CN106365952A - Method for solvent self-heating separation in acesulfame potassium synthesis - Google Patents
Method for solvent self-heating separation in acesulfame potassium synthesis Download PDFInfo
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- CN106365952A CN106365952A CN201610751007.6A CN201610751007A CN106365952A CN 106365952 A CN106365952 A CN 106365952A CN 201610751007 A CN201610751007 A CN 201610751007A CN 106365952 A CN106365952 A CN 106365952A
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C17/00—Preparation of halogenated hydrocarbons
- C07C17/38—Separation; Purification; Stabilisation; Use of additives
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C17/00—Preparation of halogenated hydrocarbons
- C07C17/38—Separation; Purification; Stabilisation; Use of additives
- C07C17/383—Separation; Purification; Stabilisation; Use of additives by distillation
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07D—HETEROCYCLIC COMPOUNDS
- C07D291/00—Heterocyclic compounds containing rings having nitrogen, oxygen and sulfur atoms as the only ring hetero atoms
- C07D291/02—Heterocyclic compounds containing rings having nitrogen, oxygen and sulfur atoms as the only ring hetero atoms not condensed with other rings
- C07D291/06—Six-membered rings
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- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The invention discloses a method for solvent self-heating separation in acesulfame potassium synthesis. The method includes the following steps of pumping solid potassium hydroxide and water of the conventional adding percents into a reactor to make potassium hydroxide and water dissolved in a neutralization kettle and release heat till the temperature is naturally raised to 60 DEG C, starting a vacuum pump connected with the neutralization kettle to vacuumize the neutralization kettle to the negative pressure of -0.4 MPa, pumping an organic phase of the conventional adding percent into the reactor to make the temperature in the kettle naturally decrease and then increase, starting the vacuum pump to conduct vacuumization till a condenser valve when the temperature of the kettle is raised to 50 DEG C, starting the condenser brine valve, controlling the temperature of the kettle at 45 DEG C by controlling the feeding ratio of the organic phase to sodium carbonate, and discharging condensed dichloromethane to a solvent collecting tank through a condenser. The method has the advantages that solvent is pressurized in the reactor and depressurized after getting out of the reactor, the boiling point of the solvent is reduced, original processes of separating, washing, separating, pre-boiling and the like are omitted through temperature control, operation is simplified, labor intensity is reduced, machines and pumps are less used, and meanwhile lots of steam is saved.
Description
Technical field
The present invention relates to acesulfame potassium synthesis technique field, particularly a kind of acesulfame potassium synthesize in neutralization reaction from thermal release
Method.
Background technology
At present in acesulfame potassium synthesis and production process, as shown in figure 1, neutralization dichloromethane separation phase complex process, be first
By former dichloromethane with sugar and water mixture by separating through stratification, then proceed to organic faciess groove, then through washing, washing
Stratification separates again afterwards, enters back into thick steaming, could use for rectification, not only needs in the process to add large number quipments, and
And a large amount of loss of phase heat energy need to be taken away with saline before manufacture, the later stage needs to consume a large amount of steam, capacity usage ratio by heating
Lowly, waste seriously.
Content of the invention
The purpose of the present invention is aiming in prior art isolation technics there is process complexity, and post operation step is many, machine
The shortcoming that pump uses in a large number and steam usage amount is big, provides solvent self-heating separation method in a kind of acesulfame potassium synthesis.
The purpose of the present invention is achieved by the following technical programs:
Solvent self-heating separation method in a kind of acesulfame potassium synthesis, comprises the following steps:
1) solid potassium hydroxide of conventional proportions amount and water are first pumped into reactor, make their exothermic dissolutions in neutralization kettle natural
It is warming up to 60 DEG C；
2) open the vacuum pump being connected with neutralization kettle, negative pressure -0.4mpa will be pumped in neutralization kettle；
3) organic faciess of conventional proportions amount are pumped in reactor, temperature in the kettle self-assembling formation first reduces and raises afterwards；
4) kettle temperature is increased to 50 DEG C, opens vacuum pump and is vented to condenser valve；
5) open condenser saline valve, by controlling the pan feeding ratio of organic faciess and soda, control kettle temperature at 45 DEG C；
6) condenser discharges the dichloromethane of condensation to solvent groove.
Technical scheme, using solid potassium hydroxide exothermic dissolution and neutralization reaction heat release, in the reactor plus
Pressure, reduces pressure after going out reactor, reduces solvent boiling point, so that dichloromethane is being evaporated rapidly after reactor, through condensing back
Receive and directly use for rectification.
