CN107868064A - A kind of method that 3,4-Dihydro-6-methyl-1,2,3-oxathiazin-4-one 2,2-dioxide potassium salt precursor ASH is synthesized in micro passage reaction - Google Patents
A kind of method that 3,4-Dihydro-6-methyl-1,2,3-oxathiazin-4-one 2,2-dioxide potassium salt precursor ASH is synthesized in micro passage reaction Download PDFInfo
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- C07—ORGANIC CHEMISTRY
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- 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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Abstract
The present invention provides the technique that acesulfame potassium (3,4-Dihydro-6-methyl-1,2,3-oxathiazin-4-one 2,2-dioxide potassium salt) is synthesized in a kind of micro passage reaction, and in particular to the key reaction in the technique --- precursor ASH Cyclization；Its main technical schemes is：By the SO that the reaction intermediate acetoacetyl amido sulfonic acid triethylamine raw material and mass concentration of concentration 20~60% are 25~100%3Cyclizing agent is transported in micro passage reaction 1 and is cyclized, and the cyclisation liquid of generation continuously enters is hydrolyzed reaction with water in micro passage reaction 2, obtain precursor ASH.In cyclisation and hydrolytic process, cyclisation and hydrolysis heat are removed rapidly using integrated micro-channel heat exchanger：Cyclization temperature control is at 30~10 DEG C.With existing caldron process ratio, the reaction time of the invention is short, and cyclization temperature is high, SO3The solvent load of cyclizing agent is few；ASK total recoverys 45~60%, can continuous operation.
Description
Technical field
The technique for synthesizing acesulfame potassium (3,4-Dihydro-6-methyl-1,2,3-oxathiazin-4-one 2,2-dioxide potassium salt) in micro passage reaction the present invention relates to one kind, and in particular in the technique
Key reaction --- precursor ASH Cyclization, i.e., in microchannel cyclisation, acesulfame potassium precursor is synthesized in hydrolysis reactor：6-
Methyl -3,4- dihydro -1,2,3- oxygen thiazine -4- ketone -2,2- dioxide (ASH).
Background technology
ASH be it is a kind of can with alkali formed acyl group sulfanilate compound, scientific name：6- methyl -3,4- dihydro -1,2,3- oxygen
Thiazine -4- ketone -2,2- dioxide, its generated after neutralizing with KOH nontoxic sylvite --- acesulfame potassium is that one kind is widely used in
The sweetener of food, dairy products and beverage industry.The characteristics of with readily soluble, high sugariness, empty calory and not being metabolized.
In the method for all synthesis acesulfame potassiums at present, such as：Using chlorine or fluorosulfonyl isocyanates as initiation material and work
The preparation method of property methylene compound addition, with chlorine or fluorosulfonyl isocyanates catabolite aminosulfonyl fluorine or aminosulfonyl
Chlorine is initiation material through being acylated the preparation method (West Germany's publication 2453063) being cyclized again with alkali, and industrialized production
In sulfamic acid (salt)-SO for generally using3Method (US4695629), the yield of this step of intermediate A SH is generated in all methods
It is all very low, and need to be reacted in -40~-25 DEG C of low reaction temperatures section, and it is a large amount of use atent solvent as reaction medium,
Convenient heat transfer, mass transport process.
In the patent and document for having synthesized acesulfame potassium method, acetylation, cyclisation, hydrolysis, into the step of salt 4 react, still
Carried out around stirred-tank reactor, or circulation material spray strengthens reaction mass transfer (CN 1927850A) by vortex mixing mode, reacts
Device periphery is with jacket for heat exchange, or circulation is taken out and expects to cool down in tubular heat exchanger in back flow reaction kettle again, cyclisation and hydrolysis by
The influence of mass-and heat-transfer is very big, and yield is not high, and energy consumption is very high.
Due to can not all avoid the committed step of Cyclization ASH compounds in existing acesulfame potassium synthetic method, and ASH is closed
Into the ultimate yield and cost for controlling whole 3,4-Dihydro-6-methyl-1,2,3-oxathiazin-4-one 2,2-dioxide potassium salt production, thus, the present invention seeks to solve cyclisation and hydrolyzed program control
System is difficult, yield is low, energy consumption (low temperature cyclisation) material consumption (SO3And solvent) it is high the problem of.
