount to 603g.
Embodiment 3
Take by weighing 1500g crystal Xylitol, add in the electromagnetic oven pan, 120 ℃ of heating and meltings stir simultaneously, make to be heated evenly, melt to fully transparent, pure liquid color duskiness, stopped heating slowly stirs cooling, mixing speed is 5 rev/mins.Along with the reduction of temperature, produce white crystals in the bottom of pot, along with stirring rapidly diffusion, subsequently, pure liquid generation fusion-crystallization also produces crystal grain.Continue to keep 5 rev/mins speed to stir, until form gradually soft dough shape.Strengthen rotating speed to 56 rev/min, the software agglomerate is stirred rapidly fragmentation, can obtain the xylitol powder of white.Can obtain 70-200 purpose xylitol micro powders through screening, amount to 635g.
Claims (1)
1. preparation method of xylitol micro powders is characterized in that this preparation technology comprises following processing step:
(1) preparation of melting Xylitol: the melting Xylitol refers to xylitol purity more than 99%, and water content is lower than 5% melt liquid shape Xylitol, is obtained through high-temperature fusion by the Xylitol crystal grain of producing, and melt temperature is controlled at 93-250 ℃; Obtain to melt to by the way the xylitol liquid of vitreous state;
(2) stir decrease temperature crystalline: get the xylitol liquid that melts to vitreous state, under 5-20 rev/mins condition, carry out slow cooling, along with the reduction wall of temperature will slowly produce small crystal grain, because the effect of stirring so that crystal grain in whole container, spread so that the liquid molten Xylitol in the whole container produces crystalline particle; Continue to stir until fully crystallization, retrogradation to soft dough shape, this moment, temperature was at 75-95 ℃;
(3) fragmentation of hot soft junction crystal block body: this is one step of key of preparation xylitol micro powders in this technique; This state only existed about 5 minutes, and the shearing force that will produce this moment to accelerate mixing speed steps up to pulverize to hot magma body, and rotating speed along with the progressively reduction of temperature, obtains the white xylitol powder of good fluidity at 50-200 rev/mins gradually.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 200910019943 CN101838181B (en) | 2009-03-20 | 2009-03-20 | Preparation method of xylitol micro powders |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 200910019943 CN101838181B (en) | 2009-03-20 | 2009-03-20 | Preparation method of xylitol micro powders |
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| Publication Number | Publication Date |
|---|---|
| CN101838181A CN101838181A (en) | 2010-09-22 |
| CN101838181B true CN101838181B (en) | 2013-01-02 |
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| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN 200910019943 Active CN101838181B (en) | 2009-03-20 | 2009-03-20 | Preparation method of xylitol micro powders |
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| CN (1) | CN101838181B (en) |
Families Citing this family (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2014106962A1 (en) * | 2013-01-07 | 2014-07-10 | 삼아제약 주식회사 | Novel fast-dissolving granule formulation having improved solubility |
| JP6774494B2 (en) | 2016-02-19 | 2020-10-21 | インターコンチネンタル グレート ブランズ エルエルシー | Process for forming multiple useful streams from a biomass source |
| CN114041519A (en) * | 2021-11-25 | 2022-02-15 | 浙江华康药业股份有限公司 | Method for preparing xylitol granules capable of being directly tabletted |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP1424319A1 (en) * | 2002-10-22 | 2004-06-02 | DHW Deutsche Hydrierwerke GmbH Rodleben | Spray-dried xylitol and process for its production |
| CN1903866A (en) * | 2006-08-01 | 2007-01-31 | 禹城福田药业有限公司 | Preparation method of crystalline xylosic alcohol powder |
-
2009
- 2009-03-20 CN CN 200910019943 patent/CN101838181B/en active Active
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP1424319A1 (en) * | 2002-10-22 | 2004-06-02 | DHW Deutsche Hydrierwerke GmbH Rodleben | Spray-dried xylitol and process for its production |
| CN1903866A (en) * | 2006-08-01 | 2007-01-31 | 禹城福田药业有限公司 | Preparation method of crystalline xylosic alcohol powder |
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| Publication number | Publication date |
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| CN101838181A (en) | 2010-09-22 |
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Effective date of registration: 20231114 Granted publication date: 20130102 |