CN212548349U - Vacuum rotary evaporation kettle for purifying high-viscosity ionic liquid - Google Patents
Vacuum rotary evaporation kettle for purifying high-viscosity ionic liquid Download PDFInfo
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- CN212548349U CN212548349U CN202020803936.9U CN202020803936U CN212548349U CN 212548349 U CN212548349 U CN 212548349U CN 202020803936 U CN202020803936 U CN 202020803936U CN 212548349 U CN212548349 U CN 212548349U
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- heating
- ionic liquid
- kettle body
- heating kettle
- rotary evaporation
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- 239000002608 ionic liquid Substances 0.000 title claims abstract description 62
- 238000002390 rotary evaporation Methods 0.000 title claims abstract description 19
- 238000010438 heat treatment Methods 0.000 claims abstract description 68
- 238000003756 stirring Methods 0.000 claims abstract description 23
- 238000000746 purification Methods 0.000 claims abstract description 14
- 238000005485 electric heating Methods 0.000 claims description 6
- 238000009833 condensation Methods 0.000 claims description 4
- 230000005494 condensation Effects 0.000 claims description 4
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 4
- 230000008878 coupling Effects 0.000 claims description 3
- 238000010168 coupling process Methods 0.000 claims description 3
- 238000005859 coupling reaction Methods 0.000 claims description 3
- 239000004033 plastic Substances 0.000 claims description 3
- 229920003023 plastic Polymers 0.000 claims description 3
- 238000007789 sealing Methods 0.000 claims description 2
- 238000004519 manufacturing process Methods 0.000 abstract description 7
- 238000002156 mixing Methods 0.000 abstract description 6
- 238000001704 evaporation Methods 0.000 abstract description 5
- 230000008020 evaporation Effects 0.000 abstract description 3
- 230000009286 beneficial effect Effects 0.000 abstract description 2
- 230000000694 effects Effects 0.000 abstract description 2
- 239000006260 foam Substances 0.000 description 24
- 239000012459 cleaning agent Substances 0.000 description 6
- 239000007788 liquid Substances 0.000 description 5
- 238000000034 method Methods 0.000 description 5
- 239000000047 product Substances 0.000 description 4
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 description 3
- XEKOWRVHYACXOJ-UHFFFAOYSA-N Ethyl acetate Chemical compound CCOC(C)=O XEKOWRVHYACXOJ-UHFFFAOYSA-N 0.000 description 3
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 description 3
- 230000005587 bubbling Effects 0.000 description 3
- 238000003786 synthesis reaction Methods 0.000 description 3
- 239000006227 byproduct Substances 0.000 description 2
- 239000002994 raw material Substances 0.000 description 2
- 150000001335 aliphatic alkanes Chemical class 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 238000004140 cleaning Methods 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- 238000007599 discharging Methods 0.000 description 1
- 150000002170 ethers Chemical class 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
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- Vaporization, Distillation, Condensation, Sublimation, And Cold Traps (AREA)
Abstract
The utility model discloses a vacuum rotary evaporation kettle for high viscosity ionic liquid purification, including the heating kettle body, explosion-proof gear motor, draft tube and heating defoaming subassembly, explosion-proof gear motor fixes the top of the heating kettle body, the position that the heating kettle body lies in explosion-proof gear motor both sides is equipped with charge door and vacuum tube respectively, the bottom of heating kettle is equipped with the discharge gate, explosion-proof gear motor's motor shaft end fixedly connected with (mixing) shaft, the lower extreme fixedly connected with agitator of (mixing) shaft, the draft tube is fixed in the stirring paddle leaf top of agitator, the (mixing) shaft passes the heating kettle body and draft tube, be connected for sealed rotation between (mixing) shaft and the heating kettle body, clearance between draft tube and the heating kettle body inner wall forms the defoaming passageway, the heating defoaming subassembly is fixed in the defoaming passageway. The utility model has the advantages of simple structure can improve production efficiency to can prevent effectively that ionic liquid from being smugglied away along with the evaporation of cleaner, beneficial effect such as purification effect is good.
Description
Technical Field
The utility model belongs to the technical field of the ionic liquid purification technique and specifically relates to a cauldron is evaporated soon in vacuum for high viscosity ionic liquid purification is related to.
Background
The production synthesis of ionic liquids generally comprises two steps of synthesis reaction and purification. After the synthesis reaction is finished, residual raw materials and byproducts are carried in the target product ionic liquid, so that further purification is needed. And cleaning agents such as ethyl acetate, acetone, toluene, alkanes, ethers and the like are required for subsequent purification. The cleaning agent is used for cleaning impurities such as residual raw materials, byproducts and the like, and the last purification step is to carry out rotary evaporation on the ionic liquid product under the vacuum condition so as to remove the cleaning agent from the ionic liquid product.