The content of the invention
The purpose of the present invention is to improve existing 3,4-Dihydro-6-methyl-1,2,3-oxathiazin-4-one 2,2-dioxide potassium salt production core link --- ASH synthetic reaction critical crafts, and
And a kind of new cyclisation that can continuously synthesize of development and hydrolysis reactor technology, and the cyclisation suitable for this reactor, water are provided
Solve technological parameter.
The present invention is using a kind of cyclisation of microchannel, hydrolysis, heat transfer reactor integrated technology.
With pumping unit by the cyclization intermediate feed acetoacetyl amido sulfonic acid triethylamine of mass concentration 20~60%,
With the SO that mass concentration is 25~100%3Cyclizing agent is transported in micro passage reaction 1 (being cyclized and heat-exchange integrated) and is cyclized,
Cyclization equation is as follows：
Control cyclization key component SO3Mol ratio (the n values in reaction equation) with intermediate is (3~6):1,
- 30~25 DEG C of cyclization temperature；The cyclisation liquid of generation enter in micro passage reaction 2 (hydrolysis with heat-exchange integrated) with it is defeated
Reaction, amount of hydrolysis water SO is hydrolyzed in the water entered33~8 times of cyclizing agent volume flow, before synthesizing 3,4-Dihydro-6-methyl-1,2,3-oxathiazin-4-one 2,2-dioxide potassium salt after hydrolysis
Body ASH；While cyclisation, hydrolysis, cyclisation and hydrolysising reacting temperature are controlled with coolant heat-removing way.
Preferably, cyclizing agent SO3Solution and midbody solution enter micro passage reaction 1 with isometric flow rate, and cyclisation is anti-
Answer key component SO3Molar feed ratio with intermediate is (3~6):1, more preferably (4.5~5.5):1.
By above-mentioned cyclization material controlling ratio requirement, used cyclizing agent and reaction intermediate are all with halogenated aliphatic hydrocarbon dichloro
Methane or dichloroethanes are solvent, it is preferable that using dichloromethane as solvent, the mass concentration of reaction intermediate raw material for 20~
50%, SO3SO in cyclizing agent3Mass concentration is 20~50%.
The present invention carries out Cyclization using micro passage reaction, because reaction stops short (liquid hourly space velocity (LHSV) in microchannel
It is high), it is desirable to cyclization speed is fast, reaction temperature is slightly higher, it is preferable that cyclization temperature control is at -10~10 DEG C, the temperature
Regulation and control are that the hot microchannel of shifting continued to flow through by coolant in the first micro passage reaction 1 is realized.Should by the first microchannel plate
The cyclisation liquid that device 1 is obtained enters the second micro passage reaction 2.Reaction is hydrolyzed in the second micro passage reaction 2, goes forward side by side
Row moves heat.Amount of hydrolysis water is SO33~8 times of cyclizing agent volume flow, guarantee and SO3Fully reaction.Hydrolytic process is sent out
Raw following reaction：
Hydrolysis essence is SO3Sulfuric acid is generated with water, is strong exothermal reaction, reaction temperature is too high during hydrolysis to make
Decomposition product, therefore must pass through coolant and remove reaction heat.Preferable hydrolysising reacting temperature is -10~10 DEG C.
First micro passage reaction and the second micro passage reaction of the present invention, cyclisation therein and hydrolysis
The characteristic size of passage is 100 μm~3mm, and the characteristic size of integrated micro- heat exchanger channels is 100 μm~3mm.Reaction
The length and quantity of passage then control according to reactant yield, and reaction velocity is unfettered in principle, because reaction is close to normal pressure
Lower progress, to obtain optimal mixed effect, simultaneous selection one appropriate cyclization time, the liquid hourly space velocity (LHSV) of cyclization
Select as 500~10000h-1, preferably 1000~4000h-1, more preferably 1500~2000h-1。
Course of reaction operating method：First it is divided to two strands to squeeze into the first micro passage reaction 1 solvent with measuring pump, solvent stream
Measure midbody solution and SO that can respectively with question response3Cyclisation agent flux is identical (no longer pump can be set to export after switching), opens
Dynamic refrigerating fluid circulating pump control temperature of reactor, then switches to intermediate feed and SO3Raw material measures conveying simultaneously, second
Hydrolysis is passed through in micro passage reaction 2 reaction is hydrolyzed with water and cyclisation liquid.When stopping reaction, SO is closed3And intermediate enters
Material, switch to solvent cleaning reactor.The spout bag sulfur acid phase and dichloromethane phase of micro passage reaction 2, sulfuric acid phase is with two
The product that chloromethanes extraction is wherein dissolved, is merged into dichloromethane phase, and the ASH extracted with pure water in dichloromethane phase is produced
Thing, finally neutralized with potassium hydroxide and produce 3,4-Dihydro-6-methyl-1,2,3-oxathiazin-4-one 2,2-dioxide potassium salt into sylvite, rectifying.
