CN109503361B - Method and device for extracting organic tin from sodium acetate as byproduct of sucralose - Google Patents
Method and device for extracting organic tin from sodium acetate as byproduct of sucralose Download PDFInfo
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- CN109503361B CN109503361B CN201811504135.6A CN201811504135A CN109503361B CN 109503361 B CN109503361 B CN 109503361B CN 201811504135 A CN201811504135 A CN 201811504135A CN 109503361 B CN109503361 B CN 109503361B
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- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C51/00—Preparation of carboxylic acids or their salts, halides or anhydrides
- C07C51/42—Separation; Purification; Stabilisation; Use of additives
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Abstract
The invention relates to a method and a device for extracting organic tin from sodium acetate as a byproduct of sucralose, which are characterized by comprising the following steps: (1) adding 450-550L of cyclohexane, 600-800 Kg of oily matter and 150-250L of DMF into an organic tin recovery kettle, stirring for 30min, heating to evaporate the cyclohexane, and keeping the temperature in the kettle at 65-75 ℃ for standing for 60min for layering; (2) dripping the lower layer into sodium hydroxide with the concentration of 4-6% to generate a mixed granular substance, and then washing and centrifuging; (3) adding 450-550L of cyclohexane, the mixed granular substances and 150-250L of DMF (dimethyl formamide) into a cyclohexane recovery kettle, adding 160-180 Kg of acetic anhydride, heating, adding 150-200L of water, stirring for 30min, and standing for 1h for layering; (4) removing DMF from the lower layer, concentrating to recover DMF, returning the concentrated residue to the esterification working section, and recovering organic tin; the upper layer is left in the kettle and heated to recover cyclohexane. The invention has the advantages that: by discontinuously recovering the oily substances, the content of the oily substances in the sodium acetate mother liquor is reduced, the processing capacity of a sodium acetate device is improved, the environmental protection pressure is reduced, the energy is saved, the emission is reduced, and the benefit is improved.
Description
Technical Field
The invention belongs to the technical field of chemical engineering, relates to the field of sucralose production, and particularly relates to a method and a device for extracting organic tin from sodium acetate additionally produced by sucralose.
Background
In the production process of sucralose, the acidic DMF at the DMF recovery working section severely restricts the development of the sucralose industry, the acidic DMF has high DMF content and contains a large amount of sodium acetate, and the prior treatment process (the patent publication No. CN 108358807A) adopts the steps of dissolving, decoloring, filtering, centrifuging and the like to remove impurities to obtain industrial grade sodium acetate; however, in the process of sodium acetate treatment, oily substances (organotin and organotin decomposition products) in the mother liquor are enriched, which causes difficult crystallization and centrifugation, reduces the treatment capacity of the sodium acetate treatment device and brings certain pressure to environmental protection.
Disclosure of Invention
The invention aims to solve the problems of low processing capacity and high environmental protection pressure of a sodium acetate processing device caused by high content of oily matters in a by-product sodium acetate mother liquor, and provides a method and a device for extracting organic tin in sodium acetate as a byproduct of sucralose.
In order to achieve the purpose, the technical scheme adopted by the invention is as follows:
an organic tin extraction device in sodium acetate as a byproduct of sucralose is characterized by adopting the following equipment:
a. the cyclohexane tank and the DMF tank are respectively connected with an inlet of an organic tin recovery kettle through pipelines, an outlet at the top of the organic tin recovery kettle is connected with the cyclohexane tank, and the bottom of the organic kettle is connected with a centrifuge;
b. the outlet of the centrifuge is connected with a cyclohexane recovery kettle through a pipeline;
c. the cyclohexane tank, the DMF tank, the purified water tank and the acetic anhydride tank are respectively connected with an inlet of a cyclohexane recovery kettle through pipelines, and an outlet at the bottom of the cyclohexane recovery kettle is connected to a DMF concentration working section through a pipeline.
