CN116983693A - Liquid medicine decompression distillation device - Google Patents
Liquid medicine decompression distillation device Download PDFInfo
- Publication number
- CN116983693A CN116983693A CN202310961268.0A CN202310961268A CN116983693A CN 116983693 A CN116983693 A CN 116983693A CN 202310961268 A CN202310961268 A CN 202310961268A CN 116983693 A CN116983693 A CN 116983693A
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- China
- Prior art keywords
- reaction kettle
- pipe
- heating
- recovery
- rectifying device
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
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- 239000007788 liquid Substances 0.000 title claims abstract description 26
- 239000003814 drug Substances 0.000 title claims abstract description 22
- 238000004821 distillation Methods 0.000 title claims abstract description 21
- 230000006837 decompression Effects 0.000 title description 4
- 238000010438 heat treatment Methods 0.000 claims abstract description 39
- 238000011084 recovery Methods 0.000 claims abstract description 37
- 239000000126 substance Substances 0.000 claims abstract description 32
- 238000005192 partition Methods 0.000 claims description 15
- 239000000498 cooling water Substances 0.000 claims description 10
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 6
- 238000004891 communication Methods 0.000 claims description 3
- 238000000034 method Methods 0.000 claims description 3
- 238000007789 sealing Methods 0.000 claims description 3
- 239000012530 fluid Substances 0.000 claims 6
- 238000005194 fractionation Methods 0.000 abstract description 4
- 238000009835 boiling Methods 0.000 description 16
- 238000004519 manufacturing process Methods 0.000 description 10
- 239000000463 material Substances 0.000 description 8
- WFDIJRYMOXRFFG-UHFFFAOYSA-N Acetic anhydride Chemical compound CC(=O)OC(C)=O WFDIJRYMOXRFFG-UHFFFAOYSA-N 0.000 description 6
- 238000005457 optimization Methods 0.000 description 6
- 238000004925 denaturation Methods 0.000 description 4
- 230000036425 denaturation Effects 0.000 description 4
- GFFGJBXGBJISGV-UHFFFAOYSA-N Adenine Chemical compound NC1=NC=NC2=C1N=CN2 GFFGJBXGBJISGV-UHFFFAOYSA-N 0.000 description 3
- 229930024421 Adenine Natural products 0.000 description 3
- 229960000643 adenine Drugs 0.000 description 3
- 230000009286 beneficial effect Effects 0.000 description 3
- 238000009833 condensation Methods 0.000 description 2
- 230000005494 condensation Effects 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 238000005485 electric heating Methods 0.000 description 2
- 238000001704 evaporation Methods 0.000 description 2
- 230000008020 evaporation Effects 0.000 description 2
- 238000004508 fractional distillation Methods 0.000 description 2
- 230000005484 gravity Effects 0.000 description 2
- 238000013021 overheating Methods 0.000 description 2
- 238000004064 recycling Methods 0.000 description 2
- 230000000630 rising effect Effects 0.000 description 2
- 238000000926 separation method Methods 0.000 description 2
- 241000894006 Bacteria Species 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- 238000002425 crystallisation Methods 0.000 description 1
- 230000008025 crystallization Effects 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 239000013067 intermediate product Substances 0.000 description 1
- 238000004321 preservation Methods 0.000 description 1
- 239000000047 product Substances 0.000 description 1
- 230000000717 retained effect Effects 0.000 description 1
- 239000002699 waste material Substances 0.000 description 1
Classifications
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D3/00—Distillation or related exchange processes in which liquids are contacted with gaseous media, e.g. stripping
- B01D3/10—Vacuum distillation
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D5/00—Condensation of vapours; Recovering volatile solvents by condensation
- B01D5/0057—Condensation of vapours; Recovering volatile solvents by condensation in combination with other processes
- B01D5/006—Condensation of vapours; Recovering volatile solvents by condensation in combination with other processes with evaporation or distillation
Landscapes
- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Vaporization, Distillation, Condensation, Sublimation, And Cold Traps (AREA)
Abstract
The invention discloses a liquid medicine reduced pressure distillation device, which comprises a reaction kettle, a condenser and a recovery box; the reaction kettle is provided with an oil bath cavity; the bottom of the oil bath cavity is provided with a heating device; a steam pipe and a return pipe are arranged at the top end of the reaction kettle; the top ends of the steam pipe and the return pipe are communicated with the rectifying device; the top end of the rectifying device is provided with an elbow, and the tail end of the elbow is communicated with the condenser; the lower part of the condenser is provided with a recovery pipe, and the lower end of the recovery pipe is inserted into the recovery box; and a vacuum pump is arranged at the top end of the recovery box. The invention adopts an oil bath heating mode to improve the heating uniformity and stability, and improves the distillation efficiency of the liquid medicine and the purity of the recovered substances by a multi-stage fractionation mode.
