CN214971873U - Ortho-aminophenol continuous crystallization device - Google Patents
Ortho-aminophenol continuous crystallization device Download PDFInfo
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- CN214971873U CN214971873U CN202120268842.0U CN202120268842U CN214971873U CN 214971873 U CN214971873 U CN 214971873U CN 202120268842 U CN202120268842 U CN 202120268842U CN 214971873 U CN214971873 U CN 214971873U
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Abstract
The utility model provides an ortho-aminophenol continuous crystallization device, belong to ortho-aminophenol production technology field, including the reaction unit who establishes ties in proper order, one-level crystallization kettle, second grade crystallization kettle and centrifugal subassembly, reaction unit provides the reaction site of o-nitrophenol and hydrogen, be provided with circulating water pipe spare among the one-level crystallization kettle, circulating water among the circulating water pipe spare is used for carrying out the heat transfer to the solution among the one-level crystallization kettle, be provided with freezing water pipe spare among the second grade crystallization kettle, freezing water among the freezing water pipe spare is used for carrying out the crystallization to the solution among the second grade crystallization kettle, circulating water among the circulating water pipe spare with there is the difference in temperature between the freezing water in the freezing water pipe spare between the two, centrifugal subassembly is used for carrying out solid-liquid separation to the solid-liquid mixture after the crystallization. Through the continuous heat exchange and the crystallization process of the first-stage crystallization kettle and the second-stage crystallization kettle, materials can be prevented from being adhered to the wall of the crystallization kettle, and meanwhile, the crystallization time of the solution is greatly shortened, so that the operation efficiency of the equipment is improved.
Description
Technical Field
The utility model belongs to ortho-aminophenol production technology field, concretely relates to ortho-aminophenol continuous crystallization device.
Background
Reacting o-nitrophenol with hydrogen in a hydrogenation reaction kettle under the catalytic action of Raney nickel to generate o-aminophenol, filtering the o-aminophenol out of a catalyst by a two-stage catalyst filter, then feeding the o-aminophenol into a jacket crystallization kettle, and cooling and crystallizing by using chilled water. But there is the material crystallization time long, causes production efficiency to hang down, and simultaneously, the heat transfer difference in the crystallization kettle is big, and the material can the adhesion at the crystallization kettle wall, needs to clear up the material of cauldron wall, is unfavorable for clean production.
SUMMERY OF THE UTILITY MODEL
In view of this, to above not enough, the utility model provides an ortho-aminophenol continuous crystallization device has shortened the crystallization time of material, has improved production efficiency, has avoided the material adhesion at the crystallizer wall simultaneously, is favorable to cleaning production.
The utility model provides an ortho-aminophenol continuous crystallization device is including the reaction unit, one-level crystallization kettle, second grade crystallization kettle and the centrifugal subassembly that establish ties in proper order, the reaction unit provides the reaction site of o-nitrophenol and hydrogen, be provided with circulating water pipe fitting on the one-level crystallization kettle, circulating water that flows in the circulating water pipe fitting is used for right solution among the one-level crystallization kettle carries out the heat transfer, be provided with freezing water pipe fitting on the second grade crystallization kettle, the freezing liquid that flows in the freezing water pipe fitting is used for right solution among the second grade crystallization kettle carries out the crystallization, circulating water among the circulating water pipe fitting with there is the difference in temperature between the freezing water in the freezing water pipe fitting between the two, centrifugal subassembly is used for carrying out solid-liquid separation to the solid-liquid mixture after the crystallization.
Preferably, the liquid inlet temperature of the liquid inlet of the primary crystallization kettle is 60 +/-3 ℃, the temperature of the circulating water is 25 +/-3 ℃, and the material is cooled to 30 +/-3 ℃ after heat exchange for a certain time and is pressed into the secondary crystallization kettle.
Preferably, the liquid inlet temperature of the liquid inlet of the secondary crystallization kettle is 30 +/-3 ℃, the primary crystallization kettle is cooled by using chilled water, the temperature of the chilled water is-10 +/-2 ℃, and the temperature of the material is cooled to 5 +/-2 ℃ after heat exchange for a certain time, so that a solid-liquid mixture is formed.
Preferably, the ortho-aminophenol continuous crystallization device further comprises a third-stage crystallization kettle, wherein a liquid inlet at one end of the third-stage crystallization kettle is connected with the second-stage crystallization kettle, the other end of the third-stage crystallization kettle is connected with the centrifugal component, and the third-stage crystallization kettle is used for standing and caching a solid-liquid mixture.