A method for extracting organic tin from sodium acetate as a byproduct of sucralose comprises the steps of adding liquid alkali to neutralize the existing acidic DMF, crystallizing, performing pressure filtration, performing primary crystallization, performing secondary crystallization, and centrifugally recovering sodium acetate, and is characterized by comprising the following steps:
(1) adding 450-550L of cyclohexane into an organic tin recovery kettle, putting 600-800 Kg of oily matters (organic tin and organic tin decomposers) collected from a centrifugal working section (on a stainless steel filter screen of a centrifugal machine) into the organic tin recovery kettle, then adding 150-250L of DMF, stirring for 30min, slowly heating by starting steam (70-80 ℃) to evaporate the cyclohexane, and then keeping the temperature in the organic recovery kettle at 65-75 ℃ and standing for 60min for layering;
(2) dropwise adding the layered lower heavy phase layer (organic tin and DMF) into sodium hydroxide with the concentration of 4-6%, reacting for 30min to generate mixed granular substances (organic tin and a small amount of decomposition products), feeding the mixed granular substances into a centrifuge, and washing and centrifuging; concentrating the upper layer light phase, recovering cyclohexane and then removing sewage treatment stations;
(3) adding 450-550L of cyclohexane into a cyclohexane recovery kettle, putting the mixed granular substance obtained after centrifugation in the step (2) into the cyclohexane recovery kettle, adding 150-250L of DMF, dropwise adding 160-180 Kg of acetic anhydride while stirring, heating to fully dissolve the mixed granular substance, adding 150-200L of water, stirring for 30min, stopping stirring, and standing for 1h for layering;
(4) the layered lower layer (DMF and a small amount of organic tin) is sent to a DMF concentration working section to recover DMF (DMF returns to the system and is extracted once by a small amount of cyclohexane before being used again), and the concentrated remainder is returned to an esterification working section to carry out inverse catalytic treatment to recover the organic tin; the upper layer (cyclohexane) is left in a cyclohexane recovery kettle, and the cyclohexane is recovered by heating and raising the temperature.
The invention has the advantages that: the oily substance is intermittently recovered, and the content of the oily substance in the sodium acetate mother liquor is reduced, so that the processing capacity of a sodium acetate device is improved, the production requirement of sucralose products is met, the yield of sucralose is improved, the environmental protection pressure is reduced, energy is saved, emission is reduced, and the benefit is improved.
Drawings
FIG. 1 is a schematic diagram of a process for extracting organotin from sodium acetate as an by-product of sucralose.
Detailed Description
The technical scheme is further explained by combining the figure 1:
an organic tin extraction element in sucralose by-product sodium acetate, includes following equipment:
a. the cyclohexane tank and the DMF tank are respectively connected with an inlet of an organic tin recovery kettle through pipelines, an outlet at the top of the organic tin recovery kettle is connected with the cyclohexane tank, and the bottom of the organic tin recovery kettle is connected with a centrifugal machine;
b. the outlet of the centrifuge is connected with a cyclohexane recovery kettle through a pipeline;
c. the cyclohexane tank, the DMF tank, the purified water tank and the acetic anhydride tank are respectively connected with an inlet of a cyclohexane recovery kettle through pipelines, and an outlet at the bottom of the cyclohexane recovery kettle is connected to a DMF concentration working section through a pipeline.
Example 1
A method for extracting organic tin from sodium acetate byproduct of sucralose comprises the following specific implementation steps:
(1) adding 500L of cyclohexane into an organic tin recovery kettle, putting 600Kg of oily matters (organic tin and organic tin decomposition products) collected from a centrifugal working section (on a stainless steel filter screen of a centrifugal machine) into the organic tin recovery kettle, then adding 200L of DMF, stirring for 30min, slowly heating by opening steam (70-80 ℃) to evaporate the cyclohexane, and then keeping the temperature in the organic recovery kettle at 65-75 ℃ and standing for 60min for layering;
(2) dropwise adding the layered lower heavy phase layer (organic tin and DMF) into 4-6% sodium hydroxide, reacting for 30min to generate mixed granular substances, feeding the mixed granular substances into a centrifuge, and washing and centrifuging; concentrating the upper layer light phase, recovering cyclohexane and then removing sewage treatment stations;
(3) adding 500L of cyclohexane into a cyclohexane recovery kettle, putting the mixed granular substance obtained after centrifugation in the step (2) into the cyclohexane recovery kettle, adding 200L of DMF, dropwise adding 175Kg of acetic anhydride while stirring, heating to fully dissolve the mixed granular substance, adding 150L of water, stirring for 30min, stopping stirring, and standing for 1h for layering;
(4) the layered lower layer (DMF and a small amount of organic tin) is sent to a DMF concentration working section to recover DMF (DMF returns to the system and is extracted once by a small amount of cyclohexane before being used again), and the concentrated remainder is returned to an esterification working section to carry out inverse catalytic treatment to recover the organic tin; the upper layer (cyclohexane) is left in a cyclohexane recovery kettle, and the cyclohexane is recovered by heating and raising the temperature.
