CN220835598U - Alpha-P continuous purification device - Google Patents
Alpha-P continuous purification device Download PDFInfo
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- CN220835598U CN220835598U CN202322687351.1U CN202322687351U CN220835598U CN 220835598 U CN220835598 U CN 220835598U CN 202322687351 U CN202322687351 U CN 202322687351U CN 220835598 U CN220835598 U CN 220835598U
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- tower
- alpha
- reactor
- deamination
- recovery
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- 238000000746 purification Methods 0.000 title claims abstract description 17
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 claims abstract description 28
- 230000009615 deamination Effects 0.000 claims abstract description 28
- 238000006481 deamination reaction Methods 0.000 claims abstract description 28
- 238000000926 separation method Methods 0.000 claims abstract description 26
- 238000011084 recovery Methods 0.000 claims abstract description 23
- 230000018044 dehydration Effects 0.000 claims abstract description 17
- 238000006297 dehydration reaction Methods 0.000 claims abstract description 17
- 238000010992 reflux Methods 0.000 claims abstract description 10
- 239000007791 liquid phase Substances 0.000 claims abstract description 5
- 238000002156 mixing Methods 0.000 claims description 21
- 229910001220 stainless steel Inorganic materials 0.000 claims description 3
- 239000010935 stainless steel Substances 0.000 claims description 3
- 239000007789 gas Substances 0.000 claims 3
- 230000008676 import Effects 0.000 claims 2
- 238000005201 scrubbing Methods 0.000 claims 2
- 239000007792 gaseous phase Substances 0.000 claims 1
- HNJBEVLQSNELDL-UHFFFAOYSA-N pyrrolidin-2-one Chemical compound O=C1CCCN1 HNJBEVLQSNELDL-UHFFFAOYSA-N 0.000 abstract description 21
- 238000005406 washing Methods 0.000 abstract description 9
- 239000012071 phase Substances 0.000 abstract description 7
- YEJRWHAVMIAJKC-UHFFFAOYSA-N 4-Butyrolactone Chemical compound O=C1CCCO1 YEJRWHAVMIAJKC-UHFFFAOYSA-N 0.000 description 10
- 239000000463 material Substances 0.000 description 10
- 239000002351 wastewater Substances 0.000 description 9
- 238000006243 chemical reaction Methods 0.000 description 7
- 239000012043 crude product Substances 0.000 description 7
- 239000007788 liquid Substances 0.000 description 7
- 239000000047 product Substances 0.000 description 7
- 238000005265 energy consumption Methods 0.000 description 6
- 238000000034 method Methods 0.000 description 5
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 description 4
- 229910021529 ammonia Inorganic materials 0.000 description 4
- 235000011114 ammonium hydroxide Nutrition 0.000 description 4
- 229930188620 butyrolactone Natural products 0.000 description 3
- 239000007795 chemical reaction product Substances 0.000 description 3
- 238000010586 diagram Methods 0.000 description 3
- 238000012432 intermediate storage Methods 0.000 description 3
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 3
- 238000010521 absorption reaction Methods 0.000 description 2
- 238000010924 continuous production Methods 0.000 description 2
- 230000007423 decrease Effects 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 206010008190 Cerebrovascular accident Diseases 0.000 description 1
- WHNWPMSKXPGLAX-UHFFFAOYSA-N N-Vinyl-2-pyrrolidone Chemical compound C=CN1CCCC1=O WHNWPMSKXPGLAX-UHFFFAOYSA-N 0.000 description 1
- 229920001007 Nylon 4 Polymers 0.000 description 1
- 208000006011 Stroke Diseases 0.000 description 1
- 239000002473 artificial blood Substances 0.000 description 1
- 230000000903 blocking effect Effects 0.000 description 1
- 230000002490 cerebral effect Effects 0.000 description 1
- 239000013064 chemical raw material Substances 0.000 description 1
- 239000002537 cosmetic Substances 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 239000000975 dye Substances 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 239000003973 paint Substances 0.000 description 1
- 210000002381 plasma Anatomy 0.000 description 1
- 235000013855 polyvinylpyrrolidone Nutrition 0.000 description 1
- 229920000036 polyvinylpyrrolidone Polymers 0.000 description 1
- 239000001267 polyvinylpyrrolidone Substances 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 239000010865 sewage Substances 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- 239000004753 textile Substances 0.000 description 1
Abstract
