CN209317064U - A kind of vacuum distillation production system preparing the chloro- 6,6- dimethyl -2- heptene -4- alkynes of 1- - Google Patents
A kind of vacuum distillation production system preparing the chloro- 6,6- dimethyl -2- heptene -4- alkynes of 1- Download PDFInfo
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- CN209317064U CN209317064U CN201822226427.XU CN201822226427U CN209317064U CN 209317064 U CN209317064 U CN 209317064U CN 201822226427 U CN201822226427 U CN 201822226427U CN 209317064 U CN209317064 U CN 209317064U
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Abstract
The utility model discloses a kind of vacuum distillation production system for preparing chloro- 6, the 6- dimethyl -2- heptene -4- alkynes of 1-, glassed steel reaction vessels, rectifying column and the first condenser in the system are sequentially communicated by pipeline.First condenser is connected with the first solvent collecting tank and product collecting tank respectively by pipeline.First solvent collecting tank and product collecting tank pass through pipeline respectively and are connected with the import of vacuum pump.Vacuum pump, the second condenser, the second solvent collecting tank and spray column are sequentially communicated by pipeline.The quantity of the active carbon adsorber is two, and is connected in parallel on the first gas outlet of the spray column.The control valve of control piper on-off is separately provided on pipeline between the active carbon adsorber and spray column.The system can be effectively reduced the content of organic solvent in tail gas, and tail gas is made to reach national VOCs discharge standard.
Description
Technical field
The utility model relates to medical equipment technical field, in particular to the intermediate 1- of a kind of terbinafine HCl is chloro-
The vacuum distillation production system of 6,6- dimethyl -2- heptene -4- alkynes.
Background technique
Chloro- 6, the 6- dimethyl -2- heptene -4- alkynes of 1-, molecular formula: C9H13Cl, molecular weight: 156.65, CAS registration numbers:
126764-17-8 is a kind of weak yellow liquid.The chloro- 6,6- dimethyl -2- heptene -4- alkynes of 1- is Allylamines antifungal drug
The important intermediate of terbinafine HCl, currently, the intermediate international market demand is being continuously increased, and the demand of European & American Market
It measures especially considerable.Due to generally use at present production technology preparation product purity generally not high (70~90%), quality reaches
Quality requirement less than drug act in relation to starting material and advanced intermediate, affects the export sales of the product.In order to mention
High product purities generally take the modes such as distillation or rectifying to improve product purity at present, but since the solvent in organic phase is dirt
Biggish organic matter is contaminated, and volatile, environmental pollution is easily caused in vacuum distillation process.Therefore, in order in raising product matter
While amount, reduce pollution to atmosphere, need to 6,6- dimethyl -2- heptene -4- alkynes chloro- to 1- vacuum distillation production system into
Row improves.
Utility model content
Subtracting for chloro- 6, the 6- dimethyl -2- heptene -4- alkynes of 1- is prepared in response to the above problems, the present invention proposes a kind of
Pressure distillation production system, environmental issue proposed in system effective solution background technique.
The technical solution adopted by the utility model to solve its technical problems is that:
A kind of vacuum distillation production system preparing chloro- 6, the 6- dimethyl -2- heptene -4- alkynes of 1-, including enamel reaction
Kettle, rectifying column, the first condenser, the first solvent collecting tank, product collecting tank and vacuum pump, further include the second condenser, second
Solvent collecting tank, spray column and active carbon adsorber, and the second condenser, the second solvent collecting tank, spray column and the work
Property charcoal absorber is sequentially communicated by pipeline, and the import of second condenser is connected with the outlet of the vacuum pump.
Further, the quantity of the active carbon adsorber is multiple and in parallel with the spray column, the active carbon
Control valve is respectively arranged on pipeline between absorber and spray column.
Further, the spray column includes tower body, and the inner space of the tower body is in turn divided into from top to bottom removes
Fog-zone, second level spraying zone, level-one spraying zone and race way are successively set from top to bottom in the level-one spraying zone and second level spraying zone
It is equipped with spray tube, many-sided ball filler and porous plate, spiral nozzle is provided on the spray tube, is provided on the tower body
The liquid outlet being connected with race way, and the liquid outlet is connected by circulating pump with the spray tube.
Further, a partition is provided in the race way, and the race way is divided by the partition
Area and storage area are stood, is provided with a deflector for tilting down setting, the liquid outlet and institute above the storage area
The storage area stated is connected.
Further, the spiral nozzle includes one in the cone curved hollow pipe of helical form, the lower end of the hollow pipe
Upper end setting for cecum, the hollow pipe is connected by connector with spray tube, has been uniformly arranged on the hollow pipe more
A spray hole.