With existing caldron process ratio, the reaction time of the invention is short, and cyclization temperature is high, SO3The solvent load of cyclizing agent
It is few；ASK total recoverys 50~70%, can continuous operation.
Embodiment
The present invention is further illustrated with example, but does not form limiting the scope of the present invention.
Before implementation, several reactant mixtures are first formulated as follows：
1. in conventional reactor, acetylization reaction is carried out by raw material of sulfamic acid, ketene dimer and triethylamine, instead
Answer equation as follows：
Synthesize the dichloromethane solution for the acetyl acetamide sulfonic triethylamine that mass concentration is 57.2%, then distinguish
21.7%, 30%, 40% concentration is diluted in a manner of adding dichloromethane, is placed in saving backup under low temperature.
2. prepare liquid SO3And SO3Mass concentration is 50% dichloromethane solution.
Above-mentioned reactant mixture is passed through cyclization in micro passage reaction in the concentration and ratio of the present invention, and is hydrolyzed to
Between product ASH.All contain the microchannel for cyclisation or hydrolysis inside used first, second micro passage reaction,
And integrated micro-channel heat exchanger, microchannel feature size (also known as hydraulic diameter) therein is 0.3mm.
For cool brine, for the required cryogenic temperature (- 10~10 DEG C) of the present invention, it is dense that quality may be selected in the coolant used
It is coolant to spend the aqueous solution such as the sodium chloride for less than 20%, calcium chloride.
Embodiment 1
Take the SO that mass concentration is 50%3- dichloromethane solution and intermediate-dichloromethane that mass concentration is 21.7%
Alkane solution, it is continuously fed into through highly pressurised liquid constant-flux pump in micro passage reaction 1 and carries out ring-closure reaction, reaction key component SO3
It is 6 with intermediate reaction mol ratio:1, the input material volume ratio of cyclizing agent and midbody solution is 1:1.6；Cyclisation liquid enters logical in a subtle way
Reaction is hydrolyzed in road reactor 2, water is excessive SO35 times.It is cyclized and is respectively with the control temperature of hydrolysis reactor
4.5℃、1.5℃.The liquid hourly space velocity (LHSV) of cyclization reactor is 1890h-1, from the product that hydrolysis reactor flows out through phase separation, dichloro
Methane extraction, water extract three times to be neutralized through the KOH aqueous solution again, takes neutralizer to be diluted with water to certain volume a little, with liquid phase color
Spectrum analysis ASK concentration simultaneously calculates ASK yields.Yield is 56.7%.
Embodiment 2
Using the pure SO of liquid3(concentration 100%) is cyclizing agent, and intermediate-dichloromethane that mass concentration is 21.7%
Alkane solution, it is continuously fed into through highly pressurised liquid constant-flux pump in micro passage reaction 1 and carries out ring-closure reaction, reaction key component SO3
It is 5.4 with intermediate reaction mol ratio:1, the input material volume ratio of cyclizing agent and midbody solution is 1:4.6；Cyclisation liquid enters in a subtle way
Reaction is hydrolyzed in channel reactor 2, water is excessive SO38 times.It is cyclized and is respectively with the control temperature of hydrolysis reactor
23℃、7℃.The liquid hourly space velocity (LHSV) of cyclization reactor is 1890h-1, from the product that hydrolysis reactor flows out through phase separation, dichloromethane
Extraction, water are extracted three times to be neutralized through the KOH aqueous solution again, takes neutralizer to be diluted with water to certain volume a little, with liquid chromatogram point
Analysis ASK concentration simultaneously calculates ASK yields.Yield is 41.5%.
Embodiment 3
Take the SO that mass concentration is 50%3- dichloromethane solution and intermediate-dichloromethane that mass concentration is 30%
Solution, it is continuously fed into through highly pressurised liquid constant-flux pump in micro passage reaction 1 and carries out ring-closure reaction, reaction key component SO3With
Intermediate reaction mol ratio is 5.6:1, the input material volume ratio of cyclizing agent and midbody solution is 1:1.2；Cyclisation liquid enters logical in a subtle way
Reaction is hydrolyzed in road reactor 2, water is excessive SO34.5 times.It is cyclized and is respectively with the control temperature of hydrolysis reactor
6℃、8℃.The liquid hourly space velocity (LHSV) of cyclization reactor is 1830h-1, from the product that hydrolysis reactor flows out through phase separation, dichloromethane
Extraction, water are extracted three times to be neutralized through the KOH aqueous solution again, takes neutralizer to be diluted with water to certain volume a little, with liquid chromatogram point
Analysis ASK concentration simultaneously calculates ASK yields.Yield is 47.8%.