The utility model relates to the technical field of continuous purification of pyrrolidone, and discloses an alpha-P continuous purification device which comprises a deamination tower, a liquid ammonia separation tower, a tail gas washing tower, a delivery pump, a dehydration tower, an alpha-P rectifying tower, a recovery tower and a connecting pipeline, wherein the deamination tower is connected with an alpha-P reactor through the connecting pipeline, a gas phase outlet at the upper part of the deamination tower is connected with the liquid ammonia separation tower, a liquid phase outlet at the bottom of the deamination tower is connected with an inlet of the dehydration tower, the top of the liquid ammonia separation tower is connected with the tail gas washing tower, the upper part of the dehydration tower is connected with the deamination tower, a bottom discharge hole is connected with an inlet of the alpha-P rectifying tower, a bottom of the alpha-P rectifying tower is connected with a feed inlet of the recovery tower, a reflux pipe is arranged at the bottom of the recovery tower and connected with the alpha-P reactor through the reflux pipe, a product output pipe is arranged at the side wall of the alpha-P rectifying tower, and a coil-shaped reactor is arranged inside the alpha-P reactor.
Description
Technical Field
The utility model relates to the technical field of continuous purification of pyrrolidone, in particular to an alpha-P continuous purification device.
Background
Alpha-pyrrolidone (alpha-P) is an important chemical raw material and is widely applied to industries such as medicine, textile, dye, paint, cosmetics and the like, for example, cerebral apoplexy, nylon 4, polyvinylpyrrolidone, artificial blood plasma and the like. Can also be used for organic synthesis (such as 1-vinyl-2-pyrrolidone, etc.), and used as solvent, etc.
CN113548995A discloses a continuous purifying device for α -P pyrrolidone and a preparation method for α -pyrrolidone, wherein γ -butyrolactone and ammonia water react in a tubular fixed bed reactor to obtain a reaction product, the reaction product enters an intermediate storage tank to release surplus ammonia, the collected surplus ammonia returns to the reaction system again, and the crude product of the intermediate storage tank is separated and purified by a three-stage continuous tower to obtain the product. The method is used for deamination in the intermediate storage tank, and can not thoroughly separate out the surplus ammonia in the crude product, and part of ammonia and wastewater still exist in the crude product and enter the subsequent rectifying section along with the crude product, so that the load of the subsequent rectifying tower is higher, the equipment investment is high, and the energy consumption is higher.
CN204589038U discloses a method for continuously preparing α -P pyrrolidone by using α -P pyrrolidone continuous purifying device, in which γ -butyrolactone is used for excessive operation, because the amount of waste water generated in α -pyrrolidone reaction is relatively large, and the waste water enters into a separation tower together under the condition of excessive butyrolactone and is distilled out from the top of the tower, the phenomenon of flooding of the separation tower is likely to be caused, the equipment investment of the separation tower is high, the energy consumption is relatively high, and the method is not an ideal α -pyrrolidone purifying device.
Disclosure of utility model
The utility model aims to provide an alpha-P continuous purification device, which solves the problems that the waste water amount generated in the alpha-pyrrolidone reaction is relatively large, and the waste water enters a separation tower to be distilled out from the top of the tower under the condition of excessive butyrolactone, so that the phenomenon of flooding of the separation tower is likely to be caused, the equipment investment of the separation tower is large, and the energy consumption is relatively high.
In a first aspect, the utility model provides an α -P continuous purification device, comprising a deamination tower, a liquid ammonia separation tower, a tail gas washing tower, a delivery pump, a dehydration tower, an α -P rectification tower, a recovery tower and a connecting pipeline, wherein the deamination tower is connected with an α -P reactor through the connecting pipeline, a gas phase outlet at the upper part of the deamination tower is connected with the liquid ammonia separation tower, a liquid phase outlet at the bottom of the deamination tower is connected with an inlet of the dehydration tower, the top of the liquid ammonia separation tower is connected with the tail gas washing tower, the upper part of the dehydration tower is connected with the deamination tower, a bottom discharge hole is connected with an inlet of the α -P rectification tower, a bottom outlet of the α -P rectification tower is connected with a feed inlet of the recovery tower, the top of the recovery tower is connected with the delivery pump, the delivery pump is provided with a reflux pipe and is connected with the α -P reactor through the reflux pipe, and a product output pipe is arranged on the side wall of the α -P rectification tower.
