CN215195499U - Durene continuous freezing crystallization equipment - Google Patents
Durene continuous freezing crystallization equipment Download PDFInfo
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- CN215195499U CN215195499U CN202121047853.2U CN202121047853U CN215195499U CN 215195499 U CN215195499 U CN 215195499U CN 202121047853 U CN202121047853 U CN 202121047853U CN 215195499 U CN215195499 U CN 215195499U
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Abstract
The utility model discloses durene continuous freezing crystallization equipment in the field of chemical separation and purification equipment, which comprises a crystallization kettle, wherein one side of the crystallization kettle is connected with a cooler, the other side of the crystallization kettle is provided with a first discharge port, a guide cylinder is arranged in the crystallization kettle, a plurality of cooling coil pipes are arranged in the guide cylinder, the cooling coil pipes are contacted with the inner wall of the guide cylinder, a stirring shaft is also arranged in the guide cylinder, the lower end of the stirring shaft is connected with a stirring paddle, and the stirring shaft passes through the crystallization kettle and extends out of the crystallization kettle to be connected with a motor; the lower part of the crystallization kettle is connected with a crystal elutriation column, the lower part of the crystal elutriation column is provided with a second discharge port, the lower part of the second discharge port is provided with a centrifugal machine, one side of the centrifugal machine is provided with a centrifugal mother liquor discharge port, and the other side of the centrifugal machine is provided with a crystal discharge port. The feeding and discharging are carried out simultaneously when the equipment works, the prepared durene does not need to be cooled and heated frequently, and the equipment has the advantages of less cold loss, low energy consumption and high crystallization efficiency.
Description
Technical Field
The utility model relates to a chemical industry separation and purification equipment field, in particular to device of continuous separation durene.
Background
Durene is an important organic chemical raw material and is mainly used for producing pyromellitic dianhydride (pyromellitic dianhydride for short), the pyromellitic dianhydride is an important raw material for producing polyimide resin and films, polyimide is a new material with high temperature resistance, low temperature resistance, radiation resistance and impact resistance and excellent electrical and mechanical properties, and has important applications which cannot be replaced by other engineering plastics in the aerospace and electromechanical industries. With the increasing market usage of polyimide, durene is used as the main raw material for synthesizing the polyimide, and the demand is increasing.
The production route of durene is divided into two types, one is a chemical synthesis method, such as a pseudocumene alkylation method, a pseudodurene isomerization method or a disproportionation method; the other is a freezing crystallization method, which uses byproducts in the processing process of petroleum and coal, mainly carbon nine/carbon ten heavy aromatics as raw materials to carry out freezing crystallization, separation and purification to obtain durene. The carbon nine/carbon ten raw material contains 8-15% durene, and the distillation is enriched to the cut fraction of 190-200 ℃. The said fraction is a mixture of durene and its homologues, and the durene and durene have high contents and similar boiling points, and can not be separated by means of rectification, but the solidifying point of durene pure product is up to 72 deg.C, while the solidifying point of durene pure product is-24 deg.C, and the durene pure product is-60 deg.C, and the durene is separated by means of freezing crystallization and centrifugal separation. In order to further improve the purity of durene, a squeezer is adopted for extrusion operation, and the purity of the extracted durene can reach more than 99 percent.
Chinese patent CN103524288B (published japanese: 2015.11.25) discloses a durene purification method, wherein durene solution is fed into a freezing crystallizer for freezing crystallization, cooling medium is fed into the freezing crystallizer and discharged from the freezing crystallizer to obtain a cold source, and durene crystals containing crystallization mother liquor are obtained after freezing crystallization; and separating the crystallization mother liquor by using a centrifugal separation device to obtain the crystallization mother liquor and a centrifuged solid product, squeezing the solid product by using a squeezer to obtain a durene product and squeezed crystallization mother liquor.
Chinese patent CN206014724U (published: 2017.03.15) discloses a device for separating durene by freezing crystallization, which comprises a solid-liquid separation tank, a filtrate concentration tank and a melting tank connected with the bottom of the solid-liquid separation tank, a rectification column a connected with the filtrate concentration tank, a rectification column B connected with the melting tank, a rectification column C connected with the rectification column B, a flaker connected with the rectification column C, and a storage tank connected with the flaker.