Description
Technical Field
The invention belongs to the technical field of adenine production, and particularly relates to a liquid medicine reduced pressure distillation device.
Background
In the adenine production process, a medicinal solution as an intermediate product is usually distilled to separate substances having different boiling points. In the traditional distillation process, steam or an electric heating rod is adopted to heat the liquid medicine. The problem with this heating method is that, first, the steam or electric heating rod is heated unevenly, which is easy to cause overheat and decompose the medicine liquid substance, and the quality of the product is unstable. Secondly, when the steam passes through the condenser, more condensed water is generated, and the efficiency of separating low boiling point substances (such as acetic anhydride and the like) is not high. Thirdly, the water vapor and the liquid medicine vapor enter the condensation pipeline together, bacteria are easy to introduce, purity of the recovered substances is affected, and recycling of the recovered substances is affected. Therefore, a novel medical liquid reduced pressure distillation apparatus is required in order to improve distillation efficiency and purity of recovered substances.
Disclosure of Invention
In order to overcome the defects in the background art, the invention provides a liquid medicine reduced pressure distillation device, which aims to improve the heating uniformity and stability by adopting an oil bath heating mode and improve the liquid medicine distillation efficiency and the purity of recovered substances by adopting a multi-stage fractionation mode.
In order to achieve the above purpose, the present invention provides the following technical solutions:
a medicinal liquid reduced pressure distillation device comprises a reaction kettle, a condenser and a recovery box; the reaction kettle is provided with an oil bath cavity for heating the liquid medicine in the reaction kettle; the bottom of the oil bath cavity is provided with a heating device for heating heat conduction oil in the oil bath cavity; a steam pipe and a return pipe are arranged at the top end of the reaction kettle; the top ends of the steam pipe and the return pipe are communicated with the rectifying device and are respectively used for conveying steam into the rectifying device and returning liquid medicine separated in the rectifying device to the reaction kettle; the top end of the rectifying device is provided with an elbow, and the tail end of the elbow is communicated with the condenser and is used for condensing low-boiling-point substances; the lower part of the condenser is provided with a recovery pipe, and the lower end of the recovery pipe is inserted into the recovery box and is used for recovering the low-boiling-point substances; the top end of the recovery tank is provided with a vacuum pump which is used for sucking gas which sequentially flows through the reaction kettle, the rectifying device, the condenser and the recovery tank to generate negative pressure in the reaction kettle.
As a further optimization, the reaction kettle and the recovery tank are arranged side by side and close to each other.
As a further optimization, the rectifying device comprises a box body, wherein a plurality of partition plates are arranged in the box body from bottom to top at intervals; one end of the partition plate is fixedly connected with the box body in a sealing way, and the other end of the partition plate is inclined downwards and is kept in a gap with the inner wall of the box body; the gaps of two adjacent baffles are opposite in orientation and are used for forming a tortuous airflow channel.
As further optimization, a cooling water coil is arranged in the partition plate; the water inlet and the water outlet of the cooling water coil pipe extend out of the side wall of the box body and are used for connecting a cooling water source.
As further optimization, the heating device comprises a heating plate positioned at the bottom of the oil bath cavity, and the heating plate is fixedly connected with a heater arranged outside the reaction kettle shell through a wire.
As a further optimization, an electric control valve is arranged on the return pipe and used for controlling the communication or closing of the return pipe.
