CN212090957U - Continuous rectification device for thermosensitive substances - Google Patents
Continuous rectification device for thermosensitive substances Download PDFInfo
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- CN212090957U CN212090957U CN202020271874.1U CN202020271874U CN212090957U CN 212090957 U CN212090957 U CN 212090957U CN 202020271874 U CN202020271874 U CN 202020271874U CN 212090957 U CN212090957 U CN 212090957U
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- 239000000126 substance Substances 0.000 title claims abstract description 12
- 239000011552 falling film Substances 0.000 claims abstract description 5
- 239000000463 material Substances 0.000 claims description 13
- 238000012856 packing Methods 0.000 claims description 10
- 150000001875 compounds Chemical class 0.000 claims description 6
- 230000003014 reinforcing effect Effects 0.000 claims description 6
- 239000000047 product Substances 0.000 description 61
- 238000010992 reflux Methods 0.000 description 20
- 238000001704 evaporation Methods 0.000 description 17
- 230000008020 evaporation Effects 0.000 description 17
- 238000005292 vacuum distillation Methods 0.000 description 14
- 238000009835 boiling Methods 0.000 description 7
- 238000000605 extraction Methods 0.000 description 7
- 239000007788 liquid Substances 0.000 description 7
- 239000000945 filler Substances 0.000 description 3
- 239000000203 mixture Substances 0.000 description 3
- 238000007789 sealing Methods 0.000 description 3
- 239000012043 crude product Substances 0.000 description 2
- 230000014759 maintenance of location Effects 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 238000005979 thermal decomposition reaction Methods 0.000 description 2
- 206010057040 Temperature intolerance Diseases 0.000 description 1
- 238000000998 batch distillation Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000009833 condensation Methods 0.000 description 1
- 230000005494 condensation Effects 0.000 description 1
- 230000001627 detrimental effect Effects 0.000 description 1
- 238000007599 discharging Methods 0.000 description 1
- 238000004821 distillation Methods 0.000 description 1
- 230000002349 favourable effect Effects 0.000 description 1
- 239000012467 final product Substances 0.000 description 1
- 230000008543 heat sensitivity Effects 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 238000009776 industrial production Methods 0.000 description 1
- 230000010354 integration Effects 0.000 description 1
- 238000000034 method Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000000746 purification Methods 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 238000005728 strengthening Methods 0.000 description 1
- 238000009834 vaporization Methods 0.000 description 1
- 230000008016 vaporization Effects 0.000 description 1
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Abstract
The present application relates to a continuous rectification apparatus for heat-sensitive substances, comprising: a front fraction vacuum rectifying tower, a front fraction evaporator, a product vacuum rectifying tower and a product evaporator; arc pipes are respectively and integrally arranged on the two rectifying towers and are connected with the evaporator through the arc pipes; the front fraction evaporator and the product evaporator are both falling film evaporators; the inner diameter of the arc-shaped pipe is 800-1000 mm; the tower diameter of the front fraction vacuum rectifying tower is 800-1000 mm; the diameter of the product vacuum rectifying tower is 1200-1800 mm.
Description
Technical Field
The application relates to a continuous rectification device for heat-sensitive substances.
Background
In the past, the heat-sensitive substances are generally not rectified, but distilled by adopting a batch evaporation kettle, namely, a crude product is placed in the evaporation kettle, the temperature is gradually increased, the solvent, a front fraction, a finished product and a rear fraction are sequentially removed along with the increase of the temperature, and the crude product is condensed by a condenser and then received by a receiving tank. However, since no reflux exists in the intermittent evaporation, the whole device has low efficiency in the production process, and the purity of the obtained product is low, so that the quality requirement is difficult to achieve.
For example, the compound represented by the following formula (1) is an important chemical intermediate, has high heat sensitivity, has been isolated by simple batch evaporation, is not only low in efficiency but also low in purity of the obtained product, has a black color, and its use as an intermediate affects the quality of the final product.
Therefore, it is necessary to rectify such a highly heat-sensitive substance under high vacuum to improve its purity.
In the high vacuum distillation of heat-sensitive substances, vacuum leakage and pressure drop are required to be reduced as much as possible, because the vacuum leakage can cause the vacuum degree of a system to be reduced and the boiling point to be increased, so that the evaporation temperature is required to be increased. Too great a pressure drop will result in less vapor being available and will also result in an increase in vaporization temperature. This is detrimental to the heat sensitive material and also affects the stability of operation.