Chinese patent CN208406149U (published: 2019.01.22) discloses a device for separating durene by freezing crystallization, which comprises a first crystallizing tank, wherein one side of the first crystallizing tank is communicated with an oil liquid separating device, one side of the oil liquid separating device is communicated with an oil storage tank, a connecting end of the first crystallizing tank is provided with a middle tank, a connecting end of the middle tank is provided with a distilling pot, connecting ends of the middle tank and the distilling pot are provided with second crystallizing tanks, and liquid through cavities are arranged inside the first crystallizing tank and the second crystallizing tanks. The utility model discloses a be equipped with fluid separator, let in the separation casing with the oily solution, get access to the closure plate after holding back through the sieve with the impurity in the solution, utilize the proportion difference of solution and fluid to carry out continuous collision and carry out accelerated motion, realize the reposition of redundant personnel and the layering of solution, the motor drives the puddler work and stirs solution, and solution carries out the layering according to the density difference, with the oil body by the oil-out discharge, reaches simple efficient separation process, improves the purity of durene crystallization.
The operation mode of the cooling crystallization equipment in the prior art is mostly an intermittent process, and the main equipment of the intermittent freezing crystallization process comprises a refrigerator, a heat exchanger, a crystallization settling kettle and a solid-liquid centrifuge. During operation, the material is thrown into a crystallization and sedimentation kettle, the material in the kettle is cooled to-20 ℃ through a refrigerator and a heat exchanger to crystallize and separate durene, and then the durene is transferred into a centrifuge to separate mother liquor to obtain solid durene. Due to the adoption of intermittent production, the problems of frequent temperature reduction and rise, serious loss of cold energy, high energy consumption and low crystallization efficiency exist.
SUMMERY OF THE UTILITY MODEL
The utility model aims at overcoming not enough among the prior art, providing a durene continuous freezing crystallization equipment, its during operation feeding ejection of compact goes on simultaneously, and the durene of preparation need not frequently to cool down and heaies up, has that cold volume loss is few, the energy consumption is low and crystallization efficiency is high advantage.
The purpose of the utility model is realized like this: a durene continuous freezing crystallization device comprises a crystallization kettle, wherein one side of the crystallization kettle is connected with a cooler, the other side of the crystallization kettle is provided with a first discharge port, a guide cylinder is arranged in the crystallization kettle, a plurality of cooling coils are arranged in the guide cylinder, the cooling coils are in contact with the inner wall of the guide cylinder, a stirring shaft is further arranged in the guide cylinder, the lower end of the stirring shaft is connected with a stirring paddle, and the stirring shaft penetrates through the crystallization kettle and extends out of the crystallization kettle to be connected with a motor; the lower part of the crystallization kettle is connected with a crystal elutriation column, a second discharge port is arranged at the lower part of the crystal elutriation column, a centrifugal machine is arranged at the lower part of the second discharge port, a centrifugal mother liquid discharge port is arranged at one side of the centrifugal machine, and a crystal discharge port is arranged at the other side of the centrifugal machine.
The utility model discloses a durene continuous refrigeration plant during operation, the feed liquid after the cooler cooling flows in the crystallization kettle in succession through the draft tube lower part in, and the stirring rake rotates and mixes the feed liquid from top to bottom, and the in-process that the feed liquid rises continues to cool off, reaches the oversaturated state, forms freezing crystallization and subsides, through centrifuge centrifugal separation, obtains durene crystal. The beneficial effects of the utility model reside in that: the continuous crystallization device has the advantages of replacing the intermittent crystallization operation of feeding and discharging of a crystallization kettle and cooling in the kettle in the prior art, stabilizing the feeding and discharging and cooling processes, effectively ensuring the continuity and stability of the product quality, continuously adding the materials to be crystallized and continuously taking out the crystallizer products from the crystallizer, simultaneously feeding and discharging, and preparing durene without frequent temperature reduction and temperature rise, has the advantages of less cold loss, low energy consumption and high crystallization efficiency, and is suitable for the continuous freezing crystallization operation in the durene production process.
Furthermore, a plurality of baffles are arranged between the inner wall of the crystallization kettle and the guide cylinder, the baffles and the stirring paddle form a circulating flow cavity of the crystal slurry mixture in the crystallization kettle. The crystal slurry mixture flows up and down in the crystallization kettle under the action of the stirring paddle, and substances in the crystallization mixture continuously collide on the baffle plate to generate acceleration, so that solid and liquid are separated, and heavier liquid and lighter liquid are layered.
Furthermore, a settling zone is arranged between the baffle and the inner wall of the lower part of the crystallization kettle, and large-particle crystals are gathered at the settling zone to provide a buffer zone for the falling of the crystals.
