CN109575069A - The recovery method of catalyst in a kind of production of Sucralose - Google Patents
The recovery method of catalyst in a kind of production of Sucralose Download PDFInfo
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- CN109575069A CN109575069A CN201811504670.1A CN201811504670A CN109575069A CN 109575069 A CN109575069 A CN 109575069A CN 201811504670 A CN201811504670 A CN 201811504670A CN 109575069 A CN109575069 A CN 109575069A
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- acetic acid
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- acid esters
- organotin
- hexamethylene
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Abstract
The present invention relates to the recovery methods of catalyst in a kind of production of Sucralose, comprising the following steps: a. will be acylated liquid heating control at 60-70 DEG C, stand the heat preservation small layered of 1-3 and obtain machine tin acetic acid esters phase and syrup phase；B. organotin acetic acid esters phase is isolated, mutually fills into hexamethylene in syrup, is stirred 1 hour at 40 DEG C or so；C. stratification goes out syrup phase, and then 60-100 DEG C of decompression of hexamethylene phase control temperature steams hexamethylene, leaves the organotin acetic acid esters that machine tin acetic acid esters merges upper step, participates in Sucralose esterification reaction as catalyst and reuses.The invention has the advantages that reducing the cost recovery of organotin acetic acid esters to the maximum extent, and improve the site environment in recycling post.Reduce solvent and steam consumption, protect environment, realize zero-emission, so that entire production procedure is realized that reaction efficiency and material utilization optimize, hence it is evident that increase Business Economic Benefit.
Description
Technical field
The present invention relates to the recovery methods of organotin acetic acid esters in a kind of production of Sucralose.
Background technique
Organotin recycles in traditional Sucralose production technology, mainly by following procedure: being dissolved in after acylation reaction
Organotin in solution exists in the form of organotin acetic acid esters (DSDA), by the way that the extraction of extractant hexamethylene is added, forms DMF
(- 6 ester of N, N- dimethylformamide, water and sucrose) layer and extract layer, organotin acetic acid esters (DSDA) are dissolved in the hexamethylene of extract layer
In alkane phase, hexamethylene is mutually placed in distillation still by being dissolved after steam heating recovery extractant hexamethylene with methanol after layering
DSDA is simultaneously pumped into high-order dropping tank, is added drop-wise in the organotin recycling kettle for being placed with sodium hydroxide solution in advance, then opens steam and add
Methanol is recycled in thermal evaporation, contains organotin solid in remaining water phase, is then placed in centrifuge and is centrifugated, with a large amount of water
It is washed till neutrality, process reaction is related to methanol, liquid alkaline, pure water, and water consumption is big, generates a large amount of sewage and needs to handle.
The technology passes through multiple technological progress, can be direct after the solvent hexamethylene of organotin acetic acid esters (DSDA) removing at present
It applies, eliminates recovery processing step compared with traditional handicraft, and reduce waste water.But DSDA recovery yield is unstable
It is fixed, and solvent hexamethylene and steam consumption are still very big.
Summary of the invention
The object of the invention is in order to overcome ring present in existing recycling organotin acetic acid esters (DSDA) recovery method
Hexane and the big disadvantage of steam consumption, the recycling new method of organotin acetic acid esters (DSDA) in the Sucralose production provided.
To achieve the goals above, present invention employs following technical solutions:
Acylation reaction generates acylated liquid in the recovery method of organotin, including Sucralose production in a kind of production of Sucralose,
Characterized by the following steps:
A. will acylated liquid heating control at 60-70 DEG C, stand 1-3 small layered of heat preservation obtain machine tin acetic acid esters DSDA phase and
Syrup phase；
B. organotin acetic acid esters DSDA phase is first isolated, the hexamethylene of 10%-30% volume syrup phase is then filled into syrup phase,
It is stirred 1 hour at 40 DEG C or so；
C. stratification first isolates syrup phase, and then 60-100 DEG C of decompression of hexamethylene phase control temperature steams hexamethylene, stays
Lower machine tin acetic acid esters DSDA merges the organotin acetic acid esters DSDA that step b is isolated, and then will merge the organotin acetic acid of recycling
Ester DSDA as catalyst, reuse by the esterification participated in Sucralose production.
The invention has the advantages that
1, production cost is further decreased, reduces the cost recovery of organotin acetic acid esters to the maximum extent, and improves recycling hilllock
The site environment of position.
2, reduce solvent and steam consumption, protect environment.Now with new technique, zero-emission is realized, is made whole
A production procedure realizes that reaction efficiency and material utilization optimize, hence it is evident that increases Business Economic Benefit.
Detailed description of the invention
Fig. 1 is process flow chart of the invention.
