CN109503680A - A kind of trichloro-cane-6-ethyl ester mother liquor ester phase processor method - Google Patents
A kind of trichloro-cane-6-ethyl ester mother liquor ester phase processor method Download PDFInfo
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- CN109503680A CN109503680A CN201811516319.4A CN201811516319A CN109503680A CN 109503680 A CN109503680 A CN 109503680A CN 201811516319 A CN201811516319 A CN 201811516319A CN 109503680 A CN109503680 A CN 109503680A
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- kettle
- ester
- crude product
- mother liquor
- cane
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07H—SUGARS; DERIVATIVES THEREOF; NUCLEOSIDES; NUCLEOTIDES; NUCLEIC ACIDS
- C07H13/00—Compounds containing saccharide radicals esterified by carbonic acid or derivatives thereof, or by organic acids, e.g. phosphonic acids
- C07H13/02—Compounds containing saccharide radicals esterified by carbonic acid or derivatives thereof, or by organic acids, e.g. phosphonic acids by carboxylic acids
- C07H13/04—Compounds containing saccharide radicals esterified by carbonic acid or derivatives thereof, or by organic acids, e.g. phosphonic acids by carboxylic acids having the esterifying carboxyl radicals attached to acyclic carbon atoms
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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 relates to a kind of trichloro-cane-6-ethyl ester mother liquor ester phase processor method, comprising the following steps: 1), obtained the first crude product mother solution ester of filters pressing mutually enter the first concentration kettle through decoloration, obtain the first concentrate；3), the first concentrate is put into the first crystallization kettle decrease temperature crystalline, obtains a filters pressing crude product investment crude product ester and is tied in molten material kettle again, the crude product ester crystallized ties mother liquor again and removes extraction kettle；4), filters pressing obtains a crude product mother solution and send the dense dry kettle concentration of mother liquor plus demineralized water, aqueous layer after layering enters once washing water phase slot, upper layer washing water, which enters, extracts miscellaneous kettle, layering obtains water phase after removal of impurities ester mutually sends the dense dry kettle of mother liquor, removal of impurities back to and is sent into extraction kettle, aqueous phase extracted send dense dry kettle, ester mutually to send to the second concentration kettle and the second crystallization kettle, obtains secondary crude product and enters crude product ester and ties molten material kettle again.The present invention has the advantages that cleaning to mother liquor washing water, makes washing water is recyclable to apply, reduce blowdown flow rate, trichloro-cane-6-ethyl ester content reaches 99% or more, Sucralose product quality is substantially improved.
Description
Technical field
The present invention relates to food additives production fields, are related to a kind of Sucralose production technology, and in particular to Yi Zhongsan
Chlorine sucrose-6-ethyl ester wastewater treatment method.
Background technique
Sucralose is a kind of white powder product, is highly soluble in water (solubility 28.2g, 20 °C), sugariness is sucrose
600 times, and sweet taste is pure.Sucralose category non-nutritive intense sweetener, is hardly absorbed, calorie value in human body
It is zero.Sucralose property is stablized, and it is many to be widely used in beverage, chewing gum, chocolate etc. for Sucralose substitution sucrose at present
It is one of comparatively ideal intense sweetener in the market in kind.
Sucralose industrially is produced frequently with monoesters method, in Sucralose production, after chlorination and neutralization reaction,
Purification by liquid extraction need to be carried out using organic solvent to the intermediate trichloro-cane-6-ethyl ester that reaction generates, can generate in purification process
A large amount of waste water contains a small amount of trichloro-cane-6-ethyl ester, organic solvent in waste water, contains more trichlorine in organic solvent
Sucrose-6-ethyl ester.At present in industrial production, the mother liquor for using ethyl acetate to obtain as filters pressing after extractant extraction is layered
The organic layer generated afterwards gets to the dense dry kettle recycling organic solvent of mother liquor, and adds pure stirring after dense dry, is put into washing kettle
Stratification deslagging, sugar residue take part trichloro-cane-6-ethyl ester out of and cause the wasting of resources.
Summary of the invention
The purpose of the present invention is to defect existing in the prior art, a kind of trichloro-cane-6-ethyl ester provided is female
Liquid ester phase processor method is recycled, Sucralose-as far as possible by handling trichloro-cane-6-ethyl ester mother liquor ester phase layer
6- ethyl ester reduces consumption.
