CN101838181B - Preparation method of xylitol micro powders - Google Patents

Preparation method of xylitol micro powders Download PDF

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Publication number
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
stirring
micropowder
temperature
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CN101838181A (en
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田强
邱学良
刘圣宽
周娟
李令平
秦海青
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Shandong Futian Pharmaceutical Co Ltd
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Shandong Futian Pharmaceutical Co Ltd
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Abstract

一种木糖醇微粉制备方法,属于功能糖生产技术领域。该制备工艺包括(1)熔融木糖醇的制备、(2)搅拌降温结晶、(3)热软结晶块体的破碎三个工艺步骤:通过将制备的熔融木糖醇,经冷却、搅拌逐渐形成晶种而结晶变稠并形成软团体,随着温度的进一步降低和搅拌的剪切力作用,形成白色的木糖醇粉末。粉末颗粒的大小取决于变稠后搅拌剪切力的大小。再经筛分就可得到不同规格、流动性好的木糖醇微粉。本发明获得的木糖醇微粉流动性好、粒径分布范围窄,纯度在99%以上,是符合要求的食品级木糖醇微粉产品。The invention discloses a method for preparing xylitol micropowder, which belongs to the technical field of functional sugar production. The preparation process includes (1) preparation of molten xylitol, (2) stirring and cooling crystallization, and (3) crushing of hot soft crystal blocks: by cooling and stirring the prepared molten xylitol, gradually Seed crystals are formed and the crystals thicken and form soft groups. With the further reduction of temperature and the shear force of stirring, white xylitol powder is formed. The size of the powder particles depends on the size of the stirring shear force after thickening. After sieving, xylitol fine powder with different specifications and good fluidity can be obtained. The xylitol micropowder obtained by the invention has good fluidity, narrow particle size distribution range and a purity of over 99%, and is a food-grade xylitol micropowder product meeting requirements.

Description

Preparation method of xylitol micro powders
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)

1.一种木糖醇微粉制备方法,其特征是该制备工艺包括以下工艺步骤: 1. a preparation method of xylitol micropowder is characterized in that the preparation process comprises the following processing steps: (1)熔融木糖醇的制备:熔融木糖醇是指木糖醇纯度在99%以上,含水量低于5%的熔融液体状木糖醇,由生产的木糖醇晶粒经高温熔融获得,熔融温度控制在93—250℃;通过上述方式获得熔融至透明状态的液态木糖醇; (1) Preparation of molten xylitol: molten xylitol refers to molten liquid xylitol with a purity of more than 99% and a water content of less than 5%. The xylitol crystal grains produced are melted at high temperature Obtained, the melting temperature is controlled at 93-250°C; the liquid xylitol melted to a transparent state is obtained through the above method; (2)搅拌降温结晶:取熔融至透明状态的液态木糖醇,在5—20转/分钟的条件下进行缓慢降温,随着温度的降低器壁就会慢慢产生微小的晶粒,由于搅拌的作用使得晶粒在整个容器中扩散,使得整个容器中的液态熔融木糖醇产生结晶颗粒;继续搅拌直至完全结晶、变稠至软面团状,此时温度在75—95℃; (2) Stir and cool down to crystallize: take liquid xylitol that melts to a transparent state, and slowly cool down under the condition of 5-20 rpm. The effect of stirring makes the crystal grains diffuse in the whole container, so that the liquid melted xylitol in the whole container produces crystal particles; continue to stir until it is completely crystallized and thickens to a soft dough shape, and the temperature at this time is 75-95 °C; (3)热软结晶块体的破碎:这是该工艺中制备木糖醇微粉的关键一步;这种状态仅存在5分钟左右,此时要以加快搅拌转速而产生的剪切力对热软块体加紧粉碎,转速在50—200转/分钟,随着温度的逐步降低,逐渐获得流动性好的白色木糖醇粉末。 (3) Breaking of hot-soft crystalline blocks: This is a key step in the preparation of xylitol micropowder in this process; this state only exists for about 5 minutes. The block is pulverized step by step, and the rotating speed is 50-200 rpm. As the temperature gradually decreases, white xylitol powder with good fluidity is gradually obtained.
CN 200910019943 2009-03-20 2009-03-20 Preparation method of xylitol micro powders Active CN101838181B (en)

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RU2015132902A (en) * 2013-01-07 2017-02-09 Сам-А Фарм. Ко., Лтд. NEW QUICKLY SOLUBLE COMPOSITION OF GRANULES WITH IMPROVED SOLUBILITY
CN108883400B (en) 2016-02-19 2021-09-17 洲际大品牌有限责任公司 Method for forming a multi-value stream 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)

* Cited by examiner, † Cited by third party
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

Patent Citations (2)

* Cited by examiner, † Cited by third party
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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