CN109678912A - A kind of processing method of Sucralose neutralizer concentrated residue - Google Patents
A kind of processing method of Sucralose neutralizer concentrated residue Download PDFInfo
- Publication number
- CN109678912A CN109678912A CN201811506092.5A CN201811506092A CN109678912A CN 109678912 A CN109678912 A CN 109678912A CN 201811506092 A CN201811506092 A CN 201811506092A CN 109678912 A CN109678912 A CN 109678912A
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- CN
- China
- Prior art keywords
- dope
- neutralizer
- cane
- trichloro
- ethyl ester
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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
-
- 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
-
- 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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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Health & Medical Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Engineering & Computer Science (AREA)
- Biochemistry (AREA)
- Biotechnology (AREA)
- General Health & Medical Sciences (AREA)
- Genetics & Genomics (AREA)
- Molecular Biology (AREA)
- Extraction Or Liquid Replacement (AREA)
- Processing Of Solid Wastes (AREA)
Abstract
The present invention relates to a kind of processing methods of Sucralose neutralizer concentrated residue, comprising the following steps: 1) neutralizer is dissolved in water after being concentrated under reduced pressure and is put into insulation still, and active carbon stirring and adsorbing dope is added；2) supernatant layer from side port is put into standing slot in insulation still after standing；3) filters pressing after clear liquid stands half an hour, removes active carbon and dope, gained filtrate add ethyl acetate to extract trichloro-cane-6-ethyl ester；4) dope retained in insulation still adds water and heating stirring, is put into washery slag kettle by bottom valve；5) solution for being put into washery slag kettle adds water and stirs heating, after 80 DEG C keep the temperature 3 hours, solution obtains waste residue filter cake through filters pressing and send solid waste center in washery slag kettle, and 25~30g/l of trichloro-cane-6-ethyl ester content send purification workshop section in obtained filtrate, and slag washing water set uses molten syrup after neutralizer is concentrated under reduced pressure.It is of the invention a little: the problem of effective solution cleaning subsider, recycled trichloro-cane-6-ethyl ester to greatest extent, reduced the pollution to environment.
Description
Technical field
The present invention relates to food additives production fields, and in particular to a kind of Sucralose neutralizer concentrated residue processing side
Method.
Background technique
In Sucralose production, after chlorated liquid removes chlorination ammonium salt and partially carbonized object after neutralizing, need to neutralizer
Vacuum distillation recycling trichloroethanes and DMF are carried out, due to 153 DEG C of DMF boiling point and Sucralose and its intermediate are all thermal sensitivity
Substance is often also easy to produce thick by-product during being recovered under reduced pressure.These by-products need to remove, after otherwise bringing into
Plane system influences product quality.The measure being usually taken look for a groove settled inside dope, extract clear liquid above
Carry out filters pressing, often settle it is insufficient cause canvas press cloth be plugged can not filters pressing, filter cloth replacing frequency is high.Subsider glues
Thick object is not easily cleaned, and people has to be dug into tank with spade, since sticky cleaning once needs 3-4 hours；The dope cleaned up
It is put into small iron car, because the inside has carried about 20% trichloro-cane-6-ethyl ester secretly, causes material waste, and be transported in solid waste
The heart can only be put in trolley, and conevying efficiency is low.
Summary of the invention
It is an object of the invention to efficiently separate out the residue dope generated when neutralizer concentration, trichlorine sugarcane is reduced
Sugar -6- ethyl ester follows dope to be pulled away, energy saving, reduces cost, increases benefit.