In a specific embodiment, the α -P reactor is internally a coil-shaped reactor.
In a specific embodiment, the deamination column and the liquid ammonia separation column are both packed columns.
In a specific embodiment, the dehydration column, the alpha-P rectification column, and the recovery column are all corrugated stainless steel packed columns.
In a specific embodiment, the tail gas scrubber is a three stage scrubber.
In a specific embodiment, a top cover is embedded at the top end of the alpha-P reactor, and mutually staggered drainage plates are fixed at two sides of the inner wall of the alpha-P reactor.
In a specific embodiment, two similar ends of the drainage plates are arc-shaped structures, and inclined grooves are formed in two sides of the top end faces of the two drainage plates.
In a specific embodiment, a mixing tube is fixed to the top end of the side wall of the alpha-P reactor, and a conveying tube is installed on the mixing tube.
In a specific embodiment, a tee is fixed on the side wall of the conveying pipe, a feed pipe is installed at one end of the tee, and the other end of the tee is fixedly connected with the return pipe.
In a specific embodiment, the mixing tube is funnel-shaped, a baffle is fixed on the side wall of the mixing tube, and a discharge chute is formed in the bottom end of the side wall of the baffle in an annular array.
According to the alpha-P continuous purification device provided by the utility model, the recycled alpha-P pyrrolidone is subjected to mixing purification processing again through the conveying pump, the process flow is reasonable, continuous production can be performed, the purity of the product alpha-pyrrolidone is improved, the operation energy consumption is low, and the heavy component materials are fully utilized.
Through being fixed with mixing tube and conveyer pipe at the lateral wall of alpha-P reactor, the internal diameter of mixing tube is greater than the conveyer pipe far away, and the lateral wall of mixing tube is fixed with the baffle, the baffle separates liquid, when entering into the direct current passageway because its flow area is less, consequently the velocity of flow is faster, form the torrent easily, when entering into the expansion passageway, its velocity of flow reduces suddenly, follow-up material strikes, thereby make the more even of material mixing, simultaneously be fixed with the drainage board of mutual crisscross at the inner wall of alpha-P reactor, because the cross-section of drainage board is convex, consequently the material can form the vortex in the drainage board voluntarily, make two kinds of materials can mix the reaction in a plurality of directions.
Drawings
In order to more clearly illustrate the technical solutions of the embodiments of the present utility model, the drawings that are needed in the embodiments will be briefly described below, it being understood that the following drawings only illustrate some examples of the present utility model and therefore should not be considered as limiting the scope, and other related drawings may be obtained according to these drawings without inventive effort for a person skilled in the art.
Fig. 1 is a schematic structural diagram of an embodiment of the present utility model.
FIG. 2 is a schematic diagram of the internal structure of an α -P reaction chamber according to an embodiment of the present utility model.
Fig. 3 is a schematic view of a tee structure according to an embodiment of the utility model.
Fig. 4 is a schematic diagram of a drainage plate according to an embodiment of the present utility model.
Icon: 1. an alpha-P reactor; 2. a liquid ammonia separation column; 3. an ammonia water recovery pipe; 4. a tail gas scrubber; 5. a transfer pump; 6. a return pipe; 7. a recovery tower; 8. a product output pipe; 9. an alpha-P rectifying tower; 10. a dehydration tower; 11. a connecting pipe; 12. a deamination tower; 13. a tee joint; 14. a drainage plate; 15. a top cover; 16. a feed pipe; 17. a delivery tube; 18. a mixing tube; 19. a discharge chute; 20. a baffle; 21. and an inclined groove.
Detailed Description
Because the waste water amount generated in the reaction of the alpha-pyrrolidone in the prior art is relatively large, and the waste water enters the separation tower together under the condition of excessive butyrolactone and is distilled out from the top of the separation tower, the phenomenon of the separation tower flooding is likely to be caused, the equipment investment of the separation tower is large, the energy consumption is relatively high, and the purification device of the alpha-pyrrolidone is not ideal. Accordingly, the inventors have studied to provide an apparatus for continuous purification of α -P to solve the above-mentioned drawbacks.
