CN109045744A - The method and apparatus for preparing acesulfame potassium crystallization of continuous-stable - Google Patents
The method and apparatus for preparing acesulfame potassium crystallization of continuous-stable Download PDFInfo
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- CN109045744A CN109045744A CN201811003080.0A CN201811003080A CN109045744A CN 109045744 A CN109045744 A CN 109045744A CN 201811003080 A CN201811003080 A CN 201811003080A CN 109045744 A CN109045744 A CN 109045744A
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- crystallization
- acesulfame potassium
- continuous
- mother liquor
- preparing
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D9/00—Crystallisation
- B01D9/0059—General arrangements of crystallisation plant, e.g. flow sheets
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D9/00—Crystallisation
- B01D9/0018—Evaporation of components of the mixture to be separated
- B01D9/0022—Evaporation of components of the mixture to be separated by reducing pressure
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D9/00—Crystallisation
- B01D9/0063—Control or regulation
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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
Abstract
The present invention relates to a kind of method and apparatus for preparing acesulfame potassium crystallization of continuous-stable, and described device includes: decompression evaporator, heat exchanger, crystallization kettle, scraper type centrifuge and mother liquor tank;Wherein, heat exchanger is provided on the decompression evaporator, the decompression evaporator is connected to the crystallization kettle, and the crystallization kettle is connected to the scraper type centrifuge, the scraper type centrifuge is connected to the mother liquor tank, and the mother liquor tank is connected to the decompression evaporator.The device for preparing acesulfame potassium crystallization of continuous-stable of the invention, it is uneven to solve that process existing for acesulfame potassium crystallization process is cumbersome, equipment intersects more, crystallization time length, crystalline solid, the technical problem of the series such as unstable quality, provide a kind of continuous crystallisation, the technique that crystal habit is uniform, quality is stable and efficiently production, industrialization degree is high, the crystallization apparatus remotely controlled can be achieved.
Description
Technical field
The invention proposes a kind of method and apparatus for preparing acesulfame potassium crystallization of continuous-stable.
Background technique
Acesulfame potassium is a kind of important sugar-free sweetener, and sugariness is 200 times of sucrose, has good mouthfeel, and do not join
With the intracorporal physiological metabolism of people, do not put aside, be ideal for the improvement that the quality of life of diabetic and overweight people has had
, safe and economical food additives, be widely used in daily use chemicals, food, drink, medical manufacture etc..Currently, acesulfame potassium
Production substantially using using sulfamic acid and ketene dimer as the processing technology routine of raw material, reaction process include synthesis,
Acylated, cyclisation, hydrolysis and neutralization step.Since hydrolytic process and washing step are added what suitable water and N-process generated
Water, acesulfame potassium solution concentration is lower, needs to be concentrated, and crystallization processes are intervals, to the yield of acesulfame potassium product, quality, production
Period, energy consumption have a significant impact.
Currently, what the preparation method about acesulfame potassium crystallization, predominantly multiple one-pot crystallisation by cooling or multiple one-pots were intersected
Crystallization mode.One-pot crystallisation by cooling unstable quality, crystal form are uneven, production production capacity is small, and production efficiency is low;Multiple one-pots are intersected
Crystallization mode although improve the crystallization production capacity of acesulfame potassium, but be not continuous crystallisation technique truly and operate
It is cumbersome.The crystallization processes of interval, show as that crystallization time is long, crystalline solid is uneven, unstable quality, and industrialization level is low.
Summary of the invention
An object of the present invention is to provide a kind of devices for preparing acesulfame potassium crystallization of continuous-stable.
The device for preparing acesulfame potassium crystallization of a kind of continuous-stable of the invention, comprising: decompression evaporator, heat exchanger, knot
Brilliant kettle, scraper type centrifuge and mother liquor tank;Wherein, be provided with heat exchanger on the decompression evaporator, the decompression evaporator with
The crystallization kettle connection, the crystallization kettle are connected to the scraper type centrifuge, the scraper type centrifuge and the mother liquor tank
Connection, the mother liquor tank are connected to the decompression evaporator.
The device for preparing acesulfame potassium crystallization of continuous-stable of the invention, solves process existing for acesulfame potassium crystallization process
Cumbersome, equipment intersects that more, crystallization time length, crystalline solid are uneven, and the technical problem of the series such as unstable quality provides one kind
Continuous crystallisation, crystal habit are uniform, quality is stable technique and efficiently production, industrialization degree is high, can be achieved remotely to control
Crystallization apparatus.