SUMMERY OF THE UTILITY MODEL
The application aims to provide a continuous rectification device suitable for thermosensitive substances, and aims to solve the problems that in the prior art, when an intermittent evaporation kettle is adopted, the production efficiency is low, and the quality of obtained products is low.
To achieve the above object, the present application provides a continuous rectification apparatus for a heat-sensitive substance, comprising: the front fraction vacuum rectifying tower, the front fraction evaporator, the product vacuum rectifying tower and the product evaporator are respectively and integrally provided with an arc-shaped pipe, the two rectifying towers are connected with the evaporator through the arc-shaped pipes, and the front fraction evaporator and the product evaporator are both falling film evaporators.
Preferably, the inner diameter of the arc-shaped pipe is 800-1000 mm.
More preferably, the diameter of the front-cut vacuum rectifying tower is 800-1000 mm.
More preferably, the diameter of the product vacuum rectifying tower is 1200-1800 mm.
Further preferably, the number of the arc-shaped pipes integrally arranged on the product vacuum rectifying tower is at least 2, and at least 2 product evaporators are connected in parallel on the product vacuum rectifying tower through the at least 2 arc-shaped pipes.
Further preferably, reinforcing plates are respectively arranged between the front fraction vacuum rectifying tower and the arc-shaped pipe and between the product vacuum rectifying tower and the arc-shaped pipe.
Still further preferably, a built-in condenser, preferably a U-tube condenser, is respectively provided in the front-cut vacuum distillation column and the product vacuum distillation column.
Still further preferably, the packing in the front-cut vacuum distillation column and the product vacuum distillation column is detachable regular block packing.
Still more preferably, the heat-sensitive substance is a compound represented by formula (1):
the continuous rectifying device effectively solves the problems of pressure drop, tightness, material residence time, evaporation efficiency and the like in high vacuum rectification, and is particularly suitable for thermosensitive materials.
In addition, the continuous rectification device comprises two rectification towers, and the two rectification towers are more favorable for improving the product quality.
Further, the continuous rectification device of the application has high efficiency, and particularly when at least 2 product evaporators are arranged, the capacity is greatly improved.
Drawings
FIG. 1 is a schematic structural view of a preferred embodiment of the continuous rectification apparatus of the present application.
Wherein, in the figures, the respective reference numerals:
1-front fraction vacuum rectifying tower, 11-front fraction condenser, 12-front fraction reflux extraction part, 121-front condensate collector, 122-front condensate reflux ratio controller, 123-front condensate reflux distributor, 13-front fraction tower kettle and 14-first filler;
2-front cut evaporator, 21-first arc pipe, 22-first reinforcing plate;
3-a product vacuum rectifying tower, 31-a product condenser, 32-a product reflux extraction part, 321-a product condensate collector, 322-a product reflux ratio controller, 323-a product reflux distributor, 33-a product tower kettle and 34-a second filler;
4-a product evaporator, 41-a second arc-shaped pipe, 42-a second reinforcing plate, 5-a front fraction tower kettle circulating pump and 6-a product tower kettle circulating pump.
Detailed Description
The structure of the continuous rectifying apparatus of the present application will be described in more detail with reference to the accompanying drawings, but the present application is not limited to the specific embodiments, and any modifications and variations may fall within the scope of the invention of the present application.
The continuous rectification device of the application comprises: a front cut vacuum rectifying tower 1, a front cut evaporator 2, a product vacuum rectifying tower 3 and a product evaporator 4.
In the existing industrial production, a rectifying tower and an evaporator are generally in separate structures which are independent from each other and are connected through a single pipe. In contrast, in the present application, the front end vacuum distillation column 1 is provided with a first arc tube 21, which is integrally provided, and is connected to the front end evaporator 2, and the product vacuum distillation column 3 is provided with a second arc tube 41, which is integrally provided, and is connected to the product evaporator 4. The integrated arrangement structure reduces the number of sealing surfaces, thereby improving the sealing performance of the system and reducing vacuum leakage.
The rectifying tower and the evaporator are connected through the arc-shaped pipe, so that the material flow is facilitated, and dead angles can not be formed.
Preferably, the pipe diameters of the first arc-shaped pipe 21 and the second arc-shaped pipe 41 are both enlarged to 800-1000 mm, which is far larger than the pipe diameters of about 200-300 mm in the conventional design. Such a large pipe diameter allows the evaporated material to enter the rectification column with almost no resistance, wherein the pressure drop is almost negligible.