Some embodiments of the present utility model are described in detail below with reference to the accompanying drawings. The following embodiments and features of the embodiments may be combined with each other without conflict.
Referring to fig. 1 to 4, an α -P continuous purifying apparatus is provided in an embodiment of the present utility model, which includes a deamination tower 12, a liquid ammonia separation tower 2, a tail gas washing tower 4, a transfer pump 5, a dehydration tower 10, an α -P rectifying tower 9, a recovery tower 7 and a connecting pipe 11, wherein the deamination tower 12 is connected with an α -P reactor 1 through the connecting pipe 11, a gas phase outlet at the upper portion of the deamination tower 12 is connected with the liquid ammonia separation tower 2, a liquid phase outlet at the bottom of the deamination tower 12 is connected with an inlet of the dehydration tower 10, a top of the liquid ammonia separation tower 2 is connected with the tail gas washing tower 4, an upper portion of the dehydration tower 10 is connected with the deamination tower 12, a bottom outlet is connected with an inlet of the recovery tower 7, a top of the recovery tower 7 adopts total reflux, a bottom of the recovery tower 7 is connected with the transfer pump 5, a reflux pipe 6 is installed at the outlet of the transfer pump 5 and is connected with the α -P reactor 1 through the reflux pipe 6, a product output pipe 8 is installed at a side wall of the α -P rectifying tower 9, ammonia water is treated by a reflux pipe 3 fixed at the bottom of the liquid ammonia separation tower 2 through the reflux pipe 3.
The inside of the alpha-P reactor 1 is a coil-shaped reactor, the deamination tower 12 and the liquid ammonia separation tower 2 are both filled towers, the dehydration tower 10, the alpha-P rectifying tower 9 and the recovery tower 7 are stainless steel corrugated filled towers, the tail gas washing tower 4 is a three-stage washing tower, the conveying pump 5 carries out mixing and purifying processing again on the recovered alpha-P pyrrolidone, the process flow is reasonable, continuous production can be carried out, the purity of the product alpha-pyrrolidone is improved, the operation energy consumption is low, and the heavy component materials are fully utilized.
Top cover 15 is embedded to be installed on the top of alpha-P reactor 1, and the inner wall both sides of alpha-P reactor 1 are fixed with crisscross drainage board 14 each other, and the one end that two drainage boards 14 are close all is the arc structure, and the top face both sides of two drainage boards 14 have all been seted up inclined groove 21, and inclined groove 21 makes the liquid on the drainage board 14 flow down, has avoided the liquid at drainage board 14 top to pile up.
The mixing tube 18 is fixed on the top end of the side wall of the alpha-P reactor 1, the conveying tube 17 is installed on the mixing tube 18, the tee joint 13 is fixed on the side wall of the conveying tube 17, the feed pipe 16 is installed at one end of the tee joint 13, the other end of the tee joint 13 is fixedly connected with the return pipe 6, the mixing tube 18 is funnel-shaped, the baffle 20 is fixed on the side wall of the mixing tube 18, the discharge groove 19 is formed in an annular array at the bottom end of the side wall of the baffle 20, as the inner diameter of the mixing tube 18 is far larger than that of the conveying tube 17, the baffle 20 is fixed on the side wall of the mixing tube 18, the baffle 20 is used for blocking liquid, when the liquid enters into the direct-flow channel, the flow velocity is relatively fast due to the small flow area, turbulence is easy to form, when the liquid velocity suddenly decreases when the liquid enters into the expansion channel, the flow velocity suddenly decreases, the subsequent materials are impacted, so that the materials are mixed more uniformly, meanwhile, the flow guide plate 14 is fixed on the inner wall of the alpha-P reactor 1, and the two materials can automatically form vortex in the flow guide plate 14 due to the circular cross section of the flow guide plate 14.
