CN103524303A - Method of auxiliary judging seed crystal adding time in erythritol crystallizing process based on specific gravity - Google Patents

Method of auxiliary judging seed crystal adding time in erythritol crystallizing process based on specific gravity Download PDF

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Publication number
CN103524303A
CN103524303A CN201310511382.XA CN201310511382A CN103524303A CN 103524303 A CN103524303 A CN 103524303A CN 201310511382 A CN201310511382 A CN 201310511382A CN 103524303 A CN103524303 A CN 103524303A
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China
Prior art keywords
erythritol
crystal seed
crystal
add
opportunity
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CN201310511382.XA
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王海蓉
张春桃
王鑫
刘帮禹
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Wuhan University of Science and Engineering WUSE
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Wuhan University of Science and Engineering WUSE
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Priority to CN201310511382.XA priority Critical patent/CN103524303A/en
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    • CCHEMISTRY; METALLURGY
    • C07ORGANIC CHEMISTRY
    • C07CACYCLIC OR CARBOCYCLIC COMPOUNDS
    • C07C29/00Preparation of compounds having hydroxy or O-metal groups bound to a carbon atom not belonging to a six-membered aromatic ring
    • C07C29/74Separation; Purification; Use of additives, e.g. for stabilisation
    • C07C29/76Separation; Purification; Use of additives, e.g. for stabilisation by physical treatment
    • C07C29/78Separation; Purification; Use of additives, e.g. for stabilisation by physical treatment by condensation or crystallisation

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Crystallography & Structural Chemistry (AREA)
  • Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
  • Preparation Of Compounds By Using Micro-Organisms (AREA)
  • Enzymes And Modification Thereof (AREA)

Abstract

The invention specifically relates to a method of auxiliary judging seed crystal adding time in an erythritol crystallizing process based on specific gravity. According to the technical scheme, specific gravity changes of the erythritol crystallization mother liquor are monitored in real time, and the seed crystal is added into erythritol crystallization mother liquor when specific gravity of the mother liquor is higher than 1.3. The method disclosed by the invention is simple to operate and easy to realize and can judge the seed crystal adding time easily, so that subjectivity and randomness in the process of judging the seed crystal adding time according to experience are avoided.