The technical solution adopted by the present invention to solve the technical problems is:
A kind of processing method of Sucralose neutralizer concentrated residue, including existing chlorination, neutralization procedure, further include following step
It is rapid:
1) neutralizer is dissolved in water after being concentrated under reduced pressure and is put into insulation still, controls trichloro-cane-6-ethyl ester external standard content in solution
In 80~90g/l, it is added the active carbon of the 0.4-0.6% of total solution weight, stirring and adsorbing dope 1 hour, insulation still temperature control
System is at 55 ± 5 DEG C；
2) stirring terminates after standing 2 hours, opens insulation still middle and lower part side port valve, supernatant layer is put into quiet from side port in insulation still
Set slot, by side port visor observation do not allow dope to standing slot；
3) filters pressing after clear liquid standing half an hour in slot is stood, removes active carbon and dope in clear liquid, gained filtrate adds acetic acid second
Ester extracts trichloro-cane-6-ethyl ester, the processing of water phase decontamination water station；
4) dope retained in insulation still adds water and is put into washery slag kettle by bottom valve after heating stirring half an hour；
5) solution for being put into washery slag kettle adds water and stirs heating, keeps the temperature 3 hours at 80 ± 2 DEG C, after heat preservation, solution in washery slag kettle
Waste residue filter cake is obtained through filters pressing, filter cake loading jumbo bag is sent to solid waste center, filter cake analysis contains trichloro-cane-6-ethyl ester 3.67%, obtains
To 25~30g/l of filtrate analysis trichloro-cane-6-ethyl ester content send purification workshop section, slag washing water set use neutralizer reduced pressure
Molten syrup afterwards.
The beneficial effects of the present invention are:
1, the obtained waste residue of new process is the filter cake pressed dry, is packed into jumbo bag and transports solid waste center to, not only facilitates clean but also safety collar
It protects.
2, the problem of new process effective solution manual cleaning subsider need to enter tank, eliminates worker and enters tank and cause
It the risks such as is poisoned, suffocates, getting injured by a fall.
3, the implementation of new process substantially increases manufacturing schedule, avoids time delayed because clearing up subsider and dense
Dry canvas press cloth plug-hole difficulty filters pressing obtains problem.
4, new process is greatly saved manually, and 2 employees have been saved compared with old technique.
5, new process has recycled trichloro-cane-6-ethyl ester to greatest extent, improves production yield, reduces consumption, subtracts
Processing cost and the pollution to environment are lacked.
Detailed description of the invention
Fig. 1 is process flow chart of the invention.
Present invention will be further explained below with reference to the attached drawings and examples.
Specific embodiment
1, after neutralizer is concentrated under reduced pressure plus the dissolution of 5000L water is put into insulation still, controls trichloro-cane-6-ethyl ester in solution
External standard content adds generation active carbon in 80~90g/l, and the active carbon after refinement use can be used is applied, and dosage exists
The 0.4-0.6% of total solution weight, stirring and adsorbing dope (the predominantly miscellaneous sugar and its coking, carbide of side reaction generation) 1 are small
When, insulation still temperature is controlled at 55 ± 5 DEG C.
2, stirring terminates after standing 2 hours, opens insulation still middle and lower part side port valve, supernatant layer (main three in insulation still
Chlorine sucrose-6-ethyl ester and a small amount of Sucralose dichloro ester, tetrachloro ester and DMF) from side port it is put into standing slot, pass through side port visor
Observation do not allow dope to standing slot.
Filters pressing after the standing half an hour stillness of night in slot is stood, wherein a small amount of active carbon and dope, gained filtrate add second for removing
Acetoacetic ester extracts trichloro-cane-6-ethyl ester, the processing of water phase decontamination water station.
3, the dope retained in insulation still assembles after 3-5 kettle (side port valve to bottom about 500L) or from insulation still
When side port blowing observation visor has dope outflow, the dope that insulation still is retained adds 1500L water and heating stirring half is small
When after washery slag kettle is put by bottom valve；
4, plus the dope after water is in washery slag kettle plus the stirring of 1500L water heats up, and keeps the temperature 3 hours at 80 ± 2 DEG C.
5, after keeping the temperature, solution obtains waste residue filter cake through filters pressing in washery slag kettle, and filter cake loading jumbo bag is sent to solid waste center,
Filter cake analysis contains trichloro-cane-6-ethyl ester 3.67%, and obtained filtrate analysis trichloro-cane-6-ethyl ester 25~30g/l of content is washed
Pulp water set uses molten sugar after neutralizer is concentrated under reduced pressure.