In addition, the device for preparing acesulfame potassium crystallization of above-mentioned continuous-stable of the invention, can also have following additional
Technical characteristic:
Further, the device for preparing acesulfame potassium crystallization of the continuous-stable, further includes temperature controller, the temperature
It spends controller to be arranged on the heat exchanger, the flow control of the heat medium of the heat exchanger is adjusted by the temperature controller
Valve processed.
Further, the device for preparing acesulfame potassium crystallization of the continuous-stable, further includes in line density real-time monitoring
Instrument, it is described line density real-time monitor be arranged in the decompression evaporator cone bottom 2/3 at.
Further, the device for preparing acesulfame potassium crystallization of the continuous-stable, further includes liquid level signal controller, institute
It states liquid level signal instrument to be arranged on the decompression evaporator, for controlling material inlet valve.
Further, the crystallization kettle includes stirring system, outer circulation pump and cooler.
Further, speed of agitator control frequency converter is provided on the stirring system.
It is another object of the present invention to the methods for preparing acesulfame potassium crystallization proposed using described device continuous-stable.
Using the method for preparing acesulfame potassium crystallization of described device continuous-stable, include the following steps: S101: first will peace
It matches sweet solution to be input in the decompression evaporator by feed pipe, forms circulation under the action of heat exchanger, control acesulfame potassium is molten
The temperature of liquid is 65 DEG C~90 DEG C, the moisture in the acesulfame potassium solution is evaporated removal under vacuum conditions, and described in control
The density range of acesulfame potassium solution is 1.15g/cm3~1.45g/cm3, concentrated liquid is then acquired into the crystallization kettle, control
Its temperature is 10 DEG C~20 DEG C, and revolving speed is 45r/min~80r/min;S102: the mother liquor is poured into the mother liquor tank, then
The mother liquor is squeezed into refining step by dnockout pumps or is added in the decompression evaporator;The crystalline substance that will be formed in the crystallization kettle
Body and liquid are imported in the scraper type centrifuge by bottom valve, by the acesulfame potassium crystalline solid by the scraper type centrifuge
Solid outlet discharging, then dry.
Further, in the step S101, vacuum degree control is -0.065MPa~-0.085MPa.
Additional aspect and advantage of the invention will be set forth in part in the description, and will partially become from the following description
Obviously, or practice through the invention is recognized.
Detailed description of the invention
Fig. 1 is the structural schematic diagram of the device for preparing acesulfame potassium crystallization of continuous-stable of the invention.
Specific embodiment
The embodiment of the present invention is described below in detail, examples of the embodiments are shown in the accompanying drawings, wherein from beginning to end
Same or similar label indicates same or similar element or element with the same or similar functions.Below with reference to attached
The embodiment of figure description is exemplary, it is intended to is used to explain the present invention, and is not considered as limiting the invention.
In a first aspect, as shown in Figure 1, being wrapped the invention proposes a kind of device for preparing acesulfame potassium crystallization of continuous-stable
It includes: decompression evaporator 110, heat exchanger 120, crystallization kettle 130, scraper type centrifuge 140 and mother liquor tank 150;Wherein, the decompression
Heat exchanger 120 is provided on evaporator 110, the decompression evaporator 110 is connected to the crystallization kettle 130, the crystallization kettle 130
It is connected to the scraper type centrifuge 140, the scraper type centrifuge 140 is connected to the mother liquor tank 150, the mother liquor tank
150 are connected to the decompression evaporator 110.
Advantageously, the device for preparing acesulfame potassium crystallization of the continuous-stable, further includes temperature controller 170, described
Temperature controller 170 is arranged on the heat exchanger 120, adjusts adding for the heat exchanger 120 by the temperature controller 170
The flow control valve of thermal medium.
Advantageously, the device for preparing acesulfame potassium crystallization of the continuous-stable, further includes in line density real-time monitor
180, it is described line density real-time monitor 180 be arranged in the decompression evaporator 110 cone bottom 2/3 at.
Advantageously, the device for preparing acesulfame potassium crystallization of the continuous-stable, further includes liquid level signal controller 190,
The liquid level signal instrument 190 is arranged on the decompression evaporator 110, for controlling material inlet valve.