Further, the diameter of the hollow pipe is gradually reduced from top to bottom.
Further, the spray hole extends radially through the hollow pipe.
Further, the active carbon adsorber includes shell, and multiple first supports are arranged at intervals in the shell
Plate and the second supporting plate are filled with active carbon filler between adjacent the first supporting plate and the second supporting plate, tail gas is in the first supporting plate and the
Broken line movement is done under the guiding role of two supporting plates.
The beneficial effects of the utility model are:
1, tail gas is handled by setting spray column and active carbon adsorber, the dirt to atmosphere can be effectively reduced
Dye makes the tail gas of discharge reach national VOCs discharge standard.
2, by the way that the second condenser is arranged between screw vacuum pump and exhaust gas processing device, and condensation is obtained organic
Solvent is collected, and can effectively reduce the volatilization of organic solvent, reduces the burden of device for absorbing tail gas.
3, the active carbon adsorber is set as two, on the one hand, can control work according to the discharge amount of tail gas
On the other hand the quantity of active carbon adsorber when needing to carry out replacement to active carbon adsorber, can not stop work
In the case of carry out, avoid impacting manufacturing schedule.
Detailed description of the invention
Fig. 1 is the structural schematic diagram of this production system；
The structural schematic diagram of Fig. 2 spray column；
Fig. 3 is the enlarged structure schematic diagram of part A in Fig. 2；
Fig. 4 is the A-A cross-sectional view in Fig. 3；
Fig. 5 is the structural schematic diagram of active carbon adsorber
Fig. 6 is the schematic diagram of internal structure of active carbon adsorber.
In figure: 1- glassed steel reaction vessels, 2- rectifying column, the first condenser of 3-, 4- the first solvent collecting tank, 5- product are collected
Tank, 6- vacuum pump, the second condenser of 71-, 72- the second solvent collecting tank, 81- spray column, the first air inlet of 811-, 812- first
Gas outlet, 813- partition, 814- deflector, 815- spray tube, 8151- spiral nozzle, 816- many-sided ball filler, 817- are porous
Plate, 818- demister, 819- liquid outlet, 82- active carbon adsorber, 821- shell, the second air inlet of 822-, the second outlet of 823-
Mouthful, the first supporting plate of 824-, the second supporting plate of 825-, 826- active carbon filler, 827- feeding port.
Specific embodiment
As shown in Figure 1, a kind of vacuum distillation production system for preparing chloro- 6, the 6- dimethyl -2- heptene -4- alkynes of 1- includes warding off
Glass reaction kettle 1, rectifying column 2, the first condenser 3, the first solvent collecting tank 4, product collecting tank 5, vacuum pump 6, second condense
Device 71, the second solvent collecting tank 72, spray column 81 and active carbon adsorber 82.
Wherein, the glassed steel reaction vessels 1, rectifying column 2 and the first condenser 3 are sequentially communicated by pipeline.Described
First condenser 3 is connected with the first solvent collecting tank 4 and product collecting tank 5 respectively by pipeline, and described first
On pipeline on pipeline between condenser 3 and the first solvent collecting tank 4 and between the first condenser 3 and product collecting tank 5
It is provided with the control valve for control piper on-off.The first solvent collecting tank 4 and product collecting tank 5 pass through pipe respectively
Road is connected with the import of vacuum pump 6.Vacuum pump 6, the second condenser 71, the second solvent collecting tank 72 and the spray column 81
It is sequentially communicated by pipeline.The quantity of the active carbon adsorber 82 is two, and is connected in parallel on the first of the spray column 81 and goes out
On port 812.Control piper on-off is separately provided on pipeline between the active carbon adsorber 82 and spray column 81
Control valve.
Be arranged herein the second condenser 71 and the second solvent collecting tank 72 the purpose is to reduce the volatilization of organic solvent, drops
The burden of low exhaust gas absorption plant.
The active carbon adsorber 82 is set as two, there are two main cause is,
First, the quantity of the active carbon adsorber 82 of work can be controlled according to the discharge amount of tail gas.
Second, when needing to carry out replacement to active carbon adsorber 82, it can carry out, keep away without stopping work
Exempt to impact manufacturing schedule.
As shown in Fig. 2, the spray column 81 includes tower body, the interior not space of the tower body from top to bottom may be used according to function
It is in turn divided into mist eliminating zone, second level spraying zone, level-one spraying zone and race way.It is located at the level-one on the tower body to spray
It is provided with the first air inlet 811 between area and race way, is located above the mist eliminating zone on the tower body and is provided with first
Gas outlet 812.