Preferably, the reaction assembly is provided with a plurality of pairs, the reaction assemblies are arranged in parallel, and a liquid outlet of the reaction assembly is connected with a liquid inlet of the first-stage crystallization kettle.
Preferably, the reaction assembly comprises a hydrogenation reaction kettle and a secondary filter which are sequentially connected in series, the hydrogenation reaction kettle provides a reaction site for the o-nitrophenol and the hydrogen, a catalyst is also present in the hydrogenation reaction kettle, and the secondary filter is used for filtering the catalyst.
Preferably, the centrifugal assembly comprises a centrifuge, a dryer and a mother liquor tank, the centrifuge is used for separating solid-liquid mixture, the solid separated by the centrifuge is conveyed to the dryer for drying, and the liquid separated by the centrifuge is conveyed to the mother liquor tank for storage.
According to the technical scheme, the utility model provides an ortho-aminophenol continuous crystallization device, its beneficial effect lies in, including reaction unit, one-level crystallization kettle, second grade crystallization kettle and the centrifugal subassembly of establishing ties in proper order, reaction unit is used for the reaction site of ortho-nitrophenol and hydrogen, be provided with circulating water pipe spare among the one-level crystallization kettle, it is right to be used for one-level crystallization kettle carries out the heat transfer, be provided with freezing water pipe spare among the second grade crystallization kettle, it is right to be used for the second grade crystallization kettle carries out the crystallization, circulating water among the circulating water pipe spare with there is the difference in temperature between the two freezing water among the freezing water pipe spare, centrifugal subassembly is used for carrying out solid-liquid separation to the solid-liquid mixture after the crystallization. Through the continuous heat transfer and the crystallization process of one-level crystallization cauldron and second grade crystallization cauldron, because the heat transfer difference in temperature of one-level crystallization cauldron and second grade crystallization cauldron is less, can avoid the crystallization kettle wall bonding material, and the heat transfer difference in temperature can be adjusted, has improved crystallization cauldron to solution cooling rate, and solution crystallization time also shortens by a wide margin simultaneously to the operating efficiency of equipment has been improved.
Drawings
FIG. 1 is a flow chart of an ortho-aminophenol continuous crystallization apparatus.
In the figure: the system comprises a reaction component 100, a hydrogenation reaction kettle 110, a secondary filter 120, a primary crystallization kettle 200, a circulating water pipe fitting 210, a secondary crystallization kettle 300, a chilled water pipe fitting 310, a tertiary crystallization kettle 400, a centrifugal component 500, a centrifuge 510, a dryer 520 and a mother liquor tank 530.
Detailed Description
The following combines the drawings of the utility model to further elaborate the technical scheme and technical effect of the utility model.
Referring to fig. 1, an ortho-aminophenol continuous crystallization device comprises a reaction assembly 100, a first-stage crystallization kettle 200, a second-stage crystallization kettle 300 and a centrifugal assembly 500 which are sequentially connected in series, wherein the reaction assembly 100 is used in a reaction site of ortho-nitrophenol and hydrogen, a circulating water pipe 210 is arranged in the first-stage crystallization kettle 200 and used for exchanging heat with the first-stage crystallization kettle 200, a chilled water pipe 310 is arranged in the second-stage crystallization kettle 300 and used for crystallizing the second-stage crystallization kettle 300, a temperature difference exists between circulating water in the circulating water pipe 210 and chilled water in the chilled water pipe 310, and the centrifugal assembly 500 is used for performing solid-liquid separation on a solid-liquid mixture after crystallization.
Specifically, o-nitrophenol reacts with hydrogen in the reaction assembly 100 under the action of a catalyst to generate an o-aminophenol solution, the generated o-aminophenol solution is introduced into the primary crystallization kettle 200 and then introduced into the secondary crystallization kettle 300, so that continuous heat exchange and crystallization of the solution are realized, a certain temperature difference exists between the heat exchange liquid of the primary crystallization kettle 200 and the heat exchange liquid of the secondary crystallization kettle 300, and the crystallized solid-liquid mixture enters the centrifugal assembly 500 for solid-liquid separation. Through the continuous heat transfer and the crystallization process of one-level crystallization kettle 200 and second grade crystallization kettle 300, because the heat transfer difference in temperature of one-level crystallization kettle 200 and second grade crystallization kettle 300 is less, can avoid the crystallization kettle wall bonding material, and the heat transfer difference in temperature can be adjusted, has improved crystallization kettle and to solution cooling rate, and solution crystallization time also shortens by a wide margin simultaneously to the operating efficiency of equipment has been improved.