As further optimization, a discharge pipe is arranged at the bottom of the recovery box, and a stop valve is arranged on the discharge pipe.
Compared with the prior art, the invention has the beneficial effects that:
(1) The vacuum pump is utilized for decompression, so that the production efficiency is improved, and the problem of liquid medicine denaturation caused by transitional heating is avoided.
(2) The heating mode of the oil bath is more uniform, local overheating is avoided, and the mixed steam is stable in production and high in efficiency.
(3) The purity of the recovered substances (namely, low boiling point substances) is improved by multistage fractionation of the rectifying device, and the recycling is facilitated.
(4) The whole structure is compact, high boiling point materials are automatically refluxed by utilizing gravity, the pipeline is shortened, and the cost is low.
In a word, this device adopts the mode of oil bath heating, improves homogeneity and the stability of heating to through the mode of multistage fractional distillation, improve the efficiency of liquid medicine distillation and the purity degree of retrieving the material.
Drawings
FIG. 1 is a schematic structural view of embodiment 1 of the present invention;
fig. 2 is a schematic structural view of a separator according to embodiment 1 of the present invention.
The corresponding relation between the technical characteristics and the reference numerals in the drawings is as follows: a reaction kettle 1; an oil bath chamber 11; a heating device 12; a steam pipe 13; a return pipe 14; a heater 15; an electric control valve 16; a rectifying device 2; a bent pipe 21; a case 22; a partition plate 23; a cooling water coil 24; a condenser 3; a recovery pipe 31; a recovery box 4; a discharge pipe 41; a shutoff valve 42; and a vacuum pump 5.
Detailed Description
The technical solutions in the embodiments of the present invention will be made clear below in conjunction with the accompanying drawings of the present invention; it is apparent that the described embodiments are only some of the preferred embodiments of the present invention, and not all of them. It should be understood by those skilled in the art that these embodiments are merely for explaining the technical principles of the present invention, and are not intended to limit the scope of the present invention.
Example 1: please refer to fig. 1-2;
the invention provides the following technical scheme: a medicinal liquid reduced pressure distillation device is applied to an acetic anhydride evaporation process in adenine production, and comprises a reaction kettle 1, a condenser 3 and a recovery tank 4; the shell of the reaction kettle 1 is provided with an oil bath cavity 11 for heating the liquid medicine in the reaction kettle 1; the bottom of the oil bath cavity 11 is provided with a heating device 12 for heating heat conduction oil in the oil bath cavity 11; the top end of the reaction kettle 1 is provided with a steam pipe 13 and a return pipe 14; the top ends of the steam pipe 13 and the return pipe 14 are communicated with the rectifying device 2 and are respectively used for conveying steam into the rectifying device 2 and returning liquid medicine separated in the rectifying device 2 to the reaction kettle 1; the top end of the rectifying device 2 is provided with a bent pipe 21, and the tail end of the bent pipe 21 is communicated with the condenser 3 and is used for condensing low-boiling-point substances; a recovery pipe 31 is arranged at the lower part of the condenser 3, and the lower end of the recovery pipe 31 is inserted into the recovery tank 4 for recovering the low boiling point substances; a vacuum pump 5 is arranged at the top end of the recovery tank 4 and is used for sucking the gas flowing through the reaction kettle 1, the rectifying device 2, the condenser 3 and the recovery tank 4 in sequence to generate negative pressure in the reaction kettle 1.
The working principle comprises that materials in the reaction kettle 1 are heated uniformly by oil bath, the heat preservation time is long, and mixed steam is generated stably and efficiently. When the mixed steam flows through the rectifying device 2, the mixed steam is gradually cooled, high-boiling-point substances are condensed first and then fall at the bottom of the rectifying device 2, and low-boiling-point substances still keep rising gas, so that the high-boiling-point substances and the low-boiling-point substances are separated first. Lays a foundation for improving the purity of the recovered substances, improves the yield of high-boiling-point substances and avoids waste. Secondly, the vacuum pump 5 is used for decompression, so that the actual boiling point of all substances is reduced, and the effects of reducing the heating temperature and accelerating evaporation are achieved. Thereby improving the production efficiency and avoiding the problem of medicine liquid denaturation caused by transitional heating.