Description

Based on proportion auxiliary judgment erythritol crystallisation process, add the crystal seed method on opportunity
Technical field
The invention belongs to cocrystallization technical field, be specifically related to a kind ofly based on proportion auxiliary judgment erythritol crystallisation process, add the crystal seed method on opportunity.
Background technology
Erythritol is a kind of natural saccharic and function sweeting agent.Unique metabolic characteristics has determined the low characteristic of erythritol calorific value, is known as " zero calorie "; And, erythritol also have diabetic subject applicable, without cariogenic tooth, high dosis tolerata, the advantage such as side effect is little, mouthfeel is good.Along with the increase day by day of the chronic metabolic disease such as subhealth state, obesity and cardiovascular and cerebrovascular of too much bringing out due to the intake of sucrose in daily life, calorific value is low, be more and more subject to cane-sugar taste safety and Health sugar-free type sweeting agent erythritol roughly the same that parent looks at, market potential is huge.The continuous growths of market to low heat value function sweeting agent demand such as the continuous expansion of erythritol Application Areas and Japan, the U.S. and European Union, cause erythritol consumers demand very vigorous.
At present, it is longer that domestic erythritol production capacity broke through for 1 Want/a,Dan domestic production enterprise crystallization operation time, Granularity Distribution heterogeneity, and production efficiency is low.Especially erythritol cooling and crystallizing process, fermented erythritol liquor temperature in crystallization initial stage evaporation concentration is higher, and water coolant water temperature is lower, near heat-transfer surface, more easily deposition is brilliant dirty for degree of supersaturation, significantly reduce heat transfer efficiency, but also easily break out nucleation, and even form conglobulation particle, affect product purity, granularity and look level.Foreign market is higher to erythritol crystalline product specification of quality, except purity, look level index, also crystalline form and size-grade distribution is had to strict restriction.For example, Japan factory requires the crystal of erythritol 30 ~ 60 orders (or 20 ~ 40 orders, 40-80 order etc.) to account for the more than 90% of total mass.Domestic production enterprise need to adopt the techniques such as grinding, screening to reprocess to erythritol crystalline product, could meet strict granularity requirements.But grinding technics can destroy the crystalline form of erythritol product, cause product poor fluidity, plane of crystal coarse, easy caking, and also grinding-sieving technology has increased complicacy and the production cost of erythritol production technique.
Adding crystal seed crystallization control is the effective ways that improve crystalline product size-grade distribution.Inventor herein's early-stage Study shows, by controlling crystal seed add-on and seed size, distributes, and can realize the controllable adjustment of erythritol crystalline product size-grade distribution.But in erythritol actual industrial production process, but exist and add the difficult problem that crystal seed is difficult for assurance opportunity.At present, the crystal seed of erythritol crystallisation process adds the temperature that opportunity, general foundation detected in crystallizer to judge, but in tank, fermented liquid temperature fluctuation when evaporation concentration is larger, and under different evaporation concentration conditions, the degree of supersaturation of the interior temperature erythritol crystalline mother solution corresponding to it of tank is also unstable, thereby cause need opportunity operative employee to judge by rule of thumb adding of crystal seed, have larger subjectivity and randomness.Therefore, seek the effective ways that a kind of stable control crystal seed adds opportunity, become the key that solves erythritol crystalline product granularity controllable adjustment.
Summary of the invention
The present invention is intended to overcome erythritol and adds in crystal seed crystallization control process crystal seed and add and be difficult to quantitatively definite technical problem opportunity, variation by monitoring fermented erythritol liquor proportion in evaporating concentration process, stably adds the method on opportunity for client provides a kind of auxiliary judgment crystal seed.
The present inventor is by evidence, and the fermented erythritol liquor of crossing through thalline separation, ion-exchange, membrane filtration and decolorizing purification, in evaporating concentration process, exists corresponding relation between its proportion and the concentration of erythritol.Therefore, can reflect the erythritol concentration in solution by detecting its proportion, and then come auxiliary judgment erythritol crystallisation process crystal seed to add opportunity by specific gravity value.
For achieving the above object, the concrete steps of the technical solution used in the present invention are: by measuring erythritol crystalline mother solution proportion, come auxiliary judgment erythritol crystallisation process crystal seed to add opportunity.More concrete technical scheme of the present invention is: when erythritol crystalline mother solution proportion is greater than 1.3, can in erythritol crystalline mother solution, add crystal seed crystallization control.
Described erythritol crystalline mother solution refers to that take the fermented erythritol liquor of crossing through thalline separation, ion-exchange, membrane filtration and decolorizing purification is raw material, the settled solution obtaining after evaporation concentration.
The described crystal seed crystallization control that adds specifically refers to: the granularity that adds crystal seed is 170 ~ 200 orders, and the add-on of this crystal seed is 1~3wt% of crystalline mother solution mesoerythrit, more than in products obtained therefrom crystal, 40 ~ 80 object crystal account for product crystal 90wt%; Or the granularity that adds crystal seed is 120 ~ 150 orders, the add-on of this crystal seed is 0.5~1.5wt% of crystalline mother solution mesoerythrit, more than in products obtained therefrom crystal, 30 ~ 60 object crystal account for product crystal 90wt%.
Owing to adopting technique scheme, the present invention compared with prior art has following positively effect:
(1) involved in the present inventionly a kind ofly based on proportion auxiliary judgment erythritol crystallisation process, add the crystal seed method on opportunity, make erythritol crystallisation process crystal seed add the criterion on opportunity to quantize, avoided operative employee to judge by rule of thumb adding crystal seed subjectivity and the randomness on opportunity, the proportion by Real-Time Monitoring crystalline mother solution provides a kind of stable control crystal seed to add the effective ways on opportunity.
(2) involved in the present inventionly a kind ofly based on proportion auxiliary judgment erythritol crystallisation process, add the crystal seed method on opportunity, beguine adds opportunity more accurate according to crystal solution temperature judgement crystal seed, because the temperature of solution is the function of its composition, the composition of every batch fermentation liquid is not quite similar, and under different evaporation concentration condition, the degree of supersaturation of the interior temperature erythritol crystalline mother solution corresponding to it of crystallizer is also unstable.
(3) involved in the present inventionly a kind ofly based on proportion auxiliary judgment erythritol crystallisation process, add the crystal seed method on opportunity, easy and simple to handle, be easy to realize, even can realize on-line monitoring.Compared in crystallization cylinder, turbidometer being set, based on turbidity, change to judge that crystal seed adds opportunity cost will lack a lot.And add often relatively lag behind opportunity based on turbidity judgement crystal seed, cause crystal seed to add in fashionable crystallization cylinder degree of supersaturation bigger than normal or had crystal to separate out.
Embodiment
Below in conjunction with embodiment, the invention will be further described, not the restriction to its protection domain.
embodiment 1
A kind ofly based on proportion auxiliary judgment erythritol crystallisation process, add the crystal seed method on opportunity, its concrete steps are: with separated through thalline, ion-exchange, the fermented erythritol liquor that membrane filtration and decolorizing purification are crossed is raw material, evaporation concentration, make erythritol crystalline mother solution, when erythritol crystalline mother solution proportion is greater than 1.3, to adding granularity in erythritol crystalline mother solution, be that 170 ~ 200 object erythritol crystal are as crystal seed, the add-on of crystal seed is 1~3wt% of crystalline mother solution mesoerythrit, growing the grain 15 ~ 30min, continuation evaporative crystallization to the suspension density of crystalline mother solution reaches 50wt%, filter, dry, obtain erythritol crystal product, more than wherein 40 ~ 80 object crystal account for product crystal 90wt%.
embodiment 2
A kind ofly based on proportion auxiliary judgment erythritol crystallisation process, add the crystal seed method on opportunity, its concrete steps are: with separated through thalline, ion-exchange, the fermented erythritol liquor that membrane filtration and decolorizing purification are crossed is raw material, evaporation concentration, make erythritol crystalline mother solution, when erythritol crystalline mother solution proportion is greater than 1.3, to adding granularity in erythritol crystalline mother solution, be that 120 ~ 150 object erythritol crystal are as crystal seed, the add-on of crystal seed is 0.5~1.5wt% of crystalline mother solution mesoerythrit, growing the grain 15 ~ 30min, crystallisation by cooling to the suspension density of crystalline mother solution reaches 50wt%, filter, dry, obtain erythritol crystal product, more than wherein 30 ~ 60 object crystal account for product crystal 90wt%.