To achieve the above object, The technical solution adopted by the invention is as follows:
A kind of trichloro-cane-6-ethyl ester mother liquor ester phase processor method is included in Sucralose production, chlorination and neutralization reaction knot
Shu Hou need to carry out purification by liquid extraction step using organic solvent to the intermediate trichloro-cane-6-ethyl ester that reaction generates, press after extraction
Filter obtained mother liquor, the organic layer generated after mother liquor layering is got to after dense dry kettle returns and isolate solvent, dense dry liquid is obtained,
Be characterized in that the following steps are included:
1), the crystal solution for adding ethyl acetate to obtain dense dry liquid, the first crude product mother solution obtained after filters pressing enter the first crude product
Mother liquor is layered slot, and the first crude product mother solution ester phase 8000L being layered is sent into decoloration kettle addition active carbon and carries out heating decoloration, controls
Bleaching temperature processed is 50 DEG C -60 DEG C, circulation heat preservation 1 hour, trichloro-cane-6-ethyl ester in destainer containing 30-40g/l,
A small amount of dichloro ester and more chlorine esters, DMF and extractant ethyl acetate；
2) after, decolourizing, by several times to the first concentration kettle into destainer, it is first put into 5000L destainer into the first concentration kettle, opens
Stirring and vacuum pump, the control of slow warming temperature take off extractant ethyl acetate at 35~40 DEG C, when 3000L acetic acid second is concentrated out
After ester, then remaining 3000L destainer entered into the first concentration kettle, destainer total volume is by 8m3It is concentrated to 2.6m3, contained
First concentration of the trichloro-cane-6-ethyl ester of 70-90g/l, a small amount of dichloro ester and more chlorine esters, DMF and extractant ethyl acetate
Liquid；
3) after, being concentrated, the first concentrate is put into the first crystallization kettle decrease temperature crystalline, 0~5 DEG C of crystallization temperature, freezes 10 hours
Laggard first filter press filters pressing obtains a filters pressing crude product, and a filters pressing crude product investment crude product ester is tied again in molten material kettle, second is added
The molten sugar of acetoacetic ester removes organic impurities, is put into ester knot kettle after molten material, by crystallizing filters pressing, removes the crude product ester obtained after a crude product
Knot mother liquor pump removes extraction kettle again；
4) 6000L demineralized water is added after being sent into the dense dry kettle concentration of mother liquor in, the crude product mother solution obtained by the first filter press,
Stirring was put into once washing kettle stratification after 1 hour, entered once washing water containing trichloro-cane-6-ethyl ester water layer after layering
A large amount of dichloro esters, more chlorine esters, denaturation trichloro-cane-6-ethyl ester and a small amount of Sucralose-are contained after static layering by phase slot in lower layer
The slag blanket of 6- ethyl ester is directly exhausted into deslagging kettle；
5) the upper layer washing water 4000L pump in once washing water phase slot, is squeezed into the miscellaneous kettle of extraction, is added 500L's in miscellaneous kettle to extracting
Extractant ethyl acetate carries out atmospheric extraction, and water phase and ester phase after removal of impurities after layering is cleaned, it is dense that removal of impurities ester mutually sends mother liquor back to
Dry kettle carries out repeating concentration；
6) water phase 4500L is sent into extraction kettle after the removal of impurities, being layered, and the crude product ester for merging a filters pressing crude product ties mother liquor again
3000L extracts the Sucralose 6- ethyl ester in liquid in extraction kettle, and it is dense that the aqueous phase extracted obtained after layering sends to neutralization
Dry kettle uses, and ester is mutually stored in organic phase slot for use after the extraction sugar being layered；
7) it when, ester mutually saves 3 batches in organic phase slot after extraction sugar, send to the second concentration kettle and is concentrated, control concentration kettle temperature
Degree is 40-50 DEG C, when organic phase is concentrated into 2500L, organic phase is sent to the second crystallization kettle, the freezing and crystallizing 10 under the conditions of 0 DEG C
After hour, filters pressing is carried out using the second filter press, obtains secondary crude product trichloro-cane-6-ethyl ester and secondary crude product mother solution, it is secondary thick
Product enter crude product ester and tie the molten material of molten material kettle progress again, are recrystallized with ester knot kettle is combined into after a molten material of crude product；It is secondary
Crude product mother solution is sent to the dense dry kettle of mother liquor and is concentrated.