The invention has the advantages that: solvent pressurizes in the reactor, reduce pressure after going out reactor, reduce solvent boiling point, pass through
Temperature control, removes the processes such as original separation, washing, separation, pre- steaming, simplifies operation, reduce labor intensity, reduce pump
Use, save a large amount of steam simultaneously.
Brief description
Fig. 1 is neutralization reaction solvent fractionation method flow chart in existing acesulfame potassium synthesis technique；
Fig. 2 neutralizes from hot solvent separation process figure in the acesulfame potassium synthesis technique of the present invention.
Specific embodiment
As shown in Fig. 2 the present invention provides solvent self-heating separation method in a kind of acesulfame potassium synthesis, using exothermic dissolution with instead
Answer heat release, pressurize in the reactor, reduce pressure after going out reactor, reduce solvent boiling point, make dichloromethane after reactor
Rapid evaporation, reclaims through condensation and replaces original standing separation, washing, the process such as separate, steam in advance again
Concrete operation step:
7) solid potassium hydroxide 0.6t/h and water 5t/h are first pumped into reactor, make neutralization kettle kettle temperature naturally rise to 60 DEG C.
8) open vacuum pump, negative pressure -0.4mpa will be pumped in neutralization kettle.
9) by organic faciess 10m3/ h pumps into temperature in the kettle in reactor first to be reduced and raises afterwards.
10) kettle temperature is increased to 50 DEG C, opens emptying to condenser valve.
11) open condenser saline valve, by controlling the organic faciess of organic faciess and the pan feeding ratio of soda, control kettle temperature to exist
45℃.
The present invention removes the processes such as original separation, washing, separation, pre- steaming, simplifies operation, reduces labor intensity.Reduce
Ice maker and the use of pump, save a large amount of steam simultaneously.780,000 degree of estimated annual using electricity wisely, 4000 tons of annual steam saving.
Above-described embodiment, as the better embodiment of the present invention, is described in detail the technology design of the present invention and implements to want
Point, is not that protection scope of the present invention is limited, all according to spirit of the invention made any simple modification and
Equivalent structure transformation or modification, all should be included within the scope of the present invention.
Claims (1)
1. solvent self-heating separation method in a kind of acesulfame potassium synthesis, comprises the following steps:
The solid potassium hydroxide of conventional proportions amount and water are first pumped into reactor, so that their exothermic dissolutions in neutralization kettle is naturally risen
Temperature is to 60 DEG C；
Open the vacuum pump being connected with neutralization kettle, negative pressure -0.4mpa will be pumped in neutralization kettle；
The organic faciess of conventional proportions amount are pumped in reactor, temperature in the kettle self-assembling formation first reduces and raises afterwards；
Kettle temperature is increased to 50 DEG C, opens vacuum pump and is vented to condenser valve；
Open condenser saline valve, by controlling the pan feeding ratio of organic faciess and soda, control kettle temperature at 45 DEG C；
Condenser discharges the dichloromethane of condensation to solvent groove.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610751007.6A CN106365952B (en) | 2016-08-30 | 2016-08-30 | Solvent self-heating separation method in a kind of synthesis of acesulfame potassium |
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|---|---|---|---|
| CN201610751007.6A CN106365952B (en) | 2016-08-30 | 2016-08-30 | Solvent self-heating separation method in a kind of synthesis of acesulfame potassium |
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| CN106365952A true CN106365952A (en) | 2017-02-01 |
| CN106365952B CN106365952B (en) | 2018-10-26 |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US10023546B2 (en) | 2016-09-21 | 2018-07-17 | Celanese International Corporation | Acesulfame potassium compositions and processes for producing same |
| US10029999B2 (en) | 2016-09-21 | 2018-07-24 | Celanese International Corporation | Acesulfame potassium compositions and processes for producing same |
| US10030000B2 (en) | 2016-09-21 | 2018-07-24 | Celanese International Corporation | Acesulfame potassium compositions and processes for producing same |
| US10029998B2 (en) | 2016-09-21 | 2018-07-24 | Celanese International Corporation | Acesulfame potassium compositions and processes for producing same |
