CN103497221A - Preparation method for D-mannose crystals - Google Patents
Preparation method for D-mannose crystals Download PDFInfo
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- CN103497221A CN103497221A CN201310485499.5A CN201310485499A CN103497221A CN 103497221 A CN103497221 A CN 103497221A CN 201310485499 A CN201310485499 A CN 201310485499A CN 103497221 A CN103497221 A CN 103497221A
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Abstract
The invention provides a preparation method for D-mannose crystals. The method includes adding activated carbon into mannose slurry to perform heating and discoloration, then performing desalination and purification, performing evaporation and concentration, and soaking in absolute ethyl alcohol for purification and drying to obtain high-purity crystal D-mannose. By the aid of the method that the activated carbon is used for discoloration and electrodialysis desalination, evaporation and concentration are performed until the slurry is almost oven dry and the absolute ethyl alcohol is used for soaking the obtained crystals, the problems of viscous mother liquid, small crystals, low yield and the like in the existing D-mannose crystallization process are solved. On the basis of the traditional technology, an advanced electrodialysis desalination technique replaces ion exchange, crystallization time ranges from 20 hours to 30 hours, a technological process is shortened, and energy conservation and consumption reduction are achieved; crystallization times are decreased, and crystallization yield of the mannose crystals is increased.
Description
Technical field
The invention belongs to the functional sugar field, be specifically related to a kind of D-MANNOSE crystal preparation method.
Background technology
D-MANNOSE is the white powder crystal, distinguishes the flavor of sweet, is about 0.6 times of sucrose, 0.86 times of glucose.Soluble in water, be slightly soluble in ethanol (0.4%), be insoluble in ether.As a kind of hexose, occurring in nature exists less with free state, and the form existence mainly with mannosans, for example be present in the konjaku of aroid, is Oligomeric manna sugar.
D-MANNOSE is used in the food-drink aspect, can be used as sweeting agent; Be used in medical aspect, some research datas of the U.S. show, seminose has sterilization, antiinflammation, and the diseases such as diabetes, obesity, constipation and hypercholesterolemia are had to good auxiliary therapeutic action.
Chinese patent CN101851689A discloses a kind of D-MANNOSE crystal preparation technology, the mixed solution that the glucose of take obtains as the raw material isomery, after simulation moving-bed separation, seminose component parting liquid carries out aqueous crystallization after twice concentrates, the coarse-grain of system, then improve purity by soaked in absolute ethyl alcohol, obtain the seminose crystal.But the aqueous crystallization defectiveness: crystallization time is grown 60-100 h, efficiency is low; The coarse-grain that aqueous crystallization obtains needs dehydrated alcohol refining, and technique is loaded down with trivial details.
Tradition crystallization D-MANNOSE aqueous crystallization has a large amount of mother liquors and produces, and the massecuite viscosity is very big, is unfavorable for centrifugally, and the finished product separation difficulty, need repeatedly recrystallization.
Summary of the invention
The object of the invention is to overcome the deficiency that above-mentioned traditional treatment method exists, a kind of preparation method of D-MANNOSE crystallization is provided, utilize activated carbon decolorizing and electrodialysis desalination, evaporation concentration, to being close to over dry, has obtained the method for crystal by soaked in absolute ethyl alcohol.Solve in existing D-MANNOSE crystallisation process and have the mother liquor thickness with this, the problem such as crystal grain is little, yield is low.
The preparation method of D-MANNOSE crystal of the present invention comprises the following steps:
1. step decolours: in the sweet dew syrup, add gac to be added heat decoloring, obtain the seminose destainer;
Step is desalination 2.: by 1. described seminose destainer of step, carry out desalting refinement, obtain the seminose refined liquid;
Step is evaporation concentration 3.: by step 2. described seminose refined liquid carry out evaporation concentration, obtain the sweet dew massecuite;
Step is crystallization 4.: by step 3. described sweet dew massecuite, drying refining through soaked in absolute ethyl alcohol obtain highly purified crystallization D-MANNOSE.