In summary, the reaction product from the alpha-PP reactor and the recovery material from the recovery tower 7 enter the deamination tower 12 together, and the gas phase is reaction tail gas (main components of ammonia gas and water vapor) and the liquid phase is crude product of alpha-P pyrrolidone; the crude product of alpha-P pyrrolidone is dehydrated in a dehydration tower 10, the water phase is extracted from the upper part and then returns to a deamination tower 12, and the crude product of alpha-P pyrrolidone is extracted from the bottom part; purifying in an alpha-PP rectifying tower to obtain alpha-P pyrrolidone product with purity over 99%; the heavy component at the bottom of the tower enters a recovery tower 7 for recovery, and the alpha-P pyrrolidone in the heavy component is fully recovered; the gas phase of the deamination tower 12 enters a liquid ammonia separation tower 2 for liquid ammonia separation, the water content of the wastewater at the bottom of the tower is more than 99 percent, the wastewater is discharged to a sewage station, the gas phase enters a tail gas washing tower 4 for safe emptying after three-stage absorption, and 10 percent of ammonia water obtained at the bottom of the absorption tower can be sold.
The above is only a preferred embodiment of the present utility model, and is not intended to limit the present utility model, but various modifications and variations can be made to the present utility model by those skilled in the art. Any modification, equivalent replacement, improvement, etc. made within the spirit and principle of the present utility model should be included in the protection scope of the present utility model.
Claims (10)
1. The utility model provides an alpha-P continuous purification device, includes deamination tower, liquid ammonia separating tower, tail gas scrubbing tower, delivery pump, dehydration tower, alpha-P rectifying tower, recovery tower and connecting tube, its characterized in that, the deamination tower is connected with alpha-P reactor through connecting tube, and deamination tower upper portion gaseous phase export links to each other with liquid ammonia separating tower, and deamination tower bottom liquid phase export links to each other with the dehydration tower import, liquid ammonia separating tower top links to each other with the tail gas scrubbing tower, and dehydration tower upper portion links to each other with deamination tower, and bottom discharge gate links to each other with alpha-P rectifying tower import, and alpha-P rectifying tower bottom export links to each other with the recovery tower feed inlet, and the recovery tower top adopts total reflux, and the recovery tower bottom links to each other with the delivery pump, and the delivery pump export is installed to return pipe and is linked to alpha-P reactor through the back flow, the product output tube is installed to the lateral wall of alpha-P rectifying tower.
2. An α -P continuous purification apparatus according to claim 1 wherein the α -P reactor is internally a coil-shaped reactor.
3. The apparatus according to claim 2, wherein the deamination column and the liquid ammonia separation column are packed columns.
4. An α -P continuous purification apparatus according to claim 3, wherein the dehydration column, α -P rectification column and recovery column are all stainless steel corrugated packed columns.
5. The α -P continuous purification apparatus of claim 4, wherein the tail gas scrubber is a three stage scrubber.
6. The alpha-P continuous purifying device according to claim 1, wherein a top cover is embedded in the top end of the alpha-P reactor, and two sides of the inner wall of the alpha-P reactor are fixed with mutually staggered drainage plates.
7. The α -P continuous purification apparatus of claim 6 wherein the two flow plates are each arcuate at one end and have inclined slots on opposite sides of their top surfaces.
8. The apparatus according to claim 6, wherein a mixing tube is fixed to the top end of the side wall of the α -P reactor, and a delivery tube is installed on the mixing tube.
9. The apparatus according to claim 8, wherein a tee is fixed to a side wall of the delivery pipe, a feed pipe is installed at one end of the tee, and the other end of the tee is fixedly connected to the return pipe.
10. The alpha-P continuous purifying apparatus according to claim 9, wherein the mixing tube is funnel-shaped, a baffle is fixed on the side wall of the mixing tube, and discharge grooves are formed in the bottom end of the side wall of the baffle in an annular array.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202322687351.1U CN220835598U (en) | 2023-10-08 | 2023-10-08 | Alpha-P continuous purification device |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202322687351.1U CN220835598U (en) | 2023-10-08 | 2023-10-08 | Alpha-P continuous purification device |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN220835598U true CN220835598U (en) | 2024-04-26 |
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Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202322687351.1U Active CN220835598U (en) | 2023-10-08 | 2023-10-08 | Alpha-P continuous purification device |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN220835598U (en) |
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2023
- 2023-10-08 CN CN202322687351.1U patent/CN220835598U/en active Active
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