At present, the conventional vacuum rotary evaporation kettle comprises a kettle body, a stirrer, a steam jacket and other structures which can be vacuumized, and as the high-viscosity ionic liquid has very high viscosity, large bubbles are very easily generated when the high-viscosity ionic liquid is subjected to vacuum rotary evaporation in the kettle body, and the evaporated cleaning agent can entrain the bubbles to form more foams, so that the ionic liquid is subjected to bumping, and meanwhile, part of the ionic liquid can be entrained to cause the loss of the ionic liquid.
The existing solutions generally include the following: firstly, the feeding amount of the ionic liquid during each purification is reduced, the generation of bubbles is inhibited, but the feeding amount is small, and the production efficiency is not improved; secondly, a traditional silk screen demister is arranged in the kettle body, but ionic liquid bubbles are gathered in the silk screen of the demister, so that the defoaming effect cannot be achieved finally, and the air resistance of the cleaning agent can be increased; the rotary evaporation temperature of the ionic liquid is increased, the viscosity of the ionic liquid is reduced (the viscosity of the ionic liquid is generally reduced along with the increase of the temperature), but a large amount of heat energy is consumed, and the product is easily discolored at high temperature; fourthly, the degree of vacuum is reduced to inhibit the generation of foam, but the rotary evaporation time is increased, and the cleaning agent cannot be removed sufficiently.
SUMMERY OF THE UTILITY MODEL
The utility model relates to a solve the above-mentioned technical problem that prior art exists, provide a simple structure, can improve production efficiency to can prevent effectively that ionic liquid from being taken away along with the evaporation of cleaner by the clamp, the purification is effectual is used for the vacuum of high viscosity ionic liquid purification to evaporate the cauldron soon.
In order to achieve the above purpose, the utility model adopts the following technical scheme:
a vacuum rotary evaporation kettle for purifying high-viscosity ionic liquid comprises a heating kettle body and an explosion-proof speed reducing motor, the explosion-proof speed reducing motor is fixed at the top of the heating kettle body, the positions of the heating kettle body, which are positioned at the two sides of the explosion-proof speed reducing motor, are respectively provided with a feed inlet and a vacuum tube, the bottom of the heating kettle is provided with a discharge outlet, the end part of a motor shaft of the explosion-proof speed reducing motor is fixedly connected with a stirring shaft, the lower end of the stirring shaft is fixedly connected with a stirrer, the vacuum rotary evaporation kettle for purifying the high-viscosity ionic liquid also comprises a guide shell and a heating defoaming component, the draft tube is fixed above the stirring blade of the stirrer, the stirring shaft penetrates through the heating kettle body and the draft tube, the stirring shaft is rotatably connected with the heating kettle body and the draft tube in a sealing manner, a defoaming channel is formed in a gap between the draft tube and the inner wall of the heating kettle body, and the heating defoaming assembly is fixed in the defoaming channel. The invention of the utility model is characterized in that: at the internal draft tube that has set up of heating kettle, make the draft tube and the internal wall of heating kettle between the space form and remove the foam passageway, it removes the foam subassembly to be provided with the heating again in removing the foam passageway, such setting up makes the cleaner of evaporation and the ionic liquid foam of being smugglied secretly can only rise and guarantee to be heated by abundant through removing the foam passageway, the ionic liquid foam of being smugglied secretly removes the foam subassembly heating back through the heating, viscosity reduces rapidly, the foam breaks and falls to the cauldron bottom again of the liquid drop that forms ionic liquid, collide with the ionic liquid foam in ionic liquid's liquid drop whereabouts in-process simultaneously, also can cause the fracture of ionic liquid foam, further reduce the production of ionic liquid foam, thereby make the utility model discloses under great vacuum and stirring speed, ionic liquid's bumping and smuggleing secretly phenomenon can not appear yet.
Preferably, the guide shell has a cylindrical structure with two closed ends, and the upper end surface of the guide shell is a spherical surface. The upper end surface of the guide cylinder is a spherical surface, so that ionic liquid is not easy to accumulate.
Preferably, the guide shell is fixed in the heating kettle body through connecting plates circumferentially arranged at intervals, one end of each connecting plate is fixedly connected with the outer wall of the guide shell, and the other end of each connecting plate is fixedly connected with the inner wall of the heating kettle body.