Specific implementation method
1, acylation liquid (- 6 ester of N, N- dimethylformamide, the water and sucrose, organotin acetic acid esters) 5000L obtained esterification
With being pumped into extraction kettle, steam is opened, rises 65 DEG C of temperature, heat preservation stands 1 hour, and acylated liquid natural layering forms syrup phase
With machine tin acetic acid esters phase.
Acylated liquid is warming up to 65 DEG C or more and is layered, and does not need to add extractant hexamethylene.And traditional handicraft is to pass through addition
A large amount of hexamethylenes are extracted into organotin acetic acid esters in acylated liquid in hexamethylene phase, and re-evaporation hexamethylene isolates organotin acetic acid
Ester.Here do not need that hexamethylene is added, but by improving acylated liquid temperature, so that it is flat to influence acylated liquid system liquid liquid phase
Weighing apparatus, by N in acylated liquid, N- dimethylformamide, water and -6 ester of sucrose and organotin acetic acid esters (65 DEG C of fusing point) are separated.
, lower layer's organotin acetic acid esters mutually separated to catalyst carrier, syrup mutually stays in and uses circulating water cooling in extraction kettle
To 40 DEG C.
3,500L hexamethylene is filled into extraction kettle from head tank, 40 DEG C of extractions are stirred 1 hour, after being then allowed to stand 1 hour
Form layering syrup phase and hexamethylene phase；
4, lower layer's syrup after layering is mutually separated into syrup slot, upper layer 500L hexamethylene mutually stays in extraction kettle, opens vacuum
Pump opens steam for hexamethylene heat phase to 100 DEG C of thorough recycling hexamethylenes to hexamethylene slot.Normal hexamethylene boiling point is 80.7
DEG C, then most of hexamethylene is i.e. recyclable at 81 DEG C, but since hexamethylene mutually has other substances such as organotin acetic acid esters, meeting
Azeotropic system is formed with hexamethylene and part hexamethylene is caused to be difficult to recycle, therefore our hexamethylenes are mutually warming up to 100 DEG C, just stop
Non-return receives extractant hexamethylene.
6. closing steam valve, opening cooling water makes material in extraction kettle be cooled to 70 DEG C, then by extraction kettle bottom organotin acetic acid
Ester is put into catalyst carrier；
7. finally regarding the organotin acetic acid esters (DSDA) of recycling as catalyst, returns to esterifying kettle participation esterification and repeat to make
With.
Organotin acetic acid esters DSDA participates in reaction as catalyst and generates cane sugar-6-acetic ester intermediate, acyl in the present invention
Change liquid (N, N- dimethylformamide, water and cane sugar-6-acetic ester, organotin acetic acid esters) through heat up extraction and separation go out syrup phase (N,
N- dimethylformamide, water and cane sugar-6-acetic ester) and about 90% organotin acetic acid esters phase (DSDA).Syrup phase (N, N- diformazan
Base amide, water and cane sugar-6-acetic ester) a small amount of hexamethylene extraction is added, the organotin acetic acid esters (DSDA) for accounting for about 10% is extracted
It takes out, then the hexamethylene is concentrated, merge organotin acetic acid esters phase (DSDA), directly recycle.
The above described is only a preferred embodiment of the present invention, being not intended to limit the present invention in any form；Appoint
What those skilled in the art, without departing from the scope of the technical proposal of the invention, all using the side of the disclosure above
Method and technology contents make many possible changes and modifications to technical solution of the present invention, or are revised as the equivalent reality of equivalent variations
Apply example.Therefore, anything that does not depart from the technical scheme of the invention according to the technical essence of the invention do above embodiments
Any simple modification, equivalent replacement, equivalence changes and modification, all of which are still within the scope of protection of the technical scheme of the invention.