Claims (1)
1. a kind of processing method of Sucralose neutralizer concentrated residue, including existing chlorination, neutralization procedure, it is characterised in that
It is further comprising the steps of:
1) neutralizer is dissolved in water after being concentrated under reduced pressure and is put into insulation still, controls trichloro-cane-6-ethyl ester external standard content in solution
In 80~90g/l, it is added the active carbon of the 0.4-0.6% of total solution weight, stirring and adsorbing dope 1 hour, insulation still temperature control
System is at 55 ± 5 DEG C；
2) stirring terminates after standing 2 hours, opens insulation still middle and lower part side port valve, supernatant layer is put into quiet from side port in insulation still
Set slot, by side port visor observation do not allow dope to standing slot；
3) filters pressing after clear liquid standing half an hour in slot is stood, removes active carbon and dope in clear liquid, gained filtrate adds acetic acid second
Ester extracts trichloro-cane-6-ethyl ester, the processing of water phase decontamination water station；
4) dope retained in insulation still adds water and is put into washery slag kettle by bottom valve after heating stirring half an hour；
5) solution for being put into washery slag kettle adds water and stirs heating, keeps the temperature 3 hours at 80 ± 2 DEG C, after heat preservation, solution in washery slag kettle
Waste residue filter cake is obtained through filters pressing, filter cake loading jumbo bag is sent to solid waste center, filter cake analysis contains trichloro-cane-6-ethyl ester 3.67%, obtains
To 25~30g/l of filtrate analysis trichloro-cane-6-ethyl ester content send purification workshop section, slag washing water set use neutralizer reduced pressure
Molten syrup afterwards.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201811506092.5A CN109678912B (en) | 2018-12-10 | 2018-12-10 | Method for treating concentrated residue of sucralose neutralized solution |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201811506092.5A CN109678912B (en) | 2018-12-10 | 2018-12-10 | Method for treating concentrated residue of sucralose neutralized solution |
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| Publication Number | Publication Date |
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| CN109678912A true CN109678912A (en) | 2019-04-26 |
| CN109678912B CN109678912B (en) | 2022-03-04 |
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| Application Number | Title | Priority Date | Filing Date |
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| CN201811506092.5A Active CN109678912B (en) | 2018-12-10 | 2018-12-10 | Method for treating concentrated residue of sucralose neutralized solution |
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Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102516320A (en) * | 2011-12-23 | 2012-06-27 | 盐城捷康三氯蔗糖制造有限公司 | Method for recovering sucralose-6-ester from chlorination residues |
| CN102816188A (en) * | 2012-08-13 | 2012-12-12 | 南通市常海食品添加剂有限公司 | Production technology of sucralose |
| CN108047283A (en) * | 2018-01-10 | 2018-05-18 | 福建科宏生物工程股份有限公司 | The method for subsequent processing of chlorination in a kind of Sucralose production |
| 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 |
| CN108191927A (en) * | 2018-01-10 | 2018-06-22 | 福建科宏生物工程股份有限公司 | The removal methods of inorganic salts and organic impurities in a kind of Sucralose chloro liquid |
| CN108249460A (en) * | 2018-01-13 | 2018-07-06 | 安徽金禾实业股份有限公司 | In a kind of Sucralose and the processing method of press filtration workshop section ammonium chloride waste residue |
-
2018
- 2018-12-10 CN CN201811506092.5A patent/CN109678912B/en active Active
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102516320A (en) * | 2011-12-23 | 2012-06-27 | 盐城捷康三氯蔗糖制造有限公司 | Method for recovering sucralose-6-ester from chlorination residues |
| CN102816188A (en) * | 2012-08-13 | 2012-12-12 | 南通市常海食品添加剂有限公司 | Production technology of sucralose |
| CN108047283A (en) * | 2018-01-10 | 2018-05-18 | 福建科宏生物工程股份有限公司 | The method for subsequent processing of chlorination in a kind of Sucralose production |
| CN108191927A (en) * | 2018-01-10 | 2018-06-22 | 福建科宏生物工程股份有限公司 | The removal methods of inorganic salts and organic impurities in a kind of Sucralose chloro liquid |
| 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 |
| CN108249460A (en) * | 2018-01-13 | 2018-07-06 | 安徽金禾实业股份有限公司 | In a kind of Sucralose and the processing method of press filtration workshop section ammonium chloride waste residue |
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| Publication number | Publication date |
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| CN109678912B (en) | 2022-03-04 |
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