1. step of the present invention is decoloured and carried out under the following conditions: the concentration of sweet dew syrup source is 10-15%, content is greater than 60%, raw material is carried out to heating in water bath, the 2-5% that the amount that adds gac is dry-matter, bleaching temperature is 75-80 ℃, stir insulation 20-30min, filter and obtain transmittance 99.7% seminose destainer.
Step of the present invention 2. desalination is carried out under the following conditions: after the seminose destainer is cooled to 35-40 ℃, introduces electrodialytic diluting compartment and utilize electrodialysis desalination, obtain the seminose refined liquid, specific conductivity is 6-8 μ s/cm.
Step of the present invention 4. crystallization is carried out under the following conditions: 3. step is added to the dehydrated alcohol of 1-2 times of volume in described sweet dew massecuite, carry out automatic temperature control instrument control and carry out the crystallization of 1-4 ℃/h gradient cooling, and stirred in temperature-fall period, intermittently add dehydrated alcohol.When temperature is down to 50 ℃, carry out the nature cooling; Centrifugal with whizzer, obtain the seminose crystal.
The present invention is on the traditional technology basis, adopts advanced electrodialysis desalination technology to replace ion-exchange, crystallization time 20-30 h, and technical process is shortened and is reached the energy-saving and cost-reducing effect of knowing clearly; Reduce the number of times of crystallization, increased the crystallization yield (more than 48%) of seminose crystal.
Embodiment
Embodiment 1
1, decolouring
The sweet dew syrup is warming up to 75 ℃, and the amount that adds gac is dry-matter 5%, stirs insulation 30 min, carries out vacuum filtration and obtains printing opacity > 99.7% destainer.
2, electrodialysis desalination
Destainer is cooled to 35 ℃, add in the decontamination chamber of electrodialyzer, specific conductivity is down to 8 μ s/cm by 2260 μ s/cm, has reached the purpose of desalination.
3, evaporation concentration
To carry out vacuum concentration at 75 ℃ through the sweet dew syrup of electrodialysis desalination, to the dry-matter refractive power, more than 96%, obtain sweet dew massecuite 600g.
4, crystallization
Add the dehydrated alcohol of 1.5 times of volumes to carry out 75 ℃ of insulations the sweet dew massecuite obtained, use the agitator uniform stirring, then use automatic temperature control instrument to control with natural cooling down after 1 ℃/h gradient cooling to 50 ℃ to room temperature.Centrifugal with whizzer, obtain the seminose crystal, drying obtains 264 g crystal, and yield reaches 44%, through high-pressure liquid phase, detects, and purity reaches 98.05%
Embodiment 2
1, decolouring
The sweet dew syrup is warming up to 80 ℃, and the amount that adds gac is dry-matter 2%, stirs insulation 20min, carries out vacuum filtration and obtains printing opacity > 99.7% destainer.
2, electrodialysis desalination
Destainer is cooled to 40 ℃, add in the decontamination chamber of electrodialyzer, specific conductivity is down to 6.38 μ s/cm by 2260 μ s/cm, has reached the purpose of desalination.
3, evaporation concentration
To carry out vacuum concentration at 80 ℃ through the sweet dew syrup of electrodialysis desalination, to the dry-matter refractive power, more than 96%, obtain sweet dew massecuite 750g.
4, crystallization
Add the dehydrated alcohol of 1 times of volume to carry out 75 ℃ of insulations the sweet dew massecuite obtained, then use automatic temperature control instrument to control with natural cooling down after 1 ℃/h gradient cooling to 50 ℃ to room temperature, the temperature-fall period discontinuous adds dehydrated alcohol, divides the dehydrated alcohol that adds again 0.5 times of volume for five times.Centrifugal with whizzer, obtain the seminose crystal, drying obtains 360 g crystal, and yield reaches 48.3%, through high-pressure liquid phase, detects, and purity reaches: 99.21%.
