CN110302688A - Material dissolution device and method - Google Patents
Material dissolution device and method Download PDFInfo
- Publication number
- CN110302688A CN110302688A CN201910719495.6A CN201910719495A CN110302688A CN 110302688 A CN110302688 A CN 110302688A CN 201910719495 A CN201910719495 A CN 201910719495A CN 110302688 A CN110302688 A CN 110302688A
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- Prior art keywords
- dissolution
- column
- temperature
- material dissolution
- cooler
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Classifications
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01F—MIXING, e.g. DISSOLVING, EMULSIFYING OR DISPERSING
- B01F21/00—Dissolving
- B01F21/10—Dissolving using driven stirrers
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01F—MIXING, e.g. DISSOLVING, EMULSIFYING OR DISPERSING
- B01F27/00—Mixers with rotary stirring devices in fixed receptacles; Kneaders
- B01F27/80—Mixers with rotary stirring devices in fixed receptacles; Kneaders with stirrers rotating about a substantially vertical axis
- B01F27/90—Mixers with rotary stirring devices in fixed receptacles; Kneaders with stirrers rotating about a substantially vertical axis with paddles or arms
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01F—MIXING, e.g. DISSOLVING, EMULSIFYING OR DISPERSING
- B01F35/00—Accessories for mixers; Auxiliary operations or auxiliary devices; Parts or details of general application
- B01F35/20—Measuring; Control or regulation
- B01F35/22—Control or regulation
- B01F35/221—Control or regulation of operational parameters, e.g. level of material in the mixer, temperature or pressure
- B01F35/2215—Temperature
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01F—MIXING, e.g. DISSOLVING, EMULSIFYING OR DISPERSING
- B01F35/00—Accessories for mixers; Auxiliary operations or auxiliary devices; Parts or details of general application
- B01F35/90—Heating or cooling systems
- B01F35/92—Heating or cooling systems for heating the outside of the receptacle, e.g. heated jackets or burners
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01F—MIXING, e.g. DISSOLVING, EMULSIFYING OR DISPERSING
- B01F35/00—Accessories for mixers; Auxiliary operations or auxiliary devices; Parts or details of general application
- B01F35/90—Heating or cooling systems
- B01F2035/98—Cooling
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- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Physical Or Chemical Processes And Apparatus (AREA)
Abstract
The invention discloses a kind of material dissolution device and methods.Wherein, which includes: dissolution column, is internally provided with agitating paddle；Temperature control layer, the periphery that dissolution column is arranged in are used to control the temperature in dissolution column；Feeder for solid materials, the top that dissolution column is arranged in are used to add solid material into dissolution column；Colvent inlet, setting is on dissolution column；And liquid material outlet, the bottom end of dissolution column is set.It applies the technical scheme of the present invention, is column structure as dissolution vessel using dissolution column, therefore unit length upper volume is small, under the disturbance of agitating paddle, dissolution of raw material is uniform, and the temperature difference is small；Feeder for solid materials can be with continuous feed, and inlet amount is small in the unit time, and dissolution of raw material is rapid；The material dissolution device of the application can be with continuous operation, and device structure is compact, and liquid holdup is small, and controllability is high.
Description
Technical field
The present invention relates to chemical production technical fields, in particular to a kind of material dissolution device and method.
Background technique
In Chemical Manufacture, it is usually necessary to use the forms of solution for solid material used, rather than directly adopt solid
Raw material, it is therefore desirable to which solid material is dissolved into laggard subsequent production.If small scale, it can be used and manually dissolved, but if
If material quantity is big, it usually needs by equipment such as reaction kettle, stirred tanks (pond), by the way that solid material and molten is added into equipment
Agent carries out mixed dissolution using agitating paddle and required solution is made.But these devices are often all not thorough in the presence of dissolution, are molten
Expect the problems such as speed is slow, solution conveying program is more, the raw materials such as small for some temperature-sensitives, half-life period are unable to satisfy in subsequent operation
Purity and yield requirement, lead to the problems such as dissolved efficiency is low, and the solution of preparation is not up to standard, while there is also automatic for these equipment
Change degree is low, expends personnel cost height, the technical problems such as inconvenience can be also brought to production.