| CN109593071A (en) * | 2018-12-10 | 2019-04-09 | 安徽金禾实业股份有限公司 | A kind of continuous controllable acesulfame potassium recrystallization centrifugal device and method |
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Cited By (25)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US10590098B2 (en) | 2016-09-21 | 2020-03-17 | Celanese International Corporation | Acesulfame potassium compositions and processes for producing same |
| US10208004B2 (en) | 2016-09-21 | 2019-02-19 | Celanese International Corporation | Acesulfame potassium compositions and processes for producing same |
| US10023546B2 (en) | 2016-09-21 | 2018-07-17 | Celanese International Corporation | Acesulfame potassium compositions and processes for producing same |
| US10029998B2 (en) | 2016-09-21 | 2018-07-24 | Celanese International Corporation | Acesulfame potassium compositions and processes for producing same |
| US10759771B2 (en) | 2016-09-21 | 2020-09-01 | Celanese International Corporation | Acesulfame potassium compositions and processes for producing same |
| US10227316B2 (en) | 2016-09-21 | 2019-03-12 | Celanese International Corporation | Acesulfame potassium compositions and processes for producing same |
| US10233163B2 (en) | 2016-09-21 | 2019-03-19 | Celanese International Corporation | Acesulfame potassium compositions and processes for producing same |
| US10759770B2 (en) | 2016-09-21 | 2020-09-01 | Celanese International Corporation | Acesulfame potassium compositions and processes for producing same |
| US11731948B2 (en) | 2016-09-21 | 2023-08-22 | Celanese International Corporation | Acesulfame potassium compositions and processes for producing same |
| US10590095B2 (en) | 2016-09-21 | 2020-03-17 | Celanese International Corporation | Acesulfame potassium compositions and processes for producing same |
| US10590096B2 (en) | 2016-09-21 | 2020-03-17 | Celenese International Corporation | Acesulfame potassium compositions and processes for producing same |
| US10590097B2 (en) | 2016-09-21 | 2020-03-17 | Celanese International Corporation | Acesulfame potassium compositions and processes for producing same |
| US10030000B2 (en) | 2016-09-21 | 2018-07-24 | Celanese International Corporation | Acesulfame potassium compositions and processes for producing same |
| US10029999B2 (en) | 2016-09-21 | 2018-07-24 | Celanese International Corporation | Acesulfame potassium compositions and processes for producing same |
| US10233164B2 (en) | 2016-09-21 | 2019-03-19 | Celanese International Corporation | Acesulfame potassium compositions and processes for producing same |
| US10781190B2 (en) | 2016-09-21 | 2020-09-22 | Celanese International Corporation | Acesulfame potassium compositions and processes for producing same |
| US10781191B2 (en) | 2016-09-21 | 2020-09-22 | Celanese International Corporation | Acesulfame potassium compositions and processes for producing same |
| US10954203B2 (en) | 2016-09-21 | 2021-03-23 | Celanese International Corporation | Acesulfame potassium compositions and processes for producing same |
| US10954204B2 (en) | 2016-09-21 | 2021-03-23 | Celanese International Corporation | Acesulfame potassium compositions and processes for producing same |
| US10961207B2 (en) | 2016-09-21 | 2021-03-30 | Celanese International Corporation | Acesulfame potassium compositions and processes for producing same |
| US10975047B2 (en) | 2016-09-21 | 2021-04-13 | Celanese International Corporation | Acesulfame potassium compositions and processes for producing same |
| US11718594B2 (en) | 2016-09-21 | 2023-08-08 | Celanese International Corporation | Acesulfame potassium compositions and processes for producing same |
| US11724993B2 (en) | 2016-09-21 | 2023-08-15 | Celanese International Corporation | Acesulfame potassium compositions and processes for producing same |
| US11724994B2 (en) | 2016-09-21 | 2023-08-15 | Celanese International Corporation | Acesulfame potassium compositions and processes for producing same |
| CN109593071A (en) * | 2018-12-10 | 2019-04-09 | 安徽金禾实业股份有限公司 | A kind of continuous controllable acesulfame potassium recrystallization centrifugal device and method |
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| CN106365952B (en) | 2018-10-26 |
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Denomination of invention: Method for solvent self-heating separation in acesulfame potassium synthesis Effective date of registration: 20191113 Granted publication date: 20181026 Pledgee: Bank of China Limited Chuzhou Branch Pledgor: Anhui Jinhe Stock Co., Ltd. Registration number: Y2019340000196 |
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Date of cancellation: 20210115 Granted publication date: 20181026 Pledgee: Bank of China Limited Chuzhou Branch Pledgor: ANHUI JINGHE INDUSTRIAL Co.,Ltd. Registration number: Y2019340000196 |