Claims (1)
1. the recovery method of catalyst in a kind of Sucralose production, including acylation reaction generates acylation in Sucralose production
Liquid, it is characterised in that the following steps are included:
A. will acylated liquid heating control at 60-70 DEG C, stand 1-3 small layered of heat preservation obtain machine tin acetic acid esters DSDA phase and
Syrup phase；
B. organotin acetic acid esters DSDA phase is first isolated, the hexamethylene of 10%-30% volume syrup phase is then filled into syrup phase,
It is stirred 1 hour at 40 DEG C or so；
C. stratification first isolates syrup phase, and then 60-100 DEG C of decompression of hexamethylene phase control temperature steams hexamethylene, stays
Lower machine tin acetic acid esters DSDA merges the organotin acetic acid esters DSDA that step b is isolated, and then will merge the organotin acetic acid of recycling
Ester DSDA as catalyst, reuse by the esterification participated in Sucralose production.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201811504670.1A CN109575069A (en) | 2018-12-10 | 2018-12-10 | The recovery method of catalyst in a kind of production of Sucralose |
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| CN201811504670.1A CN109575069A (en) | 2018-12-10 | 2018-12-10 | The recovery method of catalyst in a kind of production of Sucralose |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114133411A (en) * | 2021-11-23 | 2022-03-04 | 安徽金禾实业股份有限公司 | Method for extracting floccules from sucralose |
| CN114225438A (en) * | 2021-11-23 | 2022-03-25 | 安徽金禾实业股份有限公司 | Method for continuously concentrating sucralose tin ester |
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| EP0455390A2 (en) * | 1990-04-23 | 1991-11-06 | McNEIL-PPC, INC. | Process for delivery of organotin esters from reaction mixtures containing the same and re-use of the recovered organotin compounds |
| US5470969A (en) * | 1990-08-27 | 1995-11-28 | Mcneil-Ppc, Inc. | Catalyzed sucrose-6-ester process |
| US20110087018A1 (en) * | 2009-10-12 | 2011-04-14 | Tate & Lyle Technology Limited | Low Temperature, Single Solvent Process for the Production of Sucrose-6-Ester |
| US20120095199A1 (en) * | 2009-03-31 | 2012-04-19 | Tate & Lyle Technology Ltd. | Based-Assisted formation of Tin-Sucrose Adducts |
| US20120289693A1 (en) * | 2011-05-10 | 2012-11-15 | Tate & Lyle Technology Limited | Extraction of Carboxylic Acids with Tin Compounds |
| CN103130843A (en) * | 2013-01-21 | 2013-06-05 | 溧阳维信生物科技有限公司 | Method of recycling and reusing of dibutyltin oxide in process of cane sugars manufacturing cane suger-6-ethyl ester |
| CN105111246A (en) * | 2015-08-22 | 2015-12-02 | 安徽金禾实业股份有限公司 | Method for recycling organic tin in sucralose production |
| CN105601665A (en) * | 2015-12-30 | 2016-05-25 | 浙江新和成股份有限公司 | Treatment method of dibutyltin oxide and application of treatment method to synthesis of cane sugar-6-ethyl ester |
| CN107011394A (en) * | 2017-05-02 | 2017-08-04 | 林洪 | The acetic acid esters list solvent preparation of sucrose 6 of Dibutyltin oxide catalysis |
| CN108178445A (en) * | 2018-01-10 | 2018-06-19 | 福建科宏生物工程股份有限公司 | A kind of processing method of Sucralose production middle and high concentration organic liquid waste |
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2018
- 2018-12-10 CN CN201811504670.1A patent/CN109575069A/en active Pending
Patent Citations (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP0455390A2 (en) * | 1990-04-23 | 1991-11-06 | McNEIL-PPC, INC. | Process for delivery of organotin esters from reaction mixtures containing the same and re-use of the recovered organotin compounds |
| US5470969A (en) * | 1990-08-27 | 1995-11-28 | Mcneil-Ppc, Inc. | Catalyzed sucrose-6-ester process |
| US20120095199A1 (en) * | 2009-03-31 | 2012-04-19 | Tate & Lyle Technology Ltd. | Based-Assisted formation of Tin-Sucrose Adducts |
| US20110087018A1 (en) * | 2009-10-12 | 2011-04-14 | Tate & Lyle Technology Limited | Low Temperature, Single Solvent Process for the Production of Sucrose-6-Ester |
| US20120289693A1 (en) * | 2011-05-10 | 2012-11-15 | Tate & Lyle Technology Limited | Extraction of Carboxylic Acids with Tin Compounds |
| CN103130843A (en) * | 2013-01-21 | 2013-06-05 | 溧阳维信生物科技有限公司 | Method of recycling and reusing of dibutyltin oxide in process of cane sugars manufacturing cane suger-6-ethyl ester |
| CN105111246A (en) * | 2015-08-22 | 2015-12-02 | 安徽金禾实业股份有限公司 | Method for recycling organic tin in sucralose production |
| CN105601665A (en) * | 2015-12-30 | 2016-05-25 | 浙江新和成股份有限公司 | Treatment method of dibutyltin oxide and application of treatment method to synthesis of cane sugar-6-ethyl ester |
| CN107011394A (en) * | 2017-05-02 | 2017-08-04 | 林洪 | The acetic acid esters list solvent preparation of sucrose 6 of Dibutyltin oxide catalysis |
| CN108178445A (en) * | 2018-01-10 | 2018-06-19 | 福建科宏生物工程股份有限公司 | A kind of processing method of Sucralose production middle and high concentration organic liquid waste |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114133411A (en) * | 2021-11-23 | 2022-03-04 | 安徽金禾实业股份有限公司 | Method for extracting floccules from sucralose |
| CN114225438A (en) * | 2021-11-23 | 2022-03-25 | 安徽金禾实业股份有限公司 | Method for continuously concentrating sucralose tin ester |
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Application publication date: 20190405 |