Typically, existing technique is to carry out molten material with tank reactor, although single batch processing amount is big, equally there is also
Some disadvantages, as follows: 1) molten material speed is slow, and the time is long；2) stirring is insufficient, and yield is low；3) temperature gradient is big, and product is variable
Bad, purity is low；4) it needs multiple kettles to carry out simultaneously when producing, takes up a large area；5) inventory is big, and the small risk of controllability is high；6) existing
Some reaction kettle operations are intermittent operation, and the intermittently operated period is long, and equipment entirety utilization rate is not high；7) batch products quality is deposited
In difference, unstable product quality；8) automation degree of equipment is low, and personnel cost is high.
Summary of the invention
The present invention is intended to provide a kind of material dissolution device and method, to improve the efficiency of solid material dissolution.
To achieve the goals above, according to an aspect of the invention, there is provided a kind of material dissolution device.The material is molten
Solving device includes: dissolution column, is internally provided with agitating paddle；The periphery of dissolution column is arranged in for controlling in dissolution column in temperature control layer
Temperature；Feeder for solid materials, the top that dissolution column is arranged in are used to add solid material into dissolution column；Colvent inlet, setting
On dissolution column；And liquid material outlet, the bottom end of dissolution column is set.
Further, temperature control layer includes multiple temperature-control units, and multiple temperature-control units can individually carry out temperature control.
Further, temperature control layer is high temperature bath interlayer.
Further, material dissolution device further includes solvent reservoir, and solvent reservoir passes through solvent charge pump and dissolution
The colvent inlet of column is connected.
Further, material dissolution device further includes cooler, and the entrance of cooler and the liquid material of dissolution column export
It is connected.
Further, cooler is the heat exchanger with cryogenic thermostat reactive bath technique.
Further, it dissolves and is additionally provided with product pump in the liquid material outlet and the access of the entrance of cooler of column.
Further, material dissolution device further includes material solution storage tank, and material solution storage tank is arranged under cooler
Trip.
According to another aspect of the present invention, a kind of material dissolution method is provided.The material dissolution method uses above-mentioned
A kind of material dissolution device is dissolved.
Further, when material is Meropenem, the temperature of control dissolution column is 10~50 DEG C when material dissolution, stirring
Speed is 80~160rpm.
It applies the technical scheme of the present invention, is column structure using dissolution column as dissolution vessel, therefore unit length
Upper volume is small, and under the disturbance of agitating paddle, dissolution of raw material is uniform, and the temperature difference is small；Feeder for solid materials can be with continuous feed, unit time
Interior inlet amount is small, and dissolution of raw material is rapid；The material dissolution device of the application can be with continuous operation, and device structure is compact, holds liquid
Measure small, controllability height.
Detailed description of the invention
The accompanying drawings constituting a part of this application is used to provide further understanding of the present invention, and of the invention shows
Examples and descriptions thereof are used to explain the present invention for meaning property, does not constitute improper limitations of the present invention.In the accompanying drawings:
Fig. 1 shows material dissolution device and the structural schematic diagram of process in the embodiment of the present invention 1.
Specific embodiment
It should be noted that in the absence of conflict, the features in the embodiments and the embodiments of the present application can phase
Mutually combination.The present invention will be described in detail below with reference to the accompanying drawings and embodiments.
A kind of typical embodiment according to the present invention provides a kind of material dissolution device.The material dissolution device includes
Dissolve column, temperature control layer, feeder for solid materials, colvent inlet and liquid material outlet, wherein dissolution column is internally provided with stirring
Paddle；The periphery that dissolution column is arranged in temperature control layer is used to control the temperature in dissolution column；The top of dissolution column is arranged in feeder for solid materials
End is for adding solid material into dissolution column；Colvent inlet setting is on dissolution column；And liquid material outlet is arranged molten
The bottom end of Xie Zhu.