The present invention has the advantages that cleaning to mother liquor washing water, makes washing water is recyclable to apply, reduce blowdown flow rate.
Since material impurity is largely removed, trichloro-cane-6-ethyl ester content reaches 99% or more, makes Sucralose product quality substantially
It is promoted.
Detailed description of the invention
Fig. 1 is process flow chart of the invention.
Specific embodiment
A kind of trichloro-cane-6-ethyl ester mother liquor ester phase processor method provided by the invention is included in Sucralose production,
After chlorination and neutralization reaction, the intermediate trichloro-cane-6-ethyl ester that need to be generated to reaction is extracted using organic solvent
Purification step, the mother liquor which uses ethyl acetate to obtain as filters pressing after extractant extraction, what is generated after mother liquor layering has
After machine phase layer gets to dense dry kettle separation and recovery solvent, dense dry liquid is obtained, specific implementation step is as follows:
1) crystal solution for adding ethyl acetate to obtain dense dry liquid, the first crude product mother solution obtained after filters pressing enter the first crude product mother solution
It is layered slot, the first crude product mother solution ester phase 8000L being layered is sent into decoloration kettle addition active carbon and carries out heating decoloration, and control is de-
Color temperature is 50 DEG C -60 DEG C, circulation heat preservation 1 hour, trichloro-cane-6-ethyl ester in destainer containing 30-40g/l, a small amount of
Dichloro ester and more chlorine esters, DMF and extractant ethyl acetate.
2) after decolourizing, by several times to the first concentration kettle into destainer, 5000L decoloration is first put into the first concentration kettle
Liquid, opens stirring and vacuum pump, and slow warming temperature control takes off extractant ethyl acetate at 35~40 DEG C, when 3000L second is concentrated out
After acetoacetic ester, then remaining 3000L destainer entered into the first concentration kettle, destainer total volume is by 8m3It is concentrated to 2.6m3, obtain
The first of trichloro-cane-6-ethyl ester containing 70-90g/l, a small amount of dichloro ester and more chlorine esters, DMF and extractant ethyl acetate is dense
Contracting liquid.
3) after being concentrated, the first concentrate is put into the first crystallization kettle decrease temperature crystalline, and 0~5 DEG C of crystallization temperature, freezing 10 is small
Shi Houjin the first filter press filters pressing, the side-blown pressure of filters pressing obtain a filters pressing crude product in 6KG, 3 hours total times, primary pressure
Filter crude product investment crude product ester is tied again in molten material kettle, is added the molten sugar of ethyl acetate to remove organic impurities, ester knot kettle is put into after molten material, by knot
Brilliant filters pressing, filters pressing, which removes obtained crude product ester after a crude product, ties mother liquor pump again and removes extraction kettle.
4) 6000L desalination is added after being sent into the dense dry kettle concentration of mother liquor in the crude product mother solution obtained by the first filter press
Water, stirring are put into once washing kettle standing and are layered for 4 hours after 1 hour, 30g/l or so Sucralose -6- is contained after layering
Ethyl ester water layer enters once washing water phase slot, and a large amount of dichloro esters, more chlorine esters, denaturation trichlorine sugarcane are contained in lower layer after static layering
The slag blanket of sugar -6- ethyl ester and a small amount of trichloro-cane-6-ethyl ester is directly exhausted into deslagging kettle；
5) the upper layer washing water 4000L pump in once washing water phase slot is squeezed into the miscellaneous kettle of extraction, is added 500L's in miscellaneous kettle to extracting
Extractant ethyl acetate carries out atmospheric extraction, and extraction time is stirring 1 hour, stands 2 hours.Water phase after layering is cleaned
With ester phase after removal of impurities, the ester that cleans mutually sends the dense dry kettle of mother liquor back to and carries out repeating concentration.
6) water phase 4500L is sent into extraction kettle after the removal of impurities being layered into step 5), merges the thick of a filters pressing crude product
Product ester ties mother liquor 3000L again, extracts to the Sucralose 6- ethyl ester in liquid in extraction kettle, and the time is stirring 1 hour, quiet
It sets 2 hours, the aqueous phase extracted obtained after layering, which is sent to, neutralizes Nong Gan workshop section (dense dry kettle) use, and the organic phase being layered is (i.e.