Claims (4)

1. based on proportion auxiliary judgment erythritol crystallisation process, add the crystal seed method on opportunity, it is characterized in that, specifically by measuring erythritol crystalline mother solution proportion, come auxiliary judgment erythritol crystallisation process crystal seed to add opportunity.
2. as claimed in claim 1ly based on proportion auxiliary judgment erythritol crystallisation process, add the crystal seed method on opportunity, it is characterized in that, when erythritol crystalline mother solution proportion is greater than 1.3, can in erythritol crystalline mother solution, add crystal seed crystallization control.
3. as described in claim 1,2, based on proportion auxiliary judgment erythritol crystallisation process, add the crystal seed method on opportunity, it is characterized in that, described erythritol crystalline mother solution is that to take the fermented erythritol liquor of crossing through thalline separation, ion-exchange, membrane filtration and decolorizing purification be raw material, the settled solution obtaining after evaporation concentration.
4. as described in claim 1,2, based on proportion auxiliary judgment erythritol crystallisation process, add the crystal seed method on opportunity, it is characterized in that, the described crystal seed crystallization control that adds specifically refers to:
The granularity that adds crystal seed is 170 ~ 200 orders, and the add-on of this crystal seed is 1~3wt% of crystalline mother solution mesoerythrit, more than in products obtained therefrom crystal, 40 ~ 80 object crystal account for product crystal 90wt%; Or the granularity that adds crystal seed is 120 ~ 150 orders, the add-on of this crystal seed is 0.5~1.5wt% of crystalline mother solution mesoerythrit, more than in products obtained therefrom crystal, 30 ~ 60 object crystal account for product crystal 90wt%.
CN201310511382.XA 2013-10-28 2013-10-28 Method of auxiliary judging seed crystal adding time in erythritol crystallizing process based on specific gravity Pending CN103524303A (en)

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN114262259A (en) * 2021-08-31 2022-04-01 山东星光首创生物科技有限公司 Method for controlling granularity of functional sugar alcohol product

Citations (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1736970A (en) * 2005-07-25 2006-02-22 天津大学 Xylitol refining crystallization process
CN101438781A (en) * 2007-10-30 2009-05-27 火箭兄弟公司 Process for the evapocrystallization of maltitol
CN101979616A (en) * 2010-11-12 2011-02-23 合肥工业大学 Method for producing erythritol by using broken rice
CN102154383A (en) * 2010-12-29 2011-08-17 保龄宝生物股份有限公司 Method for producing phycite by using corn meal
CN102249855A (en) * 2011-06-03 2011-11-23 山东福田药业有限公司 Process for preparing erythritol
CN102603478A (en) * 2012-02-23 2012-07-25 山东福田药业有限公司 Method for separating and purifying erythritol from mother liquid obtained after repeated crystallization of erythritol
CN102992957A (en) * 2012-12-13 2013-03-27 武汉科技大学 Solvent-out crystallization method of erythritol

Patent Citations (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1736970A (en) * 2005-07-25 2006-02-22 天津大学 Xylitol refining crystallization process
CN101438781A (en) * 2007-10-30 2009-05-27 火箭兄弟公司 Process for the evapocrystallization of maltitol
CN101979616A (en) * 2010-11-12 2011-02-23 合肥工业大学 Method for producing erythritol by using broken rice
CN102154383A (en) * 2010-12-29 2011-08-17 保龄宝生物股份有限公司 Method for producing phycite by using corn meal
CN102249855A (en) * 2011-06-03 2011-11-23 山东福田药业有限公司 Process for preparing erythritol
CN102603478A (en) * 2012-02-23 2012-07-25 山东福田药业有限公司 Method for separating and purifying erythritol from mother liquid obtained after repeated crystallization of erythritol
CN102992957A (en) * 2012-12-13 2013-03-27 武汉科技大学 Solvent-out crystallization method of erythritol

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN114262259A (en) * 2021-08-31 2022-04-01 山东星光首创生物科技有限公司 Method for controlling granularity of functional sugar alcohol product

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Application publication date: 20140122