CN108659061A - A kind of purification processing method of Sucralose crystalline mother solution - Google Patents
A kind of purification processing method of Sucralose crystalline mother solution Download PDFInfo
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- CN108659061A CN108659061A CN201810776930.4A CN201810776930A CN108659061A CN 108659061 A CN108659061 A CN 108659061A CN 201810776930 A CN201810776930 A CN 201810776930A CN 108659061 A CN108659061 A CN 108659061A
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- Prior art keywords
- sucralose
- layer
- processing method
- purification processing
- ethyl acetate
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07H—SUGARS; DERIVATIVES THEREOF; NUCLEOSIDES; NUCLEOTIDES; NUCLEIC ACIDS
- C07H5/00—Compounds containing saccharide radicals in which the hetero bonds to oxygen have been replaced by the same number of hetero bonds to halogen, nitrogen, sulfur, selenium, or tellurium
- C07H5/02—Compounds containing saccharide radicals in which the hetero bonds to oxygen have been replaced by the same number of hetero bonds to halogen, nitrogen, sulfur, selenium, or tellurium to halogen
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07H—SUGARS; DERIVATIVES THEREOF; NUCLEOSIDES; NUCLEOTIDES; NUCLEIC ACIDS
- C07H1/00—Processes for the preparation of sugar derivatives
- C07H1/06—Separation; Purification
Abstract
The present invention provides a kind of purification processing method of Sucralose crystalline mother solution, four steps are handled by n-butyl acetate extraction, ethyl acetate extraction, Waste water concentrating and butyl acetate layer, it is generated with high-recovery, less solvent consumption and less waste water, with good economic efficiency and social benefit.
Description
Technical field
The invention belongs to food additives fields, and in particular to a kind of purification processing method of Sucralose crystalline mother solution.
Background technology
Sucralose（TGS）, it is commonly called as Sucralose（sucralose）, it is Tai Lai companies of Britain（Tate ＆ Lyle）With London
A kind of novel artificial sweetener that university develops and applied for a patent in 1976 jointly.It is uniquely using sucrose as the functionality of raw material
Sweetener, original brand name are Splenda, and sugariness is up to sucrose 320 to 1,000 times.This artificial sweetener is with no warm
The features such as amount, sugariness is high, and sweet taste is pure, and degree of safety is high.But Sucralose may decompose in the process of food（Main cause be by
Thermal decomposition, boiling water is still within safe range）, and generate harmful toxic product.
The alcohol and full-bodied mouth feel of Sucralose are sufficiently close to sucrose, and sweet taste characteristic curve is almost Chong Die with sucrose, does not appoint
Why bother taste.Institute's heat content is low, is not easy to be digested absorption, while also not allowing to be also easy to produce saprodontia.Sucralose is in use not
Other influences can be generated to food, while the unpleasant tastes such as bitterness can also be covered.Both it can be used alone or can be with other sweet tastes
Agent is used in mixed way, and Sucralose is soluble easily in water, not blistering in course of dissolution.
Currently, the method for crystallising of Sucralose is mainly crystallized by solvent of water in industrial production, and the mistake of water crystallization
Journey necessarily leads to mother liquor.Since the solubility of Sucralose in water is larger, after water crystallization, remaining Sucralose is dense in mother liquor
Degree can reach 30% or so, and the purity of Sucralose only has 92% or so in water crystallization mother liquor, cannot reach fine work trichlorine
The standard of sucrose, thus pass through organic solvent extract method improve water crystallization mother liquor in Sucralose purity, make trichlorine sugarcane
Syrup crystalline mother solution can recycled for multiple times, for improve Sucralose purity played an important role with percent crystallization in massecuite.But
Current purification processing method will produce a large amount of waste water, in the case of current pay attention to day by day environmental protection, it is difficult to meet ring
The high request of guarantor.
Invention content
It is an object of the invention to overcome the purification processing method of Sucralose crystalline mother solution in the prior art to will produce greatly
The defect of waste water is measured, and provides a kind of purification for the Sucralose crystalline mother solution that waste water yield is few, the Sucralose rate of recovery is high
Processing method.