Furthermore, a circulating pipe is arranged in the cooler, an outlet at the lower part of the circulating pipe is connected with the lower part of the guide cylinder through a feeding pipe, a pump is arranged on the feeding pipe, saturated liquid materials are continuously added to the lower part of the circulating pipe through the pump, the saturated liquid materials are mixed with mother liquid with small crystals clamped in the circulating pipe and then are pumped to the cooler, and the cooled liquid materials flow into the crystallizer through the lower part of the guide pipe.
Furthermore, one end of the lower part of the crystallization kettle, which is connected with the elutriation column, is conical, and the conical structure is favorable for liquid materials to flow downwards.
Further, the second discharge gate is wide from top to bottom narrow leaks hopper-shaped, is favorable to the feed liquid to pass through fast.
Drawings
FIG. 1 is a schematic structural view of a durene continuous freezing and crystallizing device of the present invention.
In the upper drawing, 1 a cooler, 2 a motor, 3 a crystallization kettle, 4 a guide cylinder, 5 a baffle, 6 a first discharge port, 7 a cooling coil, 8 an elutriation column, 9 a second discharge port, 10 a centrifugal machine, 11 a centrifugal mother liquor discharge port, 12 a pump, 13 a crystal discharge port and 14 a circulating pipe.
Detailed Description
As shown in fig. 1, a durene continuous freezing crystallization device comprises a crystallization kettle 3, one side of the crystallization kettle 3 is connected with a cooler 1, the other side is provided with a first discharge port 6, a draft tube 4 is arranged in the crystallization kettle 3, a plurality of cooling coils 7 are arranged in the draft tube 4, the cooling coils 7 are in contact with the inner wall of the draft tube 4, a stirring shaft is also arranged in the draft tube 4, the lower end of the stirring shaft is connected with a stirring paddle, and the stirring shaft passes through the crystallization kettle 3 and extends out of the crystallization kettle 3 to be connected with a motor 2; the lower part of the crystallization kettle 3 is connected with a crystal elutriation column 8, the lower part of the crystal elutriation column 8 is provided with a second discharge hole 9, the lower part of the second discharge hole 9 is provided with a centrifuge 10, one side of the centrifuge 10 is provided with a centrifugal mother liquid discharge hole 11, and the other side is provided with a crystal discharge hole 13.
A plurality of baffles 5 are arranged between the inner wall of the crystallization kettle 3 and the guide cylinder 4, the baffles 5 and the stirring paddle form a circulating flow cavity of the crystal slurry mixture in the crystallization kettle 3. The crystal slurry mixture flows up and down in the crystallization kettle 3 under the action of the stirring paddle, and the crystallization mixture continuously collides on the baffle 5 to generate acceleration, so that the solid and the liquid are separated, and the heavier liquid and the lighter liquid are layered.
A settling zone is arranged between the baffle 5 and the inner wall of the lower part of the crystallization kettle 3, crystal particles are gathered at the settling zone, and a buffer zone is provided for the falling of the crystals.
A circulating pipe 14 is arranged in the cooler 1, an outlet at the lower part of the circulating pipe 14 is connected with the lower part of the guide cylinder 4 through a feeding pipe, a pump 12 is arranged on the feeding pipe, saturated liquid materials are continuously added to the lower part of the circulating pipe 14 through the pump 12, the saturated liquid materials are mixed with mother liquid with small crystals in the circulating pipe 14 and then sent to the cooler 1 through the pump 12, and the cooled liquid materials flow into the crystallization kettle 3 through the lower part of the guide cylinder 4.
The lower part of the crystallization kettle 3 is connected with one end of the crystal elutriation column 8 and is conical, and the conical structure is beneficial to downward flow of liquid materials.
The second discharge hole 9 is funnel-shaped with wide top and narrow bottom, which is beneficial to the rapid passing of the feed liquid.