Preferably, the heating and defoaming assembly is arranged around the guide cylinder, the heating and defoaming assembly is a spiral steam pipe or a spiral electric heating pipe, and the surface of the spiral steam pipe or the spiral electric heating pipe is sprayed with plastic.
Preferably, a steam jacket is arranged on the outer side of the heating kettle body, a steam inlet is connected to the upper part of the steam jacket, and a condensation water port is connected to the bottom of the steam jacket.
Preferably, the end part of the motor shaft of the explosion-proof speed reduction motor and the lower end of the stirring shaft are respectively and fixedly connected with the upper end of the stirring shaft and the stirrer through shaft couplers.
Preferably, the agitator is an anchor agitator.
Therefore, the utility model discloses following beneficial effect has: through the cooperation of draft tube and heating defoaming subassembly, make the ionic liquid foam that smugglies secretly remove the heating of foam subassembly through the heating in the defoaming passageway, viscosity reduces rapidly, and the foam breaks and falls to the cauldron bottom again forming ionic liquid's liquid drop, collides with the ionic liquid foam in ionic liquid's liquid drop whereabouts in-process simultaneously, also can cause the fracture of ionic liquid foam, further reduces the production of ionic liquid foam, thereby makes the utility model discloses under great vacuum and stirring speed, ionic liquid's bumping and smuggleing the phenomenon secretly can not appear yet, solved the bumping problem that ionic liquid takes place easily when evaporating soon.
Drawings
Fig. 1 is a cross-sectional view of the present invention.
Fig. 2 is a top view of the middle guide shell of the present invention.
In the figure: the heating kettle comprises a heating kettle body 1, an explosion-proof speed reducing motor 2, a feeding port 3, a vacuum tube 4, a discharging port 5, a stirring shaft 6, a stirrer 7, a guide cylinder 8, a heating defoaming assembly 9, a defoaming channel 10, a steam jacket 11, a steam inlet 12, a condensation water port 13 and a connecting plate 14.
Detailed Description
The invention is further described with reference to the accompanying drawings and the detailed description.
As shown in fig. 1 and fig. 2, a vacuum rotary evaporation kettle for purifying high-viscosity ionic liquid comprises a heating kettle body 1, an explosion-proof speed-reducing motor 2, a draft tube 8 and a heating defoaming assembly 9, wherein the explosion-proof speed-reducing motor is fixed on the top of the heating kettle body through a motor support, a steam jacket 11 is fixed on the outer side of the heating kettle body, the upper part of the steam jacket is connected with a steam inlet 12, the bottom of the steam jacket is connected with a condensation water gap 13, the heating kettle body is provided with a feed inlet 3 and a vacuum tube 4 respectively at the positions at two sides of the explosion-proof speed-reducing motor, the bottom of the heating kettle is provided with a discharge port 5, the motor shaft end part of the explosion-proof speed-reducing motor is fixedly connected with a stirring shaft 6 through a coupling, the lower end of the stirring shaft is fixedly connected with a stirrer 7 through the coupling, the stirrer is an anchor stirrer, the draft, the up end of draft tube is established to spherical face, the draft tube is fixed in heating the cauldron internal through connecting plate 14 that circumference interval set up, connecting plate one end and draft tube outer wall fixed connection, the connecting plate other end and the internal wall fixed connection of heating cauldron, the (mixing) shaft passes the heating cauldron body and draft tube, the (mixing) shaft and the heating cauldron body, be sealed rotation between the draft tube and be connected, clearance between draft tube and the heating cauldron internal wall forms defoaming passageway 10, heating defoaming subassembly is fixed in the defoaming passageway, heating defoaming subassembly is for the spiral electric heating pipe who encircles the draft tube setting, the surface of spiral electric heating pipe is sprayed plastics.
The utility model discloses an operation principle is: opening vacuum (vacuum degree is-0.85 atm), introducing steam into a steam jacket outside the heating kettle to heat the ionic liquid in the heating kettle body, heating the ionic liquid in the heating kettle body to Ta and heating a defoaming component to (Ta + 20) DEG C (the bubbling size of the ionic liquid changes with the temperature under a certain vacuum degree and stirring speed, and has the maximum bubbling speed under a certain temperature, namely Ta, Ta is always influenced by specific process conditions, the measurement needs to be independently measured according to the process conditions, the general empirical value is between 80 and 150 ℃), starting an explosion-proof speed-reducing motor to stir the stirrer (stirring speed is 45 r/min), slowly bubbling in the heating kettle body, heating entrained ionic liquid foam in a defoaming channel through a heating defoaming component, rapidly reducing the viscosity, and breaking the foam to form droplets of the ionic liquid to fall to the bottom of the kettle again, simultaneously at ionic liquid's liquid drop whereabouts in-process and ionic liquid foam bump, cause the fracture of ionic liquid foam, further reduce the production of ionic liquid foam, thereby make the utility model discloses under great vacuum and stirring speed, ionic liquid's bumping and smuggleing the phenomenon secretly can not appear yet, solved ionic liquid and evaporated the bumping problem that takes place easily when evaporating soon, steadily evaporate soon to no bubble generation, ionic liquid purification finishes, the cooling back from the discharge gate ejection of compact can.