Claims (1)
1. A method for extracting organic tin from sodium acetate as a byproduct of sucralose comprises the steps of adding liquid alkali into the existing acidic DMF for neutralization, crystallization, filter pressing, primary crystallization, secondary crystallization and centrifugal recovery of sodium acetate, and is characterized by adopting the following equipment:
a. the cyclohexane tank and the DMF tank are respectively connected with an inlet of an organic tin recovery kettle through pipelines, an outlet at the top of the organic tin recovery kettle is connected with the cyclohexane tank, and the bottom of the organic kettle is connected with a centrifuge;
b. the outlet of the centrifuge is connected with a cyclohexane recovery kettle through a pipeline;
c. the cyclohexane tank, the DMF tank, the purified water tank and the acetic anhydride tank are respectively connected with an inlet of a cyclohexane recovery kettle through pipelines, and an outlet at the bottom of the cyclohexane recovery kettle is connected to a DMF concentration working section through a pipeline;
the method comprises the following steps:
(1) adding 450-550L of cyclohexane into an organic tin recovery kettle, putting 600-800 Kg of oily matter collected from a centrifugal working section into the organic tin recovery kettle, then adding 150-250L of DMF, stirring for 30min, starting steam to slowly heat and evaporate the cyclohexane, and then keeping the temperature in the organic recovery kettle at 65-75 ℃ and standing for 60min for layering;
(2) dropwise adding the layered lower heavy phase layer into 4-6% sodium hydroxide, reacting for 30min to generate mixed granular substances, feeding the mixed granular substances into a centrifuge, and washing and centrifuging; concentrating the upper layer light phase, recovering cyclohexane and then removing sewage treatment stations;
(3) adding 450-550L of cyclohexane into a cyclohexane recovery kettle, putting the mixed granular substance obtained after centrifugation in the step (2) into the cyclohexane recovery kettle, adding 150-250L of DMF, dropwise adding 160-180 Kg of acetic anhydride while stirring, heating to fully dissolve the mixed granular substance, adding 150-200L of water, stirring for 30min, stopping stirring, and standing for 1h for layering;
(4) the layered lower layer is sent to a DMF concentration working section to recover DMF, and the concentrated remainder is returned to an esterification working section to perform inverse catalysis treatment to recover organic tin in the concentrated remainder; the upper layer is left in a cyclohexane recovery kettle, and the cyclohexane is recovered by heating and raising the temperature.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201811504135.6A CN109503361B (en) | 2018-12-10 | 2018-12-10 | Method and device for extracting organic tin from sodium acetate as byproduct of sucralose |
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| CN201811504135.6A CN109503361B (en) | 2018-12-10 | 2018-12-10 | Method and device for extracting organic tin from sodium acetate as byproduct of sucralose |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN110590832A (en) * | 2019-08-15 | 2019-12-20 | 安徽金禾实业股份有限公司 | Purification method of organotin acetate recovered in sucralose production |
| WO2023279277A1 (en) * | 2021-07-07 | 2023-01-12 | 安徽金禾实业股份有限公司 | Method for preparing organotin-sucrose complex |
Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5470969A (en) * | 1990-08-27 | 1995-11-28 | Mcneil-Ppc, Inc. | Catalyzed sucrose-6-ester process |
| 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 |
| CN108358807A (en) * | 2018-01-13 | 2018-08-03 | 安徽金禾实业股份有限公司 | The recovery and treatment method and device of a kind of acidity DMF and waste residue sodium acetate |
Family Cites Families (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107158755A (en) * | 2017-06-21 | 2017-09-15 | 山东康宝生化科技有限公司 | The separator and method of hexamethylene DMF sucrose ester organotin mixed systems |
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Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5470969A (en) * | 1990-08-27 | 1995-11-28 | Mcneil-Ppc, Inc. | Catalyzed sucrose-6-ester process |
| 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 |
| CN108358807A (en) * | 2018-01-13 | 2018-08-03 | 安徽金禾实业股份有限公司 | The recovery and treatment method and device of a kind of acidity DMF and waste residue sodium acetate |
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