Embodiment 4
Using the pure SO of liquid3(concentration 100%) is cyclizing agent, and intermediate-dichloromethane that mass concentration is 40%
Solution, it is continuously fed into through highly pressurised liquid constant-flux pump in micro passage reaction 1 and carries out ring-closure reaction, reaction key component SO3With
Intermediate reaction mol ratio is 5.7:1, the input material volume ratio of cyclizing agent and midbody solution is 1:2.4；Cyclisation liquid enters logical in a subtle way
Reaction is hydrolyzed in road reactor 2, water is excessive SO37.5 times.It is cyclized and is respectively with the control temperature of hydrolysis reactor
24℃、10℃.The liquid hourly space velocity (LHSV) of cyclization reactor is 1830h-1, from the product that hydrolysis reactor flows out through phase separation, dichloromethane
Alkane extraction, water extract three times to be neutralized through the KOH aqueous solution again, takes neutralizer to be diluted with water to certain volume a little, with liquid chromatogram
Analysis ASK concentration simultaneously calculates ASK yields.Yield is 37.5%.
Embodiment 5
Take the SO that mass concentration is 50%3- dichloromethane solution and intermediate-dichloromethane that mass concentration is 30%
Solution, it is continuously fed into through highly pressurised liquid constant-flux pump in micro passage reaction 1 and carries out ring-closure reaction, reaction key component SO3With
Intermediate reaction mol ratio is 5.5:1, the input material volume ratio of cyclizing agent and midbody solution is 1:1.3；Cyclisation liquid enters logical in a subtle way
Reaction is hydrolyzed in road reactor 2, water is excessive SO34.6 times.Cyclisation and the control temperature of hydrolysis reactor are distinguished
For -3 DEG C, -0.5 DEG C.The liquid hourly space velocity (LHSV) of cyclization reactor is 1800h-1, from the product that hydrolysis reactor flows out through phase separation, two
Chloromethanes extraction, water extract three times to be neutralized through the KOH aqueous solution again, takes neutralizer to be diluted with water to certain volume a little, with liquid phase
Chromatography ASK concentration simultaneously calculates ASK yields.Yield is 42%.
Claims (6)
1. 3,4-Dihydro-6-methyl-1,2,3-oxathiazin-4-one 2,2-dioxide potassium salt precursor ASH method is synthesized in a kind of micro passage reaction, it is characterised in that：By mass concentration 20~60%
Cyclization intermediate feed acetoacetyl amido sulfonic acid triethylamine and the SO that mass concentration is 25~100%3Cyclizing agent conveys
It is cyclized into the first micro passage reaction, cyclization key component SO3Mol ratio with intermediate feed is (3~6):1；It is raw
Into cyclisation liquid enter in the second micro passage reaction and with water reaction, amount of hydrolysis water SO be hydrolyzed3Cyclizing agent body
3~8 times of flow of product, synthesizes 3,4-Dihydro-6-methyl-1,2,3-oxathiazin-4-one 2,2-dioxide potassium salt precursor ASH after hydrolysis；In cyclisation, hydrolysis reaction, with coolant heat-removing way control
System cyclisation and hydrolysising reacting temperature are -30~25 DEG C.
2. the method as described in claim 1, it is characterised in that SO3Cyclizing agent is with halogenated aliphatic hydrocarbon dichloromethane and/or dichloro
Ethane is solvent；SO3Mass concentration be preferably 20~50%.
3. the method as described in claim 1, it is characterised in that SO3Cyclizing agent and midbody solution are preferably entered with isometric flow
Enter micro passage reaction 1, reaction key component SO3It is preferably (4.5~5.5) with intermediate feed reaction mol ratio:1.
4. the method as described in claim 1, it is characterised in that cyclisation, hydrolysising reacting temperature are preferably -10~10 DEG C.