Demister 818 is provided in the mist eliminating zone, the demister is the prior art, and details are not described herein.
The level-one spraying zone is identical with the structure in second level spraying zone, is disposed with spray tube 815, more from top to bottom
Face ball filler 816 and porous plate 817 for many-sided ball filler 816 described in support.
Be provided with a liquid outlet 819 being connected with the race way on the tower body, the liquid outlet 819 with
The import of circulating pump (not regarding out in figure) is connected, the outlet of the circulating pump by pipeline respectively with the level-one spraying zone and two
The spray tube 815 of grade spraying zone is connected, to realize recycling for spray liquid.
It uses two-stage to spray herein primarily to coming into full contact with tail gas with spray liquid, improves the effect of tail gas absorption
Fruit.
Further, since spray liquid during the work time can be contaminated, the muddiness of change, in order to avoid miscellaneous in spray liquid
Matter causes spray blockage, as shown in Fig. 2, being provided with a partition 813 being arranged along the vertical direction in the race way, and institute
The race way is divided into the horizontal direction and stands area and storage area by the partition 813 stated, and is located on the tower body described
A deflector 814 for tilting down setting is fixedly installed above storage area, and the free end of the deflector 814 extends to
The top for standing area, the liquid outlet 819 are connected with the storage area.
The spray liquid flowed down in this way from top flows down in the guide functions of deflector 814 into standing area, miscellaneous in area standing
Matter can sink to bottom, and the impure less spray liquid on top can cross partition 813 and flow into storage area, then pass through circulation
Pump, which enters in spray tube 815, to be sprayed.
Further, in order to which the atomizing effect for improving spray liquid is set on the spray tube 815 as shown in Figure 3 and Figure 4
It is equipped with spiral nozzle 8151.The spiral nozzle 8151 includes one in the cone curved hollow pipe of helical form, and the hollow pipe
Diameter be gradually reduced from top to bottom.The lower end of the hollow pipe is cecum, and the upper end of the hollow pipe is provided with a connector, institute
The connector stated is fixedly connected by screw thread with the spray tube 815, and the hollow pipe passes through connector and the spray
Pipe 815 is connected.Be uniformly arranged multiple spray holes on the hollow pipe, and as shown in figure 4, the spray hole radially
Through the hollow pipe.
Connector described herein is an integral structure with the hollow pipe, names description merely for convenience respectively.
The connector is a vertical pipe, and the outside of the vertical pipe is provided with external screw thread.
As shown in Figure 5 and Figure 6, the active carbon adsorber 82 includes shell 821, and the lower end of the shell 821 is arranged
There is the second air inlet 822, the upper end of the shell 821 is provided with the second gas outlet 823.As shown in fig. 6, the shell 821
Multiple first supporting plates 824 and the second supporting plate 825 are inside provided with, and first supporting plate 824 and the second supporting plate 825 is spaced cloth
It sets, active carbon filler 826 is filled between adjacent the first supporting plate 824 and the second supporting plate 825.First supporting plate 824
Left-half is provided with venthole, and the right half part of second supporting plate 825 is provided with venthole.For the convenience of description, existing will
Region between adjacent first supporting plate and the second supporting plate is defined as packing area, opposite with the packing area on the shell 821
The feeding port 827 for loading active carbon filler is provided on the position answered.
In this way, at work, tail gas will mode as shown by the arrows in Figure 6 do broken line movement, under identical height, prolong
The motion path for having grown tail gas is conducive to improve adsorption effect.
Left-half and right half part described herein be only for the positional relationship in Fig. 6, it is only a kind of
Relativeness.
As a kind of specific embodiment, ceramic raschig rings are filled in rectifying column 2 described in the present embodiment.Described
First condenser 3 uses glass-lined disc-type condenser, and the vacuum pump 6 uses screw vacuum pump 6, second condensation
Device 71 uses helix tube condenser.
When work, organic phase is evaporated under reduced pressure in glassed steel reaction vessels 1, is fractionated through rectifying column 2, the first condenser 3
After condensation, entered in the first solvent collecting tank 4 or product collecting tank 5 by pipeline.The second condenser 71 is connected after vacuum pump 6
The solvent of volatilization is further cooled down, cooling solvent is collected into the second solvent collecting tank 72, on the second solvent collecting tank 72
The pipeline of side is connected to exhaust gas processing device, by spray column 81 in exhaust gas processing device and active carbon adsorber 82 to tail gas
It is handled.