The present invention provides a kind of purification processing methods of Sucralose crystalline mother solution, it is characterised in that including walking as follows
Suddenly：
（1）The middle addition mother liquor of sucralose into extraction kettle adjusts pH to weakly acidic pH；Mother liquor of sucralose is added into extraction kettle
After standing, lower aqueous layer is divided to transfer tank, upper layer butyl acetate layer point to acetic acid for the butyl acetate of quality 1/5 ~ 2/5, stirring
Butyl ester storage tank repeats to extract 2 ~ 4 times total；
（2）By step（1）The middle obtained water layer that is layered is transferred in extraction kettle, and mother liquor of sucralose quality 2/5 ~ 3/5 is added
After standing, lower aqueous layer is divided into mother liquor transfer tank for ethyl acetate stirring, and upper layer ethyl acetate layer point to distillation still repeats
Extraction is 2 ~ 4 times total, and the content that Sucralose in water layer is surveyed in sampling is less than 5%, and it is to be concentrated to squeeze into storage tank；
（3）Step（2）In obtained water layer be pumped into concentration kettle, be evaporated under reduced pressure in moisture to water layer Sucralose content 25% ~
30%, then the mother liquor after concentration is transferred back in extraction kettle, add the ethyl acetate extraction of mother liquor of sucralose quality 2/5 ~ 3/5
Take 2 ~ 4 same steps of concrete operations（2）In extracting operation, when aqueous layer contg is discharged into cesspool less than 2%；Ethyl acetate layer with
Step（2）In ethyl acetate layer merging steam after ethyl acetate to producing Sucralose after finishing room's decoloration distillation；
（4）By step（1）Butyl acetate layer after middle extracting mother liquid squeezes into butyl acetate distillation still, steams 50 ~ 60% mass
Butyl acetate postcooling to 30 ~ 40 DEG C plus water stirring, stand after, be added water quality be residual acetic acid butyl ester quality 20 ~
25%；Water layer is divided into transfer tank, again repeatedly step（3）Waste water concentrating, butyl acetate layer continues washing 1 ~ 3 time；It is remained after washing
Remaining butyl acetate vacuum distillation, cesspool is discharged into after raffinate cooling.
Preferably, the step（1）It is 6.5 ~ 7.5 that middle pH refers specifically to pH to weakly acidic pH.
Preferably, the step（1）、（2）With（4）In, stirring, the specific time stood are 0.2 ~ 1h of stirring, stand 0.2
~1h。
Preferably, the step（1）The butyl acetate quality of middle addition is the 1/5 ~ 1/3 of mother liquor of sucralose quality.
Preferably, the step（1）PH is adjusted after extraction again to 6.5 ~ 7.5.
Preferably, the step（1）Middle repetition extracts 3 times total.
Preferably, the step（2）With（3）The each addition of middle ethyl acetate be mother liquor of sucralose quality 1/2 ~
3/5。
Preferably, the step（2）In obtained water layer be pumped into before concentration kettle and first extract 1 ~ 3 with low polar organic solvent
It is secondary.
Preferably, the low polar organic solvent is selected from hexamethylene, toluene or dichloromethane.
Preferably, the addition of the low polar organic solvent is 5 ~ 10%.After low polar organic solvent extracts, water layer
The content of middle volatile organic matter substantially reduces, step（3）In the moisture that distills out can greatly reduce waste water with recycled
Yield.
The beneficial effects of the invention are as follows：The purification processing method of Sucralose crystalline mother solution provided by the invention has high return
Yield, less solvent consumption and less waste water generate, with good economic efficiency and social benefit.
Specific implementation mode
Illustrate technical scheme of the present invention below by way of specific embodiment, but the scope of the present invention is not limited thereto.