For compact structure, the length of the pipeline is reduced, crystallization of the pipe wall caused by condensation in the pipeline is avoided, and the reaction kettle 1 and the recovery tank 4 are arranged side by side and close to each other. Meanwhile, the flowing distance of steam airflow is reduced, and the production efficiency is further improved.
Illustratively, the rectifying device 2 comprises a box 22, wherein a plurality of partition plates 23 are arranged at intervals in the box 22 from bottom to top; one end of the partition plate 23 is in sealing and fixing connection with the box body 22, and the other end of the partition plate is inclined downwards and is spaced from the inner wall of the box body 22; the gaps of adjacent two of the separators 23 are oppositely directed to form a meandering air flow path. It can be seen that the mixed steam bypasses each gap in turn, the temperature is gradually reduced, and the high boiling point substances are separated by utilizing the difference of the boiling points of different substances. The use of the tortuous airflow passage increases the chance of contact between the mixed vapor and the separator 23, increases the heat exchange area, and improves separation efficiency.
A further way of improving the heat exchange efficiency is that a cooling water coil 24 is arranged in the partition 23; the water inlet and outlet of the cooling water coil 24 extends out of the side wall of the box 22 for connecting to a cooling water source. The mixed steam flows through each of the partitions 23 in turn from bottom to top to improve cooling efficiency.
Illustratively, the heating device 12 comprises a heating plate at the bottom of the oil bath chamber 11, and the heating plate is connected and fixed with a heater 15 outside the shell of the reaction kettle 1 through a wire. It can be seen that the heater 15 provides power to the heating plate to cause the heating plate to generate heat. Thereby heating the heat conductive oil.
An electrically controlled valve 16 is provided on the return pipe 14 for controlling the communication or closing of the return pipe 14. It can be seen that when return line 14 is closed, the flow of steam into rectifying device 2 is reduced, so that the heat exchange of steam with baffle 23 is more complete; when the electrically controlled valve 16 is opened, the retained high boiling point material can still flow back to the reaction vessel 1. The separation effect can be further improved by intermittently opening and closing the electric control valve 16.
In order to facilitate the output of the materials in the recovery tank 4, a discharge pipe 41 is arranged at the bottom of the recovery tank 4, and a stop valve 42 is arranged on the discharge pipe 41.
When in use, the materials in the reaction kettle 1 are heated uniformly by the oil bath, and stable mixed steam is generated. When the mixed steam flows through the rectifying device 2, the mixed steam is gradually cooled from bottom to top, high boiling point substances are firstly condensed and then fall at the bottom of the rectifying device 2, and low boiling point substances still keep rising gas, so that the high boiling point substances and the low boiling point substances are separated. The high boilers return to the reactor 1 via the return line 14 and continue to rise, via the bend 21, into the condenser 3. The condensed low boiling point substances enter the recovery tank 4 through the recovery pipe 31. Meanwhile, the vacuum pump 5 pumps the gas in the recovery tank 4, and the recovery tank 4, the recovery pipe 31, the condenser 3, the bent pipe 21, the rectifying device 2, the steam pipe 13 and the reaction kettle 1 which are sequentially connected in series reduce the gas pressure under the action of the vacuum pump 5, thereby being beneficial to generating steam, improving the production efficiency and avoiding the problem of liquid medicine denaturation caused by transitional heating.
The advantage of this embodiment over the prior art is:
(1) The vacuum pump 5 is utilized to decompress, so that the production efficiency is improved, and the problem of liquid medicine denaturation caused by transitional heating is avoided.
(2) The heating mode of the oil bath is more uniform, local overheating is avoided, and the mixed steam is stable in production and high in efficiency.
(3) The purity of the recovered substances (i.e., low boiling point substances) is improved by the multistage fractionation of the rectifying device 2, which is beneficial to reutilization.
(4) The whole structure is compact, high boiling point materials are automatically refluxed by utilizing gravity, the pipeline is shortened, and the cost is low.