Preferably, a first reinforcing plate 22 and a second reinforcing plate 42 are respectively arranged between the front fraction vacuum distillation tower 1 and the first arc-shaped pipe 21 and between the product vacuum distillation tower 3 and the second arc-shaped pipe 41 to play a role of fixing.
Both the front fraction evaporator 2 and the product evaporator 4 use falling film evaporators to enhance the evaporation process, thereby reducing the evaporation temperature, improving the evaporation speed and reducing the resistance of vapor coming out. The falling film evaporator may be any known one, and is not particularly limited.
The front fraction vacuum rectifying tower 1 is provided with a front fraction condenser 11, a front fraction reflux extraction part 12, a first filler 14 and a front fraction tower kettle 13 in sequence from top to bottom. Similarly, the product vacuum rectification column 3 is provided with a product condenser 31, a product reflux extraction part 32, a second packing 34 and a product column bottom 33 in this order from top to bottom.
The front cut vacuum distillation tower 1 and the product vacuum distillation tower 3 are preferably provided with a built-in front cut condenser 11 and a built-in product condenser 31, respectively. The built-in integrated structure is beneficial to reducing the sealing surface, and further reducing the vacuum leakage.
The front-cut condenser 11 and the product condenser 31 preferably use U-tube type condensers in view of reducing the pressure drop during condensation.
The front cut reflux extractor 12 includes a front condensate collector 121, a front condensate reflux ratio controller 122, and a front condensate reflux distributor 123. Likewise, the product reflux collection section 32 includes a product condensate collector 321, a product reflux ratio controller 322, and a product reflux distributor 323. The two reflux ratio controllers are both arranged outside the rectifying tower. These are all conventional arrangements.
The first packing 14 and the second packing 34 are preferably removable structured packing having a relatively low resistance to reduce pressure drop.
The two rectifying towers are respectively provided with a front fraction tower kettle 13 and a product tower kettle 33, gas-liquid mixtures coming out of the front fraction evaporator 2 and the product evaporator 4 respectively enter the front fraction tower kettle 13 and the product tower kettle 33, low-boiling components rise to a contact condenser at the upper part of the rectifying tower in a gas form to be condensed, and are partially extracted and partially refluxed through a reflux ratio controller, high-boiling components are remained in the two tower kettles in a liquid form and are respectively circulated through a front fraction tower kettle circulating pump 5 and a product tower kettle circulating pump 6.
The liquid levels in the two rectifying tower kettles can be controlled by controlling the feeding amount and the discharging amount, so that the residence time of liquid in the kettles is controlled to be 0.5-1 hour, and the residence time of materials in the batch kettles in the conventional batch distillation is 4-6 hours. Therefore, the continuous rectifying device can greatly shorten the retention time of the thermosensitive material in the high-temperature environment and reduce the thermal decomposition of the thermosensitive material.
In a preferred embodiment, the diameter of the front-cut vacuum distillation column 1 is increased to 800 to 1000mm, and the diameter of the product vacuum distillation column 4 is increased to 1200 to 1800mm, whereas the diameter of a conventional distillation column is generally about 600 mm. By enlarging the column diameter, the column height and the packing height of the packing are reduced, which contributes to reducing the pressure drop.
Because the quantity of product is great than the volume of preceding fraction, consequently the arc pipe that the integration set up on the preferred product vacuum distillation column 4 is at least 2, through these at least 2 arc pipes parallel connection at least 2 product evaporators, the parallel operation of a plurality of product evaporators has improved efficiency and productivity greatly.
Other conventional components required in the rectifying apparatus, such as a vacuum pump (not shown) and the like, may be of any known conventional structure and arrangement, without particular limitation.
Examples
The compound of formula (1) is rectified using a continuous rectification apparatus as described herein above.
The material to be rectified is introduced into the front cut vacuum rectifying tower 1 from a feed inlet (not shown) arranged slightly below the front cut reflux extraction part 12, and then is pumped into the front cut evaporator 2 from the top by the front cut tower kettle circulating pump 5, and the mixture of the evaporation gas and the liquid from the front cut evaporator 2 enters the front cut tower kettle 13 from the bottom of the evaporator through the first arc-shaped pipe 21. The evaporated gas from low-boiling impurities in the material rises to the upper part of the front fraction vacuum rectifying tower 1 and is condensed by a front fraction condenser 11, and the condensate is partially extracted and partially refluxed from a front fraction reflux extraction part 12. On the other hand, the high-boiling components of the feed remain in liquid form in the front cut column 13, a portion of which is pumped again from the top by the column circulation pump 5 into the front cut evaporator 2 for internal circulation, and another portion is pumped from the top into the product evaporator 4. The mixture of the evaporation gas and the liquid from the product evaporator 4 enters the product tower kettle 33 from the bottom of the evaporator through the second arc-shaped pipe 42, the evaporation gas of the target product rises to the upper part of the product vacuum rectifying tower 3 and is condensed by the product condenser 31, and the condensate is partially extracted and partially refluxed from the product reflux extraction part 32. The high boiling kettle residue is withdrawn from the product column kettle 33.