Embodiment 1
A kind of purification processing method of Sucralose crystalline mother solution, includes the following steps：
（1）The middle addition 3000kg mother liquor of sucralose into extraction kettle adjusts pH to 7；The acetic acid of 750kg is added into extraction kettle
Stirring 0.5h, butyl ester after standing 0.5h, lower aqueous layer is divided to transfer tank, upper layer butyl acetate layer point to butyl acetate storage tank,
It repeats to extract 3 times total；
（2）By step（1）The middle obtained water layer that is layered is transferred in extraction kettle, and the second of mother liquor of sucralose quality 1800kg is added
Acetoacetic ester stirring after standing, lower aqueous layer is divided into mother liquor transfer tank, upper layer ethyl acetate layer point to distillation still, repeats to extract
It takes total 3 times, the content that Sucralose in water layer is surveyed in sampling is less than 5%, and it is to be concentrated to squeeze into storage tank；
（3）Step（2）In obtained water layer be pumped into concentration kettle, be evaporated under reduced pressure in moisture to water layer Sucralose content on 25% left side
The right side, then the mother liquor 3000kg after concentration is transferred back in extraction kettle, the ethyl acetate for adding 1800kg extracts 3 times, specific to grasp
Make same step（2）In extracting operation, when aqueous layer contg is discharged into cesspool less than 2%；Ethyl acetate layer and step（2）In second
Ethyl acetate layer merging decolourizes to produce Sucralose after distillation to finishing room after steaming ethyl acetate；
（4）By step（1）Three batches of butyl acetate layers after middle extracting mother liquid amount to about 9000kg and squeeze into butyl acetate distillation still,
Steam 5000kg butyl acetates postcooling to 35 DEG C plus water stirring, stand after, be added 900kg water stirring 0.5h, stand 0.5h after；
Water layer is divided into transfer tank, again repeatedly step（3）Waste water concentrating, butyl acetate layer continue with 500kg wash 2 times；After washing
Remaining butyl acetate vacuum distillation, cesspool is discharged into after raffinate cooling.
It is computed, the rate of recovery >=98.5% of Sucralose in Sucralose crystalline mother solution is operated according to 1 method of embodiment,
Obtained sucralose purity >=99.6%.
Embodiment 2
A kind of purification processing method of Sucralose crystalline mother solution, includes the following steps：
（1）The middle addition 3000kg mother liquor of sucralose into extraction kettle adjusts pH to 7；The acetic acid of 750kg is added into extraction kettle
Stirring 0.5h, butyl ester after standing 0.5h, lower aqueous layer is divided to transfer tank, upper layer butyl acetate layer point to butyl acetate storage tank,
It repeats to extract 4 times total；
（2）By step（1）The middle obtained water layer that is layered is transferred in extraction kettle, and the second of mother liquor of sucralose quality 1800kg is added
Acetoacetic ester stirring after standing, lower aqueous layer is divided into mother liquor transfer tank, upper layer ethyl acetate layer point to distillation still, repeats to extract
It takes total 4 times, the content that Sucralose in water layer is surveyed in sampling is less than 5%；200kg toluene is added in water layer and extracts ethyl acetate, altogether
After meter extraction 2 times, it is to be concentrated that isolated water layer is squeezed into storage tank；
（3）Step（2）In obtained water layer be pumped into concentration kettle, be evaporated under reduced pressure in moisture to water layer Sucralose content on 30% left side
The right side, then the mother liquor 3000kg after concentration is transferred back in extraction kettle, the ethyl acetate for adding 1800kg extracts 4 times, specific to grasp
Make same step（2）In extracting operation, when aqueous layer contg is discharged into cesspool less than 2%；Ethyl acetate layer and step（2）In second
Ethyl acetate layer merging decolourizes to produce Sucralose after distillation to finishing room after steaming ethyl acetate；The moisture distilled out can cover
With.
（4）By step（1）Three batches of butyl acetate layers after middle extracting mother liquid amount to about 9000kg and squeeze into butyl acetate steaming
Kettle is evaporated, after steaming 5000kg butyl acetates postcooling to 35 DEG C plus water stirring, standing, 900kg water stirring 0.5h is added, stands
After 0.5h；Water layer is divided into transfer tank, again repeatedly step（3）Waste water concentrating, butyl acetate layer continue with 500kg wash 3 times；
Remaining butyl acetate vacuum distillation, cesspool is discharged into after raffinate cooling after washing.
It is computed, the rate of recovery >=98.5% of Sucralose in Sucralose crystalline mother solution is operated according to 2 method of embodiment,
Obtained sucralose purity >=99.6%；The yield of waste water is 20% or so of mother liquor of sucralose volume.