Compared to the molten material operation of traditional kettle, the material dissolution device of the application using dissolution column as dissolution vessel,
For column structure, therefore unit length upper volume is small, and under the disturbance of agitating paddle, dissolution of raw material is uniform, and the temperature difference is small；Solid charging
Device can be with continuous feed, and inlet amount is small in the unit time, and dissolution of raw material is rapid；The material dissolution device of the application can be with serialization
Operation, device structure is compact, and liquid holdup is small, and controllability is high.
Preferably, temperature control layer includes multiple temperature-control units, and multiple temperature-control units can individually carry out temperature control, therefore,
The material dissolution device of the application can carry out sectional temperature-controlled, quickening dissolution of raw material speed, and reduction raw material is rotten.In an allusion quotation of the invention
In the embodiment of type, temperature control layer is high temperature bath interlayer, and heating water bath can preferably realize the regulation of temperature.More improve
The degree of automation, it is preferred that material dissolution device further includes solvent reservoir, solvent reservoir by solvent charge pump with it is molten
The colvent inlet of Xie Zhu is connected, so as to realize being continuously added to for solvent.
A kind of typical embodiment according to the present invention, material dissolution device further include cooler, the entrance of cooler with
The liquid material outlet of dissolution column is connected.Preferably, cooler is the heat exchanger with cryogenic thermostat reactive bath technique.
Preferably, it dissolves and is additionally provided with product pump in the liquid material outlet and the access of the entrance of cooler of column, into one
Step improves the degree of automation control.In a typical embodiment of the invention, material dissolution device further includes material solution
The downstream of cooler is arranged in storage tank, material solution storage tank, convenient for the storage of material after dissolution.
In the prior art, with the increase of batch reaction kettle volume, temperature gradient is big in system, and the temperature difference is big, solution rate
It reduces, the molten material time lengthens, and local temperature is excessively high, and raw material easily degenerates and generates impurity, and product purity and yield is caused to reduce.This Shen
Continuous apparatus please use column structure, axial unit length upper volume is small, cooperate agitating device, can the smaller temperature difference, adopt simultaneously
With sectional temperature-controlled, dissolution of raw material is rapid, and impurity generates few, can be very good to solve to draw because the temperature difference is big during the molten material of batch
The dissolution of raw material speed risen is slow, and impurity generates the problem of causing yield to reduce more.In addition, between the existing molten material of reaction kettle is usually
The operation of having a rest property, not there is only the problem that the operation cycle is long, utilization rate of equipment and installations is low, variant, automation journey that there is also product qualities
Spend the problems such as low, and the material dissolution device very good solution of the application because intermittent operation there are the problem of, Ke Yijin
Row continuous production, high degree of automation save labour turnover.
A kind of typical embodiment according to the present invention provides a kind of material dissolution method, using any of the above-described kind of material
Dissolver is dissolved.It is high using the material dissolution plant automation degree, it is at low cost, it can be mass-produced, and can adopt
With continuous operation, device structure is compact, and liquid holdup is small, and controllability is high.
The material dissolution device of the application can carry out continuous-dissolution, cooling to raw material.By raw material (be not limited only to solid,
Be also possible to powder or liquid) be added in the dissolution column of piecewise temperature control, by being stirred under agitating paddle, raw material from up to
Under gradually dissolve, finally through subcooler control system temperature, it is rotten to reduce product.It is axial since equipment uses columnar design
Unit length is small in size, and dissolution rapidly, stirs evenly, the system temperature difference is small, while sectional temperature-controlled quickening solution rate is arranged, into one
It is rotten that step reduces product, and equipment closed-loop operation, reduction dust dirt are highly-safe.
Typically, when material is Meropenem, the temperature of control dissolution column is 10~50 DEG C when material dissolution, stirring speed
Degree is 80~160rpm.
Beneficial effects of the present invention are further illustrated below in conjunction with embodiment.