5. the method as described in claim 1, it is characterised in that the first described micro passage reaction and the second microchannel plate should
Device, the characteristic size of its reaction channel is 100 μm~3mm, on the first micro passage reaction and the second micro passage reaction
Integrated to have micro- heat exchanger channels, the characteristic size of its micro- heat exchanger channels is 100 μm~3mm；In first micro passage reaction
Fluid liquid hourly space velocity (LHSV) be 500~10000h-1。
6. the method as described in claim 1 or 5, it is characterised in that the liquid hourly space velocity (LHSV) of cyclisation and hydrolysis is preferably 1000
~4000h-1。
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Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110028396A (en) * | 2019-05-09 | 2019-07-19 | 江苏扬农化工集团有限公司 | A kind of method of the continuous synthesis of trans -2- hexenoic aldehyde of micro passage reaction |
| CN111377885A (en) * | 2018-12-30 | 2020-07-07 | 南通醋酸化工股份有限公司 | Method for cyclization and hydrolysis in continuous production of acesulfame potassium |
| CN111377882A (en) * | 2018-12-30 | 2020-07-07 | 南通醋酸化工股份有限公司 | Method for continuously producing acesulfame |
| CN111377880A (en) * | 2018-12-30 | 2020-07-07 | 南通醋酸化工股份有限公司 | Continuous preparation method of acesulfame potassium |
| CN111377881A (en) * | 2018-12-30 | 2020-07-07 | 南通醋酸化工股份有限公司 | Method for continuously preparing acetyl sulfanilic acid |
| CN111377886A (en) * | 2018-12-30 | 2020-07-07 | 南通醋酸化工股份有限公司 | Micro-channel reaction method and reaction system for cyclization and hydrolysis section in preparation of acesulfame potassium |
| CN113527226A (en) * | 2021-07-05 | 2021-10-22 | 南通醋酸化工股份有限公司 | Method for controlling content of ACH in acid in process of preparing acesulfame potassium |
| CN113788802A (en) * | 2021-08-31 | 2021-12-14 | 南通醋酸化工股份有限公司 | Method for preparing acesulfame potassium |
| WO2022246861A1 (en) | 2021-05-28 | 2022-12-01 | 安徽金禾实业股份有限公司 | Preparation method for acesulfame potassium |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111377882B (en) * | 2018-12-30 | 2022-03-22 | 南通醋酸化工股份有限公司 | Method for continuously producing acesulfame |
| CN111377885A (en) * | 2018-12-30 | 2020-07-07 | 南通醋酸化工股份有限公司 | Method for cyclization and hydrolysis in continuous production of acesulfame potassium |
| CN111377882A (en) * | 2018-12-30 | 2020-07-07 | 南通醋酸化工股份有限公司 | Method for continuously producing acesulfame |
| CN111377880A (en) * | 2018-12-30 | 2020-07-07 | 南通醋酸化工股份有限公司 | Continuous preparation method of acesulfame potassium |
| CN111377881A (en) * | 2018-12-30 | 2020-07-07 | 南通醋酸化工股份有限公司 | Method for continuously preparing acetyl sulfanilic acid |
| CN111377886A (en) * | 2018-12-30 | 2020-07-07 | 南通醋酸化工股份有限公司 | Micro-channel reaction method and reaction system for cyclization and hydrolysis section in preparation of acesulfame potassium |
| CN111377885B (en) * | 2018-12-30 | 2022-03-22 | 南通醋酸化工股份有限公司 | Method for cyclization and hydrolysis in continuous production of acesulfame potassium |
| CN111377886B (en) * | 2018-12-30 | 2022-11-29 | 南通醋酸化工股份有限公司 | Micro-channel reaction method and reaction system for cyclization and hydrolysis section in preparation of acesulfame potassium |
| CN110028396B (en) * | 2019-05-09 | 2022-03-04 | 江苏扬农化工集团有限公司 | Method for continuously synthesizing trans-2-hexenal by using microchannel reactor |
| CN110028396A (en) * | 2019-05-09 | 2019-07-19 | 江苏扬农化工集团有限公司 | A kind of method of the continuous synthesis of trans -2- hexenoic aldehyde of micro passage reaction |
| WO2022246861A1 (en) | 2021-05-28 | 2022-12-01 | 安徽金禾实业股份有限公司 | Preparation method for acesulfame potassium |
| CN113527226A (en) * | 2021-07-05 | 2021-10-22 | 南通醋酸化工股份有限公司 | Method for controlling content of ACH in acid in process of preparing acesulfame potassium |
| CN113788802A (en) * | 2021-08-31 | 2021-12-14 | 南通醋酸化工股份有限公司 | Method for preparing acesulfame potassium |
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Application publication date: 20180403 |