Preferably, the liquid inlet temperature of the liquid inlet of the primary crystallization kettle is 60 +/-3 ℃, the temperature of the circulating water is 25 +/-3 ℃, and the materials are cooled to 30 +/-3 ℃ after heat exchange for a certain time and are pressed into the secondary crystallization kettle.
Further, the liquid inlet temperature of the liquid inlet of the secondary crystallization kettle is 30 +/-3 ℃, the primary crystallization kettle is cooled by using chilled water, the temperature of the chilled water is-10 +/-2 ℃, and the temperature of the material is cooled to 5 +/-2 ℃ after heat exchange for a certain time, so that a solid-liquid mixture is formed.
Specifically, in the traditional heat exchange mode, the inlet temperature of the crystallization kettle is about 60 ℃, the chilled water for exchanging heat to the crystallization kettle is only-10 ℃, the heat exchange temperature difference between the inlet temperature and the chilled water is about 70 ℃, the temperature difference is large, materials are particularly easy to adhere to the wall of the crystallization kettle, so that the heat exchange efficiency is reduced, when the final outlet temperature of 5 ℃ is reached, the heat exchange time is about 12 hours, and the materials on the kettle wall need to be manually cleaned at the same time, in the device, the mode of continuous heat exchange and crystallization of the primary crystallization kettle 200 and the secondary crystallization kettle 300 is adopted, the heat exchange temperature difference of the primary crystallization kettle 200 is 35 ℃, the heat exchange temperature difference of the secondary crystallization kettle 300 is 40 ℃, the heat exchange temperature difference is reduced, when the temperature difference is small, the materials are not easy to adhere to the wall of the crystallization kettle, the manual cleaning of the kettle wall can be effectively avoided, and simultaneously, the materials only need to reach the final outlet temperature of 5 ℃ for 5 hours, the crystallization time of the solution is greatly shortened, and the o-nitrophenol is often reacted in the reaction component 100 for about 6 hours, so that the reaction component 100 and the crystallization kettle can operate together, and the operation efficiency of the equipment is improved. In addition, the heat exchange temperature difference between the first-stage crystallization kettle 200 and the second-stage crystallization kettle 300 can be adjusted, so that the heat exchange device is suitable for different heat exchange temperatures, and the heat exchange efficiency is accelerated.
Furthermore, the ortho-aminophenol continuous crystallization device further comprises a third-stage crystallization kettle 400, wherein a liquid inlet at one end of the third-stage crystallization kettle 400 is connected with the second-stage crystallization kettle 300, the other end of the third-stage crystallization kettle 400 is connected with the centrifugal component 500, a solid-liquid mixture leaving the second-stage crystallization kettle 300 enters the third-stage crystallization kettle 400, the third-stage crystallization kettle 400 is used for standing and caching the solid-liquid mixture, the third-stage crystallization kettle 400 is arranged, and when the solid-liquid mixture is stored to a certain amount, the solid-liquid mixture is transported to the centrifugal component 500.
Preferably, the reaction assembly 100 is provided with a plurality of pairs, the plurality of pairs of reaction assemblies 100 are arranged in parallel, the liquid outlet of the reaction assembly 100 is connected with the liquid inlet of the first-stage crystallization kettle 200, and all the generated o-aminophenol solution is pressed into the first-stage crystallization kettle 200.
Further, the reaction assembly 100 includes a hydrogenation reaction kettle 210 and a secondary filter 220 connected in series in sequence, the hydrogenation reaction kettle 210 provides a reaction site for o-nitrophenol and hydrogen, a catalyst is also present in the hydrogenation reaction kettle 210, the o-nitrophenol and the hydrogen generate o-aminophenol under the action of the catalyst, and the secondary filter 220 is used for filtering the catalyst. Specifically, the second-stage filter 120 is added behind each hydrogenation reactor 110, and only filters the catalyst in the ortho-aminophenol solution, so that the catalyst can be continuously used in the hydrogenation reaction, and meanwhile, the catalyst can be filtered more effectively. Furthermore, a single secondary filter 120 may be provided for filtering the catalyst in the o-aminophenol solution generated from a plurality of hydrogenation reactors 110 simultaneously.