Ester phase after extraction sugar) it is stored in organic phase slot for use；
7) it when the organic phase being layered in step 6) saves 3 batches in organic phase slot, send to the second concentration kettle and is concentrated,
Controlling concentration kettle temperature is 40-50 DEG C, when organic phase is concentrated into 2500L, and organic phase is sent to the second crystallization kettle and is carried out, at 0 DEG C
Under the conditions of after freezing and crystallizing 10 hours, using the second filter press carry out filters pressing, obtain secondary crude product trichloro-cane-6-ethyl ester (about
280KG) and secondary crude product mother solution, secondary crude product, which enters crude product ester and ties molten material kettle again, carries out molten material, and closes after a molten material of crude product
And it is recrystallized into ester knot kettle.Secondary crude product mother solution is sent to the dense dry kettle of mother liquor and is concentrated.
The invention has the advantages that can increase within 1 year about 18 tons of Sucralose yield, 1 year reduction wastewater discharge is about
4800 tons, trichloro-cane-6-ethyl ester purity improves nearly 1%, has greatly saved the energy, reduces blowdown, reduces costs,
Increase benefit.
Claims (1)
1. a kind of trichloro-cane-6-ethyl ester mother liquor ester phase processor method is included in Sucralose production, chlorination and neutralization reaction
After, purification by liquid extraction step need to be carried out using organic solvent to the intermediate trichloro-cane-6-ethyl ester that reaction generates, after extraction
The mother liquor that filters pressing obtains, the organic layer that generates is got to after dense dry kettle returns and isolate solvent after mother liquor layering, obtains dense dry liquid,
Characterized by the following steps:
1), the crystal solution for adding ethyl acetate to obtain dense dry liquid, the first crude product mother solution obtained after filters pressing enter the first crude product
Mother liquor is layered slot, and the first crude product mother solution ester phase 8000L being layered is sent into decoloration kettle addition active carbon and carries out heating decoloration, controls
Bleaching temperature processed is 50 DEG C -60 DEG C, circulation heat preservation 1 hour, trichloro-cane-6-ethyl ester in destainer containing 30-40g/l,
A small amount of dichloro ester and more chlorine esters, DMF and extractant ethyl acetate；
2) after, decolourizing, by several times to the first concentration kettle into destainer, it is first put into 5000L destainer into the first concentration kettle, opens
Stirring and vacuum pump, the control of slow warming temperature take off extractant ethyl acetate at 35~40 DEG C, when 3000L acetic acid second is concentrated out
After ester, then remaining 3000L destainer entered into the first concentration kettle, destainer total volume is by 8m3It is concentrated to 2.6m3, contained
First concentration of the trichloro-cane-6-ethyl ester of 70-90g/l, a small amount of dichloro ester and more chlorine esters, DMF and extractant ethyl acetate
Liquid；
3) after, being concentrated, the first concentrate is put into the first crystallization kettle decrease temperature crystalline, 0~5 DEG C of crystallization temperature, freezes 10 hours
Laggard first filter press filters pressing obtains a filters pressing crude product, and a filters pressing crude product investment crude product ester is tied again in molten material kettle, second is added
The molten sugar of acetoacetic ester removes organic impurities, is put into ester knot kettle after molten material, by crystallizing filters pressing, removes the crude product ester obtained after a crude product
Knot mother liquor pump removes extraction kettle again；
4) 6000L demineralized water is added after being sent into the dense dry kettle concentration of mother liquor in, the crude product mother solution obtained by the first filter press,
Stirring was put into once washing kettle stratification after 1 hour, entered once washing water containing trichloro-cane-6-ethyl ester water layer after layering
A large amount of dichloro esters, more chlorine esters, denaturation trichloro-cane-6-ethyl ester and a small amount of Sucralose-are contained after static layering by phase slot in lower layer
The slag blanket of 6- ethyl ester is directly exhausted into deslagging kettle；
5) the upper layer washing water 4000L pump in once washing water phase slot, is squeezed into the miscellaneous kettle of extraction, is added 500L's in miscellaneous kettle to extracting
Extractant ethyl acetate carries out atmospheric extraction, and water phase and ester phase after removal of impurities after layering is cleaned, it is dense that removal of impurities ester mutually sends mother liquor back to
Dry kettle carries out repeating concentration；
6) water phase 4500L is sent into extraction kettle after the removal of impurities, being layered, and the crude product ester for merging a filters pressing crude product ties mother liquor again
3000L extracts the Sucralose 6- ethyl ester in liquid in extraction kettle, and it is dense that the aqueous phase extracted obtained after layering sends to neutralization
Dry kettle uses, and ester is mutually stored in organic phase slot for use after the extraction sugar being layered；
7) it when, ester mutually saves 3 batches in organic phase slot after extraction sugar, send to the second concentration kettle and is concentrated, control concentration kettle temperature
Degree is 40-50 DEG C, when organic phase is concentrated into 2500L, organic phase is sent to the second crystallization kettle, the freezing and crystallizing 10 under the conditions of 0 DEG C
After hour, filters pressing is carried out using the second filter press, obtains secondary crude product trichloro-cane-6-ethyl ester and secondary crude product mother solution, it is secondary thick
Product enter crude product ester and tie the molten material of molten material kettle progress again, are recrystallized with ester knot kettle is combined into after a molten material of crude product；It is secondary
Crude product mother solution is sent to the dense dry kettle of mother liquor and is concentrated.