The utility model is in operation, the feed liquid to be cooled flows into the cooler 1, the circulating pipe 14 is arranged in the cooler 1, the feed liquid is cooled in the circulating pipe 14 by the reciprocating flow, the saturated feed liquid after cooling flows into the crystallization kettle 3 at the bottom of the draft tube 4 through the inlet pipe, the stirring shaft rotates under the drive of the external motor 2 to lift the feed liquid upwards from the bottom of the draft tube 4, the feed liquid circularly flows between the draft tube 4 and the baffle 5, the feed liquid is continuously cooled in the rising process to reach the supersaturation state, part of solute is deposited on the surface of suspended particles to grow the crystals, the continuous collision of the material in the feed liquid on the baffle 5 is accelerated to separate the crystals from the liquid, the heavier liquid and the lighter liquid are layered, the lighter clear liquid at the upper layer is discharged through the first discharge port 6, the rest feed liquid is settled in the settling area at the periphery of the baffle 5, the large crystal particles are gathered, the mixed mother liquor enters an elutriation column 8, in order to ensure that the granularity of a crystallized product is as uniform as possible, partial mother liquor from a settling zone is added to the bottom of the elutriation column 8, crystals with small particles return to a crystallization kettle 3 along with the solution for recrystallization by utilizing the fluid classification effect, and are finally discharged from the lower part of the elutriation column 8 and enter a centrifugal machine 10 for centrifugal separation, the centrifugal mother liquor is discharged from a centrifugal mother liquor discharge port 11, and durene crystals are discharged from a crystal discharge port 13 and collected.
The continuous operation process that waiting to crystallize the material in this device adds in succession, crystallization product takes out in succession from crystallization kettle 3, and feeding and ejection of compact go on simultaneously, and the durene of preparation need not frequently to lower the temperature and heat up, has the advantage that cold volume loss is few, the energy consumption is low and crystallization efficiency is high, is applicable to the continuous freezing crystallization operation in the durene production process.
The present invention is not limited to the above embodiments, and based on the technical solutions disclosed in the present invention, those skilled in the art can make some replacements and transformations for some technical features without creative labor according to the disclosed technical contents, and these replacements and transformations are all within the protection scope of the present invention.
Claims (6)
1. The utility model provides a durene continuous freezing crystallization equipment, includes the crystallization kettle, its characterized in that: one side of the crystallization kettle is connected with a cooler, the other side of the crystallization kettle is provided with a first discharge hole, a guide cylinder is arranged in the crystallization kettle, a plurality of cooling coils are arranged in the guide cylinder, the cooling coils are contacted with the inner wall of the guide cylinder, a stirring shaft is also arranged in the guide cylinder, the lower end of the stirring shaft is connected with a stirring paddle, and the stirring shaft penetrates through the crystallization kettle and extends out of the crystallization kettle to be connected with a motor; the lower part of the crystallization kettle is connected with a crystal elutriation column, a second discharge port is arranged at the lower part of the crystal elutriation column, a centrifugal machine is arranged at the lower part of the second discharge port, a centrifugal mother liquid discharge port is arranged at one side of the centrifugal machine, and a crystal discharge port is arranged at the other side of the centrifugal machine.
2. The tetramethylbenzene continuous freezing crystallization apparatus according to claim 1, characterized in that: and a plurality of baffles are arranged between the inner wall of the crystallization kettle and the guide cylinder, the baffles and the stirring paddle form a circulating flow cavity of the crystal slurry mixture in the crystallization kettle.
3. The durene continuous freezing crystallization device according to claim 2, characterized in that: and a settling zone is arranged between the baffle and the inner wall of the lower part of the crystallization kettle.
4. The durene continuous freezing crystallization device according to claim 1, characterized in that: the cooler is internally provided with a circulating pipe, an outlet at the lower part of the circulating pipe is connected with the lower part of the guide cylinder through a feeding pipe, and the feeding pipe is provided with a pump.
5. The durene continuous freezing crystallization device according to claim 1, characterized in that: one end of the lower part of the crystallization kettle, which is connected with the elutriation column, is conical.
6. The durene continuous freezing crystallization device according to claim 1, characterized in that: the second discharge gate is wide at the top and narrow at the bottom leaks hopper-shaped.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202121047853.2U CN215195499U (en) | 2021-05-17 | 2021-05-17 | Durene continuous freezing crystallization equipment |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202121047853.2U CN215195499U (en) | 2021-05-17 | 2021-05-17 | Durene continuous freezing crystallization equipment |
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| CN215195499U true CN215195499U (en) | 2021-12-17 |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN116492700A (en) * | 2023-06-30 | 2023-07-28 | 上海中腾环保科技有限公司 | Graded flash evaporation equipment and process |
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2021
- 2021-05-17 CN CN202121047853.2U patent/CN215195499U/en active Active
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN116492700A (en) * | 2023-06-30 | 2023-07-28 | 上海中腾环保科技有限公司 | Graded flash evaporation equipment and process |
| CN116492700B (en) * | 2023-06-30 | 2023-09-12 | 上海中腾环保科技有限公司 | Graded flash evaporation equipment and process |
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