In the rectification device, the pressure drop of the whole system is below 50Pa, and sometimes even below 20Pa, while the pressure drop of the conventional rectification device system is generally above 100 Pa.
The vacuum degree of the rectifying apparatus is very good, and the absolute pressure is 100Pa or less, whereas the conventional rectifying apparatus is about 500 Pa.
The boiling point of the compound of formula (1) in batch evaporation is about 190 ℃ and in the above-mentioned rectification apparatus is reduced to about 160 ℃. Thus lowering the evaporation temperature and reducing its thermal decomposition. The purity of the compound of the formula (1) obtained after rectification in the device reaches more than 98 percent, and the color is light yellow. And the purity of the product obtained after the batch still evaporation and purification is below 95 percent, and the color is brown yellow.
In the rectifying apparatus used in this embodiment, two product evaporators 4 are provided, and the annual capacity reaches about 6000 tons.
Industrial applicability
The continuous rectifying device effectively solves the problems of pressure drop, tightness, material retention time, evaporation efficiency and the like in high vacuum rectification through various structural strengthening measures, can be used for rectifying thermosensitive materials which cannot be processed by the conventional rectifying device in the past, and has great industrial value.
Claims (7)
1. The continuous rectification device of heat-sensitive material, characterized by including: a front fraction vacuum rectifying tower, a front fraction evaporator, a product vacuum rectifying tower and a product evaporator;
arc pipes are respectively and integrally arranged on the two rectifying towers and are connected with the evaporator through the arc pipes;
the front fraction evaporator and the product evaporator are both falling film evaporators;
the inner diameter of the arc-shaped pipe is 800-1000 mm;
the tower diameter of the front fraction vacuum rectifying tower is 800-1000 mm;
the diameter of the product vacuum rectifying tower is 1200-1800 mm.
2. The continuous rectification apparatus as claimed in claim 1, wherein the number of the arc pipes integrally arranged on the product vacuum rectification column is at least 2, and at least 2 product evaporators are connected in parallel on the product vacuum rectification column through the at least 2 arc pipes.
3. The continuous rectifying device according to claim 1 or 2, wherein the packing in the front-cut vacuum rectifying tower and the product vacuum rectifying tower is detachable regular block packing.
4. The continuous rectifying apparatus according to claim 1 or 2, wherein reinforcing plates are respectively arranged between the front fraction vacuum rectifying tower and the arc-shaped pipe and between the product vacuum rectifying tower and the arc-shaped pipe.
5. The continuous rectifying apparatus according to claim 1 or 2, wherein the front-cut vacuum rectifying tower and the product vacuum rectifying tower are respectively provided with a built-in condenser.
6. The continuous rectification plant as claimed in claim 5 wherein the condenser is a U-tube condenser.
7. Continuous rectification apparatus according to claim 1 or 2, characterized in that the heat-sensitive substance is a compound of formula (1) below:
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202020271874.1U CN212090957U (en) | 2020-03-09 | 2020-03-09 | Continuous rectification device for thermosensitive substances |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202020271874.1U CN212090957U (en) | 2020-03-09 | 2020-03-09 | Continuous rectification device for thermosensitive substances |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN212090957U true CN212090957U (en) | 2020-12-08 |
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Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202020271874.1U Active CN212090957U (en) | 2020-03-09 | 2020-03-09 | Continuous rectification device for thermosensitive substances |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN212090957U (en) |
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2020
- 2020-03-09 CN CN202020271874.1U patent/CN212090957U/en active Active
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Address after: 750300 north area of Tengger economic and Technological Development Zone, Alxa League, Inner Mongolia Autonomous Region Patentee after: Inner Mongolia Lange Biotechnology Co.,Ltd. Patentee after: Lansheng Biotechnology Group Co.,Ltd. Address before: 750300 north area of Tengger economic and Technological Development Zone, Alxa League, Inner Mongolia Autonomous Region Patentee before: Inner Mongolia Lange Biotechnology Co.,Ltd. Patentee before: HEBEI LANSHENG BIOTECH Co.,Ltd. |