Comparative example
The novel mother liquor extraction process of Sucralose, includes the following steps：
（1）2400kg finished mother liquids and 600kg butyl acetates are added in extraction kettle, stirred 30 minutes, is divided after standing 30 minutes
Upper layer butyl acetate layer is removed, water layer is left, is repeated above operation 4 times；
（2）1800kg ethyl acetate will be added in water layer in n-butyl acetate extraction step, stirs 30 minutes, stands 30 minutes,
Ethyl acetate layer squeezes into distillation still after layering, and water layer continues plus the extraction of 1000kg ethyl acetate, is repeated twice, uses for the last time
Ethyl acetate layer is left to lower batch of mother liquor of processing and uses after the extraction of 1800kg ethyl acetate；
（3）Ethyl acetate layer in ethyl acetate extraction step is concentrated under reduced pressure, ethyl acetate recovery is collected, is evaporated
Afterwards plus water enter finished product decoloration after steam finished mother liquid material again；
（4）Butyl ester distillation still is squeezed by 4 butyl acetate layers are extracted in n-butyl acetate extraction step, 240kg water is added to stir 30 points
Clock stands 30 minutes, and water layer is divided into transfer tank, and butyl ester layer continues plus 240kg water repeats the above process, the decompression of distillation still inner butyl ester
To without outflow, being dissolved in water substantially and being discharged into sewage network, water layer squeezes into finished mother liquid head tank by finished product mother liquid disposal for distillation.
It is computed, the rate of recovery that Sucralose in Sucralose crystalline mother solution is operated according to comparative example method is about 90%, is obtained
To sucralose purity be about 97%；The yield of waste water is 120% or so of mother liquor of sucralose volume.
It is enlightenment with above-mentioned desirable embodiment according to the present invention, through the above description, relevant staff is complete
Various changes and amendments can be carried out without departing from the scope of the technological thought of the present invention' entirely.The technology of this invention
Property range is not limited to the contents of the specification, it is necessary to determine its technical scope according to right.
Claims (9)
1. a kind of purification processing method of Sucralose crystalline mother solution, it is characterised in that include the following steps：
（1）Mother liquor of sucralose is added into extraction kettle, adjusts pH to weakly acidic pH；Mother liquor of sucralose matter is added into extraction kettle
After standing, lower aqueous layer is divided to transfer tank, upper layer butyl acetate layer point to acetic acid fourth for the butyl acetate of amount 1/5 ~ 2/5, stirring
Ester storage tank repeats to extract 2 ~ 4 times total；
（2）By step（1）The middle obtained water layer that is layered is transferred in extraction kettle, and mother liquor of sucralose quality 2/5 ~ 3/5 is added
After standing, lower aqueous layer is divided into mother liquor transfer tank for ethyl acetate stirring, and upper layer ethyl acetate layer point to distillation still repeats
Extraction is 2 ~ 4 times total, and the content that Sucralose in water layer is surveyed in sampling is less than 5%, and it is to be concentrated to squeeze into storage tank；
（3）Step（2）In obtained water layer be pumped into concentration kettle, be evaporated under reduced pressure in moisture to water layer Sucralose content 25% ~
30%, then the mother liquor after concentration is transferred back in extraction kettle, add the ethyl acetate extraction of mother liquor of sucralose quality 2/5 ~ 3/5
Take 2 ~ 4 same steps of concrete operations（2）In extracting operation, when aqueous layer contg is discharged into cesspool less than 2%；Ethyl acetate layer with
Step（2）In ethyl acetate layer merging steam after ethyl acetate to producing Sucralose after finishing room's decoloration distillation；
（4）By step（1）Butyl acetate layer after middle extracting mother liquid squeezes into butyl acetate distillation still, steams 50 ~ 60% mass
Butyl acetate postcooling to 30 ~ 40 DEG C plus water stirring, stand after, be added water quality be residual acetic acid butyl ester quality 20 ~
25%；Water layer is divided into transfer tank, again repeatedly step（3）Waste water concentrating, butyl acetate layer continues washing 1 ~ 3 time；It is remained after washing
Remaining butyl acetate vacuum distillation, cesspool is discharged into after raffinate cooling.
2. the purification processing method of Sucralose crystalline mother solution as described in claim 1, which is characterized in that the step（1）
It is 6.5 ~ 7.5 that middle pH refers specifically to pH to weakly acidic pH.