Advantageously, the crystallization kettle 130 includes stirring system, outer circulation pump and cooler.It is arranged on the stirring system
There is speed of agitator to control frequency converter, for controlling the revolving speed of the stirring system.
Second aspect, the invention proposes the methods for preparing acesulfame potassium crystallization using described device continuous-stable, including
Following steps:
(1) acesulfame potassium solution is input in the decompression evaporator by feed pipe first, shape under the action of heat exchanger
At circulation, the temperature for controlling acesulfame potassium solution is 65 DEG C~90 DEG C, under vacuum conditions by the moisture in the acesulfame potassium solution
Evaporation removes, and vacuum degree control is -0.065MPa~-0.085MPa.And the density range for controlling the acesulfame potassium solution is
1.15g/cm3~1.45g/cm3, concentrated liquid is then acquired into the crystallization kettle, and controlling its temperature is 10 DEG C~20 DEG C, is turned
Speed is 45r/min~80r/min.
(2) mother liquor is poured into the mother liquor tank, then the mother liquor is squeezed into refining step or supplement by dnockout pumps
Into the decompression evaporator;The crystal formed in the crystallization kettle and liquid are imported the scraper type by bottom valve to be centrifuged
In machine, the acesulfame potassium crystalline solid is discharged by the solid outlet of the scraper type centrifuge, is then dried.
To sum up, the device for preparing acesulfame potassium crystallization of continuous-stable of the invention solves the presence of acesulfame potassium crystallization process
Process is cumbersome, equipment intersects that more, crystallization time length, crystalline solid are uneven, and the technical problem of the series such as unstable quality provides
A kind of continuous crystallisation, crystal habit is uniform, quality is stable technique and efficiently production, industrialization degree is high, it is long-range to can be achieved
The crystallization apparatus of control.
Specific embodiment
Acesulfame potassium solution enters decompression evaporator by feed pipe, and circulation, acesulfame potassium solution are formed under the action of heat exchanger
Temperature controls the flow control valve for adjusting the heat medium of heat exchanger by temperature controller at 80 DEG C.Moisture in material exists
It evaporates and removes under vacuum state, vacuum degree control is in -0.075MPa.Liquidometer signal in decompression evaporator controls inlet valve
Door.Liquid on-line density real-time monitor is set at 2/3 of cone bottom in decompression evaporator, density is in 1.25g/cm3When, letter
Number to delivery pump electric motor starting, the concentrated liquid of acquisition to crystallization kettle, crystallization kettle is made of stirring, outer circulation pump and cooler,
At 16 DEG C, control mode is the cooling medium stream of thermometer signal control cooler for crystallization temperature control of the material in crystallization kettle
Measure valve;Crystallization kettle is controlled by speed of agitator in 50r/min.The crystal and liquid that crystallization is formed in crystallization kettle by bottom valve from
It flow to scraper type centrifuge, mother liquor enters mother liquor tank, and mother liquor squeezes into refining step or part adds in decompression evaporator by pumping,
Acesulfame potassium crystalline solid is discharged by the solid outlet of scraper type centrifuge to drying process.
The method for preparing acesulfame potassium crystallization of the continuous-stable of the present embodiment, solves mistake existing for acesulfame potassium crystallization process
Journey is cumbersome, equipment intersection is more, crystallization time is long, crystalline solid is uneven, and the technical problem of the series such as unstable quality provides one
Kind continuous crystallisation, the technique that crystal habit is uniform, quality is stable and efficiently production, industrialization degree height, achievable remotely control
Crystallization apparatus.
In the description of this specification, reference term " one embodiment ", " some embodiments ", " example ", " specifically show
The description of example " or " some examples " etc. means specific features, structure, material or spy described in conjunction with this embodiment or example
Point is included at least one embodiment or example of the invention.In the present specification, schematic expression of the above terms are not
It must be directed to identical embodiment or example.Moreover, particular features, structures, materials, or characteristics described can be in office
It can be combined in any suitable manner in one or more embodiment or examples.In addition, without conflicting with each other, the skill of this field
Art personnel can tie the feature of different embodiments or examples described in this specification and different embodiments or examples
It closes and combines.
Although the embodiments of the present invention has been shown and described above, it is to be understood that above-described embodiment is example
Property, it is not considered as limiting the invention, those skilled in the art within the scope of the invention can be to above-mentioned
Embodiment is changed, modifies, replacement and variant.