Claims (8)
1. a kind of vacuum distillation production system for preparing chloro- 6, the 6- dimethyl -2- heptene -4- alkynes of 1-, including glassed steel reaction vessels,
Rectifying column, the first condenser, the first solvent collecting tank, product collecting tank and vacuum pump, it is characterised in that: further include the second condensation
Device, the second solvent collecting tank, spray column and active carbon adsorber, and second condenser, the second solvent collecting tank, spray
Tower and active carbon adsorber are sequentially communicated by pipeline, the import and the outlet phase of the vacuum pump of second condenser
Even.
2. a kind of vacuum distillation production system for preparing the chloro- 6,6- dimethyl -2- heptene -4- alkynes of 1- according to claim 1
System, it is characterised in that: the quantity of the active carbon adsorber is multiple and in parallel with the spray column, the active carbon suction
Control valve is respectively arranged on pipeline between adnexa and spray column.
3. a kind of vacuum distillation production system for preparing the chloro- 6,6- dimethyl -2- heptene -4- alkynes of 1- according to claim 1
System, it is characterised in that: the spray column includes tower body, and the inner space of the tower body is in turn divided into demisting from top to bottom
Area, second level spraying zone, level-one spraying zone and race way are set gradually from top to bottom in the level-one spraying zone and second level spraying zone
Have spray tube, many-sided ball filler and porous plate, spiral nozzle be provided on the spray tube, be provided on the tower body with
The liquid outlet that race way is connected, and the liquid outlet is connected by circulating pump with the spray tube.
4. a kind of vacuum distillation production system for preparing the chloro- 6,6- dimethyl -2- heptene -4- alkynes of 1- according to claim 3
System a, it is characterised in that: partition is provided in the race way, and the race way is divided into standing by the partition
Area and storage area, are provided with a deflector for tilting down setting above the storage area, the liquid outlet and described
Storage area is connected.
5. a kind of vacuum distillation production system for preparing the chloro- 6,6- dimethyl -2- heptene -4- alkynes of 1- according to claim 3
System, it is characterised in that: the spiral nozzle includes one in the cone curved hollow pipe of helical form, and the lower end of the hollow pipe is blind
The upper end setting at end, the hollow pipe is connected by connector with spray tube, and multiple sprays have been uniformly arranged on the hollow pipe
Fluid apertures.
6. a kind of vacuum distillation production system for preparing the chloro- 6,6- dimethyl -2- heptene -4- alkynes of 1- according to claim 5
System, it is characterised in that: the diameter of the hollow pipe is gradually reduced from top to bottom.
7. a kind of vacuum distillation production system for preparing the chloro- 6,6- dimethyl -2- heptene -4- alkynes of 1- according to claim 5
System, it is characterised in that: the spray hole extends radially through the hollow pipe.
8. a kind of vacuum distillation production system for preparing the chloro- 6,6- dimethyl -2- heptene -4- alkynes of 1- according to claim 1
System, it is characterised in that: the active carbon adsorber includes shell, be arranged at intervals in the shell multiple first supporting plates and
Second supporting plate is filled with active carbon filler between adjacent the first supporting plate and the second supporting plate, tail gas is in the first supporting plate and the second support
Broken line movement is done under the guiding role of plate.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201822226427.XU CN209317064U (en) | 2018-12-27 | 2018-12-27 | A kind of vacuum distillation production system preparing the chloro- 6,6- dimethyl -2- heptene -4- alkynes of 1- |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201822226427.XU CN209317064U (en) | 2018-12-27 | 2018-12-27 | A kind of vacuum distillation production system preparing the chloro- 6,6- dimethyl -2- heptene -4- alkynes of 1- |
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| Publication Number | Publication Date |
|---|---|
| CN209317064U true CN209317064U (en) | 2019-08-30 |
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| CN201822226427.XU Active CN209317064U (en) | 2018-12-27 | 2018-12-27 | A kind of vacuum distillation production system preparing the chloro- 6,6- dimethyl -2- heptene -4- alkynes of 1- |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112791687A (en) * | 2021-01-29 | 2021-05-14 | 中国科学技术大学 | Integrated device for preparing, separating and purifying enol silyl ether |
-
2018
- 2018-12-27 CN CN201822226427.XU patent/CN209317064U/en active Active
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112791687A (en) * | 2021-01-29 | 2021-05-14 | 中国科学技术大学 | Integrated device for preparing, separating and purifying enol silyl ether |
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Address after: 251400 No. 12, Taixing East Street, Jibei Economic Development Zone, Jiyang District, Jinan City, Shandong Province Patentee after: Shandong Baoyuan Pharmaceutical Co.,Ltd. Address before: Strong in Jiyang County of Ji'nan City, 251400 North Street, Shandong Province Economic Development Zone Patentee before: SHANDONG BOYUAN PHARMACEUTICAL Co.,Ltd. |