Preferably, the centrifuge assembly 500 includes a centrifuge 510, a dryer 520 and a mother liquor tank 530, the centrifuge 510 is used for separating solid-liquid mixture, the solid separated by the centrifuge 510 is sent to the dryer 520 for drying, and the liquid separated by the centrifuge 510 is sent to the mother liquor tank 530 for storage.
The above-mentioned embodiments are only examples of the present invention, and certainly, the scope of the present invention should not be limited thereto, and all or part of the process of implementing the above-mentioned embodiments can be understood by those skilled in the art, and the equivalent changes made according to the claims of the present invention still belong to the scope covered by the present invention.
Claims (7)
1. The utility model provides an ortho-aminophenol continuous crystallization device, its characterized in that, is including reaction unit, one-level crystallization kettle, second grade crystallization kettle and the centrifugal subassembly of establishing ties in proper order, reaction unit provides the reaction site of o-nitrophenol and hydrogen, be provided with circulating water pipe spare on the one-level crystallization kettle, circulating water that flows among the circulating water pipe spare is used for right solution among the one-level crystallization kettle carries out the heat transfer, be provided with freezing water pipe spare on the second grade crystallization kettle, freezing liquid that flows among the freezing water pipe spare is used for right solution among the second grade crystallization kettle carries out the crystallization, circulating water among the circulating water pipe spare with there is the difference in temperature between the freezing water among the freezing water pipe spare and the freezing water in the two, the centrifugal subassembly is used for carrying out solid-liquid separation to the solid-liquid mixture after the crystallization.
2. An ortho-aminophenol continuous crystallization device according to claim 1, wherein the inlet liquid temperature of the liquid inlet of the primary crystallization kettle is 60 ± 3 ℃, the temperature of the circulating water is 25 ± 3 ℃, and after heat exchange is carried out for a certain period of time, the material is cooled to 30 ± 3 ℃ and is pressed into the secondary crystallization kettle.
3. The continuous crystallization device of ortho-aminophenol according to claim 2, wherein the inlet liquid temperature of the liquid inlet of the secondary crystallization kettle is 30 ± 3 ℃, the primary crystallization kettle is cooled by using chilled water, the temperature of the chilled water is-10 ± 2 ℃, and the temperature of the material is reduced to 5 ± 2 ℃ after heat exchange for a certain time, and a solid-liquid mixture is formed.
4. The continuous o-aminophenol crystallization device according to claim 3, further comprising a third crystallization kettle, wherein a liquid inlet at one end of the third crystallization kettle is connected with the second crystallization kettle, and the other end of the third crystallization kettle is connected with the centrifugal component, and the third crystallization kettle is used for standing and buffering a solid-liquid mixture.
5. The continuous crystallization device of ortho-aminophenol according to claim 1, wherein the reaction assemblies are provided with a plurality of pairs, the plurality of pairs of reaction assemblies are arranged in parallel, and liquid outlets of the reaction assemblies are connected with liquid inlets of the first-stage crystallization kettle.
6. The continuous o-aminophenol crystallization device according to claim 5, wherein the reaction assembly comprises a hydrogenation reaction kettle and a secondary filter in series, the hydrogenation reaction kettle provides a reaction site for the o-nitrophenol and the hydrogen, a catalyst is further present in the hydrogenation reaction kettle, and the secondary filter is used for filtering the catalyst.
7. An ortho-aminophenol continuous crystallization apparatus according to claim 1, wherein the centrifugal assembly comprises a centrifuge, a dryer and a mother liquor tank, the centrifuge is used for separating a solid-liquid mixture, solids separated by the centrifuge are conveyed to the dryer for drying, and liquid separated by the centrifuge is conveyed to the mother liquor tank for storage.
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| CN202120268842.0U CN214971873U (en) | 2021-01-30 | 2021-01-30 | Ortho-aminophenol continuous crystallization device |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN117920100A (en) * | 2024-03-21 | 2024-04-26 | 佛山市华希盛化工有限公司 | High-purity ferric nitrate production system and preparation method |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN117920100A (en) * | 2024-03-21 | 2024-04-26 | 佛山市华希盛化工有限公司 | High-purity ferric nitrate production system and preparation method |
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