Embodiment 1
Material dissolution device includes dissolution column 10, temperature control to material dissolution device used by the present embodiment as shown in Figure 1:
Layer, feeder for solid materials 12, colvent inlet and liquid material outlet, wherein dissolution column 10 is internally provided with agitating paddle；Temperature control layer
The periphery that dissolution column is arranged in is used to control the temperature in dissolution column；Feeder for solid materials 12 be arranged in dissolution column top be used for
Solid material is added in dissolution column；Colvent inlet setting is on dissolution column；And the bottom of dissolution column is arranged in liquid material outlet
End.Temperature control layer includes multiple temperature-control units, and multiple temperature-control units can individually carry out temperature control.In the present embodiment, temperature control
Layer is connected to high temperature water bath 11.Solvent reservoir 40 is connected by solvent charge pump 50 with the colvent inlet of dissolution column 10,
The entrance of cooler 20 is connected by product pump 30 with the liquid material outlet for dissolving column 10, and the periphery of cooler 20 is provided with
The downstream of cooler 20 is arranged in cryogenic thermostat bain-marie 21, material solution storage tank 60.
Operating procedure is as follows:
1. first preparing solution (molten material is used, and solvent is referred to as), and it is pumped into dissolution column, after dissolution column, will pumped
It is set as given flow rate charging；
2. raw material (solid/liquid) is added to feeder for solid materials, charging rate is gone out according to technology Calculation, setting is corresponding
Charging rate starts to feed；
3. the solution dissolved in column is pumped into cooler using pump to cool down；
4. the system received the operation such as to be crystallized to again, filtered, dried, sterling can be obtained.
The material dissolution device of the present embodiment has been successfully applied to the dissolution operation of the product in Meropenem production process, with
Down it is the yield and purity data of the molten material of batch and continuous material dissolving in different scales:
The results are shown in Table 1 for the molten material of bench scale:
Table 1
| Mode of operation | Yield % | Purity % |
| The molten material of batch | 80 | 98.5 |
| Continuous material dissolving | 81 | 99 |
The results are shown in Table 2 for the molten material of amplification scale:
Table 2
| Mode of operation | Yield % | Purity % |
| The molten material of batch | 45 | 90 |
| Continuous material dissolving | 80 | 98.6 |
In the present embodiment, dissolution column jacket temperature is 20~40 DEG C, and speed of agitator is 100~140rpm.
Embodiment 2
In mass ratio it is 1:18, Meropenem and water is uniformly mixed in the identical material dissolution of embodiment 1 dress
Dissolution.
Dissolving column jacket temperature is 20 DEG C, speed of agitator 100rpm.
The product yield obtained under above-mentioned condition is 80wt%, purity 98.9wt%.
Embodiment 3
With the difference of embodiment 2 are as follows: dissolution column jacket temperature is 40 degree.
Obtained product yield is 81wt%, purity 99wt%.
Embodiment 4
With the difference of embodiment 2 are as follows: dissolution column jacket temperature is 60 DEG C.
Obtained product yield is 68wt%, purity 84.66wt%.
Embodiment 5
With the difference of embodiment 2 are as follows: speed of agitator 20rpm.
Obtained product yield is 70wt%, purity 85.13wt%.
Embodiment 6
With the difference of embodiment 2 are as follows: reaction unit is batch reactor.
Obtained product yield is 80wt%, purity 98.5wt%.
It can be seen from the above description that the above embodiments of the present invention realized the following chievements:
Comparing embodiment 2 to 6, in the case where guaranteeing product purity and yield, is adopted it is found that compared to batch reactor
It can be improved the yield and purity of product with molten material system provided by the present application, and enlarge-effect is small.
Comparing embodiment 2 to 5 is conducive to it is found that jacket temperature and speed of agitator are limited in the preferred range of the application
Improve the yield and purity of product.
Comparing embodiment 2 to 4 is conducive to improve product in the preferred range of the application it is found that jacket temperature is limited to
Yield and purity.
Comparing embodiment 1 and 5 is conducive to improve product in the preferred range of the application it is found that speed of agitator is limited to
Yield and purity.
The foregoing is only a preferred embodiment of the present invention, is not intended to restrict the invention, for the skill of this field
For art personnel, the invention may be variously modified and varied.All within the spirits and principles of the present invention, made any to repair
Change, equivalent replacement, improvement etc., should all be included in the protection scope of the present invention.