Claims (4)
1. the preparation method of a D-MANNOSE crystallization, is characterized in that, comprises the following steps:
1. step decolours: in the sweet dew syrup, add gac to be added heat decoloring, obtain the seminose destainer;
Step is desalination 2.: by 1. described seminose destainer of step, carry out desalting refinement, obtain the seminose refined liquid;
Step is evaporation concentration 3.: by step 2. described seminose refined liquid carry out evaporation concentration, obtain the sweet dew massecuite;
Step is crystallization 4.: by step 3. described sweet dew massecuite, drying refining through soaked in absolute ethyl alcohol obtain highly purified crystallization D-MANNOSE.
2. preparation method as claimed in claim 1, it is characterized in that, 1. described step is decoloured and carried out under the following conditions: the concentration of sweet dew syrup source is 10-15%, content is greater than 60%, raw material is carried out to heating in water bath, the 2-5% that the amount that adds gac is dry-matter, bleaching temperature is 75-80 ℃, stir insulation 20-30min, filter and obtain transmittance 99.7% seminose destainer.
3. preparation method as claimed in claim 1, it is characterized in that, described step 2. desalination is carried out under the following conditions: after the seminose destainer is cooled to 35-40 ℃, introduces electrodialytic diluting compartment and utilize electrodialysis desalination, obtain the seminose refined liquid, specific conductivity is 6-8 μ s/cm.
4. preparation method as claimed in claim 1, it is characterized in that, described step 4. crystallization is carried out under the following conditions: 3. step is added to the dehydrated alcohol of 1-2 times of volume in described sweet dew massecuite, carry out automatic temperature control instrument control and carry out the crystallization of 1-4 ℃/h gradient cooling, and stirred in temperature-fall period, intermittently add dehydrated alcohol, when temperature is down to 50 ℃, carry out the nature cooling; Centrifugal with whizzer, obtain the seminose crystal.
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| CN201310485499.5A CN103497221A (en) | 2013-10-17 | 2013-10-17 | Preparation method for D-mannose crystals |
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| CN201310485499.5A CN103497221A (en) | 2013-10-17 | 2013-10-17 | Preparation method for D-mannose crystals |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2018103723A1 (en) * | 2016-12-10 | 2018-06-14 | 高尚先 | New use for mannose for increasing treg cell number and foxp3 factor expression level thereof |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20030222021A1 (en) * | 2001-12-31 | 2003-12-04 | Anu Ennelin | Method for the recovery of sugars |
| CN102329340A (en) * | 2011-11-01 | 2012-01-25 | 青岛明月海藻集团有限公司 | Method for preparing D-mannose |
-
2013
- 2013-10-17 CN CN201310485499.5A patent/CN103497221A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20030222021A1 (en) * | 2001-12-31 | 2003-12-04 | Anu Ennelin | Method for the recovery of sugars |
| CN102329340A (en) * | 2011-11-01 | 2012-01-25 | 青岛明月海藻集团有限公司 | Method for preparing D-mannose |
Non-Patent Citations (2)
| Title |
|---|
| 张庆胜、楼照: "电渗析技术在氨基酸、医药中间体、果汁以及高含盐废水中的脱盐应用", 《2012青岛国际脱盐大会》 * |
| 武睿，等: "电渗析在葡萄糖浆脱盐中的应用", 《食品与发酵工业》 * |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2018103723A1 (en) * | 2016-12-10 | 2018-06-14 | 高尚先 | New use for mannose for increasing treg cell number and foxp3 factor expression level thereof |
| CN108210503A (en) * | 2016-12-10 | 2018-06-29 | 高尚先 | Mannose is for improving the new application of Treg cell quantities and its Foxp3 factor expressions level |
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Effective date of registration: 20151022 Address after: 266031, 1001/1002 building, 177 Shandong Road, Sifang Road, Sifang, Shandong, Qingdao Applicant after: Shandong Futaste Technology Group Co., Ltd. Address before: 251200 Yucheng, Shandong, South Ring Road, No. 666, No. Applicant before: Shandong Futian Medicine Industry Co., Ltd. |
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Application publication date: 20140108 |