Claims (8)
1. a kind of device for preparing acesulfame potassium crystallization of continuous-stable characterized by comprising decompression evaporator, heat exchanger, knot
Brilliant kettle, scraper type centrifuge and mother liquor tank;
Wherein, heat exchanger is provided on the decompression evaporator, the decompression evaporator is connected to the crystallization kettle, the crystallization
Kettle is connected to the scraper type centrifuge, and the scraper type centrifuge is connected to the mother liquor tank, and the mother liquor tank subtracts with described
Press evaporator connection.
2. the device for preparing acesulfame potassium crystallization of continuous-stable according to claim 1, which is characterized in that further include temperature
Controller, the temperature controller are arranged on the heat exchanger, adjust adding for the heat exchanger by the temperature controller
The flow control valve of thermal medium.
3. the device for preparing acesulfame potassium crystallization of continuous-stable according to claim 1, which is characterized in that further include online
Density real-time monitor, it is described line density real-time monitor be arranged in the decompression evaporator cone bottom 2/3 at.
4. the device for preparing acesulfame potassium crystallization of continuous-stable according to claim 1, which is characterized in that further include liquid level
Signal controller, the liquid level signal instrument is arranged on the decompression evaporator, for controlling material inlet valve.
5. the device for preparing acesulfame potassium crystallization of continuous-stable according to claim 1, which is characterized in that the crystallization kettle
Including stirring system, outer circulation pump and cooler.
6. the device for preparing acesulfame potassium crystallization of continuous-stable according to claim 4, which is characterized in that the stirring system
Speed of agitator control frequency converter is provided on system.
7. using the method for preparing acesulfame potassium crystallization of the described in any item device continuous-stables of claim 1-5, feature exists
In including the following steps:
S101: acesulfame potassium solution is input in the decompression evaporator by feed pipe first, is formed under the action of heat exchanger
Circulation, the temperature of control acesulfame potassium solution are 65 DEG C~90 DEG C, and the moisture in the acesulfame potassium solution is steamed under vacuum conditions
Hair removes, and the density range for controlling the acesulfame potassium solution is 1.15g/cm3~1.45g/cm3, then acquire concentrated liquid and arrive
In the crystallization kettle, controlling its temperature is 10 DEG C~20 DEG C, and revolving speed is 45r/min~80r/min;
S102: the mother liquor is poured into the mother liquor tank, then the mother liquor is squeezed into refining step by dnockout pumps or is added to
In the decompression evaporator;The crystal formed in the crystallization kettle and liquid are imported into the scraper type centrifuge by bottom valve
In, the acesulfame potassium crystalline solid is discharged by the solid outlet of the scraper type centrifuge, is then dried.
8. the method for preparing acesulfame potassium crystallization of continuous-stable according to claim 3, which is characterized in that in the step
In S101, vacuum degree control is -0.065MPa~-0.085MPa.
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CN201811003080.0A CN109045744B (en) | 2018-08-30 | 2018-08-30 | Method and device for continuously and stably preparing acesulfame potassium crystals |
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CN201811003080.0A CN109045744B (en) | 2018-08-30 | 2018-08-30 | Method and device for continuously and stably preparing acesulfame potassium crystals |
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Cited By (3)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN111377883A (en) * | 2018-12-30 | 2020-07-07 | 南通醋酸化工股份有限公司 | Continuous post-treatment method of acesulfame potassium |
CN112110875A (en) * | 2020-09-26 | 2020-12-22 | 安徽金禾实业股份有限公司 | Preheating method for mother liquor in heavy material boiling section |
CN113512012A (en) * | 2021-06-30 | 2021-10-19 | 南通醋酸化工股份有限公司 | Continuous evaporative crystallization system and method for preparing acesulfame potassium |
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CN111377883A (en) * | 2018-12-30 | 2020-07-07 | 南通醋酸化工股份有限公司 | Continuous post-treatment method of acesulfame potassium |
CN112110875A (en) * | 2020-09-26 | 2020-12-22 | 安徽金禾实业股份有限公司 | Preheating method for mother liquor in heavy material boiling section |
CN113512012A (en) * | 2021-06-30 | 2021-10-19 | 南通醋酸化工股份有限公司 | Continuous evaporative crystallization system and method for preparing acesulfame potassium |
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