Claims (10)
1. a kind of material dissolution device characterized by comprising
Column is dissolved, agitating paddle is internally provided with；
Temperature control layer, the periphery that the dissolution column is arranged in are used to control the temperature dissolved in column；
The top of the dissolution column is arranged in for adding solid material into the dissolution column in feeder for solid materials；
Colvent inlet is arranged on the dissolution column；And
The bottom end of the dissolution column is arranged in liquid material outlet.
2. material dissolution device according to claim 1, which is characterized in that the temperature control layer includes multiple temperature-control units,
Multiple temperature-control units can individually carry out temperature control.
3. material dissolution device according to claim 1, which is characterized in that the temperature control layer is high temperature bath interlayer.
4. material dissolution device according to claim 1, which is characterized in that the material dissolution device further includes solvent storage
Storage, the solvent reservoir are connected by solvent charge pump with the colvent inlet of the dissolution column.
5. material dissolution device according to claim 1, which is characterized in that the material dissolution device further includes cooling
Device, the entrance of the cooler are connected with the liquid material outlet of the dissolution column.
6. material dissolution device according to claim 5, which is characterized in that the cooler is to react with cryogenic thermostat
The heat exchanger of bath.
7. material dissolution device according to claim 5, which is characterized in that the liquid material outlet of the dissolution column and institute
It states and is additionally provided with product pump on the access of the entrance of cooler.
8. material dissolution device according to claim 5, which is characterized in that the material dissolution device further includes that material is molten
The downstream of the cooler is arranged in liquid storage tank, the material solution storage tank.
9. a kind of material dissolution method, which is characterized in that filled using such as material dissolution described in any item of the claim 1 to 8
It sets and is dissolved.
10. material dissolution method according to claim 9, which is characterized in that described when the material is Meropenem
The temperature that the dissolution column is controlled when material dissolution is 10~50 DEG C, and preferably 20~40 DEG C, mixing speed is 80~160rpm；
Preferably 100~140rpm.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201910719495.6A CN110302688A (en) | 2019-08-05 | 2019-08-05 | Material dissolution device and method |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201910719495.6A CN110302688A (en) | 2019-08-05 | 2019-08-05 | Material dissolution device and method |
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| Publication Number | Publication Date |
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| CN110302688A true CN110302688A (en) | 2019-10-08 |
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ID=68083077
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|---|---|---|---|
| CN201910719495.6A Pending CN110302688A (en) | 2019-08-05 | 2019-08-05 | Material dissolution device and method |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111187902A (en) * | 2020-01-09 | 2020-05-22 | 中国原子能科学研究院 | Aluminum matrix mercury catalysis technology dissolving system |
| CN114805162A (en) * | 2022-04-26 | 2022-07-29 | 湖北华洲药业有限公司 | Continuous production method and device for meropenem side chain key intermediate O powder |
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| CN110052188A (en) * | 2019-05-17 | 2019-07-26 | 平顶山学院 | A kind of pharmacy solid reagent dissolver |
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| DE1171609B (en) * | 1961-08-25 | 1964-06-04 | Phrix Werke Ag | Process and device for the continuous production of polyacrylonitrile solutions in sulfuric acid |
| US4212848A (en) * | 1977-07-20 | 1980-07-15 | Champion International Corporation | Apparatus and process for the manufacture of fibrils |
| RU2484885C1 (en) * | 2012-02-08 | 2013-06-20 | Открытое акционерное общество "Сибирский химический комбинат" | Device for uranium concentrate dissolution |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111187902A (en) * | 2020-01-09 | 2020-05-22 | 中国原子能科学研究院 | Aluminum matrix mercury catalysis technology dissolving system |
| CN114805162A (en) * | 2022-04-26 | 2022-07-29 | 湖北华洲药业有限公司 | Continuous production method and device for meropenem side chain key intermediate O powder |
| CN114805162B (en) * | 2022-04-26 | 2024-05-31 | 湖北华洲药业有限公司 | Continuous production method and device for meropenem side chain key intermediate O powder |
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