3. the purification processing method of Sucralose crystalline mother solution as described in claim 1, which is characterized in that the step（1）、
（2）With（4）In, stirring, the specific time stood are 0.2 ~ 1h of stirring, stand 0.2 ~ 1h.
4. the purification processing method of Sucralose crystalline mother solution as described in claim 1, which is characterized in that the step（1）
The butyl acetate quality of middle addition is the 1/5 ~ 1/3 of mother liquor of sucralose quality.
5. the purification processing method of Sucralose crystalline mother solution as claimed in claim 2, which is characterized in that the step（1）
PH is adjusted after extraction again to 6.5 ~ 7.5.
6. such as the purification processing method of claim 1 ~ 5 any one of them Sucralose crystalline mother solution, which is characterized in that described
Step（2）With（3）The each addition of middle ethyl acetate is the 1/2 ~ 3/5 of mother liquor of sucralose quality.
7. the method for the purification processing method such as claim 1 ~ 5 any one of them Sucralose crystalline mother solution, feature exist
In the step（2）In obtained water layer be pumped into before concentration kettle and first extracted 1 ~ 3 time with low polar organic solvent.
8. the method for the purification processing method of Sucralose crystalline mother solution as claimed in claim 7, which is characterized in that described low
Polar organic solvent is selected from hexamethylene, toluene or dichloromethane.
9. the method for the purification processing method of Sucralose crystalline mother solution as claimed in claim 7, which is characterized in that described low
The addition of polar organic solvent is 5 ~ 10%.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111499672A (en) * | 2019-01-30 | 2020-08-07 | 山东新和成精化科技有限公司 | Extraction method for purifying sucralose |
| CN112480186A (en) * | 2020-11-30 | 2021-03-12 | 安徽金禾实业股份有限公司 | Method for treating primary mother liquor of sucralose |
| CN114195837A (en) * | 2021-11-23 | 2022-03-18 | 安徽金禾实业股份有限公司 | Continuous treatment device and method for mother liquor of secondary crude sucralose ester product |
| CN114230620A (en) * | 2021-11-23 | 2022-03-25 | 安徽金禾实业股份有限公司 | Method for treating sucralose crystallization mother liquor |
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| WO2008004246A1 (en) * | 2006-07-06 | 2008-01-10 | Alembic Limited | An improved process for the preparation of sucralose of high purity |
| US20090281295A1 (en) * | 2008-04-03 | 2009-11-12 | Tate & Lyle Technology Limited | Crystallization of sucralose from sucralose-containing feed streams |
| CN103242384A (en) * | 2013-05-27 | 2013-08-14 | 南通市常海食品添加剂有限公司 | Novel sucralose mother liquor extraction process |
| CN104861003A (en) * | 2015-04-24 | 2015-08-26 | 吉安市新琪安科技有限公司 | Sucralose mother liquor processing method |
| CN106674292A (en) * | 2016-12-09 | 2017-05-17 | 福建科宏生物工程股份有限公司 | Method for purification treatment of sucralose water crystallization mother liquor |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| WO2008004246A1 (en) * | 2006-07-06 | 2008-01-10 | Alembic Limited | An improved process for the preparation of sucralose of high purity |
| US20090281295A1 (en) * | 2008-04-03 | 2009-11-12 | Tate & Lyle Technology Limited | Crystallization of sucralose from sucralose-containing feed streams |
| CN103242384A (en) * | 2013-05-27 | 2013-08-14 | 南通市常海食品添加剂有限公司 | Novel sucralose mother liquor extraction process |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111499672A (en) * | 2019-01-30 | 2020-08-07 | 山东新和成精化科技有限公司 | Extraction method for purifying sucralose |
| CN111499672B (en) * | 2019-01-30 | 2021-07-20 | 山东新和成精化科技有限公司 | Extraction method for purifying sucralose |
| CN112480186A (en) * | 2020-11-30 | 2021-03-12 | 安徽金禾实业股份有限公司 | Method for treating primary mother liquor of sucralose |
| CN114195837A (en) * | 2021-11-23 | 2022-03-18 | 安徽金禾实业股份有限公司 | Continuous treatment device and method for mother liquor of secondary crude sucralose ester product |
| CN114230620A (en) * | 2021-11-23 | 2022-03-25 | 安徽金禾实业股份有限公司 | Method for treating sucralose crystallization mother liquor |
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