The above-described embodiments are only preferred embodiments of the present invention, and are not intended to limit the present invention in any way, and other variations and modifications may be made without departing from the scope of the claims.
Claims (7)
1. A vacuum rotary evaporation kettle for purifying high-viscosity ionic liquid comprises a heating kettle body (1) and an explosion-proof speed reducing motor (2), wherein the explosion-proof speed reducing motor is fixed at the top of the heating kettle body, a feed inlet (3) and a vacuum tube (4) are respectively arranged at the positions of the heating kettle body, which are positioned at the two sides of the explosion-proof speed reducing motor, a discharge port (5) is arranged at the bottom of the heating kettle, a stirring shaft (6) is fixedly connected with the end part of a motor shaft of the explosion-proof speed reducing motor, and a stirrer (7) is fixedly connected with the lower end of the stirring shaft, and is characterized in that the vacuum rotary evaporation kettle for purifying high-viscosity ionic liquid further comprises a guide cylinder (8) and a heating defoaming component (9), the guide cylinder is fixed above a stirring paddle of the stirrer and penetrates through the heating kettle body and the guide cylinder, the stirring shaft is connected with the heating kettle body and the guide cylinder in a sealing rotation manner, the heating defoaming component is fixed in the defoaming channel.
2. The vacuum rotary evaporation kettle for purifying high-viscosity ionic liquid as claimed in claim 1, wherein the guide shell is a cylindrical structure with two closed ends, and the upper end surface of the guide shell is a spherical surface.
3. The vacuum rotary evaporation kettle for purifying high-viscosity ionic liquid according to claim 1 or 2, wherein the guide shell is fixed in the heating kettle body through connecting plates (14) arranged at intervals in the circumferential direction, one end of each connecting plate is fixedly connected with the outer wall of the guide shell, and the other end of each connecting plate is fixedly connected with the inner wall of the heating kettle body.
4. The vacuum rotary evaporation kettle for purifying high-viscosity ionic liquid according to claim 1, wherein the heating and defoaming assembly is arranged around the guide cylinder, the heating and defoaming assembly is a spiral steam pipe or a spiral electric heating pipe, and the surface of the spiral steam pipe or the spiral electric heating pipe is sprayed with plastic.
5. The vacuum rotary evaporation kettle for high-viscosity ionic liquid purification according to claim 1, wherein a steam jacket (11) is arranged on the outer side of the heating kettle body, a steam inlet (12) is connected to the upper part of the steam jacket, and a condensation water port (13) is connected to the bottom of the steam jacket.
6. The vacuum rotary evaporation kettle for purifying high-viscosity ionic liquid according to claim 1, wherein the motor shaft end part of the explosion-proof speed reduction motor and the lower end of the stirring shaft are respectively and fixedly connected with the upper end of the stirring shaft and the stirrer through shaft couplings.
7. The vacuum rotary evaporation kettle for high-viscosity ionic liquid purification according to claim 1 or 6, wherein the stirrer is an anchor stirrer.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202020803936.9U CN212548349U (en) | 2020-05-14 | 2020-05-14 | Vacuum rotary evaporation kettle for purifying high-viscosity ionic liquid |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202020803936.9U CN212548349U (en) | 2020-05-14 | 2020-05-14 | Vacuum rotary evaporation kettle for purifying high-viscosity ionic liquid |
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| Publication Number | Publication Date |
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| CN212548349U true CN212548349U (en) | 2021-02-19 |
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| CN202020803936.9U Active CN212548349U (en) | 2020-05-14 | 2020-05-14 | Vacuum rotary evaporation kettle for purifying high-viscosity ionic liquid |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114225458A (en) * | 2021-12-25 | 2022-03-25 | 东营威联化学有限公司 | Extractive distillation device for separating aromatic hydrocarbon |
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2020
- 2020-05-14 CN CN202020803936.9U patent/CN212548349U/en active Active
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114225458A (en) * | 2021-12-25 | 2022-03-25 | 东营威联化学有限公司 | Extractive distillation device for separating aromatic hydrocarbon |
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