In a word, this device adopts the mode of oil bath heating, improves homogeneity and the stability of heating to through the mode of multistage fractional distillation, improve the efficiency of liquid medicine distillation and the purity degree of retrieving the material.
The invention has not been described in detail in the prior art; it should be understood by those skilled in the art that any combination of the features of the foregoing embodiments may be adopted, and that all possible combinations of the features of the foregoing embodiments are not described for brevity of description, however, such combinations are not to be considered as a contradiction between the features. The scope of the invention is defined by the appended claims and equivalents thereof.
Claims (7)
1. A medicinal liquid reduced pressure distillation device comprises a reaction kettle (1), a condenser (3) and a recovery box (4); the method is characterized in that: the reaction kettle (1) is provided with an oil bath cavity (11) for heating the liquid medicine in the reaction kettle (1); the bottom of the oil bath cavity (11) is provided with a heating device (12) for heating heat conduction oil in the oil bath cavity (11); a steam pipe (13) and a return pipe (14) are arranged at the top end of the reaction kettle (1); the top ends of the steam pipe (13) and the return pipe (14) are communicated with the rectifying device (2) and are respectively used for conveying steam into the rectifying device (2) and returning liquid medicine separated in the rectifying device (2) to the reaction kettle (1); the top end of the rectifying device (2) is provided with an elbow (21), and the tail end of the elbow (21) is communicated with the condenser (3) and is used for condensing low-boiling-point substances; a recovery pipe (31) is arranged at the lower part of the condenser (3), and the lower end of the recovery pipe (31) is inserted into the recovery box (4) for recovering the low-boiling-point substances;
the top end of the recovery box (4) is provided with a vacuum pump (5) for sucking gas flowing through the reaction kettle (1), the rectifying device (2), the condenser (3) and the recovery box (4) in sequence to generate negative pressure in the reaction kettle (1).
2. The reduced pressure distillation apparatus for medical fluid according to claim 1, wherein: the reaction kettle (1) and the recovery tank (4) are arranged side by side and close to each other.
3. A reduced pressure distillation apparatus for medical fluid according to claim 2, wherein: the rectifying device (2) comprises a box body (22), wherein a plurality of partition plates (23) are arranged in the box body (22) from bottom to top at intervals; one end of the partition plate (23) is fixedly connected with the box body (22) in a sealing way, and the other end of the partition plate is inclined downwards and is kept in a gap with the inner wall of the box body (22); the gaps of two adjacent partition plates (23) are opposite in orientation and are used for forming a tortuous airflow channel.
4. A reduced pressure distillation apparatus for medical fluid according to claim 3, wherein: a cooling water coil pipe (24) is arranged in the partition plate (23); the water inlet and outlet of the cooling water coil pipe (24) extend out of the side wall of the box body (22) and are used for connecting a cooling water source.
5. The reduced pressure distillation apparatus for medical fluid according to claim 4, wherein: the heating device (12) comprises a heating plate positioned at the bottom of the oil bath cavity (11), and the heating plate is fixedly connected with a heater (15) arranged outside the shell of the reaction kettle (1) through a wire.
6. The reduced pressure distillation apparatus for medical fluid according to claim 5, wherein: an electrically controlled valve (16) is arranged on the return pipe (14) and is used for controlling the communication or closing of the return pipe (14).
7. The reduced pressure distillation apparatus for medical fluid according to claim 6, wherein: a discharge pipe (41) is arranged at the bottom of the recovery box (4), and a stop valve (42) is arranged on the discharge pipe (41).
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202310961268.0A CN116983693A (en) | 2023-08-01 | 2023-08-01 | Liquid medicine decompression distillation device |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202310961268.0A CN116983693A (en) | 2023-08-01 | 2023-08-01 | Liquid medicine decompression distillation device |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN116983693A true CN116983693A (en) | 2023-11-03 |
Family
ID=88526090
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202310961268.0A Pending CN116983693A (en) | 2023-08-01 | 2023-08-01 | Liquid medicine decompression distillation device |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN116983693A (en) |
-
2023
- 2023-08-01 CN CN202310961268.0A patent/CN116983693A/en active Pending
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