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| CN201811516319.4A CN109503680A (en) | 2018-12-12 | 2018-12-12 | A kind of trichloro-cane-6-ethyl ester mother liquor ester phase processor method |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112125938A (en) * | 2020-09-26 | 2020-12-25 | 安徽金禾实业股份有限公司 | Method for extracting sucralose-6-ethyl ester from sugar residues |
| CN112457356A (en) * | 2020-11-30 | 2021-03-09 | 安徽金禾实业股份有限公司 | Method for removing ethyl ester from secondary esterified crude product in sucralose production |
| CN113677689A (en) * | 2021-07-07 | 2021-11-19 | 安徽金禾实业股份有限公司 | Method for purifying sucralose-6-ester |
| 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 |
| WO2022099606A1 (en) * | 2020-11-13 | 2022-05-19 | 安徽金禾实业股份有限公司 | Method for purifying sucralose |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103012509A (en) * | 2012-12-13 | 2013-04-03 | 福建科宏生物工程有限公司 | Method of separating and purifying sucrose-6-acetate mother liquor by salt fractionation |
| 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 |
| CN108191929A (en) * | 2018-01-13 | 2018-06-22 | 安徽金禾实业股份有限公司 | A kind of trichloro-cane-6-ethyl ester wastewater treatment method |
| CN108299522A (en) * | 2018-01-13 | 2018-07-20 | 安徽金禾实业股份有限公司 | A kind of extracting process of trichloro-cane-6-ethyl ester |
-
2018
- 2018-12-12 CN CN201811516319.4A patent/CN109503680A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103012509A (en) * | 2012-12-13 | 2013-04-03 | 福建科宏生物工程有限公司 | Method of separating and purifying sucrose-6-acetate mother liquor by salt fractionation |
| 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 |
| CN108191929A (en) * | 2018-01-13 | 2018-06-22 | 安徽金禾实业股份有限公司 | A kind of trichloro-cane-6-ethyl ester wastewater treatment method |
| CN108299522A (en) * | 2018-01-13 | 2018-07-20 | 安徽金禾实业股份有限公司 | A kind of extracting process of trichloro-cane-6-ethyl ester |
Non-Patent Citations (1)
| Title |
|---|
| 朱建锋: "低造价三氯蔗糖生产线的设计", 《中国优秀博硕士学位论文全文数据库（硕士） 工程科技I辑》 * |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112125938A (en) * | 2020-09-26 | 2020-12-25 | 安徽金禾实业股份有限公司 | Method for extracting sucralose-6-ethyl ester from sugar residues |
| WO2022099606A1 (en) * | 2020-11-13 | 2022-05-19 | 安徽金禾实业股份有限公司 | Method for purifying sucralose |
| CN112457356A (en) * | 2020-11-30 | 2021-03-09 | 安徽金禾实业股份有限公司 | Method for removing ethyl ester from secondary esterified crude product in sucralose production |
| CN113677689A (en) * | 2021-07-07 | 2021-11-19 | 安徽金禾实业股份有限公司 | Method for purifying sucralose-6-ester |
| 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 |
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Application publication date: 20190322 |